CA2242239A1 - Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature - Google Patents
Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature Download PDFInfo
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- CA2242239A1 CA2242239A1 CA002242239A CA2242239A CA2242239A1 CA 2242239 A1 CA2242239 A1 CA 2242239A1 CA 002242239 A CA002242239 A CA 002242239A CA 2242239 A CA2242239 A CA 2242239A CA 2242239 A1 CA2242239 A1 CA 2242239A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
- C08B37/0096—Guar, guar gum, guar flour, guaran, i.e. (beta-1,4) linked D-mannose units in the main chain branched with D-galactose units in (alpha-1,6), e.g. from Cyamopsis Tetragonolobus; Derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
- A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
- A23G3/346—Finished or semi-finished products in the form of powders, paste or liquids
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/238—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seeds, e.g. locust bean gum or guar gum
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G2200/00—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents
- A23G2200/06—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents containing beet sugar or cane sugar if specifically mentioned or containing other carbohydrates, e.g. starches, gums, alcohol sugar, polysaccharides, dextrin or containing high or low amount of carbohydrate
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- Materials Engineering (AREA)
- Nutrition Science (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Jellies, Jams, And Syrups (AREA)
- Seeds, Soups, And Other Foods (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Functionally modified guar products are provided, particularly for food grade applications, characerized by reduced viscosity, low ash and high fiber content, prepared by high shear treatment under acid conditions at elevated temperature.
Description
WO 97125354 PCTnB9S/(71171 _ .
MODIFIED GUAR, PREPARED BY HIGH SHEAR TREATMENT UNDER ACIDIC CONDITIONS AT ÉLE
VATED TEMPERATURE
FTELD OF T~E IN~N1iON
This invention reiates to the provision of 5 ~unctionally modified guar products and their u e, particularly in food grade applications. More particular}y, there is descri~ed an at least semi-continuous process for the treatment of suar particulate to provide a relatively hu~u~ eous, uniform, stable 10 product for application in the food industry, providing in a~ueous solution a re~ hlP v~c~-oc; ty under controlled condit~ons ~r~hl~ of efficient conversion into processing aids, thir~n~rs, hi nr~r~;, S~hi1; 7ers and ~ ~n~; ty b~ ~rS to ~m~nt food products such as c~ salad drec~i n7~ h~F~c~ and o7~ products, providing ~ u~ P texture and mouthfeel, among other desira~le organo~eptic properties. Moreover, the product as pro~C~A in accorda~ce with the inventive princ$ples more fully descrihed herein is free of unaccepta~le ash levels providing a visually and functionally attractive adiunctive agent in food use, to ~id in dispersion, gelation, moisture retention, preservation, stabilization or viscosity E~LLU1.
Additionally, the product provides a rich source of dietary fi~er without excessive viscosity as is evi~enoe~ with no~m~l, non-fu~ctinn~7 i ~ gu~r gum.
BA~ UND OF ~ NV~NllON
- Guar is derived ~rom the endosperm of the leg~min~ plant Cy~ ss tetra~onolobus (Llnue~ T~ub 3 or Cv~.,~is Psoraloides ~Lami) D.C. ~Fam. Le~mi nn~ 3;
W O 97/25354 - PCT~B95/01171 _. . = =
1 ft iS a high molerl~~r weight non-ionic l.y~lr~ oida poly5~r~h~idc, a galact~nn~n cn~ro-c~ of ~alactose and ~nnoqe units. Guar seeds comprise a seed coat or hull, a pair of tough endosperm sections, re~erred to as 5 'guar splits', which contain the gum and the ~L~yu. In prO~qc; n~, the hull is ~ ~d and the ~ nts separated ~y grin~ , st4t-ng and scr~enin~ in one or more stages. The splits are ~-o~u,d and prnc~seA to provide a gum or gum precursor.
The splits may ~e pro~c~A to recover .,ents thereof which may include all mem~rane, inorganic salts, and th~ pr~r~i n~nt gal aCt~Ann~, poly~r~hA-ide as well as ~ori~ted prot~in~r~o~s material and water insolu~le gels. The extraction has 15 typically ~een achieved by way o~ hydration and/or ~1~A1 ;n~ digestion or re~n;n~ y.~ eeC as repre~"L~~
by U.s. Patent No. 4,269,97~ to Nat;nn~7 Starch and Ch~i ~1 Corporation and U.S. Patent No- 4,659,811 to R~n~e~. In the f ormer, a hydrationfextrus~on operation 20 is said to proYide _ hi~h ~;C~t~cityr e.g. 5000 cps ~ine-y diYided, moisturized suar gum which could be dried and gro~n~ _or future use. The '811 patent tand cited references such as U.~. Patent No. ~06,327) recites the use of an A 1 ~ ~1; n~ m~ ~ at elevated 25 temperature to separate ~ y~ frcm ~yu and r~s~ husk. The pat~nt~ still employs upwards of 60 percent of water in the reaction mixture, and utiliz~s a pH above 12, with a ~;ni~-m of 150 parts ~y weight of aqueous ~ . ~he resulting wet c~ may be 3o partially neutr~ to a p~ below about 11, e.g., pH 9 ~Example 9).
3~
W O 97/25354 PCT~B95/01171 1 Other industrial processes have refined natural guar splitfi with acid solutions, heating the mixture, and then neutrAl; ~ng the acid with sodium hydroxide or another ~lkAli nP material. The resultant 5 product is a functionally modified guar controlled primarily by the pH and time of heat proc~cc;ng~
Neutralization by al k~31in~ treatment has ten-l~.l to result in a high ash content, vari~hi1;ty and other characteristics inconsistent with food ingredient use.
10 In these processes effects tend to be concentrated on the exterior portion of the endosperm le~i n~ to an irregular non-uniform product with differential levels of functional modification. The property of stringiness manifests itself in processed and dried guar qum 15 products and presents difficulties in food applications where smoothness, slipperiness or greasiness are important qualities to achieve or retain. While modification with ch~mio~l proc~ nq may min;~i~e this problem it is at~ended with the rea~y development o~
20 ash, rapidly approA~hin~ levels of 1.5~ or more, ~nArcepta~le for food use.
It is accordingly desirable to provide a process for the reftnPm~nt of natural guar products to afford a uniform, homogeneous particulate product 25 c~r~hle of forming aqueous solutions, pastes and gums of consistent, stable and r~ hl e low vi~s;ty and ash contents ~elow 1.5%, generally below 1.0~ for use in food product compositions of enh~nr~ aesthetic character including desirable th;ckf~n;ng and smooth~on~ ng properties with enh~nced mouthfeel in addition to other favorable organo1eptic properties.
W O 97/25354 PCT~B95/Q1171 _.
~4~
1 BRIEF SU~ RY OF ~ E IN~rE~rrION
T n accordanCe with the present invention r free-flowing particulate me~h~ni cally processed guar endo-~perm ic su~iected to a~ueous procec~; n~ under 5 acidic conditions with min~l a~ueous di7ution and hence controlted, limited hydration and relatively high shear tO produce a converted guar product of modified rheological characteristics.
More specifically, there is pro~ided a lO functionally modified guar product for food use, comprising low ashr a shorter te~Lu~ than co~,v~.-Lional guar products and elch ihi ting a novel low viscc~s'tty profile eSp~ci~lly at about 1% con~L.L~tion or less under conditions of conventi nn~l refri~eration r~nq-nq 15 to mildly elevated temperatures in food ~Tro~itions such as ~ eeC, salad dr~ssi n~c a~d the like.
These desira~le characterist-cs are achieved ~y su~jecting ~ree-~lowing guar endosperm part;c~7~te to high shear refining under controlled conditions of acid 20 hydration; the resultin~ product i5 then su~jected to a heat treatment under static or stirred conditions. The acid refining is effected so to control the amount of water av~ hl e for hydration relative to the con~entration of guar, i.e., at relatively high solids 25 level. The re~ining at high shear i5 maint~n~ for a period of time su~ficient to s~n;f;~ant7y reduce the viscosity of guar to levels in the r~nge of 0 to 2,S00 cps; preferab7y 0 to 1,500 cps; an~ most pre~era~y 0-l,OOQ cps. Many uses are found that uti~ize the lower 3o viscosities. The a~solute acid level ic relatively low in cnmr~ison to direct acid refining o~ whole hydrated W O 97/25354 PCT~B95/01171 1 guar splits as practiced in the art such that degradation leading to ash levels unacceptable in food use is controlled and minim;zed. Even at relatively low acid levels it may never~h~le~c be de~irahle to pro~ide 5 a fully neutralized product, hence for this purpose reaction with AlkA1i to effect neutralization may be employed to m;n;m; ze salt levels.
BRIEF DESCRIPTION OF TEE DRAWIN~S
10 Fig. I (Effect o~ Acid on Guar Modification) is a plot of Viscosity (cps) as the a~scissa and hydration time (minutes~ e~i~nc;n~ ch~ng~ in rheological characteri~tic in accordan~e with the invention.
D~.TAIT~D DESCRIPTION OF THE Ihv~NLlON
The native guar may be simply purified, i.e., split with hull removed or ~hnllP~ and screened one or more times to ~ ve detritus, and then y r ~u~d to a 20 particulate rauging from a coarse gr~nlllAr material to a fine powder. Coarser materials tend to ~;~p~rse more readi~y, whereas finer grinds are more rapidly hydrated.
The guar starting material employed is at least 66% galac~nm~nn~n and ~rh;~; ts cnmro!;;~;on~l 25 elements consistent with the Food Chemicals Codex 3d Ed.
(1981), p.1~1 incorporated herein by re_erence;
specifically after proce ~n~ it contains no more ash than eYcee~s 1 to 1.5~ by weight of the guar. Course gums p~.cc;ng through a 40 ~esh screen but min;m~lly through a lQ0 mesh screen; and fine gums ~f;n~ as those cont~;n;ng a pre~nm~n~nce of particles p~;n~
W O 97/253~4 PCT~B95/01171 1 through a 200 mesh screen, can be used to prepare a satisfactory product. It will be understood that sources of guar may be mixed such that a certain bimodal distri~ution may result, for example, where a coarse 5 grind and fine powder are used together.
Guar gums of varying initial v;~o~;ty, reflective of variations in molecular weight, cn~o~ition, and degree o~ br~nrhi n~ are readily av~ hl e, in the range of 1000 to 6000 cps measured as 10 a 1% solution (Broo~field RVF vi~m~ter, 5~;nAl~ 3 or 4, 20 rpm). While any guar gum starting material may be employed, Uniguar 40 av~ hle from Rhone Poulenc with a v~scosity of 2000 cps or Dycol 4000 FC, also available from Rhone Poulenc with a typical viscosity of 4000 cps 15 (both viscosities determ;nP~ as a 1% (w/w) solution using a Brookfield RVF viscometer (Spindle 3, 20 rpm) is preferred.
The guar is intro~ to a high shear m; ~; ng zone cont~; n; ng or to which is added an agueous acidic 20 medium with or without A~cohnl. Pre~erably, acid with a limited amount of water with or without alcohol is gradually added to the guar under condit~ons of high shear agitation. The rate of addition may be empirically se~ected to mi nim; ~e cll~mri n~ or the 25 formation of gummy particles and may be af~ected by the rate of shear or the advance of the material to be treated, all o~ which i5 easily de~m; n~l by one skilled in the art-By high shear mixing, it is inten~e~ to denote 3o a ~;~n~ process in a cont~;~PA zone ;n~ A;n~ stirringunder conditions to ef~ect in ad~acent zones o~ the --_ 1 substrate being wor~ed the application o~ differential forces, (as, differential velocity) between said zones, which may be in l~i n~r or tur~ulent flow. ~s is well known to those sk;l1e~ in these arts, the differential 5 forccs may be effected by the geometry of the stirring blade, the clea~ance of the ~lade ~er with the cont~; n~r or fixed or moveahle ohstructions in the cont~ne~ and the velocity of the stirrer, and will naturally be affected by the temperature o~ the system 10 relati~e to the viscosity characteristics o~ the stirred medium. Under conditions of high velocity, low clearances and~or high viscosit~, high shear miX; n~
expressed in units of reciprocal s~co~ is readily achieved.
The treatment regimen is selected to maintain a high solids system with mi n;mllm moisture level; in addition, the acid addition is adjusted to maintain p~
yet avoid undesira~le formation o~ ash from the action of ~ cs acid. For experimental purposes, a 20 prototypical~batch system employed a Cl~;sin~rt food processor with the basic cutting blade providing shear to the m~X;ng zone cont~'n;n~ about SOQ grams of guar gum granulate and acid (2N HCl 1:6 dilution o~ 12 N HCL
in ethanol) was added at a rate of about S mltmin~ to a 25 total of 10 to 35 ml with continuous mixin~; after the completion o~ acid addition, the system was agitated for another 10 to 15 s~con~. Conditionc for larger semi-continuous and continuous systems may ~e adapted consistently within the knowledge of one skilled in the art.
1 Thus, any high shear mixer may be utilized in an open or closed system under am~ient conditions. Some increase in temperature as a conse~uence o~ the work performed will be experienced but generally normal heat 5 dissipation is readily achieved without cooling. Any mineral acid may be utilized such as hydrochloric, sul~uric or nitric acid ~ut hydrochloric is preferred for retention o~ ~avora~le color; phosphoric acid or other food acceptable acids are naturally pre~erred for 10 regulated app~ications. Generally a more concentrated acid source is desirable in the range of 2 to 3N but will ~p~n~ in part on the amount of material be~ng processed, and particle size.~ Typically, ~rom about 5 to a~out 10 parts of acid (calculated at 2N) are used 15 per 100 parts ~y weight of guar. tn selecting conditions it may be necessary to establish the leve~ of acid sensitivity of the guar gum source an~ this may be re~dily accompli sh~ by a test using different acid concentration, as shown in Example III.
In some ins~ances (relative to source o~ guar) it has been found convenient to utilize a small amount of alkanol in concert with the acid addition. This is understood to act essentially as a wetting agent facilitating access to the guar surfaces. Ethanol was 25 representatively employed ~ut any non-toxic straight chain or br~nche~ Cl-c~ alcohol could be used. For ~ood grade products, the use of ethanol is most preferred.
The processed guar is then treated at an 30 elevated temperature ~or a period o~ time to provide a product of selected viscosity when redispersed in an W O 97/25354 PCT~B95/01171 _ _9_ l aqueous medium. Thus, the material may be heat treated in a circulating oven for a period from one minute to several hours at a temperature of 30 to 180~C preferably 50 to 130~C. The time o~ treatment will ~p~n~ largely 5 upon the nature of the native guar gum with longer treatment times usually associated with higher v;~c~;ty materials. Generally, it is preferred to avoid hi gh~r temperatures conc~mitant however with reA~n~hle processing times.
Generally, treatment is contin~ for a period and under conditions to provide a product wh~ch when dried, then redispersed in ambient water at 1 percent concentration, will ev;~n~e a selected initial viscosity of from 0 to 2500 centipoise, prefera~ly from 15 0 to 1500 cps; and most preferably from 0 to 1000 cps.
It is often preferred to prepare a fully neutr~li 7PA
product and for this purpose one may employ an essentially equivalent amount of ~1 kA l; to neutralize the re~ Al acLd. In the case of a hatch operation and 20 for ready and rapid pro~C~;ng, it can be convenient to use a high shear mixer to facilitate this step. As with the acid treatment gradual addltion is preferahle to control exposure of the product to the A l kA l; . It has also been ~ound preferable to utilize the ~lk~l; in the 25 form of a caustic ethano~ic solution.
To provide the most uniform product in batch operations, lag time to neutralization ~hs~ e co~ tently maintained.
In some ciL~"~Lances, the level o~ re~;n~
30 moisture may be excessive relative to storage or use W O 97/25354 PCT~B95/01171 1 conditions in which event a further convective drying step may be suita~ly employed.
Tt is an important aspect of the present invention that low ash levels are realized in the 5 resulting product; usually less than 1.5% by weight and most often below 1 percent. Ash levels o~ from 0.5 to 1.00% are easily obtAin~. Also significant is the viscosity pro~ile of ~he product, that is, the controllahle v;~os~ty characteristic deve~oped by 10 varying the concentration over the range of about 0.75 to 1.5%, or by varying temperature of fo~mll~tion from 90~C. to re~rigeration storage conditions.
The functionally modi~ied guar of the present invention may he used alone or with other gums such as 15 locust bean gum, carrageenan, xa~than or tara gum, starch or gelatin in a wide variety o~ food products such as ice cream, pie f;lling5, icings and frostings, pet ~oods, ~rozen novelties, whipped torp; nq~, sour cream and yogurt products, s~ll~eC, cream soups, salad 20 dressings, cottage cheese dre~Q;ngs, egg substit~tes and dipping hatters. The product may also be derivatized where food accept~ble substituents are employed. The compositions may employ food acceptable salts of mono-, di- or trivalent cations, preservatives such as ~o~ m 25 benzoate, citric acid or sorbic acid, or ~on se~uestering agent such as citric, tartaric or orthophosphoric acids. The product may be dried and stored then, when converted to gel or sol form by hydration in cold or warm water ~y~ , the thi~o~Lo~ic 3o viscous col 10;~A1 disper~ion thus formed may be used directly in ~ood compositions. The viscosity developed .
-W O 97/25354 PCT~B95/01171 l is somewhat shear sensitive at low concentration and is dependent on temperature, concentration, pH, ionic strength as well as the induced agitation. Viscosities may be measured by a rotational, she~r type ~iscometer 5 capillary viscometer at low concentrations and extrusion rheometers at higher concentrations. Typically viscosity is measured by a Broo~ield RYT Viscometer (Broo~field Engineering Laboratories, Stou~hton, MA
02072) at 20 rpm using spindle 3.
While the process according to the invention may be understood to achieve a certain chain cleavage of the native guar galactnm~nn~n, it is believed without limitation that the ~avora~le characteristics att~; n~
in the resultant product both as to viscosity and shear 15 related properties under different conditions and cirCumst~n~e-c of use are a consequence in part of a certain selectivity in hydrolytic cleavage. It is believed that the processed product has shorter chain lengths which leads to avoidance o~ nn~irable 20 stringiness while ret~n;ng dietary fi~er ~roperties and some viscosity building characteristics.
In the following Examples all parts are by weight except where otherwise stated. Ash is det~rm~ne~
as set forth in The Food Chemical Codex 3d Ed ~1981) 25 P466, incorporated herein by reference.
CA 02242239 l998-07-03 W O 97/25354 PCT~B95/01171 1 E~UU~PLE 1 A. A~out 500 grams of Uniguar 80 (Rhone Poulenc Food Ingredients) native guar of initial viscosity 3075 cps (Brookfield RVF, Spindle 3, 20 rpm, 5 25~C) and 20 ml water was placed into a Cllisin~rt food processor, f~tted with a regular stee- cutting ~lade to a level of about 1/3 full and while the mixer was operating continuously, a volume o~ water (Control A) or 2N HCl ~ see Ta~le I below) was added gradually at a rate lO of about 5 ml/minute. Followin~ completion of addition, product which collected on the sides and bottom of the cont~;ner was scraped into the main mass, and the whole mixed for another 10 to 15 secondc be~ore collecting the product. The product was heated for one hour at 90~C.
15 in a convection oven and then characterized.
The viscosity of a 1% aqueous solution of samples of the processed material after hydration for 4 hours, the moisture level, p~ and the ash are set forth in Tahle I.
TABLE I
.x~ r~L Vl~Cu~l ~ pH MOISTOR~ ASH
(cp8) (%) (%) A 20 mL water 2477 5.38 9.2 0.76 B 10 mL HCl 2698 6.23 11 0.69 C 20 mL HCl 1637 4.75 11.~ 0.53 ~5 mL HCl 669 4.36 14 0.55 B. Additional samples of A, B, C and D were 30 then allowed to hydrate at 1% conc~ntration by weight in water under ambient conditions over two hours. The viscosity of the solutions were measured at 15 minutes, W O 97/25354 PCT~B95/01171 l 30 minutes, 60 minutes and 120 minutes. The results, plotting hydration time vs. viscosity are set forth in Figure 1. The viscosity profile generally provided an envelope of curves with similar viscosity develo~,~ ,L
5 from a ~ase line of lower viscosity for hiqh~r level of acid treatment.
C. Unigar ~O was treated ac in Sa~ple D
except that heating times at 90~C. were varied to study the e~fect on ~inal product. Product was treate~ with 10 35 ml 2n NaOH to neutralize be~ore performing the indicated tests. The resu~ts for samples heated for 6Q
minutes, 120 minutes and 180 minutes, are set forth in Table II together with ~nmr~ative properties o~
unprocessed guar products.
TABLB II
~V ~ ~ I ' L pH~ ~ ~ ~ K ASH
(Cp8) (%) (~) E 60 min heating 8255.45 17.2 0.67 F 120 nlin heating 275 5.28 17 0.62 G 180 min heating 50 5.25 15 0.75 Unigllar '303075 5.05 LO.8 0.52 As the above results indicate, increasing the heating period progressively decreases viscosity.
- 3~
W O 97/~5354 PCT~B95/01171 1 EXAMP~E II
Uniguar 80 was proc~cs~ in a similar m~nner to Example I, except that the acid component was 35 ml 2N HCL in 80~ ethanol.
Aliquots of resulting material were heated at 90~C in a convection oven for periods of 1, 2 and 3 hours, then neutralized under m; ~i n~ conditions with an equivalent ~..ou~ of caustic (NaOH) in 75~ ethanol. The results are set forth in Table III in ~mr~ri~on to 10 unprocesse~ and processed romm~cial guar pro~ucts. The tests were condu~ted as set ~orth in ~Amrle I. The viscosity was detPrmtned after 4 hours of hydration.
TABLE III
~ r ~ x I ~J p~
(cp~ (%) (%3 H (lh. 775 5.S9 8.8 0.80 heating) I (2h. 150 5.06 Ç.8 0.79 heating) 20 J (3h. no visc - - _ heating) K 3075 5.05 10.8 0.52 Uniguar The samp~c heat treated for three hours had essentiall~ no viscosity in water and was not further tested. The r~m~i n; ng samples showed r~ e~ vi-ecoe;ty and accepta~le ash levels.
W O 97/25354 PCT~B95N1171 _, A. 100 g of Dycol 4000 FC aV~ hl e from Rhone Poulenc Food Ingredients and having a viscosity of 4110 cps (Brookfield RVF, Spindle 3, 20 rpm, 25~) was 5 processed as set forth in Example I except that 7 ml o~
various concentrations of HCL in 80% ethanol were utilized, ranying from O.SN to 2.ON. Each of the samples was then heated in a 90~C oven f~r lS minutes.
Viscosity values after hydration at 1% f~r 2 hours are lO set forth in Table IV- Viscosity results for untreated and 5;m;1 ~r}y treated Uniguar 80 with 2N ~ICL is given for comparative purposes.
TABLE I~
CO~JC. HCl VT~t~C~ VT~ lY
(N) DYCOL 4000 FC UNIGUAR 80 (Cp8) (CpS~
MODIFIED GUAR, PREPARED BY HIGH SHEAR TREATMENT UNDER ACIDIC CONDITIONS AT ÉLE
VATED TEMPERATURE
FTELD OF T~E IN~N1iON
This invention reiates to the provision of 5 ~unctionally modified guar products and their u e, particularly in food grade applications. More particular}y, there is descri~ed an at least semi-continuous process for the treatment of suar particulate to provide a relatively hu~u~ eous, uniform, stable 10 product for application in the food industry, providing in a~ueous solution a re~ hlP v~c~-oc; ty under controlled condit~ons ~r~hl~ of efficient conversion into processing aids, thir~n~rs, hi nr~r~;, S~hi1; 7ers and ~ ~n~; ty b~ ~rS to ~m~nt food products such as c~ salad drec~i n7~ h~F~c~ and o7~ products, providing ~ u~ P texture and mouthfeel, among other desira~le organo~eptic properties. Moreover, the product as pro~C~A in accorda~ce with the inventive princ$ples more fully descrihed herein is free of unaccepta~le ash levels providing a visually and functionally attractive adiunctive agent in food use, to ~id in dispersion, gelation, moisture retention, preservation, stabilization or viscosity E~LLU1.
Additionally, the product provides a rich source of dietary fi~er without excessive viscosity as is evi~enoe~ with no~m~l, non-fu~ctinn~7 i ~ gu~r gum.
BA~ UND OF ~ NV~NllON
- Guar is derived ~rom the endosperm of the leg~min~ plant Cy~ ss tetra~onolobus (Llnue~ T~ub 3 or Cv~.,~is Psoraloides ~Lami) D.C. ~Fam. Le~mi nn~ 3;
W O 97/25354 - PCT~B95/01171 _. . = =
1 ft iS a high molerl~~r weight non-ionic l.y~lr~ oida poly5~r~h~idc, a galact~nn~n cn~ro-c~ of ~alactose and ~nnoqe units. Guar seeds comprise a seed coat or hull, a pair of tough endosperm sections, re~erred to as 5 'guar splits', which contain the gum and the ~L~yu. In prO~qc; n~, the hull is ~ ~d and the ~ nts separated ~y grin~ , st4t-ng and scr~enin~ in one or more stages. The splits are ~-o~u,d and prnc~seA to provide a gum or gum precursor.
The splits may ~e pro~c~A to recover .,ents thereof which may include all mem~rane, inorganic salts, and th~ pr~r~i n~nt gal aCt~Ann~, poly~r~hA-ide as well as ~ori~ted prot~in~r~o~s material and water insolu~le gels. The extraction has 15 typically ~een achieved by way o~ hydration and/or ~1~A1 ;n~ digestion or re~n;n~ y.~ eeC as repre~"L~~
by U.s. Patent No. 4,269,97~ to Nat;nn~7 Starch and Ch~i ~1 Corporation and U.S. Patent No- 4,659,811 to R~n~e~. In the f ormer, a hydrationfextrus~on operation 20 is said to proYide _ hi~h ~;C~t~cityr e.g. 5000 cps ~ine-y diYided, moisturized suar gum which could be dried and gro~n~ _or future use. The '811 patent tand cited references such as U.~. Patent No. ~06,327) recites the use of an A 1 ~ ~1; n~ m~ ~ at elevated 25 temperature to separate ~ y~ frcm ~yu and r~s~ husk. The pat~nt~ still employs upwards of 60 percent of water in the reaction mixture, and utiliz~s a pH above 12, with a ~;ni~-m of 150 parts ~y weight of aqueous ~ . ~he resulting wet c~ may be 3o partially neutr~ to a p~ below about 11, e.g., pH 9 ~Example 9).
3~
W O 97/25354 PCT~B95/01171 1 Other industrial processes have refined natural guar splitfi with acid solutions, heating the mixture, and then neutrAl; ~ng the acid with sodium hydroxide or another ~lkAli nP material. The resultant 5 product is a functionally modified guar controlled primarily by the pH and time of heat proc~cc;ng~
Neutralization by al k~31in~ treatment has ten-l~.l to result in a high ash content, vari~hi1;ty and other characteristics inconsistent with food ingredient use.
10 In these processes effects tend to be concentrated on the exterior portion of the endosperm le~i n~ to an irregular non-uniform product with differential levels of functional modification. The property of stringiness manifests itself in processed and dried guar qum 15 products and presents difficulties in food applications where smoothness, slipperiness or greasiness are important qualities to achieve or retain. While modification with ch~mio~l proc~ nq may min;~i~e this problem it is at~ended with the rea~y development o~
20 ash, rapidly approA~hin~ levels of 1.5~ or more, ~nArcepta~le for food use.
It is accordingly desirable to provide a process for the reftnPm~nt of natural guar products to afford a uniform, homogeneous particulate product 25 c~r~hle of forming aqueous solutions, pastes and gums of consistent, stable and r~ hl e low vi~s;ty and ash contents ~elow 1.5%, generally below 1.0~ for use in food product compositions of enh~nr~ aesthetic character including desirable th;ckf~n;ng and smooth~on~ ng properties with enh~nced mouthfeel in addition to other favorable organo1eptic properties.
W O 97/25354 PCT~B95/Q1171 _.
~4~
1 BRIEF SU~ RY OF ~ E IN~rE~rrION
T n accordanCe with the present invention r free-flowing particulate me~h~ni cally processed guar endo-~perm ic su~iected to a~ueous procec~; n~ under 5 acidic conditions with min~l a~ueous di7ution and hence controlted, limited hydration and relatively high shear tO produce a converted guar product of modified rheological characteristics.
More specifically, there is pro~ided a lO functionally modified guar product for food use, comprising low ashr a shorter te~Lu~ than co~,v~.-Lional guar products and elch ihi ting a novel low viscc~s'tty profile eSp~ci~lly at about 1% con~L.L~tion or less under conditions of conventi nn~l refri~eration r~nq-nq 15 to mildly elevated temperatures in food ~Tro~itions such as ~ eeC, salad dr~ssi n~c a~d the like.
These desira~le characterist-cs are achieved ~y su~jecting ~ree-~lowing guar endosperm part;c~7~te to high shear refining under controlled conditions of acid 20 hydration; the resultin~ product i5 then su~jected to a heat treatment under static or stirred conditions. The acid refining is effected so to control the amount of water av~ hl e for hydration relative to the con~entration of guar, i.e., at relatively high solids 25 level. The re~ining at high shear i5 maint~n~ for a period of time su~ficient to s~n;f;~ant7y reduce the viscosity of guar to levels in the r~nge of 0 to 2,S00 cps; preferab7y 0 to 1,500 cps; an~ most pre~era~y 0-l,OOQ cps. Many uses are found that uti~ize the lower 3o viscosities. The a~solute acid level ic relatively low in cnmr~ison to direct acid refining o~ whole hydrated W O 97/25354 PCT~B95/01171 1 guar splits as practiced in the art such that degradation leading to ash levels unacceptable in food use is controlled and minim;zed. Even at relatively low acid levels it may never~h~le~c be de~irahle to pro~ide 5 a fully neutralized product, hence for this purpose reaction with AlkA1i to effect neutralization may be employed to m;n;m; ze salt levels.
BRIEF DESCRIPTION OF TEE DRAWIN~S
10 Fig. I (Effect o~ Acid on Guar Modification) is a plot of Viscosity (cps) as the a~scissa and hydration time (minutes~ e~i~nc;n~ ch~ng~ in rheological characteri~tic in accordan~e with the invention.
D~.TAIT~D DESCRIPTION OF THE Ihv~NLlON
The native guar may be simply purified, i.e., split with hull removed or ~hnllP~ and screened one or more times to ~ ve detritus, and then y r ~u~d to a 20 particulate rauging from a coarse gr~nlllAr material to a fine powder. Coarser materials tend to ~;~p~rse more readi~y, whereas finer grinds are more rapidly hydrated.
The guar starting material employed is at least 66% galac~nm~nn~n and ~rh;~; ts cnmro!;;~;on~l 25 elements consistent with the Food Chemicals Codex 3d Ed.
(1981), p.1~1 incorporated herein by re_erence;
specifically after proce ~n~ it contains no more ash than eYcee~s 1 to 1.5~ by weight of the guar. Course gums p~.cc;ng through a 40 ~esh screen but min;m~lly through a lQ0 mesh screen; and fine gums ~f;n~ as those cont~;n;ng a pre~nm~n~nce of particles p~;n~
W O 97/253~4 PCT~B95/01171 1 through a 200 mesh screen, can be used to prepare a satisfactory product. It will be understood that sources of guar may be mixed such that a certain bimodal distri~ution may result, for example, where a coarse 5 grind and fine powder are used together.
Guar gums of varying initial v;~o~;ty, reflective of variations in molecular weight, cn~o~ition, and degree o~ br~nrhi n~ are readily av~ hl e, in the range of 1000 to 6000 cps measured as 10 a 1% solution (Broo~field RVF vi~m~ter, 5~;nAl~ 3 or 4, 20 rpm). While any guar gum starting material may be employed, Uniguar 40 av~ hle from Rhone Poulenc with a v~scosity of 2000 cps or Dycol 4000 FC, also available from Rhone Poulenc with a typical viscosity of 4000 cps 15 (both viscosities determ;nP~ as a 1% (w/w) solution using a Brookfield RVF viscometer (Spindle 3, 20 rpm) is preferred.
The guar is intro~ to a high shear m; ~; ng zone cont~; n; ng or to which is added an agueous acidic 20 medium with or without A~cohnl. Pre~erably, acid with a limited amount of water with or without alcohol is gradually added to the guar under condit~ons of high shear agitation. The rate of addition may be empirically se~ected to mi nim; ~e cll~mri n~ or the 25 formation of gummy particles and may be af~ected by the rate of shear or the advance of the material to be treated, all o~ which i5 easily de~m; n~l by one skilled in the art-By high shear mixing, it is inten~e~ to denote 3o a ~;~n~ process in a cont~;~PA zone ;n~ A;n~ stirringunder conditions to ef~ect in ad~acent zones o~ the --_ 1 substrate being wor~ed the application o~ differential forces, (as, differential velocity) between said zones, which may be in l~i n~r or tur~ulent flow. ~s is well known to those sk;l1e~ in these arts, the differential 5 forccs may be effected by the geometry of the stirring blade, the clea~ance of the ~lade ~er with the cont~; n~r or fixed or moveahle ohstructions in the cont~ne~ and the velocity of the stirrer, and will naturally be affected by the temperature o~ the system 10 relati~e to the viscosity characteristics o~ the stirred medium. Under conditions of high velocity, low clearances and~or high viscosit~, high shear miX; n~
expressed in units of reciprocal s~co~ is readily achieved.
The treatment regimen is selected to maintain a high solids system with mi n;mllm moisture level; in addition, the acid addition is adjusted to maintain p~
yet avoid undesira~le formation o~ ash from the action of ~ cs acid. For experimental purposes, a 20 prototypical~batch system employed a Cl~;sin~rt food processor with the basic cutting blade providing shear to the m~X;ng zone cont~'n;n~ about SOQ grams of guar gum granulate and acid (2N HCl 1:6 dilution o~ 12 N HCL
in ethanol) was added at a rate of about S mltmin~ to a 25 total of 10 to 35 ml with continuous mixin~; after the completion o~ acid addition, the system was agitated for another 10 to 15 s~con~. Conditionc for larger semi-continuous and continuous systems may ~e adapted consistently within the knowledge of one skilled in the art.
1 Thus, any high shear mixer may be utilized in an open or closed system under am~ient conditions. Some increase in temperature as a conse~uence o~ the work performed will be experienced but generally normal heat 5 dissipation is readily achieved without cooling. Any mineral acid may be utilized such as hydrochloric, sul~uric or nitric acid ~ut hydrochloric is preferred for retention o~ ~avora~le color; phosphoric acid or other food acceptable acids are naturally pre~erred for 10 regulated app~ications. Generally a more concentrated acid source is desirable in the range of 2 to 3N but will ~p~n~ in part on the amount of material be~ng processed, and particle size.~ Typically, ~rom about 5 to a~out 10 parts of acid (calculated at 2N) are used 15 per 100 parts ~y weight of guar. tn selecting conditions it may be necessary to establish the leve~ of acid sensitivity of the guar gum source an~ this may be re~dily accompli sh~ by a test using different acid concentration, as shown in Example III.
In some ins~ances (relative to source o~ guar) it has been found convenient to utilize a small amount of alkanol in concert with the acid addition. This is understood to act essentially as a wetting agent facilitating access to the guar surfaces. Ethanol was 25 representatively employed ~ut any non-toxic straight chain or br~nche~ Cl-c~ alcohol could be used. For ~ood grade products, the use of ethanol is most preferred.
The processed guar is then treated at an 30 elevated temperature ~or a period o~ time to provide a product of selected viscosity when redispersed in an W O 97/25354 PCT~B95/01171 _ _9_ l aqueous medium. Thus, the material may be heat treated in a circulating oven for a period from one minute to several hours at a temperature of 30 to 180~C preferably 50 to 130~C. The time o~ treatment will ~p~n~ largely 5 upon the nature of the native guar gum with longer treatment times usually associated with higher v;~c~;ty materials. Generally, it is preferred to avoid hi gh~r temperatures conc~mitant however with reA~n~hle processing times.
Generally, treatment is contin~ for a period and under conditions to provide a product wh~ch when dried, then redispersed in ambient water at 1 percent concentration, will ev;~n~e a selected initial viscosity of from 0 to 2500 centipoise, prefera~ly from 15 0 to 1500 cps; and most preferably from 0 to 1000 cps.
It is often preferred to prepare a fully neutr~li 7PA
product and for this purpose one may employ an essentially equivalent amount of ~1 kA l; to neutralize the re~ Al acLd. In the case of a hatch operation and 20 for ready and rapid pro~C~;ng, it can be convenient to use a high shear mixer to facilitate this step. As with the acid treatment gradual addltion is preferahle to control exposure of the product to the A l kA l; . It has also been ~ound preferable to utilize the ~lk~l; in the 25 form of a caustic ethano~ic solution.
To provide the most uniform product in batch operations, lag time to neutralization ~hs~ e co~ tently maintained.
In some ciL~"~Lances, the level o~ re~;n~
30 moisture may be excessive relative to storage or use W O 97/25354 PCT~B95/01171 1 conditions in which event a further convective drying step may be suita~ly employed.
Tt is an important aspect of the present invention that low ash levels are realized in the 5 resulting product; usually less than 1.5% by weight and most often below 1 percent. Ash levels o~ from 0.5 to 1.00% are easily obtAin~. Also significant is the viscosity pro~ile of ~he product, that is, the controllahle v;~os~ty characteristic deve~oped by 10 varying the concentration over the range of about 0.75 to 1.5%, or by varying temperature of fo~mll~tion from 90~C. to re~rigeration storage conditions.
The functionally modi~ied guar of the present invention may he used alone or with other gums such as 15 locust bean gum, carrageenan, xa~than or tara gum, starch or gelatin in a wide variety o~ food products such as ice cream, pie f;lling5, icings and frostings, pet ~oods, ~rozen novelties, whipped torp; nq~, sour cream and yogurt products, s~ll~eC, cream soups, salad 20 dressings, cottage cheese dre~Q;ngs, egg substit~tes and dipping hatters. The product may also be derivatized where food accept~ble substituents are employed. The compositions may employ food acceptable salts of mono-, di- or trivalent cations, preservatives such as ~o~ m 25 benzoate, citric acid or sorbic acid, or ~on se~uestering agent such as citric, tartaric or orthophosphoric acids. The product may be dried and stored then, when converted to gel or sol form by hydration in cold or warm water ~y~ , the thi~o~Lo~ic 3o viscous col 10;~A1 disper~ion thus formed may be used directly in ~ood compositions. The viscosity developed .
-W O 97/25354 PCT~B95/01171 l is somewhat shear sensitive at low concentration and is dependent on temperature, concentration, pH, ionic strength as well as the induced agitation. Viscosities may be measured by a rotational, she~r type ~iscometer 5 capillary viscometer at low concentrations and extrusion rheometers at higher concentrations. Typically viscosity is measured by a Broo~ield RYT Viscometer (Broo~field Engineering Laboratories, Stou~hton, MA
02072) at 20 rpm using spindle 3.
While the process according to the invention may be understood to achieve a certain chain cleavage of the native guar galactnm~nn~n, it is believed without limitation that the ~avora~le characteristics att~; n~
in the resultant product both as to viscosity and shear 15 related properties under different conditions and cirCumst~n~e-c of use are a consequence in part of a certain selectivity in hydrolytic cleavage. It is believed that the processed product has shorter chain lengths which leads to avoidance o~ nn~irable 20 stringiness while ret~n;ng dietary fi~er ~roperties and some viscosity building characteristics.
In the following Examples all parts are by weight except where otherwise stated. Ash is det~rm~ne~
as set forth in The Food Chemical Codex 3d Ed ~1981) 25 P466, incorporated herein by reference.
CA 02242239 l998-07-03 W O 97/25354 PCT~B95/01171 1 E~UU~PLE 1 A. A~out 500 grams of Uniguar 80 (Rhone Poulenc Food Ingredients) native guar of initial viscosity 3075 cps (Brookfield RVF, Spindle 3, 20 rpm, 5 25~C) and 20 ml water was placed into a Cllisin~rt food processor, f~tted with a regular stee- cutting ~lade to a level of about 1/3 full and while the mixer was operating continuously, a volume o~ water (Control A) or 2N HCl ~ see Ta~le I below) was added gradually at a rate lO of about 5 ml/minute. Followin~ completion of addition, product which collected on the sides and bottom of the cont~;ner was scraped into the main mass, and the whole mixed for another 10 to 15 secondc be~ore collecting the product. The product was heated for one hour at 90~C.
15 in a convection oven and then characterized.
The viscosity of a 1% aqueous solution of samples of the processed material after hydration for 4 hours, the moisture level, p~ and the ash are set forth in Tahle I.
TABLE I
.x~ r~L Vl~Cu~l ~ pH MOISTOR~ ASH
(cp8) (%) (%) A 20 mL water 2477 5.38 9.2 0.76 B 10 mL HCl 2698 6.23 11 0.69 C 20 mL HCl 1637 4.75 11.~ 0.53 ~5 mL HCl 669 4.36 14 0.55 B. Additional samples of A, B, C and D were 30 then allowed to hydrate at 1% conc~ntration by weight in water under ambient conditions over two hours. The viscosity of the solutions were measured at 15 minutes, W O 97/25354 PCT~B95/01171 l 30 minutes, 60 minutes and 120 minutes. The results, plotting hydration time vs. viscosity are set forth in Figure 1. The viscosity profile generally provided an envelope of curves with similar viscosity develo~,~ ,L
5 from a ~ase line of lower viscosity for hiqh~r level of acid treatment.
C. Unigar ~O was treated ac in Sa~ple D
except that heating times at 90~C. were varied to study the e~fect on ~inal product. Product was treate~ with 10 35 ml 2n NaOH to neutralize be~ore performing the indicated tests. The resu~ts for samples heated for 6Q
minutes, 120 minutes and 180 minutes, are set forth in Table II together with ~nmr~ative properties o~
unprocessed guar products.
TABLB II
~V ~ ~ I ' L pH~ ~ ~ ~ K ASH
(Cp8) (%) (~) E 60 min heating 8255.45 17.2 0.67 F 120 nlin heating 275 5.28 17 0.62 G 180 min heating 50 5.25 15 0.75 Unigllar '303075 5.05 LO.8 0.52 As the above results indicate, increasing the heating period progressively decreases viscosity.
- 3~
W O 97/~5354 PCT~B95/01171 1 EXAMP~E II
Uniguar 80 was proc~cs~ in a similar m~nner to Example I, except that the acid component was 35 ml 2N HCL in 80~ ethanol.
Aliquots of resulting material were heated at 90~C in a convection oven for periods of 1, 2 and 3 hours, then neutralized under m; ~i n~ conditions with an equivalent ~..ou~ of caustic (NaOH) in 75~ ethanol. The results are set forth in Table III in ~mr~ri~on to 10 unprocesse~ and processed romm~cial guar pro~ucts. The tests were condu~ted as set ~orth in ~Amrle I. The viscosity was detPrmtned after 4 hours of hydration.
TABLE III
~ r ~ x I ~J p~
(cp~ (%) (%3 H (lh. 775 5.S9 8.8 0.80 heating) I (2h. 150 5.06 Ç.8 0.79 heating) 20 J (3h. no visc - - _ heating) K 3075 5.05 10.8 0.52 Uniguar The samp~c heat treated for three hours had essentiall~ no viscosity in water and was not further tested. The r~m~i n; ng samples showed r~ e~ vi-ecoe;ty and accepta~le ash levels.
W O 97/25354 PCT~B95N1171 _, A. 100 g of Dycol 4000 FC aV~ hl e from Rhone Poulenc Food Ingredients and having a viscosity of 4110 cps (Brookfield RVF, Spindle 3, 20 rpm, 25~) was 5 processed as set forth in Example I except that 7 ml o~
various concentrations of HCL in 80% ethanol were utilized, ranying from O.SN to 2.ON. Each of the samples was then heated in a 90~C oven f~r lS minutes.
Viscosity values after hydration at 1% f~r 2 hours are lO set forth in Table IV- Viscosity results for untreated and 5;m;1 ~r}y treated Uniguar 80 with 2N ~ICL is given for comparative purposes.
TABLE I~
CO~JC. HCl VT~t~C~ VT~ lY
(N) DYCOL 4000 FC UNIGUAR 80 (Cp8) (CpS~
0.5 3460 B. In the same mAnner four, 100 g portions of Dycol 4000 FC were processed each with 7 ml of 1 ~ HCl in 80% ethanol, incu~ated at 90~c for 75 minutes in a 25 convection oven and neutralized in the processor with 11 ml of 1 N NaOH in 80% ethanol. These samples were dried for 5 days at 21~C. and analyzed. The results are set forth in Table V as follows:
3~
CA 02242239 l998-07-03 W O 97/2~354 PCT~B95/01171 _.
TP;BLE V
SANPLFVlS~Sl ~ pH ~.Jl~K~ ASH
(cp8) (%) (%) Sample 1 925 6.50 8.4 0.7fi Sample 2 1025 6.58 8.0 0.71 Sample 3 1200 6.60 7.8 0.72 Sample 4 l375 6.71 8.6 0.73 Dycol 4000 4225 5.58 9.2 0.49 FC
The viscosity variance (925-137~ cps) is believed to be due to the lag time at t~r~ratures above ambient before the neutralization step occurred. Ash levels are all within accepta~le limits.
CA 02242239 l998-07-03 W O 97/2~354 PCT~B95/01171 _.
TP;BLE V
SANPLFVlS~Sl ~ pH ~.Jl~K~ ASH
(cp8) (%) (%) Sample 1 925 6.50 8.4 0.7fi Sample 2 1025 6.58 8.0 0.71 Sample 3 1200 6.60 7.8 0.72 Sample 4 l375 6.71 8.6 0.73 Dycol 4000 4225 5.58 9.2 0.49 FC
The viscosity variance (925-137~ cps) is believed to be due to the lag time at t~r~ratures above ambient before the neutralization step occurred. Ash levels are all within accepta~le limits.
Claims (15)
1. A method for processing guar gum to a reduced viscosity product of low ash content comprising treating particulate guar gum with aqueous acid or aqueous acid containing non-toxic straight chain or branched C1 - C4 alcohol under conditions of high shear, heating the acid-treated guar at elevated temperature for a period sufficient to reduce the viscosity and optionally neutralizing the product.
2. The method of Claim 1, wherein the moisture content of the guar during treatment with said acid is not in excess of 25%.
3. The method of Claim 1, wherein the acid is added incrementally to the particulate guar in the presence of 1 to 15 parts by weight of water per 100 parts of guar.
4. The method of Claim 1 wherein 1 to 15 parts by weight of 0.1 to 3N acid is added gradually to 100 parts by weight of guar at a rate of between about 1 and 15 parts acid per minute.
5. The method of Claim 1 wherein the guar has a particle size of between about 20 and 400 mesh.
6. The method of Claim 5 wherein 80% of the guar has a particle size within the range of 80 and 200 mesh.
7. The method of Claim 1 wherein the product is neutralized with alkali under conditions of high shear.
8. A method for preparing processed guar comprising:
(1) incrementally introducing an acid solution either aqueous or aqueous ethanolic to particulate guar in a high shear mixing zone in an amount and at a rate insufficient to cause clumping or the formation of gummy particles;
(2) heating the resulting admixture to a material temperature of between about 50 and 130°C for a period of time from about 5 min. to about 3 hours sufficient to effect at least partial depolymerization of the guar;
(3) incrementally introducing an alkaline solution to the partially depolymerized guar under conditions of high shear mixing to provide an essentially neutralized product relative to the acid supplied in the first stage; and (4) optionally heating the thus treated product at an elevated temperature to remove moisture therefrom.
(1) incrementally introducing an acid solution either aqueous or aqueous ethanolic to particulate guar in a high shear mixing zone in an amount and at a rate insufficient to cause clumping or the formation of gummy particles;
(2) heating the resulting admixture to a material temperature of between about 50 and 130°C for a period of time from about 5 min. to about 3 hours sufficient to effect at least partial depolymerization of the guar;
(3) incrementally introducing an alkaline solution to the partially depolymerized guar under conditions of high shear mixing to provide an essentially neutralized product relative to the acid supplied in the first stage; and (4) optionally heating the thus treated product at an elevated temperature to remove moisture therefrom.
9. Food grade particulate guar having a uniform low ash and a viscosity profile in aqueous solution affording a smooth textural quality to food products thickened or stabilized thereby prepared by the method of Claim 1.
10. A method of preparing sauces, pastes, gels, or gums for food use comprising incorporating a stabilizing, thickening or otherwise functional amount of the processed guar of Claim 9 in a food composition suitable therefore.
11. A viscous aqueous solution comprising guar processed in accordance with Claim 1.
12. A food composition of enhanced textural qualities comprising at least one edible food having a pourable or spreadable consistency comprising guar processed in accordance with Claim 1.
13. Viscous, creamy, gelled, or frozen food products modified with the processed guar of Claim 1.
14. Functionally modified particulate guar predominately having a molecular weight of 20,000 to 500,000, a particle size of 20 to 400 mesh, a viscosity in dispersed 1% aqueous solution in the range of 0 to 1500 cps and a viscosity variability of less than 20%.
15. Guar modified viscous creamy or frozen food products having a uniform, smooth, textural mouthfeel comprising the processed guar of Claim 1.
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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PCT/IB1995/001171 WO1997025354A1 (en) | 1996-01-05 | 1996-01-05 | Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature |
BR9510685A BR9510685A (en) | 1996-01-05 | 1996-01-05 | Modified guar prepared by high shear treatment under acidic conditions at elevated temperature |
EP95944707A EP0871674A1 (en) | 1996-01-05 | 1996-01-05 | Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature |
CA002242239A CA2242239A1 (en) | 1996-01-05 | 1996-01-05 | Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature |
AU48404/96A AU4840496A (en) | 1996-01-05 | 1996-03-20 | Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature |
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PCT/IB1995/001171 WO1997025354A1 (en) | 1996-01-05 | 1996-01-05 | Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature |
CA002242239A CA2242239A1 (en) | 1996-01-05 | 1996-01-05 | Modified guar, prepared by high shear treatment under acidic conditions at elevated temperature |
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AU (1) | AU4840496A (en) |
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---|---|---|---|---|
US3346556A (en) * | 1965-10-14 | 1967-10-10 | Marine Colloids Inc | Treatment of manno galactan gums |
JP2593724B2 (en) * | 1990-04-04 | 1997-03-26 | 明治製菓株式会社 | Method for producing low-viscosity indigestible polysaccharide and food containing it |
DE4137237A1 (en) * | 1991-11-13 | 1993-05-19 | Gruenau Gmbh Chem Fab | CONTINUOUS METHOD FOR DEGRADING HETEROPOLYSACCHARIDES |
AU3594893A (en) * | 1992-01-31 | 1993-09-01 | Dow Chemical Company, The | Process for reducing the viscosity of natural carbohydrate gums |
DE4344156A1 (en) * | 1993-12-23 | 1995-06-29 | Gruenau Gmbh Chem Fab | Process for the degradation of polygalactomannans |
-
1996
- 1996-01-05 CA CA002242239A patent/CA2242239A1/en not_active Abandoned
- 1996-01-05 WO PCT/IB1995/001171 patent/WO1997025354A1/en not_active Application Discontinuation
- 1996-01-05 EP EP95944707A patent/EP0871674A1/en not_active Ceased
- 1996-03-20 AU AU48404/96A patent/AU4840496A/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
AU4840496A (en) | 1997-08-01 |
EP0871674A1 (en) | 1998-10-21 |
WO1997025354A1 (en) | 1997-07-17 |
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