PatentDe  


Dokumentenidentifikation EP0319129 30.03.1995
EP-Veröffentlichungsnummer 0319129
Titel Lösliches getrocknetes Cassiagummi und Verfahren zu dessen Herstellung.
Anmelder FMC Corp., Philadelphia, Pa., US
Erfinder Renn, Donald Walter, Glen Cove Maine 04846, US;
Lauterbach, George Ervin, Thomaston Maine 04861, US;
Hemmingsen, Peter, DK-2650 Hvidovre, DK
Vertreter Vossius & Partner, 81675 München
DE-Aktenzeichen 3853138
Vertragsstaaten AT, BE, CH, DE, ES, FR, GB, GR, IT, LI, LU, NL, SE
Sprache des Dokument En
EP-Anmeldetag 04.10.1988
EP-Aktenzeichen 883092405
EP-Offenlegungsdatum 07.06.1989
EP date of grant 22.02.1995
Veröffentlichungstag im Patentblatt 30.03.1995
IPC-Hauptklasse C08L 5/14
IPC-Nebenklasse A23L 1/05   C08L 5/00   

Beschreibung[en]

A homogeneous composition and process is provided for an alloy gum extracted from seeds of the genus Cassia which will form a clear, stable colloidal solution in an aqueous medium.

The demand for natural gums, polysaccharides, used in gelling and thickening compositions, has been increasing worldwide. Many of these natural gums are derived from plants, and as a result both the availability and the properties of these gums are subject to wide variations year-to-year. Recently it has been proposed that the seeds of plants of the genus Cassia could be utilized as a new source of natural galactomannan gums (Farooqi et al., "Seeds of Genus Cassia as Possible Sources of Industrial Gums," Indian Forester, November 1978, pages 729-732).

U. S. Patent No. 4,661,475 discloses that galactomannan gums are useful substances which are added to an aqueous medium in order to achieve the desired consistency or viscosity. Like virtually all natural gelling agents and thickeners with the exception of gelatin, galactomannan gums are derivatives of polysaccharides, that is, high-polymeric carbohydrates.

Polysaccharides are water-soluble or strongly swellable substances, and include compounds which in aqueous systems give colloidal, more or less highly viscous solutions or dispersions having plastic or pseudo-plastic flow and having functional properties such as a thickening action, water-binding capacity, stabilization of suspensions and emulsions in polyphase systems, and gel formation.

Galactomannans, like the starches, are vegetable reserve polysaccharides. They occur in the endosperm cells of numerous seeds of legumes. The collective term "galactomannan" or "polygalactomannan" comprises all polysaccharides which are built up of galactose and/or mannose residues and in addition can also contain minor amounts of other sugar residues. There is a relatively large number of galactomannans, which vary in composition depending on their origin. The materials principally occur in the endosperm portions of legumes such as guar, locust bean, tara, honey bean, flame tree and sesbania. Galactomannans are built up of a linear mannose chain which itself is built up of mannopyranose rings linked by β-(1,4)-glucoside bonds. To these rings are attached, as branches, isolated galactopyranose residues by α-(1,6)-glucoside bonds. Galactomannan gums when dried and ground to a powder are well known to be particularly difficult to disperse into an aqueous solution and instead clump together, according to U.S. Patent No. 3,8&sl0;8,195.

In particular, locust bean gum, guar gum and tara gum have been the principal galactomannan gums of commerce. Cassia species contain potentially useful endosperm galactomannans analogous to locust bean gum, tara gum, and guar gum. Cassia gum, like locust bean gum, exhibits gel strength synergy with carrageenan, xanthan, and agar according to U.S. Patent 4,661,475. However, it has been found that unlike other galactomannan gums, the Cassia gum when dried to a solid fails to redissolve completely in water. When the solid is dispersed in water and heated, a portion will redissolve, but a substantial part will only imbibe water and swell. The mixtures may sometimes appear to be clear solutions until examined closely, and on standing the solutions become cloudy.

Cassia gum can be extracted from Cassia seeds, preferably the meal or solvent-washed meal of the ground seeds, by use of water or aqueous solutions at a variety of temperatures, reagent concentrations, and the like. These freshly extracted solutions do not contain insoluble, swollen particles and do not develop a haze on standing. The residual insolubles can be removed, by conventional methods, such as centrifuging and/or filtering. The resulting solutions, when processed to a solid state, fail to fully dissolve. Dry mixing ground Cassia gum with other regents (like sorbitol, sucrose, inorganic salts, or other gelling and thickening agents) yields a two phase mixture from which the Cassia gum fails to dissolve in an aqueous medium completely. The resulting aqueous composition appears to be a suspension or dispersion of insoluble swollen particles within the solution which do not eventually dissolve. The resulting aqueous composition, if originally clear, forms a haze on standing. This haze is accelerated by heating and appears to be caused by a white film surrounding the insoluble, swollen particles. This haze makes it undesirable for dried Cassia gum formulations to be employed when product clarity is important. Further, the insoluble portion of the Cassia gum is no longer available to gel or impart viscosity to an aqueous medium.

It is undesirable to be required to prepare fresh Cassia gum extract from ground Cassia seed meal because of the inconvenience of the extra steps, extracting the Cassia gum from the seeds and separating the extract from the spent meal, because of the need to dispose of the spent meal, and because of the variability of the gum content of the meal.

EP-A-0139913 discloses gelling agents and thickeners based on Cassia-galactomannans and comprising a synergistic mixture of (a) Cassia-galactomannan and (b) carrageenan, agar and/or xanthan. However, the components are present as physical mixtures and are not coprecipitated to form a solid alloy gum.

The present invention provides a solid alloy gum composition as defined in claim 1 of the accompanying claims, a process for its preparation as defined in claim 4, and a process for its rehydration as defined in claim 13.

The alloy gum composition is prepared by extracting seeds of the genus Cassia with an aqueous medium to form a soluble extract portion and an insoluble residue portion, optionally separating the soluble extract portion from the insoluble residue portion, incorporating into the soluble extract portion a solubilizing quantity of said gelling and thickening agent and coprecipitating therefrom an alloy gum composition which forms on rehydration a substantially clear, stable colloidal aqueous solution, optionally containing the insoluble residue portion.

For some applications it is desirable to include inert materials into the alloy gum composition such as gelling or thickening agents which do not form an alloy gum when coprecipitated with a Cassia seed extract or other inert materials, such as the insoluble residue portion of extracted Cassia seeds. In such a case it is not necessary to separate the extract portion from the insoluble residue portion of the Cassia seeds or meal (or of the coextracted). However, for the purpose of describing the properties of the alloy gum compositions it is preferable to separate the insoluble residue portion from the soluble extract portion prior to coprecipitating the alloy gum composition. The scope of the present invention is intended to include the alloy gums and the process of producing them whether or not inert materials are incorporated therein.

The term "gelling and thickening agent" as used herein includes polysaccharide gums, hydrocolloids, which are compounds yielding a gel on combination with water, and/or compounds which in aqueous systems give colloidal, more or less highly viscous solutions or dispersions having plastic or pseudo-plastic flow including properties such as a thickening action, water-binding capacity, stabilization of suspensions and emulsions in polyphase systems, and gel formation.

The term "solution" as used herein is a homogeneous composition and includes a gel or colloidal dispersion in a medium which does not contain a substantial quantity of a persistently insoluble polysaccharide gum portion and which does not form a haze on standing.

The term "homogeneous" as used herein comprises a single phase of matter which is uniform in chemical composition. A homogeneous composition includes alloy gums comprising two or more chemically different compounds such as a galactomannan gum and a xanthan gum as distinguished from a two phase physical mixture of a galactomannan gum and a xanthan gum. A homogeneous composition of a polysaccharide gum coprecipitated with one or more gelling and thickening agents selected from the group consisting of carrageenan, furacellaran, agar, agarose, agaropectin, dextran, xanthan, algin, carboxymethylcellulose, gellan, low methoxyl pectin, hydroxyethylcellulose, locust bean gum, deacetylated chitin, polyacrylamide, polyethylene glycol and polyvinyl alcohol is termed an alloy gum.

Water-soluble Cassia gum can be extracted with an aqueous medium by conventional methods, preferably from the meal or solvent-washed meal of ground Cassia seeds. The extraction temperature can range from the freezing point to the boiling point of the aqueous medium. Elevated temperatures of 4&sl0;°C to 1&sl0;&sl0;°C are desirable. The residual insolubles can be separated by centrifuging, filtering or the like. The aqueous medium may comprise water or aqueous solutions containing salts or other compounds.

Any seeds of the genus Cassia may be employed as the source of Cassia gum, Cassia tora and Cassia occidentalis are preferred because of their commercial availability.

Cassia meal can also be coextracted with gelling and thickening agents in the crude form. For example, Cassia meal can be coextracted with locust beans or an alkali-modified ground seaweed powder which releases carrageenan when mixed with heated aqueous solutions.

At least one gelling and thickening agent may be incorporated into the aqueous medium prior to, during or after extracting the Cassia gum from the Cassia seed. However, unless a gelling and thickening agent selected from carrageenan, furacellaran, agar, agarose, agaropectin, dextran, xanthan, algin, carboxymethylcellulose, gellan, low methoxyl pectin, hydroxyethylcellulose, locust bean gum, deacetylated chitin, polyacrylamide, polyethylene glycol and polyvinyl alcohol is incorporated into the extract of the Cassia seed meal prior to coprecipitating the aqueous extract, the resulting Cassia gum composition will usually fail to redissolve to form a solution.

Although the exact proportion of Cassia gum and the gelling and thickening agent employed in the present invention can be varied over a wide range generally it requires at least one part by weight of the gelling and thickening agent to about four parts by weight Cassia gum to be a solubilizing quantity. If less than &sl0;.2 parts by weight of Cassia gum is employed per part by weight of the gelling and thickening agent, the composition may be too reduced in Cassia gum to exhibit sufficient synergy to be considered a Cassia alloy gum composition. Other gums and hydrocolloids such as guar gum and tara gum can be incorporated into the alloy gum composition but do not appear to enhance the solubilizing of the Cassia gum composition.

One unexpected benefit of the Cassia alloy gum compositions of the present invention is that many of the gelling and thickening agents, and in particular, galactomannan gums, when added to an aqueous solution as a powder have a tendency to "clump". If the gum is soluble these clumps will gradually disappear together with any temporary haze which might be observed. The Cassia alloy gum compositions of the present invention appear to have a significantly decreased tendency to form clumps compared to the gelling and thickening agents alone. This increased dispersion ability has been observed in particular with Cassia alloy gum compositions containing xanthan, algin, gellan, hydroxyethylcellulose and polyacrylamide. This property provides an added utility for the Cassia alloy gum compositions.

An additional unanticipated property is the high water absorptivity of solid Cassia:xanthan alloy gum compositions whether in the form of a powder, a fibrous coprecipitate or as a continuous film. A 5&sl0;:5&sl0; Cassia:xanthan alloy gum powder (about equal parts by weight) has been found to absorb up to 1,&sl0;&sl0;&sl0; times its weight of distilled water and, according to an external evaluation, the dry fibers absorb 5&sl0; times their weight of human urine, compared with 25 times the weight absorbed by a starch-polyacrylamide graft copolymer used as a control.

The solid Cassia alloy gum compositions of the present invention can be coprecipitated or separated from the aqueous extract by any convenient method. When carrageenan is the gelling and thickening agent, the Cassia alloy gum composition can be precipitated with potassium ions (KCl). In general, any alloy gum composition can be coprecipitated by evaporating the aqueous medium or by adding a water-miscible organic solvent to form a precipitate or coagulum which can be separated from the liquid by filtering or centrifuging. Isopropanol is the preferred water-miscible solvent. The coprecipitated wet homogeneous solids can be dried in a vacuum or with hot air.

The properties of some alloy gums appear to differ somewhat after precipitation and drying depending on the treatment or by pretreatment employed, such as alcohol pretreatment of Cassia meal prior to extraction, or air drying instead of vacuum drying the precipitated alloy gum. These minor differences in property can be determined by one skilled in the art without undue experimentation.

The best method for practising the present invention will be clear to one skilled in the art from the following nonlimiting examples.

EXTRACTION

Unless otherwise specified an aqueous extract of Cassia gum was prepared by adding 1.&sl0; g of Mucilose 39H (Diamalt AG, Munich) Cassia meal to 1&sl0;&sl0; ml of water, the mixture stirred and brought to boiling using a microwave oven. After heating for 1 hour at about 85°C, 2.5 g of filter aid was added, the mixture stirred to completely disperse the filter aid, then pressure filtered (0.24mPa; 20 psi) through filter paper. The filtrate (85 ml) was combined with a 25 ml hot water wash.

PRECIPTATION WITH AN ORGANIC AND DRYING

The extract was precipitated by adding twice the volume of 99% isopropanol (2-propanol) with stirring. The coagulum was collected by filtration through a nylon cloth, squeezed, then suspended in 1&sl0;&sl0; ml 8&sl0;% 2-propanol (aq.) as a wash, collected, then dried in a 6&sl0;°C forced-air oven, ground to 4&sl0; mesh to yield &sl0;.34 g of a tan powder, (34% yield). When 1&sl0;&sl0; mg was dispersed in 1&sl0; ml of distilled water and heated to boiling, a light brown mass of swollen particles in a viscous solution was observed by examining with an oblique light. Upon standing, this material developed an opalescent haze, which could be attributed to a coating around the swollen, undissolved particles.

Alcohol-washed Cassia meal (Diamalt AG) resulted in nearly white material with similar properties.

TESTING PROCEDURES

The Breakforce Value is the numerical value given for gel strength. In determining gel strength, the gel is cast in a 7&sl0; x 5&sl0; mm crystallizing dish, then the dish containing the gel placed on a scale. A plunger with a 1 cm² area is driven electrically into the gel at constant rate. The value recorded on the scale at which the plunger breaks through the surface of the gel is the Breakforce Value (gel strength) and reported as g/cm².

"Solubilizing Effect" is determined by comparing the light scattered by a solution or gel of Cassia gum alone and an equivalent alloy gum. Usually a range of alloy gum compositions is employed of 25:75, 5&sl0;:5&sl0; and 75:25 by weight. Results are reported on a semi-quantitative scale of strong, medium and weak.

EXAMPLE 1 Coprecipitation with Carrageenan using Potassium Chloride

An aqueous extract of Mucilose 39H extract was obtained by heating a 2% slurry in water at about 9&sl0;°C for two hours, then filtering. A filtrate containing &sl0;.71% 2-propanol insolubles and a 9&sl0;°C viscosity (Brookfield) of 25 mpa.s was obtained. The carrageenan used was a plant extract containing 2.42% 2-propanol precipitables, 3&sl0; mpa.s viscosity. This and the Cassia extract were combined to form five gum compositions which were coprecipitated (1:4) in 3% KCl (aq.) and the Cassia alloy gum recovered.

The gel strengths are reported in Table I.

EXAMPLE 2 Coprecipitation with carrageenan in 2-propanol

  • (a) Fifty ml of Cassia aqueous extract filtrate was added to 25 ml of an aqueous solution of &sl0;.25 g of kappa-carrageenan, the mixture was stirred, heated to 6&sl0;°C and the mixture recovered as a homogeneous composition by filtration, then precipitated in 2-propanol. The dry Cassia alloy gum powder was readily completely soluble in hot water, remained clear, and formed a clear gel upon cooling. The approximate gum ratio composition of the coprecipitated recovered powder was 1 part Cassia gum:1 part carrageenan extract.
  • (b) A series of experiments were run to determine maximum synergy ratios and minimum carrageenan necessary in the coprecipitate to facilitate solubility. Forty grams of the Cassia meal was extracted in 4 liters of water. Based on a control sample, the Cassia extract was &sl0;.7%. Using this value, sufficient kappa-carrageenan was dissolved in the Cassia extract to form a series of compositions and the gel strength was determined. The solutions were coagulated in 2-propanol and the coprecipitates recovered as in Example 2(a). Results are presented as Table II.

EXAMPLE 3 Coprecipitation with xanthan in 2-propanol

Eight grams of alcohol-washed Cassia meal (Diamalt AG) was slurried with 8&sl0;&sl0; ml of water, extracted at 8&sl0;°C for one hour, then 25 g filter aid added and the mixture pressure filtered (0.17-0.41mPa; 10-45 psi). The filtrate was divided into four parts, with the first precipitated in two volumes of 91% 2-propanol (aq.), washed and dried (6&sl0;°C). Recovery:&sl0;.81 g. Sufficient xanthan (Kelco "Keltrol T,") was added to the other three portions (&sl0;.27 g, &sl0;.81 g, 2.43 g, respectively) to give compositions having 1&sl0;&sl0;:&sl0;, 75:25, 5&sl0;:5&sl0; and 25:75 ratios of Cassia:xanthan by weight. These were precipitated with 2-propanol as described for the control, dried, and ground. Properties were determined. The 75:25 sample was substantially soluble with the 5&sl0;:5&sl0; and 25:75 fully soluble. The results are presented as Table III.

The dry powder and the dry coagulum fibers of the 5&sl0;:5&sl0; Cassia:xanthan compositions were extremely water absorbent, with the powder taking up 1,&sl0;&sl0;&sl0; times its weight of distilled water (forming a clear swollen particle mass), less of 1% NaCl (aq.) - showing ionic strength dependency. Continuous films prepared from a hot solution of the 5&sl0;:5&sl0;, then dried, readily absorbed distilled water, and became hydrated.

Many gels fracture after at least one freeze-thaw cycle, releasing the fluid used to make up the gel. This is particularly troublesome in some applications as the freeze-thaw cycle destroys the gel structure. Gels having freeze-thaw stability are very uncommon. Unexpectedly, gels of 5&sl0;:5&sl0; Cassia:xanthan are freeze-thaw stable.

EXAMPLE 4 Coprecipitation with agar

Following the procedure described in Example 3, substituting agar (Bacto Difco) for xanthan, coprecipitated samples containing a constant 2% gum were prepared and tested.

From the results appearing in Table IV, it is obvious that Cassia extract could be a valuable diluent for agar, imparting significant synergistic added gel strength as well as solubilizing the Cassia gum. Without synergy effects the gel strength of samples b, c and d would be expected to be 115, 23&sl0; and 345 respectively.

EXAMPLE 5 Cassia compositions

Homogeneous aqueous compositions were produced in weight ratios of 75:25; 5&sl0;:5&sl0; and 25:75 of Cassia gum and other gelling and thickening agents. Results are presented as Table V. Cassia alloy gums were precipitated with isopropanol unless otherwise indicated.

Solubilizing effect summarizes in semi-quantitative terms the solubility of the Cassia gum alloy compared with the Cassia gum alone.

Gel synergy is considered to be present if the gel strength of the alloy gum is greater than the individual gums. As some gums do not form a gel (gel strength is zero) the gel synergy is reported on a semi-quantitative scale.

Gel synergy was observed in some homogeneous compositions similar to the known locust bean gum synergy with kappa-carrageenan, xanthan and agar. The known synergy with locust bean gum is included in Table V for convenience to illustrate the present invention.

Not shown in Table V are similar Cassia compositions with other galactomannans, guar and tara. These two galactomannans do not have a synergistic effect with Cassia gum. EXAMPLE 1 - GEL STRENGTH Sample Weight Ratio Cassia:Carrageenan Gel Strength g/cm² a &sl0;:1&sl0;&sl0; 99&sl0; b 9:91 1,325 c 19:81 1,91&sl0; d 31:69 1,885 e 46:54 1,96&sl0;

GEL STRENGTH OF CASSIA:XANTHAN GUMS Sample a b c d e % Cassia 1&sl0;&sl0; 75 5&sl0; 25 &sl0; % Xanthan &sl0; 25 5&sl0; 75 1&sl0;&sl0; 1.5% Viscosity (75°C) (mpa.s) 75 2&sl0;&sl0;&sl0; 17&sl0;&sl0; 23&sl0;&sl0; 26&sl0;&sl0; 2% Gel strength (g/cm²) &sl0; 1&sl0;6 412 457 &sl0;
(Gels were very elastic)

Sample c (5&sl0;:5&sl0;) exhibited a gelling temperature of 57.&sl0;°C and a melting temperature of 59.&sl0;°C. GEL STRENGTH OF CASSIA:AGAR GUMS Sample a b c d e % Cassia 1&sl0;&sl0; 75 5&sl0; 25 &sl0; % Agar &sl0; 25 5&sl0; 75 1&sl0;&sl0; Gel strength (g/cm²) &sl0; 27&sl0; 7&sl0;2 1392 46&sl0;
SOLUBILITIES AND/OR SYNERGISTIC EFFECTS OF COMPOSITIONS OF <u>CASSIA</u> GUM ALLOYS WITH COMMON GELLING AND THICKENING AGENTS Alloy Agent Solubilizing Effect Synergy with Cassia Locust Bean Gum Kappa A-H carrageenan strong v.strong strong Kappa A-H carrageenan (air dried) strong strong - HWG kappa-carrageenan strong v.strong - Furcellaran strong v.strong - Iota carrageenan strong none none Sodium lambda carrageenan medium none none Agar strong v.strong strong Agarose (SeaKemR LE) medium none none Agaropectins strong none none SeaPlaqueR agarose weak(25:75 only) none none Xanthan (Keltrol T) strong v.strong strong Xanthan (Keltrol T) (air dried) strong strong - Xanthan (M.Colloids) strong v.strong - Algin (Kelmar) strong strong none Carboxymethylcellulose strong medium none Gellan (Kelco) strong none none Low methoxyl pectin medium none none Hydroxyethylcellulose strong medium none Deacetylated chitin medium none none Polyacrylamide (NP1O) strong none none Dextran medium none none Polyethylene glycol (6&sl0;&sl0;&sl0;) medium none none Polyvinyl alcohol medium none none Clarified locust bean gum medium none - Clarified locust bean gum/carrageenan mixture strong strong -
Note: In the cases of xanthan, algin, gellan, HEC, and Cassia-polyacrylamide extract coprecipitated powders, dispersion was significantly improved over the gum by itself.


Anspruch[de]
Patentansprüche für folgende Vertragsstaaten : AT, BE, CH, DE, FR, GB, IT, LI, LU, NL, SE

  1. Feste Gummizusammensetzung, gekennzeichnet durch Galactomannangummi, das aus Samen der Gattung Cassia mit einem wäßrigen Medium extrahiert und zusammen mit einer löslichmachenden Menge eines Gelier- und Verdickungsmittels ausgefällt wurde, welches aus der Gruppe bestehend aus Carrageen, Furcellaran, Agar, Agarose, Agaropectin, Dextran, Xanthan, Algin, Carboxymethylcellulose, Gellan, nieder-methoxyliertes Pectin, Hydroxyethylcellulose, Johannisbrotgummi, deacetyliertes Chitin, Polyacrylamid, Polyethylenglykol und Polyvinylalkohol ausgewählt ist, um eine feste Gummizusammensetzung zu bilden, die 0,2 bis 4 Gew.-Teile Cassia-galactomannan-Gummi je Gew.-Teil des Gelier- und Verdickungsmittels umfaßt und nach Rehydration eine klare, stabile, kolloidale, wäßrige Lösung bildet.
  2. Gummizusammensetzung nach Anspruch 1, dadurch gekennzeichnet, daß das Gelier- und Verdickungsmittel Xanthan ist und in etwa gleichen Gewichtsteilen wie Galactomannan, das aus Samen der Gattung Cassia extrahiert ist, vorliegt.
  3. Gummizusammensetzung nach Anspruch 1 oder 2, gekennzeichnet durch Galactomannangummi das aus Samen der Gattung Cassia mit einem wäßrigen Medium extrahiert und zusammen mit mindestens zwei oder mehr Gelier- und Verdickungsmitteln ausgefällt wurde.
  4. Verfahren zur Herstellung einer festen hydratisierbaren Gummizusammensetzung nach Anspruch 1, 2 oder 3, gekennzeichnet durch Extraktion der Samen der Gattung Cassia mit einem wäßrigen Medium unter Bildung eines löslichen Extraktanteils und eines unlöslichen Restanteils, Einbringen einer löslichmachenden Menge des Gelier- und Verdickungsmittels in den löslichen Extraktanteil und Mitfällen einer festen Gummizusammensetzung daraus.
  5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die Gummizusammensetzung durch Einbringen einer ausreichenden Menge eines wassermischbaren Lösungsmittels in den löslichen Extraktanteil unter Bildung eines Koagulats in einer überstehenden Flüssigkeit mitgefällt, das Koagulat von der überstehenden Flüssigkeit abgetrennt und das abgetrennte Koagulat getrocknet wird.
  6. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß das wassermischbare Lösungsmittel Isopropanol ist.
  7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß das Gelier- und Verdickungsmittel Carrageen ist und der lösliche Extraktanteil zusammen mit Kaliumionen ausgefällt, der Niederschlag von dem löslichen Extrakt abgetrennt und der abgetrennte Niederschlag getrocknet wird.
  8. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die Gummizusammensetzung durch Verdampfen des wäßrigen Mediums mitgefällt wird.
  9. Verfahren nach einem der Ansprüche 4 bis 8, dadurch gekennzeichnet, daß der unlösliche Restanteil vom löslichen Extraktanteil vor dem Mitfällen der Gummizusammensetzung abgetrennt wird.
  10. Verfahren nach Anspruch 9, gekennzeichnet durch das Einbringen etwa eines Gew.-Teils Xanthangummi je Gew.-Teil Galactomannan-Feststoff in den wäßrigen Extraktanteil und Mitfällen der Gummizusammensetzung.
  11. Gummizusammensetzung, die Galactomannangummi aus Samen der Gattung Cassia umfaßt, das zusammen mit einer löslichmachenden Menge eines Gelier- und Verdickungsmittels ausgefällt wird, so daß es nach Rehydration zur Bildung einer im wesentlichen klaren, stabilen, kolloidalen wäßrigen Lösung fähig ist.
  12. Hydratisierbare Gummizusammensetzung, die einen Galactomannangummi aus Samen der Gattung Cassia und eine löslichmachende Menge eines Gelier- und Verdickungsmittels umfaßt.
  13. Verfahren zur Herstellung einer kolloidalen Lösung des Galactomannangummis, das die Rehydration einer festen Gummizusammensetzung nach einem der Ansprüche 1 bis 3, 11 und 12 umfaßt.
Patentansprüche für folgende Vertragsstaaten : ES, GR

  1. Verfahren zur Herstellung einer festen Gummizusammensetzung, die nach Rehydration eine klare, stabile, kolloidale, wäßrige Lösung bildet und Galactomannangummi, das aus Samen der Gattung Cassia mit einem wäßrigen Medium extrahiert wurde und eine löslichmachende Menge eines Gelier- und Verdickungsmittels umfaßt, welches aus der Gruppe, bestehend aus Carrageen, Furcellaran, Agar, Agarose, Agaropectin, Dextran, Xanthan, Algin, Carboxymethylcellulose, Gellan, nieder-methoxyliertes Pectin, Hydroxyethylcellulose, Johannisbrotgummi, deacetyliertes Chitin, Polyacrylamid, Polyethylenglykol und Polyvinylalkohol ausgewählt ist, dadurch gekennzeichnet, daß das Galactomannangummi und das Gelier- und Verdickungsmittel zusammen ausgefällt werden, um eine feste Gummizusammensetzung zu bilden, die 0,2 bis 4 Gew.-Teile Cassia-galactomannan-Gummi je Gew.-Teil des Gelier- und Verdickungsmittels umfaßt.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Gelier- und Verdickungsmittel Xanthan ist und in etwa gleichen Gewichtsteilen wie Galactomannan, das aus Samen der Gattung Cassia extrahiert ist, vorliegt.
  3. Verfahren nach Anspruch 1 oder 2, gekennzeichnet durch Galactomannangummi, das aus Samen der Gattung Cassia mit einem wäßrigen Medium extrahiert und zusammen mit mindestens zwei oder mehr Gelier- und Verdickungsmitteln ausgefällt wurde.
  4. Verfahren nach Anspruch 1, 2 oder 3, gekennzeichnet durch Extraktion der Samen der Gattung Cassia mit einem wäßrigen Medium unter Bildung eines löslichen Extraktanteils und eines unlöslichen Restanteils, Einbringen einer löslichmachenden Menge des Gelier- und Verdickungsmittels in den löslichen Extraktanteil und Mitfällen einer festen Gummizusammensetzung daraus.
  5. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß die Gummizusammensetzung durch Einbringen einer ausreichenden Menge eines wassermischbaren Lösungsmittels in den löslichen Extraktanteil unter Bildung eines Koagulats in einer überstehenden Flüssigkeit mitgefällt, das Koagulat von der überstehenden Flüssigkeit abgetrennt und das abgetrennte Koagulat getrocknet wird.
  6. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß das wassermischbare Lösungsmittel Isopropanol ist.
  7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß das Gelier- und Verdickungsmittel Carrageen ist, und der lösliche Extraktanteil zusammen mit Kaliumionen ausgefällt, der Niederschlag von dem löslichen Extrakt abgetrennt und der abgetrennte Niederschlag getrocknet wird.
  8. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die Gummizusammensetzung durch Verdampfen des wäßrigen Mediums mitgefällt wird.
  9. Verfahren nach einem der Ansprüche 4 bis 8, dadurch gekennzeichnet, daß der unlösliche Restanteil vom löslichen Extraktanteil vor dem Mitfällen der Gummizusammensetzung abgetrennt wird.
  10. Verfahren nach Anspruch 9, gekennzeichnet durch das Einbringen etwa eines Gew.-Teils Xanthangummi je Gew.-Teil Galactomannan-Feststoff in den wäßrigen Extraktanteil und Mitfällen der Gummizusammensetzung.
  11. Verfahren zur Herstellung einer Gummizusammensetzung, die nach Rehydration zur Bildung einer im wesentlichen klaren, stabilen, kolloidalen, wäßrigen Lösung fähig ist, dadurch gekennzeichnet, daß Galactomannangummi aus Samen der Gattung Cassia zusammen mit einer löslichmachenden Menge eines Gelier- und Verdickungsmittels ausgefällt wird.
  12. Verfahren zur Herstellung einer kolloidalen Lösung von Galactomannangummi, das die Rehydration einer festen, gemäß dem Verfahren nach einem der Ansprüche 1 bis 11 hergestellten Gummizusammensetzung umfaßt.
Anspruch[en]
Claims for the following Contracting States : AT, BE, CH, DE, FR, GB, IT, LI, LU, NL, SE

  1. A solid alloy gum composition characterized by galactomannan gum extracted by an aqueous medium from seeds of the genus Cassia coprecipitated with a solubilizing quantity of a gelling and thickening agent selected from the group consisting of carrageenan, furacellaran, agar, agarose, agaropectin, dextran, xanthan, algin, carboxymethylcellulose, gellin, low methoxyl pectin, hydroxyethylcellulose, locust bean gum, deacetylated chitin, polyacrylamide, polyethylene glycol and polyvinyl alcohol to form a solid alloy gum composition which comprises from 0.2 to 4 parts by weight Cassia-galactomannan gum per part by weight of the gelling and thickening agent and which forms a clear, stable colloidal aqueous solution on rehydration.
  2. The alloy gum composition of claim 1 characterized in that the gelling and thickening agent is xanthan and is present in about equal parts by weight with the galactomannan extracted from seeds of the genus Cassia .
  3. The alloy gum composition of claims 1 or 2 characterized by galactomannan gum extracted from an aqueous medium from the seeds of the genus Cassia coprecipitated with at least two or more gelling and thickening agents.
  4. A process for producing a solid hydratable alloy gum composition according to claim 1, 2 or 3 characterized by extracting the seeds of the genus Cassia with an aqueous medium to form a soluble extract portion and an insoluble residue portion, incorporating into the soluble extract portion a solubilizing quantity of said gelling and thickening agent and coprecipitating therefrom a solid alloy gum composition.
  5. The process of claim 4 characterized in that the alloy gum is coprecipitated by incorporating a sufficient quantity of a water-miscible solvent into the soluble extract portion to form a coagulum in a supernatant liquid, separating the coagulum from the supernatant liquid and drying the separated coagulum.
  6. The process of claim 5 characterized in that the water-miscible solvent is isopropanol.
  7. The process of claim 6 characterized in that the gelling and thickening agent is carrageenan and the soluble extract portion is coprecipitated with potassium ions, the precipitate is separated from the soluble extract and the separated precipitate is dried.
  8. The process of claim 4 characterized in that the alloy gum is coprecipitated by evaporating the aqueous medium.
  9. The process of any of claims 4 to 8, characterized in that the insoluble residue portion is separated from the soluble extract portion prior to coprecipitating the alloy gum.
  10. The process of claim 9 characterized by incorporating into the aqueous extract portion about one part by weight of xanthan gum per part by weight of galactomannan solids, and coprecipitating the alloy gum.
  11. A gum composition comprising galactomannan gum from seeds of the genus Cassia coprecipitated with a solubilising quantity of a gelling and thickening agent so as to be capable on rehydration of forming a substantially clear stable colloidal aqueous solution.
  12. A hydratable gum composition comprising a galactomannan gum from seeds of the genus Cassia and a solubilising quantity of a gelling and thickening agent.
  13. A process for making a colloidal solution of a galactomannan gum which comprises rehydrating a solid alloy gum composition as claimed in any of claims 1 to 3, 11 and 12.
Claims for the following Contracting States : ES, GR

  1. A process for making solid alloy gum composition which forms a clear, stable colloidal aqueous solution on rehydration, said composition comprising galactomannan gum extracted by an aqueous medium from seeds of the genus Cassia and a solubilizing quantity of a gelling and thickening agent selected from the group consisting of carrageenan, furacellaran, agar, agarose, agaropectin, dextran, xanthan, algin, carboxymethylcellulose, gellin, low methoxyl pectin, hydroxyethylcellulose, locust bean gum, deacetylated chitin, polyacrylamide, polyethylene glycol and polyvinyl alcohol characterised in that the galactomannan gum and the gelling and thickening agent are coprecipitated to form a solid alloy gum composition which comprises from 0.2 to 4 parts by weight Cassia-galactomannan gum per part by weight of the gelling and thickening agent.
  2. The process of claim 1 characterized in that the gelling and thickening agent is xanthan and is present in about equal parts by weight with the galactomannan extracted from seeds of the genus Cassia .
  3. The process of claims 1 or 2 characterized by galactomannan gum extracted from an aqueous medium from the seeds of the genus Cassia coprecipitated with at least two or more gelling and thickening agents.
  4. A process according to claim 1, 2 or 3 characterized by extracting the seeds of the genus Cassia with an aqueous medium to form a soluble extract portion and an insoluble residue portion, incorporating into the soluble extract portion the solubilizing quantity of said gelling and thickening agent and coprecipitating therefrom the solid alloy gum composition.
  5. The process of any preceding claim, characterized in that the alloy gum is coprecipitated by incorporating a sufficient quantity of a water-miscible solvent into the soluble extract portion to form a coagulum in a supernatant liquid, separating the coagulum from the supernatant liquid and drying the separated coagulum.
  6. The process of claim 5 characterized in that the water-miscible solvent is isopropanol.
  7. The process of claim 6 characterized in that the gelling and thickening agent is carrageenan and the soluble extract portion is coprecipitated with potassium ions, the precipitate is separated from the soluble extract and the separated precipitate is dried.
  8. The process of claim 4 characterized in that the alloy gum is coprecipitated by evaporating the aqueous medium.
  9. The process of any of claims 4 to 8, characterized in that the insoluble residue portion is separated from the soluble extract portion prior to coprecipitating the alloy gum.
  10. The process of claim 9 characterized by incorporating into the aqueous extract portion about one part by weight of xanthan gum per part by weight of galactomannan solids, and coprecipitating the alloy gum.
  11. A process for making a gum composition which is capable on rehydration of forming a substantially clear stable colloidal aqueous solution characterized by the step of coprecipitating galactomannan gum from seeds of the genus Cassia with a solubilising quantity of a gelling and thickening agent.
  12. A process for making a colloidal solution of a galactomannan gum which comprises rehydrating a solid alloy gum composition made by the process of any of claims 1 to 11.
Anspruch[fr]
Revendications pour les Etats contractants suivants : AT, BE, CH, DE, FR, GB, IT, LI, LU, NL, SE

  1. Composition solide de gomme combinée, caractérisée par une gomme de galactomannane, extraite par un milieu aqueux à partir de graines du genre Cassia, coprécipitée avec une quantité solubilisante d'un agent gélifiant et épaississant choisi dans le groupe constitué de la carraghénine, de la furcellarane, de la gélose, de l'agarose, de l'agaropectine, du dextrane, du xanthane, de l'algine, de la carboxyméthylcellulose, de la géline, de la pectine à faible teneur en groupes méthoxyles, de l'hydroxyéthylcellulose, de la gomme de caroube, de la chitine désacétylée, du polyacrylamide, du polyéthylèneglycol et de l'alcool polyvinylique, pour former une composition solide de gomme combinée qui comprend de 0,2 à 4 parties en poids de gomme de galactomannane-Cassia par partie en poids de l'agent gélifiant et épaississant, et qui forme une solution colloïdale aqueuse stable, transparente après réhydratation.
  2. Composition de gomme combinée selon la revendication 1, caractérisée en ce que l'agent gélifiant et épaississant est le xanthane et en ce qu'il est présent en parties en poids à peu près égales avec le galactomannane extrait de graines du genre Cassia.
  3. Composition de gomme combinée selon les revendications 1 ou 2, caractérisée par la gomme de galactomannane, extraite d'un milieu aqueux à partir des graines du genre Cassia, coprécipitée avec au moins deux agents gélifiants et épaississants ou plus.
  4. Procédé pour produire une composition solide de gomme combinée, hydratable, selon la revendication 1, 2 ou 3, caractérisé par l'extraction des graines du genre Cassia avec un milieu aqueux pour former une fraction d'extrait soluble et une fraction de résidu insoluble, l'incorporation, dans la fraction d'extrait soluble, d'une quantité solubilisante dudit agent gélifiant et épaississant, et la coprécipitation, à partir de celle-ci, d'une composition solide de gomme combinée.
  5. Procédé selon la revendication 4, caractérisé en ce que la gomme combinée est coprécipitée en incorporant une quantité suffisante d'un solvant miscible à l'eau dans la fraction d'extrait soluble pour former un coagulum dans le liquide surnageant, en séparant le coagulum du liquide surnageant et en séchant le coagulum séparé.
  6. Procédé selon la revendication 5, caractérisé en ce que le solvant miscible à l'eau est l'isopropanol.
  7. Procédé selon la revendication 6, caractérisé en ce que l'agent gélifiant et épaississant est la carraghénine et en ce que la fraction d'extrait soluble est coprécipitée avec des ions potassium, le précipité est séparé de l'extrait soluble et le précipité séparé est séché.
  8. Procédé selon la revendication 4, caractérisé en ce que la gomme combinée est coprécipitée en évaporant le milieu aqueux.
  9. Procédé selon l'une quelconque des revendications 4 à 8, caractérisé en ce que la fraction de résidu insoluble est séparée de la fraction d'extrait soluble avant la coprécipitation de la gomme combinée.
  10. Procédé selon la revendication 9, caractérisé par l'incorporation, dans la fraction d'extrait aqueux, d'environ 1 partie en poids de gomme de xanthane par partie en poids de matières solides de galactomannane, et la coprécipitation de la gomme combinée.
  11. Composition de gomme comprenant de la gomme de galactomannane, provenant de graines du genre Cassia, coprécipitée avec une quantité solubilisante d'un agent gélifiant et épaississant de façon à être capable, après réhydratation, de former une solution colloïdale aqueuse stable substantiellement transparente.
  12. Composition de gomme hydratable comprenant une gomme de galactomannane provenant de graines du genre Cassia et une quantité solubilisante d'un agent gélifiant et épaississant.
  13. Procédé pour fabriquer une solution colloïdale d'une gomme de galactomannane, qui comprend la réhydratation d'une composition solide de gomme combinée selon l'une quelconque des revendications 1 à 3, 11 et 12.
Revendications pour les Etats contractants suivants : ES, GR

  1. Procédé pour fabriquer une composition solide de gomme combinée qui forme une solution colloïdale aqueuse stable transparente après réhydratation, ladite composition comprenant une gomme de galactomannane extraite par un milieu aqueux à partir de graines du genre Cassia et une quantité solubilisante d'un agent gélifiant et épaississant choisi dans le groupe constitué de la carraghénine, de la furcellarane, de la gélose, de l'agarose, de l'agaropectine, du dextrane, du xanthane, de l'algine, de la carboxyméthylcellulose, de la géline, de la pectine à faible teneur en groupes méthoxyles, de l'hydroxyéthylcellulose, de la gomme de caroube, de la chitine désacétylée, du polyacrylamide, du polyéthylèneglycol et de l'alcool polyvinylique, caractérisé en ce que la gomme de galactomannane et l'agent gélifiant et épaississant sont coprécipités pour former une composition solide de gomme combinée qui comprend de 0,2 à 4 parties en poids de gomme de galactomannane-Cassia par partie en poids de l'agent gélifiant et épaississant.
  2. Procédé selon la revendication 1, caractérisé en ce que l'agent gélifiant et épaississant est le xanthane et en ce qu'il est présent en parties en poids à peu près égales avec le galactomannane extrait de graines du genre Cassia.
  3. Procédé selon les revendications 1 ou 2, caractérisé par la gomme de galactomannane, extraite d'un milieu aqueux à partir des graines du genre Cassia, coprécipitée avec au moins deux agents gélifiants et épaississants ou plus.
  4. Procédé selon la revendication 1, 2 ou 3, caractérisé par l'extraction des graines du genre Cassia avec un milieu aqueux pour former une fraction d'extrait soluble et une fraction de résidu insoluble, l'incorporation, dans la fraction d'extrait soluble, d'une quantité solubilisante dudit agent gélifiant et épaississant, et la coprécipitation, à partir de celle-ci, de la composition solide de gomme combinée.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la gomme combinée est coprécipitée en incorporant une quantité suffisante d'un solvant miscible à l'eau dans la fraction d'extrait soluble pour former un coagulum dans le liquide surnageant, en séparant le coagulum du liquide surnageant et en séchant le coagulum séparé.
  6. Procédé selon la revendication 5, caractérisé en ce que le solvant miscible à l'eau est l'isopropanol.
  7. Procédé selon la revendication 6, caractérisé en ce que l'agent gélifiant et épaississant est la carraghénine et en ce que la fraction d'extrait soluble est coprécipitée avec des ions potassium, le précipité est séparé de l'extrait soluble et le précipité séparé est séché.
  8. Procédé selon la revendication 4, caractérisé en ce que la gomme combinée est coprécipitée en évaporant le milieu aqueux.
  9. Procédé selon l'une quelconque des revendications 4 à 8, caractérisé en ce que la fraction de résidu insoluble est séparée de la fraction d'extrait soluble avant la coprécipitation de la gomme combinée.
  10. Procédé selon la revendication 9, caractérisé par l'incorporation, dans la fraction d'extrait aqueux, d'environ 1 partie en poids de gomme de xanthane par partie en poids de matières solides de galactomannane, et la coprécipitation de la gomme combinée.
  11. Procédé pour fabriquer une composition de gomme qui est capable, après réhydratation, de former une solution colloïdale aqueuse stable substantiellement transparente, caractérisé par l'étape de coprécipitation de la gomme de galactomannane, provenant de graines du genre Cassia, avec une quantité solubilisante d'un agent gélifiant et épaississant.
  12. Procédé pour fabriquer une solution colloïdale d'une gomme de galactomannane, qui comprend la réhydratation d'une composition solide de gomme combinée fabriquée par le procédé selon l'une quelconque des revendications 1 à 11.






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