CN103710147B - A kind of preparation method of granada seed oil vesica - Google Patents

Abstract

A method for preparing pomegranate seed oil vesicles belongs to the technical field of surface chemistry. In the present invention, firstly, the pomegranate seed oil, surfactant and cholesterol are heated to a certain temperature to completely dissolve them to form an oil phase; then, a vortex mixer is used to oscillate the preheated phosphate buffer solution at high speed, and the oil phase is quickly injected to obtain Emulsion: The above emulsion is centrifuged at high speed, and the paste in the middle layer is the pomegranate seed oil vesicle. The test results show that pomegranate seed oil vesicles can significantly improve the stability of pomegranate seed oil, and have high encapsulation efficiency and high drug loading capacity. The invention has simple process and convenient operation, and overcomes the defects that the pomegranate seed oil is not easy to preserve at normal temperature, has poor stability, and the like.

Description

A kind of preparation method of pomegranate seed oil vesicle

technical field

A method for preparing pomegranate seed oil vesicles belongs to the technical field of surface chemistry.

Background technique

Pomegranate ( Punica granatum L ) is a deciduous shrub or small tree of the Pomegranate family. It is widely planted in Lintong, Shaanxi, Zaozhuang, Shandong, Huaiyuan, Anhui, Huili, Sichuan, Mengzi, Yunnan, and Yecheng, Xinjiang. Among the pomegranate extracts, pomegranate seed oil has high utilization value. Domestic and foreign studies have shown that: pomegranate seed oil has significant antioxidant activity, can improve skin quality, resist free radicals and collagen degrading enzymes, and has the ability to lower blood sugar. , Prevent coronary heart disease, enhance the strength of blood vessel walls, reduce varicose arteries and so on.

Pomegranate seed oil contains a variety of fatty acids, the main component of which is punicic acid, which is an unsaturated fatty acid. Its chemical properties are very active, and it is very sensitive to light, heat, and oxidants. Bring a lot of inconvenience, and lose original health care function, produce some harmful substances. Therefore, it is of great significance to coat pomegranate seed oil to delay its oxidation rate.

At present, the main methods of pomegranate seed oil coating include microcapsule method, liposome and vesicle method. Microencapsulation technology refers to the technology of using film-forming materials such as β-cyclodextrin, gum arabic, modified starch, sucrose or protein to encapsulate solids, liquids or gases in them to form tiny containers of tens of microns to thousands of microns. Wen Youying et al. used octenyl succinic acid starch lipid HI-CAP100 as the capsule material, prepared pomegranate seed oil microcapsules by spray drying method, and compared the stability of pomegranate seed oil microcapsules through high temperature, high humidity, strong light irradiation and other experiments. The results show that the stability of pomegranate seed oil has been improved to a certain extent (Wen Youying. Research on the extraction process and microencapsulation of pomegranate seed oil [D]: [Master's Thesis] Shandong: Qingdao University of Science and Technology, 2011). Liposomes are microvesicles formed by encapsulating drugs in lipid bilayers by substances such as phospholipids and cholesterol. Liposomes can coat both hydrophilic drugs and lipophilic drugs. However, due to the disadvantages of easy oxidation and degradation of phospholipids, easy leakage of encapsulated substances, and easy aggregation of liposomes, surfactants are used instead of phospholipids to prepare liposomes. Vesicles. A vesicle system with a closed bilayer membrane structure is formed by self-assembly in a hydrophilic medium using surfactants and cholesterol.

The preparation methods of surfactant vesicles mainly include injection method, thin film method, reverse phase evaporation method and melting method (Jiang Shuhong, Ge Yanru, Wang Zhuyan, Research progress of nonionic surfactant vesicles. Chinese Modern Medicine Application, 2007, 1 (11):98-101). The injection method, thin film method and reverse phase evaporation method all have the problem that the organic solvent is difficult to remove, while the melting method injects the surfactant in the molten state into the water phase at a certain temperature and high-speed stirring, so no organic solvent is needed. .

Contents of the invention

The purpose of the present invention is to provide a preparation method of pomegranate seed oil vesicles, so as to improve the stability of pomegranate seed oil and overcome the defects of difficult storage at room temperature and poor stability.

Technical scheme of the present invention: a preparation method of pomegranate seed oil vesicles, using pomegranate seed oil as the core material, surfactant and cholesterol as the wall material, the preparation steps are as follows:

(1) Put 1 part of pomegranate seed oil, 0.5~1.5 parts of surfactant and 0.05~0.25 parts of cholesterol in a beaker by mass, and heat to 40~80°C to completely dissolve them to form an oil phase;

(2) Preheat 5~10 parts of 5.0~10.0 mmol/L pH 7.5 phosphate buffer solution to 40~80°C;

(3) Place the buffer solution obtained in step (2) in a vortex mixer for high-speed vibration at a speed of 1000~3000r/min, and use a syringe preheated to 40~80°C to inject the oil phase obtained in step (1) within 5s Quickly inject into the buffer, and then continue to shake for 1~5min to form an emulsion;

(4) Centrifuge the emulsion obtained in step (3) in a high-speed centrifuge at 10,000 to 15,000 r/min for 10 to 15 minutes, and the paste in the middle layer is pomegranate seed oil vesicles.

The surfactant described in the present invention can be polyoxyethylene fatty alcohol ether, polyoxyethylene sorbitan fatty acid ester, sorbitan fatty acid ester, mono/diglycerin fatty acid ester, mono/dialkyl phosphoric acid ester one or more of. The hydrophobic chain group of the surfactant is a saturated or unsaturated linear alkyl group containing twelve, fourteen, sixteen or eighteen carbons.

The pomegranate seed oil of the present invention is obtained by using pomegranate seeds as raw materials, ultrasonically assisted extraction with an organic solvent or cold pressing technology, and the organic solvent is one of petroleum ether, ethyl acetate and n-hexane.

The vortex mixer of the present invention can fully mix the oil phase and the buffer solution, the rotating speed is 1000-3000r/min, and the time is 1-5min.

The encapsulation rate of the pomegranate seed oil vesicles of the present invention is as high as over 90%, the oil loading capacity is as high as over 70%, and the particle diameter of the pomegranate seed oil vesicles is 50-500nm.

The stability of the pomegranate seed oil vesicles of the present invention: a certain amount of pomegranate seed oil vesicles are dispersed in water to form a pomegranate seed oil vesicle solution with a concentration of 0.05-0.50 mg/mL, which can still be stabilized within 180 days. Keep good stability.

The pomegranate seed oil vesicles of the invention can obviously improve the stability of the pomegranate seed oil and protect the anti-oxidation active components in the pomegranate seed oil from being oxidized.

Stability determination of vesicle-coated pomegranate seed oil:

Take an appropriate amount of pomegranate seed oil and pomegranate seed oil vesicles, put them into a sealed sample bottle, keep away from light, and store them in a constant temperature oven at 60±0.5°C. Accurately weigh a certain amount of pomegranate seed oil and vesicles with the same content of pomegranate seed oil, and dissolve them with ethanol. The absorbance at 273nm was measured by ultraviolet-visible spectrophotometer, and the stability of pomegranate seed oil and vesicle-coated pomegranate seed oil was compared according to the change of absorbance. The results are shown in Figure 1. The results showed that the stability of pomegranate seed oil vesicles was significantly higher than that of pomegranate seed oil.

Beneficial effects of the present invention: test results show that pomegranate seed oil vesicles can significantly improve the stability of pomegranate seed oil, and have high encapsulation efficiency and high drug loading capacity. The invention has simple process and convenient operation, and overcomes the defects that the pomegranate seed oil is not easy to preserve at normal temperature, has poor stability, and the like.

Description of drawings

Fig. 1 Stability curves of pomegranate seed oil and pomegranate seed oil vesicles

Figure 2 TEM images of pomegranate seed oil vesicles.

Detailed ways

The following examples will further explain the present invention, but the present invention is not limited to these examples.

Example 1

formula:

                                                                                                                                                

                                                     

Cholesterol 0.073g

                                             

Phosphate buffer solution pH 7.5 10.0mL

Preparation process: Weigh stearyl polyoxyethylene ether-3, didodecanyl phosphate, cholesterol and pomegranate seed oil in a beaker, heat to 40°C to dissolve completely, and form an oil phase. At the same time, preheat 10.0mL 5.0 mmol/L pH 7.5 phosphate buffer solution to 40°C, place the buffer solution in a vortex mixer for high-speed oscillation at a speed of 3000r/min, and use a syringe preheated to 40°C to Quickly inject into the buffer solution for less than 5 seconds, and keep shaking for 4 minutes to form an emulsion. Centrifuge the above emulsion in a high-speed centrifuge at 10,000 r/min for 15 minutes, and the paste in the middle layer is pomegranate seed oil vesicles. The encapsulation efficiency of the obtained vesicles was 96.32%, and the oil loading capacity was 79.27%.

Disperse a certain amount of pomegranate seed oil vesicles in water to prepare a pomegranate seed oil vesicle solution with a concentration of 0.05-0.50 mg/mL, which can still maintain good stability within 180 days.

Example 2

formula:

Glyceryl monostearate 1.040g

Cholesterol 0.073g

                                             

Phosphate buffer solution pH 7.5 5.0mL

Preparation process: Weigh the prescribed amount of glyceryl monostearate, cholesterol and pomegranate seed oil in a beaker, heat to 75°C to dissolve them completely, and form an oil phase. At the same time, preheat 5.0mL 5.0 mmol/L phosphate buffer solution with pH 7.5 to 75°C, place the buffer solution in a vortex mixer for high-speed oscillation at a speed of 3000r/min, and use a syringe preheated to 75°C to Quickly inject into the buffer solution for less than 5 seconds, and keep shaking for 4 minutes to form an emulsion. Centrifuge the above emulsion in a high-speed centrifuge at 10,000 r/min for 15 minutes, and the paste in the middle layer is pomegranate seed oil vesicles. The encapsulation efficiency of the obtained vesicles was 90.28%, and the oil loading capacity was 71.77%.

Disperse a certain amount of pomegranate seed oil vesicles in water to prepare a pomegranate seed oil vesicle solution with a concentration of 0.05-0.50 mg/mL, which can still maintain good stability within 180 days.

Claims (2)

1. a preparation method for granada seed oil vesica, it is characterized in that taking granada seed oil as core, tensio-active agent and cholesterol are wall material, and its preparation process is as follows:

(1) in mass 1 part of granada seed oil, 0.5 ~ 1.5 part of tensio-active agent and 0.05 ~ 0.25 part of cholesterol are placed in beaker, are heated to 40 ~ 80 DEG C and make it to dissolve completely, form oil phase;

(2) phosphate buffer soln of 5 ~ 10 part of 5.0 ~ 10.0 mmol/L pH 7.5 is preheated to 40 ~ 80 DEG C;

(3) step (2) gained damping fluid is placed in the vibration of vortex mixer high speed, rotating speed is 1000 ~ 3000r/min, with the syringe being preheated to 40 ~ 80 DEG C, the oil phase of step (1) gained is injected damping fluid fast in 5s, then sustained oscillation 1 ~ 5min, form milk sap;

(4) by step (3) gained milk sap centrifugal 10 ~ 15min in the supercentrifuge of 10000 ~ 15000r/min, middle level paste is granada seed oil vesica;

The encapsulation rate of granada seed oil vesica is up to more than 90%, and fuel load is up to more than 70%, and the particle diameter of granada seed oil vesica is 50 ~ 500nm;

The stability of granada seed oil vesica: be scattered in water by a certain amount of granada seed oil vesica, is made into the granada seed oil vesica liquid that concentration is 0.05 ~ 0.50mg/mL, in 180 days, still can keeps satisfactory stability.

2. the preparation method of granada seed oil vesica according to claim 1, it is characterized in that: step (1) described tensio-active agent select in polyoxyethylene aliphatic alcohol ether, polyoxyethylene sorbitan carboxylic ester, sorbitan carboxylic esters, list/diglycerine fatty acid ester, list/bis-alkyls phosphoric acid ester one or more, the hydrophobic chain group of tensio-active agent is the saturated or unsaturated straight chained alkyl containing 12,14,16 or 18 carbon.