WO2014059649A1

WO2014059649A1 - Lycopene microcapsule preparation method

Info

Publication number: WO2014059649A1
Application number: PCT/CN2012/083157
Authority: WO
Inventors: 冯敏; 黄景苏; 冯鹏; 沈建; 钱一帆; 王连安
Original assignee: 南京中科药业有限公司
Priority date: 2012-10-18
Filing date: 2012-10-18
Publication date: 2014-04-24

Abstract

Disclosed is a lycopene microcapsule preparation method, comprising the steps of: firstly preparing the lycopene into a core material, and then homogeneously emulsifying and spray-drying the core material and a wall material; the wall material is prepared from gelatin, sporoderm-broken ganoderma lucidum spore powder, cane sugar and skim milk powder in a weight ratio of 1: 1: 1: 1.2-1.6, and the core material is prepared from the lycopene, salad oil and sucrose ester. The present invention employs a specific microcapsule technique to embed the lycopene, and improves both stability and water solubility of the lycopene microcapsule, thus further expanding the application scope.

Description

Preparation method of lycopene microcapsule

Technical field

The invention belongs to the technical field of traditional Chinese medicine, and particularly relates to a preparation method of a lycopene microcapsule.

Background technique

Lycopene is a type of carotenoid that is widely found in plants such as tomatoes, watermelons, grapes, and carrots. Since lycopene does not have the physiological activity of vitamin A, its role has not been taken seriously. However, recent studies have shown that lycopene has superior performance to other carotenoids, such as 100 times more vitamin E, and more than twice as much as beta carotene. Lycopene can increase the body's immunity, inhibit cancer cell proliferation, reduce DNA loss, prevent low-density lipoprotein oxidation, and lower blood cholesterol levels, thus reducing the incidence of multiple diseases.

Lycopene is usually a dark red powder or an oily liquid. The pure product is a needle-like deep red crystal. It is orange-yellow in a lower concentration solution and has a melting point of 174 ° C (trans) and can be burned. As an aliphatic hydrocarbon, lycopene is insoluble in water, and is insoluble in polar organic solvents such as methanol and ethanol. It is soluble in ether, petroleum ether, ethane, acetone, and easily soluble in chloroform, carbon disulfide, benzene, and oil. The higher the purity of lycopene, the more difficult it is to dissolve, and the solubility in various solvents increases with increasing temperature. Lycopene contains a large amount of unsaturated structure, which is easily degraded and isomerized by heat, light, oxygen, additives and the like during processing and storage, thereby reducing physiological activity.

In order to make full use of lycopene, lycopene can be embedded by microcapsule technology, which avoids direct contact between lycopene and the external environment, thereby improving stability. The so-called microcapsule technology is a technique of coating liquid, solid or even gas (core material) into tiny particles by selecting a suitable film-forming material (wall material). After microcapsule treatment, the core material is not in direct contact with external environmental factors. , is effectively protected. However, the existing process of microencapsulation of lycopene is difficult to ensure the long-term stability of the water solubility of lycopene microcapsules and the content of active ingredients.

Summary of the invention

SUMMARY OF THE INVENTION The object of the present invention is to provide a preparation method of lycopene microcapsules which improves stability and can improve water solubility, thereby expanding the application field of lycopene microcapsules.

The object of the invention is achieved in the following ways:

A method for preparing a lycopene microcapsule, which comprises preparing a lycopene into a core material, and then subjecting the wall material to a homogeneous emulsification and spray drying step, wherein the wall material is prepared by the following method : In the weight ratio of 1: 1: 1: 1.2~1.6 gelatin, broken ganoderma lucidum spore powder, sucrose, skim milk powder as the wall material, add the above materials 3~5 times the amount of distilled water, heated to 40~45 °C, stirred to form a uniform suspension, which is the wall material. Preferably, the wall material is prepared by the following method: gelatin, broken ganoderma lucidum spore powder, sucrose, skim milk powder as a wall material in a weight ratio of 1: 1: 1: 1.4, adding 4 times of distilled water of the above materials, heating to 45 ° C, stirring into a uniform suspension, that is, a wall material.

The core material is prepared by the following method: Dissolving 0.5 to 0.8 g of lycopene per 1 ml of salad oil, adding sucrose ester as an emulsifier, stirring uniformly to obtain a core material, lycopene and sucrose The weight ratio of the ester is 10 to 14: 1; Preferably, the core material is prepared by the following method: 0.68 g of lycopene is dissolved in 1 ml of salad oil, and sucrose ester is added as an emulsifier, and the mixture is uniformly stirred. The weight ratio of lycopene to sucrose ester was 8.5: 0.7.

Wherein, the salad oil may be a common edible salad oil such as soybean salad oil, rapeseed salad oil, sunflower seed salad oil, rice bran salad oil or the like. Broken Ganoderma lucidum spore powder should be selected from broken wall Ganoderma lucidum spore powder with a wall breaking rate greater than 95%.

The above homogeneous emulsification comprises the following steps: using a mixture of a core material and a wall material as an oil phase, slowly adding the oil phase while stirring in water, and the weight ratio of water to oil phase is 3 to 3.5:5 to 6, and then placed In the colloid mill, it is ground at 5000 to 10,000 rpm, and the grinding time is 20 to 40 min.

Preferably, the homogeneous emulsification comprises the following steps: taking a mixture of the core material and the wall material as an oil phase, slowly adding the oil phase while stirring in water, the weight ratio of water to oil phase is 3:5, and then placing it in the colloid mill. Grinding was carried out at 6000 rpm, and the grinding time was 30 min.

The spray drying conditions are as follows: spray drying inlet air temperature is 170-180 ° C, outlet air temperature is 80-100 ° C, feed temperature is 45-50 ° C, and feed rate is 0.6-1.0 kg/min. , the blowing speed is 50~60 l/min. Preferably, the spray drying conditions are: spray drying inlet air temperature is 180 ° C, outlet air temperature is 80 to 100 ° C, feed temperature is 50 ° C, feed rate is 0.6 1.0 kg / min, and blowing speed is 50 to 60 liters. /minute.

Compare the advantages of the present invention with the prior art:

The invention adopts a material which can form a film, meets the requirements of the national food additive, is non-toxic to the human body, and easily releases the core material in water, and adopts a suitable microencapsulation method to coat the lycopene in a minute and closed. Inside the membrane, it is converted into a manageable powder solid that protects sensitive lycopene from oxidation. In particular, the wall material made of the new material of the invention can realize the slow release of the core material, prolong the action time of the functional factor, and the stability of the lycopene microcapsule is remarkably improved, and the core material prepared by using the formula of the invention is further improved. The wall material used in the present invention is more easily coated. The invention adopts a specific microcapsule technology to embed lycopene, and improves the stability of the active ingredient, and also improves the water solubility of the lycopene microcapsule, thereby expanding the application field.

Specific real fc^:

The present invention will be further described below based on the embodiments, and the specific embodiments of the following embodiments are only more specifically The present invention is not limited to the contents of the following embodiments. The lycopene, lycopene raw material described in the following examples, is produced by Israel's Lycored Company with a purity of 98%; the salad oil is arowana soy salad oil, and the manufacturer is Shanghai Kerry Grain and Oil Industry Co., Ltd.; Sucrose ester (ie sucrose fatty acid ester) manufacturer is Liuzhou Aigfu Food Technology Co., Ltd.; Broken Ganoderma lucidum spore powder (breaking rate greater than 95%) Manufacturer is Nanjing Zhongke Pharmaceutical Co., Ltd.; Manufacturer of skim milk powder It is Heilongjiang Feihe Dairy Co., Ltd.; commercially available lycopene microcapsule 1 is produced by Parry Nutraceutical, India; and commercially available lycopene microcapsule 2 is produced by Israel's Lycored.

Example 1

1. Preparation of core material: 8.5 g of lycopene was added to 12.5 ml of salad oil, and 0.7 g of sucrose ester was added as an emulsifier, and the mixture was uniformly stirred. This was oil phase eight.

2, wall material preparation: Take a weight ratio of 1: 1: 1: 1.4 gelatin, broken ganoderma lucidum spore powder, sucrose, skim milk powder (that is, wall material), add 4 times the amount of wall material raw water, heated to 45 °C, stir to make it a homogeneous suspension, this is the oil phase 8.

3. Homogeneous emulsification: Slowly add a mixture of oil phase A and oil phase B while stirring in water. The weight ratio of water to oil phase (ie, the sum of oil phase A and oil phase B) is 3:5. It was placed in a colloid mill, ground at 6000 rpm, and the grinding time was 30 min. The lycopene was uniformly dispersed in the wall material to obtain a homogenized emulsion.

The homogenized emulsion is spray-dried to obtain powdery lycopene microcapsules. The spray drying control conditions are: spray drying inlet air temperature of 180 ° C, outlet air temperature of 90 ° C, feed temperature of 50 ° C, feed rate of 0.8 kg / min, blowing speed of 50 ~ 60 l / min .

The stability test and detection result of the lycopene microcapsule content of the present embodiment:

The prepared lycopene microcapsules, the unmicroencapsulated lycopene raw materials, and the commercially available lycopene microcapsules 1 and the commercially available lycopene microcapsules 2 are respectively stored in a transparent sample bottle and sealed and stored at room temperature. At (20 ± 5 °C), natural light was used to measure the lycopene content of the sample at intervals, and the retention rate was compared with the lycopene content of the sample before storage. Table 1 shows the results of determination of lycopene in different samples, wherein the method for determining lycopene content is in accordance with national standards: GB/T22249-2008.

Table 1

Starting 1 week 2 weeks 4 weeks 24 weeks 48 weeks 96 weeks lycopene raw material 98% 20% 3.5% 0 0 0 0 This embodiment lycopene microcapsules 20% 20.2% 20.1% 20.0% 19.6% 18.9% 17.2% Buy lycopene microcapsules 1 20% 19.8% 19.6% 17% 12.5% 10.6% 8.2% Commercially available lycopene microcapsules 2 20% 19.6% 19.2% 16.3% 11.4% 8.9% 7.0% The detection results of the lycopene microcapsules in this example are shown in Table 2, using the 2010 edition of the Chinese Pharmacopoeia appendix method three times. Parallel detection:

Table 2

Example 2

1. Preparation of core material: 8 g of lycopene was added to 12.5 ml of salad oil, and 0.7 g of sucrose ester was added as an emulsifier, and the mixture was uniformly stirred. This was oil phase eight.

2, wall material preparation: Take the weight ratio of 1: 1: 1: 1.2 gelatin, broken ganoderma lucidum spore powder, sucrose, skim milk powder (that is, wall material), add 3 times the amount of distilled water, wall material, heated to 45 °C, stir to make it a homogeneous suspension, this is the oil phase 8.

3. Homogeneous emulsification: Slowly add a mixture of oil phase A and oil phase B while stirring in water. The weight ratio of water to oil phase is 3:5, and then placed in a colloid mill at 8000 rpm. Under the grinding, the grinding time is 25 min, that is, the lycopene is uniformly dispersed in the wall material to obtain a homogenized emulsion.

The homogenized emulsion is spray dried to obtain a powdery lycopene product. The spray drying control conditions are: spray drying inlet air temperature of 180 ° C, outlet air temperature of 80 ° C, feed temperature of 45 ° C, feed rate of 0.6 kg / min, blowing speed of 50 ~ 60 l / min .

The stability test results of the lycopene content in the lycopene microcapsules of the present embodiment are shown in Table 3, and the detection method is the same as in the embodiment 1:

table 3

The time limit for disintegration of lycopene microcapsules in this example was tested by the 2010 edition of the Chinese Pharmacopoeia appendix method, and the average disintegration time was 46 min in three parallel tests.

Example 3

1. Preparation of core material: 9 g of lycopene was added to 12.5 ml of salad oil, and 0.7 g of sucrose ester was added as an emulsifier, and the mixture was uniformly stirred, which was oil phase eight. 2, wall material preparation: Take a weight ratio of 1: 1: 1: 1.6 gelatin, broken ganoderma lucidum spore powder, sucrose, skim milk powder (that is, wall material), add 5 times the amount of distilled water, wall material, heated to 40 °C, stir to make it a homogeneous suspension, this is the oil phase 8.

3. Homogeneous emulsification: Slowly add a mixture of oil phase A and oil phase B while stirring in water. The weight ratio of water to oil phase is 3.5:5, and then placed in a colloid mill at 5000 rpm. Under the grinding, the grinding time was 35 min, and lycopene was uniformly dispersed in the wall material to obtain a homogenized emulsion.

The homogenized emulsion is spray dried to obtain a powdery lycopene product. The spray drying control conditions are: spray drying inlet air temperature of 170 ° C, outlet air temperature of 100 ° C, feed temperature of 50 ° C, feed rate of 1.0 kg / min, blowing speed of 50 ~ 60 l / min .

The stability test results of the lycopene content in the lycopene microcapsules of the present embodiment are shown in Table 4, and the detection methods are the same as the examples.

1:

Table 4

The time limit for disintegration of lycopene microcapsules in this example was tested by the 2010 edition of the Chinese Pharmacopoeia appendix method, and the average disintegration time was 48 min.

Claims

claims

1. A method for preparing lycopene microcapsules. This method mainly prepares lycopene into a core material, and then homogeneously emulsifies and spray-dries it with the wall material. It is characterized in that the wall material is made by the following method Prepared: Gelatin, broken Ganoderma spore powder, sucrose, and skimmed milk powder with a weight ratio of 1:1:1:1.2~1.6 are used as wall material raw materials, add 3~5 times the amount of distilled water to the above materials, and heat to 40~45 °C, stir to form a uniform suspension, which is the wall material.

2. The preparation method of lycopene microcapsules according to claim 1, characterized in that the wall material is prepared by the following method: gelatin and broken wall in a weight ratio of 1:1:1:1.4 Ganoderma spore powder, sucrose, and skimmed milk powder are the raw materials for the wall material. Add 4 times the amount of distilled water to the above materials, heat to 45°C, and stir to form a uniform suspension, which is the wall material.

3. The preparation method of lycopene microcapsules according to claim 1, characterized in that the core material is prepared by the following method: Dissolve every 0.5~0.8g lycopene in 1ml of salad oil , and add sucrose ester as an emulsifier. The weight ratio of lycopene to sucrose ester is 10 to 14: 1, which is the core material.

4. The preparation method of lycopene microcapsules according to claim 3, characterized in that the core material is prepared by the following method: Dissolve 0.68g of lycopene in 1ml of salad oil, and Add sucrose ester as emulsifier, and the weight ratio of lycopene to sucrose ester is 8.5:0.7, which is the core material.

5. The preparation method of lycopene microcapsules according to claim 1, characterized in that the homogeneous emulsification includes the following steps: using the mixture of core material and wall material as the oil phase, stirring and slowing down in water. Slowly add the oil phase, the weight ratio of water to oil phase is 3~3.5:5~6, then place it in a colloid mill, grind at 5000~10000 rpm, the grinding time is 20~40min.

6. The preparation method of lycopene microcapsules according to claim 5, characterized in that the homogeneous emulsification includes the following steps: using the mixture of core material and wall material as the oil phase, stirring and slowing down in water. Slowly add the oil phase, the weight ratio of water to oil phase is 3:5, then place it in a colloid mill and grind at 6000 rpm for 30 minutes.

7. The preparation method of lycopene microcapsules according to claim 1, characterized in that the spray drying conditions are: the spray drying air inlet temperature is 170~180°C, and the air outlet temperature is 80~100°C , the feeding temperature is 45~50°C, the feeding speed is 0.6~1.0kg/min, and the blowing speed is 50~60 liters/min.

8. The preparation method of lycopene microcapsules according to claim 7, characterized in that the spray drying conditions are: the spray drying air inlet temperature is 180°C, the air outlet temperature is 80~100°C, The material temperature is 50°C, the feeding speed is 0.6-1.0 kg/min, and the blowing speed is 50~60 liters/min.