CN116869835B

CN116869835B - Hydroxytyrosol inclusion with stabilizing effect and preparation method thereof

Info

Publication number: CN116869835B
Application number: CN202310956689.4A
Authority: CN
Inventors: 常宽; 林伯川
Original assignee: Jiangnan University
Current assignee: Jiangnan University
Priority date: 2023-07-28
Filing date: 2023-07-28
Publication date: 2024-12-27
Anticipated expiration: 2043-07-28
Also published as: CN116869835A

Abstract

The invention discloses a hydroxytyrosol inclusion with a stabilizing effect and a preparation method thereof. The raw materials of the hydroxytyrosol inclusion of the invention include hydroxytyrosol, solid lipids, an emulsifier and water. The invention adopts a water-in-oil method to prepare the hydroxytyrosol inclusion, combines supramolecular technology with solid nanolipid technology, and dissolves hydroxytyrosol in solid fats and oils by designing and screening solid lipids, and rapidly emulsifies and rapidly cools to prepare the hydroxytyrosol inclusion with a stabilizing effect. The hydroxytyrosol inclusion prepared by the invention has good stability, and long-term storage will not cause precipitation and discoloration of active substances. At the same time, the application scenarios are wider and can better meet the system types of most daily chemical products.

Description

Hydroxytyrosol inclusion with stabilizing effect and preparation method thereof

Technical Field

The invention belongs to the technical field of daily chemical industry, and particularly relates to a hydroxytyrosol inclusion with a stabilizing effect and a preparation method thereof.

Background

Whitening cosmetics are one of important cosmetic categories, and with the increase of economic level, consumers are increasingly demanding whitening cosmetics. Therefore, the development and utilization of the novel raw materials of the whitening agent have important practical significance for the development of whitening cosmetics.

Hydroxytyrosol (3, 4-Dihydroxyphenylethanol, figure 1) is a novel whitening agent molecule as the main active ingredient of olive leaf. Studies have shown that the melanin formation process starts with the oxidation of L-tyrosine to dopaquinone by tyrosinase, followed by a series of enzymatic oxidation of dopaquinone to melanin, both eumelanin (brownish black) and pheomelanin (reddish yellow), tyrosinase being the only key enzyme involved in melanin synthesis in organisms known to date. The hydroxytyrosol has tyrosinase inhibitory activity, can interfere in multiple stages of melanin formation, and has whitening effect. Meanwhile, the hydroxytyrosol has various effects of oxidation resistance, aging resistance and the like, and is a natural active molecule with great potential. However, as with many polyphenols, hydroxytyrosol is extremely sensitive to temperature and pH, is prone to discoloration, greatly hampering its use in cosmetics.

Currently, encapsulation techniques are commonly used to address the active discoloration problem, such as nanoemulsions, microemulsions, liposomes, solid lipid nanoparticles, and the like. However, these techniques are generally directed to oil-soluble actives, and the problem of discoloration of water-soluble actives is not effectively addressed. Because of the small molecular weight and the hydrophilic nature, the hydroxytyrosol is extremely soluble in water, can be mixed with water in any proportion, and is insoluble in common oil phases. Development of stabilized formulation technology for hydroxytyrosol is very challenging.

The problem of the easy discoloration of hydroxytyrosol as a whitening agent component greatly limits the application of hydroxytyrosol in product formulation. Patent document CN114099357a proposes a polyol-in-oil type nanoemulsion, which can improve the stability of hydroxytyrosol and inhibit its oxidation. However, the application of the polyol-in-oil type nanoemulsion in daily chemical products is quite limited. Most daily chemical products use water as a continuous phase, and cream emulsions of manufacturers belong to water-in-oil emulsion formulations. Therefore, the development of the hydroxytyrosol encapsulation technology in the aqueous phase has higher technical value and practical significance.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a hydroxytyrosol inclusion with a stabilizing effect and a preparation method thereof. The invention combines the supermolecular technology and the solid nano lipid technology, designs and screens solid lipid, utilizes the complexation property between the solid lipid and hydroxytyrosol, dissolves the hydroxytyrosol in solid grease, and prepares the hydroxytyrosol inclusion with stabilizing effect by rapid emulsification and rapid cooling. The inclusion containing hydroxytyrosol has better stability and can not separate out and change color of active substances after long-term storage.

The technical scheme of the invention is as follows:

A hydroxytyrosol inclusion with stabilizing effect is prepared from hydroxytyrosol, solid lipid, emulsifier and water.

Further, the solid lipid is a fatty acid, and the fatty acid comprises one or more of lauric acid, myristic acid, palmitic acid, eicosanoic acid and behenic acid.

Further, the emulsifier is a fatty alcohol polyether product corresponding to solid lipid, the number of units of polyether in the fatty alcohol polyether product is 5-40, and the emulsifier comprises one or more of laureth, myristyl alcohol polyether, cetyl alcohol polyether, stearyl alcohol polyether, eicosanol polyether and behenyl alcohol polyether.

Further, the mass ratio of solid lipid to hydroxytyrosol is >2:1, preferably 3-5:1.

Further, the mass ratio of the emulsifier to the solid lipid is 1:5-10, preferably 1:5-8.

Further, the preparation method comprises the following steps:

(1) Mixing and heating hydroxytyrosol and solid lipid to obtain a liquid oil phase, and adding an emulsifier to stir and dissolve to obtain a phase a;

(2) Taking water as a b phase, homogenizing the b phase under the water bath condition, and gradually adding the a phase prepared in the step (1) in the homogenizing process to obtain emulsion;

(3) Pouring the emulsion obtained in the step (2) into water, stirring, dissolving and cooling to form solid lipid nanoemulsion, namely the oil-in-water hydroxytyrosol inclusion.

Further, in the step (1), the heating temperature is 60-90 ℃ and the time is 15-25min, the stirring is mechanical stirring, the rotating speed is 200-300rpm, and the time is 3-5min.

Further, in step (2), the mass ratio of water to solid lipid is 4-9:1, preferably 4-8:1.

Further, in the step (2), the temperature of the water bath is 80-90 ℃, the homogenizing time is 3-5min, and the rotating speed is 10000-18000rpm.

Further, in the step (3), the mass ratio of the emulsion to the water is 1:3-10, the cooling is specifically that the homogenized emulsion is poured into the water and is rapidly cooled to 20-30 ℃ through rapid stirring, the stirring is mechanical stirring, the stirring speed is 300-400rpm, and the time is 10-15min.

The beneficial technical effects of the invention are as follows:

The invention combines the supermolecular technology and the solid nano lipid technology, screens solid lipid by design, utilizes the complexing property between the solid lipid and hydroxytyrosol, realizes a relatively stable supermolecular structure through secondary bonds such as hydrogen bonds and the like, so that the hydroxytyrosol is dissolved in the solid grease, and selects the emulsifier corresponding to the solid grease to construct the environment which is favorable for forming the supermolecular structure. The hydroxytyrosol inclusion with the stabilizing effect is prepared by rapid emulsification and rapid cooling, and the core is that hydroxytyrosol is encapsulated in solid oil drops of the nano emulsion and isolated from the external environment, so that the oxidation of hydroxytyrosol is avoided.

The inclusion containing hydroxytyrosol has better stability and can not separate out and change color of active substances after long-term storage. The hydroxytyrosol inclusion prepared by the invention has wider application scene and can more meet the system types of most daily chemical products.

Drawings

FIG. 1 is a structural diagram of hydroxytyrosol.

Fig. 2 is a hydroxytyrosol standard graph.

FIG. 3 is a graph showing the change of the retention rate of hydroxytyrosol with time under 50 ℃ storage conditions of hydroxytyrosol inclusion prepared in example 1 of the present invention.

FIG. 4 is a comparative graph of the preservation of hydroxytyrosol inclusion prepared in example 1 of the present invention at a constant temperature of 50℃for 14 d.

In the figure, 1, the initial state of the hydroxytyrosol inclusion prepared in the example 1 and 2, the state of the hydroxytyrosol inclusion prepared in the example 1 after being stored for 14d at the constant temperature of 50 ℃.

FIG. 5 shows hydroxytyrosol inclusions prepared in examples 1-12.

In the figures, 1, hydroxytyrosol inclusion prepared in example 1, 2, hydroxytyrosol inclusion prepared in example 2, 3, hydroxytyrosol inclusion prepared in example 3,4, hydroxytyrosol inclusion prepared in example 4,5, hydroxytyrosol inclusion prepared in example 5, 6, hydroxytyrosol inclusion prepared in example 6, 7, hydroxytyrosol inclusion prepared in example 7, 8, hydroxytyrosol inclusion prepared in example 8, 9, hydroxytyrosol inclusion prepared in example 9, 10, hydroxytyrosol inclusion prepared in example 10, 11, hydroxytyrosol inclusion prepared in example 11, 12, hydroxytyrosol inclusion prepared in example 12.

FIG. 6 shows the formation of a supramolecular system of behenic acid and hydroxytyrosol in hydroxytyrosol inclusion prepared in example 1 of the present invention.

FIG. 7 is an emulsion prepared in comparative example 1 of the present invention.

FIG. 8 is an emulsion prepared according to comparative examples 2-4 of the present invention.

FIG. 9 is an emulsion prepared in comparative example 5 of the present invention.

Detailed Description

The present invention will be described in detail below with reference to the drawings and examples.

Example 1:

The preparation method of the hydroxytyrosol inclusion with the stabilizing effect comprises the following steps:

Adding 4g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase, homogenizing the b phase with 80g of water serving as the b phase at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the a phase during homogenization to obtain emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 2:

Adding 4g of hydroxytyrosol and 20g of palmitic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of hexadecyl alcohol polyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the mixture to a clear and transparent state to obtain a phase a, homogenizing at 18000rpm for 3min with 80g of water serving as a phase b under the water bath condition at 80 ℃ to gradually add the phase a during the homogenizing process to obtain emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 3:

Taking a 100ml beaker, adding 4g of hydroxytyrosol, 10g of palmitic acid and 10g of behenic acid, heating at 60 ℃ for 25min to obtain a liquid oil phase, adding 2g of behenate polyether-20, mixing 2g of hexadecyl polyether-20 as an emulsifying agent, stirring at 200rpm for 5min to completely dissolve the mixture to a clear and transparent state to obtain a phase, taking 80g of water as a b phase, homogenizing the b phase at 10000rpm for 5min under the condition of 80 ℃ water bath, and gradually adding the a phase in the homogenizing process to obtain the emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 15min at 300rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 4:

Adding 4g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 3.3g of behenpolyether-20 serving as an emulsifier, stirring at 300rpm for 3min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase a, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath by taking 80g of water as the phase b, and gradually adding the phase a in the homogenizing process to obtain emulsion. In addition, 1000g of water is added into a 2L ml beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 5:

adding 4g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 90 ℃ for 15min to obtain a liquid oil phase, adding 2.5g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase a, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath by taking 80g of water as the phase b, and gradually adding the phase a in the homogenizing process to obtain emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 6:

Adding 4g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 2g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase, homogenizing the b phase with 80g of water serving as the b phase at 18000rpm for 3min under the condition of a 90 ℃ water bath, and gradually adding the a phase during homogenization to obtain emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 7:

Adding 4g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase, homogenizing the b phase with 120g of water serving as the b phase at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the a phase during homogenization to obtain emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 8:

Adding 4g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase, homogenizing the b phase with 160g of water serving as the b phase at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the a phase during homogenization to obtain emulsion. And adding 400g of water into a 1L beaker, homogenizing the emulsion, pouring the homogenized emulsion into 1200g of water, cooling to 20 ℃, stirring at 400rpm for 10min to completely dissolve the emulsion, and forming a solid lipid nano emulsion to obtain the hydroxytyrosol inclusion containing the active substances.

Example 9:

Adding 4g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase, homogenizing 180g of water serving as a phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain emulsion. In addition, a 1000ml beaker is prepared, 400g of water is added, the emulsion is homogenized and poured into 1200g of water, stirring is carried out for 10min at 400rpm, the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 10:

Taking a 100ml beaker, adding 5g of hydroxytyrosol and 20g of behenic acid, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase a, taking 80g of water serving as a phase b, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain the emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 11:

Taking a 100ml beaker, adding 6.7g of hydroxytyrosol and 20g of behenic acid, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase a, taking 80g of water as a phase b, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Example 12:

Adding 10g of hydroxytyrosol and 20g of behenic acid into a 100ml beaker, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase, homogenizing the b phase with 80g of water serving as the b phase at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the a phase during homogenization to obtain emulsion. In addition, 400g of water is added into a 1L beaker, the emulsion is homogenized and poured into 400g of water, and the mixture is stirred for 10min at 400rpm, so that the emulsion is completely dissolved and cooled to 20 ℃ to form solid lipid nano emulsion, and the hydroxytyrosol inclusion containing the active substances is obtained.

Comparative example 1:

The solid lipid in example 1 was replaced with behenyl alcohol, the remainder being unchanged, as comparative example 1. In particular, the method comprises the steps of,

Taking a 100ml beaker, adding 4g of hydroxytyrosol and 20g of behenyl alcohol, heating at 80 ℃ for 20min, adding 4g of behenyl alcohol polyether-20 serving as an emulsifier, and stirring at 200rpm for 5min, wherein the hydroxytyrosol cannot be dissolved in the oil phase.

Comparative example 2:

The solid lipid in example 1 was replaced with lauric acid, and the remainder was unchanged, as comparative example 2. Specifically, taking a 100ml beaker, adding 4g of hydroxytyrosol and 20g of lauric acid, heating at 80 ℃ for 20min, adding 4g of behenyl polyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the mixture to a clear and transparent state to obtain a phase a, taking 80g of water as a phase b, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain emulsion. A1L beaker was additionally prepared, 400g of water was added, the emulsion was homogenized, poured into 400g of water, stirred at 400rpm for 10min, cooled to 20℃and the resulting emulsion had solids precipitated, and the solids were allowed to stand to agglomerate and delaminate.

Comparative example 3:

The emulsifier of example 1 was replaced with tween 20 and the remainder was unchanged as comparative example 3. Specifically, taking a 100ml beaker, adding 4g of hydroxytyrosol and 20g of behenic acid, heating at 80 ℃ for 20min, adding 4g of tween 20 as an emulsifying agent, stirring at 200rpm for 5min to completely dissolve the mixture to a clear and transparent state to obtain a phase a, taking 80g of water as a phase b, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain emulsion. A1L beaker was additionally prepared, 400g of water was added, the emulsion was homogenized, poured into 400g of water, stirred at 400rpm for 10min, cooled to 20℃and the resulting emulsion had solids precipitated, and the solids were allowed to stand to agglomerate and delaminate.

Comparative example 4:

The amount of the emulsifier behenpolyether-20 used in example 1 was changed to 1g, and the remainder was unchanged, as comparative example 4. Specifically, a 100ml beaker is taken, 4g of hydroxytyrosol and 20g of behenic acid are added, heating is carried out for 20min at 80 ℃, then 1g of behenpolyether-20 is added as an emulsifying agent, stirring is carried out for 5min at 200rpm, the mixture is completely dissolved to a clear and transparent state, a phase a is obtained, 80g of water is taken as a phase b, the phase b is homogenized for 3min at 18000rpm under the condition of 80 ℃ water bath, and the phase a is gradually added in the homogenizing process, so that the emulsion is obtained. A1L beaker was additionally prepared, 400g of water was added, the emulsion was homogenized, poured into 400g of water, stirred at 400rpm for 10min, cooled to 20℃and the resulting emulsion had solids precipitated, and the solids were allowed to stand to agglomerate and delaminate.

Comparative example 5:

The amount of water used in example 1 was changed to 50g, and the remainder was unchanged, as comparative example 5. Specifically, taking a 100ml beaker, adding 4g of hydroxytyrosol and 20g of behenic acid, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase a, taking 50g of water as a phase b, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain emulsion. A1L beaker is additionally prepared, 400g of water is added, the emulsion is homogenized and poured into 400g of water, the mixture is stirred for 10min at 400rpm and cooled to 20 ℃, and the obtained emulsion is stored for 7 days at a constant temperature of 50 ℃ and has obvious color change.

Comparative example 6:

The "emulsion homogenized in example 1 was poured into 400g of water" was replaced with the "emulsion homogenized and poured into 200g of water", and the rest was the same, as comparative example 6. Specifically, taking a 100ml beaker, adding 4g of hydroxytyrosol and 20g of behenic acid, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase a, taking 80g of water as a phase b, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain emulsion. In addition, 200g of water is added into a 1L beaker, the emulsion is homogenized and poured into 200g of water, the mixture is stirred for 10min at 400rpm and cooled to 20 ℃, the lipid in the obtained emulsion is not cooled in time, and hydroxytyrosol is dissolved into the water phase, so that the encapsulation efficiency is low, the color change is obvious, and the stabilizing effect is poor.

Comparative example 7:

"stirring at 400rpm for 10min" in example 1 was replaced with "stirring at 100rpm for 5min", the remainder being the same as comparative example 7. Specifically, taking a 100ml beaker, adding 4g of hydroxytyrosol and 20g of behenic acid, heating at 80 ℃ for 20min to obtain a liquid oil phase, adding 4g of behenpolyether-20 serving as an emulsifier, stirring at 200rpm for 5min to completely dissolve the liquid oil phase into a clear and transparent state to obtain a phase a, taking 80g of water as a phase b, homogenizing the phase b at 18000rpm for 3min under the condition of 80 ℃ water bath, and gradually adding the phase a in the homogenizing process to obtain emulsion. In addition, a 1L beaker is prepared, 400g of water is added, the emulsion is homogenized and poured into 400g of water, stirring is carried out for 10min at 400rpm, the temperature is cooled to 20 ℃, the lipid in the obtained emulsion is not cooled in time, and hydroxytyrosol is dissolved in the water phase, so that the encapsulation rate is low, the color change is obvious, and the stabilizing effect is poor.

Test example:

(1) Hydroxytyrosol thermal stability:

The hydroxytyrosol inclusion prepared in example 1 is taken, the change of the retention rate of the hydroxytyrosol with time is detected, the specific detection method is that ① is used for respectively preparing 0.3, 0.6, 1.0, 1.3 and 1.5mg/ml of hydroxytyrosol methanol solution, an absorbance value is measured by an ultraviolet spectrophotometer to obtain a hydroxytyrosol standard curve, as shown in figure 2, ② is used for storing the prepared hydroxytyrosol inclusion at 50 ℃, a small amount of hydroxytyrosol inclusion is taken at regular time every day, methanol is used for diluting for a certain multiple (the absorbance is caused to fall within a range of 0.2-0.6), the absorbance value is measured by the ultraviolet spectrometer, the hydroxytyrosol standard curve is compared and multiplied by the dilution multiple to obtain the hydroxytyrosol content in the hydroxytyrosol inclusion, and ③ is used for calculating the hydroxytyrosol retention rate, namely, the n day hydroxytyrosol retention rate is=n day hydroxytyrosol content/0 day hydroxytyrosol content multiplied by 100% (the initial state of the hydroxytyrosol inclusion prepared in example 1). The results are shown in FIGS. 3 and 4. The graph of the change of the hydroxytyrosol retention rate with time is observed, the solid nano lipid emulsion prepared in the embodiment 1 is slow in decrease of the hydroxytyrosol retention rate with time under the storage condition of 50 ℃, the hydroxytyrosol retention rate is 90% in 25 days, meanwhile, the comparison between the solid nano lipid emulsion and the initial state at the temperature of 50 ℃ is observed, the active hydroxytyrosol is not precipitated in the emulsion, and the problems of color change, layering and the like are not caused.

(2) Relationship between hydroxytyrosol solubility and oil phase type:

The emulsion prepared in comparative example 1 was taken and observed for dissolution, and the results are shown in FIG. 7. It can be seen from the figure that the common oil phase such as fatty alcohol, triglyceride, mineral wax, higher fatty acid higher ester and other solid lipid can not dissolve hydroxytyrosol, and the type of the oil phase is critical to the formation of the emulsion proposed by the invention. The reason for this is that the carbonyl group of fatty acids can act as hydrogen bond acceptor and the hydroxyl group of hydroxytyrosol can act as hydrogen bond donor, both of which form a supramolecular system, as shown in fig. 6. After the formation of the supramolecules, hydrophilic groups are masked, the number is reduced, and the oil solubility is increased.

(3) Relationship of hydroxytyrosol solubility to oil phase/emulsifier adaptation:

The emulsion prepared in comparative example 2 was taken and observed for dissolution, and the results are shown in FIG. 8. From the figure, it can be seen that the emulsion prepared in comparative example 2 shows the phenomena of solid precipitation, solid agglomeration by standing and delamination, which indicates that the adaptation of the oil phase to the emulsifier is important for the formation of hydroxytyrosol inclusion as proposed in the present invention.

(4) Relationship of hydroxytyrosol solubility to emulsifier type:

The emulsion prepared in comparative example 3 was taken and observed for dissolution, and the results are shown in FIG. 8. From the figure, it can be seen that the emulsion prepared in comparative example 3 shows the phenomena of solid precipitation, solid agglomeration by standing and delamination, and the selection of the type of the emulsifier is critical to the formation of hydroxytyrosol inclusion as proposed in the present invention.

(5) Relationship between hydroxytyrosol solubility and emulsifier usage:

The emulsion prepared in comparative example 4 was taken and observed for dissolution, and the results are shown in FIG. 8. From the figure, it can be seen that the emulsion prepared in comparative example 4 shows the phenomena of solid precipitation, solid agglomeration by standing and delamination, and the selection of the amount of the emulsifier is critical to the formation of hydroxytyrosol inclusion as proposed in the present invention.

(6) Relationship between hydroxytyrosol stability and oil-water ratio:

The emulsion prepared in comparative example 5 was taken and observed for dissolution, and the results are shown in FIG. 9. From the graph, the emulsion prepared in comparative example 5 is stored for 7 days at a constant temperature of 50 ℃, and the color change is obvious, which indicates that the selection of the oil-water ratio is critical to the stability of the hydroxytyrosol inclusion provided by the invention, and the emulsion prepared in comparative example 5 has poor effect on the encapsulation of hydroxytyrosol.

The above is only a preferred embodiment of the present invention, and the present invention is not limited to the above examples. It is to be understood that other modifications and variations which may be directly derived or contemplated by those skilled in the art without departing from the spirit and concepts of the present invention are deemed to be included within the scope of the present invention.

Claims

1. A hydroxytyrosol inclusion with a stabilizing effect, characterized in that the raw materials of the hydroxytyrosol inclusion include hydroxytyrosol, solid lipids, an emulsifier and water;

The solid lipid is a fatty acid, and the fatty acid includes one or more of palmitic acid, eicosanoic acid, and behenic acid;

The emulsifier is a fatty alcohol polyether product corresponding to the solid lipid; the number of polyether units in the fatty alcohol polyether product is 5-40; the emulsifier includes one or more of cetyl alcohol polyether, eicosanol polyether, and behenyl alcohol polyether;

The mass ratio of the solid lipid to hydroxytyrosol is >2:1;

The mass ratio of the emulsifier to the solid lipid is 1:5-10;

The preparation method of the hydroxytyrosol inclusion body comprises the following steps:

(1) mixing hydroxytyrosol and solid lipids and heating them to obtain a liquid oil phase, and then adding an emulsifier and stirring to dissolve them to obtain a phase a;

(2) using water as phase b, homogenizing phase b in a water bath, and gradually adding phase a prepared in step (1) during the homogenization process to obtain an emulsion;

(3) pouring the emulsion of step (2) into water, dissolving by stirring and cooling to form a solid lipid nanoemulsion, i.e., hydroxytyrosol inclusion bodies;

In step (2), the mass ratio of water to solid lipid is 4-9:1;

In step (3), the mass ratio of the emulsion to water is 1:3-10; the cooling is specifically pouring the homogenized emulsion into water and rapidly cooling it to 20-30°C by rapid stirring; the stirring is mechanical stirring at a speed of 300-400 rpm for 10-15 min.

2. Hydroxytyrosol inclusion body according to claim 1, is characterized in that, the mass ratio of described solid lipid and hydroxytyrosol is 3-5:1.

3. Hydroxytyrosol inclusion body according to claim 1, is characterized in that, the mass ratio of described emulsifier and solid lipid is 1:5-8.

4. The hydroxytyrosol inclusion body according to claim 1, characterized in that, in step (1), the heating temperature is 60-90° C. and the time is 15-25 min; the stirring is mechanical stirring, the rotation speed is 200-300 rpm, and the time is 3-5 min.

5. The hydroxytyrosol inclusion body according to claim 1, wherein in step (2), the mass ratio of water to solid lipid is 4-8:1.

6. The hydroxytyrosol inclusion body according to claim 1, characterized in that, in step (2), the temperature of the water bath is 80-90°C; the homogenization time is 3-5min, and the rotation speed is 10000-18000rpm.