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

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 the field of food and relates to a microemulsion which can be added to other foods to form a new product, in particular to a microemulsion carrier with 1,3-diglyceride as an oil phase and a preparation method thereof.

Background technique

Diacylglycerol is a small amount naturally occurring in edible vegetable oils, and it has two isomers (1,2-diglyceride and 1,3-diglyceride). Multiple safety assessments on 1,3-diglyceride found that 1,3-diglyceride is non-toxic and harmless to the human body, and has been identified as a "generally recognized safe" substance by the US FDA. Although 1,3-diglycerides and triglycerides (the main components of natural oils) are basically the same in terms of energy value and absorption rate, there are large differences in their metabolism in the body. Short-term and long-term animal and human experiments have shown that , Compared with triglycerides containing the same or similar fatty acid composition, 1,3-diglyceride has the effect of controlling and treating hypertriglyceridemia, obesity and its complications. So far, diglycerides have not been widely used. Diacylglycerol is a kind of oil, which is insoluble in water and has a large molecular weight. In the actual production and application of food, to make it fully dissolved and dispersed in water, it can be considered to be made into an ordinary emulsion, but it is well known that ordinary emulsions It is a thermodynamically unstable system, which is prone to oil-water stratification during storage, which not only affects the appearance of the product, but also affects the bioavailability of the product, and the emulsion particles are relatively large, and the bioavailability is not high. Therefore, it is necessary to invent A diglyceride delivery system that is more stable and can improve the bioavailability of the diglyceride, so as to expand the application range of the diglyceride in food.

Contents of the invention

The technical problem to be solved by the present invention is to provide a nano-diglyceride microemulsion carrier capable of dissolving in water, having good stability and high bioavailability and a preparation method thereof.

In order to solve the above technical problems, the present invention provides a nano-diglyceride microemulsion carrier, which is composed of the following components in percentage by weight: 1,3-diglyceride 25-30%, surfactant 6.5-11.5% , co-surfactant 5-7.5% and co-solvent 10-25%, the rest is distilled water, and distilled water> 25%.

As the improvement of the nano-diglyceride microemulsion carrier of the present invention: the surfactant is a nonionic surfactant with an HLB value greater than 10 and less than 20, or a nonionic surfactant and an HLB value with an HLB value greater than 10 and less than 20 A composite surfactant mixed with surfactants less than 10, the HLB value of the composite surfactant is greater than 10 and less than 20; the co-surfactant is a short-chain fatty alcohol, and the co-solvent is a polyol and/or sugar.

As a further improvement of the nano-diglyceride microemulsion carrier of the present invention: the nonionic surfactant with an HLB value greater than 10 and less than 20 is polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan At least one of monopalmitate, polyoxyethylene sorbitan monostearate and polyoxyethylene sorbitan monooleate;

The surfactant having an HLB value of less than 10 is sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate or sorbitan monooleate;

The short-chain fatty alcohol is absolute ethanol; the polyol is 1,2-propanediol or glycerol, and the sugar is glucose, fructose or sucrose.

The present invention also provides a preparation method for the above-mentioned nano diglyceride microemulsion carrier, comprising the following steps:

1), take each component by weight percentage;

2), uniformly stir and mix the surfactant, co-surfactant and 1,3-diglyceride at 20-30°C; then keep the temperature of 20-30°C and add dropwise the distilled water dissolved in the co-solvent under stirring state, After the dropwise addition, a transparent nano-diglyceride microemulsion carrier is obtained.

In the selection of surfactants, the present invention mainly selects non-ionic surfactants that can be used in the food range, have low toxicity, are not easily affected by strong electrolytes, inorganic salts, acids and bases, and have little hemolysis. Because what the present invention will prepare is the microemulsion of oil-in-water (O/W) type, so select the nonionic surfactant with HLB value greater than 10 and less than 20 for use, generally selected from polyoxyethylene sorbitan monolauric acid Compounds of esters, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan monooleate ; In addition, when surfactants with high HLB values and surfactants with low HLB values are mixed together, they will adsorb on the interface to form a "complex", which will be closely oriented and form a higher strength, which can well prevent Coalescing, thereby increasing the stability of the microemulsion, therefore also selected one of the surfactants whose HLB value is less than 10 to compound with one or more of the above-mentioned surfactants, so as to obtain an HLB value greater than 10 and Composite surfactant less than 20, the surfactant with HLB value less than 10 can be selected from sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, Sorbitan Monooleate.

The co-surfactant used in the present invention is dehydrated alcohol, though other alcohols can also be used as food additives, they will be removed at last, and the taste is more pungent, which will affect the smell of the product. The addition of absolute ethanol can not only further reduce the interfacial tension, but also increase the flexibility of the interface, making the interface easy to bend and forming a larger microemulsion area.

The co-solvent used in the present invention is one of 1,2-propanediol, glycerol, glucose, fructose and sucrose or a compound of one of the above polyols and one of sugars. Since the molecular weight of 1,3-diglyceride is relatively large, the above-mentioned co-solvent and absolute ethanol play a synergistic effect, which can increase the solubility of diglyceride.

The water used in the present invention is distilled water. In the present invention, 1,3-diglyceride is added as an oil phase. All components of the present invention can be obtained through commercial means, for example, 1,3-diglyceride can be purchased from Kao Corporation of Japan. In the preparation method of the present invention, the stirring temperature is preferably 25°C.

The nano-diglyceride microemulsion carrier of the present invention is a homogeneous, stable, and transparent system. The size of the liquid beads is 10-100nm, and the range of water dilution is wide. It is placed at room temperature for 3 months without delamination. Phase separation does not occur in centrifugation under high gravitational acceleration. Because what the present invention prepares is the O/W type microemulsion, has greatly improved the dispersibility of diglyceride in water and its bioavailability, it can be used in water phase food system such as milk, beverage etc. conveniently, very Greatly expanded its scope of application.

The nano-diglyceride microemulsion carrier of the present invention belongs to food additives because all component ingredients belong to food additives, so the nano-diglyceride microemulsion carrier of the present invention can be applied in food; For sauce, candy, chocolate and other foods, the dosage is generally to add 66.7-80g of nano-diglyceride microemulsion carrier per kg of food, and stir evenly. Eaters can reduce fat accumulation in the body, control body weight and regulate blood lipids by taking the functional food containing nano-scale diglyceride microemulsion.

Detailed ways

Embodiment 1, a kind of preparation method of nano diglyceride microemulsion carrier, carries out following steps successively:

1), take by weight 25 parts of 1,3-diglyceride, 6.25 parts of polyoxyethylene sorbitan monooleate, 3.12 parts of polyoxyethylene sorbitan monolaurate, 6.25 parts of no Water ethanol, 8 parts of glycerin, 16 parts of sucrose, 35.38 parts of distilled water.

2), first dissolving glycerol and sucrose in distilled water for subsequent use; then 1,3-diglyceride, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monolaurate Mix with absolute ethanol at 25°C and stir evenly (stirring for 2 minutes), then keep the temperature at 25°C, and slowly add (1 drop/2 minutes) the above spare distilled water dissolved in glycerol and sucrose, stirring while adding (2400 rev/min), and the transparent nano-diglyceride microemulsion carrier is obtained after the dropwise addition.

In order to prove the advantages of the present invention, the inventor set up the following experiments respectively to the nano-diglyceride microemulsion carrier obtained in Example 1:

Experiment 1.1 Stability Test

The above-mentioned nano-diglyceride microemulsion carrier was centrifuged for 5 minutes under the acceleration of gravity of 100 times, and no oil-water stratification phenomenon occurred, indicating that its stability is very good.

Experiment 1.2 Water Solubility Test

The above-mentioned nano-diglyceride microemulsion carrier is mixed with water according to the weight ratio of 1:100, and there is no stratification phenomenon, which shows that it has good solubility in water.

Experiment 1.3 Particle size test

The average particle size of the product of the invention measured by a laser particle size analyzer is 33nm, which is very small and can improve the bioavailability of diglyceride.

Embodiment 2, a kind of preparation method of nano diglyceride microemulsion carrier, carries out following steps successively:

1), take by weight 25 parts of 1,3-diglyceride, 6.25 parts of polyoxyethylene sorbitan monooleate, 1.56 parts of sorbitan monooleate, 5 parts of absolute ethanol, 13 parts of glycerin, 49.19 parts of distilled water.

2), first dissolve glycerol in distilled water for later use; then mix 1,3-diglyceride, polyoxyethylene sorbitan monooleate, sorbitan monooleate and absolute ethanol After stirring evenly at 25°C, keep the temperature at 25°C, slowly add dropwise (1 drop/2 minutes) the above-mentioned spare distilled water dissolved in glycerin, stir while adding, and obtain transparent nano-glycerol di Ester microemulsion carrier.

The nano diglyceride microemulsion carrier of embodiment 2 gained carries out following experiment respectively:

Experiment 2.1 Stability test

The above-mentioned nano-diglyceride microemulsion carrier was centrifuged for 5 minutes under the acceleration of gravity of 100 times, and no oil-water stratification phenomenon occurred, indicating that its stability is very good.

Experiment 2.2 Water Solubility Test

The above-mentioned nano-diglyceride microemulsion carrier is mixed with water according to the weight ratio of 1:100, and there is no stratification phenomenon, which shows that it has good solubility in water.

Experiment 2.3 Particle size test

The average particle size of the product of the invention measured by a laser particle size analyzer is 36.24nm, which is very small and can improve the bioavailability of diglyceride.

Embodiment 3, a kind of preparation method of nano diglyceride microemulsion carrier, carries out following steps successively:

1), take by weight 28 parts of 1,3-diglyceride, 2.8 parts of polyoxyethylene sorbitan monooleate, 1.4 parts of sorbitan monolaurate, 2.66 parts of polyoxyethylene sorbitan monolaurate, Sorbitan monolaurate, 7 parts absolute ethanol, 18 parts sucrose, 40.14 parts distilled water.

2), first dissolve sucrose in distilled water for later use; then 1,3-diglyceride, polyoxyethylene sorbitan monooleate, sorbitan monolaurate, polyoxyethylene sorbitan Mix alcohol anhydride monolaurate and absolute ethanol at 29°C and stir evenly, keep the temperature at 29°C, slowly add the above-mentioned spare distilled water dissolved in sucrose dropwise, stir while adding, and obtain transparent nano Diacylglycerol microemulsion carrier.

The nano diglyceride microemulsion carrier of embodiment 3 gained carries out following experiment respectively:

Experiment 3.1 Stability test

The above-mentioned nano-diglyceride microemulsion carrier was centrifuged for 5 minutes under the acceleration of gravity of 100 times, and no oil-water stratification phenomenon occurred, indicating that its stability is very good.

Experiment 3.2 Water Solubility Test

The above-mentioned nano-diglyceride microemulsion carrier is mixed with water according to the weight ratio of 1:100, and there is no stratification phenomenon, which shows that it has good solubility in water.

Experiment 3.3 Particle size test

The average particle size of the product of the invention measured by a laser particle size analyzer is 50nm, which is very small and can improve the bioavailability of diglyceride.

Embodiment 4, a kind of preparation method of nano diglyceride microemulsion carrier, carries out following steps successively:

1), take by weight 30 parts of 1,3-diglyceride, 3 parts of polyoxyethylene sorbitan monolaurate, 3 parts of polyoxyethylene sorbitan monopalmitate, 4 parts of polyoxyethylene sorbitan monopalmitate, Oxyethylene sorbitan monostearate, 1.23 parts of polyoxyethylene sorbitan monooleate, 7.48 parts of absolute ethanol, 4 parts of 1,2-propylene glycol, 6.67 parts of sucrose, 40.62 parts of distilled water.

2), first dissolve 1,2-propanediol and sucrose in distilled water for later use; then 1,3-diglyceride, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monolaurate Mix palmitate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan monooleate and absolute ethanol at 20°C and stir evenly, keep the temperature at 20°C, slowly Add dropwise the distilled water in which 1,2-propanediol and sucrose are dissolved, stir while adding, and obtain a transparent nano-diglyceride microemulsion carrier after the dropwise addition.

The nano diglyceride microemulsion carrier of embodiment 4 gained carries out following experiment respectively:

Experiment 4.1 Stability test

The above-mentioned nano-diglyceride microemulsion carrier was centrifuged for 5 minutes under the acceleration of gravity of 100 times, and no oil-water stratification phenomenon occurred, indicating that its stability is very good.

Experiment 4.2 Water Solubility Test

The above-mentioned nano-diglyceride microemulsion carrier is mixed with water according to the weight ratio of 1:100, and there is no stratification phenomenon, which shows that it has good solubility in water.

Experiment 4.3 Particle size test

The average particle diameter of the product of the invention measured by a laser particle size analyzer is 39.63nm, which is very small and can improve the bioavailability of diglyceride.

Finally, it should be noted that the above examples are only some specific embodiments of the present invention. Obviously, the present invention is not limited to the above embodiments, and many variations are possible. All deformations that can be directly derived or associated by those skilled in the art from the content disclosed in the present invention should be considered as the 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.