CA1180250A - Polyglycerol ester emulsion gel concentrates - Google Patents

Abstract

ABSTRACT

Polyglycerol esters are made readily dilutable with fats or oils and/or water using simple mixing techniques by first forming an alpha crystalline gel concentrate of the ester, fat or oil, and water. The concentrates are stable for prolonged periods and even when diluted with fat, oil or water, remain stable. The concentrates also exhibit markedly enhanced functionally in end use applications.

Description

5~) 20071 POL~Gl.YCEKOI ES~ E~I~SION CEL CONC~NT~AT~

The prese.nt inv~ntion relates to novel polyglycerol ester con-taining water es~llsion concentra~es and method for n~ing the same. For purposes of the pre~ent application, the term "concentrate" m~ans an ernulsion having a ~ter concentration of less t~n 80% based on the total weight o~ the emulsion. A minina~l water conten~ of at least 5Z, based on the weight of the emulsi~n, is required.
In particular, the polyglycerol es~er emulsion concentrates of the present invention are characterized as alpha crystallLne ge~s at room temperature. As such, they remain stable as alpha crystalline gels for prolon~ed periods of time, retain a hi~h degree of ac~ivity for such periods? and cfln readily be further diluted with either pha~e of t.he emulsion, that is with oll, ~æt or water, by the use of simple mix m g procedures.
By "activity" it is m~an~ the degree of fwnctionality of the polyglycerol ester in food and cosmetic applications, prln~rily with regard to aeration e~pabil~ty, textwre improvem~nt and dlspersion of fat~.
BAC~GRO~l~D OF ~ E PI~ESE~l` INV~rION
Polyglycexol ester~ o~ high~r Eatty aclds are not normally ~at or 2Q otl dispersib:le ~ven though they provide a ~arkecl interface mDcliylng pow~r ~hen elllpl~yed a~ ~prov~.ng agents ~n ~atty n~t~rials. l~is is pointPcl out in the ~ei5s pat~l~ No. 3~3~,090~ eh indicates that when the poly ~lycerol e~ter~ axe added to ats in mel~ed condition during shortening m~n~actl~e, the e~ters are t distributed throu~hout ~he fat, but tend to settle out as a tarry residue, sti~king to the walls of containers, pipe~
and other equipn~ . This disadvant~ge ~as overco~e in -the Weiss pat~nt ~y uslng a coupling agPnt such as propyl~ne glycol ~ith the pol~glycerol ester.
Even in the pxe~ence of water, or with a couplin~ agent such as proplyene glycol, heating to elevated temperature and intensive mixi.ng are usually required -to form polyglycerol ester containing emulsions.
Also there ;.s a tendency for mix-tures containi.ng water and polyglycerol esters to be metastable. The emulsions can be characteri.zed as exist--ing in a lattice structure with water sandwiched between the polygly-cerol ester hydrocarbon chains. Over a period oE time the water can be expelled, and when this occurs the emulsion is transformed into a microcrystalline suspens:ion o:E emulsifier in water, re:Eerred to as a cogel. In the cogel form~ the polyglycerol esters clemonstrate a much more reduced activity than might be expected.
In the manufacture of many consumer items~ for instance bread doughs, icings, non-dairy toppings, :Eace creams, and other such appli-catlons where polyglycerol esters are used, it would be advantageous for the end user to be able to simply blend the polyglycerol esters with fat, oil, or other lipid, and addi-tional water, by simple mixing without complicated processi.ng. However, because o:E the above in-stability, thi.s is usually not possible.
It is ~nown that emulsi:Ei.ers can be mixed with water and pro-cessed to form a stable gel structure wh:ich retains activi-ty Eor pro-

2~ longed periods. This is discussed :in Sritish pat.en-t No. 1,501~106~
with regard to C~ C~ mono- di.glycerides. It -is pointed out in the patent that when simple mo~oglycericlR composi-tions havc to be dis-persed in water~ the monoglyceride-water mixtures must, in general, be heated above the chain-melting temperature of the monoglyceride (Krafft point, Tc). This results in a formation of a liquid crys~al-line dispersion with a high degree of activity. ~hen such dispersions are cooled to be:low approximately ~10C they transform to gels with a similar hi.gh clegree o activity. IZoweverJ i.n a short space o:E time, the gels tend to revert -to crystalline cogels with poor activity. To reactivate such cogels i.t is necessary to redisperse the system at temperatures above the Kra:Eft point.

'`i,l-`~
,~

In the British patent, it was found that addition of an anionic surfactant ~e.g. soap) prevented the reversion to a crystalline-cogel state.
The patent makes no mention of polyglycerol esters or emulsions containing the same.
The publication Food Emulsions, edited by Marcel Dekker, 1976, on pages 96 and 97, discloses that tetraglycerol esters ~a polyglycerol ester) may be mixed with water and heated to above the Krafft point. Then, when cooled below the KrafEt polnt, the tetraglycerol ester formed a gel phase with water, said to be useful in the baking industry. No reference was made in this publication to forming gel concentrates having increased stability and activity and capable of being diluted with water and/or fat or oil by simple mixing.
BRIEF DESCRIPTION OF THE PRESENT INVENTION
The present invention resides in the discovery that a stable polyglycerol esteT containing water/oil emulsion concentrate suitable for dilution with additional oil or water or bo-th by simple mixing~ the water content being at least 5% by weight of the concentrate but less than ~0%, the ratio by weight of oil to polyglycerol ester being in the range of abou-t 1:10 to about 10:1, the proportions of ingredients being those necessary to form the alpha crystalLine gel structure, can be made `by a process compris-ing the steps of mixing said water, oil and polyg:lycerol ester and hea*ing the same to abo-~e the Krafft point ~Tc~ o~ -th~ concentrate to form a liquid crystalline disperslon; and cooling said dispersion to 5-10F below the Krafft point ~Tc) of the concentrate to form an alpha crystalline gel structure.
The concentrate on cooling below the Krafft point, which is necessary to form a stable alpha crystalline gel, is stable for prolonged i periods of 12-18 months J or longer.
The present invention also resides in the product of the above process, namely a stable polyglycerol ester-containing water/oil emulsion concentrate suitable for dilution with additional oi.l or water or both by simple mixing, consisting essentially o:t polyglycerol ester, oil, and water in the proportion based on the weight of the concentrate of at least about 5% water, but less than 80%, the ratio of oil to polyglycerol ester being in the range of about 1:10 to about 10:1, the concentrate being an alpha crystalline gel.
Preferably9 the polyglycerol ester-containing emulsion concentrate of the present inventi.on is subjected to high shear mixing or homogeniæa-tion subsequent to mixing to produce a particle size of the cooled con-centrate, less than about 1-2 microns.
Preferably, the polyglycerol ester of the present invention has an HLB value o:F more than about 5.
Advantages of the present invention are that the emulsion con-centrate can be shipped to an end user and -then simply blended with add-itional fat or oil, and/or water~ depencling upon applicat:lon, by simple mixing procedures not requiring heating or homogeniæation. Subsequent to such blending or dilution, the emulsions continue -to sllow excellent s-tabil-ity :~or prolonged periods.
~ or :final use~ the emulsi:fier concentra-te exhib:its excellen-t activity. Shlpping can bc carried out wi-th a minlm~ml of water conten~.
The present invention llas many applications embracing all of those where polyglycerol esters may be used, for instance including non-dairy applications such as toppings and imitat.i.on cheese; iclngs or fillings;
and face creams and other cosmetics, drugs, and coffee whiteners.

5~

The present inven-tion therefore also provides a food, drug or cosmetic prodwct containing the concentrate prepared by diluting said concentrate by simple ml~ing witll additional ingredients including oil or water, or both oil and water, the concentrate providing a high degree of activity and stabili-ty.
DETAILED DESCRIPTION OF TIIE PRESENT INVENTION
The emulsions of the present invention are alpha crystalline gels as distinguished from hydrates or cogels.
In the text Food Emlllsions, mentioned above, on pages 83 and 84 it is indicated that certain polar surEactan-ts in the solid crystalline form (before addition of water) are oriented wi-th the polar groups against each other ancl the lipophilic hydrocarbon chains parallel and densely packed.
As water is introduced and the temperature is increasecl to the Kra~Et temp-erature, Tc, ~temperature at which the hydrocarbons transform to -the liquid state) the hydrocarbon chains become less rigid and the water penetrates between the polar layers. Thls is known as a liquld crystalline mesophase of the lamellar type. As the mesophase cools below Tc, the - 4a -~ ~ 5~ 11 20071 hydrocarbon chams crystalllze into a regular lattice structure. I~e water may still remain between the pol~r groups forming a serni-rigid "gel".
~lowever, S~U~I gels are normally n~tas~able, eventually changing by a reduction of t~e water layer. ~hen all th~ water is e~pelled~ the gel phase is trans~ormed into a micro-crys~alline suspension of the emulsifier in ~ater. Ihe so-called hydrate form of emulsifiers are predomil~tely in the cogel form. However, depending upon tempera~ure, concentration, and chemical configuration of the sur~actarlt, it was found that certain non-pol~norphic emulsi~iers were alpha~ ding and associa~ed with water ~o form stable cry~alline gel structures~ rDhey tended to func~ion more like ~ats ~i~:h little or no polymorphic activity. Speci~ic exL~mples cited in the text Food ~Dulsions, pages 67-135~ are stearoyl lactylates and poly-sorbates. Also, reference again can be had to British patent No. 1,501,106, mentioned abave with rega~d to ~onoglyceride emwlsions containing an ionic surfactantO
The existance o an alpha crystalline gel structure can be observed vls~ally as being very smooth and homogeneous in ~ppear~nce. By contras~, a gel struc~ure which i8 not an alpha crys~alline gel ls granier in appearance and will tend to destabilize and e~hihit at least 9c~e water separation.
Under a Bausch and L~b polariæed lig~lt mic-roscope using a ~ wav~
length ~iltar ecruipped with a ~bttler ~P52 heat~n~ and cooling stage ~to control ~h~ temperature of the specimen being observed) ancl at 250-600~
pow~r, the unique structure of an al-pha crystalline gel becomes even more ¦ dramatic, llle gel has a long randon needle-like structure as contrasted with a ti~ht sphere-like structure for conventional gels.
'l~e pres~nt invention resides in part in the discovery that certain polyglycerol esters, depending upon confi~uration and concentration of ingredients in the emulsion~ are capable of on~lng with an oil or ~at and water alld alpha crystalline gel concentrate when heated to ab~ve the lli~V;~50 Krafft point of the concentra~e ~nd then coolecl. The polyglycerol esters useful in the presen~ invention are ~phiphilic m character and are those having an ~LB value above five (5~.
The polyglycerol esters are higher fatty acid ester~ of poly-glycerols havlng several glycerol radicals and can be prepared by poly-merizing glycerol in the presence of alkali to fonm a mi~ture of glycerol9 diglycerol, triglycerol, tetraglycerol, pe~taglycerol, etc., up to and including decaglycerol. The poly~lycerol ~xture is then reacted ~ith higher fatty acid~ m an e~teriflcation process or is ca-taly~ically inter-esterified with triglyceride such ~s the naturally occurring fats a~d oils to produce nixed esters of polyglycerols wlth the fatty acyl gro~ps being randomly distributed on indivldual glycerol radicals. In addition to an ~L6 above about five (5)~ the polyglycerol esters useful in the present lnvention are the polyglycerol esters of higher fatty acidæ having 2-10 glycerol units, preferably 2~8 glycerol units. The acyl components preferably are esters of fatty acids of 10-22 carbons. Polyglycerol esters conta~n~ng ~3S the ~tty acyl conponent ~atty acids and ~xed ~atty acid~ derivecl frc~
ar~mal, vegetRble and n~rlne triglycerides, are convenientl~ prepared by e~terifying cottonseed fat~y acicl~ ~o~bean att~ acid~, pean~lt oil fat~y acid~, tallQw a~ty acids, etc. with pol~glycerol ~r by int~rester~fying the nat~al t~iglycerlde wl~h poly~lycerol.
Examples o~ ~peci~c polyglycerol cst~rs within the scope o~ the pres~lt ln~ention are triglycerol ~ono~teara~e; tr~glycerol monoshortening;
tetraglycerol ~nnostearate; h~x~glycerol di~te~rate; octaglycerol no steara~e; oc~aglycerol ~onDol~ate; and decaglycerol distearate.
The fat or oil compQnent o.~ ~he prese~t invention broadly can be any oil or fat which is v~getable or anin~l derlvPd. Preferred oils or ~a~s3 ho~ever, are those h~ving a ~lley ~ ng Point in the rc~nge of about 35-120F. O~her ~h~n the ~bove ~w~ requiren~nts, the particulc~r fat or oil employed depe~d~ upon the end u~e or applleation involved.

118~ 50 20071 For instance, a cake system will typically use a partially hydrogenated soybe~n fa~ in liq~Lid form havin~ a Wiley Meltu ~ Point of about 65F. An ex~mple of 5uch an oil is D~lrkex 100 (traden~rk) marketed by SCM Corporation, having an IV of abou~ 95. On the o-~her hand, an end use such a~ an icing may typically u~e a plastic hydrogenated veg~table f.at tsoybean, palm or cottonseed) haviu~ a Wiley Melting Point of about 111-119F, one such fat being marketed by SCM Corporaticn as a shortening under the traden~rk Crea~ex (IV about 70)~ A viscous cream filling will use a partially hydrogenated vegetable oil (cottonseed or soybean~ such as Duromel (trade~ark, SCM Cor~)ora~ion) h~ving a Wiley Melting Po m~ of abo~L
101-105F, ~nd an ~FI of 56 at 50F; 43 at 70F; 36 a~ 80F/ 16 at 92F and 4 at 100F~ A suitable fat for an alcoholic beverage mix may be corn oil haying an IV o 120-140. Corn oll w~uld also be u~eful for filled ~lk I phaImaceutical products or drug delivery ~intravenous) feedLng systens.
Finally, a face cream type of product may u3e a nuneral oil ~e.g. Nujol, a mQxture oE liquid hydrocarbons fron petrole~n). Again, ~he particular ~at or oil employed depends upon end use or application and its selection w~uld be within the skill of those in the art.
The proportions o~ ingredie~s ln the en~l~ion conce~ra~e~ o the presen~ in~entlon are crltical~ At least 5% wa~er must be presen~, al-~hou~h t~la wa~er content should not be above abo~t ~OZ, based on the ~o~al ~ei~ht o~ tha emulsion conc~n~rate.
~e ratio o.~ ~at or oil ~o polyglycerol e~ter should be more than about 1:10 and le~ ~han about lOsl.
With m the above constraints, ~he proportions sh~uld be those necessary to fonm the alpha crystalline ~el structure. For inst~nce, depending upon relative proportions of polyglycerol eæ~er, fat or oil, and ~ater, the gel which i8 ~ormed ~ay or may not be alpha crystallin~, For ins~ance, optimun stability, activity and formativn of an alpha crystalline ~el structure ls obtained with the polyglycerol ester SanLone 3 1 SH

~ Wil~y ~bl~in~ Po~nt about 3SF.

~ 31J ~ 5 ~

20071 (triglycerol ~onoshortening, trade~ark SCM Corporation) by using about 10%
polyglycerol ester, about 60% water and about 30% Eat. At proportions of abowt 10% ester, less than 30% water and more than 60% fat, no stable alpha crystalline struct~lre is obtained. Similarly, with the polyglycerol ester San~one 8-l S, the concentrate of the present invention exhi~its optimum activity and stability in the relative proportion of 10% ester, 45~ water and 45% fat~ At a proportion of more than 30% ester, regardless of fat and water content, no stable alpha crystallin~ structure is obtained.
In the practice of the present invention, the respective in-gredients are nuxed together at an elev~ted temperature above the Krafft Ten~erature (Tc) for the concentrate, preferably that temperature at whlch the lipid ingredients are l-ten. The follownng table gives the Krafft Tem~erature for several concentrate examples.
TABLE I
Optin~n concentrations for Concentrate Krafft Te~perature EhlulsiEier ~e~ c ~ TeL~ }~ ne~5

3-l-SH 10:60:30 about 32C (90F) Caprol 3GVS
(triglycerol, mono-shorterling, traden~ark Capitcll Cities~ lO:3Q:60 about 38C (100F) Sarltone 8-1-0 (octaglycerol mon~oleate~
~5 trademarlc SCM Corporation) 30:50:~0: about 10C (50F) San~on~ S
(octc~lycerol monostearate, tra~le~a-rk SCM Corporation)) 10:45:45 about 45C (113F) Follo~ing mixing and prior to cooling, the concentrate is subjected to homogenization if a fine particle size is desired. HomDgenization pressures employed follow conv~ntional dairy practice. Hcmogenization pressures o~ 2500:500 in a two-stage homogenizer give a particle size of less thc~ 1-2 ~icrons, in st cases.
No particular cooling proc~dure need be ~ollowed in cooling the concentrates Qf the present inven~ion and mere exposure to ambien~ conditions I ~ 5~

20071 suffice. It is import~nt ~hat the cooling be carried out to a te~perature 5-10 below Krafft T~mpera~ure Tc, ~nd that th~ concentrates be held at said temperature or at lea~t below the Kra~f~ polnt until use. Thus, exposing the concen~rates to ordinary rocxn temper~ture for the m~8t part is sufficient. In ~he case of oc~aglycerol monooleate concentrates having a Tc of about lO~C (50~), exposure to and maint~nance a~ refrigeration temperature is necessary.
Ew~nples where homogenization may be desired are ln ~he prepara-Lion of such products as cof:fee whiteners~ whipped ~OppLng8 ~d ice cxeam, in accor~ance wi~h ~ criterla.
Follo~Qng cooling, the concentrate~ of the present invention can be stored for prolonged periods of 12-18 months or longer ancl remain stable for such periods (stable belng ~efined ~8 free of any cli6cernible emul~ion breakdown or lipid-~ater separation). Sub~eqwently, the concentra~es can be blended with or diluted by additional ~at~ oil or water and other ingredients to ~ake a final product. 'l~e blending, with either oil (or fat) or w~ter, can be carried o~t by simple mixing and the resulting emulsion product wLll continue to exhibit excellent emulfiion stabllity.
Addition~lly, th~ conc~ntrates wlll have excell~nt f~mc~ionality or act:lvity ~n the ~in~ll product.
EX~lE~, ~
A single-stage ~i~ yello~ calce olmula ha~ln~ the ~ollow~ng fol~nulati~l was prepared:
'rABLE I~
~5 HIGH-RAIIO YELLOW G~KE FD~M~LATION
. ", ~
~aker's Percent In~ di~nt ..
100 Cake 10ur 130 ~gar Shortening with e~ulslfier Milk solids 3 Salt 7 Baker's p~wder ~0 Liquid whole e~gs 110 Water ~ s~

20071 Prior to preparing the above formulati~n, two concentrates were fo~ned, as follaw~;
Concentrate 1 10% ~aprol 3C~S (trig].ycerol monoshortening) 30~ W~ter 60% Cre~ntex (plastic partially hydrogenated vegetable oil) Concentr~te 2 10% Santone 3-1-SH (triglycerol ~no-shvrte~ing) 1 60% ~ater 30~ Creamtex (plastic pr~rtially hydrogenated v~getable oil) The concentrates each ~ere proces~ed in~o alpha crystalline gel~ by n~ing at an elevated tempera~ure sufficient to melt the lipid ingredients and then cool~ng the ~ixes to belcw the temperatures Tc Eor the concentrates (see l`able I), Storage tes~s indi~ated the gels to bP very stable :Eor prolonged per~od~
Each concentrate was then blended by slmple n~xing procedures ~ith o~her iqgredients, Lncluding added fat ~nd added water to nake up the ~ormulation of Table II. For instance, the water content of 110 include~
water fran the coneentrate p~us added wa~er.
Three control examples were alæo prepared, the ~irst being a s~anc~ld yellow cake onmulation o~ e~s~ntially the ~me proportions w~in~, as ~he shorter~n~ ~lunt-W~sorl Super Quick Blend t~ de~rk)~ Super ~uLok Blend ls n st~ndard comm~rcial blend ~hor~.enin~ .~or thi~ ~ype o~ nppli~ation 2S contclining a pla~tic ~at, poly~Qrbate 6Q ancl ~ono- ~nd diglycer~de~ TWD
aclditional con~rol~ were prepared using Santone 3~1-S~l ~nd Caprol 3 GVS
simply cliæper~ed in the :E~nal formulatLons. In botll of these latter examples, am~unts o~ mono- and diglyceride were also used to obtain optim~m results, ~le results are giv~n in the follo~ing Table III. The percentagPs given are pere~nt e~ lsi~ier ~polysorbate 60~ ~noglyceride, Santone 3 or Caprol 3GVS~ based on total shortelling weight.

* Baker's pero~nt ~ 3'~

~,) ~1 ~1 o , n H 1~ ~ O O _ I
" ~1 . ~,~
~'~
!~

1~ ~ al ~ o o ,~

Table III shows -that both Santone 3-1-SH and Caprol 3GVS
added ~rom the alpha crystalline concentrates gavc speci-Ei.c volumes and overall scores comparable to or better than those ob-tainable polysorbate 60, but with the use o:E much less total emulsiEier (1-2% vs ~.2%). Wi.th regard to the use of the triglycerol monoshortenings simply dispersed i.n the cake -formulations, much higher emulsifier amounts were re~uired to obtain satisEactory results ~abou-t 5% combined triglycerol mon~-shortening and monoglyceride).
XAMPLE II
A Eluid whipped topping was prepared using the ~ollowillg :Eormulation:
TA LE IV
rLUID ~IIPPED TOPPING FO~LATION
Per.cent Ingredient 30.0 Vegetable Fat 10.0 Sugar 2.0 Sodium caseinate 0.5 Cellulose gum 0.3 Emu]si:Eier - S~m-tone 8-1-S
~octaglycerol monos-teara-te) Balance ~a-ter The vegetable fat employed was Paramoun-t C ~trademark~ SCM
Corporation), a hard bu-tter in Elake :Eorm prepared :~rom ~pa-r-tially llyclrogenated vegetable o;.l, having a Wiley Mel-ting Poi.n-t o:E abou-t 101-103 F and S~I o:E 66 a-t 50 F; 53 at 70 F; 38 a-t ~0F; 13 a-t 92F; 'I.S
maximum at 100 F; and O at 110 F.
An alpha crystalline gel concentrate was ~irst prepared using the following proportions;

polyglycerol ester 10%
water 50%
Eat ~0%
The concentrate was homogenized at 80 C prior to cooling in -two stages at 2sno:soo psig. Subsequent to cooling below the Kra:E:Et point :~or -the concentrate~ it was ~ound to have e~cellent s-tab;.lity.

5~

For preparation o:E whipped topping, the concentrate was diluted with additional fat and water (to arrive at the proportions of Table IV) and other ingredien-ts o~ the Table IV formulation. The whipped topping was compared with an optimized control employi.ng polysorba-te 60 (Dur:Eax 60, trademark SCM Corporation) having essentially the same proportion of ingredients but an optimum amount oE emulsi.fi.er. The results are given in the :Eo:llowing Table V.

TABLE V
EVALllATION OF SANTONE ~-l-S-IN FLUID WlIIPPED TOPPINGS

DURFAX 60 SANTON~ 8-1-S

Concentration (%)0.3 0.3 Separation (cm) :Eollowing Eirst Ereeze/thaw cycle2.5 2.0 Whip Ti.me (mi:n)12.00 10.75 AppearanceFi.rm, sl~ curdy creamy, smooth As shown in Table V, the concentrate o:E -the present inventi.on gave a product showing less separation ~aEter :Eirst Ereeze/thaw cycle) : than the control. Whipping to achieve a 500% overrun was less and the texture o:E the produc-t was better.

EYA~I~L~ III

An ice cream was prepared using -the :Eollowin~ :Eormula-tlon.

TABI.E VI

ICF. CR~AM ~ORMULATION

Perc~nt Ingrediellt __ _. _ __ ____ 10.0 Milk Eat (from 36% milk Eat cream) 12.0 Sugar 5.0 Corn syrup solids 10.0 Non-fat milk solids 0.15 Stabi.lizer 0.15 EmulsiEier - Santone 8-1-0 ~octaglycerol monooleate) Balance Water The alpha crystalline gel concentrate in this e~ample containecl 5% ~-1-0 ~5% Milk fat cream havi.ng 36% :Eat~ -the balance bel-ng water ~' 5~

27001 l l~e concen~rate was homogenized in two stages (2500:500 psig) at 60C prior to coolin~ helow the l~rafft point (in preparation of the con-centrate), Subsequent to cooling, it wa~ di.luted with additional 36% ~Llk fat cream and water, to the proportions of Table VI, and other ingredients of the Table VI for~ulation.
T~e product was cc~pared with a control of e~sent:Lally Lhe same formulation usIng poly~orbate 80 and the following resul.t~ were obtained.
TAi~E VII
EVALU~TION OF CINlr~E ~ ~ ~ IN IC3 ~ n ~ Santone 8-1-O
Concentration t%) 0.03 0.1 ~ono-di.glyceride ~) 0.12 Whipp~~ e to obtaln 100% overrun (~nin) 9~0 7~5 Meltdown - serun collected ater 60 mln at ambient tcmperature tml) 6.0 7.0 Appearance cl~ing meltdown Falr, ~ry, Sti~f Good,Creclmy,Stlff The pro~lct of the present invention exhiblted bet~er te~ture than the control and ~airly equlvnl~nt ~eltdown a~. m~ch le98 ~al18i~ier concentratlonO
EXA*PIE IV
A night cream base W~6 prepkared rcn1 the followin~ orm~1ation TADL~ blII
~5 ''~ Y~I,L~GLib~

12 Santone 3~1-S (triglycerol monosteaIate) M~neral oil S ~hite petrolatum 1 Aluminum stearate 72 ~ater Prior to preparation of the above formulation, an alpha crystalline gel concentrate wcl~ prepared according to the concepts o~ this in\rention, ha~ing the f~llo~ng ln~recllent~:

20071 polyglycerol es~er 20%
water 40~
¦ mineral oil 40%
l Then subseq~nt to cooling, ~he concentrate was readily diluted by simple mix~ng with addltlonfll ~ineral oilf water and the othex ingr~dient~
of Table VIII. After dilution, the texture was excellent and the product remained stable for a prolonged period of time.
LXA~ V
An i~ing/filling concen~ra~e ~as prepared in tWD parts, the first part being an alpha cry~talline gel having the followqng formulation:
Part 1 35% Tri~lycerol monostearate (Santone 3~1-S) 35~ PartLally hydro~enated cottonseed oil having a Wlle.y Melt mg Point of about g5F.
30% hater.
The alpha cry~talli~le gel w~3 then readLly blended by simple mixing into the following formulation:
T ~ IX
Percen~ ~b~ we:L~ In~edient 40% Pow~ered sugar 5.75% Non-fat dxy mllk po~er 0.25~ Salt 34~ Par~ 1 concentrate ~0% Water ~h~ prote-ln c~nt~nt could have been any protein suitable for this p~lrpoæe, SU~I a~ Ca8~ln 0~ wh~y prot~in ln place o~ the milk powder.
ulting product aerated het~er, had hetter t~c~re and was ~ore st~hle a~alns~ oilJwater separation than a comparable product in which ~he polyglycerol e~ter wa~ ~imply blended .unto the total formulation along with other ingredients.
All o~ the polyglycerol e~ters of the present invention have HLB
~alues eq~l to or above about 5. The followlng Table gives representative ~ILB v~lues:

~ ~ 5~

~ nt A~proxImate ~LB
triglyc.erol mono~tearate 7.2 oc~aglycerol monooleate 13 oc-taglycerol nostearate 13 triglycerol ~noshortening 7.2 hexaglycerol distearate 5 By contrast, a poly~lycerol ester such as decaglycerol decaoleate has an HLB value o~ about two (2) and w wld not be suitable in the presen~ invention

Claims (14)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:

1. A stable polyglycerol ester containing water/oil emulsion concentrate suitable for dilution with additional oil or water or both by simple mixing, consisting essentially of polyglycerol ester, oil and water in the proportion based on the weight of the concentrate of at least 5%
water, but less than 80%, the ratio by weight of oil to polyglycerol ester being in the range of about 1:10 to about 10:1, the concentrate being an alpha crystalline gel.

2. The concentrate of claim 1 wherein said polyglycerol ester has an HLB value more than about 5.

3. The concentrate of claim 1 having a particle size less than about 2 microns

4. The concentrate of claim 1 wherein said oil is fluid or solid, having a Wiley Melting Point in the range of about 35-120°F.

5. A food, drug or cosmetic product containing the concentrate of claim 1, the concentrate providing a high degree of activity and stability,

6. A stable polyglycerol ester containing water/oil emulsion concentrate stable for dilution with additional oil or water or both by simple mixing prepared by mixing said water, oil and polyglycerol ester and heating the same to above the Krafft point (Tc) of the concentrate to form a liquid crystalline dispersion; and cooling said dispersion to 5-10°F below the Krafft point (Tc) of the concentrate to form an alpha crystalline gel structure, the water content being at least 5% by weight of the concentrate but less than 80%, the ratio by weight of oil to polyglycerol ester being in the range of about 1;10 to about 10:1, the proportions of ingredients being those necessary to form the alpha crystalline gel structure.

7. The concentrate of claim 6 wherein said polyglycerol ester has an HLB value of more than about 5.

8. The concentrate of claim 6 wherein the liquid crystalline dispersion is subjected to homogenization prior to cooling, the concentrate having a particle size less than about 2 microns.

9. The concentrate of claim 6 wherein said oil is fluid or solid having a Wiley Melting Point in the range of about 35-120°F.

10. A food, drug or cosmetic product containing the concentrate of claim 6 prepared by diluting said concentrate by simple mixing with additional ingredient including oil or water, or both oil and water, the concentrate providing a high degree of activity and stability.

11. A method for making a stable polyglycerol ester containing water/oil emulsion concentrate suitable for dilution with additional oil or water or both by simple mixing, the water content being at least 5% by weight of the concentrate but less than 80%, the ratio by weight of oil to poly-glycerol ester being in the range of about 1:10 to about 10:1, the propor-tions of ingredients being those necessary to form the alpha crystalline gel structure, which method comprises the steps of:
mixing said water, oil and polyglycerol ester and heating the same to above the Krafft point (Tc) of the concentrate to form a liquid crystalline dispersion; and cooling said dispersion to 5-10°F below the Krafft point (T
of the concentrate to form an alpha crystalline gel structure.

12. The method of claim 11 wherein the liquid crystalline dis-persion is subjected to homogenization prior to cooling, the concentrate having a particle size less than about 2 microns.

13. The method of claim 11 wherein said polyglycerol ester has an HLB
value of more than about 5.

14. A method for making a food, drug or cosmetic product, which method comprises diluting the concentrate prepared according to the method of claim 11 by simple mixing with additional ingredients including oil or water or both.