Process for producing pure guarseed flour

Organic compounds -- part of the class 532-570 series – Organic compounds – Carbohydrates or derivatives

Reexamination Certificate

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C536S001110, C426S622000, C426S615000

Reexamination Certificate

active

06664381

ABSTRACT:

BACKGROUND OF THE INVENTION
The object of the present invention is a process for producing guarseed flour which, when it is dissolved in water, produces a transparent solution of high viscosity, where the process produces good yields of the pure flour despite extensive cleaning. Transparent, high-viscosity solutions of pure guarseed flour are of great importance primarily in the food industry.
Guarseed flour is used as a thickening agent in the textile and explosives sectors, as a binding agent in the paper industry, as a flocculant in ore extraction and as an auxiliary material in the extraction of natural gas and oil, in the pharmaceutical and cosmetic fields, and as a thickener, emulsifier and (co-)stabilizer in the areas of foods and food technology.
In pharmaceutics guarseed flour is used for example for spray embedding of vitamins, in order to increase their shelf stability. In addition, the use of guarseed flour in sprays guarantees nearly monomolecular distribution of the active ingredients and consequently improved, uniform resorption, which is desirable in the case of asthma medications and various allergy remedies. Because of the extremely low protein content of the pure guarseed flour there is no danger of the development of an allergic reaction to a medication which contains this substance. Additional applications in this field are the formulation of delayed-action tablets and as a means of lowering the cholesterol level. In the field of medicine guarseed flour is also used as an emulsifier and stabilizer in contrast agents.
Among other applications, guarseed flour has also proven to be an ideal dietetic substance, since its building blocks, the so-called galactomannans, are not attacked by human stomach and intestinal enzymes. This is to be expected, since in the human digestive system up to the large intestine there are neither &bgr;-mannanases nor &agr;-glacto-sidases present, which would be necessary to break down these building blocks. Since the building blocks of guarseed flour do not enter into the human metabolism, there is no reason to regard guarseed flour as a carrier or supplier of calories. Since guarseed flour is constituted of completely neutral polysaccharides, or more precisely of galactomannans, which have neither uronic acid nor other ionogenic groups, they represent a completely harmless material in physiological terms.
An additional advantage in terms of its use as an ingredient in foods is its complete neutrality of taste. It is used in reduced-calorie or reduced-fat foods or drinks which are often perceived as “thin” by the consumer. Adding guarseed flour to these products lends them a “creamier” consistency. In the production of fruit juices guarseed flour is used in order to re-suspend the fruit pulp uniformly, in puddings and cremes it functions as a thickener, in ice creams, milkshakes, mousses and similar products it works as a stabilizer. With traditional guarseed flour preparations, only mild molecular interaction with the biopolymer xanthane was found. While mixing these two colloids did produce a synergistic increase in viscosity, a specific formation of gel as in the case of carubin, carob seed flour and xanthane, did not occur. If a 1:1 mixture of the guarseed flour in accordance with the invention and xanthane is heated together and allowed to cool at 4° C. (refrigerator temperature), a gel forms. An advantage of this combination of guarseed flour and xanthane lies in the fact that the gel from these two components melts at body temperature, so that it is superbly suited for the production of gelatin-like foods, as a vehicle for the delivery of medications in pill form, and the like. Furthermore, guarseed flour and xanthane are used in combination as co-stabilizers in the production of salad dressings, since this combination, in contrast to guarseed flour used alone, is resistant to acids.
Guarseed flour is obtained from the endosperm of the guar bean (
cyamopsis tetragonobolus
). Guarseed flour consists in large measure of galactomannans, i.e. of polysaccharides whose fundamental chain is linked in the 1→4 direction by &bgr;-glycoside bonds and is made up of mannose which is joined to galactose via primary OH groups. The ratio of unsubstituted mannose to mannose substituted with galactose is about 2:1, with the substituted units not alternating strictly but arranged in the polygalactommannan molecules in groups of two or three. The guar-galactomannans form highly viscous solutions in water even in slight concentrations. Acueous solutions of 1 percent by weight of common commercial guarseed flour produce viscosities of around 3000 to 6000 mPa·s.
Guar-galactomannans are divided into cold water soluble, hot water soluble and insoluble galactomannans on the basis of chemical and physiochemical differences.
To obtain and purify the guarseed flour the guarseed is treated mechanically; this produces approximately 35 parts unrefined guar endosperm halves and approximately 60 parts guar germ flour. The guar germ flour consists primarily of the germ of the seed, the scraped off bean skin, and small pieces of the endosperm. The endosperm completely encloses the germ and is in turn surrounded by the seed skin. A protein-rich, aleuron-like cell layer encloses the endosperm, whose cells are closely interlocked with the endosperm. This protein-rich layer adjoins the seed skin.
The unrefined endosperm halves can be further cleaned mechanically and produce splits of varying quality in terms of their protein content, their components which cannot by hydrolyzed by acid (A.I.R.) and the amount of skin present. The term “split,” which is usual among the specialists, is synonymous with the term “endosperm halves.”
Although guarseed flour is already in wide use as a thickening agent, there is a desire to improve its purity and, related thereto, its physical and physiological properties. For its use in foods, in particular, the purity of the guarseed flour is of great importance. Also desirable is more complete utilization of the main components of the endosperm, so that the latter can be used to a greater degree in the corresponding branches of industry in place of cellulose derivatives or other polysaccharides which are clearly soluble in water, or synthetic polymers which are clearly soluble in water.
If the products consisting of pure guarseed flour which are currently available on the market, when processed into flour, are dissolved in water at 25° C. or at 86 to 89° C. for 10 minutes, they produce cloudy solutions. If the insoluble material in these solutions is centrifuged out at high centrifugal forces (>35,000×g), it turns out that 23-35% of the guarseed flour comprises material which is centrifuged out. Microscopic investigations have shown that the centrifuged precipitate is made up primarily of skin fragments, protein materials, insoluble peripheral cells, intact unopened cells of the inner endosperm and other impurities of the seeds or splits. Chemical derivatization of the guarseed flour (etherification, hydroxypropylation, cationization, etc.) makes it possible to produce products with significantly improved dissolving behavior in water, and along with that, greater transparency of the solutions.
One of the processes used heretofore for obtaining pure guarseed flour uses chlorinated solvents, such as trichlorethylene (see EP 0 130 946, Meyhall Chemical AG). The solution was fractionated by simply being left to stand or by centrifuging, which led to the formation of a protein-rich fraction (floating fraction) and the separation of a protein-poor fraction (precipitating fraction).
It has been possible to show that the highest floating fraction of endosperm processed into flour, such as guar CSA 200/50, can contain up to 25% proteins, and the precipitating fraction, which makes up 75% of the pure flour, contains about 1.5 to 1.6% protein. The precipitating fraction is used for example to produce cationic derivatives, which can be dissolved to produce clear aqueous solutions. A disadvantage of this process is that finely-groun

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