United States Patent (19) 11 Patent Number: 4,980,186 Sharafabadi 45 Date of Patent: Dec

United States Patent (19) 11 Patent Number: 4,980,186 Sharafabadi 45 Date of Patent: Dec. 25, 1990

(54) PSEUDOPLASTIC YELLOW MUSTARD Mucilages as Examples of Polysaccharide Denatura GUM tion'. Weber et al., J. Food. Sci. (1974), 39, pp. 461–466 76 Inventor: Soheil K. Sharafabadi, Suite 808 400 "Functional Characteriscs of Mustard Mucilage'. Stradbrook, Winnipeg, Manitoba, Vose, Cereal Chem., (1974) 51, 658-665 "Chemical and Canada, R3L 2P8 Physical Studies of Mustard & Rapeseed Coats'. Theander et al., J Agri Food Chem. (1977), 25 pp. (21) Appl. No.: 393,657 270-273 "Carbohydrates, Polyphenols & Lignin. In 22 Filed: Aug. 14, 1989 Seed Hulls'. 511 Int. Cl...... C08B 37/00; A23L 1/225 “Woods et al., Can J. Plant Sci. (1980) 60, pp. 1031-33 (52) U.S.C...... 426/425; 426/430; Mucilage From Yellow Mustard'. 426/431; 426/506; 426/511; 426/629; 426/655; Primary Examiner-Donald E. Czaja 426/658 Assistant Examiner-Evan Federman 58) Field of Search ...... 426/425, 429, 430, 431, Attorney, Agent, or Firm-Robert W. B. Bailey 426/629, 658, 655, 506, 511 57 ABSTRACT (56) References Cited An improved process of gum extraction from whole U.S. PATENT DOCUMENTS yellow mustard seed is described. The process is time temperature interdependent. In a first step the seed is 3,615,648 10/1971 Barros ...... 426/431 treated in water, preferably at elevated temperature, the FOREIGN PATENT DOCUMENTS extract is then separated, preferably mechanically, more preferably by a perforated centrifuge, or even more 671499 la 1963 Canada ...... 426/431 preferably by a slitted centrifuge. The aqueous extract OTHER PUBLICATIONS on precipitation and drying gives a gum with pseudo plastic properties similar to those of xanthan gum. The Siddiqui et al., Food Microstructure (1986) pp. 157-162 extraction using mechanical separation, especially by a "Mucilage in Yellow Mustard Seeds'. perforated bowl centrifuge, which can be slitted, is Bailey et al., Biochem. J. (1932), 26, pp. 1609-1623 "The suitable for industrial scale extraction of the yellow Nature & Composition of the Seed of White Mustard mustard seed. A centrifuge adapted for juice extraction (Brassica alba)'. is suitable. The gum produced under these conditions Bailey, Biochem. J. (1935), 29, pp. 2477-2485 "Cress exhibits unique properties dramatically different from Seed Mucilage'. those reported from other previous processes, in both Hirst et al., Biochem. J. (1965) 95, pp. 453-458 "Seed composition and viscosities. Polysaccharides & Their Role in Germination'. Grant et al., Chem. Comm (1969) pp. 805-806 “Seed 20 Claims, 4 Drawing Sheets U.S. Patent Dec. 25, 1990 Sheet 1 of 4 4,980,186

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OO O.OO OO O. SHEAR RATE ki/s FG.8 PRIOR ART 4,980, 186 1. 2 minor components. The hot water kernel fraction poly PSEUDOPLASTIC YELLOW MUSTARD GUM saccharides after hydrolysis contained in rough order of concentration arabinose as major component and Xy This invention relates to natural products from oil lose, galactose and galacturonic acid as minor compo seeds. Especially it relates to extraction of gum from nents. A large scale extraction of the kernals produced yellow mustard seed, including a suitable industrial a polysaccharide almost entirely composed of arabi process. Such extracts are called gums or mucilages, nose, yielding 6.3% with cold water, and boiling water and are generally hydrocolloids containing polysaccha gave a further 6.1%. rides. While such gums may be designated as specific to Grant et al. Chem. Comm., (1969) 805 extracted a particular plant species seed, in fact the composition 10 yellow mustard seed with cold water to obtain gum, depends to some extent on the method of extraction. which appeared to consist of 50% cellulose solubilized The term "mucilage' describes a viscous gum of plant by acidic polysaccharides. These polysaccharides in origin, forming a viscous aqueous solution. Mucilage cluded as components galacturonic acid, rhamnose, may either refer to gum present in the seed or gum galactose, arabinose, and xylose. extracted from the seed, which varies with extraction 15 Weber et al. J. Food Sci. (1974) 39, 461 defatted method. In this application the word gum is used in yellow mustard seed hulls with a hexanye-ethanol preference to mucilage. water mixture, then extracted the dried defatted residue Mustard has two major commercial species, namely with water at an undefined temperature. The extracted Brassica juncea (varieties Canadian brown, Stoke and gum was precipitated by ethanol addition, in 15 to 25% oriental mustard) and Sinapic alba, also referred to as 20 yield, freeze dried and tested for rheological properties. Brassica hirta, or Brassica alba (varieties white and yel The composition suggested by Bailey (above) was con low mustard). firmed as an acidic polysaccharide comprising about 50% cellulose, 10 to 18% uronic acids, mainly galact BACKGROUND AND PRIOR ART uronic acid, including as well arabinose, xylose, and The Cruciferae family of plants includes several in 25 glucose in 5:2:1 ratio, two unidentified saccharides were dustrial oilseed crops. Oilseeds typically comprise an also present. This gum was shown to be a hydrocolloid inner kernel, an outer hull, shell or husk, and a coating, of thixotropic properties, comparable to guar, traga gum is found in the hull and coating. Yellow mustard is canth, carrageen and karaya gums. one such variety, although more commonly used as a Vose Cereal Chem. (1974) 51, 659 defatted hulls condiment than an oilseed. Yellow mustard seed con 30 from mustard and rape (canola) species, followed by tains glucosinolates which have thioglucoside groups, sequential extraction obtaining 22.6% gum with cold these are toxins, which regarded rendering the seed water, and a further 1.1% with hot water from yellow unfit for consumption, especially human. The presence mustard seed, compared to 2.2 to 3.7% with cold water of these thioglucoside groups presents problems in re and a further 0.6 to 2.2% with hot water from brown fining oil. Glucosinolates are both water and oil soluble. 35 mustard (Brassica juncea species), and 0.9 to 1.2% with Gum present in some of these oilseed crops also pro cold water, and a further 1.0 to 1.3% with hot water duces storage and extraction problems in the oilseed from rapeseed (Brassica campestris, Brassica napus). Hy industry. drolysis of the cold water gums showed that the brown mustard and rape gums were similar with arabinose (40 PRIOR ART YELLOW MUSTARD GUM to 50%), xylose (18 to 25%), glucose (10 to 14%), EXTRACTIONS uronic acids (6 to 12%), with traces of fructose, galac Yellow mustard seed has been extracted in various tose, and rhamnose. Yellow mustard gum was about ways on a laboratory scale, to analyze and identify the 35% hydrolyzable (1M sulfuric acid at reflux for 4 gum and its components. The results are not consistent. hours), the residue being cellulose, the hydrolyzable Bailey et al. Biochem. J. (1932) 26, 1609) and Bailey 45 portion was galacturonic acid (30%), arabinose (20%), Biochem. J. (1935) 29, 2477), extracted whole seed glucose (20%), xylose (6%), fructose (6%), rhamnose with cold water to obtain 2% gum, which was identi (6%). The hot water gums were similar. The viscosity fied as including cellulose, and two acidic polysaccha of yellow mustard gum was much greater than those of rides, each containing galactose, galacturonic acid and brown mustard and rape, as was those of slurries pre arabinose. 50 pared by milling whole hulls. Hirst et al. Biochem. J. (1965) 95, 453 extracted Theander et al. J. Agri. Food Chem. (1977) 25, 270 yellow mustard seed hulls and kernels separately using extracted hulls of white mustard seed (similar to yellow a sequential extraction scheme. Hull extraction gave mustard) with 80% ethanol to give chloroform and 6.4% with cold water, boiling water then gave a further water soluble fractions, the water soluble fraction was 8.6%. The cold water hull fraction polysaccharides 55 further split into acidic, neutral, and basic fractions. The after hydrolysis contained in rough order of concentra neutral unhydrolyzed water soluble fraction consisted tion galactose, arabinose, and galacturonic acid, as mainly of sucrose, stachyose and fructose. The ex major components and xylose, glucose and mannose as tracted hulls were further extracted with benzene minor components. The hot water hull fraction polysac ethanol, to give polysaccharides, which were then hy charides after hydrolysis contained in rough order of 60 drolyzed (12M sulfuric acid room temperature for 2 concentration arabinose, galactose, and galacturonic hours, then 0.358M sulfuric acid under reflux for 6 acid, as major components and xylose, rhamnose, glu hours) and analyzed shown to consist of glucose 39.3%, cose and mannose as minor components. Kernel extrac arabinose 25.4%, galactose 17.9%, xylose 7.0%, man tion gave 2.4% with cold water, boiling water gave a nose 5.4%, rhamnose 4.0%, fucose 1.0%, the uronic further 3.4%. The cold water kernel fraction polysac 65 acids present were not identified, nor was their content charides after hydrolysis contained in rough order of measured. concentration arabinose, and glucose as major compo Woods et al. Can. J. Plant Sci. (1980) 60, 1031) ex nents and xylose, galactose, and galacturonic acid as tracted dried whole yellow mustard seed with water 4,980, 186 3 4. - containing 0.25% volume chloroform, obtaining be respectively. Although this process is useful, and pro tween 0.8 to 2% of gum, after precipitation with acidi vides a useful product it is not easily adapted to indus fied acetone. trial scale extraction, because of the long extraction Siddiquiet al. Food Microstruct. (1986) 5, 157 stud time, and high seed:water ratio. Desirably an industrial ied the surface of yellow mustard seeds using optical process has as short extraction time and as low a seed:- and electron micrographs, at the same time extracting water ratio as possible. the seeds. The hulls were extracted with boiling water In an especially convenient version, the second step for 35 min, then the filtered extract was precipitated comprises mechanically separating the seed and the with isopropanol to give one gum. Another was ob water, preferably by centrifuging in a perforated centri tained by rubbing moistened whole seed, dissolving the 10 fuge, which can also be a screened or slitted centrifuge. product in water and precipitating with isopropanol. A slitted centrifuge is especially preferred, as the seed is Hydrolysis of the polysaccharides of these gums less likely to plug the slits. The first step preferably showed they comprised in component molar order ga comprises treating the seed at an elevated temperature, lactose, glucose, arabinose and mannose (roughly equal preferably at least about 550' C., which may be carried mole ratio), rhamnose and xylose, extracted gum con 15 out at a seed:water ratio of about 1:2, preferably for tained about 30% uronic acid, compared to 18% for about 10 minutes. Alternatively the elevated tempera rubbed gum. The gums were concluded to include pec ture may be 100 C., the seed:water ratio about 1:3, and tic polysaccharides. Differences in galactose:glucose the seed may be treated for about 2.5 minutes. The first ratios (depending on the acid concentration in the hy step may be applied in a microwave oven, at a seed:wa drolysis) were attributed to the presence of a xyloglu 20 ter ratio of about 1:2, the temperature is raised from can (amyloid). room temperature to about 85 C., in about 3 minutes. Reported gum yield varies depending on variety and The first step may also take place at about 25 C., at a location. The differences in gum extraction results are seed:water ratio of about 1:2, preferably for about 30 attributable to differential extraction of seed hull com minutes. In this version an additional third step may ponents, and varietal differences. However to date no 25 comprise treating the resulting separated water extract industrial process for mustard gum extraction has been at an elevated temperature. The first and second steps reported. are preferably repeated, for example when the tempera ture is at least about 55' C., the first and second steps are DESCRIPTION OF THE INVENTION preferably repeated four times and the resulting water The object of the invention is to provide an improved 30 extracts combined. When the temperature is 100° C. process of extraction of yellow mustard seeds (some they are preferably repeated twice and the resulting yellow mustard seed may be called white mustard seed, water extracts combined. When the treatment is carried as there is no absolute distinction). out in a microwave oven they are preferably repeated Applicant has discovered a novel process of extrac three times and the resulting water extracts combined. tion which gives a high viscosity nearly ideal pseudo 35 When the treatment is at room temperature (25 C.) the plastic gum. This process is time-temperature interde treatment may be repeated ten times, 10 minutes each. pendent. The centrifuges considered appropriate for use in the The invention in one broad aspect comprises an im process of the invention are selected from those centri provement in a process of water extraction of gum from fuges having perforated bowls, which may be perfo dried yellow mustard seed, the improvement compris rated, slitted, or screened. As would be understood by ing treating the mustard seed with water in at least a those skilled in the art many such conventional centri first step, and separating the resulting water extract fuges may be appropriately used in the process of the from the seed in a second step. Applicant has found that invention. Also as would be understood by those skilled mechanical separation, preferably by centrifugation, is in the art, equivalent conventional mechanical devices advisable for an industrial process. 45 may be used in the process of the invention. Preferably in one variation the first step comprising The results demonstrate that extraction could be sat initially treating the mustard seed with water at ele isfactorily carried out in the range 55 C. to 100 C. with vated temperature, then extracting the whole seed with numerous seed: water ratios. The short extraction time water cooled to room temperature. The first step may and low seed: water ratio is preferred in industrial appli comprise initially treating the mustard seed at about 50 cation. The experiments also confirm that the extraction 100 C. for about 5 minutes at a seed:water ratio of can be successfully carried out over the entire range of about 1:2.5, and the extraction takes place at room tem 55 C. to 100 C., and that extraction at other tempera perature at a seed:water ratio of about 1:7. More prefer tures is feasible. ably the mustard seed is treated at about 75 C. for about These treatments generated several gums, elevated 25 minutes at a seed:water ratio of about 1:2.5, after 55 temperature gums TC55, TC65, TC85, microwave treatment at about 100° C. Optionally the process may oven gun MT85, high temperature gum TC100, low include the additional step of treating the dried yellow temperature gum TC25, and heat treated low tempera mustard seed with steam, before treating the seed at ture gum TC25+H, all in approximately 4% yield, with elevated temperature with water. extraction times ranging from 5 to 130 minutes. TC25, The gum can be precipitated from the water portion TC65, MT85 were tested and found to have pseudoplas by any water miscible alcohol, for example isopropanol tic properties, the higher temperature extracts being or ethanol. more viscous, more pseudoplastic and having less hyste Four gums F1, F2, F3 and F4 were successively resis. The gums obtained by high temperature extrac isolated in yields of 2.25%, 0.75%, 0.54%, 0.45% re tion process were very viscous and comparable to xan spectively for a total of 3.99%, overall, which is approx 65 than gum, while the cold extracted guns were lower in imately twice that obtained previously from whole seed viscosity, as shown in Tables II to IX. extraction. The four fractions were obtained after con In another broad aspect the invention is a yellow secutive extraction periods of 16, 7, 17 and 24 hours mustard seed gum, preferably highly viscous, having 4,980, 186 5 6 pseudoplastic properties. "Pseudoplastic' is defined in TABLE I this application as having shearthinning properties, that YELLOW MUSTAR GUM COMPOSITIONS is, as the shear rate increases the viscosity drops and the (Sugars are weight % of total identified sugars liquid thins. This is unusual in natural and other guns, except PA which is molar %) over the broad range of shear rate. The only yellow Constituent F1 F2 F3 F4 PA mustard gum for which shear rate properties were mea Xylose 3.03 3.24 3.38 3.67 3.75 sured was that extracted by Weber et al. (op. cit.) from Rhamnose 3.85 3.67 3.38 3.52 6.0 the hulls, which was shown to have thixotropic proper Arabinose 7.02 6.91 5.28 5.27 11.71 ties, which are distinct from the pseudoplastic proper Mannose 0.59 10.72 0.43 10.54 1.24 O Galactose 33.29 32.29 32.16 31.47 37.24 ties shown by the gums of this application. The seven Glucose 42.23 43.16 45.37 45.53 29.98 tested gums, all exhibit nearly ideal viscosity/shear rate Protein 8.40 7,10 7.20 9.10 6,0 relationships expected for an ideal pseudoplastic mate Yield 26 2.25 0.75 0.54 0.45 rial. The utility of such a pseudoplastic material is wide spread as a viscosity changing additive, especially in Four other unidentified sugars were noted as present food and pharmaceuticals. The currently used additive 15 in minor amounts. is xanthan gum, a biosynthetically prepared polysaccha Tables II to IX present viscosity measurements for ride, which is widely used for viscosity effects. The mustard gums extracted under specific extraction con gums of this invention would be superior, as they are ditions together with those of xanthan gum for compari already known to be used in foods and condiments, son. These tables show mustard gum is very viscous and since the dawn of civilization, and probably substan 20 comparable to xanthan gum. tially earlier. FIGS. 1 to 4 show log plots of viscosity vs shear rate The gum may be in clear white dry fibrous form. The for gums F1, F2, F3, and F4. Although not identical, all gum includes a polysaccharide, having monosaccharide clearly demonstrate nearly ideal pseudoplastic behav components, which comprise in order of decreasing ior, exhibiting similar viscosity-shear rate relation concentration glucose, galactose, mannose, arabinose, 25 ships. These figures show that yellow mustard gums are with rhamnose and xylose approximately equal in con highly viscous, which has never been reported before. centration but less than arabinose. The rhamnose may FIGS. 5 to 8 show log plots of viscosity vs shear rate be greater in concentration than the xylose, or the xy (X) and shear stress vs shear rate (O) for gums TC25, lose may be greater in concentration than the rhamnose, TC65, MT85 and xanthan gum. Although not identical, they also can be equal in concentration. The polysac 30 all clearly demonstrate nearly ideal pseudoplastic be charide may have a monosaccharide composition by havior, exhibiting similar viscosity-shear rate relation weight of xylose 3.03 to 3.67%, rhamnose 3.38 to ships. TC65 and MT85, the heat treated extracts, exhibit 3.85%, arabinose 5.27 to 7.02%, mannose 10.43 to nearly ideal pseudoplastic behavior comparable to that 10.72%, galactose 31.47 to 33.29%, glucose 42.23 to 35 of xanthan gum, with virtually minimal hysteresis. By 45.53%. comparison TC25, the cold extract, is of lower viscos In a further aspect the invention is directed to the ity, and exhibits more hysteresis. MT85, the microwave water extracted, yellow mustard seed, having a Sweet extract, shows higher viscosity and less hysteresis than pleasant taste. Heat extracted seed was found to have a TC65. sweet pleasant taste, while cold extracted seed had an The figures indicate that all mustard gum samples associated bitter taste, presumably caused by natural have shear thinning properties and nearly ideal pseudo toxins present. plastic behavior. It is tendered as a non binding hypothesis by appli Heat extracted seed was found to have a Sweet pleas cant that the glucose represents the cellulosic backbone ant taste, while cold extracted seed has an associated of the polysaccharide, while the residual components 45 bitter taste, presumably caused by natural toxins pres represent polysaccharide chains grafted to the back ent. bone, oligosaccharides grafted to the cellulose back bone, and possibly polysaccharides, oligosaccharides, EXPERIMENTAL DETAILS and monosaccharides adsorbed onto the polysaccha Throughout, the term "seed" refers to whole seed. ride, it is also possible that the polysaccharide was syn 50 Experiment 1: Extraction of Gum thesized in some way by the heat treatment from smaller units to form an elongated polysaccharide. First Extraction DESCRIPTION OF PREFERRED 250 ml of boiled distilled water, at 100° C., was added EMBODIMENTS to 100 g of dried yellow mustard seed in a flask, and the 55 container maintained at 100 C. for 5 min. The container Properties of preferred embodiments are indicated in was cooled to 75 C., and was maintained at this temper the drawings where: ature for 25 min. The container was then cooled to 25 FIGS. 1 to 4 show plots of viscosity vs shear rate for C. and 450 ml of cold (room temperature) distilled gums F1, F2, F3, and F4, respectively. water was added to adjust the seed:water ratio to 1:7.2 FIGS. 5 to 8 show plots of viscosity vs shear rate (X) ml of chloroform was added to prevent microbial fer and shear stress vs shear rate (O) for gums TC25, TC65, mentation. The seed was then stirred in the water using MT85, and xanthan gum (prior art), respectively. a magnetic stirrer for 16 hours at room temperature. The general description of the invention is now ex The viscous aqueous liquid containing the extracted panded by reference to the experimental results, which material was then strained through a strainer, to sepa illustrate preferred embodiments of the invention. 65 rate the gum from the seed to yield about 500 ml of In Table I, the chemical properties of the extracted viscous aqueous liquid. The dried seed tends to absorb gums (F1, F2, F3, F4) are given together with that of at least its own weight of water during the process. The Siddiqui et al., (PA - prior art). aqueous extract was then treated by addition of 4 vol 4,980, 186 7 8 umes of 95% ethanol (21), and stirred with a glass rod precipitate was then filtered, pressed and dissolved in 50 to recover the gum in a cotton like mass which easily ml water and reprecipitated by 200 ml ethanol to give a separates from the soluble matter. In this process the second precipitate. This second precipitate was then precipitated gummy material aligns in the direction of filtered, pressed and dissolved in 50 ml water and re shear to produce a cottony form of the gun. After 5 precipitated by 200 ml ethanol to give a third precipi separation of the gum from the liquid, the cottonlike tate. The third precipitate, was filtered and pressed, and fibrous appearing mass, was pressed to remove solvent. The gum was then dissolved in 50 ml of water and was then washed with acetone to remove any water reprecipitated by 200 ml of ethanol. This precipitate present in the gum. The acetone washed product was was then filtered, pressed and dissolved in 50 ml water O then vacuum dried to give 0.54 g of product (fraction 3 and reprecipitated by 200 ml ethanol to give a second Ot precipitate, in the same way as discussed above. This Fourth Extraction second precipitate was then filtered, pressed and dis solved in 50 ml water and reprecipitated by 200 ml The strained residual yellow mustard seed was placed ethanol to give a third precipitate. This third precipi 15 in a flask with 500 ml of cold (room temperature) dis tate, was filtered and pressed, and was then washed tilled water and 2 ml of chloroform. The seed was then with acetone to remove any water present in the gum. stirred in the water using a magnetic stirrer for 24 hours The acetone washed product was then vacuum dried to at room temperature. The water containing the ex give 2.25 g of product (fraction 1 or F1). tracted material was then strained through a strainer, to remove the gum from the seed to yield about 500 ml of Second Extraction viscous aqueous liquid. This acqueous extract was then The strained residual yellow mustard seed from the treated by addition of 4 volumes of 95% ethanol (21), first extraction was placed in a flask with 500 ml of cold and stirred with a glass rod to recover the gum in a (room temperature) distilled water and 2 ml of chloro cotton like mass which easily separates from the soluble form. The seed was then stirred in the water using a 25 magnetic stirrer for 7 hours at room temperature. The matter. In this process the precipitated gummy material water containing the extracted material was then aligns in the direction of shear to produce a cottony strained through a strainer, to remove the gum from the form of the gum. After separation of the gum from the seed to yield about 500 ml of viscous aqueous liquid. liquid, the cottonlike fibrous appearing mass, was This aqueous extract was then treated by addition of 4 30 pressed to remove solvent. The gum was then dissolved volumes of 95% ethanol (21), and stirred with a glass in 50 ml of water and reprecipitated by 200 ml of etha rod to recover the gum in a cotton like mass which nol. The precipitate was then filtered, pressed and dis easily separates from the soluble matter. In this process solved in 50 ml water and reprecipitated by 200 ml the precipitated gummy material aligns in the direction ethanol to give a second precipitate. This second pre of shear to produce a cottony form of the gum. After 35 cipitate was then filtered, pressed and dissolved in 50 ml separation of the gum from the liquid, the cottonlike water and reprecipitated by 200 ml ethanol to give a fibrous appearing mass, was pressed to remove solvent. third precipitate. The third precipitate, was filtered and The gum was then dissolved in 50 ml of water and pressed, and was then washed with acetone to remove reprecipitated by 200 ml of ethanol This precipitate was any water present in the gum. The acetone washed then filtered, pressed and dissolved in 50 ml water and reprecipitated by 200 ml ethanol to give a second pre product was then vacuum dried to give 0.45 g of prod cipitate. This second precipitate was then filtered, uct (fraction 4 or F4). pressed and dissolved in 50 ml water and reprecipitated In this experiment each aqueous extract, was replaced by 200 ml ethanol to give a third precipitate. This third with an equal volume of water to maintain the water:- precipitate, was filtered and pressed, and was then 45 dried seed ratio at approximately 7:1. washed with acetone to remove any water present in Experiment 2: Alternative Extraction of Gum the gum. The acetone washed product was then vac uum dried to give 0.75 g of product (fraction 2 or F2). The identical procedure to experiment 1, first extrac tion step was followed with the additional step of first Third Extraction 50 preheating the seeds with steam for 10 minutes, before The strained residual yellow mustard seed from the adding the boiling water, a gum was obtained in practi second extraction was placed in a flask with 500 ml of cally identical yield to that of experiment 1, first extrac cold (room temperature) distilled water and 2 ml of tion step. chloroform. The seed was then stirred in the water In the following experiments, the centrifuge was a using a magnetic stirrer for 17 hours at room tempera 55 Braun Juice Extractor KMZ3 (either the KM32/321 or ture. The water containing the extracted material was MX 32 version is suitable). The strainer, or basket, is a then strained through a strainer, to remove the gum corrugated cylinder with vertical slits at the outer api from the seed to yield about 500 ml of viscous aqueous ces of the corrugations, this arrangement does not allow liquid. This aqueous extract was then treated by addi tion of 4 volumes of 95% ethanol (21), and stirred with seed to plug the slits, and separation of the viscous a glass rod to recover the gum in a cotton Iike mass extract presents no difficulty. As would be appreciated which easily separates from the soluble matter. In this by those skilled in the art, any centrifuge adapted for process the precipitated gummy material aligns in the juice extraction, with a perforated, or slitted bowl, or direction of shear to produce a cottony form of the equivalent strainer element would be suitable for use in gum. After separation of the gum from the liquid, the 65 the process of the invention. Equivalent conventional cottonlike fibrous appearing mass, was pressed to re mechanical strainers, as would be appreciated by those move solvent. The gum was then dissolved in 50 ml of skilled in the art, can be substituted for the centrifuges water and reprecipitated by 200 ml of ethanol. This noted above. 4,980, 186 9 10 Experiment 3: Mechanical Industrial Extraction of Experiment 8: Mechanical Industrial Extraction of Gum using a Perforated Centrifuge Gum using a Perforated Centrifuge 200 g of distilled water at 65° C., was added to 100 g 200 g of distilled water, at 25 C., was added to 100 g of dried yellow mustard seed in a flask, this was 10' C. 5 of dried yellow mustard seed in a flask, and maintained higher than the extraction temperature, which resulted at 25 C. for 30 min, with occasional hand shaking. The in fast equilibrium of the seed-water mixture at 55° C. mixture was then passed through a perforated centrie The temperature was maintained at 55 C. for 10 min., fuge and about 100 ml of thick gummy solution sepa with occasional hand shaking. The mixture was then rated from the seed, which remained in the centrifuge passed through a perforated centrifuge and about 100 10 basket. The seed was replaced in the container 100 g of distilled water at 25 C. was added, and maintained at ml of thick gummy solution separated from the seed, 25 C. for 10 min., with occasional hand shaking, the which remained in the centrifuge basket. The seed was mixture was separated as described previously. The replaced in the container, 100 g of distilled water at 65 seed was extracted a further nine times with 100g water C. was added, allowed to equilibrate to 55 C., and 15 at 25 C. for 10 min, each time. The collected extracts maintained at 55' C. for 10 min., with occasional hand were then combined, filtered through a synthetic filter shaking, the mixture was separated as described previ to remove any solid contaminants. The gum was precip ously. The seed was extracted a third and fourth time as itated by addition of 4 volumes of 85% ethanol, washed described previously. The collected extracts were then and dried in an oven at 75 C., to yield 4.1 g of gum combined, filtered through a synthetic filter to remove 20 (TC25). any solid contaminants. The gum was precipitated by In this experiment each extract was replaced with an addition of 4 volumes of 85% ethanol, washed and dried equal volume of water to maintain the water:dried seed in an oven at 75° C., to yield 4.25 g of gum (TC55). ratio at approximately 2:1. In this experiment each extract was replaced with an equal volume of water to maintain the water:dried seed 25 Experiment 9: Mechanical Industrial Extraction of ratio at approximately 2:1. Gum using a Perforated Centrifuge In experiments 4 to 6, the extraction water had an The method of experiment 8 was repeated, the com initial temperature 10° C. greater than the extraction bined extracts, were then heated at 65 C. for 30 min., temperature to allow for fast equibrilation of the seed before precipitating the gum by addition of 4 volumes water mixture at the extraction temperature. 30 of 85% ethanol, washed and dried in an oven at 75 C., to yield 4.1 g of gum (TC25--H). Experiment 4: Mechanical Industrial Extraction of Gum using a Perforated Centrifuge Experiment 10: Mechanical Industrial Extraction of Gm using a Perforated Centrifuge The method of experiment 3 was repeated at 65 C., to yield 4.0 g of gum (TC65). 35 200 g of distilled water, at 25 C., was added to 100 g of dried yellow mustard seed in a container, and heated Experiment 5: Mechanical Industrial Extraction of in a microwave oven for 3 min. attaining a temperature Gum using a Perforated Centrifuge of 85 C. The mixture was then passed through a perfo rated centrifuge and about 100 ml of thick gummy solu The method of experiment 8 was repeated at 75 C., tion separated from the seed, which remained in the to yield 4.2 g of gum (TC75). centrifuge basket. The seed was replaced in the con Experiment 6: Mechanical Industrial Extraction of tainer 100 g of distilled water at 25°C. was added, and Gum using a Perforated Centrifuge the container replaced in the microwave oven, and heated for 3 min. The mixture was again separated as The method of experiment 3 was repeated at 85°C., 45 described previously. The seed was extracted a third to yield 4.0 g of gum (TC85). time as described previously. The collected extracts Experiment 7: Mechanical Industrial Extraction of were then combined, filtered through a synthetic filter Gum using a Perforated Centrifuge to remove any solid contaminants. The gum was precip itated by addition of 4 volumes of 85% ethanol:15% 300 g of distilled water, at 100° C., was added to 100 50 methanol, washed and dried in an oven at 75 C., to g of dried yellow mustard seed in a flask, and main yield 4.0 g of gum (MT85). tained at 100° C. for 2.5 min. The mixture was then In this experiment each extract was replaced with an passed through a perforated centrifuge and about 200 equal volume of water to maintain the water:dried seed ml of thick gummy solution separated from the seed, ratio at approximately 2:1. which remained in the centrifuge basket. The seed was 55 replaced in the container 200 g of distilled water at 100 CHEMICAL ANALYSIS OF GUMS C. was added, and maintained at 100 C. for 2.5 min., Protein Analysis of F1, F2, F3, F4 with occasional hand shaking, the mixture was sepa Each extract was analyzed for protein using the rated as described previously. The collected extracts method of Lowry et al. (J. Biol. Chem. (1951) 193,265). were then combined, filtered through a synthetic filter to remove any solid contaminants. The gum was precip Monosaccharide Hydrolysis of F1, F2, F8, F4, itated by addition of 4 volumes of 85% ethanol, washed The extracts were hydrolyzed to monosaccharides and dried in an oven at 75 C., to yield 4.0 g of gum using a modified version of Saeman et al. TAPPI (TC100). 65 (1954) 37, 336). The gum fractions F1, F2, F3, F4, 5 to In this experiment each extract was replaced with an 10 mg each, were hydrolyzed by aqueous 72% sulfuric equal volume of water to maintain the water:dried seed acid (0.2 ml) under nitrogen gas in a closed test tube for ratio at approximately 3:1. 1 hour at room temperature, the acid was diluted to 1M 4,980, 186 11 12 then heated at 100 C., on a water bath for 2 hours under temperature of 200° C. for 25 min, followed by 210 C. nitrogen gas. The hydrolyzate was then neutralized for 15 min, with a ramp temperature of 10 C./min, was with finely powdered CaO using the exact amount re established for peak separation. Peak areas were deter quired to neutralize the sulfuric acid, and pH measure mined by HP computing integrator. The flow rate of ments were taken to allow complete neutralization of 5 the carrier gas was regulated at 1 ml/min by use of a the hydrolyzate. A calcium sulfate milky suspension 100/1 splitter. The eluate was continuously mixed with was produced. The test tube was then vibrated to mix the scavenger gas (nitrogen) 138 ml/min and the mix the contents thoroughly, and the test tube centrifuged. ture was introduced into the detector. The top liquid layer was removed, 2 ml of water was VISCOSITY MEASUREMENTS OF GUMS added to the test tube, which was then vibrated again, 10 centrifuged again, and the top liquid layer removed. Shear sweep, and viscosity of solutions of the gums This process was repeated four times. The combined F1, F2, F3, F4, TC25, TC65, MT85 and xanthan gum liquid layers of sugar solutions were collected in a ro were measured at various concentrations in water using tary vacuum drier, and concentrated with the addition a Bohlin Rheometer System. of ethanol as a water evaporation aid. The concentrated 15 The data in Tables II to V was used to plot FIGS. 1 sugars were collected and 0.5 ml placed in a double to 4, and was taken at 25 C., and 0.5% concentration chamber test tube for freeze drying. with a Bohlin Rheometer System, with torque element 93.2 g-cm, initial delay time 2 seconds, constant delay Methylation of Monosaccharide Mixtures time 5 seconds, sensitivity lix, integration time 2 sec The freeze dried sugars were methylated following 20 onds, and measurement interval 82 seconds. Exponen the method of Honda et al. J. Chromatography, (1979) tial figures are used, e.g. 3.682E-2 is 0.03682. The varia 169, 287), 20 ul ethanethiol-trifluoroacetic acid (2:1, tion in shear rate is the same in all tables and is increased v/v) was added to the residue in a reaction tube, which to a maximum and then decreased. was then closed tightly with polyethylene stopper and The data in Tables VI to IX was used to plot FIGS. kept for 10 min at 25 C. Pyridine (50 ul), hexame 25 5 to 8, and was taken at 25 C., and 0.3% concentration thylenedisilazane (100 ul), and trimethylchlorosilane (50 in a Bohlin Rheometer System, with torque element ul), and the mixture incubated for 30 min at 50 C., with 91.4g-cm, initial delay time 2 seconds, constant delay occasional shaking. The mixture was then centrifuged, time 5 seconds. sensitivity lix, integration time 10 sec and 1 ul of the supernatant analyzed by gas liquid chro onds, and measurement interval 100 seconds. Exponen matography. A mixture of standard sugars were treated 30 tial figures are used. The variation in shear rate is the in the identical manner, as a standard. same in all tables and is increased to a maximum and then decreased. Gas Liquid Chromatography of Methylated Heat extracted seed was found to have a sweet pleas Monosaccharide Mixtures ant taste, while cold extracted seed had an associated The gas liquid chromatography of the methylated 35 bitter taste, presumably caused by natural toxins pres monosaccharide mixtures was performed with a Sigma et. column (0.314 mm I.D., 30 m long, SM30). An initial TABLE II MUSTARD GUM F1 VISCOSITY DATA SHEAR SHEAR RATE STRESS VISCOSITY l/s Pa Pas 3.682E-2 1.661E- 4.5E-0 5,833E-2 7.023E-1 i.204E-4- 9.246E-2 1.210E-10 309E-0 1.465E-1 1.125E-0 7.679E-0 2.326E-1 1.172E--0 5.04E--0 3.686E-1 1.217E--0 3.302E--0 5.833E-1 1.288E--0 2.208E -- 0 9.232E- 1.428E--0 1.547E-O 1,467E--0 1479E-0 1008E--0 2.322E--0 .544E--0 6.650E. 3.682E-0 .559E--0 4234E 5.833E--0 1868E--0 3.202E-1 9.246E--0 2.05E-0 2.218E-1 1.465E-1 2.138E--0 1.459E-1 2.326E-1 2.461E--0 1.058E-1 3.686E-1 2.828E--0 7.672E-2 5.833E-1 3.289E-0 5.638E-2 9.232E-- 1 3.921E--0 4,247E-2 1.467E-2 4.677E-0 3.188E-2 2.322E-2 5.875E-0 2.530E-2 3.682E--2 7.714E-O 2.095E-2 5.833E-2 1.044E- 1789E-2 9.246E--2 1.452E-1-1 57OE-2 5.833E-2 1.023E-1-1 i.754E-2 3.682E-2 7.419E--0 2.015E-2 2.322E-2 5.626E--0 2.423E-2 1.467E-2 4.508E--0 3.073E-2 9,232E-1 3.739E-0 4.050E-2 5.833E-1 3.186E--0 5.462E-2 3.686E-- 2.590E--0 7.029E.2 2.326E-- 2.258E--0 9.709E-2 1.465E-- 2.121E--0 .448E-1

4,980, 186 17 18 3. The process of claim 2, wherein (a) comprises TABLE VIII-continued treating said seed in seed-water mixture at a seed water MUSTARD GUMMT85 VISCOSITY DATA ratio of about 1:2 5, for about 5 minutes, then subse SHEAR SHEAR quently (d) cooling said seed-water mixture to a temper RATE STRESS VISCOSITY ature of about 75 C., and maintaining said seed-water 1/s Pa. Pas mixture at 75 C., for about 25 minutes, then (e) increas 7.335E-1 1.441E--0 1.964E-2 4.616E-- 1.55E--0 2.50E-2 ing said seed:water ratio to about 1:7, cooling said seed 2.934E-1 9.525E- 3.246E-2 water mixture to about 25 C., and maintaining said 1.86E-1 7.987E-1 4.293E-2 seed-water mixture at about 25 C. for about 16 hours. 1.164E-1 7.346E-1 6.31 E-2 O 4. The process of claim 2, additionally comprising 7.343EO 6.344E- 8.640E-2 treating said seed with steam before step (a). 4.634E--0 5.364E-1 1.158E 2.923E--0 4.795E-1 1.640E-1 5. The process of claim 4, wherein said seed is treated 1.846E--0 4.140E-1 2.242E-1 with steam for about 10 minutes. 1.163E--0 3.822E-i 3.286E-1 6. The process of claim 1, wherein (b) comprises 7.335E-1 3.347E-1 4.562E-1 5 mechanically separating said water extract from said seed, in a perforated centrifuge. 7. The process of claim 6, wherein said temperature is TABLE IX about 55 C. XANTHAN GUM WISCOSITY DATA 8. The process of claim 6, wherein said temperature is SHEAR SHEAR 20 about 65 C. RATE STRESS VISCOSITY 9. The process of claim 6, wherein said temperature is 1/s Pa Pas about 75 C. 7.335E-1 1.432E--0 1952-0 10. The process of claim 6, wherein said temperature 1.163E--0 1.612E--0 1.386E-0 is about 85 C. 1.846E--0 1.820E--0 9.858E-1 25 2.923E--0 2.020E--0 6.909E-1 11. The process of claim 6, wherein (a) comprises 4.634E--0 2.249E--0 4.854E-1 treating said seed at a temperature in the range of from 7.343E--0 2.50OE-0 3.404E-1 about 55 C. to about 85 C., at a seed:water ratio of " 1.164E-1 2.773E--0 2.382E-1 about 1:2, for about 10 minutes, 1.861E-1 3.029E-0 1.628E-1 12. The process of claim 6, wherein said temperature 2.934E-1 3.346E--0 1.140E-1 4.616E-1 3.749E-0 8.122E-2 30 is about 100° C. 7.335E-1 4.218E--0 5.750E-2 13. The process of claim 12, wherein (a) comprises 1.63E-2 4.820E--0 4.45E-2 treating said seed at a seed:water ratio of about 1:3, for 1.846E-2 5.606E--0 3.062E-2 about 2.5 minutes. 2.923E-2 6.663E--0 2.279E-2 14. The process of claim 6, wherein (a) comprises 4.634E-2 8,063E--0 1.740E-2 7.343E-2 1.00E-1 .363E-2 35 treating said seed and water with microwaves. 1.164E-3 1.265E-0 1.086E-2 15. The process of claim 14, wherein (a) comprises 7.343E-2 1.001E--0 1.363E-2 treating said seed and water at a seed:water ratio of 4.634E--2 8.084E--0 1.745E-2 about 1:2, for about 3 minutes as the temperature is 2.923E-2 6.667E--0 2.281E-2 1.846E-2 5.638E--0 3.053E-2 raised to about 85. C., 1.163E-2 4.862E--0 4.181E-2 16. In a process of water extraction of gum from dried 7.335E-1 4.250E--0 5.792E-2 yellow mustard seed, including the steps of 4.616E-1 3.771E--0 8.170E-2 (a) treating said mustard seed with water 2.934E-- 3.383E--0 53E-1 (b) separating the resulting water extract from said 1.861E-1 3.057E--0 1.64.3E-1 1.164E-- 1 2.819E--0 2,422E seed, the improvement comprising 7.343E--0 2.56 E--0 3.488E 45 (c) the resulting water extract being heated at a tem 4.634E--0 2.310E--0 4.984E-1 perature of about 65° C. 2.923E--0 2.069E-0 7.077E-1 17. The process of claim 16, wherein (b) comprises 1.846E--0 1.887E--0 1,022E--0 mechanically separating said water extract from said 1.163E--0 1.675E-0 1.440E--0 seed, in a perforated centrifuge. 7.335E-1 1.505E--0 2.052E--0 18. The process of claim 17, wherein (a) comprises treating said seed at about 25 C., at a seed:water ratio of Although this invention is described in terms of spe about 1:2 for about 30 minutes, wherein and said resul cific embodiments, it is not limited thereto, as would be tant extract is heated at about 65 C. for about 30 min understood by those skilled in the art, numerous varia uteS. tions are possible within the scope of the invention as 55 19. A yellow mustard seed gum, having pseudoplastic described and claimed in the application, without de properties in aqueous solution, wherein said gum in parting from the scope and nature thereof. cludes a polysaccharide, having monosaccharide com I claim: ponents comprising in order of decreasing concentra 1. In a process of water extraction of gum from dried tion glucose, galactose, mannose, arabinose, with rham yellow mustard seed, including the steps of nose and Xylose approximately equal in concentration (a) treating said mustard seed with water but less than arabinose. (b) separating the resulting water extract from said 20. The gum of claim 19, said polysaccharide having seed, the improvement comprising a monosaccharide composition by weight, of xylose (c) said water being at a temperature in the range 3.03 to 3.67%, rhamnose 3.38 to 3.85%, arabinose 5.27 from about 55 C. to about 100 C. 65 to 7.02%, mannose 10.43 to 10.72%, galactose 31.47 to 2. The process of claim 1, wherein said temperature is 33.29%, and glucose 42.23 to 45.53%. about 100 C. k ck k xk sk