CN101690585B - Nano diglyceride microemulsion carrier and preparation method thereof - Google Patents

Nano diglyceride microemulsion carrier and preparation method thereof Download PDF

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Publication number
CN101690585B
CN101690585B CN2009101544365A CN200910154436A CN101690585B CN 101690585 B CN101690585 B CN 101690585B CN 2009101544365 A CN2009101544365 A CN 2009101544365A CN 200910154436 A CN200910154436 A CN 200910154436A CN 101690585 B CN101690585 B CN 101690585B
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diglyceride
acid anhydride
parts
polyoxyethylene sorbitan
distilled water
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CN101690585A (en
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李铎
陈莹
张辉
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a nano diacylglycerol microemulsion carrier, which consists of the following compositions in percentage by weight: 25 to 30 percent of 1,3-sn-diacylglycerols, 6.5 to 11.5 percent of surfactant, 5 to 7.5 percent of cosurfactant, 10 to 25 percent of cosolvent and the balance of distilled water which is over 25 percent. The invention also discloses a method for preparing the nano diacylglycerol microemulsion carrier, which comprises the following steps: evenly stirring and mixing the surfactant, the cosurfactant and the 1,3-sn-diacylglycerols at a temperature between 20 and 30 DEG C; and maintaining the temperature between 20 and 30 DEG C, dropwise adding the distilled water in which the cosolvent is dissolved with stirring, and obtaining the nano diacylglycerol microemulsion carrier after the dropwise addition is finished. The nano diacylglycerol microemulsion carrier can be dissolved in water, and has good stability and high bioavailability.

Description

A kind of nano diglyceride microemulsion carrier and preparation method thereof
Technical field
The invention belongs to field of food, relate to a kind of microemulsion that forms a kind of new product that can add in other food, be specifically related to a kind ofly with 1, the 3-diglyceride is micro emulsion carrier of oil phase and preparation method thereof.
Background technology
Diglyceride is the natural minor constituent that is present in the edible plants oil, and it has two kinds of isomers (1,2-diglyceride and 1,3-diglyceride).To 1, the multinomial safety evaluation of 3-diglyceride finds, 1, and the 3-diglyceride is harmless to human non-toxic, is regarded as " It is generally accepted safety " material by U.S. FDA.Though 1; 3-diglyceride and triglycerides (main component of natural oil) can be worth and absorptivity on basic identical; But exist in their metabolism in vivo than big-difference, short-term and long-term animal and human's body test show, compare with the triglycerides that contains same or similar aliphatic acid composition; 1, the 3-diglyceride has control and treats the effect of high blood triglyceride disease, obesity and complication thereof.Up to the present, diglyceride all also is not widely used.Diglyceride is a kind of oil, and itself is water insoluble, and molecular weight is big; In the actual production application of food, it is fully dissolved and be scattered in the water, can consider to make common emulsion; But well-known common emulsion is thermodynamic unstable system, in depositing process, occurs the profit lamination easily, has not only influenced the outward appearance of product; Also influenced the bioavilability of product, and the emulsion particle is bigger, bioavilability is not high; Therefore, need the carrying system of the diglyceride of a kind of stable more, bioavilability that can improve diglyceride of invention, to enlarge diglyceride in the Application in Food scope.
Summary of the invention
The technical problem that the present invention will solve provides that a kind of ability is water-soluble, good stability, nano diglyceride microemulsion carrier that bioavilability is high and preparation method thereof.
In order to solve the problems of the technologies described above; The present invention provides a kind of nano diglyceride microemulsion carrier; It is made up of following components in weight percentage content: 1; 3-diglyceride 25-30%, surfactant 6.5-11.5%, cosurfactant 5-7.5% and cosolvent 10-25%, all the other are distilled water, and distilled water>25%.
Improvement as nano diglyceride microemulsion carrier of the present invention: surfactant be the HLB value greater than 10 and less than 20 non-ionic surface active agent, or for the HLB value greater than 10 and the complexed surfactant that mixes less than 10 surfactant less than 20 non-ionic surface active agent and HLB value, this complexed surfactant HLB value is greater than 10 and less than 20; Cosurfactant is a short chain fatty alcohol, and cosolvent is polyalcohol and/or carbohydrate.
Further improvement as nano diglyceride microemulsion carrier of the present invention: the HLB value is greater than 10 and be at least a in polyoxyethylene sorbitan acid anhydride monolaurate, polyoxyethylene sorbitan acid anhydride monopalmitate, polyoxyethylene sorbitan acid anhydride monostearate and the polyoxyethylene sorbitan acid anhydride monoleate less than 20 non-ionic surface active agent;
The HLB value is anhydrous sorbitol acid anhydride monolaurate, anhydrous sorbitol acid anhydride monopalmitate, sorbitan monostearate or anhydrous sorbitol acid anhydride monoleate less than 10 surfactant;
Short chain fatty alcohol is an absolute ethyl alcohol; Polyalcohol is 1, and 2-propane diols or glycerine, carbohydrate are glucose, fructose or sucrose.
The present invention also provides the nano diacylglycerol microemulsion carrier preparation method simultaneously, may further comprise the steps:
1), takes by weighing each component by weight percentage;
2), with surfactant, cosurfactant and 1, the 3-diglyceride evenly mixes in 20-30 ℃; Keep 20-30 ℃ temperature to drip the distilled water that has dissolved cosolvent down then, dropwise the nano diglyceride microemulsion carrier that promptly gets transparence in stirring.
The present invention on surfactant selection, mainly select for use in the food scope can use, toxicity is lower, be not subject to the little non-ionic surface active agent of influence, haemocylolysis of strong electrolyte and inorganic salts and soda acid.Because what the present invention will prepare is the microemulsion of oil-in-water (O/W) type; Therefore select for use the HLB value greater than 10 and less than 20 non-ionic surface active agent, generally be selected from several kinds of composite compounds in polyoxyethylene sorbitan acid anhydride monolaurate, polyoxyethylene sorbitan acid anhydride monopalmitate, polyoxyethylene sorbitan acid anhydride monostearate, the polyoxyethylene sorbitan acid anhydride monoleate; In addition; Be mixed together the high surfactant of HLB value and the low surfactant of HLB value when using; They adsorb formation " compound " on the interface; Align closely, form higher intensity, can well prevent coalescence; Thereby increase the stability of microemulsion; Therefore it is composite also to have selected the HLB value to carry out less than in a kind of and above-mentioned surfactant in 10 the surfactant one or more, thereby obtains the HLB value greater than 10 and less than 20 complexed surfactant, the HLB value can be selected from anhydrous sorbitol acid anhydride monolaurate, anhydrous sorbitol acid anhydride monopalmitate, sorbitan monostearate, anhydrous sorbitol acid anhydride monoleate less than 10 surfactant.
The used cosurfactant of the present invention is an absolute ethyl alcohol, though other alcohols some also can be used as the food additives auxiliary agent, all will remove at last, and taste is more pungent, can influence the smell of product.The adding of absolute ethyl alcohol not only can further reduce interfacial tension, can also increase the flexibility at interface, makes the interface be easy to bending, and it is bigger to form the micro emulsion zone.
The used cosolvent of the present invention is 1,2-propane diols, glycerine, glucose, a kind of compound in a kind of and carbohydrate in a kind of or above-mentioned polyalcohol in fructose and the sucrose.Because 1, the molecular weight ratio of 3-diglyceride is bigger, therefore above-mentioned cosolvent and absolute ethyl alcohol play the effect of Synergistic, and the molten amount of diglyceride is increased.
The used water of the present invention is distilled water.In the present invention, 1, the 3-diglyceride adds as oil phase.All components of the present invention all can obtain through commercial mode, and for example 1, the 3-diglyceride can be available from Japanese Kao company.In preparation method of the present invention, whipping temp is good with 25 ℃.
Nano diglyceride microemulsion carrier of the present invention is a kind of homogeneous phase, stable, transparent system; The size of liquid pearl is 10-100nm; The water dilution range is wide, and layering did not take place the normal temperature held in 3 months, even centrifugally under 100 times acceleration of gravity also phenomenon of phase separation can not take place.Because the present invention's preparation is O/W type microemulsion, has greatly improved dispersiveness and the bioavilability thereof of diglyceride in water, makes it can be advantageously used in greatly having enlarged its range of application in water food system such as milk, the beverage etc.
Nano diglyceride microemulsion carrier of the present invention is because all component batchings all belong to food additives, and therefore nano diglyceride microemulsion carrier of the present invention can be applied in the food; For example it is joined in the food such as healthy beverage, flavouring, mayonnaise, candy, chocolate, consumption is generally the nano diglyceride microemulsion carrier that adds 66.7-80g in every kg food, evenly stirs to get final product.The eater can reach the purpose that the minimizing body fat is accumulated, controlled body weight and regulates blood fat through taking in the above-mentioned functional food that contains nanoscale diglyceride microemulsion liquid.
The specific embodiment
The preparation method of embodiment 1, a kind of nano diglyceride microemulsion carrier, carry out following steps successively:
1) takes by weighing 25 part 1, by weight, 3-diglyceride, 6.25 parts of polyoxyethylene sorbitan acid anhydride monoleates, 3.12 parts of polyoxyethylene sorbitan acid anhydride monolaurates, 6.25 parts of absolute ethyl alcohols, 8 parts of glycerine, 16 portions of sucrose, 35.38 parts of distilled water.
2), earlier that glycerine and sucrose dissolved is subsequent use in distilled water; Then with 1; After 3-diglyceride, polyoxyethylene sorbitan acid anhydride monoleate, polyoxyethylene sorbitan acid anhydride monolaurate and absolute ethyl alcohol are mixed in 25 ℃ and stir (stirring 2 minutes); Keep 25 ℃ temperature; Slowly drip (1/2 minutes) above-mentioned subsequent use distilled water that is dissolved with glycerine and sucrose, the limit edged stirs (2400 rev/mins), dropwises and promptly gets transparent nano diglyceride microemulsion carrier.
In order to prove advantage of the present invention, the inventor is provided with following experiment respectively to the nano diglyceride microemulsion carrier of embodiment 1 gained:
Test 1.1 stability tests
With above-mentioned nano diglyceride microemulsion carrier under 100 times acceleration of gravity centrifugal 5 minutes, the profit lamination does not appear, explain that its stability is fine.
Test 1.2 water-soluble tests
Above-mentioned nano diglyceride microemulsion carrier is mixed according to 1: 100 weight ratio with water, lamination can not occur, explain that its dissolubility in water is good.
Test the test of 1.3 particle diameters
The average grain diameter that records product of the present invention through laser particle analyzer is 33nm, and particle diameter is very little, can improve the bioavilability of diglyceride.
The preparation method of embodiment 2, a kind of nano diglyceride microemulsion carrier, carry out following steps successively:
1) takes by weighing 25 part 1, by weight, 3-diglyceride, 6.25 parts of polyoxyethylene sorbitan acid anhydride monoleates, 1.56 parts of anhydrous sorbitol acid anhydride monoleates, 5 parts of absolute ethyl alcohols, 13 parts of glycerine, 49.19 parts of distilled water.
2), be dissolved in the distilled water glycerine subsequent use earlier; Then with 1; 3-diglyceride, polyoxyethylene 20 sorbitan monooleate, anhydrous sorbitol acid anhydride monoleate and absolute ethyl alcohol be mixed in 25 ℃ stir after; Keep 25 ℃ temperature; Slowly drip (1/2 minutes) above-mentioned subsequent use distilled water that is dissolved with glycerine, the limit edged stirs, and dropwises and promptly gets transparent nano diglyceride microemulsion carrier.
The nano diglyceride microemulsion carrier of embodiment 2 gained is tested respectively as follows:
Test 2.1 stability tests
With above-mentioned nano diglyceride microemulsion carrier under 100 times acceleration of gravity centrifugal 5 minutes, the profit lamination does not appear, explain that its stability is fine.
Test 2.2 water-soluble tests
Above-mentioned nano diglyceride microemulsion carrier is mixed according to 1: 100 weight ratio with water, lamination can not occur, explain that its dissolubility in water is good.
Test the test of 2.3 particle diameters
The average grain diameter that records product of the present invention through laser particle analyzer is 36.24nm, and particle diameter is very little, can improve the bioavilability of diglyceride.
The preparation method of embodiment 3, a kind of nano diglyceride microemulsion carrier, carry out following steps successively:
1) takes by weighing 28 part 1, by weight, 3-diglyceride, 2.8 parts of polyoxyethylene sorbitan acid anhydride monoleates, 1.4 parts of anhydrous sorbitol acid anhydride monolaurates, 2.66 parts of polyoxyethylene sorbitan acid anhydride monolaurates, 7 parts of absolute ethyl alcohols, 18 portions of sucrose, 40.14 parts of distilled water.
2), earlier that sucrose dissolved is subsequent use in distilled water; Then with 1; 3-diglyceride, polyoxyethylene 20 sorbitan monooleate, anhydrous sorbitol acid anhydride monolaurate, polyoxyethylene sorbitan acid anhydride monolaurate and absolute ethyl alcohol be mixed in 29 ℃ stir after; Keep 29 ℃ temperature; Slowly drip the above-mentioned subsequent use distilled water that is dissolved with sucrose, the limit edged stirs, and dropwises and promptly gets transparent nano diglyceride microemulsion carrier.
The nano diglyceride microemulsion carrier of embodiment 3 gained is tested respectively as follows:
Test 3.1 stability tests
With above-mentioned nano diglyceride microemulsion carrier under 100 times acceleration of gravity centrifugal 5 minutes, the profit lamination does not appear, explain that its stability is fine.
Test 3.2 water-soluble tests
Above-mentioned nano diglyceride microemulsion carrier is mixed according to 1: 100 weight ratio with water, lamination can not occur, explain that its dissolubility in water is good.
Test the test of 3.3 particle diameters
The average grain diameter that records product of the present invention through laser particle analyzer is 50nm, and particle diameter is very little, can improve the bioavilability of diglyceride.
The preparation method of embodiment 4, a kind of nano diglyceride microemulsion carrier, carry out following steps successively:
1), takes by weighing 30 part 1 by weight; 3-diglyceride, 3 parts of polyoxyethylene sorbitan acid anhydride monolaurates, 3 parts of polyoxyethylene sorbitan acid anhydride monopalmitates, 4 parts of polyoxyethylene sorbitan acid anhydride monostearates, 1.23 parts of polyoxyethylene sorbitan acid anhydride monoleates, 7.48 parts of absolute ethyl alcohols, 4 part 1; The 2-propane diols, 6.67 portions of sucrose, 40.62 parts of distilled water.
2), earlier with 1,2-propane diols and sucrose dissolved are subsequent use in distilled water; Then with 1; 3-diglyceride, polyoxyethylene sorbitan acid anhydride monolaurate, polyoxyethylene sorbitan acid anhydride monopalmitate, polyoxyethylene sorbitan acid anhydride monostearate, polyoxyethylene sorbitan acid anhydride monoleate and absolute ethyl alcohol be mixed in 20 ℃ stir after; Keep 20 ℃ temperature, slowly drip and above-mentionedly subsequent use be dissolved with 1, the distilled water of 2-propane diols and sucrose; The limit edged stirs, and dropwises and promptly gets transparent nano diglyceride microemulsion carrier.
The nano diglyceride microemulsion carrier of embodiment 4 gained is tested respectively as follows:
Test 4.1 stability tests
With above-mentioned nano diglyceride microemulsion carrier under 100 times acceleration of gravity centrifugal 5 minutes, the profit lamination does not appear, explain that its stability is fine.
Test 4.2 water-soluble tests
Above-mentioned nano diglyceride microemulsion carrier is mixed according to 1: 100 weight ratio with water, lamination can not occur, explain that its dissolubility in water is good.
Test the test of 4.3 particle diameters
The average grain diameter that records product of the present invention through laser particle analyzer is 39.63nm, and particle diameter is very little, can improve the bioavilability of diglyceride.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.

Claims (4)

1. the preparation method of a nano diglyceride microemulsion carrier is characterized in that carrying out successively following steps:
1) takes by weighing 25 part 1, by weight, 3-diglyceride, 6.25 parts of polyoxyethylene sorbitan acid anhydride monoleates, 3.12 parts of polyoxyethylene sorbitan acid anhydride monolaurates, 6.25 parts of absolute ethyl alcohols, 8 parts of glycerine, 16 portions of sucrose and 35.38 parts of distilled water;
2), earlier that glycerine and sucrose dissolved is subsequent use in distilled water; Then with 1; 3-diglyceride, polyoxyethylene sorbitan acid anhydride monoleate, polyoxyethylene sorbitan acid anhydride monolaurate and absolute ethyl alcohol be mixed in 25 ℃ stir stirred in 2 minutes after; Keep 25 ℃ temperature; Slowly drip the above-mentioned subsequent use distilled water that is dissolved with glycerine and sucrose with 1/2 minutes speed, stir, dropwise and promptly get transparent nano diglyceride microemulsion carrier with 2400 rev/mins rotating speed limit edgeds.
2. the preparation method of a nano diglyceride microemulsion carrier is characterized in that carrying out successively following steps:
1) takes by weighing 25 part 1, by weight, 3-diglyceride, 6.25 parts of polyoxyethylene sorbitan acid anhydride monoleates, 1.56 parts of anhydrous sorbitol acid anhydride monoleates, 5 parts of absolute ethyl alcohols, 13 parts of glycerine and 49.19 parts of distilled water;
2), be dissolved in the distilled water glycerine subsequent use earlier; Then with 1; 3-diglyceride, polyoxyethylene 20 sorbitan monooleate, anhydrous sorbitol acid anhydride monoleate and absolute ethyl alcohol be mixed in 25 ℃ stir after; Keep 25 ℃ temperature; Slowly drip the above-mentioned subsequent use distilled water that is dissolved with glycerine with 1/2 minutes speed, the limit edged stirs, and dropwises and promptly gets transparent nano diglyceride microemulsion carrier.
3. the preparation method of a nano diglyceride microemulsion carrier is characterized in that carrying out successively following steps:
1) takes by weighing 28 part 1, by weight, 3-diglyceride, 2.8 parts of polyoxyethylene sorbitan acid anhydride monoleates, 1.4 parts of anhydrous sorbitol acid anhydride monolaurates, 2.66 parts of polyoxyethylene sorbitan acid anhydride monolaurates, 7 parts of absolute ethyl alcohols, 18 portions of sucrose and 40.14 parts of distilled water;
2), earlier that sucrose dissolved is subsequent use in distilled water; Then with 1; 3-diglyceride, polyoxyethylene 20 sorbitan monooleate, anhydrous sorbitol acid anhydride monolaurate, polyoxyethylene sorbitan acid anhydride monolaurate and absolute ethyl alcohol be mixed in 29 ℃ stir after; Keep 29 ℃ temperature; Slowly drip the above-mentioned subsequent use distilled water that is dissolved with sucrose, the limit edged stirs, and dropwises and promptly gets transparent nano diglyceride microemulsion carrier.
4. the preparation method of a nano diglyceride microemulsion carrier is characterized in that carrying out successively following steps:
1), takes by weighing 30 part 1 by weight; 3-diglyceride, 3 parts of polyoxyethylene sorbitan acid anhydride monolaurates, 3 parts of polyoxyethylene sorbitan acid anhydride monopalmitates, 4 parts of polyoxyethylene sorbitan acid anhydride monostearates, 1.23 parts of polyoxyethylene sorbitan acid anhydride monoleates, 7.48 parts of absolute ethyl alcohols, 4 part 1; The 2-propane diols, 6.67 portions of sucrose and 40.62 parts of distilled water;
2), earlier with 1,2-propane diols and sucrose dissolved are subsequent use in distilled water; Then with 1; 3-diglyceride, polyoxyethylene sorbitan acid anhydride monolaurate, polyoxyethylene sorbitan acid anhydride monopalmitate, polyoxyethylene sorbitan acid anhydride monostearate, polyoxyethylene sorbitan acid anhydride monoleate and absolute ethyl alcohol be mixed in 20 ℃ stir after; Keep 20 ℃ temperature, slowly drip and above-mentionedly subsequent use be dissolved with 1, the distilled water of 2-propane diols and sucrose; The limit edged stirs, and dropwises and promptly gets transparent nano diglyceride microemulsion carrier.
CN2009101544365A 2009-10-27 2009-10-27 Nano diglyceride microemulsion carrier and preparation method thereof Expired - Fee Related CN101690585B (en)

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CN116077422B (en) * 2023-01-04 2024-02-13 成都大学 Pomegranate seed oil diglyceride nanoemulsion gel

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5160759A (en) * 1989-06-07 1992-11-03 Kao Corporation Edible oil-in-water emulsion

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5160759A (en) * 1989-06-07 1992-11-03 Kao Corporation Edible oil-in-water emulsion

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JP特开2002-176952A 2002.06.25
JP特开2007-195564A 2007.08.09
陈福明等.双甘酯的生产及应用.《中国油脂》.1997,第22卷(第5期),第49-51页. *

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