CN1468063A - Product containing corn oil and corn meal obtained from high oil corn - Google Patents

Abstract

Corn oil and corn meal from high oil corn are useful products. Corn oil is extracted from high oil corn to produce corn meal. Since most or all of the corn kernel, not just the germ, is used in the extraction process, this corn oil typically contains nutritional levels not found in commercially available corn oil. Such corn kernels typically include the steps of flaking corn kernels having a total oil content of at least about 6 wt.% and extracting corn oil from the flaked corn kernels. Such corn oil is useful for making nutritionally enhanced edible or cooking oils, lubricants, biodiesel, dyes, cosmetics, and oil-based or oil-containing chemical products. The extracted corn meal is also useful for making improved animal feed rations, snacks, blended food products, cosmetics, and fermentation broth additives.

Description

Products containing corn oil and corn meal obtained from high-oil corn

field of invention

The present invention relates to products from oil and meal extracted from corn having an oil content of about 6 wt.% or higher.

Background of the invention

Maize, Zea Mays L., is grown for many reasons, including its use in food and industry. Corn oil and corn flour are two of the useful products derived from corn.

Commercial refiners that extract corn oil from conventional corn by conventional methods separate the corn seed into its constituent parts, such as endosperm, germ, tipcap, and epidermis, and then extract corn oil from the corn germ fraction. Corn germ produced by wet or dry milling is either pressed to remove the oil or the germ is flaked and the oil is extracted with a solvent. In both methods, since the germ is separated from the remainder of the corn kernel, most or all of the valuable components of the endosperm portion are absent from the oil.

The corn-based feed product known as corn feed is obtained by dry milling and is a mixture of corn bran, corn germ and endosperm with a minimum of 4% oil. The manufacture of corn feed requires steps including crushing, grinding, sieving, and blending, resulting in a particle size of corn feed that is smaller than that of corn flour produced by the extraction process described herein.

Since products made with conventional corn lack certain essential nutrients, industry and health advocates have been searching for more nutritious corn-derived products. Accordingly, there is a need for improved products from corn oil and corn flour.

Summary of the invention

End products from conventional corn containing corn oil and/or corn flour include, for example, cooking oils, animal feed, paper and paper products, various food products such as salad dressings, pressed and/or puffed snacks, products containing corn syrup , cornflakes, chips, puddings, cakes and breads.

In one aspect of the present invention there is provided a nutritious animal feed comprising cornmeal remaining after extraction of oil from high oil corn having an oil content of about 6 wt. % or greater. The animal feed may also contain other nutritional ingredients such as vitamins, minerals, oilseed derived meal, meat and bone meal, salt, amino acids, feather meal and many others used in the field of feed supplements. The animal feed composition can be used for special purposes, such as poultry feed, pig feed, cattle feed, horse feed, aquaculture feed, pet food, and can be used for the growth stage of the animal. Particular embodiments of animal feeds include growing chicken feeds, finishing feeds for pigs and finishing feeds for poultry laying eggs. Oil-extracted corn meal can be used to make feed products that contain a relatively higher proportion of protein and a relatively lower proportion of oil than similar products made from conventional corn.

Some embodiments of the invention include: 1) cornmeal having a fiber content of about 3%, a starch content of about 65%, a protein content of about 12%, and a moisture content of about 10%; 2) the total oil content of high oil corn kernels The content is at least about 6wt.%, at least about 7wt.%, at least about 8wt.%; at least about 10wt.%; at least about 12wt.%; at least about 14wt.%; or from about 7wt.% to About 30wt.%; 3) The corn kernels that are compressed are whole corn kernels or broken corn kernels; 4) The corn kernels are used in oil extraction processes such as solvent extraction, hydraulic or screw pressing, aqueous solution and enzyme extraction; 5) the total protein content of high oil corn kernels is at least about 7wt.%, at least about 9wt.%, at least about 11wt.%, or from about 7% to about 20wt.%; 6) the total protein content of high oil corn kernels The lysine content is at least about 0.15wt.%, at least about 0.5wt.%, or from about 0.25wt.% to about 2.0wt.%; and/or 7) the total tryptophan content of high oil corn kernels is at least About 0.03 wt.%, at least about 0.20 wt.%, or from about 0.03 wt.% to about 2.0 wt.%.

A preferred embodiment provides a method for obtaining corn oil and solvent extracted corn meal (SEC) from high oil corn. The method includes the steps of: 1) softening the corn; 2) cracking the softened corn; 3) wetting the cracked corn; 4) flaking the moistened corn; 5) extracting the flaked corn; and 6) The solvent is removed from the corn oil and the corn flour is extracted with the solvent. This method provides a higher total corn oil and also increases the protein content of the cornmeal. In addition, solvent-extractable pigments can be removed from SEC.

Another aspect of the present invention is to provide a corn oil-based product containing corn oil obtained by extracting at least endosperm and germ of high oil corn. This corn oil-based product may contain other ingredients such as vinegar, spices, vitamins, salt, hydrogen to form hydrogenated products, and water. The corn oil used in the products of the present invention generally contains a higher proportion of beta-carotene, lutein or tocotrienols than products obtained from corn oil extracted from conventional corn by conventional methods. The corn oil used in the products of the present invention is generally prepared by using whole corn kernels, cracked corn kernels or flaked corn kernels for extraction without separating the germ from the endosperm. Thus, the solvent-extractable nutrients in the endosperm are extracted into the corn oil extracted from the germ and endosperm. Products that can be made from oils prepared by the methods described herein include, but are not limited to, salad dressings, cooking oils, margarines, food or feed sprays, bread, pancakes, snacks, lubricants, and fuel.

Other embodiments of the invention include: 1) the high oil corn kernels are crushed, moistened, flaked and solvent extracted; 2) the high oil corn kernels have a total oil content of at least about 6 wt.%, at least about 7 wt.%, at least about 8 wt.%; at least about 10 wt.%; at least about 12 wt.%; at least about 14 wt.%; or from about 7 wt.% to about 30 wt.%; 3) corn oil is crushed by extrusion 4) corn oil is extracted by subjecting flaked corn kernels to a solvent-based extraction process; 5) solvents used to extract miscible or soluble substances from the flaked kernels include any form of Commercially available hexane, isopropanol, ethanol, supercritical carbon dioxide, or mixtures thereof; 6) the extracted oil is given as an oil and solvent mixture; 7) corn oil is refined by other methods; and 8) Corn oil is extracted by subjecting flaked corn kernels to hydraulic and/or screw pressing, aqueous and/or enzymatic extraction.

In a third aspect of the present invention there is provided a method of using expressed corn meal in an animal feed ration comprising: 1) flaking at least high oil corn to produce flaked corn and extracting the flaked corn to obtain removing a portion of the corn oil thereby providing an extracted corn meal; and 2) using the extracted corn meal in animal feed rations.

A fourth aspect of the present invention is to provide a method of using extracted corn oil in food, comprising: 1) flaking at least high oil corn to produce flaked corn, extracting the flaked corn to remove a portion of the corn oil and forming extracted corn oil, thereby providing extracted corn oil; and 2) using the extracted corn oil in food products.

In a fifth aspect of the present invention there is provided a method of using extracted corn oil as a feedstock in an oil refining process. The method comprises the steps of: 1) flaking at least high oil corn to produce flaked corn, extracting the flaked corn to remove a portion of the corn oil and form extracted crude corn oil, thereby providing the extracted crude corn oil; and 2) use of the extracted crude corn oil as a feedstream to an oil refining process.

The sixth aspect of the present invention is to provide various methods of manufacturing the oil-expressed mixed flour. A first embodiment of this aspect provides a method of making an expressed mixed meal, including an expressed meal obtained from high oil corn and one or more other oilseed meals. This method includes the steps of: 1) combining high oil corn kernels and one or more other oilseed particles to form a pellet mixture; Mix powder with oil. A second embodiment provides a method comprising the steps of: 1) combining cracked and wetted high oil corn with cracked and wetted other oilseeds to form a wetted mixture; 2) combining the wetted and 3) tableting the granule mixture and using it in an extraction process to remove the oil therein and form an oil-expressed blended powder. A third embodiment provides a method comprising the steps of: 1) combining cracked, moistened, and flaked high oil corn and cracked, moistened, and flaked other oilseeds to form a flaking mixture; and 2 ) The granule mixture is compressed and used in an extraction process to remove the oil therein and form an oil-expressed blend. A fourth embodiment provides a method comprising the step of combining expressed corn flour and one or more other oilseed flours to form a blended meal, wherein the expressed corn flour is obtained by At least that obtained by flaking high-oil corn and extracting it to form pressed corn meal. A fifth embodiment provides a blended expressed meal product made by any of the methods described above.

A seventh aspect of the present invention is to provide a method of using extracted corn oil as a cosmetic ingredient. The method comprises the steps of: 1) flaking at least high oil corn to produce flaked corn, extracting the flaked corn to remove a portion of the corn oil and form extracted crude corn oil, thereby providing the extracted crude corn oil; and 2) use of extracted crude corn oil in cosmetic products. These beauty products include, but are not limited to, lipsticks and eyeliners.

Another aspect of the present invention provides the use of cornmeal obtained after extraction of corn oil from whole kernels of high oil corn for animal feed or human food.

Another aspect of the present invention provides the application of corn oil in animal feed or human food, wherein the corn oil is obtained by extracting whole grains of high-oil corn.

In other aspects of the invention there are provided corn oil-containing and/or corn flour-containing products produced by the methods described herein.

Unless defined otherwise, all technical and scientific terms and abbreviations used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice of the present invention, it is not intended that such methods and materials limit the invention described herein. All patent applications and formal analytical methods mentioned herein are hereby incorporated by reference in their entirety. Other features and advantages of the present invention will be apparent from the following description of the exemplified embodiments of the invention and from the claims.

Brief description of the drawings

Figure 1 shows the total amount of ethanol production and glucose consumption by yeast grown on yellow dent corn (YD), yellow dent corn meal (YDM), high oil corn (HOC) and high oil corn meal (HOCM).

Figure 2 shows the pH of yeast cultures containing yellow dent corn (YD), yellow dent corn meal (YDM), high oil corn (HOC) and high oil corn meal (HOCM).

Detailed description of the invention

It is known that corn oil can be rapidly and efficiently extracted from oily corn kernels on an industrial scale by optionally crushing the kernels, rewetting and flaking, and extracting the corn oil. The total oil content of corn kernels effective to the new flaking treatment is greater than about 6 wt.%. Increased oil content in corn kernels can increase the efficiency of flaking during processing. Suitable tableting apparatus and methods include those conventionally used for tableting soybeans and other similar oilseeds. Suitable extraction devices and methods include those conventionally used to extract oil from soybean flakes and other similar oilseeds.

High oil corn seeds or "pellets" obtained from any of several different types of corn plants are useful in the present invention. Such maize plants may be hybrids, selfed, transgenic plants, genetically modified plants or plants of a specific population. An improved extracted meal can be produced by using the improved high oil corn in the extraction process described herein. Useful types of corn kernels include, for example, hard corn, popcorn, flour corn, dent corn, white corn, and sweet corn. High oil corn kernels may be in any form, including whole corn, cracked corn, or other processed corn or parts thereof, which are capable of flaking but differ from the germ separation used in dry and wet milling methods Standard method for subsequent oil recovery from germ.

As used herein, the term "whole kernel" or "whole corn" means that the kernel has not been separated into individual components, eg, the outer shell, endosperm, terminal bud, pericarp and germ have not been purposely separated from one another. Whole corn may or may not be ground, crushed, cracked, flaked or ground. Purposeful separation of one corn component from other components does not include random segregation that may occur during storage, handling, transportation, crushing, flaking, breaking, grinding, or grinding. Purposeful separation of components means at least 50% separation of a certain component (eg germ) from other components.

The term "high oil corn" as used herein refers to corn kernels containing at least about 6 wt.% or higher, preferably at least about 7 wt.% or higher, most preferably at least about 8 wt.% or higher oil . High oil corn has a higher oil content than conventional yellow dent corn which has an oil content of about 3 wt.% - 5 wt.%. Additionally, the total oil content of corn kernels suitable for the present invention can be, for example, an oil content of at least about 9 wt.%, at least about 11 wt.%, at least about 12 wt.%, at least about 15 wt.%, at least about 18 wt.%, at least about 20 wt.%, about 8 wt.% to about 20 wt.%, about 10 wt.% to about 30 wt.%, about 14 wt.% to about 30 wt.%, and particles within these ranges. Although oil content can be determined at any moisture content, it should be corrected to the oil content at approximately 15.5% moisture.

High oil corn useful for making oils and meals described here is available from Cargill, Inc. (Minneapolis, Minnesota) or Pfister Hybrid Corn (El Paso, Illinois). Other suitable high oil corns include the varieties known as Illinois High Oil Corn (IHO) and Alexander High Oil Corn (Alexo), available from the University of Illinois Maize Cooperative Stock Center (Urbana, Illinois) to obtain samples of them.

Corn kernels with increased total oil content can be identified by any of a number of methods known to those of ordinary skill in the art. The American Oil and Chemical Society Official Method, Fifth Edition, March 1998, ("AOCS Method Ba 3-38") may be used to identify the oil content of corn kernels, including the fat content of corn flour extracted from corn kernels. AOCS method BA3-38 quantifies the substances extracted with petroleum ether under the test conditions. Oil content or oil concentration is the weight percent of oil relative to the total weight of the seed sample. Oil content can be corrected and recorded at any desired moisture condition.

Other suitable methods for identifying high oil corn kernels are described herein. According to one of these methods, ears of corn are sorted with a near infrared (NIR) oil detector to select ears of corn containing corn kernels with increased oil content. Likewise, NIR detectors can also be used to select individual kernels with elevated corn oil levels. However, the selection of corn ears and/or kernels with increased oil content cannot inexpensively identify high oil kernels suitable for processing using the methods described herein. Generally, corn seed that produces corn plants that produce corn kernels having an increased total oil content is planted and harvested using known harvesting methods. Methods for developing maize selfing, hybrid, transgenic varieties and populations that produce maize plants capable of producing corn kernels with increased oil content are known and described in Lambert [Specialty Corns, CRC Publishing Company, Bibl. Clayton, FL, pp. 123-145 (1994)].

A suitable high oil corn used as a feedstock in the present invention to prepare corn oil and corn meal has the nutritional properties shown in Table 1. Values are expressed as "as is" or "as fed" moisture levels. Protein, oil and starch levels vary among the many possible combinations of high oil corn used in this invention as a feedstock for producing meal and oil. Table 1 lists acceptable amounts of moisture, oil, protein, starch, lysine, and tryptophan. However, other combinations not shown as indicated amounts in the table, such as 12 wt.% protein and 12 wt.% oil, are also within the scope of corn kernels that can be used to make oils and meals for use in the present invention.

Table 1. Element Content1(wt.%) Content 2 (2wt.%) Content3(wt.%) Average content (wt.%) moisture 14 14 14 5-45 Oil 8 12 20 6-30 protein 9 9 17 5-20 starch 61 54 41 35-80 Lysine 0.35 0.50 1.0 0.15-2.0 Tryptophan 0.088 0.11 0.15 0.03-2.0

Other corn kernels suitable for use as feedstock to make the corn oil and corn meal used in the present invention have the nutritional characteristics shown in Table 2. Values are expressed as "as is" or "as fed" moisture levels. The values shown in Table 2 are exemplified for corn kernels containing 12 wt.% oil and 9 wt.% protein.

Table 2. Element Content (wt.%) Average content (wt.%) moisture 14 5-45 Oil 12 6-30 protein 9 5-20 starch 65 35-80 fiber 3 1-5 Ash 1.18 0.59-4.72 Lysine 0.33 0.2-2.0 Tryptophan 0.09 0.03-2.0 Methionine 0.25 0.13-1.00 total sulfur amino acids 0.46 0.23-1.84 Valine 0.45 0.23-1.80 Isoleucine 0.34 0.17-1.36 arginine 0.45 0.23-1.80 threonine 0.34 0.17-1.36 Leucine 1.03 0.52-4.12 Histidine 0.27 0.14-1.08 Phenylalanine 0.44 0.22-1.76 Alanine 0.70 0.35-2.80 aspartic acid 0.74 0.37-2.96 cysteine 0.22 0.11-0.88 glutamic acid 1.9 0.95-7.6 Glycine 0.46 0.23-1.84 proline 0.86 0.43-3.44 Tyrosine 0.06 0.03-0.54 serine 0.46 0.23-1.84

Table 3 shows the amino acid levels (based on kernels with approximately 10% moisture) for two samples of high oil kernels and normal yellow kernels. The oil and protein levels of high oil corn sample 1 (HOC 1 ) were 13.3 wt.% and 10.7 wt.%, respectively, expressed on a dry matter basis. The oil and protein levels of High Oil Corn Sample 2 (HOC 2) were 13.0 wt.% and 11.2 wt.%, respectively, expressed on a dry matter basis. For comparison, common yellow corn kernels contain about 4.2 wt.% oil and about 9.2 wt.% protein on a dry matter basis.

table 3. amino acid HOC 1(%) HOC 2(%) Yellow corn (%) aspartic acid 0.71 0.68 0.48 threonine 0.33 0.30 0.19 serine 0.37 0.27 0.19 glutamic acid 1.84 1.79 1.16 proline 0.83 0.78 0.52 Glycine 0.40 0.42 0.24 Alanine 0.77 0.74 0.47 Valine 0.51 0.52 0.33 cystine 0.21 0.23 0.16 Methionine 0.46 0.47 0.39 Isoleucine 0.30 0.30 0.20 Leucine 1.19 1.08 0.74 Tyrosine 1.11 0.11 0.06 Phenylalanine 0.52 0.47 0.32 Tryptophan 0.06 0.07 0.05 Lysine 0.34 0.38 0.21 Histidine 0.29 0.29 0.18 arginine 0.45 0.48 0.28

High oil corn is typically used in the oil extraction process described herein to provide the enhanced corn oil and corn meal contained in the final product of the present invention. The term "end product" or "product" as used herein refers to the technique or product of combining the corn oil and/or corn flour of the present invention with various other ingredients. The exact ingredients contained in the product will be determined by the end use of the product. Exemplary products include animal feed, chemically modified raw materials, biodegradable plastics, mixed food products, edible oils, cooking oils, lubricants, biodiesel, snacks, cosmetics, and raw materials for fermentation processes. Products include the foods described here, but also grown or partially grown pig, poultry and cattle feed, pet food and human food such as extruded snacks, bread and as food binders, aquaculture feed, fermented compounds, Food additives, sports drinks, nutritional food bars, multivitamin supplements, diet drinks and cornflakes.

For example, starting with one corn type (eg, containing 12 wt.% oil and 9 wt.% protein), multiple types of corn flour can be made that can meet certain nutritional requirements. The importance of this adaptation lies in the nutrient density in the feed product and the dietary needs of the animal. One advantage of using this type of high oil corn and extraction method is that the extracted corn meal can be made to have a specific oil content depending on the degree of oil extraction. Once the oil is removed from the flakes, the remaining cornmeal contains a nutrient concentration of protein, amino acids, and other nutrients not removed by processing that is greater than or different than that of regular corn kernels and greater than that of the starting corn, e.g., 12 wt. .% oil and 9 wt.% protein.

According to an extraction process described herein for use in the manufacture of corn oil and corn meal, whole high oil corn kernels are optionally softened, optionally broken, and then moistened and flaked. After flaking, the flaked corn was extracted for oil as described here.

Whole corn may optionally be softened prior to the extraction process. The term "softening" is used herein interchangeably with the terms "heat soaking" or "steaming" and refers to allowing added moisture to be evenly distributed throughout the corn kernel. Any softening method known in the art can be used. Generally, the corn is soaked in a suitable amount of water for any suitable period of time, such as at least 20 minutes, preferably at least 4 hours, more preferably at least 12 hours, most preferably at least 24 hours. After the corn has been steeped for the desired time, its moisture content is determined. Corn can be stored for short periods of time, but is better processed within 24 hours, preferably immediately.

Whole kernels may optionally be broken. In a preferred embodiment, whole high oil corn is cracked after softening but before moistening. pass the whole kernel of corn through two rollers with corrugated teeth rotating in opposite directions with a certain amount of porosity, and/or through a grinder (in which a rotating toothed disk rotates at a certain distance from a fixed disk), and/or Or use a hammer mill (in which two rotating metal "hammers" rotate the units one after the other so that high-oil corn is broken. The method of breaking corn or high-oil corn kernels is described in Watson, S.A. & P.E. Ramstad ed. Corn : Chemistry and Technology Chapter 11 (1987, American Association of Cereal Chemist Inc., St. Paul, MN), which is hereby incorporated by reference. "Cracked" corn is corn that has undergone the crushing process described above.

Whether the corn is broken or not, it can be moistened by methods known to those of ordinary skill in the art or as described herein. The term "wetting" as used herein refers to the process by which corn kernels are softened or plasticized to make them easier to flake and extract. Wetting may include adding steam (saturated and/or unsaturated steam) and/or water to the high oil corn. This is done using a rotary adjuster. During the addition of steam, both temperature and moisture are increased. The temperature ranges from about 140°F to 210°F, with a moisture increase of about 1% or about 15%.

The high oil corn kernels are then pressed into various useful sizes. The term "flaking" as used herein refers to a process in which corn kernels are passed one or more times through a flaking roller to produce flakes. The final thickness of the flaked corn is about 5/1000-100/1000 inch (about 0.12 mm-2.0 mm) or preferably about 0.01 inch (0.25 mm), although other thicknesses can also be used. Useful flake thicknesses depend on external limiting parameters such as the oil content of the corn, the moisture content, the type of corn (eg, dent or hard corn), and the type of oil press. Suitable methods for flaking high oil corn are detailed here and in D.R. Erickson, Practical Handbook of Soybean Processing Utilization (1995, AOCS Press), which is hereby incorporated by reference. Suitable tabletting methods also include those known to those of ordinary skill in the art of oilseed processing.

After the corn is softened, cracked and/or moistened and flaked, the flaked corn is used in an oil extraction process to extract the oil to form oil extracted corn meal (ECM). Corn oil is extracted from the flaked pellets by one or more extraction steps by any extraction method. Usually, all or nearly all of the oil is extracted in one oil extraction process. Useful oil expression methods include solvent extraction, continuous solvent extraction, hydraulic pressing, screw pressing, aqueous and/or enzymatic extraction, and the like. Effective solvents for solvent extraction include, for example, all forms of commercially available hexane, isopropanol, ethanol, supercritical carbon dioxide, combinations thereof, or other similar solvents. For example, corn oil can be extracted from flaked granules using a hexane-based solvent extractor. Solvent extractors include osmotic and immersion types of extractors. In a preferred embodiment, the continuous solvent extraction process maintains the flaked corn in contact with the solvent for at least 10 minutes, preferably at least 30 minutes, more preferably at least 60 minutes, and most preferably at least 90 minutes.

Materials removed from solvent-based extractors include wet flakes and miscellaneous oils. Trash oil is a mixture of raised oils and solvents. Wet flakes are the material that remains after partial or total extraction of solvent-soluble material. Wet flakes also contain a certain amount of solvent. Solvent recovery from miscellaneous oils and wet flakes by methods such as rising film evaporation or drying and elevated temperatures with flash tanks and/or desolventizers/ovens etc. For example, wet flakes or miscellaneous oils are heated under atmospheric pressure, high pressure or vacuum to evaporate the solvent. The evaporated solvent is then condensed and optionally dewatered in a separate recovery system before being recycled back to the extractor.

Trash oil after solvent removal is generally referred to as crude oil, which can be stored and/or further processed. Crude oils can be refined into final product oils. Methods of refining crude oils to obtain product oils are known to those of ordinary skill in the art. Hui (1996) provides a detailed review of oils and oilseeds (Bailey's Industrial Oil and Fat Products, Fifth Edition, Volume 2, Wiley and Sons Company, New York, 1996). Chapter 3 of Hui's review (pp. 125-158, which is hereby incorporated by reference) specifically describes the composition and processing of corn oil. The crude oil isolated by pelleting as described here is of high quality but can be further purified by conventional oil refining if desired.

In a preferred embodiment, the invention relates to a method for recovering lighter particles, such as fines, during the processing of high oil corn. The term "fines" as used herein refers to any particle during corn processing that can pass through a #18 sieve with 1.00 mm openings, as defined by ASTM E-11 specification. The recovery of these granules can be performed before, after or at any stage in the processing process (eg during the removal of moisture, during the crushing step or before or after the tableting process). Typically, fines are recovered by passing a gas stream (e.g., air, nitrogen, argon) over the corn at an appropriate velocity and direction to carry the small, light particles out of the steam, leaving the larger, heavier particles behind . Alternatively, a liquid spray (eg, water, process water) can also separate the lighter particles from the heavier particles. Liquids are widely used to physically remove lighter, airborne particles. Liquid sprays can include ingredients that add value to the final product, such as vitamins, minerals, enzymes, and combinations thereof. In addition, the liquid spray may further include a caustic solution. Regardless of the separation method used, these fine particles can be captured or recovered by methods known in the art such as baghouses. Preferably, the recovered lighter particles can be added to a starch-containing product stream to recover the starch. In addition, this fine powder can also be sold as animal feed.

Corn endosperm includes valuable components such as carotenoids, lutein, zeaxanthin. The carotenoids in the granules are divided into two major groups, carotene and xanthools. Carotene is important because they are precursors of vitamin A. Blessin et al [Cereal Chem.40:582-586 (1963)] found that more than 90% of carotenoids, mainly β-carotene, exist in the endosperm of yellow molar maize, and only less than 5% exist in the germ. Vitamin A is mainly derived from beta-carotene.

Another valuable component of endosperm includes tocotrienols. Grams et al. (1970) found that in maize, tocotrienols were only found in the endosperm, while the germ contained most of the tocopherols. Tocotrienols can be extracted from plant materials using various solvents. Methods for the recovery of tocotrienols from plant material are described by Lane et al. in US Patent No. 5,908,940, which is hereby incorporated by reference in its entirety.

Thus, the methods described herein provide a nutritionally fortified corn oil enriched with lutein, zeaxanthin, and/or beta-carotene, and optionally one or more other nutrients.

Oil-based products made with corn oil obtained by the extraction methods described herein contain higher amounts of important nutrients than similar products made with conventionally prepared corn oil. Corn oil obtained by the extraction methods described herein includes corn oil obtained from the germ and endosperm and one or more other components extracted from the remainder of the kernel. The one or more components here may be oils from endosperm, tocotrienols, tocopherols, carotenoids, carotene, xanthools and sterols.

Tocopherol (vitamin E) and vitamin A are antioxidants and are fat-soluble vitamins. They all have health benefits when included in the diet. It is considered within the scope of the present invention to mix the oils of the present invention with other oils or substances to obtain suitable levels of beta-carotene, vitamin E and tocotrienols. In some embodiments, extracted corn oil made as described herein contains about 0.1 wt.% to about 0.5 wt.% tocopherol.

The oil produced according to the method of the present invention may contain about 200%-300% more tocotrienols than crude corn oil produced by conventional methods. Corn oil is extracted by optionally softening, breaking and/or moistening and/or flaking and extracting high oil corn and then analyzed for tocotrienol content. The actual maximum and minimum levels of tocotrienol will depend on the particular high oil corn used.

The Oxidative Stability Index (OSI), measured in hours, is a measure of the relative stability of an oil to oxidation. In general, the greater the OSI, the less susceptible the oil is to oxidation and the longer it takes to oxidize the oil under test or use conditions. Also, the higher the unsaturated fatty acid content of the oil, the lower the OSI. Exemplary oils made using the extraction methods described herein typically have OSI values between about 10-22 hours.

Blessin [Cereal Chem. 39, 236-242 (1962); incorporated by reference in its entirety] describes in detail the extraction of carotene and zeaxanthin, as well as other pigments. Carotene and zeaxanthin can be extracted from corn using a combination of solvents, mainly ethanol and hexane. The oils of the present invention can be produced on an industrial scale using ethanol, hexane, other combinations of solvents in various proportions.

Exemplary embodiments of crude oils obtained using the extraction methods described herein generally possess the partial compositional properties shown in Table 4 below.

Table 4 Element Exemplary extracted high oil corn Extracted High Oil Corn (Range) FFA (%) C16: 0C18: 0C18: 1. Cis C18: 1. Anti C18: 2. Cis C18: 2. Anti C18: 3 1.4511.42.133500.8 0.7-3.0010-141.5-3.526-5042-600.6-1.6 Phosphorus (ppm) 190 100-400 Total Tocopherols (ppm) 0.13 0.1-.50

Fatty acids typically found in corn oil typically include palmitic, stearic, oleic, linoleic, and linolenic acids.

Crude oils produced by the methods described herein may be partially or fully hydrogenated. Suitable methods for partial or complete hydrogenation of oils are described in D.R. Erickon, Practice Handbood of Soybean Processing Utilization (1995, AOCS Press), which is hereby incorporated by reference in its entirety.

When oil-based products are made according to the invention, those products may contain conventional corn oil, soybean oil, canola oil, olive oil, palm oil, sunflower oil, safflower oil, antioxidants, flavorings, hydrogenated oils , partially hydrogenated oils and/or animal fats. Blended oil products can be prepared by blending the corn oil herein with one or more other oils. Corn oil-based products may also contain food supplements, salt, fat, food coloring, beta-carotene, annatto extract, curcumin or turmeric, beta-apo-delta'-carotene and its methyl and Ethyl esters, natural or synthetic flavoring agents, antioxidants, propyl gallate, butylated hydroxytoluene, butylated hydroxyanisole, natural or synthetic tocopherols, ascorbyl palmitate, ascorbyl stearyl Ester, Lauryl Thiodipropionate, Antioxidant Synergist, Citric Acid, Sodium Citrate, Isopropyl Citrate, Phosphoric Acid, Glyceryl Monocitrate, Antifoaming Agent, Dimethicone Alkanes, crystallization inhibitors, stearyl oxide, amino acids, vitamins, minerals, carbohydrates, sugars, herbs, spices, acidity regulators, curing agents, enzyme preparations, flour treatment agents, viscosity control agents, enzymes, lipids and/or vegetable or animal protein. Additionally, these edible products can be fortified or enriched with protein supplements containing available protein. Exemplary food products such as breakfast corn flakes may contain powders such as the present invention, wheat and oat flour, sugar, salt, corn syrup, corn flour, fruit juice concentrate, vitamin C, B vitamins, folic acid, baking soda and Formulations such as flavoring agents.

Other exemplary oil-based products may contain the oils prepared herein, including edible oils, cooking oils, edible oils, and blended oils.

Equipment for extracting oil from oilseeds such as soybean and canola can be used to make the corn oil and oil-extracted corn meal described herein. Effective flakes of oilseed for industrial scale are available from French Oil Mill Machinery, Pink, Ohio; Roskamp Champion, Waterloo, Iowa; Buhler, headquartered in Switzerland, with offices in Plymouth, Minnesota Bauermeister, Germany; and Consolidated Process Machinery Roskamp, World Wide Web at http://www.cpmroskamp.com and Crown Iron Works, Minneapolis, MN.

Industrial scale methods and apparatus are capable of extracting corn oil from at least about 1 ton of corn per day. In some embodiments, the industrial scale processing capacity is from about 100 tons of corn to about 3000 tons of corn per day, or from about 700 tons of corn to about 1700 tons of corn per day. Industrial scale operations are also possible that process more than about 3000 tons of corn per day.

The quality of corn oil or corn flour can be determined by evaluating one or more quality parameters such as oil yield, phosphorus content, percent free fatty acid, percent neutral starch, protein content, and moisture content. Any method can be used to calculate one or more quality parameters to evaluate the quality of the oil or meal.

The phosphorus content of crude oil can be identified by AOCS method Ca 12-55. The AOCS method Ca 12-55 recognizes phosphorus or equivalent phosphorus zinc oxide, and then uses spectrophotometry to measure the phosphorus that forms the blue phosphomolybdic acid complex. AOCS method Ca 12-55 is applicable to crude, degummed and refined vegetable oils. Multiply the phosphorus content by 30 to convert it to the phospholipid content, which is the gum content. In some embodiments, corn oil produced according to the present invention contains about 100-400 ppm phosphorus.

The percentage of free fatty acids in the oil can be identified using the AOCS method Ca 5a-40. The AOCS method Ca 5a-40 identifies free fatty acids present in oil samples. AOCS method Ca 5a-40 is applicable to all crude and refined vegetable oils, mineral oils and animal fats. Adding together the percent gum and the percent free fatty acid gives the neutral oil lost during processing. The amount of free fatty acids in extracted corn oil depends on the amount of fatty acids found in the high oil corn used for oil extraction. In some embodiments, the content of free fatty acids in the extracted oil is between about 0.70 wt.% and 3.00 wt.%.

The color of the oil can be determined by AOCS method Cc 13a-45. AOCS method Cc 13a-45 allows the determination of the color of an oil sample by comparing the oil sample with known color characteristics. AOCS method Cc13a-45 is suitable for both fats and oils as long as the sample is not turbid. Color can be assessed qualitatively by visual inspection of the oil. Typically, the results of visual inspection separate the oil into light and dark oils compared to the known oil color. Chromaticity can be quantified by measuring the red value and yellow value with AOCS method Ccl3a-45. Typically, crude corn oil isolated by conventional dry grinding has a red value of about 7-10 and a yellow value of about 60-70. Corn oil isolated by the flaking method described here is lighter in color and generally lighter than crude corn oil obtained by wet or dry milling techniques. The yellow value determined by AOCS method Cc 13b-93 is about 60-70, and the red value is about 7-10.

Extracted corn oil can be used as raw material for chemical modification, component of biodegradable plastics, component of mixed food products, component of edible or cooking oil, lubricant or component thereof, biodiesel or component thereof, component of snack food, Raw materials for fermentation processes and ingredients for cosmetic products. Since the oil obtained by the extraction method herein contains one or more components obtained from the non-endosperm portion of the corn kernel, the oil is improved. In some embodiments, the oil contains 20%-80%, or 25%-50% oleic acid, whereas conventional corn only contains 25%-40% oleic acid in the oil. When making oil blends from extracted oils, the blending can be done before, during or after the extraction process.

The corn oil extracted by the invention can be used to produce biodiesel. Biodiesel is a general term for various ester-based oxidation dyes. Biodiesel produced today is a mixture of fatty acid methyl esters produced by methylating refined vegetable oils. Mainly due to the quality of the glycerin by-product, refined oils are better than crude oils or used frying oils. The main disadvantages of previous biodiesel products and related vegetable oil lubricants are low temperature properties, oxidation and polymerization reactivity. Preferred biodiesel products include low cloud point, reduced stearic acid and polyunsaturated fatty acid content, and high oleic acid content. The pour point is related to low temperature properties and is influenced by the saturated fatty acid content of the oil. Polyunsaturated fatty acids are more prone to oxidation and polymerization.

Solvent extracted corn (SEC) oil has better cloud point properties than soybean when the chemical stability is similar.

table 5 Oil % Palmitic Acid (16:0) Stearic acid% (18:0) Oleic Acid % (18:1) Linoleic Acid % (18:2) % Linolenic Acid (18:3) Sinapinic Acid % (22:1) rapeseed 3 1 14 12 7 49 canola 4 1 60 20 9 2 soybean 8-10 4 19-28 53-56 6-10 0 SEC 11 2 27 56

SEC oil corn can be further processed to form lubricants, such as by published methods currently employed in the art (see, eg, US Patent No. 6,174,501, incorporated herein).

The powder obtained by the tableting and oil-extraction methods described here is used to produce unique plastic products. The cornmeal used here is obtained from whole high-oil corn kernels after oil extraction, in which the kernel has not been separated into its component parts, although the kernel may be ground, flaked, cracked, sliced, or ground, or are not treated as such. The process of removing oil from corn by extraction is used to concentrate the remaining nutrients such as protein and key amino acids.

Feed products made primarily of cornmeal by extraction require less protein addition from other sources such as soybeans than feed products primarily composed of regular corn kernels. Since ingredients can be added through processing, this powder makes it possible for feed manufacturers to produce feed that cannot be produced by other methods. The use of the expressed cornmeal of the present invention as an ingredient in animal feed rations can produce animal feed rations with specific physical properties (eg, bulk density, texture, grainability, and water holding capacity) and/or specific nutritional properties. Oil-extracted cornmeal isolated by the flaking and extraction methods described here can itself be used as a low-fat cornmeal. Alternatively, it can be used in combination with other cornmeal or nutritional ingredients to make feed rations and foods. Extracted corn meal can also be used in combination with meal made from soybeans, canola, sunflower, rapeseed, cotton, and other crops. Genetically modified corn may also be used to make expressed corn meal and/or combined with meal made from transgenic oilseed particles to form fortified meal or fortified products.

The extracted corn meal can be provided as a loose product or a pelleted product, which can optionally be combined with other ingredients. For example, a granular product may include expressed corn flour (either by itself or in combination with other ingredients) that has been granulated and then coated with zein. Cornmeal may be included in blended powder products provided in loose or granular form.

Feed rations made from oil-extracted cornmeal generally meet dietary and quality standards established by CODEX ALIMENTARIUS or the National Research Council. This powder typically contains the following ingredients in the approximate amounts listed in Table 6.

Table 6 Element Sample A content (%) Sample B content (%) Sample C content (%) moisture 5-45 5-25 5-45 starch 40-70 40-80 40-70 protein 8-20 7-20 8-20 fat (oil) 0.75-6 0.75-6.0 0.75-12 crude fiber 2-4 2-4 Ash 1.5-3 0.5-2.0 fructose 0.15-0.3 glucose 0.2-0.5 sucrose 1.5-2.5 Lysine 0.2-2.0 Tryptophan 0.03-2.0

The corn flour described above may further contain ingredients that are not quantified, ie the amounts of these ingredients are not indicated.

Different animals require different levels of nutrients, depending on species, age and husbandry. The high-oil corn is subjected to different degrees of extraction, that is, the higher the degree of extraction of the high-oil corn, the more oil is removed from the corn, and feed rations with different levels of nutrients can be prepared. Thus, by controlling the degree of extraction of the high oil corn, feed rations containing the extracted corn meal of the present invention can be made to contain varying amounts of fat, protein and carbohydrates. Table 7 details the amounts at which the specified ingredients are present in animal feed rations containing extracted corn meal, indicating specific content ranges for exemplary rations containing extracted corn meal as the main ingredient, Also indicates the general characteristics of rations that may contain one or more other ingredients (e.g., carbohydrate-based energy sources such as sorghum, wheat, and/or other grains or their by-products, or other non-cereal ingredients). content range.

Table 7 ingredients General content range Exemplary content range cornmeal as described here 2-95% 50-90% Oilseed Meal ¹ 3-35% 10-30% meat and bone meal 0-12% 0-7% feather powder 0-6% 0-4% Fat 0-10% 1-6% Salt 0.1-0.5% 0.1-0.5% Lysine 0-0.4% 0-0.4% Methionine 0-0.3% 0-0.3% Nutrient Ingredients Premix 0.01-1.0% 0.01-1.0%

¹ Oilseed flours include, but are not limited to, soybean, sunflower, canola, cottonseed, and other plant-based flours that may or may not be used in the oil extraction process.

Meat and bone meal were obtained from suppliers such as Darling International (Irving, Texas). Oilseed meal was obtained from suppliers such as Cargill Oilseeds (Cedar Rapids, Iowa). Feather meal was obtained from suppliers such as Agri Trading Company, (Hetchinson, MN). Amino acids were obtained from suppliers such as DuCoa (Highland, IL).

Feed rations are formulated by mixing various substances, such as grains, seed meal, vitamins, and/or purified amino acids, to form a complex that meets dietary requirements for protein, energy, fat, vitamins, minerals, and other nutrients made of substance. The process of blending involves grinding and blending ingredients to create a relatively uniform mixture of nutrients. The physical properties of feed ingredients and mixed feed can affect the nutritional status, storage performance and overall value of the product. Suitable methods of making feed rations are disclosed in Feed Manufacturing Techniques IV (1994, American Feed Industry Association), which is incorporated herein by reference in its entirety.

The digestibility of the starch portion of oil-expressed corn flour and steam-flaked corn is relatively similar, but due to differences in processing conditions, the former has better digestibility in ruminants. As discussed herein, specific oil levels in the oiled meal can be achieved by varying processing conditions. The protein, amino acid and oil levels of this oiled meal cannot be achieved in steam-flaked conventional corn, while steam-flaked high-oil corn contains more oil, which is detrimental to ruminant health.

Many types of animal feed rations can be produced from this type of oil-extracted corn meal. For industrial purposes, the following diet types will be described here: (1) Meal from corn kernels used in hog finishing diets , wherein the oil content of the corn kernels is 12wt.%, the protein content is 9wt.%, and the oil content of the flour obtained from this corn is 1.5wt.%. (2) Meal obtained from corn kernels used in poultry chicken diets, wherein said corn kernels have an oil content of 12 wt.% and a protein content of 9 wt.%, the oil content of the meal obtained from this corn is 4.0 wt.%.

When used as an aquaculture feed product, the expressed corn meal of the present invention has several advantages over conventional corn kernels. In agriculture, pigments such as carotenoids in feed are often precipitated in adipose tissue during use and lead to undesired colors. For some fish species, consumers prefer lighter colored tissues. In other species, such as salmon, consumers prefer pink or red tissue. One of the benefits of using extracted cornmeal for aquafeeds is that some unwanted pigments can be removed through the process of making extracted cornmeal; solvent-soluble pigment mixtures (e.g. carotenoids) Remove from flour and concentrate in corn oil. A second advantage of oiled corn flour over dry or wet milled corn products is the increased protein content and quality due to the fact that the oil has been substantially removed from the kernel so that the protein in the meal product is concentrated . Since this meal is derived from all parts of the kernel, including most or all of the endosperm, its protein is generally of higher quality and quantity than that of grits from oil extraction. The use of oil-extracted cornmeal in aquafeeds will potentially produce animals with fewer unwanted pigment compounds in their tissues.

Solvent extracted corn flour is also useful for the production of fermentation-based compounds such as ethanol, lactic acid, and vitamins. Solvent extracted corn flour from high oil corn can be hydrolyzed to provide suitable sugars. This flour can be used as a carbon and energy source for bacterial, fungal or yeast cultures. Biotin and other vitamins can be produced by culturing microorganisms. (Micro)organisms include Pseudomonas mutans (ATCC 31014), Corynebacterium primorioxydans (ATCC 31015), soil bacteria, Gibberella, Penicillium or combinations thereof.

Nutrients used in cultures of these and other microorganisms include, for example, starch, glucose, alcohols, ketones, and as nitrogen sources, peptone, corn steep liquor, soybean flour, ammonium chloride, ammonium sulfate, ammonium nitrate, pressed Oil of cornmeal or urea. The culture medium can also contain various salts and trace elements to cultivate microorganisms. The pH of the medium is about 4-9, preferably about 6-8, most preferably about 7 for the bacterial species. For mold or yeast, the pH is about 5-7. During the culturing, the temperature is maintained at 10°C-100°C, preferably between 20°C-80°C, more preferably between 20°C-40°C, most preferably about 25°C.

The production of biotin is described in US Patent No. 3,859,167, which is incorporated herein by reference. cis-tetrahydro-2-oxo-4-n-pentane-thieno[3,4 -d] imidazoline. Usually, the microorganisms are cultured for 1-10 days, preferably 1-8 days, more preferably 2-7 days, after which biotin is separated and purified. In one embodiment, to purify biotin, cells are removed from the culture medium, the filtrate is absorbed on charcoal, and purified using an ion exchange column. Other purification methods can also be used, such as adjusting the pH of the biotin-containing solution near the isoelectric point to crystallize it.

Solvent extracted cornmeal can also be further processed to make biodegradable substances. For example, powders of the invention may be contained in a thermoplastic agent. The powders of the present invention may also be used in the methods described in US Patent No. 5,320,669, which is incorporated herein by reference. The thermoplastic material was fabricated from solvent extracted corn flour (as obtained by the processing method described here). In one embodiment, milled corn kernels prepared from powders of the present invention are treated with an organic solvent and optionally a cross-linking agent to interconnect the starch and protein in the expressed corn kernels. Cross-linking agent refers here to any compound capable of linking starch and protein, such as, for example, aldehydes, anhydrides or epoxides. Compositions thus formed from the powders of the invention can be used to make extruded or molded articles that are biodegradable, waterproof and/or have a high level of physical strength.

Combination products containing extracted corn meal and one or more other oilseed meals are produced by one or more of the following methods: 1) blending high oil corn and other oilseeds, followed by crushing and/or pressing flakes, all seed mixtures are flaked and used in the extraction process described here to form a blended meal; 2) high oil corn is crushed and moistened before blending with other oilseeds, flaked and all 3) flake high oil corn before blending it with other oilseeds and use all of the seed mixture in the extraction process described here to form a blended meal; forming a blended meal; 4) blending the expressed corn meal with pressed or unexpressed other oilseed meal to form a blended meal; or 5) combining the above flours to form a blended meal. At any time during the above process, additional ingredients can be added to the blended powder to make a blended product.

Extracted cornmeal can also be used in foods like snacks, mixed foods, breads, fermented ingredients, breakfast corn flakes, concentrated foods (such as canned juices), puffed or extruded foods, and porridge.

When used in human or animal edible products, extracted corn flour may be mixed with other flours, other oilseed meals, grains, other corn, sorghum, wheat, by-products of wheat milling, barley, cassava, Ingredients such as corn bran meal, corn bran feed, barley by-products, whole rice bran and rice hulls are mixed.

Oil-extracted corn flour is also used as a feedstock for the production of corn protein isolate, fermentation, further chemical processing, and enzymes such as amylase and protease can be added to the flour to help break down starch and protein.

The extracted corn flour can optionally be used in conventional methods of separating the starch and protein components. These methods include, for example, dry milling, wet milling, high pressure pumping, or cryogenic processing. These methods and other suitable methods are described in Watson, S.A. and P.E. Ramstad eds. Corn: Chemistry and Technology, Chapters 11 and 12 (1987, American Association of Cereal Chemist Inc., St. Paul, MN), which are incorporated herein by reference for reference. Since the oil has been removed from the cornmeal, the starch and protein components are more easily separated from the other components in the oil-expressed cornmeal than in the meal from which the corn oil has not been extracted.

Several important quality parameters of expressed meal include fat, starch, protein and moisture content. Methods for evaluating quality parameters of oilseed meal are described in the AOCS method, and the relevant method is incorporated herein by reference. These methods can also be used for extracted corn flour prepared by the methods described herein.

The moisture content of the granules can affect the tableting process. It is necessary to increase the moisture content of the corn kernels to about 1%-15% prior to flaking the seeds. Optimizing the moisture content of the particles facilitates adequate processing, as is known to those of ordinary skill in the art.

The cornmeal was calibrated to a conventional moisture content and compared with cornmeal separated by different methods or separated at different times. The moisture content of oilseed protein concentrates (such as cornmeal or whole corn) is determined by AOCS method Ba 2b-82. The crude fiber content of corn flour is determined by AOCS method Ba 6-84. AOCS method Ba 6-84 can be used for pellets, flour, flour, feed and all fibrous substances from which fat can be extracted leaving a processable residue. The crude protein content of corn flour is determined by AOCS method Ba 4e-93. The starch content of corn flour is determined by AOCS method Ba 4e-93. The starch content of corn flour was determined by Method A-20 ("Corn Refiners A-20 Method") in Standard Analytical Methods (Second Edition, April 15, 1986), a member company of the Corn Refiners Association, Inc.

It should be understood that the analytical methods provided herein are examples of efficient methods for calculating the various quality parameters of the oils and meal described herein. Other suitable methods are known and can also be used to calculate the quality parameters described and claimed herein.

The following examples are provided to illustrate specific embodiments of the invention. Those skilled in the art should understand that the techniques suggested in the following examples represent techniques that the inventors have found to work well in the practice of the present invention, and thus can be regarded as examples of practice. However, having regard to the disclosure herein, those skilled in the art should appreciate that many modifications can be made to the specific embodiments disclosed herein without departing from the spirit and scope of the invention and still obtain a like or similar result. .

Example 1

Treatment of high oil corn by crushing, wetting and flaking

This example describes the process of obtaining corn oil and corn meal from high oil corn. A 45 lb sample of high oil corn was crushed using a Roskamp Series 6.5 (two 9” units) with a roller distance of 0.27 inches. One sample was used for analysis and the remaining sample was divided into 4 sub-samples. At different temperatures (120° F, 150°F, 180°F, 200°F) Wet each subsample individually. Heat the samples in a Crown ^™ 18" Desolventizer/Oven. When each sample reaches its wetting temperature, pass the sample through Tablet roller. The tablet roller used is Ross 10 inches with a gap set at 0.007 inches. Take a sample of flakes and extract about 500 g of sample. Wash 4 times with 1200 ml of hexane for 20 minutes each time, within 80 minutes A total of 4800ml of solvent was removed. Solvent temperature was approximately 120°F. Trash oil was collected and filtered through a #4 qualitative disc of 185mm diameter. The filtered trash oil was then rotovaped to evaluate percent oil recovery. At room temperature The powder was air dried. Samples of oil and powder were taken and analyzed for fatty acid properties, starch, protein and fiber. Sieve analysis was performed and flake thickness was measured during extraction.

Other equipment used for analysis included a Mettler Toledo ^™ HR73 Halogen Moisture Analyzer, OhausExplore ^™ Balance, Büchi R-114 Roto-Vap ^™ , Crown ^™ Extractor Screen (0.032 mesh) and Easy Load Flex 17529-30 Model Pump.

The color of the crude oil was visually determined to be light yellow in comparison to the crude oil (dark black) isolated by conventional wet milling.

Desolvated corn flour was characterized by AOCS methods Ba 3-38, Ba 2b-82, Ba 6-84, and Ba 4e-93 and Corn Refining Method A-20. When corrected to a moisture content of 10%, corn flour contains about 3.2% fiber, about 65% starch, and about 14% protein. The fat content of the flour was determined to be about 1.07% by AOCS method 3-38. For comparison, a corn bran feed prepared by conventional wet milling and corrected for moisture content to 10% has an oil content of about 4%, a protein content of about 20%, and a fiber and other carbohydrate content of about 60%. Also for comparison, a corn bran feed produced by conventional wet milling and corrected for moisture content to 10% may contain about 3% oil, about 60% protein and about 22% fiber and other carbohydrates.

Table 8 shows the nutritional characteristics of the two flours (containing 1.5 wt.% oil and 4.0 wt.% oil) prepared by this method. Contents are expressed based on "as is" or "as fed" moisture levels.

Table 8 Element Powder sample 1 content (%) Powder sample 2 content (%) moisture 12 12 Oil 1.5 4 protein 10.5 10.2 starch 58.0 56.3 neutral detergent fiber 11.3 11 acid detergent fiber 2.8 2.8 Ash 1.4 1.3 Lysine 0.39 0.37 Tryptophan 0.105 0.102 Methionine 0.29 0.28 cysteine 0.25 0.24 total sulfur amino acids 0.54 0.52 Valine 0.53 0.51 Isoleucine 0.40 0.39 arginine 0.53 0.51 threonine 0.40 0.39 Leucine 1.20 1.17 Histidine 0.32 0.31 Phenylalanine 0.51 0.5 Alanine 0.82 0.79 serine 0.54 0.52 True metabolizable energy (TMEn; kcal/kg) 3023 3133 Pig metabolizable energy (ME; kcal/kg) 3191 3301

When compared to flour made from conventional corn, the expressed corn flour described herein provides higher amounts of certain key nutrients, such as vitamins, folic acid, pantothenic acid, lysine, tryptophan, and/or niacin. For example, powder samples 1 and 2 prepared as described above contained nutrients in the amounts shown in Table 9. Amounts of the same ingredients were compared to their levels in unprocessed yellow corn as described here.

Table 9 Element yellow corn Powder sample 1 Powder sample 2 Vitamin B6 (mg/100g) 0.400 0.820 0.660 Vitamin B12 (mg/100g) 0.500 0.500 0.500 Folic acid (μg/100g) - 25.0 25.0 Pantothenic acid (mg/100g) - 0.660 0.890 Niacin (mg/100g) 2.05 2.30 1.15

Advantageously, the expressed corn meal produced as described herein may contain a specified level of oil and, in particular, may contain a specified ratio of oil:protein, oil:carbohydrate or oil:protein:carbohydrate. For example, regular corn contains 8 wt.% protein and 4 wt.% oil for a protein:oil ratio of 2.0, while high oil corn contains 9 wt.% protein and 12 wt.% oil for a protein:oil ratio of 0.75. The powder produced by extraction contained 10.5 wt.% protein and 1.5 wt.% oil, for a protein:oil ratio of 7.0. This high ratio makes this type of meal, and products made from it, desirable for certain applications, an example being finishing feed for pigs.

The present invention provides an extracted corn oil having a higher content of lutein, zeaxanthin and beta-carotene than commercially available crude oil from common yellow #2 dent corn. Conventional crude oils are available from suppliers such as Cargill Corporation (Minneapolis, MN). For example, corn oil produced by the method described above contains the components shown in Table 10, the amounts of which are listed in comparison to commercially available crude oils.

Table 10 sample Lutein (mg/g) Zeaxanthin (mg/g) β-carotene (IN/100g) commercial crude corn oil 0.005 0.005 15.5 Oil sample 1 0.04 0.012 72.3 Oil sample 2 0.330 0.112 302

Example 2

Meal from flaked and extracted corn used as an ingredient in finishing feed rations for hogs

This example details a comparison of two different feed rations: a first feed ration containing conventional corn without solvent extraction and a second feed ration containing oil-extracted corn meal. Feed rations containing extracted cornmeal are used when lean pork is the desired end product. Hog finisher feed rations containing oil-extracted corn meal with an oil content of less than or about 1.5 wt. % were prepared with the following ingredients at the levels listed in Table 11. Such feed rations are usually prepared by tempering, mixing and pelleting the ingredients; however, one or more of these steps may be omitted in manufacturing the feed ration. Table 11 shows a comparison of pig feed rations made with normal corn (non-high oil corn) and oil-extracted corn flour obtained from high-oil corn containing 12 wt.% oil, 9 wt.% protein, wherein Oily cornmeal contains about 1.5 wt.% or less oil (fat). Contents are expressed based on "as is" or "as fed" moisture levels.

Table 11 Element pig finishing feed Normal content (%) Oil-extracted corn flour (%) corn 79.98 - Oil-pressed cornmeal (about 1.5% oil) - 83.55 soy flour 12.45 6.60 meat and bone meal 6.59 7.22 feather powder - - Fat 0.10 1.50 Salt 0.40 0.70 Lysine 0.08 0.15 Methionine - - Premix 0.15 0.15 nutrient content Crude protein, % 15.44 15.78 ME, kcal/kg 3200 3200 Crude fiber, % 1.96 2.12 calcium,% 0.85 0.85 phosphorus,% 0.58 0.58 Amino acid, % arginine 0.96 0.93 cysteine 0.28 0.29 Histidine 0.40 0.42 Isoleucine 0.57 0.58 Leucine 1.39 1.49 Lysine 0.81 0.81 Methionine 0.26 0.34 Phenylalanine 0.70 0.72 threonine 0.56 0.58 Tryptophan 0.14 0.14 Tyrosine 0.47 0.48 Valine 0.72 0.75

In Table 11, the absolute values of the percentages of ingredients are given, however, in practice, ingredients using the proportions of inclusions listed in other tables in the text are also included.

Some advantages of this new feed ration are that the user of the meal does not need to grind the corn, thus saving an energy-intensive step, less soybean or other oilseed meal is required to meet the required protein levels, and this Seed flour has better digestibility than corn kernels.

Example 3

Meal from flaked and extracted corn used as an ingredient in poultry finisher feed rations

This feed ration is used to meet the high energy requirements of growing birds such as chicks. Chicken finisher feed rations for poultry containing extracted corn meal with an oil (fat) content of less than or about 4 wt. % were prepared with the following ingredients at the levels listed in Table 12. Such feed rations are typically prepared by tempering, mixing and pelleting the ingredients; however, one or more of these steps may be omitted in manufacturing the feed ration.

Table 12 shows a comparison of pig feed rations made with normal corn (non-high oil corn) and oil-extracted corn flour obtained from high-oil corn containing 12 wt.% oil, 9 wt.% protein, wherein Oily cornmeal contains about 4 wt.% or less oil (fat). Contents are expressed in absolute terms based on "as is" or "as fed" moisture levels and percentages of ingredients given, however, in practice, ingredients are included using the percentages of inclusions listed in other tables herein.

Table 12 Element growing chicks Normal content (%) Oil-extracted corn flour (%) normal corn 66.85 - Oil-pressed cornmeal (about 4% oil) - 70.86 soy flour 20.96 16.42 meat and bone meal 5.00 5.00 feather powder 2.00 2.00 Fat 3.29 3.76 Salt 0.37 0.37 Lysine 0.13 0.19 Methionine 0.15 0.09 Premix 0.10 0.10 nutrient content Crude protein, % 19.48 19.52 ME, kcal/kg 3100 3100 Crude fiber, % 1.97 2.12 calcium,% 0.94 0.94 phosphorus,% 0.63 0.62 Amino acid, % arginine 1.27 1.23 cysteine 0.38 0.39 Histidine 0.47 0.48 Isoleucine 0.78 0.79 Leucine 1.68 1.74 Lysine 1.06 1.06 Methionine 0.44 0.44 Phenylalanine 0.92 0.92 threonine 0.74 0.75 Tryptophan 0.19 0.20 Tyrosine 0.61 0.62 Valine 0.95 0.96

Example 4

Use of oil from flaked and extracted corn as a food ingredient or as a raw material for purified kernel components

In this example, an oil is described having a tocotrienol content approximately 200%-300% greater than conventionally produced crude corn oil. Using the tabletting and extraction methods of Example 1, corn oil was extracted from high-oil corn with an oil content of about 12 wt.%. The corn oil was then analyzed for tocotrienol content. The following table includes data relating to the alpha- and gamma-tocotrienol content of conventional corn oil prepared from conventional corn by conventional methods and extracted corn oil prepared according to the method of Example 1. Conventional crude oil refers to the unrefined corn oil sample. This sample is representative of most common products currently manufactured. As described below, it was found that the tocotrienol content of oil extracted from whole kernel (EWKO) samples solvent-extracted from two different high oil corn samples at 120-200°F was approximately 2-3 times that of oil samples. The tocotrienol content of the EWKO samples ranged from about 26ppm-33ppm alpha-tocotrienol and about 48ppm-84ppm gamma-tocotrienol. In general, increasing the extraction temperature will increase the tocotrienol content of the extracted corn oil. The actual minimum and maximum tocotrienol levels will depend on the particular high oil corn used.

Table 13 sample Alpha Tocotrienol (ppm) Gamma Tocotrienol (ppm) Conventional crude oil (control) 11.88 29.94 EWKO 1 120-200F 29.36-33.19 48.11-59.36 EWKO 2 120F 26.05-28.43 79.55-84.21

Thus, the method of Example 1 was used to produce extracted corn oil containing enhanced levels of tocotrienols.

Example 5

Meal from flaked and extracted corn used as an ingredient in mixed animal feed products containing corn meal and oilseed meal

This example describes a novel feed ingredient comprising a mixture of corn meal prepared by flaking and oil extraction and another meal of plant origin, such as oilseed meal. This mixed substance can be simply a loosely aggregated mixture of these two powders, or it can be a granulated product. Since the methods of making corn and oilseed flours are similar, ie crushing, moistening, flaking and solvent extraction, it is possible to produce both flours together and blend them before selling to consumers. An advantage of this is that various levels of protein and energy can be achieved with one powder. Additional ingredients may optionally be added at the powder mixing stage or at the final stage. For example, an energy-intensive step in feed manufacturing involves grinding corn kernels in a feed mill and mixing it with other ingredients. Compared to conventional mixes, the mixes of the present invention generally require less energy to manufacture the final feed product.

Table 14 shows soybean meal (SBM), oil-extracted corn meal (ECM), a mixture of 20% SBM and 80% ECM (S20-C80), a mixture of 10% SBM and 90% ECM (S10-C90), and Nutrient profiles of nutrient requirements of poultry and swine diets. Nutrient requirements for poultry and swine are listed according to National Research Council (NRC) guidelines. ECMs were fabricated according to Example 1.

Table 14 parameter SBM ECM 20% SBM and 80% ECM Poultry Daily Nutrient Requirements 10% SBM and 90% ECM Pig Daily Nutrient Requirements crude protein (CP) 47.5 10.2 17.66 18 13.93 13.2 Pig ME, kcal/kg 3380 3301 3316.8 3308.90 3265 Poultry ME, kcal/kg 2440 3133 2994.4 3200 3063.70 Crude fat, % 3 4 3.8 3.90 Neutral detergent fiber, % 8.9 11.3 10.82 11.06 Acid detergent fiber, % 5.4 2.8 3.32 3.06 arginine 3.48 0.45 1.06 1.00 0.75 0.19 Histidine 1.28 0.27 0.47 0.27 0.37 0.19 Isoleucine 2.16 0.34 0.70 0.62 0.52 0.33 Leucine 3.66 1.03 1.56 0.93 1.29 0.54 Lysine 3.02 0.33 0.87 0.85 0.60 0.60 Methionine 0.67 0.25 0.33 0.32 0.29 0.16 cysteine 0.74 0.21 0.32 0.28 0.26 0.35 Phenylalanine 2.39 0.44 0.83 0.56 0.64 0.34 Tyrosine 1.82 0.29 0.60 0.48 0.44 0.55 threonine 1.85 0.34 0.64 0.68 0.49 0.41 Tryptophan 0.65 0.09 0.20 0.16 0.15 0.11 Valine 2.27 0.45 0.81 0.70 0.63 0.40 Total Essential Amino Acids (EAAs) 23.99 4.49 8.39 6.85 6.44 4.17 EAA/CP 0.505 0.440 0.45 0.381 0.45 0.316

Example 6

Processing high oil corn by flake method

Perten ^™ volumetric near-infrared (NIR) seed tester (TM) (Model: 9100-HF), Perten Instruments (Reno, Nevada) was used to test the shells of individual ears of yellow dent corn with a total oil content greater than about 7 wt.%. The grains are screened. Kernels from ears with an oil content of at least 7 wt. % were further screened in a Brimrose ^™ Seed Expert Single Kernel NIR Tester (Brimrose Corporation, Baltimore, MD) to select individual kernels with an oil content of at least 13%. The kernels were stored at a moisture content of approximately 13.5%. When processed, the moisture content of the seeds is about 10%.

Whole kernels were flaked using a bench-top flaking apparatus consisting of a two-inch stainless steel rod and flat plate. The whole kernel flakes are passed through the rollers four times to give a final flake thickness of about 0.01 inches. Trash oil was extracted from flaked corn kernels using hot (60-65°C) n-hexane and a Kimble ^™ Model 585050 Soxhlet extractor. The resulting miscella and cornmeal were desolvated. The miscella was heated under 25 inches of mercury vacuum to remove solvent. Corn flour was desolvated according to AOCS method Ba 2a-38.

All recovered oil represented 14.74 wt.% of all kernel samples. The phosphorus content of the desolvated crude oil was 365 ppm as determined by AOCS method Ca 12-55. The phospholipid concentration was determined to be 1.095% (0.0365%*30). The free fatty acid content determined by AOCS method Ca5a-40 is 0.2%. The loss of neutral oil during processing was 1.3% (1.095%+0.2%). Using the same method, the phosphorus content of the crude oil extracted from conventional (that is, the total oil content is 3-4wt.%) corn kernels by conventional wet milling is about 600ppm-800ppm, and the free fatty acid content is about 0.5%-1.0 %, the neutral oil lost during processing is about 3%-4%.

The color of the crude oil was visually determined to be light yellow in comparison to the crude oil (dark black) isolated by conventional wet milling.

Desolvated corn flour was characterized by AOCS methods Ba 3-38, Ba 2b-82, Ba 6-84, and Ba 4e-93 and Corn Refining Method A-20. When corrected to a moisture content of 10%, corn flour contains about 3.2% fiber, about 65% starch, and about 14% protein. The fat content of the flour was determined to be about 1.07% by AOCS method 3-38. For comparison, a corn bran feed prepared by conventional wet milling and corrected for moisture content to 10% has an oil content of about 4%, a protein content of about 20%, and a fiber and other carbohydrate content of about 60%. Also for comparison, a corn bran feed produced by conventional wet milling and corrected for moisture content to 10% may contain about 3% oil, about 60% protein and about 22% fiber and other carbohydrates.

Example 7

Method for Refining High Oil Corn

This example hereinafter describes the continuous solvent extraction process. This extraction method basically consists of four parts: pre-extraction, extraction, powder desolvation and oil desolvation. These different stages are described in more detail below.

(A) Prefetching

5.4 tons of complete high-oil corn (about 12 wt.% oil) kernels are softened, and then the material is sent to the crusher from the door of the material box through the chain bucket elevator. Through the crusher, the shredded material (i.e., kernels of whole corn) is sent to the conditioner, which sends the material to a segregated transport system. This system includes a second bucket elevator, air mechanical conveyor, hot steam jacket conveyor and chutes connected in series. Via the conveyor system, the corn flakes are fed to the flaking rollers.

Water was added to the "as is" wet corn in a 350 liter Toronto Coppersmithing ^™ Toreo R-12 ribbon mixer to soften the whole corn to a moisture content of 14.5% prior to sending to the crusher. Sprinkle the container with water at a rate of 2 liters/hour. After adding the appropriate amount of water, the corn was stirred for an additional hour. Corn was soaked for 24 hours before its moisture content was measured. The softened corn is then stored for 11-15 days.

After storage, the softened corn was crushed at room temperature with a Roskamp ^™ (Waterloo, Iowa) model 6.5 series, dual-frame crushing rollers with 9" diameter 12" long rollers. Set both the upper and bottom rollers so that one turns faster than the other. The fast roller rotates at 1065 revolutions per minute (rpm) and has 6 helical RBV cut corrugations per inch. The slow scroll wheel cuts the same but spins at 708rpm. Crushing humidity is 13.3%-15.7%. Crumbs produced the following average particle size distribution ranges: 15.9% retained by US #4 mesh sieve, 39.9% retained by US #6 mesh sieve, 27.8% retained by US #8 mesh sieve, 6.8% retained by US #10 mesh sieve , 4.3% was retained by US #18 mesh sieve and 5.3% was retained by US #18 mesh sieve.

Then in the double-layer regulator (Simon-Rosedowns, now owned by De Smet; Prins Boudewi jnlaan 265; B-2650 EDEGEM; Antwerp) with a rotating cleaning arm, which claims to have a processing capacity of 100 kg (each layer is 36 inches in diameter and 20 inches high. inches) to moisten the cracked corn. The bottom layer is running at full capacity. The residence time in the steam injection stage was 55 minutes. The crushing depth of the top layer was adjusted so that the average residence time in the directly heated section was 39 minutes and the total residence time was 94 minutes. Inject steam at a rate of 0-5kg/hr. Wet exit humidity is 12.1%-14.5%. The exit temperature is 75°C-85°C.

The cracked corn was then flaked using a Roskamp (Waterloo, Iowa) Model 2862 flaker. The tablet press has rollers 62 inches long by 28 inches wide. The master unit was set to rotate the fast roller at 300 rpm with an inner roller drive (IRD) rate of 8%. Keep roller pressure at 500 psig. The exit humidity of the tablet is 9.1%-11.7%, and the exit temperature is 60°C-83°C. The thickness of the sheet is between 0.3mm-0.7mm, and the gap of the roller is preferably set to 0.2mm (0.008 inches).

(B) extract

The flaked corn was processed with a Crown ^™ (Roseville, CA) Model II pilot extractor at a continuous 150 kg/hr. This pilot-scale extractor uses mixed hexane as the solvent and has five reverse trash wash sections and a tail wash section. Install 6 miscellaneous oil recirculation pumps together with fresh hexane at 50°C-60°C to the upper part of the extractor. The dimensions of the extractor are 29 feet long, 7.8 inches wide and 4.5 feet deep. 23 feet of the 29 feet extractor were wetted, of which 19.5 feet were washed. The average processing speed is about 75kg/hr. The residence time is about 60 minutes. The solvent to powder ratio was adjusted between 0.75:1 and 1.33:1. Send all miscellaneous oils to the oil desolventizer at 27°C-34°C.

(C) Powder to remove solvent

Peripheral and indirect heat desolvation was performed first in a Schnecken ^™ (Crown Iron Works, Roseville, CA) steam jacket conveyor (SJC). The SJC contains empty scraper screws in steam jackets (12 feet long and 10 feet in diameter). As the open scraper screw transports the oiled material through the conveyor, it creates an overturning action, ensuring that all material is exposed to the hot walls. A gas pressure regulator regulates the amount of steam supplied to the jacket. Regulate the temperature at the outlet of the conveyor and use this as the basis for controlling the steam supplied to the jacket. Vapor from the conveyor is collected in the low vacuum condenser by a small negative pressure created by the system fan. A double deck desolventizer and oven (DT) (36 inches in diameter, 20 inches high per deck) with a claimed 100 kg process capacity was used with rotating sweep arms. Steam is sprayed through the upper sweep arm only. The exit humidity of the powder is 9.4%-17.7%, and the exit temperature is 57°C-104°C. Hexane recovered from the SJC is condensed, dehydrated and recycled in the extractor.

(D) Oil desolventization

Oil desolvation was performed with a rising film evaporator (RFE). This apparatus contained 16 test tubes with a diameter of 1.5 cm in a large jacket. The jacket is filled with steam to heat the test tubes. The extracted load liquid (regular oil in hexane, known as miscellaneous oil) was charged to the bottom of the test tube. As it rises inside the test tube, the heat of the vapor causes the liquid to boil. The liquid-laden vapor leaves the tube wall to a thin rising membrane. At the top, liquid and vapor are separated. The oil flows into the overflow pipe to the oil wiper (OS), while the steam is carried to the condenser. The test tube is placed under vacuum so the liquid boils at low temperature.

The oil scraper is a disc and ring shaped distillation column. The liquid spreads out in a thin film inside the disc and drips into the ring at the back of the disc, which causes the oil to cascade in the column. At the same time, steam is passed through the bottom of the oil scraper, and the steam passes through the liquid, thereby removing the solvent remaining in the liquid. There is a vapor jacket for liquid and vapor insulation around the disc and annular column. Oil scrapers can also operate under vacuum. Hexane recovered from the rising film evaporator and OS is condensed, dehydrated and recycled in the extractor.

(E) Analysis of oil obtained from high oil corn

The oil is recovered and analyzed for vitamins, fatty acids and trace elements. As a control, 800 lbs. of yellow #2 corn was extracted in the same manner while the oil was recovered and analyzed for the same components. Vitamin A and beta-carotene are analyzed by a contract lab using a proprietary method. Other published procedures include Bates et al., Proc. Fla. State Hort Soc., 88, 266-271 (1975). On gas chromatography (GC), use CP88 cyanopropyl column (100m×0.265mm, 0.5mm film thickness) and flame ion detector according to American OilChemist Society (AOCS) method Ce 1c-82, Ce 2-65, Cd 3a- 94 and Cd 1c-85 for analysis of free fatty acids.

Tocopherols and tocotrienols were analyzed on a high performance liquid chromatography (HPLC, Waters 2590 type) using a conventional silica column with hexane-isopropanol as the mobile phase, and a fluorescence detector (Waters 2690 type), according to AOCSCe 8-89 described in the detection method. Lutein was analyzed by HPLC with C30 reversed-phase column with water-acetonitrile as mobile phase and detected with UV detector.

Table 15, shown below, presents a comparison of the oil composition obtained from high oil corn and yellow #2 corn. For comparison, the composition of oil from yellow #2 corn extracted by corn wet milling is also given.

Table 15 Element high oil corn yellow#2 Yellow #2, wet ground corn Palmitic acid% 11.4 10.7 10.7 Stearic acid% 2.2 1.9 2.0 Oleic acid % 35.6 25.5 27.5 Linoleic acid % 48 58.4 57.1 Linolenic acid % 0.7 1.2 1.1 α-Tocotrienol(ppm) 184 48 12 α-tocopherol (ppm) 237 231 136 Vitamin B1, mg/100g 0.390 NA 0.260 Vitamin B2, mg/100g 0.090 NA 0.080 Vitamin B6, mg/100g 0.82 NA 0.4 Vitamin B12, mg/100g 0.5 NA 0.5

Example 8

Recovery of lighter particles in the dehumidification step

This example outlines a method for recovering lighter particles (eg, fines) produced during the dehumidification step during the processing of high oil corn.

High oil corn was cracked and flaked as described in Example 7. Whole flaked corn resulting from the flaking process is heated to remove moisture using standard processing equipment, such as a Kice SSI model A2612 zigzag separator. During the dehumidification step, an adjustable airflow is controlled so that smaller and lighter particles can be entrained, thereby separating them from the heavier flakes. An example of such controlled airflow is the Crown ^TM multi-stage suction system, which can handle 2600 cubic feet per minute. Recover the lighter particles with standard disposal such as a baghouse. The recovered lighter granules are added to the starch-containing product stream to recover the starch.

Example 9

A method of recovering lighter particles with air during the crushing step

This example outlines a method for recovering lighter particles (such as fines) produced during the breaking step during the processing of high oil corn.

Whole kernels of high oil corn are broken using a standard breaker wheel such as the Roskamp 6.5 series (Waterloo, Iowa). During the crushing step, an adjustable airflow is passed over the crusher rollers and the speed of the airflow is adjusted so that smaller and lighter particles are carried along with the airflow, thereby separating them from the heavier particles. An example of such controlled airflow is the Crown ^TM multi-stage suction system, which can handle 2600 cubic feet per minute. Recover the lighter particles with standard disposal such as a baghouse. The recovered lighter granules are added to the starch-containing product stream to recover the starch.

Example 10

Method for recovering lighter particles with liquid spray

This example illustrates the recovery of fine powders produced before and after the tableting process by liquid spraying.

High oil corn was cracked and flaked as described in Example 7. The cracked corn before flaking and the corn flakes after flaking are sprayed or caged in a liquid with sufficient coverage to physically remove the lighter airborne particles. Water can be used as this liquid. Alternatively, the liquid spray can be a substance that increases the value of the final product and restores the value of the fine powder. Liquid sprays are usually pure water, process water or water with nutritional additives such as vitamins, enzymes or minerals. In all cases, the particle-laden liquid stream is carried away from the heavier particles and collected. Separate the particles from the liquid using standard processing equipment including hydrocyclones or centrifuges. Optionally, the recovered fine powder can be dried for further use. The recovered lighter granules are added to the starch-containing product stream to recover the starch.

Example 11

molded food

This example describes the manufacture of a biodegradable material with improved tensile strength using the expressed corn meal of the present invention.

The cornmeal of the present invention was suspended in hexane in a closed vessel at a cornflour:solvent ratio of 2:3. Let the mixture sit at room temperature for 18 hours without stirring. The organic solvent was removed from the extracted cornmeal, and the extracted cornmeal residue was washed with a fraction of hexane in a residue:solvent weight ratio of 1:1 during filtration. The residue was dried in a conventional oven at 50°C for 16 hours. Sprinkle water over the dried residue and stir until the residue has a moisture content of 10.7%-11.3%. The solvent-treated, extracted cornmeal composition was pressed at 5000 psi at 140° C. to 160° C. for 10 minutes using a pressure former (Wabash Metal Products, Inc., Wabash, Indiana) and molded into an ASTM standard dog bone shape. product (dogbone). The untreated cornmeal composition may have 10.7%-11.3% water incorporated and pressed into an ASTM standard dogbone shaped product. Products made with solvent-treated expressed corn flour had significantly improved tensile strength compared to unsolvent-treated expressed corn flour.

Alternatively, the corn flour of the present invention is separately suspended in an aqueous solution of ethanol (95%) at a flour:oil weight ratio of 1:3, and boiled for 2 hours while refluxing and mechanically stirring. The powder was filtered and the residue was washed with ethanol (1:1 residue:ethanol). The residue was dried, dehumidified and molded as above. The tensile strength and water absorption of powders treated with ethanol at boiling point for 2 hours were similar to powders treated at room temperature for 18 hours.

Example 12

ethanol production

(A) Starch Hydrolysis

Solvent extracted corn flour of the present invention prepared as described herein is a sufficient source of fermentable starch. One way to provide soluble sugars suitable for fermentation is to hydrolyze the starch molecules contained in solvent extracted corn flour. Make about 300g of corn flour prepared by the method of the present invention pass through a 1mm sieve, and mix them with 700ml of water at 99°C-100°C and 0.5ml of α-amylase in a closed container. The pH was adjusted to 5.9 with base. The mixture was stirred for 45 minutes and additional alpha-amylase was added. After 45 minutes of incubation, the pH of the mixture was adjusted to 4.5 with acid. Half a milliliter (0.5 ml) of glucoamylase (Optimax 7525) and 0.5 g of protease (FungalProtease 5000) were added and incubated with the two enzymes at 62°C for 22-24 hours. After this treatment, the degree of starch hydrolysis was detected on HPLC (Waters 2690 Separations module) with an organic acid column (Aminex HPX-87H ion exchange column, 300 mm × 7.8 mm, BioRad).

The total nitrogen content of each sample was determined with a Leco 2000 CN. Free amino acid nitrogen (FAN) was determined by the AOAC method (15th edition, 1990. p. 735). For comparison, cracked corn kernels were prepared and fermented in a similar manner. In Table 16 the amount of glucose produced from starch by comminution and the amount of amino acid obtained in the corn samples is listed. YDM represents the highest glucose content and HOC represents the lowest.

Both high oil corn (HOC) and high oil corn meal (HOCM) showed higher total nitrogen than yellow dent (YD) and yellow dent meal (YDM). HOC and HOCM contained more free amino acids than YD and YDM, respectively. In general, the grinding method was essentially the same for all samples, and the weight loss due to evaporation remained between 4% and 5%.

Table 16 corn sample Glucose (g/L) ^* FAN (ppm) Total nitrogen (ppm) YD 242.40 261.15 3437.6 YDM 311.28 195.84 4009.6 HOC 228.02 302.95 4916.0 HOCM 240.68 232.65 5032.0

^* Stated values are obtained after treatment with amylase and protease

(B) fermentation

Forty-five grams (45 g) of enzyme-treated corn grits and solvent-extracted corn meal (approximately 20% carbohydrates) were added to a 125 ml flask. Yeast extract was added at 1 g/L to ensure no nitrogen limitation. The culture was inoculated with 10% yeast from an overnight culture (a typical Altech ethanol yeast of Saccharomyces cerevisiae) and incubated for 42 hours at 30° C. on a rotary shaker at 125 rpm. Ethanol production was determined by HPLC.

Previous studies have shown that yeast grown on YD corn with a sugar content close to or above 25% did not achieve maximum ethanol production after 42 hours. Therefore, the fermentation medium is corrected on a weight basis so that the final fermented sugar content is about 20%. The initial glucose contents of cultures containing YD, YDM, HOC and HOCM were 212.21, 236.19, 187.85 and 222.77 g/L, respectively (Fig. 1). Cultures grown on HOC fully utilized the glucose present, while other cultures consumed glucose to a final concentration of less than 1 g/L. The fastest rate of glucose consumption was also observed in cultures grown with ground HOC. YD, YDM and HOCM cultures showed similar glucose utilization curves. The HOC and HOCM cultures exceeded 80 g/L ethanol but stopped production after 19 hours, which may be due to a lack of essential nutrients. No culture was able to reach 50% of the maximum theoretical ethanol production, however, the YD culture reached 45%, YDM 43%, HOC 41% and HOCM 38% (Table 17). The maximum ethanol production was relatively close, and it is possible that minimal growth condition adjustments accounted for this difference.

Examination of ethanol production showed that yeast grown on HOC produced the highest yield, producing more than 5 g/L/h of ethanol after 7 hours (Table 17). After 19 hours, the productivity of these cultures decreased, however all glucose was consumed before then. The remaining culture reached maximum productivity (greater than 4.5 g/L/h) after 19 hours. The ethanol production values for these four cultures were very similar.

Table 17 The fermentation medium is added with: Ethanol yield (g EtOH/g sugar) Ethanol production rate (g/L/h) 7h 19h 26 hours 42 hours 7h 19h 26 hours 42h YD 0.10 0.40 0.45 0.41 3.51 4.92 3.97 2.26 YDM 0.12 0.38 0.43 0.40 3.65 4.6 3.81 2.21 HOC 0.19 0.41 0.39 0.39 5.14 4.11 2.91 1.76 HOCM 0.11 0.38 0.36 0.36 3.78 4.6 3.22 2.01

To ensure that the acidic conditions created during fermentation did not affect yeast growth and subsequent ethanol production, the pH of the medium was adjusted (Figure 2). After a period of time, the pH of all cultures decreased in a similar trend, with a final pH between 3.75 and 3.9. No significant pH fluctuations would cause differences in ethanol production.

Example 13

Aquafeeds containing cornmeal derived from high oil corn

This example outlines the use of extracted cornmeal in aquafeed products.

Two rearing methods were used for two species of fish:; tilapia (tillapia) and catfish. One feeding method is to use a feed containing corn grits obtained from dry-ground yellow corn. Another feeding method uses a feed containing ECM from high oil corn. The feed was manufactured with the following ingredients (Table 18):

Table 18

Composition Percentage

Herring Meal 8

Soybean flour 50

Corn 34.3

Wheat semolina 5

Dicalcium Phosphate 1

Vitamin Blend 1.5

Trace element mixture 0.2

Crude protein (N×6.25) 32

In the feed rations shown in Table 18, oil-extracted corn meal (ECM) can be substituted at various levels for some or all of the corn, some or all of the wheat meal, and/or some of the soybean The desired nutritional profile varies with the species of fish.

A group of tilapia were fed a diet containing oil-extracted cornmeal. Another group of tilapia were fed a diet containing corn grits. Likewise, one group of catfish were fed a diet containing oil-extracted cornmeal and another group of catfish were fed a diet containing corn grits.

The experimental design used 4 pounds per treatment and 1 pound per 100 fish, for a total of 16 pounds and 1,600 fish. Each fish has an approximate size and weight. In each species and in each treatment, the fish were fed at a feeding rate necessary to meet growth rates typical in conventional aquaculture production. Raise fish from one finger to a size that reflects conventional market weight (eg, about a pound or half a pound).

Catch the fish and use a method to create visually comparable fillets. Tissue color can be determined using a color reference guide to assess the effect of extracted cornmeal on meat quality. Let trained and experienced sensory testers estimate consumer preference factors such as color and appearance.

The process of producing extracted corn meal separates some solvent-soluble colorants from the meal. Thus, fish fed oil-extracted cornmeal received less pigment in their diets than fish fed a diet containing corn. When pigments such as carotenoids are included in the feed, they can settle in tissues. Consequently, fish fed diets containing extracted cornmeal had lighter-colored tissues compared to fish fed diets containing corn. Growth of fish fed diets containing extracted cornmeal was similar to that of fish fed diets containing corn, but adjustments to the ratios of ration ingredients may be required to optimize starch digestibility, amino acid availability, and and fatty acid content vary.

Example 14

Biodiesel Containing Corn Oil From High Oil Corn

This example describes the use of oil from high oil corn as a source of improved biodiesel fuel.

In a continuous process, approximately 62 kg/hr (137 lbs/hr) of oil extracted from high oil corn and refined by known industrial methods was mixed with 18 kg/hr (40 lbs/hr) of methanol in a stirred tank reaction unit. At the same time, 0.08 kg/hr (0.1775 lbs/hr) of sodium hydroxide was added to the stirred tank reaction unit, which was operated at 20 psig and about 80°C. These conditions can convert added triglycerides to fatty acids and methyl esters with 100% conversion.

The two phases of the reaction mixture were allowed to stand and separated to obtain the methyl ester in the upper phase and glycerol and about 10-15 wt.% of the residual methyl ester, methanol and base mixture in the lower phase. Approximately 6.4 kg/hr (14 lbs.hr) of the glycerol phase was neutralized, the methanol was flashed off, and the residue was sent to a continuously stirred reaction unit operating at 320 psig and 80°C. This reaction unit also contained about 4 wt. % Amberlyst-15 catalyst with a residence time of 2 hours and about 7.9 kg/hr (17.5 lbs/hr) of isobutene was fed into the reaction unit. Biodiesel fuel is produced at a rate of approximately 66 kg/hr (145 lbs.hr), with a dynamic viscosity and cloud point greater than current biodiesel without glycerides.

All references cited herein, including publications, patent applications, and patents, are hereby incorporated by reference to the same extent as if each individual reference was individually and specifically indicated to have been incorporated by reference in its entirety Same.

Use of the terms "a" and "the" and similar words in the text describing the invention (especially in the following claims) should be construed to include both the singular and the plural unless otherwise stated herein or otherwise clearly contradicted by context. Recitation of ranges of values herein are merely intended to serve as a shorthand method of referring individually to each separate value falling within the range, unless otherwise indicated herein, and each separate value is incorporated into the specification as if it were individually stated herein. All methods described herein can be performed in any suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (eg, such as) provided herein, is intended merely to better illuminate the invention and should not be construed to limit the scope of the invention unless otherwise claimed. No language in this specification should be construed as identifying any non-claimed element as essential to the practice of the invention.

Preferred embodiments of this invention are described herein, including the best mode known to the inventors for carrying out the invention. Of course, variations of those preferred embodiments will become apparent to those of ordinary skill in the art upon reading the foregoing description. The inventors expect skilled artisans to employ such variations as appropriate, and the inventors intend for the invention to be employed other than as specifically described herein. Accordingly, this invention includes all modifications and appended equivalents of the subject matter recited in the claims as recognized by applicable law. Moreover, unless otherwise indicated herein or otherwise clearly contradicted by context, all possible combinations of the above-mentioned elements are also encompassed by the invention.

Claims (48)

1. Semen Maydis powder remaining behind the complete high oil corn extract oil.

2. Semen Maydis powder as claimed in claim 1 is characterized in that the oil-contg of complete high oil corn is about 6wt.% or higher.

3. Semen Maydis powder as claimed in claim 1 is characterized in that oil-contg is about 7wt.%-30wt.%.

4. Semen Maydis powder as claimed in claim 2 is characterized in that, before the extract oil, complete corn is softened.

5. Semen Maydis powder as claimed in claim 4 is characterized in that, before the extract oil, the remollescent corn is broken.

6. Semen Maydis powder as claimed in claim 5 is characterized in that, before the extract oil, broken corn is by compressing tablet.

7. Semen Maydis powder as claimed in claim 5 is characterized in that, before the extract oil, the remollescent corn is broken.

8. Semen Maydis powder as claimed in claim 7 is characterized in that, before the extract oil, broken corn is wetted.

9. Semen Maydis powder as claimed in claim 8 is characterized in that, before the extract oil, broken corn is by compressing tablet.

One kind processing complete high oil corn method, it comprises:

1) will soften and broken complete high oil corn wetting.

2) with the complete high oil corn compressing tablet of fragmentation; And

3) extraction is pressed into the corn of thin slice to make Semen Maydis powder and Semen Maydis oil.

11. method as claimed in claim 10, it further comprises complete high oil corn remollescent step.

12. method as claimed in claim 11 is characterized in that, wetting step is that complete high oil corn is being carried out before the softening step.

13. method as claimed in claim 10, it further comprises the step with complete high oil corn fragmentation.

14. method as claimed in claim 11, it further comprises complete high oil corn remollescent step.

15. method as claimed in claim 13 is characterized in that, broken step is to carry out before with the wetting step of complete high oil corn.

16. method as claimed in claim 14 is characterized in that, broken step is after softening step, and before complete high oil corn is carried out wetting step, carry out.

17. method as claimed in claim 10 is characterized in that, the oil-contg of complete corn is about 6wt.% or higher.

18. method as claimed in claim 10 is characterized in that, the oil-contg of complete corn is about 7wt.%-30wt.%.

19. method as claimed in claim 10 is characterized in that, extraction step is to finish by extracting Semen Maydis oil with continuous solvent-extraction process from the corn grain that is pressed into thin slice.

20. method as claimed in claim 19 is characterized in that, the corn that is pressed into thin slice contacts one period that is enough to extract the oil of aequum with solvent.

21. method as claimed in claim 19 is characterized in that, the corn and the solvent that are pressed into thin slice kept in touch 10 minutes at least.

22. method as claimed in claim 10 is characterized in that, the thickness of thin slice is about 0.1mm-1.0mm.

23. method as claimed in claim 19 is characterized in that, contains hexane in the solvent.

24. produce the alcoholic acid method for one kind, it comprises:

1) with Semen Maydis powder as claimed in claim 1 and water and α-Dian Fenmei mixing;

2) cultivate mixture and in mixture, add at least a additive; And

3) mixture is mixed to produce ethanol with microorganism that can fermenting carbon source.

25. method as claimed in claim 24 is characterized in that, additive is selected from glucoamylase and proteolytic enzyme.

26. biofuel that contains the Semen Maydis oil that makes by extract oil from complete high oil corn.

27. the method that produces in the process that is recovered in the processing high oil corn than light grains, it be included in feed air-flow on the high oil corn particle so that lighter particle along with air-flow is taken out of, thereby particle that will be lighter and heavier particle separation.

28. method as claimed in claim 27 is characterized in that, gas is selected from air, nitrogen and argon gas.

29. the method than light grains that produces in the process that is recovered in the processing high oil corn, it is included in and feeds liquid spray on the high oil corn particle taking lighter particle out of, thus particle that will be lighter and heavier particle separation.

30. method as claimed in claim 29 is characterized in that, liquid spray is a water.

31. method as claimed in claim 30 is characterized in that, liquid spray further contains at least a composition that is selected from VITAMIN, mineral substance, enzyme and their combination.

32. method as claimed in claim 31 is characterized in that, liquid spray further contains caustic liquor.

33. biodegradable product that origin is made from the Semen Maydis powder through solvent extraction of high oil corn.

34. biodegradable product as claimed in claim 33 is characterized in that the Semen Maydis powder of solvent extraction is handled through organic solvent.

35. biodegradable product as claimed in claim 33 is characterized in that the Semen Maydis powder of extraction is further handled through linking agent.

36. biodegradable product as claimed in claim 35 is characterized in that, linking agent is selected from aldehyde, acid anhydrides, epoxide or their combination.

37. feed that contains the Semen Maydis powder that makes by the oil of solvent extraction from complete high oil corn.

38. feed as claimed in claim 37 is characterized in that, feed is animal-feed or aquaculture feed.

39. feed as claimed in claim 38 is characterized in that, animal-feed is the chicken feed.

40. feed as claimed in claim 39 is characterized in that, feed is an aquaculture feed.

41. extract Semen Maydis oil from the laminar corn gained of complete oily corn.

42. Semen Maydis oil as claimed in claim 41 is characterized in that, the oil-contg of complete high oil corn is about 6wt% or higher.

43. Semen Maydis oil as claimed in claim 42 is characterized in that oil-contg is about 7wt.%-30wt.%.

44. Semen Maydis oil as claimed in claim 42 is characterized in that, extracts to be pressed into before the corn of thin slice, complete corn is softened.

45. Semen Maydis powder as claimed in claim 44 is characterized in that, extracts to be pressed into before the corn of thin slice, the remollescent corn is broken.

46. Semen Maydis powder as claimed in claim 45 is characterized in that, extracts to be pressed into before the corn of thin slice, broken corn is by compressing tablet.

47. Semen Maydis powder as claimed in claim 45 is characterized in that, extracts to be pressed into before the corn of thin slice, the remollescent corn is broken.

48. Semen Maydis powder as claimed in claim 47 is characterized in that, extracts to be pressed into before the corn of thin slice, broken corn is wetted.

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