CN118141097A - A kind of policosanol nano preparation and preparation method thereof - Google Patents

Abstract

The present invention provides a policosanol nanoformulation and a preparation method thereof, and belongs to the technical field of policosanol preparation. The present invention first prepares a protein solution, then mixes policosanol, an emulsifier and ethanol to prepare a policosanol solution; the two solutions are mixed and an emulsifier stabilizer is added to mix, the ethanol is removed, and the policosanol nanoformulation is obtained through freeze drying. The policosanol nanoformulation of the present invention has good embedding rate, solubility and dispersibility, and can effectively improve the water solubility of policosanol.

Description

A kind of policosanol nano preparation and preparation method thereof

Technical Field

The invention relates to the technical field of policosanol preparation, and in particular to a policosanol nano preparation and a preparation method thereof.

Background technique

Policosanol is a naturally occurring higher alcohol, the main component of which is octacosanol. It appears as white powder or flaky crystals, is soluble in organic solvents but insoluble in water, and is mainly found in natural products such as cane wax, rice bran wax, wheat germ oil, beeswax, and insect wax. Many studies have shown that policosanol has unique physiological functions such as enhancing endurance, resisting fatigue, lowering blood lipids, resisting inflammation, and protecting the liver. However, due to its poor water solubility and low bioavailability, the application of policosanol in food or medicine is limited.

Summary of the invention

In order to solve the problem of poor water solubility of policosanol, the purpose of the present invention is to provide a method for preparing a policosanol nanoformulation. The policosan nanoformulation prepared by the present invention has good embedding rate, solubility and dispersibility, and can effectively improve the water solubility of policosanol.

A method for preparing a policosanol nanoformulation in the present invention comprises the following steps:

(1) dispersing and dissolving the protein in deionized water, and then hydrating the solution to obtain a protein solution;

(2) adding policosanol and an emulsifier into ethanol, and then stirring in a water bath to dissolve uniformly to obtain a policosanol solution;

(3) mixing the protein solution of step (1) and the policosanol solution of step (2) under stirring, adding an emulsion stabilizer under stirring and mixing them evenly, and then subjecting the mixture to homogenization and microfluidization to obtain a mixed emulsion;

(4) removing ethanol from the mixed emulsion in step (3) to obtain a mixed emulsion from which ethanol has been removed, and then freeze-drying the mixed emulsion from which ethanol has been removed to obtain a policosanol nanoformulation.

Furthermore, the protein in step (1) is ovotransferrin.

Furthermore, in the protein solution of step (1), the mass volume ratio of protein to deionized water is 1 to 3 mg/mL.

Furthermore, the hydration temperature in step (1) is 0 to 10° C., and the hydration time is 6 to 24 hours.

Furthermore, the emulsifier in step (2) is phospholipid.

Furthermore, in step (2), the mass ratio of policosanol to emulsifier is 1:(1-5).

Furthermore, in step (2), the mass volume ratio of the emulsifier to ethanol is 10 to 30 mg/mL.

Furthermore, in step (2), the water bath stirring temperature is 80-100° C., and the water bath stirring time is 1-5 min.

Furthermore, the emulsion stabilizer in step (3) is gum arabic.

Furthermore, in step (3), the mass ratio of the emulsion stabilizer to the emulsifier is 1:(1-5).

Furthermore, the volume ratio of the protein solution to the policosanol solution in the mixed emulsion of step (3) is 10:(1-3).

Furthermore, the rotation speed of the homogenization treatment in step (3) is 3000-10000 rpm, and the time of the homogenization treatment is 3-8 min.

Furthermore, the pressure of the microfluidization treatment in step (3) is 30 to 90 MPa, and the number of microfluidization treatments is 1 to 5 times.

Furthermore, in step (4), the method of removing ethanol from the mixed emulsion is rotary evaporation; the temperature of the rotary evaporation is 40 to 50° C., and the vacuum degree of the rotary evaporation is 0.04 to 0.1 MPa.

Furthermore, before freeze-drying in step (4), the mixed emulsion from which ethanol has been removed is diluted with deionized water to a mass before rotary evaporation.

Furthermore, the freeze-drying time in step (4) is 24 to 48 hours.

Another object of the present invention is to provide a policosanol nanoformulation prepared by the above preparation method.

Compared with the prior art, the present invention has the following beneficial effects:

The present invention selects ovotransferrin, which is a protein with film-forming property. It is used as a wall material in the present invention to have an embedding effect on other substances. In addition, ovotransferrin has good interfacial activity and can be used as a natural emulsifier to improve the emulsification effect on policosanol, thereby reducing the particle size of the policosanol nanoformulation. At the same time, ovotransferrin also has multiple biological properties such as anti-oxidation, antibacterial, anti-tumor and anti-inflammatory. Therefore, the ovotransferrin used in the present invention can not only improve the water solubility and bioavailability of policosanol, but also has multiple biological properties, which is conducive to expanding the application of policosanol in food and medicine.

Detailed ways

The present invention will be further described below in conjunction with the embodiments.

Example 1

A method for preparing a policosanol nanoparticle preparation comprises the following steps:

(1) dispersing and dissolving ovotransferrin in deionized water at a mass volume ratio of ovotransferrin to deionized water of 2 mg/mL at room temperature and under magnetic stirring, and then placing the solution in a refrigerator at 4° C. for full hydration for 12 h to obtain a protein solution;

(2) adding policosanol and phospholipids to ethanol at a mass ratio of 1:2 and a mass volume ratio of phospholipids to ethanol of 15 mg/mL, and fully dissolving them in a 95° C. water bath with magnetic stirring for 2 min to obtain a policosanol solution;

(3) adding the policosanol solution to the protein solution at a volume ratio of 5:1, adding gum arabic to the phospholipid at a mass ratio of 1:5 under stirring and mixing, then homogenizing at a rotation speed of 5000 rpm for 5 min, and then microfluidizing at a pressure of 80 MPa for 2 times to obtain a mixed emulsion;

(4) placing the mixed emulsion obtained in step (3) in a distillation flask, and performing rotary evaporation to remove ethanol at a temperature of 45° C. and a vacuum degree of 0.09 MPa, diluting the mixed emulsion from which ethanol has been removed by rotary evaporation with deionized water to the mass before rotary evaporation, and then freeze-drying the mixed emulsion for 24 hours to obtain a policosanol nanoformulation.

Example 2

A method for preparing a policosanol nanoformulation comprises the following steps:

(1) dispersing and dissolving ovotransferrin in deionized water at a mass volume ratio of ovotransferrin to deionized water of 2 mg/mL at room temperature and under magnetic stirring, and then placing the solution in a refrigerator at 4° C. for full hydration for 12 h to obtain a protein solution;

(2) adding policosanol and phospholipids to ethanol at a mass ratio of 1:3 and a mass volume ratio of phospholipids to ethanol of 20 mg/mL, and fully dissolving them in a 95° C. water bath with magnetic stirring for 2 min to obtain a policosanol solution;

(3) adding the policosanol solution to the protein solution at a volume ratio of 5:1, adding gum arabic to the phospholipid at a mass ratio of 1:5 under stirring and mixing, then homogenizing at a rotation speed of 5000 rpm for 5 min, and then microfluidizing at a pressure of 80 MPa for 2 times to obtain a mixed emulsion;

(4) placing the mixed emulsion obtained in step (3) in a distillation flask, and performing rotary evaporation to remove ethanol at a temperature of 45° C. and a vacuum degree of 0.09 MPa, diluting the mixed emulsion from which ethanol has been removed by rotary evaporation with deionized water to the mass before rotary evaporation, and then freeze-drying the mixed emulsion for 24 hours to obtain a policosanol nanoformulation.

Example 3

A method for preparing a policosanol nanoformulation comprises the following steps:

(1) dispersing and dissolving ovotransferrin in deionized water at a mass volume ratio of ovotransferrin to deionized water of 3 mg/mL at room temperature and under magnetic stirring, and then placing the solution in a refrigerator at 4° C. for 12 hours to obtain a protein solution;

(2) adding policosanol and phospholipids to ethanol at a mass ratio of 1:3 and a mass volume ratio of phospholipids to ethanol of 20 mg/mL, and fully dissolving them in a 95° C. water bath with magnetic stirring for 2 min to obtain a policosanol solution;

(3) adding the policosanol solution to the protein solution at a volume ratio of 5:1, adding gum arabic to the phospholipid at a mass ratio of 1:5 under stirring and mixing, then homogenizing at a rotation speed of 5000 rpm for 5 min, and then microfluidizing at a pressure of 80 MPa for 2 times to obtain a mixed emulsion;

(4) placing the mixed emulsion obtained in step (3) in a distillation flask, and performing rotary evaporation to remove ethanol at a temperature of 45° C. and a vacuum degree of 0.09 MPa, diluting the mixed emulsion from which ethanol has been removed by rotary evaporation with deionized water to the mass before rotary evaporation, and then freeze-drying the mixed emulsion for 24 hours to obtain a policosanol nanoformulation.

Comparative Example 1

Comparative Example 1: In Comparative Example 1, the ovotransferrin in Example 3 was replaced with soy protein isolate, and the remaining steps were the same as those in Example 3.

The embedding efficiency, particle size, Zeta potential and PDI of the policosan nanoparticles prepared in Examples 1 to 3 and Comparative Example 1 were tested.

Embedding rate: The embedding rate of the prepared policosanol nanoformulation was determined by gas chromatography:

Embedding rate = (1-surface policosan amount/total policosan amount) × 100%

Particle size, Zeta potential and PDI: The particle size, Zeta potential and PDI of the prepared policosanol nanoformulation were measured using a particle size potential analyzer.

The experimental results are shown in Table 1.

Table 1

The above data show that the policosanol nanoformulations prepared in Examples 1 to 3 have good embedding rate, redissolubility (redissolved particle size) and dispersibility (PDI), and can effectively improve the water solubility of policosanol.

The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims (10)

1. The preparation method of the polycosanol nanometer preparation is characterized by comprising the following steps:

(1) Dispersing and dissolving protein in deionized water, and then hydrating to obtain a protein solution;

(2) Adding polycosanol and an emulsifying agent into ethanol, and then stirring in a water bath to dissolve uniformly to obtain polycosanol solution;

(3) Mixing the protein solution in the step (1) and the polycosanol solution in the step (2) under a stirring state, adding an emulsion stabilizer under the stirring state, uniformly mixing, and carrying out homogenization treatment and micro-jet treatment to obtain mixed emulsion;

(4) And (3) removing the ethanol in the mixed emulsion in the step (3) to obtain the mixed emulsion with the ethanol removed, and then freeze-drying the mixed emulsion with the ethanol removed to obtain the polycosanol nanometer preparation.

2. The method of preparing a polycosanol nanoparticle formulation according to claim 1, wherein the protein of step (1) is ovotransferrin; in the protein solution, the mass volume ratio of the protein to the deionized water is 1-3 mg/mL.

3. The method for preparing a polycosanol nanometer preparation according to claim 1, wherein the hydration temperature in the step (1) is 0-10 ℃ and the hydration time is 6-24 h.

4. The method of preparing a polycosanol nanoparticle formulation according to claim 1, wherein the emulsifier of step (2) is a phospholipid; the mass ratio of the common Li Chunhe emulsifying agent is 1 (1-5); the mass volume ratio of the emulsifier to the ethanol is 10-30 mg/mL.

5. The method for preparing the polycosanol nanometer preparation according to claim 1, wherein the water bath stirring temperature in the step (2) is 80-100 ℃, and the water bath stirring time is 1-5 min.

6. The method of preparing a nanoparticulate formulation of polycosanol according to claim 1, wherein the emulsion stabilizer of step (3) is acacia; the mass ratio of the emulsion stabilizer to the emulsifier is 1 (1-5); the volume ratio of the protein solution to the polycosanol solution in the mixed emulsion is 10 (1-3).

7. The method for preparing a polycosanol nanometer preparation according to claim 1, wherein the rotational speed of the homogenizing treatment in the step (3) is 3000-10000 rpm, and the homogenizing treatment time is 3-8 min; the pressure of the micro-jet treatment is 30-90 MPa, and the times of the micro-jet treatment are 1-5 times.

8. The method of claim 1, wherein the step (4) of removing ethanol from the mixed emulsion is rotary evaporation; the temperature of the rotary evaporation is 40-50 ℃, and the vacuum degree of the rotary evaporation is 0.04-0.1 MPa.

9. The method of preparing a polycosanol preparation according to claim 1, wherein the mixed emulsion from which ethanol is removed is diluted with deionized water to a mass before rotary evaporation before the freeze drying in step (4); the freeze drying time is 24-48 h.

10. A polycosanol nanometer preparation, characterized in that the preparation is prepared by any one of the methods of claims 1-9.