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MXPA99005362A - High temperature countercurrent solvent extraction of capsicum solids - Google Patents

High temperature countercurrent solvent extraction of capsicum solids

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Publication number
MXPA99005362A
MXPA99005362A MXPA/A/1999/005362A MX9905362A MXPA99005362A MX PA99005362 A MXPA99005362 A MX PA99005362A MX 9905362 A MX9905362 A MX 9905362A MX PA99005362 A MXPA99005362 A MX PA99005362A
Authority
MX
Mexico
Prior art keywords
solids
extract
edible
capsicum
pressing
Prior art date
Application number
MXPA/A/1999/005362A
Other languages
Spanish (es)
Inventor
N Todd George
Original Assignee
Kalamazoo Holdings Inc
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Filing date
Publication date
Application filed by Kalamazoo Holdings Inc filed Critical Kalamazoo Holdings Inc
Publication of MXPA99005362A publication Critical patent/MXPA99005362A/en

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Abstract

Principal components of paprika, red pepper, pungent chili, or other spice plants, e.g., of the genus Capsicum containing carotenoid pigments, are simultaneously extracted and concentrated with an edible solvent in a series of mixing and high temperature and pressure mechanical pressing steps using edible solvent and a countercurrent extraction procedure. The extract containing the carotenoid pigments may be hydrated and then centrifuged to remove fine particulate solids and gums. A solution having several times the concentraton of the carotenoid pigments and other flavor and aroma components of the starting raw material is obtained. The residual press solids may be cooled and hydrated following the last pressing operation.

Description

EXTRACTION BY SOLVENT TO COUNTERCORRIENT, TO HIGH TEMPERATURE, OF SOLIDS. OF CAPSICUM FIELD OF THE INVENTION The extraction of the main significant components of spice plats, especially of the Capsicum genus, ground pepper, red pepper and chili, representatively, containing carotenoid pigments using food-grade, edible solvent.
BACKGROUND OF THE INVENTION AND PREVIOUS TECHNIQUE The present invention relates to a method for increasing color stability and reducing the microbial count of spice oleoresin, for example, Capsicum, and the residual cake from which the oleoresin has been extracted. The process simultaneously extracts and concentrates the flavoring, flavoring, coloring and other major active compounds of the Capsicum genus, produces a concentrated and standardized food grade extract of active compounds, and a standardized food grade residual solid, with both the extract and the residual solids having improved resistance to color loss and having significantly reduced microbial counts.
REF .: 30478 Concentrated extracts of the genus Capsicum, are universally used to flavor and color foods, beverages and drugs. These extracts are traditionally used where a standardized, sterile and uniform concentrate offers the control benefits that are inherently difficult to obtain from raw spices, or where the raw material volume is not necessary or undesirable. Capsicum solids are universally used to flavor, color and impart other favorable characteristics to foods and beverages, where the volume, functional characteristics and appearance of the food or drink is important. The traditional extraction processes for the manufacture of concentrated extracts (concentrated several times in comparison with the raw material) imply not only the use of several inedible solvent systems, but also a large proportion of the solvent in relation to the compounds of interest. Many require the use of petroleum distillates, chlorinated solvents or highly flammable solvents, which must be almost completely removed from the finished products to make them safe for consumption. These systems require expensive distillation equipment, and special precautions must be taken to ensure worker safety, and to limit environmental impact. The intensive processing required, often destroys, modifies, or causes to lose some of the most unstable compounds, delicate flavors, flavors or pigments. More significantly, the last traces of undesirable inedible solvents are difficult to separate from the concentrated extract. The residual solid must necessarily contain the same residual inedible solvents, which are removed only with difficulty. Such residual solvents limit the potential use of the residual solid for human consumption, and are potential environmental contaminants. Other concentration techniques depend on the high-pressure equipment to obtain good solvation properties of the gases, for example, liquid or supercritical C02 (US Pat. No. 4,490,398). Extraction by high pressure or supercritical liquefied gas requires expensive equipment and has limited solvation capacities for some compounds that require the addition of cosolvents, or solvents such as propane and butane, which are also difficult to control and can be environmentally sensitive or undesirable in a finished product. After extraction and desolvation, the concentrated extract is often standardized with edible solvents and emulsifiers to provide a concentrate with reproducible levels of the active or major compounds of interest to the user. In an effort to overcome the drawbacks and risks associated with the processes mentioned above, the extraction has been carried out using edible solvents such as vegetable oils and lard. Typical extraction procedures are described in US Pat. Nos. 3,732,111; 2,571,867; and 2,571,948. These methods require a relatively large volume of solvent relative to the compounds of interest and result in a dilute extract, which is limited in its application, and which has few of the advantages of the concentrates that can be produced using volatile solvents. USP 4,681,769 describes a method for simultaneously extracting and concentrating in a series of mechanical processes in countercurrent, at high pressure, using relatively small quantities of edible oil as a solvent in an attempt to overcome the dilution problem inherent in the above processes. This method suffers from severe limitations in temperature and pressure ranges in an attempt to avoid unacceptable oxidative damage, loss of color, loss of performance, and taste changes with the end result being that contact times must be unduly prolonged to 16 -24 hours, adding greatly to the cost of the process. The extraction cycle times are unduly prolonged for a pressing operation of a given size, and the process does not provide a controlled degree of browning or sterilization of the extract or residual solid. This is also limited to temperatures of less than 37.77 ° C (100 ° F), and thus does not allow the use of edible solvents that have a melting point of more than 37.77 ° C (100 ° F) or that are highly viscous at temperatures below 37.77 ° C (100 ° F). It is said that maximum pressures of up to about 35.15 kgf / cm2 (500 PSI) (conical pressure), severely limit the efficiency and performance for a given size pressing operation, as the description of this patent shows. Traditional methods for the sterilization of ground spices, including Capsicum, involve the use of extremely toxic substances, such as ethylene oxide and methylene bromide, irradiation, or steam and wet treatment to reduce the plate count to less than 100,000. The chemical sterilization and irradiation of the spices are unpleasant to the consumer, due to the perceived risk of residual chemical compounds and / or radiation remaining in the plant material and, as a result, several processes using added moisture, such as water or steam, have been developed. , at high pressures, as alternatives. Typical sterilization procedures are described in U.S. Patent Nos. 4,210,678, 4,790,995, and 4,910,027. All sterilization processes are inherently expensive since they require a separate processing step or steps to achieve sterilization, and also present the possibility of further degradation of the most unstable components. In addition to moisture or water vapor, as described in U.S. Patent Nos. 4,210,678 and 4,910,027, before or during the heating and sterilization process results in a non-typical baked flavor of the fresh, dehydrated spices and also results in a steam distillation and loss of some of the volatile aromatic and flavor constituents. U.S. Patent Nos. 4,790,995 and 4,910,027 require the addition of an animal protein coating to protect the spice from the loss of the volatile aromatics during the steam sterilization process. US Patent No. 4,210,678 requires bringing spice moisture to about 8-14%, in some cases up to 16-20%, and keeping the spice for a prolonged period of time before sterilization to balance moisture. This additional step is expensive and time consuming. In the case of Capsicums, severe browning and loss of aromas and flavors develops in the presence of units exceeding 8% at elevated temperatures above -82.22 ° C (180 ° F). Traditional methods to control the browning or degree of caramelization of Capsicum, to improve its visual appearance, involve the use of elevated temperatures and the addition of vegetable or animal fats or oils to color and polish the surface of the ground spice. This requires a separate and expensive processing operation. In all of the above, there is the unresolved problem of obtaining satisfactory yields, quality and production rates of acceptable extracts having an acceptable content of active ingredient in the edible solvent without undesirable oxidative damage to, and reduced stability of, the main compounds of interest, and at the same time to provide simultaneous sterilization of the solids and spice extracts. Obviously, the existing prior art methods leave much to be desired, and the main objective of the present invention is to provide a process for the production of Capsicum products which have improved color stability and which in other circumstances obviates the drawbacks of the art. previous.
OBJECTS OF THE INVENTION Accordingly, an object of the present invention is to provide a process for rapidly and simultaneously extracting and concentrating the main Capsicum solids components, at temperatures of at least 54.44 ° C (130 ° F), preferably from 54.44 (130 ° F) to approximately 232.22 ° C (450 ° F), in a process which is completely free of petroleum, chlorinated or highly flammable, which does not require equipment that handles high pressure gas, which does not require distillation for solvent removal, which uses only edible food grade solvents, which are typically used commercially to standardize the resulting extract to a desired concentration, and provide a product, which is free from adulterants and impurities. Another object of this invention is to prepare such concentrated extract by a process which is simple, environmentally friendly and economical. A further object of this invention is to prepare a residual solid or press cake, which is edible, is free of residual petroleum distillates, chlorinated solvent or other adulterants, which was standardized with respect to the main components of commercial interest, which has a predictable and controlled degree of browning or caramelization, and which has a controlled level of water activity with its increased resistance aimed at oxidative deterioration of the carotenoid pigments and loss of color. A further object of this invention is to provide a process wherein antioxidants can be added to the edible solvent system to protect the concentrated extract and the residual solids against the oxidative degradation of the main components of interest, ie flavor, aroma and color, that are extracted from the raw plant material or left in the residual solids. Still another object of the invention is to provide an edible extract and an edible residual solid with reduced microbiological activity by a process wherein the moisture of the Capsicum spice remains below 8%, thus avoiding the loss of constituents flavorings and volatile aromatizers and preventing the development of uncontrolled browning and development of loss of flavor at temperatures greater than 54.44 ° C (130 ° F), which are necessary to obtain high efficient extraction, reduced microbial activity and improved stability of the carotenoid pigments in both the extract and the residual solids. Still another object of this invention is to prepare an extract with greater resistance to the oxidative degradation of the carotenoid pigments and the consequent loss of color. Other objects will be apparent to one skilled in the art to which this invention pertains and others will still be apparent here later as the description proceeds.
BRIEF DESCRIPTION OF THE DRAWINGS FIGURE 1 illustrates the process of the present invention, which includes the different process steps involved in the simultaneous extraction and concentration of Capsicum solids, to produce the desired sterilized residual extract and solid, both of which It has greater resistance to oxidative degradation, and which can be easily standardized to the desired levels of the components of interest. Although the illustrated process comprises three extraction steps, the number of steps can be decreased to two or increased to more than three, to effect the concentration of the desired main relative component in the extract and in the residual solid. FIGURE 2 illustrates the relationship between water activity and the relative lipid stability of food systems as described - incorrectly in the current literature and as it is currently.
BRIEF DESCRIPTION OF THE INVENTION The invention, consequently, inter alia, comprises the following, alone or in combination: A process of continuous mixing of multiple stages, pressed at high pressure and countercurrent extraction for the production of a concentrated edible extract and edible residual solids, both with a reduced bacterial content, with the extract having greater resistance to oxidative deterioration of the carotenoid pigments thereof, and both of which contain carotenoid pigments, flavor and aroma, of solids of plant material of the genus Capsicum, comprising the following steps: subjecting the Capsicum solids to a countercurrent extraction process involving a plurality of mixing and pressing stages, including first and second Last mixing steps and first and last pressing steps, together with five to about fifty weight percent of an edible solvent, to produce a residual extract and solid, continuously return the extract from each pressing step to the pre-mixing stage , and finally separate the extract from the first - pressing stage and separates r the residual solids of the last pressing step, all the pressing steps are carried out at a temperature of at least 54.44 ° C (130 ° F); such as a process, where the temperature is 54.44 (130), up to about 232.22 ° C (450 ° F); such as a process, where Capsicum solids are subjected to internal pressures in the pressing stages of at least 421.8 kilograms force per square centimeter (6,000 pounds per square inch); such as a process, wherein the weight of the edible solvent is from 5% to about 20% by weight of the Capsicum solids; such as a process, wherein the moisture content of the starting Capsicum solids is less than 6% by weight, and where the reduction of the bacterial count is carried out at this low moisture content, thereby avoiding the undesirable loss of volatile flavoring and flavoring constituents and preventing the development of baked flavors and aromas that occur at high moisture contents; such as a process, in which the Capsicum solids extracted in the process are selected from the group consisting of ground hot pepper, red pepper and chili; such as a process, wherein the edible solvent is selected from the group consisting of soybean oil, corn oil, cottonseed oil, rape seed oil, peanut oil, mono-, di- or triglycerides, lecithin, edible essential oils, sesame oil, edible alcohols, hydrogenated or partially hydrogenated fats or oils, polyoxyethylene sorbitan ethers, limonene, fats or edible animal oils, mixtures thereof, and edible derivatives thereof; such as a process, wherein the fine particulate solids are filtered or centrifuged from the extract and alternatively discarded, returned to a stage of mixing or processing the process, or incorporated into the final residual solids; such as a process, which includes the steps of hydrating the final extract by adding water in a degree of 5% to 200% by weight of the gums, and fine particulate solids included in it, and filtering or centrifuging to remove the gums and solids; such as a process, which includes the step of returning the hydrated gums and separated solids to the final residual solids; such as a process, which includes the step of rehydrating the final residual solids with water to a water activity greater than 0.3 Aw for the color stabilization thereof; such as a process, where the solids are rehydrated to a water activity of about 0.4 to 0.6 Aw; such as a process, wherein an effective color stabilizing amount of an antioxidant or edible chelator is included in an edible solvent; such as a process, wherein the antioxidant comprises an antioxidant selected from the group consisting of lecithin, ascorbic acid, citric acid, tocopherol, ethoxyquin, BHA, BHT, TBHQ, tea catechins, sesame, and the antioxidant activity of an herb of the family Labiatae; such as a process, wherein the antioxidant comprises an antioxidant which is found in the nature of an herb of the Labiatae family or powdered ascorbic acid; such as a process, wherein the antioxidant comprises the antioxidant activity of an herb selected from the group consisting of rosemary, thyme and sage, and such a process, wherein the temperature is above 82.22 ° C (180 ° F), and preferably between about 82.22 ° C (180 ° F) and about 112.22 ° C (235 ° F). In addition, an extract of plant solids of the Capsicum genus, produced by the process that has greater color stability due to the high temperature used in its production; such as an extract of plant solids of the genus Capsicum, produced by the process that has a high color value and low bacterial count, due to the high temperature used in its production, and due to the water content of less than 6% in the starting Capsicum solids; and solids of the rehydrated cake produced by the extraction of the Capsicum solids according to the process that has a high degree of stability due to the high temperature used in the production thereof and due to the level of water activity Aw present in them; and an extract of a plant of the genus Capsicum, produced by the process in the form of a clear solution with gums and particulate solids therein, converted to its soluble hydrates and then removed from the extract; and a hydrated extract of a Capsicum plant, produced in the process and having gums and particulate solids therein in its insoluble hydrated form; and finally an extract of plant solids the genus Capsicum, which has improved color stability, produced according to the process due to an edible antioxidant in it.
THE PRESENT INVENTION IN GENERAL Raw Capsicum spice solids, either ground (usually to pass a US 40 mesh, and preferably to pass at least one US 20 mesh) or unground if coarse particles are desired in the solid or residual cake, for example, Capsicum solids having a moisture range of from about 0.5% to 16% by weight, preferably 0.5% to 8% by weight, and more preferably from 1.5% to 6% by weight ( ASTA 2.0 method), is subjected to a mixing step, preferably high cutting, and at least one stage of edible solvent is perfectly dispersed through the solids of the vegetable raw material. The vegetable raw material of typical Capsicum includes, for example, but without limitation, dried ripe fruits of Capsicum frutescens L. (Chiles), Capsicum annum L. (Spanish peppers), Capsicum annum L. var. Longum Sendt, its Mutant Hybrid Pepper from Louisiana, and Chinese Capsicum (Scottish or Habanero cap), all by way of example and not by way of limitation. The crushed or non-crushed plant material is subjected to a plurality of mechanical processing steps, whereby a concentrated extract of the main components is obtained and a final residual solid is produced which can be used and preferably standardized. The selected edible solvent is introduced into the residual solid in a mixing step at the same point before the last pressing stage. The edible solvent, which now contains extract, is cycled back to the previous stage, thus always supplying a solvent extract with a concentration of the main component increasing to the previous mixing or pressing steps. When the extract / edible solvent is it passes through each stage upstream against the flow of solids, a portion of the edible solvent is squeezed or pressed, thereby extracting a portion of the major components of interest. When the edible solvent / extract passes countercurrent to the solids, the extracted main components are progressively concentrated in the extract in a continuous process and the residual main components that end up in the final residual solids are known as the cake. By varying the pressure, temperature, spice solids feed rate, solvent addition rate, and the number of mixing and pressing steps, the concentration of the major components in both the extract and the residual solid can be controlled.
As will be apparent to those skilled in the art, variations in the present process can be employed to produce variations in the result, the most advantageous of which are the production of extract of the plant material of remarkable potency and edible residual solid plant material as well. characterized by a remarkable power. For example, using 200 ASTA milled hot pepper stock with approximately 5% moisture, a 20% addition of soybean oil, and leaving a removable residual cake with a yield of 9.8% by weight of vegetable solids material. Starting, you get an extract with a color value of 850 ASTA and a color value of the residual cake of approximately 50 ASTA. In contrast, using a 10% soybean oil addition (instead of 20%) a cake is obtained having a color value of about 65 ASTA e, increasing the extractable residual cake to a yield of 12.5% by weight of the starting vegetable solids material, the color value of the residual cake is raised to approximately 100 ASTA and that of the extract to approximately 1400 ASTA. The lowest colored extract for the spicy ground pepper commonly marketed is 1,000 ASTA. Although less than 20% of the edible oil addition is highly desirable and can be used in many cases, with some edible solvent systems where the main components of interest have a limited solubility, or when a more dilute extract and / or lower concentration of the major compounds in the residual solids is desired, more than 20% by weight addition of edible solvent will be required given that the proper concentration of the major components in the finished extract and in the residual solid it can in some cases be produced only by the use of a higher dilution. Due to the successive treatment of high pressure and pressure release, with pressures ranging from 421.8 to 2109 kgf / cm2 (6,000 to 30,000 PSI) in the pressing stages of the operation, in the presence of added edible solvent, for example, oil plant, and due to the frictional heat generated in those high-pressure zones, both the residual solid and the extract coming out of the process surprisingly have a significantly reduced microbial load compared to the starting material even at significantly lower moisture levels than those indicated by the prior art and, also surprisingly, exhibit greater resistance to the oxidative degradation of the carotenoid pigments, which are responsible for the yellowish-red color characteristic of Capsicums.
The extract from the first or any selected stage of the pressing can be centrifuged or filtered to provide the finished extract free of particulate solids. Preferably, the fine particulate solids and gums in the extract can be hydrated from about 5% to 200% by weight of the gums and solids before centrifugation or filtration to give a clear crystalline extract. If water is not used to hydrate the solids and gums, the fine particulate solids of the extract can be conveniently combined with the final residual solids, recycled back to the mixing and pressing steps of the process, or alternatively, discarded. If water is used to hydrate the solids and gums, it is preferred that the solids and gums be added back to the final pressed or discarded solids. The edible solvent used according to the process of the present invention, according to the process of the present invention, according to what is illustrated by the following examples, can be any edible solvent, especially those selected from the group consisting of soybean oil, corn oil, cottonseed oil, rape seed oil, sesame oil, peanut oil, mono, di, and triglycerides, lecithin, essential oils of spices, herbs, or other plants, edible alcohols, propylene glycol, glycerin, hydrogenated or partially hydrogenated fats or oils, limonene, polyoxyethylene sorbitan esters, or any other edible vegetable or animal fat or oil, or mixtures thereof, or edible derivatives thereof, the essential aspects of the solvent are that they serve as an extraction aid in which the main components of the material being extracted are soluble and that is edible. The edible solvent, according to the present invention, is combined with the solids of the raw material to be processed in a proportion of about 5% to about 50% by weight, and often in amounts as low as 5 to 20% in weight they are possible, based on the weight of the solids of the starting raw material to be extracted. The lower percentages frequently produce a more acceptable and remarkable concentration of major components of interest in both the extract and the residual solids. The temperature to be employed during processing and especially in the pressing steps of the process of the invention can vary widely, but the process is generally carried out at a temperature below about 232.22 ° C (450 ° F), and between about 54.4 ° C and 162.8 ° C (130 ° F and 325 ° F), more preferably above 82.22 ° C (180 ° F) and especially between about 82.22 ° C and 112.8 ° C (180 ° F and 235 ° C) F). Temperatures exceeding 54.4 ° C (130 ° F) are advantageously employed to achieve acceptable yields and higher production speeds compared to the prior art. Higher temperatures are used to control an increasing degree of browning and, more importantly, to reduce the microbial load of both the solids and the extract and at the same time to impart greater resistance to the oxidative degradation of the carotenoid pigments both in the extract as the residual solids. In this way, when it is desired that the residual solids of the process have a darkened, caramelized and / or desirable appearance, a reduced microbial load, a greater resistance to oxidation, this is easily obtained by increasing the temperature of the solids and the extract. during the process, especially during the pressing stages of the same. When an oxidant or chelant is introduced into the process for the protection of the species being processed, this is preferably another plant material or an extract thereof, preferably from the Labia tae family., such as rosemary, thyme, or sage, which are known for their protective antioxidant activity (USP 5,209,870) or sesame, or tea catechins, but can, alternatively, be an adequate and preferably approved edible food grade additive such such as ethoxyquin, BHA, BHT, TBHQ, tocopherol, Vitamin C (for example, as in US Pat. No. 5,290,481, 5,296,249, or 5,314,686), citric acid, EDTA, or the like. The process of the present invention is particularly adaptable to the extraction of any solids of Capsicum plant material containing carotenoid pigments or other components which provide color and / or taste, spicy flavor, or aroma to a food with which they are combined.
DETAILED DESCRIPTION OF THE INVENTION The following examples are given to illustrate the present invention but do not constitute a limitation.
Example 1, Extraction of Ground Hot Pepper Dehydrated Ground Hot Pepper (5.5% moisture) is milled in a hammermill and the resulting ground shredded hot pepper (95% of which passes through a US 40 mesh) is mixed with about 10% by weight of soybean oil and processed in a countercurrent extraction system involving three (3) pressing stages, each of which uses a Screw Press Model KEK-100 by Egon Keller, with the extracts of the second and third stage being returned to the preceding mixing stage before being removed from the process at the end of the first pressing step. A high-cut, high-speed equivalent pin mixer is used to mix the soybean oil or the extracts of the second and third pressing stages in the ground or residual solid spice of the preceding step. This recycling is continuous. The hot pepper solids milled in the raw material are fed continuously at a rate of approximately 108.96 kilograms per hour (240 pounds per hour) with a cake contact time in each mixing stage of approximately 15-60 seconds. The residence time in each press is 5-60 seconds. The pressing steps are operated at an internal pressure of approximately 703 kgf / cm2 (10,000 PSI) and up to approximately 93.3 degrees centigrade (200 degrees Fahrenheit), which is kept cooling with water through the hole in the press shafts. The starting color value of the ground shredded hot pepper solids is 200 ASTA. The main extracted and standardized components of both the extract and the residual solid are the carotenoid pigments. The resulting final milled hot pepper-soy extract has a color value of about 1.375 ASTA and the residual hot ground pepper crushed in the (3rd) final pressing step has a color value of about 85 ASTA.
Example 1A - Variation: By varying the percentage of edible solvent used of. approximately 5% to 20%, the pressure of approximately 421.8 to 210.9 kgf / cm2 (6,000 to 30,000 PSI), the number of stages of mixing and pressing upstream from 2 to 5, with the return of the extract from each pressing step to the preceding mixing stage before the final removal of the process in the first stage of the pressing, varying the temperature from approximately 54.4 ° C to 137.8 ° C (130 ° F and 280 ° F), and removing the seed from the solids of ground hot pepper before grinding, the resulting extract fluctuates in color value from approximately 2,700 ASTA to approximately 800 ASTA and the residual solids range in color value from 180 ASTA to 35 ASTA. By grinding again the residual solids (from the final stage) just as it was done with the fresh, dehydrated ground pepper, a product is produced in some way comparable to the commercially available crushed ground pepper solids available. After filtering or centrifuging the fine particulate solids, the extract can be directly substituted for the commercially available hot ground pepper oleoresin available in each aspect. By varying the process pressing temperature of approximately 54.4 ° C and 162.8 ° C (130 ° F and 325 ° F), the tone of the regrind residual solids varies from slightly brown to a dark chocolate brown, demonstrating that the degree of browning it can be controlled by the pressing temperature used. The degree of "browning" is measured using a Hunter Labscan Spectrocolorimeter with an illumination of 0 degrees, a circumferential view of 45 degrees, illuminant D65, with observer at 10 degrees, a coordinate system Ceilab. The pitch of ground pepper powder is measured by placing the powder in a 6.35 centimeter (2.5 inch) diameter bucket, shaking gently to ensure uniform coverage, and measuring through the bottom of the bucket. The results of the variable operating temperatures of the process are shown in Table I. The designation L * is indicative of the "luminosity" of the sample with the larger numbers being lighter or less brown, and the lower numbers being more dark or more brown. Processing Temperature Visual Appearance Values of L * 54. 4 ° C (130 ° F) Red 40.18 65.6 ° C (150 ° F) Tan-Red 37.25 93.3 ° C (200 ° F) Light Brown Red 33.22 137.8 ° C (280 ° F) Red Brown 29.16 Dark 162.7 ° C ( 325 ° F) Chocolate Red 22.85 Table 1 The data clearly shows that the degree of browning can be controlled by varying the pressing temperature at which the process is conducted. This broadens the applications or uses of the residual solid to include a base of toasted chili powder and as a replacement for the darkened, caramelized ground pepper. The residual solid may be substituted by ground shredded hot pepper or chili powder in many common applications and a separate processing step is not required to brown or darken to a desired degree. The ground crushed hot pepper solids have an aerobic plate count (Analysis performed according to the Bacterial Analytical Manual by AOAC, 8th edition, 1995, and the ISO-GRID Methods Manual, 3rd edition, 1989) of approximately 14,000,000. The residual solids leaving the extraction system have a count of approximately 2,000 to 200,000, with the lowest count being achieved at higher temperatures. This is a significant reduction and makes residual solids per se suitable for any application where treatment with ethylene oxide or irradiation would normally be required.
Example IB - Addition of Antioxidant: The previous example was repeated with all the materials and conditions being the same, except that the edible solvent of soybean oil is supplemented with an antioxidant mixture at a concentration of 3% by weight of the pepper solids spicy ground crushed original. The mixture consisted of approximately 29% lecithin, 20% pulverized ascorbic acid, 5% citric acid, 15% tocopherol, - and 1% rosemary plant extract (according to Chang and Wu US Patent No. 5,077,069 ). The stability (1) of the resulting extract and (2) the residual solids was compared in each case with an untreated control. In such evaluation, the ground pungent pigment extracts were plated on salt in flour to a degree of 2.4% by weight with mortar and pestle. Two grams of sample were weighed in 13 x 100 mm test tubes. The test tubes were stored in a thermostatically controlled oven at 65 ° C. Samples, extracted with acetone, 460 nm of a standard dilution (%) in acetone were periodically removed, determined spectrophotometrically. In the evaluation of the residual solids, samples of two grams of the regrind residual solid were replaced by salt dispersions in flour. The procedure for "standard dilution" is as follows'. The initial color of the dispersion was determined by pouring two grams of the original dispersion into a 100 ml flask. Acetone was added to the 100 ml level. The bottle was inverted several times. The salt with flour was allowed to settle for 5 minutes. Next, three ml of the dilution was pipetted into a 25 ml flask and diluted to the 25 ml level. The absorbance was read at 460 nm. The color 460 nm was determined by the formula: , v "^? (absorbance at 460/12) color at 460 nm = (% dispersion / 100) where the percent dispersion was determined by the formula: -. ,,. . , units of color on the flour at 460 nm% dispersion = color of the test sample at 460 nm to solvate the ASTA, the color was multiplied at 460 nm by 820. The color was plotted against time, and the time for 1/3 of the starting color until the fading was reported as the 2/3 life. That is, a highly reproducible measurement, which is accurate enough to evaluate the effectiveness of antioxidants and which will help the practitioner to optimize formulations for specific uses.
The final extract of the first stage of pressing of the unprotected or unstabilized process has a color value of approximately 1375 ASTA and a life 2/3 of 6.5 hours compared to the color value of approximately 1600 ASTA and a life of 2 / 3 of 63 hours for the extract of the protected material. The color value of unprotected or unstabilized residual solids is approximately 85 ASTA with a 2/3 life of 54 hours, compared to the protected solids, which have a color value of approximately 95 ASTA and a 2/3 life of 155 hours. This clearly demonstrates that the inclusion of antioxidants can not only improve the color yields of the extraction process, but also, at the same time, improve the color stability of both the extract and the residual solids. Suitable antioxidant compounds (for example, lecithin, ethoxyquin, butylated hydroxy anisole (BHA), butylated hydroxy toluene (BHT), butyl hydroxy quinone tertiary (TBHQ), sesame, tea catechins, and antioxidant activity of herbs of the Labiatae family, acid finely divided ascorbic acid, tocopherol, citric acid) can be replaced in whole or in part by the specific antioxidant mixture employed with similar desirable color-protection results, preferably a natural antioxidant of an herb of the Labia tae family, for example , rosemary, sage or thyme, or powdered ascorbic acid.
Example 2 - Effect of variation of operating temperatures: Dehydrated milled hot pepper solids (2.5% moisture) were crushed in a hammer mill, and the resulting crushed ground pepper (95% of which passed through a US mesh) 40) was processed with about 15% by weight of soybean oil in a countercurrent extraction system as in Example 1, which involves two (2) pressing steps, with the extracts from the second stage of pressing being returned ( first) preceding mixing stage before being removed from the process in the first pressing step. After leaving the first pressing stage, distilled water was dosed continuously to the crude extract in a percentage of 7-5% by weight of the gums and solids by means of a static static mixer in line.- The weight of the gums and the Fine particulate solids in the extract was determined by diluting one gram of the crude extract, nine grams of acetone. The mixture was pelleted by centrifugation for three minutes at 2000 G in a laboratory centrifuge. The separated solids were air dried, and the weight of the gums and solids was calculated as the weight percentage of the starting extract. The gums and hydrated solids removed from the extract were continuously returned to the final residual pressed solids via a continuous, high-cut bolt mixer, installed immediately after a water-jacketed cooling screw, which received the residual solids from the second stage of pressing. Prior to hydration and centrifugation, the extract contained approximately 10% by weight gums and fine particulate solids as determined by the method described above. After hydration and centrifugation, the gums and particulate solids contributed no more than 1% by weight of the extract and the extract was a clear crystalline solution, free of any insoluble suspended materials. The color value of the ground crushed ground pepper was about 150 ASTA. The pressing steps were carried out at approximately 1406 up to 2109 kgf / cm2 (20,000 to 30,000 PSI) The extraction process began with the operation of the presses at approximately 26.66 ° C (80 ° F) as measured by the temperature of the cake leaving the presses. The temperature of the presses was controlled by the flow rate of the cooling water through the hole in the press shafts and the screen cages to maintain operating temperatures in the range of 26.66 ° C (80 ° F) to 82.22 ° C (180 ° F). During the duration of the extraction, the operating temperature of the presses, as measured by the temperature of the cake leaving the presses, gradually increased to approximately 123.88 ° C (255 ° F) decreasing first and continue stopping the flow of cooling water to obtain operating temperatures of 82.22 ° C-93.33 ° C (180-200 ° F) and then replacing the steam with water in the shaft and the cages to gradually increase the pressure to reach • temperatures of 93.33-123.88 ° C (200-255 ° F). Samples of the extracted oil and the pressed residual solids were obtained at various temperature intervals, when the temperatures increased. Samples of residual solids were obtained at two points, the first (not rehydrated) immediately after leaving the cooling screw of the cake that follows the (second) final pressing step, and the second after the residual pressed solids so chilled were rehydrated to a moisture content of approximately 10%. Samples were tested for ASTA color, aerobic and anaerobic plate count, and color stability over time using the methods employed in Examples IA and IB. The advantages of operating the process at a temperature above 54.44 ° C (130 ° F), as indicated by the cake temperature that comes out of the presses, can be clearly observed. The counts of the extract and cake plates were progressively reduced as the temperatures increased (Tables 2 and 3) EFFECT OF THE INCREASE IN TEMPERATURE ON THE COUNTING OF THE EXTRACT PLATES Temperature Plate Count Plate Count Grades C Aerobic Anaerobic (Grades F) 26.66 (80) 1,900,000 790,000 54.44 (130) 1,700,000 800,000 65.55 (150) 1,700,000 660,000 76.66 (170) 1,600,000 500,000 79.44 (175) 1,500,000 425,000 82.22 (180) 1,300,000 380,000 87.77 (190) 360,000 150,000 93.33 (200) 300,000 200,000 101.66 (215) 240,000 150,000 107.22 (225) 190,000 65,000 112.77 (235) 170,000 32,000 118.33 (245) 69,000 8, 600 123.88 (255) 3,800 830 Table 2 EFFECT OF THE INCREASE IN TEMPERATURE ON THE COUNTING OF THE PRESSED SOLIDS Temperature Plate Count Plate Count Grades C Aerobic Anaerobic (Grades F) 26.66 (80) 220,000 55,000 54.44 (130) 160,000 35,000 65.55 (150) 160,000 25,000 76.66 (170) 100,000 20,000 79.44 (175) 32,000 15,000 82.22 (180) 80,000 7,400 87.77 (190) 3,500 800 93.33 (200) 9,800 3,400 101.66 (215) 5,800 2,300 107.22 (225) 4,100 500 112.77 (235) 1, 900 1,100 118.33 (245) 5,400 100 123.88 (255) 800 100 Table 3 The extraction efficiency improved dramatically as evidenced by the progressively decreasing ASTA values, and the progressively decreasing residual extractable yields of the pressed residual solids. It is evident that, to achieve residual extractable yields of less than about 20% by weight of the cake, it is necessary to operate the presses at 54.44 ° C (130 ° F) or more. (Table 4) Further, for obvious efficiency reasons, temperatures in excess of 82.22 C (180 F), and especially between 82.22 ° C (180 ° F) and about 112.22 ° C (235 ° F) are greatly preferred.
PRESSED CAKE HANDLE AND RESIDUAL YIELDS A PROGRESSIVELY HIGHER TEMPERATURES ASTA Temperature of Solids Residual Performance Pressed grades of Pressed Solids (Degrees F) 26.66 (80) 87 28.28% 54.44 (130) 76 16.40% 65.55 (150) 65 15.72% 76.66 (170) 61 15.72% 79.44 (175) 53 12.36% 82.22 (180) 43 13.88% 87.77 (190) 42 10.84% 93.33 (200) 44 10.72% 101.66 (215) 41 9.96% Table 4 PRESSED CAKE ASTA AND RESIDUAL YIELDS AT PROGRESSIVELY HIGHER TEMPERATURES ASTA Temperature of Solids Residual Yield Pressed grades of Pressed Solids (Degrees F) 107.22 (225) 39 9.50% 11.2.77 (235) 33 9.28% 118.33 (245) 32 9.00% 123.88 (255) 35 9.80% Table 4 (Continued) More importantly, the stability of the extract was not adversely affected and this, in fact, increased. The results, of Example 2, of an accelerated study on the stability of the extract generated at various operating temperatures of the press can be seen in Table 5. An accelerated study was carried out according to the procedures described in Example IB with the colors reported as a percent of the starting color for each respective sample to adjust the variable color yields at the respective temperatures. These results show that the extract produced at higher operating temperatures exhibit greater resistance to oxidative deterioration of color. This is surprising, as explained in the following.
STABILIDAE (FROM THE EXTRACT OF) PRESSED, ACCELERATED OLEOOR®, 65 ° C Temperature Grades C (F) Hour Time Hour Time Hour 2 4 8 12 17 26.7 (80) 94% 88% 81% 73% 62% 54. 4 (130) 94% 89% 82% 75% 64% 76. 7 (170) 93% 89% 82% 76% 65% 107. 2 (225) 94% 90% 82% 78% 67% 112. 8 (235) 94% 90% 82% 77% 69% 123. 9 (255) 95% 90% 84% 78% 72% Table 5 It is commonly believed that systems containing lipids, when exposed to heat, will exhibit a greater speed of lipid oxidation that, once initiated, will proceed at an increasing rate. (Rancidity and its Measurement in Edible Oils and Snacks, A Review, Robards, Kerr, and Patsalides, Analyst, February 1988, Vol 113). Indeed, the prior art (U.S. Patent 4,681,769) claims a process for high pressure extraction, countercurrent of Capsicums at less than 37.8 ° C (100 ° F) and less than 35.15 kgf / cm2 (500 PSI) for the reason express to protect the oil extracted from oxidation.
To confirm the positive effect of the high temperature treatment under more controlled conditions, a forty gram sample of ground pepper oleoresin extracted with hexane, without additional diluents, was heated in an oven on a hot agitator plate at 100 ° C for eight hours. hours and a half A control sample which was not heated, a sample obtained from the hot oven after four hours, and a sample of the hot material during the eight and a half hours were dispersed salt with flour to make dispersions of 1.2% by weight of oleoresin salt with flour. Two gram portions of the dispersions were weighed into test tubes and placed in an oven at 65 ° C. An initial ASTA color was resolved in each dispersion and then ASTA colors were tested periodically and the results plotted against time to determine the relative stability of the heated and unheated samples. The results are shown in Table 6. It can easily be seen that the thermally treated samples, although they lose some of the initial color during the heating process, have improved stability over time, thereby confirming the improved oxidation resistance observed in the Table 5 VALUES ASTA DEL (ABSTRACT) PICANTE PICANTE MOLIDO WITH OLEORRESINA HEATED AND NOT HEATED, WITH TIME Hours Not heated Heated 4 @ Heated 8 @ 100 ° C 100 ° C 0 32.5 31.5 26.0 2 29.0 29.0 25.8 4 26.0 28.0 25.7 6 24.0 27.0 25.5 8 22.5 25.8 25.3 10 21.0 24.5 25.0 12 20.0 23.0 24.8 14 19.0 22.3 24.5 16 18.0 21.8 24.0 18 17.0 21.0 23.5 20 16.0 20.0 23.0 22 15.1 19.0 22.5 24 14.2 18.5 22.1 26 13.4 18.0 21.8 28 12.9 17.5 21.4 30 12.5 17.0 21.0 Table 6 The non-rehydrated pressed residual solids produced in Example 2 exhibit lower resistance to oxidative color loss when press operating temperatures are increased as predicted by the prior art (Bennett et al, USP 4,681,569) and as Observe in Table 7.
STABILITY OF PRESSED SOLIDS NON-REHYDRATED TO VARIOUS TEMPERATURES OF PRESS OPERATION, EXPRESSED AS THE PERCENT OF THE RETAINED START COLOR Temperature Week Week Week Degrees C (F) 2 4 6 26.7 (80) 86.7% 82.2%. 85.5-s 54. 4 (130) 89.6% 85.5% 84.6% 76. 7 (170) 73.3% 65.3% 58.1% 107. 2 (225) 61.7% 35.8 -s 2. • "5 118.3 (245) 68.2% 31.0% 19.3% Table 7 But, very importantly, it can be observed that the pressed residual solids that were rehydrated immediately after leaving the second pressing step of the process (Example 2) exhibit a significantly higher stability (Table 8) in relation to the non-rehydrated solids, thus overcoming the disadvantages claimed for operation at temperatures above 37.8 ° C (100 ° F) exposed at USP 4,681,769 STABILITY OF PRESSED SOLIDS REHYDRATED TO VARIOUS OPERATING TEMPERATURES D? THE PRESS, EXPRESSED AS? L PERCENT OF COLOR D? DEPARTURE R? T? NIDO Temperature Week Week Week Degrees C (F) 2 4 6 26.7 (80) 90% 92% 91% 54.4 (130) 93% 91% 92% 76.7 (170) 92% 92% 91% 107.2 ( 225) 94% 93% 91% 118.3 (245) 95% 94% 93% Table 8 clearly the supposed obstacle of operating at high pressures and pressures.
It is also surprising that the color stability of the residual pressed solids is significantly improved by controlling the water activity (Aw) of the solids at intervals higher than those suggested for the stabilization of lipid-containing systems by extensive studies and particularly by Nelson and Labuza, Science of Water Activity and Food Polymers: State Implications on the Arrhenius and WLF Models in the Shelf Life Projection, KA Nelson and TP Labuza, Journal of Food Engineering 22, 271-289 (1994 ). The water activity is defined as the ratio of the water vapor pressure in a food at the vapor pressure of pure water at the same temperature. The prior art suggests that the maximum stability of the lipidium systems will be attained at water activities of about 0.3 with a development of decreased stability when the water activity increases above this level. In this example we find precisely the inverse effect on the stability of the carotenoid pigments for a given water activity. To confirm the effect of high temperatures in the pressing operation, and to confirm the effect of the added moisture, a controlled test is carried out at laboratory scale where the effect of the levels of the extractable yield on the cake could be controlled to eliminate the effect of the residual presscake yields variable on the stability of the carotenoids. A sample of 3,000 grams of ground crushed hot pepper solids (175 ASTA, 9.8% extractable yield) was dried in a laboratory tray dryer at 37.8 ° C (100 ° F) for 16 hours at a moisture content of approximately the 2%. Half of this sample was then heated in an oven at 104.4 ° C (220 ° F) for twenty minutes at about the temperature in the pressing operation according to the invention. The other unheated sample served as a control. One hundred gram samples of each of the two materials were rehydrated at intervals of about 1% to about 12% moisture. The water activity Aw of each was determined using an instrument to determine the water activity Rotronics Hygroskop DT, model DT2 / 1-00IV. The samples were weighed in sealed test tubes, stored at ambient temperatures of approximately 22.2 ° C (72 ° F) in the dark, and the ASTA colors were determined over a period of eighteen weeks to determine the relative percent degradation of the sample. color. The color retained (as a percentage of the starting color for each sample to compensate for the effect of color dilution with the rehydration water) was plotted against time.
BY RETAINED COLOR CITIZEN OF PICANTE MOLIDO PIMI NTO CRUSHED WITHOUT LIMITING TO VARIOUS INTELLECTUAL ACTIVITIES OF WATER Water Activity Aw Week 1 Week 5 Week 18 O.15 74% 57% 42% 0.30 50% 45% 12% 0.40 68% 50% 43% 0.60 83% 68% 55% 'Table 9 PERCENT D? COLOR R? T? NIDO D? PICANT PICANT? GROUND HEAT SHREDDED AT VARIOUS ACTIVITY INTERVALS D? WATER Water Activity Aw Week 1 Week 5 Week 18 0.15 66% 56% 41% 0.30 60% 50% 45% 0.40 80% 62% 57% 0.60 98% 82% 78% Table 10 It can be seen in Tables 9 and 10 that the stability of the carotenoid pigments follows almost precisely "the inverse of the curve predicted by Nelson and Labuza (Figure 2). It can also be observed from these tables that the temperature controlled (with concurrent browning) ) significantly increases the stability of carotenoids above a water activity of 0.3 and particularly in the water activity range of 0.4 to 0.6 Water activity ranges greater than 0.6 were tested since levels marginally greater than this range would support microbial growth, which is not acceptable in a dry spice product.It can be concluded that the stability of the carotenoid pigments found in Capsicums does not follow, unpredictably, the commonly accepted and predicted pattern for lipid oxidation with respect to temperature and water activity as suggested in U.S. Patent 4,681,769, or in the literature cited (Nelson and Labuza, Science of the Activity of Water and Food Polymers: State Implications on the Models of Anius and WLF in the Projection of Shelf Life, KA Nelson and TP Labuza, Journal of Food Engineering 22, 271 -289 (1994); Rancidity and its Measurement in Edible Oils and Snacks, A Review, Robards, Kerr, and Patsalides, Analyst, February 1988, Vol 113); which describes the stability of lipid systems. In fact, the treatment at high temperature, combined with the rehydration of the pressed solids at a water activity higher than 0.3, preferably from 0.4 to 0.6, significantly improves the stability instead of decreasing it. This is a very surprising and unexpected result. It is well known that the lipid profile of Capsicum and its extracts, without the addition of any diluent, comprises a mixture of saturated and unsaturated fatty acids, being 60-70% linoleic and linolenic unsaturated, Lipid Content and Antioxidant Red Pepper , Daood, Biacs, et al., Central Food Research Institute, Budapest, Hungary (1989) and The Nature of Fatty Acids and Esters of Capsanthin in Spicy Hot Pepper, Nawar et al., Journal of Food Science, Vol 36 ( 1971). In fact, Daood et al., Suggest that "... the presence of triglycerides- that contain high amounts of unsaturated fatty acids can be an important factor that contributes to the fading or discoloration of hot pepper ground during processing and storage." The discoveries of the present are just opposite. Without being limited in any way by theoretical considerations, the hypothesis was constructed that the surprising and undescribed inverse relationship shown (in Tables 9 and 10) between the stability of carotenoid pigments to given water activities is due to the fact that Fatty acids in the substrate are preferably attacked by the oxidation reaction at the low water activity ranges (from about 0.05 to 0.2 Aw) and higher (above 0.3, preferably from about 0.4 to 0.6 Aw), protecting from this way to the carotenoids. At intermediate water activity intervals (0.2 to 0.4 Aw), where the best protected lipids, the carotenoids are more easily and preferably attacked and exhibit less resistance to oxidative degradation. Another controlled test was conducted to demonstrate the effect of different extractable performances on the presscake of residual solids. The effect of higher amounts of unsaturated fatty acids is evident from the results illustrated in Table 11 where fresh soybean oil was added, refined, bleached and deodorized without antioxidants at various percentages based on the weight of the ground hot pepper. The color with time was compared with the untreated control in an accelerated study at 65 ° C. A typical, bleached and deodorized soybean oil has a fatty acid composition of 22.3% oleic acid (18: 1), 51% linoleic acid (18: 2), and 6.8% linolenic acid (18: 3) . (Riegel's Handbook of Industrial Chemistry, 9th Edition, page 278). It can be concluded that higher levels of unsaturated fatty acids, such as oleic, linolenic, and linoleic acids, which are found in most vegetable oils, improve the color stability of pressed residual solids. The levels of extractable yields in the residual solids above 15-20% by weight of the residual solids are undesirable since the residual Capsicum solids become difficult to handle for most uses and the efficiency of the extraction is reduced , ie, that less color can be removed from the spices since the residual yield is allowed to increase by decreasing the pressure or temperature used.
BY RETAINED COLOR CITIZEN WITH VARIABLE AMOUNTS OF SOYBEAN OIL ADDED TO PEPPY GRINDING MIXED GRINDING Percent Addition Time 2 Time 4 Time 6 Time 8 0% 65% 59% 52% 50% 5% 90% 83% 74% 72% 10% 92% 84% 75% 74 % 15% 94% 87% 80% 78% 20% 96% 91% 83% 81 ^ Table 11 It is readily apparent, by comparing the results of the controlled test (Tables 9 and 10) on the stability of the heated vs. unheated material, where the oil was controlled at a constant level, at an added soybean oil content given in the pressed residual solids, the color stability of the residual pressed solids improved significantly when the Capsisum was exposed to higher temperatures. This conclusion is not readily apparent from the results shown in Table 8 where the amount of residual vegetable oil left in the heavy residual solids is higher in the lower temperature ranges due to the lower efficiency of the extraction process at lower temperatures (Table 4) The presence of larger amounts of residual oils offers some protection which overshadows the greater protective effect at higher temperatures. This is evident in Tables 9 and 10. Therefore, it can be concluded that most, if not all, of the protection offered by the operation of presses at temperatures below 37.8 ° C (100 ° F) (as claimed in US Patent 4,681,769) compared to temperatures above 37.8 ° C (100 ° F) is simply due to higher levels of residual oil (reduction of extraction efficiency) and that, for a given residual oil content, and with rehydrated residual solids, operating temperatures above 54.4 ° C (130 ° F) give superior results, not only the increase in extraction efficiency that allows a high speed process, continuous with higher, production speeds and significantly reduced microbial activity, but rather more surprising is the greater color stability of both the extract and the residual pressed solids, particularly when the pressed solids are rehydrated.
Comparative Example: according to USP 4,681,769 Bennet, - low temperature and pressure As can be seen in Table 4, the residual yield of pressed solids in much higher at temperatures below 37.77 ° C (100 ° F) and much higher (yield residual of 28.3%) than described in USP 4,681,769 (residual yield of 10-15%). In Example 2, Table 4, the Model KEK 100 Screw Press was used for the test operated at approximately 100% of its nominal capacity of 108.84 kilograms per hour (240 pounds per hour) for typical oilseeds. In an effort to approximate more closely the model of 10-15% residual yields (of oil) in the cake as described in USP 4,681,769, the feed rate of this test was set at approximately 43.05 kilograms per hour (95 pounds per hour), thus allowing a longer press resistance time to produce more extract and reduce the residual yield of the pressed residual solids to 10-15%. The following Example according to Bennett is a two-step production trial.
One batch, which comprised approximately 136.05 kilograms (300 pounds) of 160 ASTA chili, crushed to pass through a 20 mesh (USSS), was transferred to a mix and mixed with 13.7% by weight of crushed chili pepper oil. fortified soybean that had an oleoresin of 500 ASTA for approximately 15 minutes and then allowed to stand for approximately 16 hours at room temperature (23.88 ° C (75 ° F)) before transferring to the feed hopper of a KEK Model Screw Press -100 by Egon Keller. The feed hopper provided a controlled flow of chili and fortified oil mixture to the press at speeds of approximately 43.05 kilograms per hour (95 pounds per hour) of fresh shredded chili, the equivalent of approximately 362.81 kilograms per hour (800 pounds per hour) in an F-44 French Oil Mill Machinery Company press. Both of these feed rates represent approximately 40% of the nominal capacity of the respective screw presses on the complete oil seeds. The production trial began with the establishment of approximately 0.0762 centimeters (0.030 inches) and with the internal worms configured to provide an essentially small or no pressure gradient greater than 35.15 kgf / cm2 - (500 pounds per square inch). At those low pressures and feed rates, the effluent oil temperatures were maintained at less than 37.77 ° C (100 ° F) with cooling water as at Bennett, and the residual yield (oil) at the pressed residual solids averaged approximately 12.5. %, as prescribed by Bennett, who states that: "Temperatures above 37.77 ° C (100 ° F) should be avoided because higher temperatures cause oxidation with a diffusion resulting from the delicate taste and / or color principle " With the press operating as described, the extracted oil, after centrifugation to remove residual spice fines, is tested at approximately 1000 ASTA and the fraction of residual solids from the press cake had a corresponding reduction in ASTA to approximately 115. The pressed cake of the fresh ground spices, once extracted from the first thought, was further processed following the same procedure described above for the first pressure mixing / extraction sequence using, however, fresh soybean oil as an additive instead. of soybean oil fortified with oleoresin. The extracted "fortified soybean oil" was tested at approximately 500 ASTA.This 500 ASTA fortified soybean oil extract was recycled as a fresh crushed chili extractor.The chili powder cake extracted from this extraction step had a corresponding reduction in the ASTA value by an average of approximately 65 ASTA (which fluctuates from 41 to 95 ASTA) .The results of this test at low temperature, low pressure, were compared with the results of the conditions at high temperature, high pressure at Example 2, and are shown in Table 12.
Comparison of Low Temperature / Low <at Pressure and High Temperature / High Pressure Low Temperature / High Temperature / Low Pressure, High Pressure mixing the batch Continuous from 16 hours Example 2 Temp. Grades C 35 (95) 112.22 (235) (Grades F) Pressure, kgf / cm2 < 35.15 (< 500) 1406-2109 (psi) (20,000-30,000) Residual Solids 65 33 Finals (ASTA) Yield of 12.5% 9.3% Final Residual Solids Comparison of Low Temperature / Low Pressure and High Temperature / High Pressure Low Temperature / High Temperature / Low Pressure, High Pressure mixing the Continuous batch of 16 hours Example 2 Residual Solids 41.5% 22% Final ASTA as percent of ASTA from Chile Cool ASTA loss in 7% 0% the 1st . mixing stage ASTA loss in 10.5% 0% the 2nd. Oleoresin ASTA 1,000 1,000 Final mixing stage TABLE 12 It can be clearly seen, as shown in Example 2 (Effect of Variation of Operating Temperatures), that the batch process at low temperature / low pressure with long contact times incurs significant color losses during contact times prolonged temperature required for low temperature / low pressure extraction. In addition, the batch process at low temperature / low pressure, does not remove the color as efficiently as at high temperatures and pressures for any press operation of a given size. The above example can be scaled and scientifically extrapolated in a comparative, two-step production trial using French Oil Mill Machinery Company, Model 44-F presses, as follows: A solid comprising approximately 1741.5 kilograms (3840 pounds) of solids of chili (Capsicum annum), crushed, fresh, with a humidity of 5%, ASTA of 160, 20 mesh,. was passed through a high-speed, high-cut blade mixer, with a steam jacket, on a continuous base, and fed directly into the feed hopper of the press in one step, through a first stage of pressed, to the second stage of the vane mixer, and then to the second pressing step. Soybean oil was added continuously through a metering pump to the paddle mixer in the second stage with a percentage of 13.7% by weight of the crushed starting chili solids (238.1 kilograms (525 pounds) of oil for the 1741.5 test). kilograms (3840 pounds)). The raw material chili solids were fed continuously at a rate of approximately 1133.78 kilograms per hour (2500 pounds per hour) to the system with a total contact time in each paddle mixer of approximately 15 seconds. The temperature of the chili / oil mixture leaving the paddle mixer was maintained at about 82.22 ° C (180 ° F) in stage 2, and at about 65.55 ° C (150 ° F) in step 1. The oil / extract ejected from the second pressing step was returned on a continuous basis to the paddle mixer at a stage where the oil / extract and ground shredded fresh pepper were mixed in preparation for the first pressing step. The oil / extract and fresh ground milled hot pepper leaves the first stage of the paddle mixer and enters the first pressing stage at approximately 65.55 ° C (150 ° F), the temperature is controlled by the amount of steam on the shirt of the paddle mixer. The oil / concentrated extract projecting from the first pressing step is hydrated with water to approximately 75% by weight of fines (fine particulate solids) and gums, and then centrifuged, and the fines and hydrated gums are added to the pressed solids residual (second) final pressing stage in a high shear mixer, then the solids have to pass through a cooling screw with a water jacket.
The arrangements of that collar and the inner shaft of the press are configured to provide internal pressures of approximately 1406 to 2109 kgf / cm2 (20, 000 to 30,000 PSI) and the cooling water is maintained at a flow rate through the shaft bore and through the cooling sleeves of the cage to maintain an exit oil temperature on the outer surface of the housing. about 82.22 ° C (180 ° F) at 93.33 ° C (200 ° F), and a salty residual cake temperature of about 112.22 ° C (235 ° F). The solid of the residual cake is cooled in a screw conveyor with a water jacket to approximately 29.44 ° C (85 ° F) and water, in addition to the water of hydration used to remove fines and gums from the extract, injected into the mixer. fine and high cut gums to rehydrate the cake to a water activity of approximately 0.6. The concentrated extract leaving the pressing step has an ASTA value of about 1,000 and the residual pressed solid cake leaving step two has an ASTA value of about 45. The residual pressed solid cake has a red appearance Typical brown-brown powder of lightly toasted chile powder. The aerobic plate count of residual solids is approximately 70,000.
The same test was repeated (according to the Bennett Example). No heat was applied during the mixing steps and the internal presses were reconfigured to provide minimal friction and compression and the minimum generation of heat resulting during the pressing operations. Work compression is mainly provided by the cone at the cake discharge and was maintained at approximately 35.15 kgf / cm2 (500 PSI). Oil was added to a percentage of about 13.7% by weight of the ground milled hot pepper solids (238.1 kilograms (525 pounds) for the 1741.5 kilograms (3840 pounds) lot), and mixed in a ribbon mixer for 16 days. hours, and then fed at room temperature (approximately 23.88 ° C (75 ° F)) to the pressing system. The feed rate through the pressing stages was maintained at 362.81 kilograms per hour (800 pounds per hour). Cooling water was supplied to the inner bore of the shafts and the cooling jackets to maintain the "oil temperatures". output less than 37.77 ° C '(100 ° F), both in the ejected oil and in the residual pressing cake. The extract that comes out of the first pressing stage of the press is centrifuged without hydration of the gums and fine particulate solids. The concentrated extract leaving the pressing stage one has an ASTA value of about 1,000 and the residual cake solids have an ASTA value of about 65. The appearance of the cake is that it lacks the characteristic browning of the hot pepper ground, crushed, like commercially available chili powder and require a browning step or separate caramelization to make it acceptable for common uses. The material is difficult to re-crush due to the high level of extractable residual performance left on the cake, it does not flow, and must be combined with other solid materials to produce an acceptable product for sale. The aerobic plate count is approximately 220,000. A comparison of the results of the two tests is shown in Table 13.
- Pressed to High Pressed at Low Temperature Temperature Mixing Time, Continuous, 16 Hours Soybean Oil (Seconds) Oil Temperature 23.88 (75) 23.88 (75) Fresh, ° C (° F) Oil / Chile, Stage 1 65.55 (150) 23.88 (75) to Press Feeding, ° C (° F) Oil / Chile, Stage 2 82.22 (180) 23.88 (75) a Press Feeding, ° C (° F) Pressed at High Pressing at Low Temperature- Temperature Cake after the 107.22 (225) 35 (95) Stage 1 of the Pressing, ° C (° F) Cake after the 112.77 (235) 35 (95) Stage 2 of Pressing, ° C (° F) Value of ASTA, Extract 1000 995 Life 2/3, Extract, 25 16 65 ° C, Hours Value of ASTA, Cake 45 65 Pressed Life 2/3, Cake, 32 10 22.22 ° C (72 ° F), Weeks Color Recovery, 75% 51% Extract Plate Count 70,000 2,000,000 Aerobic, Excerpt Plate Count 2,000 220,000 Aerobic, Cake Total Recovery 98% 91% of Color (Extract and Cake) Pressed to High Pressed at Low Temperature Temperature Visual appearance, Red-brown Red-toasted Cake Speed of 2,500 800 production, kg per. hour (pounds per hour) TABLE 13 It is readily apparent that there are substantial advantages at higher temperatures and pressures. Color recovery improves, there is a 50% increase in extract yield, the speed for a given press size is increased by more than 300%, the color stability of the extract improves by 65%, the color stability of the cake of residual solids improves by 300%, and the aerobic plate count is reduced by a factor greater than 30 both from the extract and in the residual cake; all without the oxidative color losses that are alleged as an obstacle in USP 4,681,769. * Therefore it is observed that an improved countercurrent process for the extraction of Capsicum solids using an edible solvent, therefore improving the yield of both the extract and the residual solids obtained, therefore, both the extract and the residual solids have improved color stability and are free of bacterial contamination due to the higher temperatures used, so that due to the optional advantageous rehydration of the residual solids and the water activity level employed, a better color stability in the residual solids is achieved, whereby an extract in the form of a transparent solution can be obtained by removing the gums and particulate solids in In the form of insoluble hydrates, therefore, a greater color stability can be obtained by the use of edible antioxidants in the solvent used, and therefore, a controlled browning or caramelization of the residual solids can be conveniently obtained, all without the disadvantages expected from using higher temperatures as clearly indicated in n the prior art, and therefore all the objects of the invention have been achieved, and provided. It should be understood that the invention is not limited to the details of the extraction operation, or to the compositions, methods, procedures or exact modalities shown and described, since the obvious modifications and equivalents will be apparent to those skilled in the art, and therefore both the invention is limited only by the full scope that can be legally agreed by the appended claims.
It is noted that in relation to this date, the best method known to the applicant to carry out the aforementioned invention, is that which is clear from the present description of the invention.

Claims (29)

CLAIMS? Having described the invention as above, the content of the following claims is claimed as property:
1. A multistage, continuous, high-pressure pressing and countercurrent extraction process for the production of a concentrated edible extract and edible residual solids, both with a reduced bacterial content, with the extract possessing greater resistance to oxidative deterioration. the carotenoid pigments therein, and both of which contain carotenoid pigments, flavor, and aroma, of solids of plant material of the genus Capsicum, characterized in that it comprises the following steps: subjecting the Capsicum solids to a countercurrent extraction process involving a plurality of mixing and pressing steps, including the first and last mixing steps and first and last pressing steps, together with five to about fifty weight percent of an edible solvent, to produce a residual extract and solid, return Continuously extracting each stage of pressing to the mixing stage pr evia, and finally separating the extract from the first pressing stage and separating the residual solids from the last pressing step, all the pressing steps are carried out at a temperature of at least 54.44 ° C (130 ° F).
2. The process according to claim 1, characterized in that the temperature is from 54.44 (130) to approximately 232.22 ° C (450 ° F).
3. The process according to claim 1, characterized in that the Capsicum solids are subjected to internal pressures in the pressing stages of at least 421.8 kilograms force per square centimeter (6,000 pounds per square inch). ~
4. The process according to claim 1, characterized in that the weight of the edible solvent is from 5% to about 20% by weight of the Capsicum solids.
5. The process according to claim 1, characterized in that the moisture content of the starting Capsicum solids is less than 6% by weight, and wherein the reduction of the bacterial count is affected at this low moisture content, avoiding hence the undesirable loss of volatile flavoring and flavoring constituents and preventing the development of unpleasant baking flavors and aromas that occur at high moisture contents.
6. The process according to claim 1, characterized in that the Capsicum solids extracted in the process are selected from the group consisting of ground hot pepper, red pepper and chili. The process according to claim 1, characterized in that the edible solvent is selected from the group consisting of soybean oil, corn oil, cottonseed oil, rape seed oil, peanut oil, mono-, di- or triglycerides, lecithin, edible essential oils, sesame oil, edible alcohols, hydrogenated or partially hydrogenated fats or oils, polyoxyethylene sorbitan ethers, limonene, fats or edible animal oils, mixtures thereof, and edible derivatives thereof. The process according to claim 1, characterized in that the fine particulate solids are filtered or centrifuged from the extract and alternatively discarded, returned to a stage of mixing or pressing the process, or incorporated in the final residual solids. The process according to claim 1, characterized in that it includes the steps of hydrating the final extract by adding water in a degree of 5% to 200% by weight of the gums, and fine particulate solids included therein, and filtering or centrifuging to remove gums and solids. 10. The process according to claim 9, characterized in that it includes the step of returning the gums and separated hydrated solids to the final residual solids. 11. The process according to claim 1, characterized in that it includes the step of rehydrating the final residual solids with water to a water activity greater than 0.3 Aw for color stabilization thereof. 12. The process according to claim 11, characterized in that the solids are rehydrated at a water activity of about 0.4 to 0.6 Aw. The process according to claim 1, characterized in that an effective color stabilizing amount of an edible antioxidant or chelator in the edible solvent is included. The process according to claim 13, characterized in that the antioxidant comprises an antioxidant selected from the group consisting of lecithin, ascorbic acid, citric acid, tocopherol, ethoxyquin, BHA, BHT, TBHQ, tea catechins, sesame, and activity antioxidant of an herb of the family Labia tae. 15. The process according to claim 14, characterized in that the antioxidant comprises a natural antioxidant of an herb of the family Labia tae or powdered ascorbic acid. 16. The process according to claim 15, characterized in that the antioxidant comprises the antioxidant activity of an herb selected from the group consisting of rosemary, thyme and sage. 1
7. The process according to claim 1, characterized in that the temperature is greater than 82.22 ° C (180 ° F). 1
8. The process according to claim 1, characterized in that the temperature is between about 82.22 ° C (180 ° F) and 112.22 ° C (235 ° F). 1
9. An extract of plant solids of the Capsicum genus produced by the process according to claim 1, characterized in that it has greater color stability due to the high temperature used in its production. 20. An extract of plant solids of the Capsicum genus produced by the compliance process of claim 5, characterized in that it has a high color value and a low bacterial count due to the high temperature used in its production and due to the low water content not greater than 6% in the starting Capsicum solids. 21. The solids of the cake, rehydrated, produced by the extraction of Capsicum solids according to the process of claim 11, characterized in that they have a high degree of color stability due to the high temperature used in their production and due to the level of water activity Aw present in them. 22. The solids of the cake, rehydrated, produced by the extraction of Capsicum solids according to the process of claim 12, characterized in that they have a high degree of color stability due to the high temperature used in their production and to the water activity level Aw present in them. 23. An extract of a plant of the genus Capsicum, characterized in that it is produced by the process according to claim 9, in the form of a transparent solution, with gums and particulate solids therein, converted to its insoluble hydrates, and then removed from the abstract. 24. A hydrated extract of a plant of the genus Capsicum, characterized in that it is produced in the process of claim 9, and because it has gums and particulate solids therein in its soluble hydrated form. 25. An extract of plant solids of the genus Capsicum, characterized in that it has a color stability produced in accordance with the process of claim 13 due to the edible antioxidant therein. 26. The product according to claim 25, characterized in that the antioxidant comprises an antioxidant selected from the group consisting of lecithin, ascorbic acid, citric acid, tocopherol, ethoxyquin, BHA, - BHT, TBHQ, tea catechins, sesame seeds, and the antioxidant activity of an herb of the Labiatae family 27. The product according to claim 26, characterized in that the antioxidant comprises a natural antioxidant of an herb of the family Labia tae or powdered ascorbic acid. with claim 27, characterized in that the antioxidant comprises the antioxidant activity of an herb selected from the group consisting of rosemary, thyme and sage. 29. A multi-stage, continuous, high-pressure pressing and countercurrent extraction process for the production of a concentrated edible extract and edible residual solids, both with a reduced bacterial content, with the extract having greater resistance to deterioration oxidation of the pigments therein, and both of which contain pigments, flavor and aroma, of solids of spice plant materials, characterized in that it comprises the following steps: subjecting the solids of material from spice plants to an extraction process to countercurrent involving a plurality of mixing and pressing steps, including first and last mixing steps and first and last pressing steps, together with up to about fifty weight percent of an edible solvent, to produce an extract and residual solids, continually return the extract from each pressing step to the pre-mixing stage, and finally When separating the extract from the first pressing step and separating the residual solids from the last pressing stage, all the pressing steps are carried out at a temperature of at least 54.44 ° C (130 ° F).
MXPA/A/1999/005362A 1996-12-13 1999-06-09 High temperature countercurrent solvent extraction of capsicum solids MXPA99005362A (en)

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