CN109924491A - A kind of dihydromyricetin solid-state self-emulsifying material and its preparation method and application - Google Patents

A kind of dihydromyricetin solid-state self-emulsifying material and its preparation method and application Download PDF

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CN109924491A
CN109924491A CN201910255323.8A CN201910255323A CN109924491A CN 109924491 A CN109924491 A CN 109924491A CN 201910255323 A CN201910255323 A CN 201910255323A CN 109924491 A CN109924491 A CN 109924491A
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dihydromyricetin
solid
emulsifying
self
state self
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夏强
王丹彤
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Southeast University
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Southeast University
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Abstract

The invention discloses a kind of dihydromyricetin solid-state self-emulsifying materials and its preparation method and application, which includes following components by mass parts: 2~7 parts of dihydromyricetin, 20~43 parts of lipid components, 15~20 parts of hydrophilic surfactant active, 5~14 parts of hydrophobic surfactant, 35~60 parts of solid absorbent;Preparation method is as follows: 1) dihydromyricetin and lipid components being mixed to clarification as oily phase;2) oily phase, hydrophilic surfactant and hydrophobic surfactant are mixed to form uniform phase system;3) by uniform phase system and solid absorbent liquid dispersed in dehydrated alcohol, being sufficiently stirred, which is adsorbed on it sufficiently in solid absorbent, obtains dispersion liquid;4) dispersion liquid rotary evaporation is dispelled into dehydrated alcohol, be then ground up, sieved to obtain the final product.The material has good water-soluble and stability, and preparation process is simple controllable, reproducible, can be applied to the preparation of functional food.

Description

A kind of dihydromyricetin solid-state self-emulsifying material and its preparation method and application
Technical field
The present invention relates to a kind of dihydromyricetin solid-state self-emulsifying materials and its preparation method and application, belong to functional food Carrier system technical field in technology of preparing.
Background technique
China is the country of early start wine brewing in the world, and spirits culture is also permeated in many Social Cultures, early had become Essential a part in daily life.However insobriety, cause alcohol to accumulate, can make all multi visceras such as liver and spleen stomach by Damage, has become a more serious public health problem at present.So far, U.S. FDA only has approved 3 and can be used for The oral drugs of alcoholism are treated, i.e. naltrexone, Acamprosate and support adjoins ester.But it is found in animal experiment and clinical research, Many Chinese traditional herbs ingredients, such as hoveniae semoveniae semen, fructus lycii, pueraria lobata also show the preferable effect for improving alcoholism.Through Constituents extraction analysis is crossed it is found that the main active that these Chinese herbal medicines play effect is mostly natural plants flavone compound, Compared with horn of plenty and wherein there is significant physiological activity with the content of dihydromyricetin (DMY) again, Chinese Soclety of Nutrition is also recommended Daily DMY intake is 960mg.Dihydromyricetin, also known as ampeloptin, ampelopsin, molecular formula C15H12O8, average molecular matter Amount 320.25 is a kind of natural polyphenol hydroxyl flavanonol, belongs to flavone compound, is widely present in ampelopsis grossdentata plant In the cauline leaf of object, content may be up to 30%.
Research confirms that dihydromyricetin can extend drunk tolerance time, and shortening is sobered up the time, plays and resists alcoholism It is acted on alcohol dependence, there is preferable anti-intoxication alcohol neutralizing effect.Its play effect molecular mechanism at present it is believed that with DMY can be acted on the Benzodiazepine action site on ethyl alcohol competitive binding GABAARs without Benzodiazepine sample, to inhibit Influence of the alcohol to GABAARs is closely related.In addition, DMY also shows preferable therapeutic effect to Ethanol hepatic injury, can have Effect reduces the level of malonaldehyde and triacylglycerol in liver, improves reduced glutathione level, mitigates hepatic cell fattydegeneration, The effect may be by improving liver cell oxidation resistance, to inhibit membrane lipid peroxidatio caused by ethyl alcohol to realize. But the water solubility of dihydromyricetin and fat-soluble poor and stability of molecule are poor, easily by Fe during processing and storage3+、 Al3+、Cu2+Equal metal ions, oxygen and light oxidation, and the raising of pH value and temperature can accelerate its oxidation course.Therefore, It is significantly limited in the bioavilability and application of functional food field.
Self-emulsifying systems are made of lipid and surfactant, are generally used for load fat-soluble active ingredient, are situated between in water The O/W nanoemulsions of partial size about 100nm can be formed in matter through gentle agitation;If directly entering in vivo by oral administration, can also disappear Change and spontaneously forms uniform O/W nanoemulsions in aqueous medium under the creeping effect in road.Common self-emulsifying systems include liquid With two kinds of dosage forms of solid-state.Liquid self-emulsifying systems can dramatically increase the absorption and utilization of active constituent, and determine formula group Cheng Hou, it is only necessary to active constituent is dissolved in specific formula, preparation process very simple is suitble to large-scale production.But Since its rouge content is higher, oral bad adaptability is often packaged applies in soft, hard capsule.In addition, liquid self-emulsifying systems are made For a kind of liquid formulation will necessarily exist as between liquid active ingredient interaction, between active constituent and auxiliary material and capsule shells The limiting factors such as interaction, low-temperature precipitation, inconvenient to carry and stability is poor.Therefore, liquid is adsorbed using solid absorbent Self-emulsifying systems in conjunction with freeze-drying, spray drying, solvent evaporation, squeeze out the-different drying means such as round as a ball, so that it may Controllable solidification liquid self-emulsifying systems, obtain solid-state self-emulsifying systems.In the high load that reservation liquid self-emulsifying systems have While the advantage of amount and bioavilability, defect existing for liquid preparation is overcome.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of dihydromyricetin solid-state self-emulsifying material and preparation method thereof and Using carrying out package processing to dihydromyricetin using solid-state self-emulsifying systems, prepare a kind of two applied in functional food Hydrogen myricetin solves low-solubility, low stability and low bioavilability of dihydromyricetin etc. using bottleneck, makes it preferably Move towards commercialization process.
Technical solution: the present invention provides a kind of dihydromyricetin solid-state self-emulsifying materials, and the material is according to mass parts packet Include following components:
Wherein:
The lipid components are linseed oil, Miglyol 812N, olive oil, coconut oil, grape seed oil, Australia heavily fortified point One of fruit oil, sunflower oil, camellia seed oil or corn oil are a variety of.
The hydrophilic surfactant active is polysorbas20, polysorbate40, polysorbate60, Tween 80, six polyglycerol monooleates, ten One of polyglycerol monooleate, six polyglycereol monolaurates or ten polyglycereol monolaurates are a variety of.
The hydrophobic surfactant be polyglycerol polyricinoleate, polyglycerol monooleate, ten polyglycereol, ten oleate, Any one in span 40, sorbester p18 or sorbester p17.
The solid absorbent is silica, calcium phosphate dibasic anhydrous, porous-starch, maltodextrin, PVP K30, low Replace any one in hydroxypropyl cellulose or microcrystalline cellulose.
The partial size that the dihydromyricetin solid-state self-emulsifying material is dispersed in micro emulsion formed in aqueous medium is less than 500nm。
The present invention also provides a kind of preparation method of dihydromyricetin solid-state self-emulsifying material, this method includes following step It is rapid:
1) it is stirred at room temperature to solution to become after in proportion mixing dihydromyricetin and lipid components and be clarified, as oil Phase;
2) oily phase, hydrophilic surfactant and hydrophobic surfactant are thoroughly mixed to form in room temperature in proportion One phase obtains dihydromyricetin liquid self-emulsifying systems;
3) by dihydromyricetin liquid self-emulsifying systems and solid absorbent liquid dispersed in dehydrated alcohol, at room temperature It is sufficiently stirred, is adsorbed on dihydromyricetin liquid self-emulsifying systems sufficiently in solid absorbent, obtain dihydromyricetin solid-state certainly Emulsification system alcohol dispersion liquid;
4) dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid rotary evaporation is dispelled into dehydrated alcohol, it is then ground It sieves up to dihydromyricetin solid-state self-emulsifying material.
Wherein:
In proportion by dihydromyricetin liquid self-emulsifying systems and solid absorbent liquid dispersed in nothing described in step 3) In water-ethanol, the mass parts ratio of dihydromyricetin liquid self-emulsifying systems and solid absorbent is 45~65 parts: 35~55 parts.
The temperature of rotary evaporation process described in step 4) is 40 DEG C~50 DEG C;Described is then ground up, sieved up to dihydro In myricetin solid-state self-emulsifying material, refer to that dihydromyricetin solid-state self-emulsifying material passes through 60 meshes.
The present invention also provides a kind of application of dihydromyricetin solid-state self-emulsifying material, the dihydromyricetin solid-state is certainly newborn Change the preparation that material is applied to functional food.
The utility model has the advantages that compared with prior art, present invention has the advantage that
1) present invention carries out package processing to dihydromyricetin using solid-state self-emulsifying systems, and obtained dihydromyricetin is solid State self-emulsifying material, it is with good stability, the dissolubility of dihydromyricetin is improved, to improve its bioavilability;
2) each component has very high safety in the formula of dihydromyricetin solid-state self-emulsifying material, non-stimulated to body Property, non-toxic, can be used as nutritional additive is used in compounding with food formula, and compatibility is good, can be widely used for functional food field;
3) preparation method is simply controllable, reproducible.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of dihydromyricetin solid-state self-emulsifying material of the present invention.
Specific embodiment
The invention will be further described with reference to embodiments.These embodiments are not limited to for illustrating the present invention It limits the scope of the invention.Implementation condition used in the examples can do further adjustment according to the condition of specific producer.
Embodiment 1
A kind of dihydromyricetin solid-state self-emulsifying material, the partial size for being dispersed in micro emulsion formed in aqueous medium are less than 500nm, Include following components according to mass parts:
Preparation method the following steps are included:
1) 0.6g dihydromyricetin, 6g linseed oil are weighed, after dihydromyricetin and linseed oil are mixed at room temperature Magnetic agitation is until solution becomes clarification, as oily phase;
2) six polyglycerol monooleate of 4.5g, 2.4g sorbester p18 are weighed, by oily phase, six polyglycerol monooleates and sorbester p18 Homogeneous phase is thoroughly mixed to form after mixing in room temperature, obtains dihydromyricetin liquid self-emulsifying systems;
3) dihydromyricetin liquid self-emulsifying systems 13.5g and microcrystalline cellulose 16.5g then are weighed, by dihydromyricetin Liquid self-emulsifying systems and microcrystalline cellulose are scattered in appropriate dehydrated alcohol, are sufficiently stirred at room temperature, and dihydromyricetin is made Liquid self-emulsifying systems are sufficiently adsorbed in solid absorbent microcrystalline cellulose, obtain dihydromyricetin solid-state self-emulsifying systems ethyl alcohol Dispersion liquid;
4) dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid is dispelled into dehydrated alcohol in 40 DEG C of rotary evaporations, then Ground 60 mesh of mistake is up to dihydromyricetin solid-state self-emulsifying material.
1.0g dihydromyricetin solid-state self-emulsifying material is added in 100g deionized water, after evenly dispersed, utilizes grain Average grain diameter is 147.3 ± 2.4nm after degree instrument obtains dihydromyricetin solid-state self-emulsifying systems water dispersion, and 25 DEG C are placed at room temperature for 1 Its average grain diameter is 152.7 ± 3.1nm after a month, and change of size no significant difference shows that it has good stability.
Embodiment 2
The partial size that a kind of dihydromyricetin solid-state self-emulsifying material is dispersed in micro emulsion formed in aqueous medium is less than 500nm, Include following components according to mass parts:
Preparation method the following steps are included:
1) 0.8g dihydromyricetin, 6g olive oil are weighed, magnetic force at room temperature after dihydromyricetin and olive oil are mixed Stirring is until solution becomes clarification, as oily phase;
2) ten polyglycerol monooleate of 6g and 4.2g sorbester p18 are weighed, by oily phase, ten polyglycerol monooleates and sorbester p18 Homogeneous phase is thoroughly mixed to form after mixing in room temperature, obtains dihydromyricetin liquid self-emulsifying systems;
3) dihydromyricetin liquid self-emulsifying systems 17g and calcium phosphate dibasic anhydrous 13g then are weighed, by dihydromyricetin liquid State self-emulsifying systems and calcium phosphate dibasic anhydrous are scattered in appropriate dehydrated alcohol, are sufficiently stirred at room temperature, and dihydromyricetin is made Liquid self-emulsifying systems are sufficiently adsorbed in solid absorbent calcium phosphate dibasic anhydrous, obtain dihydromyricetin solid-state self-emulsifying systems second Alcohol dispersion liquid;
4) dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid is dispelled into dehydrated alcohol in 50 DEG C of rotary evaporations, then Ground 60 mesh of mistake is up to dihydromyricetin solid-state self-emulsifying material.
1.0g dihydromyricetin solid-state self-emulsifying material is added in 100g deionized water, after evenly dispersed, utilizes grain Average grain diameter is 98.5 ± 1.2nm after degree instrument obtains dihydromyricetin solid-state self-emulsifying systems water dispersion, and 25 DEG C are placed at room temperature for 1 Its average grain diameter is 101.2 ± 2.2nm after month, and change of size no significant difference shows that it has good stability.
Embodiment 3
The partial size that a kind of dihydromyricetin solid-state self-emulsifying material is dispersed in micro emulsion formed in aqueous medium is less than 500nm, Include following components according to mass parts:
Preparation method the following steps are included:
1) 1g dihydromyricetin, 8g corn oil are weighed, magnetic force stirs at room temperature after dihydromyricetin and corn oil are mixed It mixes until solution becomes clarification, as oily phase;
2) ten polyglycereol monolaurate of 5g and 2g polyglycerol monooleate are weighed, by oily phase, ten polyglycereol mono laurates It is thoroughly mixed to form homogeneous phase in room temperature after ester and polyglycerol monooleate mixing, obtains dihydromyricetin liquid self-emulsifying body System;
3) dihydromyricetin liquid self-emulsifying systems 16g and porous-starch 14g then are weighed, certainly by dihydromyricetin liquid Emulsification system and porous-starch are scattered in appropriate dehydrated alcohol, are sufficiently stirred at room temperature, make dihydromyricetin liquid from cream Change system is sufficiently adsorbed in solid absorbent porous-starch, obtains dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid;
4) dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid is dispelled into dehydrated alcohol in 50 DEG C of rotary evaporations, then Ground 60 mesh of mistake is up to dihydromyricetin solid-state self-emulsifying material.
1.0g dihydromyricetin solid-state self-emulsifying material is added in 100g deionized water, after evenly dispersed, utilizes grain Average grain diameter is 198.5 ± 1.2nm after degree instrument obtains dihydromyricetin solid-state self-emulsifying systems water dispersion, and 25 DEG C are placed at room temperature for 1 Its average grain diameter is 201.2 ± 2.2nm after a month, and change of size no significant difference shows that it has good stability.
Embodiment 4
The partial size that a kind of dihydromyricetin solid-state self-emulsifying material is dispersed in micro emulsion formed in aqueous medium is less than 500nm, Include following components according to mass parts:
Preparation method the following steps are included:
1) 1.2g dihydromyricetin, 8.8g camellia seed oil are weighed, in room temperature after dihydromyricetin and camellia seed oil are mixed Lower magnetic agitation is until solution becomes clarification, as oily phase;
2) 3g Tween 80,2g polysorbas20 and 3g span 40 are weighed, after oily phase, Tween 80, polysorbas20 and span 40 are mixed It is thoroughly mixed to form homogeneous phase in room temperature, obtains dihydromyricetin liquid self-emulsifying systems;
3) dihydromyricetin liquid self-emulsifying systems 18g and silica 1 2g then are weighed, certainly by dihydromyricetin liquid Emulsification system and silica are scattered in appropriate dehydrated alcohol, are sufficiently stirred at room temperature, make dihydromyricetin liquid from cream Change system is sufficiently adsorbed in solid absorbent silica, obtains dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid;
4) dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid is dispelled into dehydrated alcohol in 45 DEG C of rotary evaporations, then Ground 60 mesh of mistake is up to dihydromyricetin solid-state self-emulsifying material.
1.0g dihydromyricetin solid-state self-emulsifying material is added in 100g deionized water, after evenly dispersed, utilizes grain Average grain diameter is 305.2 ± 5.1nm after degree instrument obtains dihydromyricetin solid-state self-emulsifying systems water dispersion, and 25 DEG C are placed at room temperature for 1 Its average grain diameter is 309.5 ± 2.4nm after a month, and change of size no significant difference shows that it has good stability.
Embodiment 5
The partial size that a kind of dihydromyricetin solid-state self-emulsifying material is dispersed in micro emulsion formed in aqueous medium is less than 500nm, Include following components according to mass parts:
Preparation method the following steps are included:
1) 1.5g dihydromyricetin, 12g coconut oil are weighed, magnetic force at room temperature after dihydromyricetin and coconut oil are mixed Stirring is until solution becomes clarification, as oily phase;
2) 4.5g polysorbate60 and 1.5g polyglycerol polyricinoleate are weighed, oily phase, polysorbate60 and polyglycerol polyricinoleate are mixed Homogeneous phase is thoroughly mixed to form after conjunction in room temperature, obtains dihydromyricetin liquid self-emulsifying systems;
3) dihydromyricetin liquid self-emulsifying systems 19.5g and maltodextrin 10.5g then are weighed, by dihydromyricetin liquid State self-emulsifying systems and maltodextrin are scattered in appropriate dehydrated alcohol, are sufficiently stirred at room temperature, and dihydromyricetin liquid is made Self-emulsifying systems are sufficiently adsorbed in solid absorbent maltodextrin, obtain the dispersion of dihydromyricetin solid-state self-emulsifying systems ethyl alcohol Liquid;
4) dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid is dispelled into dehydrated alcohol in 45 DEG C of rotary evaporations, then Ground 60 mesh of mistake is up to dihydromyricetin solid-state self-emulsifying material.
1.0g dihydromyricetin solid-state self-emulsifying material is added in 100g deionized water, after evenly dispersed, utilizes grain Average grain diameter is 472.1 ± 0.2nm after degree instrument obtains dihydromyricetin solid-state self-emulsifying systems water dispersion, and 25 DEG C are placed at room temperature for 1 Its average grain diameter is 489.5 ± 5.4nm after a month, and change of size no significant difference shows that it has good stability.

Claims (10)

1. a kind of dihydromyricetin solid-state self-emulsifying material, it is characterised in that: the material includes following components according to mass parts:
2. a kind of dihydromyricetin solid-state self-emulsifying material as described in claim 1, it is characterised in that: the lipid components are Linseed oil, Miglyol 812N, olive oil, coconut oil, grape seed oil, macadimia nut oil, sunflower oil, camellia seed oil Or one of corn oil or a variety of.
3. a kind of dihydromyricetin solid-state self-emulsifying material as described in claim 1, it is characterised in that: the hydrophilic surface Activating agent be polysorbas20, polysorbate40, polysorbate60, Tween 80, six polyglycerol monooleates, ten polyglycerol monooleates, six gather it is sweet One of oily monolaurate or ten polyglycereol monolaurates are a variety of.
4. a kind of dihydromyricetin solid-state self-emulsifying material as described in claim 1, it is characterised in that: the hydrophobic surface Activating agent is polyglycerol polyricinoleate, polyglycerol monooleate, ten polyglycereol, ten oleate, span 40, sorbester p18 or sapn Any one in 80.
5. a kind of dihydromyricetin solid-state self-emulsifying material as described in claim 1, it is characterised in that: the solid absorbent For silica, calcium phosphate dibasic anhydrous, porous-starch, maltodextrin, PVP K30, low-substituted hydroxypropyl cellulose or micro- Any one in crystalline cellulose.
6. a kind of dihydromyricetin solid-state self-emulsifying material as described in claim 1, it is characterised in that: the dihydromyricetin The partial size that plain solid-state self-emulsifying material is dispersed in micro emulsion formed in aqueous medium is less than 500nm.
7. a kind of preparation method of the dihydromyricetin solid-state self-emulsifying material as described in Claims 1 to 5 is any, feature exist In: method includes the following steps:
1) it is stirred at room temperature to solution to become after in proportion mixing dihydromyricetin and lipid components and be clarified, as oily phase;
2) oily phase, hydrophilic surfactant and hydrophobic surfactant are thoroughly mixed to form in room temperature in proportion uniform Phase obtains dihydromyricetin liquid self-emulsifying systems;
3) by dihydromyricetin liquid self-emulsifying systems and solid absorbent liquid dispersed in dehydrated alcohol, at room temperature sufficiently Stirring, is adsorbed on dihydromyricetin liquid self-emulsifying systems sufficiently in solid absorbent, obtains dihydromyricetin solid-state self-emulsifying System alcohol dispersion liquid;
4) dihydromyricetin solid-state self-emulsifying systems alcohol dispersion liquid rotary evaporation is dispelled into dehydrated alcohol, be then ground up, sieved i.e. Obtain dihydromyricetin solid-state self-emulsifying material.
8. a kind of preparation method of dihydromyricetin solid-state self-emulsifying material as claimed in claim 6, it is characterised in that: step 3) described in proportion by dihydromyricetin liquid self-emulsifying systems and solid absorbent liquid dispersed in dehydrated alcohol, dihydro The mass parts ratio of myricetin liquid self-emulsifying systems and solid absorbent is 45~65 parts: 35~55 parts.
9. a kind of preparation method of dihydromyricetin solid-state self-emulsifying material as claimed in claim 6, it is characterised in that: step 4) temperature of the rotary evaporation process described in is 40 DEG C~50 DEG C;Described is then ground up, sieved up to dihydromyricetin solid-state certainly In emulsified material, refer to that dihydromyricetin solid-state self-emulsifying material passes through 60 meshes.
10. a kind of application of the dihydromyricetin solid-state self-emulsifying material as described in Claims 1 to 5 is any, it is characterised in that: The dihydromyricetin solid-state self-emulsifying material is applied to the preparation of functional food.
CN201910255323.8A 2019-04-01 2019-04-01 A kind of dihydromyricetin solid-state self-emulsifying material and its preparation method and application Pending CN109924491A (en)

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CN113966839A (en) * 2021-10-14 2022-01-25 恒枫食品科技有限公司 Composite emulsion containing walnut oil and dihydromyricetin and preparation method thereof
CN113966839B (en) * 2021-10-14 2024-05-14 恒枫食品科技有限公司 Composite emulsion containing walnut oil and dihydromyricetin and preparation method thereof
CN115252455A (en) * 2022-07-02 2022-11-01 堇色生物科技(中山)有限责任公司 Dihydromyricetin nanoemulsion and preparation method and application thereof

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