HK1096033B - Process for preparing phytosterol dispersions for application in beverages - Google Patents

Description

Preparation method of plant sterol dispersion liquid for beverage

Background

Technical Field

The present invention relates to aqueous compositions, such as beverages, containing human and veterinary plant sterols and to a process for their preparation. Typical beverages include fruit and vegetable juices. Other typical beverages include sports drinks, beverages, or beverages used to restore electrolytes lost due to illness. Other typical beverages include carbonated beverages, which include soft drinks and so-called "botanical flavor" beverages such as colas and other natural and artificial flavor beverages.

Prior Art

Researchers have investigated methods of preventing atherosclerosis, which is a root cause of cardiovascular disease, and have shown that cholesterol plays a role in this disease to contribute to the formation of atherosclerotic plaques in blood vessels, impeding blood circulation to the heart muscle, kidneys, brain and limbs. Some data show that a 1% reduction in total serum cholesterol in humans will reduce the risk of coronary heart disease by 2% and a 10% reduction can prevent approximately 100,000 deaths per year in the united states. As early as 1953, the scientific literature reported that phytosterols had the effect of lowering atherosclerosis in mammals, lowering serum cholesterol in humans, and lowering serum cholesterol in young people with atherosclerotic heart disease. (Pollak, Circulation 7, 696 701; 702 706 (1953); Farquhar et al, Circulation, 14, 77-82 (1956)). Other scientific literature has established that phytosterols and stanols actually reduce human serum cholesterol levels, however, due to their low solubility in water, it is difficult to prepare products containing these phytosterols and stanols suitable for human and veterinary consumption.

For the most part, phytosterols or stanols are used in margarines and other so-called coatings or similar food products due to their hydrophobic nature. U.S. patents 3,881,005 and 4,195,084, both assigned to Eli Lilly, describe pulverizing or grinding phytosterols to increase their solubility. Eli Lilly sold sterol preparations from tall oil and soybean oil once under the trademark Cytellin, which lower serum cholesterol by about 9%. Kuccodkar et al, Atherosclosis, 23: 239-248(1976). However, this product has never been accepted by a wide range of consumers.

Fruit juice-containing products, i.e., water-based beverages and fruit juice-containing products (as well as concentrates for preparing such beverages and products), are used in the art and have achieved considerable market acceptance. Adding hydrophobic components to these products is a well-known difficulty in the art due to the hydrophobic component having a different density than water, and as a result, the hydrophobic component may separate and float to the surface or sink to the bottom when the product is purchased and consumed. For example, hydrophobic components that float on the surface produce an undesirable "ringing" that is found in beverages, such as fruit juices, that contain hydrophobic components that are less dense than water, and cause the product to be non-uniform throughout the container.

Since aesthetically undesirable separation of products affects consumer acceptance, juice-containing products packaged in transparent or translucent (e.g., glass or plastic) containers must avoid such separation. Stirring the juice-containing product in its container prior to use causes the hydrophobic component to be temporarily dispersed, however, this is only a short term solution, since the hydrophobic component will separate again after stirring, and therefore the hydrophobic, fat-soluble or oleophilic components, including vitamins, oils, extracts, flavours and sterols, need to be ensured to be incorporated when added to the juice-containing product by a specific treatment that suspends or disperses in the juice-containing product so that they do not separate.

The prior art attempts to overcome these difficulties have generally used several methods including homogenizing, encapsulating and/or adding stabilizers, gums, emulsifiers, etc.; however, these methods increase the cost of the product and in some cases are illegal in certain standardized products such as citrus juices, e.g. orange juice. Consumers also find some of these products undesirable from a labeling, texture, and viscosity standpoint. Stabilizers and gums often increase viscosity, even if the juice-containing product thickens, thereby reducing its sensory impression. In addition, dispersing the phytosterols in the juice or beverage provides the beverage with a powdered texture, which also negatively impacts consumer acceptance.

Some juice beverages should maintain a cloudy appearance and should not create rings on the surface of the juice when in a container or glass due to consumer identification and acceptance, thus necessitating the provision of juice and/or juice concentrate containing hydrophobic materials in a stable dispersion. In some fruit juice products, such as citrus juice, for example orange juice, consumer identification and acceptance of turbidity requires that the product be stable during refrigeration or shelf life of the product, as well as upon consumption.

U.S. Pat. No. 6,129,944 to Tiainen et al describes a process for preparing a product containing phytosterols by forming a homogeneous suspension of microcrystalline phytosterols and sweetener in an aqueous solution.

Vulfson et al, WO 00/41491, disclose hydrophobic compounds such as phytosterols and lycopene as supplements for food and beverages such as margarines, beverages, soups, sauces, dips, salad dressings, mayonnaises, candies, breads, cakes, biscuits, breakfast cereals and yogurt-like products. Vulson et al, in mixing phytosterols or lycopene with food, determine that the food, having both hydroxyl and carboxyl groups, interacts with the surface of the sterol or lycopene.

This reference continues to describe the production of fine suspensions of phytosterols in water without surfactants and without milling the phytosterols with sugars, as described in us patent 3,085,939; 4,195,084, respectively; 3,881,005, respectively; and GB 934,686. In contrast, Vulfson et al, described by the inventors as a "coating material", forms a suspension or slurry of phytosterols in water at from about 10% to about 30% by weight sterol by deep homogenization using conventional methods and a small amount of an aqueous food concentrate.

Haarasilta et al, WO 98/58554, describe premixes for the food industry containing comminuted phytosterols and conventional food ingredients such as fruit, vegetable or berry-like materials, particularly in powder form, and methods of making the premixes. This result is obtained by comminuting phytosterols and foodstuffs such as berries, fruits or vegetables according to the method and apparatus disclosed in Finnish patent applications FI 963904 and FI 932853 and using a comminuting machine operating on the so-called impact comminution principle, for example the Atrex mill manufactured by Megatrex Oy. The inventors have noticed that when the method of said invention is applied to cereals and phytosterols, the temperature of the cereal grains is raised by the effect of mechanical energy, thereby providing a heat treatment of the cereals while being comminuted.

Zawistowski, WO 00/45648, describes a process for the preparation of microparticles of phytosterols and phytostanols, or mixtures of both, by dispersing and suspending the phytosterols and phytostanols in a semi-fluid, fluid or viscous carrier and exposing the carrier so formed to an impact force. The method comprises dispersing or suspending the phytosterols and/or phytostanols in a suitable semi-fluid, fluid or viscous carrier and then subjecting the carrier to impact forces to produce microparticles. Zawistowski achieves these impact forces by creating high shear with an air atomizing nozzle, pneumatic nozzle, high shear mixer, or colloid mill, but is preferably a microfluidizer commercially available from Microfluidics Incorporation, Newton, Massachusetts.

Zawistowski observes that phytosterols and/or phytostanols prepared in this manner not only have greater "solubility" in oil-based delivery systems, but also in other media, and can be added to beverages such as colas, fruit juices or dietary supplements, and/or milk substitute beverages.

Gottemoller, WO 01/37681A1, also describes a method of combining phytosterols and/or phytostanols with water-soluble proteins and optionally an emulsifier by comminuting or granulating the phytosterols and phytostanols to produce a powdered product which is then added to an aqueous material.

Tarr et al, WO 94/27451, describe a process for preparing a thickener from citrus fruit for beverages comprising preparing a slurry of water and citrus pulp having a solids content of 0.15% to 10% by weight (anhydrous), then heating the slurry to a temperature of 70 ℃ to 180 ℃ (158 ° F to 356 ° F) for 2 to 240 minutes and allowing the slurry to stand at 20,000sec^-1～100,000,000sec^-1By subjecting to high shear treatment at a pressure of 1,000psig to 15,000psig and milling with a colloid mill.

Its advantage is that it overcomes at least one of the difficulties in this related art. At least one other advantage is achieved according to the present invention, which provides a method of preparing a substantially stable dispersion consisting essentially of hydrophobic plant sterols and an aqueous material, such as an aqueous beverage concentrate, and products made therefrom, all of which substantially eliminate one or more of the limitations or drawbacks of the related art methods and compositions, such as lack of viscosity increase, development of off-flavors or powdery tastes, addition of undesirable components, or development of undesirable appearance.

Additional features of the invention will be set forth in the description which follows, and in part will be readily apparent to those skilled in the art from that description or recognized by practicing the invention, as well as the objects and other advantages of the invention which are achieved by the methods and compositions particularly pointed out in the written description and claims hereof.

Disclosure of Invention

To achieve at least one of these and other benefits and in accordance with the purposes of the present invention, as embodied and broadly described, the present inventors have discovered a method of making a substantially stable dispersion consisting essentially of a hydrophobic plant sterol and an aqueous material, such as an aqueous beverage concentrate, e.g., a juice concentrate, wherein the plant sterol is selected from the group consisting of plant sterols and plant stanols. The term "phytosterol" as used in the present specification and claims is intended to include phytosterols and phytostanols, unless otherwise indicated. The method comprises mixing hydrophobic plant sterol with an aqueous material to form a first dispersion of hydrophobic plant sterol particles and the aqueous material, wherein the particle size of the hydrophobic plant sterol particles in the first dispersion is from about 0.1 microns to about 100 microns. The process further comprises homogenizing the first dispersion to obtain a second dispersion of hydrophobic plant sterol particles and an aqueous material, wherein the particle size of the hydrophobic plant sterol particles in the second dispersion is from about 0.1 micron to about 100 microns.

The process of the present invention and the resulting composition do not require the use of gums and/or emulsifiers to obtain a stable dispersion of phytosterols in an aqueous material without segregation, flavor impact and texture impact, particularly during the preparation of a juice concentrate, e.g., a citrus juice concentrate, e.g., an orange juice concentrate.

The substantially stable dispersions of the present invention comprise dispersions of hydrophobic plant sterols produced according to the process of the present invention in an aqueous material that, after subjecting the dispersion to several heating and cooling cycles and/or shelf storage for that period of time, result in dispersions from which the plant sterols do not separate for a period of up to about 12 months. When used in citrus juice concentrates, if the phytosterols precipitate, it precipitates with the precipitating pulp, which is a natural phenomenon of citrus juice.

Citrus beverages such as orange juice have two types of pulp, one floating and the other precipitating. Pulp imparted to orange juice floes includes settled pulp while floating pulp rises to the surface of the juice and container. Phytosterols have a lower density than water and as a result will float on top of aqueous beverages such as citrus beverage concentrates or juices. If not properly dispersed, the phytosterols form white rings on top of the citrus beverage. An advantage of the present invention includes providing a dispersion of phytosterols and aqueous material, such as citrus beverage concentrate or citrus beverage, without separation of the phytosterols and formation of white rings on the beverage. The present inventors have found that the phytosterols of the present invention, including those mixed with juice concentrates, citrus juice concentrates or beverages such as orange juice, do not rise to the surface of the beverage, but rather can remain dispersed in the beverage and cause an increase in the volume of the settled pulp at the bottom of the beverage. This increased volume of precipitated pulp suggests the presence of phytosterols in the precipitated pulp. In any event, the juice, citrus beverage concentrate or citrus beverage formulated in accordance with the present invention can be substantially free of, or free of, phytosterols floating on the surface, in accordance with the present invention.

One novel finding is that the process of the present invention does not require heating of the first dispersion prior to homogenization or heating of the second dispersion after homogenization. However, heating is desirable to sterilize and prevent spoilage of the products produced by the process of the present invention. Thus, the process of the present invention may optionally further comprise one or more heating steps. In an optional embodiment, the process can further comprise a heating step wherein the first dispersion of hydrophobic plant sterol particles and the aqueous material is heated to a temperature of from about 43 ℃ to about 100 ℃ (about 110 ° F to about 212 ° F) for from about 1 second to about 20 seconds to form a heated first dispersion. In another optional embodiment, this optional heating step may be performed after homogenization.

In another embodiment, forming the dispersion of the present invention optionally comprises cooling the optionally heated first dispersion to a temperature of from about 22 ℃ (about 72 ° F) to about 71 ℃ (about 160 ° F) for from about 1 second to about 12 seconds, followed by homogenization.

In yet another embodiment, the method can include homogenizing at different pressures and stages, optionally at different temperatures from about 22 ℃ (about 72 ° F) to about 71 ℃ (about 160 ° F).

In yet another embodiment of the present invention, the aqueous material may comprise an aqueous beverage concentrate, such as a citrus juice concentrate, e.g., an orange juice concentrate.

Another aspect of the present invention relates to the discovery that a process for preparing the compositions of the present invention that avoids separation of the plant sterol requires the use of a beverage concentrate, beverage or aqueous medium having a viscosity of from about 100cps to about 30,000cps, alternatively from about 5,000cps to about 30,000cps, alternatively from about 6,000cps to about 18,000 cps. When the beverage concentrate, beverage, or aqueous medium does not fall within these viscosity ranges, the compositions of the present invention can be prepared to form the first and second dispersions using the processing steps used in the present invention, or any other method, but using processing aids used in the art to bring the viscosity within these ranges.

The present invention also relates to the discovery that dispersions of hydrophobic plant sterols in aqueous materials can avoid the difficulties of the prior art of imparting a powdery taste to dispersions when the particle size of the hydrophobic plant sterol particles is from about 0.1 microns to about 50 microns, or when the majority of the hydrophobic plant sterol particles within this range is from about 0.2 microns to about 10 microns, or in any event substantially following a bell curve distribution for any of these particle size distributions. The term "majority" as used in the present specification and claims means greater than 50%.

Brief Description of Drawings

FIG. 1 is an example of the particle size distribution of a sample of micronized phytosterols having a total phytosterol content greater than about 93% and consisting of beta-sitosterol, beta-sitostanol, campesterol, campestanol, stigmasterol, spinasterol (spinosterol), avenasterol and brassicasterol, which mixture has a melting point of about 138 ℃ to about 141 ℃, which are derived from vegetable oil and tall oil and supplied by MB Multi Bene Health Oy Ltd. of Finland.

FIG. 2 shows the volume distribution of the micronized phytosterols of FIG. 1.

Detailed Description

Accordingly, the present invention relates to a process for the preparation of a substantially stable dispersion comprising at least one hydrophobic phytosterol and an aqueous material such as an aqueous beverage concentrate, wherein the at least one phytosterol is selected from the group consisting of phytosterols and phytostanols (stanols), and wherein the dispersion is free of any added emulsifiers and thickeners and other so-called "processing aids" used in the food art, such as encapsulating materials.

Another aspect of the present invention relates to the discovery that the process of making the compositions of the present invention avoids separation of the plant sterol requiring the use of a beverage concentrate, beverage or aqueous medium having a viscosity of from about 100cps to about 30,000cps, alternatively from about 5,000cps to about 30,000cps, alternatively from about 6,000cps to about 18,000cps, alternatively from about 8,000cps to about 15,000 cps. The viscosity measurements described in the present specification and claims are measured using a Brookfield viscometer model # LVDV-11+ using Spindle #3 at 20 rpm. Further, where the beverage concentrate, beverage, or aqueous medium does not fall within these viscosity ranges, the compositions of the present invention can be prepared to form the first and second dispersions using the processing steps used in the present invention, or to use processing aids used in the food arts to bring the viscosity within these ranges. These processing aids may be added to the composition before processing begins or at any stage during processing.

When the hydrophobic plant sterol is mixed with an aqueous material, such as an aqueous beverage concentrate, to form particles of the at least one hydrophobic plant sterol and the first dispersion and/or the second dispersion of the aqueous material, the particle size of the particles of the at least one hydrophobic plant sterol in the first dispersion and/or the second dispersion is from about 0.1 micron to about 100 microns, or from about 0.1 micron to about 50 microns, or from about 0.1 micron to about 30 microns, or from about 0.1 micron to about 10 microns, and in one embodiment substantially follows a bell curve distribution. In another embodiment, to substantially avoid a powdery taste in the aqueous beverage, or concentrate, or beverage, the particle size of the at least one hydrophobic plant sterol particle in the first dispersion and/or the second dispersion is from about 0.1 micron to about 30 microns, or wherein the majority of the particles have a size in any of the preceding ranges from about 0.2 microns to about 10 microns, or from about 0.2 microns to about 2.5 microns, or from about 0.4 microns to about 1.5 microns, or from about 0.3 microns to about 0.4 microns, and in another embodiment substantially follows a bell curve distribution. All of the foregoing particle sizes and particle size ranges may also vary by + -about 30%, alternatively + -about 20%, alternatively + -about 10%. Hydrophobic plant sterol particles of all hydrophobic particle sizes and particle size ranges are well known in the art and are available from suppliers such as Cargill Co.

One aspect of the present invention includes a process for preparing a substantially stable dispersion comprising at least one hydrophobic plant sterol and an aqueous material, wherein the plant sterol is selected from the group consisting of plant sterols and plant stanols, the process comprising:

(a) mixing the hydrophobic plant sterol with the aqueous material to form a first dispersion of the hydrophobic plant sterol particles and the aqueous material; and

(b) homogenizing said heated mixture to obtain a second dispersion of said hydrophobic plant sterol particles and said aqueous material, wherein the particle size of said hydrophobic plant sterol particles in said first dispersion is from about 0.1 microns to about 100 microns, or the particle size of said hydrophobic plant sterol particles in said second dispersion is from about 0.1 microns to about 100 microns, or wherein the particle size of said hydrophobic plant sterol particles in both said first dispersion and said second dispersion is from about 0.1 microns to about 100 microns.

In one embodiment, the method may further comprise heating the first dispersion prior to the homogenizing step to form a heated first dispersion prior to homogenizing. In another embodiment, the method may also optionally include heating the second dispersion to form a heated second dispersion. In yet another embodiment, the method may optionally include heating both the first dispersion and the second dispersion.

Another aspect of the process of the present invention is that a composition of matter which is a substantially stable dispersion of at least one hydrophobic phytosterol or phytostanol and an aqueous material may be prepared which includes hydrophobic phytosterol or phytostanol particles as described above in order to substantially avoid a powdery taste in the aqueous material, or concentrate, or beverage. A composition of matter having such particle size, or particle size and particle size distribution, to substantially avoid a powdery taste in an aqueous material, or concentrate, or beverage product, can be prepared according to the method of the present invention, or by any other method used in the food arts, so long as it contains a phytosterol or phytostanol having such particle size, or particle size and particle size distribution, to avoid a powdery taste in the final product, and when not prepared according to the method of the present invention, may optionally contain processing aids used in the food arts. These processing aids can be used in amounts of about 0.001 wt% to about 50 wt% of the phytosterol, alternatively about 0.01 wt% to about 30 wt% of the phytosterol, alternatively about 0.01 wt% to about 25 wt% of the phytosterol or phytostanol, alternatively about 0.1 wt% to about 20 wt% of the phytosterol or phytostanol, all on an aqueous material, or concentrate, or beverage product basis.

By "processing aids" we include encapsulation aids, starches, gums used as thickeners in the food field, and pectins, demethylated pectins and other pectin derivatives used in the food field. Emulsifiers include modified food starches and other similar food-based emulsifiers, while gums include gum arabic, seaweed extracts, alginates, plant or seed gums such as guar gum, or animal derived products such as gelatin as well as xanthan gum, locust gum, carrageenan, and the like. Other water-soluble gums used in addition to gum arabic include brazil gum, saber gum, trachurus gum, cedar gum, and ghatti gum, while the sparingly water-soluble gums include tragacanth gum, karaya gum, sterculia gum, like apple gum, and basswood gum, or gums that swell in water such as cherry gum, jalapenom gum, or broom gum. In thatHackh′s Chemical Dictionary3d ed., p.392 defines other gums encompassed by this aspect of the invention.

The scientific literature describes at least 44 phytosterols and one skilled in the art can select any of these from those obtained in the practice of the present invention. The present invention also encompasses the use of some of the phytosterols employed in the art. Some phytosterols in this regard include sitosterol, campesterol, stigmasterol, spinasterol, taraxasterol, brassicasterol, 24-dehydrocholesterol, chalinosterol (chalinosterol), poriferasterol, clionasterol, and ergosterol. The present invention also uses phytosterols, such as two-component, three-component, and four-component mixtures.

Sources of these and other phytosterols are rice bran, corn germ, wheat germ oil, corn oil, safflower oil, oat oil, olive oil, cottonseed oil, soybean oil, peanut oil, black tea, green tea, taro (colocosia), kale, broccoli, sesame, african butter, grapeseed oil, rapeseed oil, linseed oil, canola oil, tall oil and other oils obtained from wood pulp.

Phytosterols may also be hydrogenated to produce phytostanols. Thus, the phytostanols of the present invention are described as the hydrogenation products of various phytosterols, such as sitosterol, but may also be obtained naturally from various plants used in the art without hydrogenating the phytosterols. Thus, the term "hydrogenation product of phytosterols" as used herein with respect to phytostanols includes not only synthetic phytostanols, but also those obtained from natural sources. Some phytostanols of this aspect include sitostanol, campestanol, stigmastanol, spinasterol, taraxostanol, brassicastanol, cholestanol, spongosterol, poriferostanol, clionastanol, and ergostanol. One skilled in the art can also select any phytostanol from those commercially available. The present invention also contemplates the use of phytostanols, e.g., mixtures of two, three and four, and mixtures of phytosterols and phytostanols, e.g., mixtures of two, three and four components.

Both phytosterols and phytostanols include the various positional isomers and stereoisomeric forms used in the art, such as the alpha and beta isomers, as well as phytosterols and phytostanols having small (1 to about 4 carbon atoms) side chains. Beta-sitosterol and beta-sitostanol comprise one of the most effective phytosterols and one of the most effective phytostanols, respectively, for lowering serum cholesterol in mammals.

In one embodiment of the present invention, the mixing of at least one hydrophobic plant sterol with an aqueous beverage concentrate to form a first dispersion of particulates can be carried out at a temperature of from about-10 ℃ to about 100 ℃ (about 14 ° F to about 212 ° F), alternatively from about 0 ℃ to about 82 ℃ (about 32 ° F to about 180 ° F), alternatively from about 18 ℃ to about 64 ℃ (about 64 ° F to about 148 ° F), alternatively from about 24 ℃ to about 57 ℃ (about 75 ° F to about 135 ° F) for from about 0.1 minute to about 120 minutes, alternatively from about 5 minutes to about 60 minutes, alternatively from about 15 minutes to about 30 minutes, to form the first dispersion.

Apparatus for preparing a first dispersion of at least one hydrophobic plant sterol particle and an aqueous material, such as a beverage concentrate, includes a high shear mixer (e.g., Arde-Barinco model CJ-4) or any high capacity (e.g., about 50 to about 300 gallons) high shear mixer. The commercial equipment used to prepare the first dispersion includes "liquidver" (trade mark) available under the trade designation APV liquidver model 200# CLV, manufactured by APV, an Invensys Company.

In another embodiment, the at least one phytosterol supplied may be micronized to a size of about 0.5 to about 10 microns. FIG. 1 shows an exemplary particle size distribution of micronized phytosterols according to one embodiment of the present invention. In fig. 1, "DF × position diff.distribution" refers to a dilution factor multiplied by the total differential distribution, i.e., the count of each channel multiplied by the factor of sample dilution, to obtain a count of pure samples. FIG. 2 shows an exemplary volume distribution of micronized phytosterols according to one embodiment of the present invention. In fig. 2, "Volume-Wt-diff.distribution" refers to the Volume-weight differential distribution, i.e., the distribution of each particle size channel over the entire Volume of the sample is determined by taking all particles and observing their Volume. U.S. Pat. No. 6,129,944 describes a method and apparatus for preparing the phytosterol compositions of FIGS. 1 and 2; however, the food industry also uses spray drying techniques to form these compositions.

In fig. 1, the numerical value of each "count" reported (the value of ordinate) and the numerical value of each particle diameter reported (micrometer) (the value of abscissa) may be arbitrarily changed within a range of ± about 30% or ± about 20% or ± about 10%, whereas in fig. 2, the numerical value of each relative percentage reported (the value of ordinate) and the numerical value of each particle diameter reported (micrometer) (the value of abscissa) may be arbitrarily changed within a range of ± about 30% or ± about 20% or ± about 10%. Although the data of fig. 1 and 2 are directed to a particular phytosterol product, these data may also define the particle size and particle size distribution of any phytosterol used in the present invention, such as those described in the present specification and used in the art.

It is believed that in forming the first dispersion of the at least one hydrophobic plant sterol and the aqueous material, the shear stress and/or shear rate applied to the hydrophobic plant sterol and the aqueous medium is sufficient to form a somewhat stable dispersion of particles of the at least one hydrophobic plant sterol and the aqueous material; however, the first dispersion does not have sufficient long-term stability to enable its use in edible products such as juices, beverages, fruit drinks and the like.

The particle size of the at least one hydrophobic plant sterol in both the first dispersion and the second dispersion may substantially follow a bell curve particle size distribution as is well known to those of ordinary skill in the art.

The aqueous material may include water, water and other compounds, and compositions dissolved or dispersed therein, either as a dispersion of a solid in water or an emulsion of a liquid in water or water in a liquid. This defines the aqueous material of the present invention prior to mixing with at least one hydrophobic plant sterol. When aqueous materials having dissolved or dispersed compounds or compositions are used, the solids content of the aqueous material, e.g., aqueous beverage concentrate, is from about 200g/l to about 1000g/l aqueous material, alternatively from about 400g/l to about 900g/l, alternatively from about 600g/l to about 800 g/l. The term "solids content" as used in the context of the "aqueous material" of the present invention also includes any liquid added to water to form the "aqueous material" in the form of an emulsion as defined herein.

The at least one hydrophobic plant sterol may be present in the first dispersion and/or the second dispersion in an amount of from about 1g to about 100g/l or from about 10g to about 60g/l, or from about 20g to about 30g/l of the aqueous material, concentrate or beverage product. In one embodiment, the at least one hydrophobic plant sterol is present in the first dispersion and/or the second dispersion in an amount of from about 15g to about 30g per liter of aqueous material, concentrate or beverage product.

In one embodiment, the method may further comprise heating the first dispersion prior to the homogenizing step to form a heated first dispersion prior to homogenizing. In another embodiment, the method may also optionally include heating the second dispersion to form a heated second dispersion. In yet another embodiment, the method may optionally include heating both the first dispersion and the second dispersion.

In one embodiment, the first dispersion is optionally heated to a temperature of from about 18 ℃ (about 64 ° F) to about 64 ℃ (about 148 ° F) for from about 0.1 minute to about 120 minutes. In another embodiment of the present invention, the first dispersion is optionally heated to a temperature of from about 110 ° F to about 212 ° F for from about 1 second to about 20 seconds.

In another embodiment, the first dispersion is optionally heated to a temperature of about 49 ℃ (about 120 ° F) to about 88 ℃ (about 190 ° F) for about 1 second to about 20 seconds.

In another embodiment of the present invention, the heated first dispersion is optionally cooled to a temperature of from about 0 ℃ to about 100 ℃ (about 32 ° F to about 212 ° F), alternatively from about 13 ℃ to about 87 ℃ (about 55 ° F to about 189 ° F), alternatively from about 26 ℃ to about 75 ℃ (about 78 ° F to about 167 ° F) for from about 1 second to about 30 seconds, alternatively from about 2 seconds to about 10 seconds, alternatively from about 5 seconds to about 7 seconds, prior to homogenization to form a second dispersion of particles of the at least one hydrophobic plant sterol and the aqueous material.

In yet another embodiment, the optionally heated first dispersion is cooled to a temperature of about 22 ℃ (about 72 ° F) to about 71 ℃ (about 160 ° F) for about 1 second to about 12 seconds prior to homogenization.

In another embodiment of the present invention, the second dispersion is optionally heated to a temperature of from about 0 ℃ (about 32 ° F) to about 100 ℃ (about 212 ° F) for from about 1 second to about 20 seconds to form a heated second dispersion.

In yet another embodiment, the second dispersion is optionally heated to a temperature of from about 49 ℃ (about 120 ° F) to about 88 ℃ (about 190 ° F) for from about 1 second to about 20 seconds to form a heated second dispersion.

In yet another embodiment, the optionally heated second dispersion is cooled to a temperature of from about-8 ℃ to about 32 ℃ (about 17 ° F to about 90 ° F), alternatively from about 2 ℃ to about 4 ℃ (about 35 ° F to about 40 ° F) for from about 1 second to about 12 seconds, alternatively from about 3 seconds to about 7 seconds.

Homogenizing the first dispersion to obtain particles of at least one hydrophobic plant sterol and a second dispersion of an aqueous beverage concentrate is carried out in a homogenizer (e.g., APV # APV 1000 type), which can be acted upon by passing the dispersion through small orifices under high pressure. The homogenization can be conducted at a pressure of from about 100psi to about 14,500psi, or from 500psi to about 10,000psi, or from 1,000psi to about 5,000 psi. In one embodiment, the homogenizing is performed at a pressure of about 2,000psi to about 5,000 psi.

The invention also relates to homogenization in one or more stages, such as one, two, three, four or more stages, at different pressures.

Homogenization at high and low pressures may also be carried out, for example, according to any of the following parameters and combinations thereof:

high pressure Low pressure

About 2000psi and about 300psi

About 3000psi and about 400psi

About 3000psi and about 500psi

About 5000psi and about 1000psi

About 3400psi and about 600psi

The sequence is typically first homogenised at high pressure and then at low pressure, but the method of the invention also includes homogenisation at different pressure sequences and in one embodiment, with a plurality of homogenisers.

Various beverage concentrates can be used as the aqueous material according to the process of the present invention, however, in one embodiment, the process involves preparing a substantially stable dispersion comprising at least one hydrophobic plant sterol and an aqueous citrus juice concentrate, such as an orange juice concentrate.

In its broader aspects, the aqueous materials of the present invention include water, and combinations of water with nutrients, flavors, sweeteners, carbon dioxide and other gases, and combinations thereof. In another aspect, the aqueous material is a fruit juice or fruit-flavored concentrate, such as citrus juices including orange, lemon, grapefruit, tangerine, mandarin orange, and grape juices, and other juice and fruit-flavored concentrates such as acerola, grape, pear, passion fruit, pineapple, banana, apple, cranberry, cherry, raspberry, peach, plum, grape, currant, cranberry, blackberry, blueberry, strawberry, brazzy, watermelon, honeydew melon, muskmelon, mango, papaya, botanical flavors such as those derived from cola, tea, coffee, chocolate, vanilla, almond, vegetable juices and flavors such as tomato, cabbage, celery, cucumber, spinach, carrot, lettuce, watercress, dandelion, rhubarb, beet, coconut, guava, hanguo, and mixtures thereof, such as two-component, three-component and four-component mixtures.

The aqueous material of the present invention may also include concentrates of typical sports drinks, and beverages for treating liquids lost due to illness and containing sucrose syrup, glucose-fructose syrup, citric acid, sodium citrate, monopotassium phosphate and potassium salts, and other materials for replenishing lost electrolytes, whether or not the product requires the addition or mixing with water.

The concentrate of the present invention may be diluted with water to form a juice or beverage. For example, where the concentrate includes a sugar or mixture of sugars, it can be diluted with water to about 2 ° Brix to about 20 ° Brix, alternatively about 6 ° Brix to about 16 ° Brix, alternatively about 11 ° Brix to about 13 ° Brix. The sugars used in accordance with the present invention may generally include carbohydrate materials such as fructose, sucrose, glucose, and the like, as well as other sugars used in the art, such as McMurry,Organic Chemistry，Third Edition，pp.916-950、Hawley′s Condensed Chemical Dictionarytwolfth Edition, p.1100 andHackh′s Chemical Dictionarythird Edition, pp.815-817. Mixtures of sugars, such as two-component, three-component, or four-component mixtures, may also be used.

The process for preparing a substantially stable dispersion comprising the at least one hydrophobic plant sterol and the aqueous material may further comprise adding at least one water soluble vitamin, such as vitamin C, vitamin B6 and/or vitamin B12, folic acid, and/or at least one oil soluble vitamin, such as vitamin a, beta carotene, vitamin B, e.g., D vitamins, vitamin E and vitamin K, and any mixtures thereof, e.g., two-component, three-component and four-component mixtures, to the substantially stable dispersion of the invention before, during or after preparing the substantially stable dispersion, e.g., by adding the one or more vitamins to the step of preparing the first dispersion or the step of preparing the second dispersion, or both. The addition of vitamins, such as vitamins B and E, is modified to obtain an RDA of about 1% to about 100%, alternatively about 5 to about 30%, alternatively about 15 to about 20% RDA per unit serving of each vitamin.

The following examples illustrate the invention.

Example 1:

the following components are mixed to provide a base mixture of the hydrophobic plant sterol and the aqueous material, which is then processed to form the first dispersion.

The following compositions were formulated and obtained:

base component

Required volume 2.2 gallons

2,079.4 g of water

Orange concentrate 7,837.0 g

Orange flavour 119.6 g

Orange oil 6.3 g

Plant sterol 198.1 g

Total 10,240.8 g

Final product components

Required volume 4.4 gallons

13,262.9 g of water

Base material 4,178.3 g

Base material specification	OPT.	MIN.	MAX.
				Percent soluble solids	49.7	49.4	50.5
Refractometer Brix	49.8	49.5	50.6
				% acid w/w based on citric acid	2.8	2.5	3.1
Brix/acid ratio	17.5	15.7	19.8

The substantially stable dispersion of lipophilic phytosterol and orange juice concentrate as an aqueous material has a concentration of 48.9 ° Brix (refractometer Brix, acid corrected).

The mixture was mixed using an Arde-Barinco model CJ-4 high shear mixer at 7000rpm to produce a first dispersion having an average particle size of about 10 microns and a particle size distribution of about 0.5 microns to about 30 microns with a maximum particle size of about 30 microns for about 15 minutes.

This first dispersion was homogenized in An APV Homogenizer model APV 1000 from APV homogenerizer Group (An Invensys company) at 2,500psi and then 500psi to produce a second dispersion.

The second dispersion comprises a substantially stable dispersion consisting essentially of a hydrophobic plant sterol and orange juice concentrate as the aqueous material. Adding water to the substantially stable dispersion, an orange juice product of 12.0 Brix is produced. The following specifications were made:

product specification	OPT.	MIN.	MAX.
				Percent soluble solids	12.0	11.9	12.2
Refractometer Brix	11.9	11.8	12.1
				% acid w/w based on citric acid	0.67	0.65	0.69
Brix/acid ratio	18.0	17.3	18.8

Example 2:

the following components are mixed to provide a base mixture of the hydrophobic plant sterol and the aqueous material, which is then processed to form the first dispersion.

The following compositions were formulated and obtained:

base component

The required volume is 0.8 gallon

180.2 g of water

Orange concentrate 3,363.0 g¹

Orange flavour 53.1 g

Orange oil 2.7 g

Phytosterol 76.7 g²

Total 3,675.5 g

1 refractometer ° Brix, 65 (acid corrected); acid, 3.71% (wt./wt.).

2ADM 09/2001 consisting essentially of beta sitosterol, beta sitostanol, campesterol, campestanol, stigmasterol, spinasterol, avenasterol, or brassicasterol, having a particle size of from about 0.5 micron to about 30 microns.

Final product components

Required volume 4.8 gallons

4.1 gallons of water

Base 0.8 gallon

Base material specification	OPT.	MIN.	MAX.
				Percent soluble solids	61.6	61.1	62.4
Refraction of lightBrix of degree	61.6	60.7	62.0
				% acid w/w based on citric acid	3.4	3.1	3.7
Brix/acid ratio	18.0	16.4	20.0

The substantially stable dispersion of lipophilic phytosterol and orange juice concentrate as an aqueous material has a concentration of 61.2 ° Brix (refractometer Brix, acid corrected).

The mixture was stirred at 7000rpm using an Arde-Barinco model CJ-4 high shear mixer for about 15 minutes and heated to 82.2 ℃ (180 ° F) over 8 seconds and cooled to about 43.3 ℃ to about 60 ℃ (about 110 ° F to about 140 ° F) in about 5 seconds to produce a first dispersion having an average particle size of about 10 microns and a particle size distribution of about 0.5 microns to about 30 microns with a maximum particle size of about 30 microns.

This first dispersion was homogenized in An APV homogenizer model APV 1000 from APV homogene Group (An Invensys company) at 60 deg.C (140 deg.F), 3,400psi and then 600psi to produce a second dispersion.

The second dispersion comprises a substantially stable dispersion consisting essentially of a hydrophobic plant sterol and orange juice concentrate as the aqueous material. Adding water to the substantially stable dispersion, an orange juice product of 12.0 Brix is produced. The following specifications were made:

product specification	OPT.	MIN.	MAX.
				Percent soluble solids	12.0	11.9	12.2
Refractometer Brix	11.9	11.8	12.1
				% acid w/w based on citric acid	0.67	0.65	0.69
Brix/acid ratio	18.0	17.3	18.8

Example 3:

the following components are mixed to provide a base mixture of the hydrophobic plant sterol and the aqueous material, which is then processed to form the first dispersion.

The following compositions were formulated and obtained:

base component

Required volume 2,000.0 gallons

4,158.8 pounds of water

Orange concentrate 15,674.0 pounds

239.2 pounds of orange flavor

Orange oil 12.7 pounds

396.2 lbs. phytosterols

Total 20,480.9 pounds

Final product components

Required volume 1,000 gallons

6,631.5 pounds of water

Base 2,089.1 pounds

Base material specification	OPT.	MIN.	MAX.
				Percent soluble solids	49.7	49.4	50.5
Refractometer Brix	49.8	49.5	50.6
				% acid w/w based on citric acid	2.8	2.5	3.1
Brix/acid ratio	17.5	15.7	19.8

The substantially stable dispersion of lipophilic phytosterol and orange juice concentrate as an aqueous material has a concentration of 50.1 ° Brix (refractometer Brix, acid corrected).

The mixture was mixed under constant agitation in a 2200 gallon batch tank prior to addition of the phytosterols or stanols. The dispersion was then pumped through a 200 gallon NormanMachinery co.ds 200 high shear mixer and the phytosterols were gradually added to the high shear mixer through an 1/2 inch mesh screen to produce a first dispersion having an average particle size of about 10 microns and a particle size distribution of about 0.5 microns to about 30 microns with a maximum particle size of about 30 microns.

The first dispersion was homogenized at 2500psi and then 500psi by passing through a 30 gallon/minute APV homogenizer to produce a second dispersion. The second dispersion was then heated to 72.7 ℃ (163 ° F) over 8 seconds and cooled to about 2 ℃ to about 4 ℃ (about 35 ° F to about 40 ° F) in about 5 seconds.

The second dispersion comprises a substantially stable dispersion consisting essentially of a hydrophobic plant sterol and orange juice concentrate as the aqueous material. Adding water to the substantially stable dispersion, an orange juice product of 12.0 Brix is produced. The following specifications were made:

product specification	OPT.	MIN.	MAX.
				Percent soluble solids	12.0	11.9	12.2
Refractometer Brix	11.9	11.8	12.1
				% acid w/w based on citric acid	0.67	0.65	0.69
Brix/acid ratio	18.0	17.3	18.8

The various ranges describing the invention as described herein also include any combination of the lower limits of the ranges described herein and the upper limits of the ranges, and any single experimental value or other single value described herein which will either increase or decrease the lower limit of the range or the upper limit of the range, where the range includes, inter alia, time, temperature, pressure, concentration of compounds and compositions, including ° Brix, the ratio of such compounds and compositions to each other, particle size distribution, percentage variations, etc., and all whole and/or fractional values included in such ranges, and ranges included within such ranges. The term "about" as used for individual values and values recited in the ranges of the specification means that these values vary slightly. For example, concentration values given in ° Brix may vary by ± 2%, time values given in seconds may vary by ± 1 second, time values given in minutes may vary by ± 1 minute, temperature values given in ° c or ° F may vary by ± 2%, pressure values given in psi may vary by ± 10%, particle size values given in microns may vary by ± 5%, solids content values given in g/L may vary by ± 2%, viscosity values given in cps may vary by ± 10%. The term "substantially" as used in this specification means completely what is meant or what is meant by a large or large fraction, particularly those terms (i.e., "about", "substantially") as understood by those of ordinary skill in the art. U.S. patents or other patents and other printed publications cited in this specification are herein incorporated by reference in their entirety, including any references cited therein. All amounts in percent are by weight unless otherwise indicated.

The foregoing written description describes the principles, various embodiments and modes of operation of the present invention. However, the invention claimed in this application, i.e., the invention claimed, should be construed to include variations or modifications that may be resorted to by those skilled in the art without departing from the spirit of the invention.

Claims (21)

1. A process for preparing a substantially stable dispersion comprising at least one hydrophobic plant sterol and an aqueous material, the process comprising:

mixing said at least one hydrophobic plant sterol with said aqueous material to form a first dispersion of particles of said at least one hydrophobic plant sterol and said aqueous material;

homogenizing the first dispersion to obtain particles of said at least one hydrophobic plant sterol and a second dispersion of said aqueous material, wherein the particle size of said at least one hydrophobic plant sterol particles in said first dispersion is from 0.1 micron to 100 microns, or the particle size of said at least one hydrophobic plant sterol particles in said second dispersion is from 0.1 micron to 100 microns, or wherein the particle size of said hydrophobic plant sterol particles in both said first dispersion and said second dispersion is from 0.1 micron to 100 microns, with the proviso that said first and/or second dispersion does not use emulsifiers, thickeners and/or processing aids to obtain a substantially stable dispersion of said at least one hydrophobic plant sterol in said aqueous material.

2. The method of claim 1, wherein said particle size of said at least one hydrophobic plant sterol in said first dispersion is from 0.1 microns to 50 microns, or from 0.1 microns to 30 microns, or from 0.1 microns to 10 microns, or alternatively

The particle size of the at least one hydrophobic plant sterol in the second dispersion is 0.1 microns to 50 microns, or 0.1 microns to 30 microns, or 0.1 microns to 10 microns, or

The particle size of the at least one hydrophobic plant sterol in at least one of the first and second dispersions is from 0.1 micron to 50 microns, or from 0.1 micron to 30 microns, or from 0.1 micron to 10 microns.

3. The method of claim 1, wherein the particle size of the majority of the at least one hydrophobic plant sterol is in the range of 0.2 microns to 10 microns, or 0.2 microns to 2.5 microns, or 0.4 microns to 1.5 microns, or 0.3 microns to 0.4 microns.

4. The method of claim 1, wherein said at least one hydrophobic plant sterol is selected from the group consisting of:

sitosterol, campesterol, stigmasterol, spinasterol, taraxasterol, brassicasterol, 24-dehydrocholesterol, spongosterol, bolifrasterol, clionasterol, and ergosterol.

5. The process of claim 1 wherein said at least one hydrophobic phytosterol is selected from the group consisting of the hydrogenation products of phytosterols.

6. The method of claim 1, wherein said at least one hydrophobic plant sterol is selected from the group consisting of:

sitostanol, campestanol, stigmastanol, spinastanol, taraxostanol, brassicastanol, cholestanol, spongosterol, bolifrastanol, clionastanol, and ergostanol.

7. The method of claim 1, wherein the aqueous material comprises a solid material dissolved or dispersed therein, and wherein the solid content of the aqueous material is 200-.

8. The method of claim 1, wherein, in said first dispersion, said at least one hydrophobic plant sterol is present in an amount of from 1 to 100g/l, or from 10 to 60g/l, or from 15 to 30g/l of said aqueous material.

9. The method of claim 1, wherein said homogenizing is performed at a pressure of from 100psi to 14,500psi, or from 500psi to 10,000psi, or from 1,000psi to 5,000psi, or from 2,000psi to 5,000 psi.

10. The method of claim 1, wherein the homogenizing is performed in multiple stages at different pressures, such as a first homogenizing at 2000psi to 5000psi followed by a second homogenizing at 300psi to 1000 psi.

11. The method of claim 1, wherein the aqueous material comprises at least one fruit juice concentrate.

12. The method of claim 11, wherein said aqueous material comprises at least one citrus juice concentrate.

13. The process according to claim 11 or 12, wherein water is added to said particles of said at least one hydrophobic plant sterol and said second dispersion of said fruit juice or said citrus juice concentrate to obtain an aqueous beverage mixture.

14. The method of claim 13, wherein the aqueous beverage mixture has a concentration of 11 ° Brix to 13 ° Brix.

15. The method of claim 12, wherein the at least one citrus juice concentrate is an orange juice concentrate.

16. The method of claim 1, wherein the viscosity of the substantially stable dispersion is from 100cps to 30,000cps, or from 5,000cps to 30,000cps, or from 6,000cps to 18,000cps, or from 8,000cps to 15,000 cps.

17. The method of claim 1, further comprising adding at least one vitamin before, during, or after preparing the substantially stable dispersion.

18. The method of claim 17, wherein the at least one vitamin is selected from the group consisting of water soluble vitamins and oil soluble vitamins.

19. A method of preparing a substantially stable dispersion comprising at least one hydrophobic plant sterol and an aqueous material, the method comprising:

mixing the at least one hydrophobic plant sterol with the aqueous material to form a first dispersion of particles of the at least one hydrophobic plant sterol and the aqueous material;

homogenizing said first dispersion to obtain particles of said at least one hydrophobic plant sterol and a second dispersion of said aqueous material, wherein the particle size of said at least one hydrophobic plant sterol particle in said first dispersion is from 0.1 micron to 100 microns, or the particle size of said at least one hydrophobic plant sterol particle in said second dispersion is from 0.1 micron to 100 microns, or the particle size of said hydrophobic plant sterol particles in both said first dispersion and said second dispersion is from 0.1 micron to 100 microns; and

heating the particles of the at least one hydrophobic plant sterol and the second dispersion of the aqueous material to produce a heated second dispersion, with the proviso that the first and/or second dispersion does not use emulsifiers, thickeners and/or processing aids to obtain a substantially stable dispersion of the at least one hydrophobic plant sterol in the aqueous material.

20. The method of claim 19, wherein said second dispersion of particles of said at least one hydrophobic plant sterol is heated to 32 ° F to 212 ° F for 1 second to 20 seconds, or to 120 ° F to 190 ° F for 1 second to 20 seconds.

21. The process of claim 19, wherein the heated second dispersion is cooled to 17 ° F to 90 ° F for 1 second to 12 seconds, or to 35 ° F to 40 ° F for 3 seconds to 7 seconds.