CH629973A5 - Method for preparing an emulsion of the water-in-oil type - Google Patents

Description

The present invention relates to a method for producing a water-in-oil type emulsion with a phase instability temperature in the range of 10-40 ° C. from oil or fat, a partial glyceride emulsifier and water.

A problem that occurs very often with emulsions, especially emulsions with a so-called low calorie content, is that insufficient flavoring occurs when the product is chewed in the mouth, since a substantial part of water droplets that contain the flavoring material, the papillary Do not reach your mouth, but remain trapped in the continuous fat phase.

An improvement in the delivery of the flavors can basically be achieved by giving the product a rougher emulsion structure than the usual products, so that an unstable emulsion is formed which will cause a better delivery of the flavors to the palate when chewed. From the microbiological point of view, however, such emulsions are dangerous since, during storage, water can be separated very easily, which usually causes an unacceptable bacteriological infection of the product.

The present invention thus relates to a process for the preparation of an emulsion of the water-in-oil type with a phase instability temperature in the range from 10-40 ° C., which is characterized in that oil or fat, a partial glyceride emulsifier and water produces an emulsion, the emulsion obtained 50-65 wt .-% of a dispersed aqueous phase with a pH of 4 ^ 6 and 50-35 wt .-% of a continuous fat or oil phase containing a smaller amount of has a partial glyceride emulsifier, the fat or oil having a solids content of 10-35% at all temperatures of 10-20 ° C, a difference in solids content at 10 and 20 ° C of not more than 10% and a solids content at 30 ° C of less than 5% and the emulsion has a phase instability temperature that is 10-40 ° C.

The emulsion produced according to the invention has a phase instability temperature of 10-40 ° C, preferably a temperature of at least 15 ° C and in particular a temperature of 20-35 ° C.

“Phase instability temperature” (PIT) is understood to mean the temperature at which the emulsion under shear conditions is similar to that which occurs on the palate and is measured by the PIT test, which is described below, and where there is a pronounced increased tendency to conduct electricity consists.

The terms "dispersed phase" and "continuous phase" refer to the condition of the emulsion

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at room temperature, namely at a temperature of about 20 ° C.

All percentages given are by weight and are calculated on the total weight of the low fat emulsion (except for the solids content) unless otherwise stated. The solids content is given in percent by weight and is based on the weight of the fat mixture. The solids content was measured by the method of Haighton, Vermaas and Den Hollander, described in J.A.O.C.S., vol. 48, pages 7-10, and.

An advantage of the low fat emulsion obtained according to the invention resides in the fact that a substantial part of the dispersed aqueous phase is released in the mouth, whereby the water-soluble emulsifiers dissolve in the saliva, which causes the former continuous fat phase to emulsify in the saliva and thereby in the mouth creates an oil-in-water emulsion. In the low-fat emulsion produced according to the invention, up to 90% or even more of the dispersed aqueous phase can be released within about 10 seconds under the conditions prevailing in the palate. This results in an extremely rapid release of the flavor, not only because the water-soluble flavors are released, but also because there is a very rapid distribution of the essentially oil-soluble flavor components in the saliva, which is part of the continuous aqueous phase among those in the palate prevailing conditions, which is due to the high surface effect of the oil-in-water emulsion that has formed.

The expansion properties of the fat mixture in the emulsion obtained according to the invention will essentially avoid the formation of high-melting triple-saturated triglycerol by recrystallization at the temperature differences occurring in the emulsion during storage; said glycerides would have W / O emulsion stabilization properties at a relatively low level under the conditions of the palate.

The expansion properties of the fat blend also affect the instability of the product, especially under the shear conditions found on the palate. In the process according to the invention, a fat mixture is used which has a solids content which is as unchangeable as possible at a temperature of 10-20 ° C., namely a difference in solids content of between 10 and 20 ° C. of not more than 10%. Products that have a fat mixture of such solids with the temperature curves mentioned will have a minimum of melting and recrystallization of the glycerides at the temperature differences within a range of e.g. 10-20 ° C, they have an improved cooling sensation on the palate during the melting of the glycerides and a lower solids content at a temperature of 30 ° C, which will help to avoid a greasy feeling of the melted product on the palate.

The type and ratio of both the emulsifier system and the fat mixture are important so that a sufficient degree of instability of the product is achieved under the palate conditions. Suitable amounts of partial glycerides are preferably in a range of 0.1-0.8% by weight. It is preferred to use partial glycerides that are not fully saturated, e.g. B. glycerides of fatty acids with 16-22 carbon atoms, these glycerides having an iodine number of 20-100, preferably 30-60.

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Among the monoglycerides with an iodine number of 30-60, in particular 35-50, e.g. Unhydrated pork fat or tallow very preferred. The partial glycerides can be present in amounts whose ranges are given above; however, the content of partial glycerides is preferably adjusted to the fat content of the emulsions according to the invention with a low fat content.

Suitable weight ratios of fat: partial glycerides are e.g. from (50: 1) to (500: 1), preferably from (100: 1) to (300: 1), present.

Preferred emulsions may additionally contain auxiliary oil-in-water emulsifiers, such as. B. phosphatides, especially partially hydrolyzed phosphatides and synthetic emulsifiers, such as. B. fatty acid sugar esters, "tweens" etc., namely in an amount of 0.01, preferably 0.02-0.6 wt .-%. If phosphatides are used in the emulsions which can be prepared according to the invention and have a low fat content, they preferably contain 5-25% of monocaylglycerol phosphatides, in particular a-mono-acylglycerol phosphatides, calculated on the total weight of the phosphatides. Such phosphatides can be produced synthetically or by chemical hydrolysis (see British patent application 18, 163/68) or by enzymatic hydrolysis of diacylglycerophosphatides under known conditions (see British patent specification No. 1 215 868).

Proteins can similarly be used as auxiliary emulsifiers for the oil-in-water emulsions.

Although not more than 0.01-0.6% by weight thereof is sufficient for an effective phase inversion of the emulsion with a low fat content under palate conditions, amounts of up to 12%, preferably up to 8%, can be used since the excess is Proteins do not destabilize the emulsion under normal process conditions and during storage conditions, provided that an appropriate amount of the partial glycerides is present. Such oil-in-water auxiliary emulsifiers therefore help to balance the water-in-oil properties of the partial glycerides under the palate conditions without having an effect on the destabilization of the emulsion during normal storage, use and transport.

Purely vegetable phosphatides, namely non-chemically treated or fractionated phosphatides, derived e.g. of soybeans, rapeseed or corn, preferably require a firmer fat mixture than emulsifiers with higher HLB values, such as. B. Lysolecithin, which contains partially hydrolyzed phosphatides, proteins, etc. Such low HLB emulsifiers most likely require the grinding action of firmer fat crystals at the beginning of chewing, so that the destabilization of the low-fat emulsion on the palate can be promoted.

Suitable fully vegetable phosphatides can be used in low fat emulsions that have a fat blend that has a solids content of 26-35% at 10 ° C and preferably 18-25% at 20 ° C.

Emulsifiers, which, like vegetable phosphatides, present less effective emulsifiers for oil-in-water emulsions, namely those with HLB values of approximately 10-16, are preferably used together with a fat mixture which has a high solids content at 10 and 20 ° C.

In particular, proteinaceous water-soluble emulsifiers are preferred because they are very powerful emulsifiers and, moreover, they can protect the fat mixture from oxidation. Finally, such

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Emulsifiers naturally contain flavorings, namely those that are obtained during their culture.

If a fat mixture with an appropriate solids content is used, the desired phase instability temperature can be obtained by properly balancing the following factors:

1. The nature and amount of fat-soluble partial glyceride emulsifiers.

2. The nature and amount of water-soluble emulsifiers.

The emulsion can also contain hydrocolloids in the aqueous phase to increase the stability between the surfaces and also to increase the emulsion-stabilizing properties of the fat crystals during use and during storage. The concentration of the hydrocolloids should be chosen in such a way that a correct balance of the viscosity in the continuous fat phase and the dispersed aqueous phase is achieved. A suitable content of hydrocolloids can vary from 0.1-1.5% by weight.

Further advantages of using hydrocolloids, in particular gum from robinia beans, are based on the influence of reducing the hardness of the plastic emulsion which can be prepared according to the invention, and in addition the hydrocolloids mentioned help to control the taste buds of the released aqueous phase in relation to the viscosity.

It has surprisingly been observed that gum from robinia beans and milk proteins have a synergistic effect on increasing the viscosity.

PIT test

A Haake Rotovisko apparatus is equipped with an MV measuring system. The Haake MVII pendulum is used at a speed of 1, under which conditions a shear rate of 441 sec-1 is used, which is rather high, but representative of the conditions on the palate. Electrodes made of aluminum foil are placed between the MVII pendulum and the Haake measuring vessel wall. (The electrodes have a width of 1 cm and are 15 cm long.) Those parts of the electrodes that come into contact with the wall of the vessel are insulated with a layer of glue with the trade name «Aralide».

The electrodes are connected to a conductivity bridge to measure the conductivity of the emulsion during the test.

The conductivity and viscosity measurements are made at 5 C intervals, starting at 20 ° C or lower in relation to the PIT, which is the temperature at which the conductivity increases markedly, namely at least 104Mhos, or up to 70 ° C, if there is no inversion (with no significant increase in conductivity). The emulsion is held at each of the temperatures for 15 minutes to be sure that equilibrium has been established and the Rotovisko pendulum is rotated at a speed of 1 throughout the experiment.

The present invention is explained in more detail below by the examples, in which all amounts and percentages are by weight and have been calculated on the weight of the low-fat emulsion, unless stated otherwise.

Example I

A fat phase consisting of palm oil middle fraction (30 parts) and sunflower oil (70 parts) was prepared

cleaned and deodorized. The solids content of this mixture was as follows: 24% at 10 ° C, 17% at 20 ° C, 2% at 30 ° C and 0% at 35 ° C. The palm oil middle fraction was obtained by fractionation from palm oil with acetone as follows:

(a) 300 g of refined, deodorized palm oil with a 53.4 iodine value were mixed with 1 Vi liter of acetone and then the mixture was heated until a clear solution was obtained (30 ° C.). The solution was then cooled to a temperature of 6.5 ° G over half an hour while gently stirring with a glass stirrer. The mixture was left to stand at 6.5 ° C. for 1 hour and then filtered through a cooled Buchner funnel under vacuum. The cake was pressed with a glass stopper and then washed twice on the filter with 250 ml of acetone at 5 ° C, using 250 ml of acetone for each wash. The cake was pressed between each wash. It was then removed from the filter and the remaining acetone was distilled off under vacuum. 93.9 g of a fraction with an iodine value of 28.9 were obtained.

(b) To 80 g of the product from step (a) was added 80 ml of acetone and then the mixture was heated to a temperature of 45 ° C. 400 ml of acetone were added to this mixture at 19 ° C. with stirring and the final temperature of the mixture was set at 26 ° C. The mixture was left to stand at this temperature for 20 minutes and filtered through a Buchner funnel, it was pressed off and washed on the filter with 250 ml of acetone at a temperature of 26 ° C. The filtrate and the washing liquid were combined and the acetone was removed by distillation in vacuo. 67.5 g were obtained. The properties of the product are summarized in the following table:

Ingredient / properties palm oil

Middle fraction

Iodine value 34.4

Melting point (° C) 33.4

Refractionation index N6SD 1.4 468

f.f.a. (%) 0.1

Monoglycerides (%) traces

Diglycerides (%) 1.5

Triglycerides * (%) 98.5

S3 (% of triglycerides) 3.1

S2U (% triglycerides) 83.6

SU2 (% of triglycerides) 9.8

U3 (% of triglycerides) 3.5 fatty acid composition **

C 14: 0 0.4

C 16: 1 57.1 C 16: 1 C 17: 0

C 18: 0 7.5

C 18: 1 32.0

C 18: 2 3.0

C20: 0 lanes C 20: 1

* S = saturated; U = unsaturated

** e.g. C 18: 1 = mono-unsaturated C18 fatty acid.

39.8% of the palm oil middle fraction / sunflower oil mixture were melted at a temperature of 40 ° C. under nitrogen and in this melt 0.2% of commercially available monoclycerides of non-hydrogenated lard, which had an iodine value of 44, was dissolved. on.

In addition to the above mixture, oil-soluble flavors and colorants were added.

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The aqueous phase of the product was prepared by dissolving 1.75% sodium chloride in 58.25% water.

0.05% of a water-soluble lecithin fraction obtained by partial hydrolysis with phospholipase A of soybean phosphatides, as described in the description of British Patent 1 215 868, was then dispersed in the water phase. (The content of a-monoacyl glycerophosphatides was approximately 12%, based on the total phosphatide content.)

A viscosity modifier was added to the aqueous phase, namely 0.75% gum from carob beans.

The pH of the water phase was adjusted to 4.5-5.5 by adding citric acid.

An emulsion of the aqueous phase in the fat phase was prepared by slowly adding the water phase to the fat phase with gentle stirring at a temperature of 35 ° C.

The emulsion formed was then processed further in a conventional votator consisting of two A units (roughened surface of the cooler) in which the product was processed and cooled to 15-20 ° C. The above-mentioned votator apparatus also contained a unit for post-crystallization. The PIT was about 28 ° C.

Example II

A fat phase consisting of 32.15% soybean oil (hardened to a melting point of 35 ° C), 21.53% partially hardened rapeseed oil, 9.32% soybean oil (hardened to a melting point of 42 ° C) and 37.0 % Sunflower oil was cleaned and deodorized (% based on the weight of the fat mixture).

The solids content of this mixture was as follows: 32% at 10 ° C, 24% at 20 ° C, 2.5% at 30 ° C and 0% at 35 ° C.

39.7% of the above mixture was melted at a temperature of 40 ° C under nitrogen and in this mixture 0.3% of commercially available monoclycerides of non-hydrogenated lard, which had an iodine value of 44, was dissolved.

Oil-soluble flavorings were added to the mixture mentioned above.

The water phase of this product was made by dissolving 0.5% buttermilk powder in 53.8% water.

The buttermilk solution was dissolved at a temperature of 95 ° C and 1.75% salt, 0.1% sodium tripolyphosphate, 0.1% potassium sorbate and 0.75% gum of carob beans were dissolved in this solution.

The solution was cooled to a temperature of 45 ° C. and 3% culture buttermilk was added.

The pH of the mixture was adjusted to 4.5-5.0 by adding tartaric acid.

An emulsion of the aqueous phase in the fat phase was prepared by adding the aqueous phase to the oil with gentle stirring.

The emulsion obtained was then further processed in a conventional votator system, which contained an A unit with a roughened surface of the cooler, and also a device for recrystallization.

The product was packed in tubes at a temperature of 15 ° C.

The PIT was about 20 ° C.

Example III

A fat phase was prepared which consisted of a palm oil middle fraction (25%) together with sunflower oil (75%), this phase was cleaned and deodorized. The palm oil middle fraction was obtained in the same manner as described in Example 1. The solids content of the fat blend was as follows:

19% at 10 ° C, 12% at 20 ° C, 1% at 30 ° C and 0% at 35 ° C.

39.7% of the palm oil middle fraction / sunflower oil mixture was melted at a temperature of 40 ° C and in this melt 0.2% of commercially available monoglycerides of non-hydrogenated lard, which had an iodine value of 44 and 0, was dissolved , 1% of total soybean phosphatides.

The water phase of the product was then made by dissolving 1.75% sodium chloride in 58.25% water.

The pH of the aqueous phase was adjusted to 4.5-5.5 using citric acid.

An emulsion of the aqueous phase in the fat phase was prepared by slowly adding the aqueous phase to the fat phase with effective stirring at a temperature of 35 ° C.

The emulsion was then processed further in a conventional votator apparatus which had 2 A units (roughened surfaces of the coolers) and a post-crystallization working unit.

The product was packed in tubes at a temperature of 10-15 ° C.

The amount of the aqueous phase that was freed under artificial palate conditions (440 sec-1, 37 ° C, 10 sec) was 70%.

The PIT was about 26 ° C.

Example IV

In this example, the fat phase from Example 3 was used.

38% palm oil middle fraction / sunflower oil was melted under nitrogen at a temperature of 45 ° C and in this melt 0.5% of commercially available monoglycerides of non-hydrogenated lard, which had an iodine value of 44, were dissolved.

56.75% water was heated to a temperature of 95 ° C and in this water 1.0% salt and 0.75% gum from carob bean beans were dissolved by stirring vigorously to give a complete solution of the gelling agent.

The resulting mixture was cooled to 45 ° C and 3% culture buttermilk was added to this mixture.

The pH of the mixture was adjusted to 4.5-5.0 by adding tartaric acid; by adding this acid, a relatively large drop in pH was obtained without the product obtained having an excessively acidic taste.

An emulsion of the aqueous phase in the fat phase could be prepared by slowly adding the aqueous phase to the fat phase at a temperature of 45 ° C with gentle stirring.

The emulsion was then further processed in the usual Votator apparatus, which had an A unit (roughened cooler surface) and a post-crystallization unit.

The product was packed in tubes at a temperature of 10-15 ° C.

The amount of the aqueous phase that was exposed under simulated palate conditions was 90% (440 sec "1.37 ° C, 10 sec).

The PIT was about 20 ° C.

Example V

A low fat emulsion was prepared as described in Example 1 by making 59% of the

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mentioned fat mixture, which was used in the example and also:

Monoglyceride from non-hydrogenated lard

(Iodine number 44) 0.2%

Water 32.4%

Sodium caseinate 6.2%

Salt 1.5%

Potassium sorbate 0.1%

Sodium tripolyphosphate 0.1%

Gum of carob beans 0.5%

The pH was adjusted to 5.8 by adding citric acid.

The PIT was 20 ° C.

Example VI

The procedure of Example 1 was repeated, except that the fat mixture from Example 2 was used, that the partially hydrolyzed phosphatides were replaced by the total soybean phosphatides (0.05%) and that the monoglyceride content was set to 0. 3% increased.

The ratio at the water was adjusted accordingly.

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The PIT was just over 30 ° C.

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Claims (19)

629973 1. A process for the preparation of an emulsion of the water-in-oil type, with a phase instability temperature in the range from 10-40 ° C., characterized in that an emulsion is produced from oil or fat, a partial glyceride emulsifier and water, wherein the emulsion obtained contains 50-65% by weight of a dispersed aqueous phase with a pH of 4-6 and 50-35% by weight of a continuous fat or oil phase which has a smaller amount of a partial glyceride emulsifier , the fat or oil having a solids content of 10-35% at all temperatures of 10-20 ° C, a difference in solids content at 10 and 20 ° C of no more than 10% and a solids content at 30 ° C of less than 5% and the emulsion has a phase instability temperature that is 10-40 ° C. 2. The method according to claim 1, characterized in that the phase instability temperature is 20-35 ° C in the emulsion obtained. 2nd PATENT CLAIMS 3. The method according to claim 1 or 2, characterized in that in the emulsion obtained the solids content of the fat or oil at a temperature of 35 ° C is not more than 0.5%. 4. The method according to any one of claims 1 to 3, characterized in that in the emulsion obtained the solids content of the fat or oil at a temperature of 35 ° C is not more than 0.1%. 5. The method according to any one of claims 1 to 4, characterized in that in the emulsion obtained, the difference in solids content between 10 and 20 ° C is not more than 5%. 6. The method according to any one of claims 1 to 5, characterized in that the content of partial glycerides in the emulsion obtained is in a range of 0.1-0.8 wt .-%. 7. The method according to claim 6, characterized in that in the emulsion obtained, the partial glycerides of fatty acids with 16-22 carbon atoms and have an iodine value of 20-100. 8. The method according to claim 7, characterized in that in the emulsion obtained the iodine value is 30-60. 9. The method according to any one of the preceding claims, characterized in that in the emulsion obtained, the weight ratio of fat or oil to partial glycerides (50: 1) to (500: 1). 10. The method according to claim 9, characterized in that in the emulsion obtained the weight ratio (100: 1) to (300: 1). 11. The method according to any one of claims 1 to 10, characterized in that the emulsion obtained contains oil-in-water auxiliary emulsifiers. 12. The method according to claim 7, characterized in that in the emulsion obtained the content of oil-in-water auxiliary emulsifiers is 0.02-0.6% by weight. 13. The method according to claim 11, characterized in that in the emulsion obtained, the oil-in-water auxiliary emulsifiers are phosphatides. 14. The method according to claim 1, characterized in that in the emulsion obtained, the phosphatides contain 5-25% monoacyl-glycerophosphatide. 15. The method according to claim 13, characterized in that in the emulsion obtained, the phosphatides are vegetable phosphatides and that the emulsion contains a fat or oil mixture which has a solids content of 26-35% at a temperature of 10 ° C. 16. The method according to claim 11, characterized in that in the emulsion obtained, the oil-in-water auxiliary emulsifiers are proteins. 17. The method according to claim 16, characterized in that the emulsion obtained contains up to 12% proteins. 18. The method according to any one of claims 1 to 17, characterized in that the emulsion obtained contains hydrocolloids in the aqueous phase. 19. The method according to claim 18, characterized in that in the emulsion obtained the hydrocolloid content is 0.1-1.5% by weight.