阅读说明：本技术 一种可用于香精及药物无定型化的微胶囊及其制备方法 (Microcapsule for essence and medicine amorphous and preparation method thereof ) 是由 杨成 范赛英 王靖 于 2020-08-10 设计创作，主要内容包括：本发明公开了一种可用于香精及药物无定型化的微胶囊及其制备方法；其中,一种可用于香精及药物无定型化的微胶囊纳米乳液的制备方法,其包括,制备复合脂质油相；用辛烯基琥珀酸酯化淀粉制备水相；混合所述水相和所述油相,均质后高压均质,即得高载量高热稳定性微胶囊纳米乳液；所述制备复合脂质油相,其为将乳木果油、蜡和有效成分加热搅拌,融化至充分混溶；本发明制备的微胶囊流动性好,载量高,包封率高,具有非常优异的热稳定性,降低保存要求且延长了保存期限。(The invention discloses a microcapsule for the amorphous of essence and medicine and a preparation method thereof; the preparation method of the microcapsule nano emulsion for the amorphous essence and medicine comprises the following steps of preparing a composite lipid oil phase; preparing an aqueous phase from starch esterified with octenyl succinate; mixing the water phase and the oil phase, homogenizing under high pressure to obtain high-loading high-thermal-stability microcapsule nano emulsion; the preparation of the composite lipid oil phase comprises the steps of heating and stirring shea butter, wax and active ingredients, and melting the materials until the materials are fully mixed and dissolved; the microcapsule prepared by the invention has good fluidity, high loading capacity, high encapsulation rate, excellent thermal stability, reduced storage requirement and prolonged storage life.)

1. A method for preparing microcapsule nano emulsion for essence and medicine amorphous is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,

preparing a composite lipid oil phase;

preparing an aqueous phase from starch esterified with octenyl succinate;

and mixing the water phase and the oil phase, homogenizing under high pressure to obtain the high-loading high-thermal-stability microcapsule nano emulsion.

2. The method for preparing the microcapsule nano emulsion for the amorphization of the essence and the medicine according to claim 1, wherein the method comprises the following steps: the preparation of the composite lipid oil phase comprises the steps of heating and stirring shea butter, wax and active ingredients, and melting the materials until the materials are fully mixed and dissolved.

3. The method for preparing the microcapsule nano emulsion for the amorphization of the essence and the medicine according to claim 2, wherein the method comprises the following steps: the mass ratio of the shea butter, the wax and the effective components is (1-7): (0-12): (3-15).

4. The process for preparing the microcapsule nanoemulsion usable for the amorphization of flavors and drugs according to claim 2 or 3, wherein: the effective components include one or more of menthol, eugenol, vanillin, camphor, citronellal, eucalyptol, limonene, curcumin, resveratrol, furan aniline acid, propranolol and flurbiprofen.

5. The process for preparing the microcapsule nanoemulsion usable for the amorphization of flavors and drugs according to claim 2 or 3, wherein: the wax comprises one or more of candelilla wax, beeswax, carnauba wax, microcrystalline wax, and ozokerite; the octenyl succinate starch comprises one or more of Capsul, Purity Gum Ultra, HI-CAP 100.

6. The method for preparing the microcapsule nanoemulsion usable for the amorphization of flavors and drugs according to any one of claims 1 to 5, characterized in that: the homogenizing time is 0.5-3 min, and the rotating speed is 8000-15000 rpm/min; and (3) performing high-pressure homogenization, wherein the homogenization pressure is 600-1000 bar, and performing circulation.

7. The use of the microcapsule nanoemulsion as claimed in any one of claims 1 to 6 for the amorphization of flavors and drugs, wherein the microcapsule nanoemulsion comprises: can be used in one or more of lipstick, soap, toilet powder, deodorant stick, lotion, cream, and facial mask.

8. A method for preparing the microcapsules for the amorphization of essences and drugs according to any one of claims 1 to 6, which is characterized in that: spray drying the microcapsule nano emulsion for the amorphous essence and medicine;

wherein the mass ratio of the oil phase to the water phase is 0.8-1.5; the mass ratio of the effective components to the octenyl succinic acid esterified starch is (3-12): (18-27).

9. The process for preparing microcapsules useful in the amorphization of fragrances and pharmaceuticals of claim 8, wherein: the spray drying is carried out, wherein the feeding amount is 10-30 ml/min, the air inlet temperature is 160-190 ℃, and the air outlet temperature is 75-90 ℃.

10. A microcapsule for perfume and drug amorphization according to any of claims 8 to 9, characterized in that: the loading is more than or equal to 15 percent.

Technical Field

The invention belongs to the technical field of microcapsules, and particularly relates to a microcapsule for amorphization of essence and medicines and a preparation method thereof.

Background

The volatile active compounds, wherein the flavors and fragrances occupy a large category, have wide application in the cosmetic, food and pharmaceutical industries. However, volatile actives are unstable, sensitive to light, heat, oxygen and moisture, and due to their volatile nature, are easily lost during processing and use, are not conducive to transportation and storage, and limit the practical use of volatile compounds. In order to solve these problems, active materials can be encapsulated in microcapsules by microencapsulation technology, which has the effects of changing the existing state of the materials, protecting sensitive components, reducing volatility, controlling release, prolonging storage time, and the like.

The other class of active ingredients, i.e., the second class (poor water solubility and permeability) and the fourth class (poor water solubility and permeability) of the biopharmaceutical classification system, such as curcumin, resveratrol, indomethacin, progesterone, etc., have low drug bioavailability and influence on drug administration effect due to easy crystallization and poor water solubility. One of the important ways to improve the solubility and dissolution rate of such drugs and thus the bioavailability is by destroying or preventing the long-range crystalline molecular order of the drug, making it amorphized, to form an amorphous state.

The spray drying method is the most widely adopted method in the preparation method of the essence and flavor microcapsule, and has the characteristics of simple operation, low cost, easy continuous production, high drying speed, good product dispersibility and solubility and the like. The conventional spray drying process steps can be described simply as: uniformly dispersing the core material in the wall material solution to prepare a solution, an emulsion or a suspension, sending the test solution into spray drying equipment, atomizing the test solution into liquid drops by airflow, uniformly dispersing the liquid drops in hot airflow to quickly evaporate the solvent for dissolving the wall material, and solidifying the wall material to form the microcapsule. There are three main classes of wall materials commonly used for spray drying: carbohydrates, hydrocolloids, proteins.

Solid Lipid Nanoparticles (SLNs) are emulsion-type coating carriers, one or more high-melting-point solid lipids are used as carriers, active substances are coated in lipid cores, and the active substances are dispersed in surfactant aqueous solution to form a dispersion. Numerous studies have shown that SLN inhibits the crystallization of active species.

Menthol, also known as menthol, is the main component of essential oils of peppermint and is an important flavor. Menthol has a fresh mint fragrance, can stimulate cold receptors on the skin without causing actual temperature change, has the effects of local itching relieving, pain relieving, cooling and slight local anesthesia, and is widely applied to the production of foods, medicines, toothpaste, oral hygiene products, cosmetics, cigarettes and the like. In the food industry, menthol can be used as an aromatizer for foods such as beverages, cakes, candies, chewing gums and the like to improve the flavor of the foods. It can be used as irritant in medicine, and has effects in refreshing and relieving itching; it can be used for treating headache, and inflammation of nose, pharynx, and larynx by oral administration. Can be used in toothpaste and oral hygiene products for deodorizing and refreshing. In the cosmetic industry, the product can be used as a freshener, a penetration enhancer or an essence and added into products of various formulations.

However, menthol is poor in stability, volatile (especially, the volatile loss is more serious under high temperature conditions), easily crystallized, poor in water solubility (0.4mg/L), irritating to the skin and eyes, affecting the use effect, and being safely and effectively applied to cosmetic formulations, which is a problem. The volatility of the menthol can be reduced through microcapsule embedding, external components are isolated, and the menthol is released in a controlled manner, so that the effects of protecting a core material, slowly releasing, durably cooling and improving the thermal stability are achieved.

The essence and flavor microcapsule prepared by the spray drying method mostly adopts polymer wall materials, such as modified starch, Arabic gum, polyvinyl alcohol and the like, but the problems of low loading capacity, high surface oil content, poor thermal stability and the like generally exist.

Disclosure of Invention

This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.

The present invention has been made in view of the above-mentioned technical drawbacks.

Therefore, as one aspect of the present invention, the present invention overcomes the defects existing in the prior art, and provides a microcapsule for the amorphous of essence and medicine and a preparation method thereof.

In order to solve the technical problems, the invention provides the following technical scheme: a method for preparing microcapsule nanometer emulsion for flavoring essence and medicine amorphous comprises preparing composite lipid oil phase; preparing an aqueous phase from starch esterified with octenyl succinate; and mixing the water phase and the oil phase, homogenizing under high pressure to obtain the high-loading high-thermal-stability microcapsule nano emulsion.

The preferable scheme of the preparation method of the microcapsule nano emulsion for the amorphous essence and medicine is as follows: the preparation of the composite lipid oil phase comprises the steps of heating and stirring shea butter, wax and active ingredients, and melting the materials until the materials are fully mixed and dissolved;

the preferable scheme of the preparation method of the microcapsule nano emulsion for the amorphous essence and medicine is as follows: the mass ratio of the shea butter, the wax and the effective components is (1-7): (0-12): (3-15).

The preferable scheme of the preparation method of the microcapsule nano emulsion for the amorphous essence and medicine is as follows: the effective components include one or more of menthol, eugenol, vanillin, camphor, citronellal, eucalyptol, limonene, curcumin, resveratrol, furan aniline acid, propranolol and flurbiprofen.

The preferable scheme of the preparation method of the microcapsule nano emulsion for the amorphous essence and medicine is as follows: the wax comprises one or more of candelilla wax, beeswax, carnauba wax, microcrystalline wax and ozokerite; the octenyl succinate starch comprises one or more of Capsul, Purity Gum Ultra, HI-CAP 100;

the preferable scheme of the preparation method of the microcapsule nano emulsion for the amorphous essence and medicine is as follows: the homogenizing time is 0.5-3 min, and the rotating speed is 8000-15000 rpm/min; and (3) performing high-pressure homogenization, wherein the homogenization pressure is 600-1000 bar, and performing circulation.

As another aspect of the invention, the invention provides an application of the microcapsule nano emulsion for the amorphous of the essence and the medicine, which can be used for one or more of lipstick, perfumed soap, talcum powder, deodorant stick, emulsion, cream and facial mask cosmetics.

As another aspect of the present invention, the present invention provides a method for preparing microcapsules for perfume and pharmaceutical amorphization, comprising the following steps: spray drying the microcapsule nano emulsion for the amorphous essence and medicine; wherein the mass ratio of the oil phase to the water phase is 0.8-1.5; the mass ratio of the effective components to the octenyl succinic acid esterified starch is (3-12): (18-27).

As a preferable scheme of the preparation method for the amorphous essence and medicine, the preparation method comprises the following steps: the spray drying is carried out, wherein the feeding amount is 10-30 ml/min, the air inlet temperature is 160-190 ℃, and the air outlet temperature is 75-90 ℃.

As another aspect of the invention, the invention provides a microcapsule which can be used for the amorphous of essence and medicine, and the loading amount is more than or equal to 15%.

The invention has the beneficial effects that: the microcapsule prepared by the invention has good fluidity, high loading capacity (> 30%), high encapsulation efficiency (surface menthol content is low (< 1%)), excellent thermal stability, loss of menthol of less than 7% after being placed for 12h at 100 ℃, convenient processing at high temperature, stable performance after being stored for 6 months at normal temperature, reduced storage requirement and prolonged storage life.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:

FIG. 1 is an SEM detection diagram of menthol microcapsules with different serial numbers in the example, and the left and right are detection diagrams of the menthol microcapsules with different serial numbers under different multiples;

FIG. 2 shows the results of the test of the menthol content on the surface of the menthol microcapsules of each number in the examples;

FIG. 3 shows the results of the thermal stability test of menthol microcapsules of each number in examples;

FIG. 4 shows XRD test results of various numbers of menthol microcapsules and raw materials in examples;

figure 5 is a comparison of XRD test results for menthol microcapsules prepared No. 23 after placement for 60d, 90d and 180d and thermal stability after placement for 180 d.

Detailed Description

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.

In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.

Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.

Surface menthol content test:

accurately weighing a certain mass m₁(about 3G) of menthol microcapsules, 80mL of absolute ethanol was added, the mixture was stirred gently at room temperature for 1min with magnetic stirring, and the mixture was poured into a G3 sand-core funnel (m was weighed in advance)₂) Filtering, washing with small amount of anhydrous ethanol for 3 times, air drying the sand core funnel and the filter residue in a fume hood overnight, volatilizing ethanol, and weighingWeight m₃. The calculation formula of the surface menthol content is as follows:

surface menthol content ═ m₁+m₂-m₃)/(m₁X capacity)

Menthol loading test:

accurately weighing and accurately weighing a certain mass m₄(about 3g) menthol microcapsules placed on petri dish m₅Adding 80g of deionized water and 20g of ethanol, and drying in an oven at 100 ℃ to obtain the menthol with weight loss. Repeatedly adding deionized water and ethanol (mass ratio of 4:1), drying in oven at 100 deg.C until constant weight m₆。

Menthol loading ═ m₆﹣m₅)/m₄