Stable fat-soluble active ingredient composition, microcapsule and process of preparation and use thereof

Abstract

The present invention provides a stable fat-soluble active ingredient composition, microcapsule and process for preparation and use thereof. The fat-soluble active ingredient composition comprises tocopherol, vitamin C palmitate and a fat-soluble active ingredient; wherein the weight ratio of tocopherol to vitamin C palmitate is 2-8:1, the weight ratio of a combination of tocopherol with vitamin C palmitate to the fat-soluble active ingredient is 7-13:100. The present invention obtains a novel antioxidant composition without hidden dangers for improving the stability of the fat-soluble active ingredient by screening a combination of antioxidants and adjusting their proportion and dose.

Claims

1. A fat-soluble active ingredient microcapsule, comprising a stable fat-soluble active ingredient composition for increasing stability of a fat-soluble active ingredient, said stable fat-soluble active ingredient composition comprising tocopherol, vitamin C palmitate and a fat-soluble active ingredient, wherein the weight ratio of tocopherol to vitamin C palmitate is 2-8:1, the weight ratio of a combination of tocopherol with vitamin C palmitate to the fat-soluble active ingredient is 7-13:100, wherein the fat-soluble active ingredient is selected from the group consisting of docosahexaenoic acid acetate, linoleic acid glyceride, and linolenic acid phosphate.

2. The fat-soluble active ingredient microcapsule according to claim 1, wherein the weight ratio of tocopherol to vitamin C palmitate is 3-7:1.

3. The fat-soluble active ingredient microcapsule according to claim 2, wherein the weight ratio of tocopherol to vitamin C palmitate is 4-6:1.

4. The fat-soluble active ingredient microcapsule according to claim 1, wherein the weight ratio of a combination of tocopherol with vitamin C palmitate to the fat-soluble active ingredient is 8-12:100.

5. The fat-soluble active ingredient microcapsule according to claim 4, wherein the weight ratio of the combination of tocopherol with vitamin C palmitate to the fat-soluble active ingredient is 9-11:100.

6. The fat-soluble active ingredient microcapsule according to claim 1, wherein the stable fat-soluble active ingredient composition is used in the preparation of foods, beverages, animal feeds, cosmetics or pharmaceuticals.

Description

DETAILED DESCRIPTION OF THE INVENTION AND PREFERRED EMBODIMENTS THEREOF

(1) Hereafter, the present invention will be described specifically with reference to the examples. The examples are given only for illustration of the technical solution of the present invention and should not be construed to limit the present invention.

Example 1

(2) Vitamin A ester crystal, vitamin C palmitate and α-tocopherol are blended and melted at 75° C. under nitrogen protection to form a vitamin A molten oil. Factor level setting table of Table 1 and Orthogonal experiment schedule of Table 1 are determined based on weights of vitamin A ester crystal, vitamin C palmitate and α-tocopherol. The vitamin A ester molten oil is placed in a sample bottle and sealed from light, and stored at 40° C., and respectively detected its content in 0, 2, 4, 6 days.

(3) TABLE-US-00001 TABLE 1 Factor Level Setting Table Factor (ratio) level Vitamin C palmitate A α-tocopherol B 1 1% 6% 2 1.5%   8% 3 2% 10% Note: The percentage value of Table 1 is the weigh ratio of antioxidant to vitamin A.

(4) TABLE-US-00002 TABLE 2 Orthogonal experiment schedule Experiment factors NO. A B 1 1 1 2 1 2 3 1 3 4 2 2 5 2 3 6 2 1 7 3 3 8 3 1 9 3 2

(5) Analyzing results of 2, 4, 6 days respectively, conducting a comprehensive judgment as a final experiment result, and conducting a range analysis on a content retention, and selecting a primary and secondary relation and excellent combination.

(6) TABLE-US-00003 TABLE 3 Orthogonal Experiment Analysis Table of Content Retention Rate Experiment factors Content retention rate NO. A B 2 days 4 days 6 days 1 1 1 98.80% 96.10% 95.50% 2 1 2 99.00% 98.20% 97.50% 3 1 3 98.40% 96.50% 96.10% 4 2 2 98.80% 97.90% 97.00% 5 2 3 98.00% 96.50% 95.50% 6 2 1 99.20% 98.00% 97.50% 7 3 3 98.80% 97.20% 97.00% 8 3 1 99.10% 98.10% 97.50% 9 3 2 99.80% 98.30% 97.60% content k1 0.987 0.990 Comprehensive judgment: retention k2 0.987 0.992 Primary and secondary rate in k3 0.992 0.984 B > A 2 days R 0.006 0.008 Excellent combination Primary and B > A A3B2 secondary Excellent A3B2 combination content k1 0.969 0.974 retention k2 0.975 0.981 rate in 4 k3 0.979 0.967 days R 0.009 0.014 Primary and B > A secondary Excellent A3B2 combination content k1 0.964 0.968 retention k2 0.967 0.974 rate in 6 k3 0.974 0.962 days R 0.010 0.012 Primary and B > A secondary Excellent A3B2 combination

(7) It may be seen from the Orthogonal experiment table of Table 2 and Table 3 that affecting the stability of vitamin A content is mainly tocopherol, is secondly vitamin C palmitate. According to the comprehensive judgment, the excellent combination is A3B2, namely, 2% vitamin C palmitate and 8% α-tocopherol.

Example 2

(8) Vitamin A palmitate, vitamin C palmitate and β-tocopherol are blended and melted at 65° C. under nitrogen protection to form vitamin A palmitate molten oil. Gelatin and glucose are dissolved in water at 65° C. to form a gelatin and glucose aqueous phase solution. The vitamin A palmitate molten oil is poured into the gelatin and glucose aqueous phase solution and then emulsified under high-speed shear condition, degassed and homogenized, to obtain a stable emulsion. The stable emulsion (that is, vitamin A palmitate emulsion) is placed in a sample bottle and sealed from light, stored at 40° C., and respectively detected its content in 0, 1, 2, 3 weeks. Data of content retention rates of different antioxidant ratio emulsion are listed in the Table 4.

(9) TABLE-US-00004 TABLE 4 Statistical Table of Content Retention Rate of Vitamin A Palmitate Emulsion of Different Antioxidant Combination Content retention rates of Vitamin A Vitamin C palmitate NO. β-tocopherol palmitate 0 week 1 week 2 weeks 3 weeks 1 2.0% 0.0% 100% 92.5% 90.0% 86.1% 2 4.0% 0.0% 100% 92.2% 89.8% 86.5% 3 6.0% 0.0% 100% 92.9% 89.7% 87.5% 4 8.0% 0.0% 100% 93.0% 90.2% 88.2% 5 10.0% 0.0% 100% 93.1% 90.1% 89.5% 6 0.0% 0.5% 100% 92.6% 89.6% 85.8% 7 0.0% 1.0% 100% 92.8% 88.9% 85.9% 8 0.0% 1.5% 100% 92.7% 89.5% 86.5% 9 0.0% 2.0% 100% 93.0% 89.6% 86.8% 10 0.0% 2.5% 100% 92.8% 89.4% 86.6% 11 5.0% 2.5% 100% 97.2% 94.8% 92.8% 12 6.0% 2.0% 100% 97.6% 95.9% 93.6% 13 8.0% 2.0% 100% 98.5% 96.8% 95.2% 14 10.0% 2.0% 100% 98.4% 96.9% 95.3% 15 9.6% 1.6% 100% 98.3% 96.7% 95.1% 16 10.0% 1.4% 100% 97.8% 96.2% 94.2% 17 10.0% 1.2% 100% 97.5% 95.8% 93.3%

(10) It may be obviously seen from datum of Table 4 that the content retention rate of the vitamin A palmitate emulsion is higher in the range of formula ratio of the present invention.

Example 3

(11) 50 kg of vitamin A acetate crystal and 0.5 kg of vitamin C palmitate and 3.5 kg of synthetic tocopherol are blended and melted at 85° C. under nitrogen protection to form a vitamin A acetate molten oil. 75 kg of gelatin and 50 kg of glucose are dissolved in 130 kg of water at 60° C., to form a 49% gelatin and glucose aqueous phase solution.

(12) The vitamin A acetate molten oil is poured into the 49% gelatin and glucose aqueous phase solution and emulsified under high-speed shear condition, and then degassed and homogenized to obtain a stable emulsion; and then the stable emulsion is delivered into a starch bed to conduct a pray granulation, and then fluidized dried and crosslinked under high temperature to obtain 218 kg of water-repellent vitamin A acetate microcapsule. The content of vitamin A acetate is 520,000 IU/g and the microencapsulated yield is 95%, by the HPLC analysis. The vitamin A ester microcapsule is placed in a sample bottle and sealed from light, stored at 40° C. for 6 weeks, and the content of vitamin A ester is 490,000 IU/g, and the content retention rate is 94.2%.

Example 4

(13) 50 kg of coenzyme Q10 crystal and 0.5 kg of vitamin C palmitate and 3 kg of natural γ-tocopherol are blended and melted at 45° C. under nitrogen protection to form a coenzyme Q10 oil. 75 kg of gelatin and 50 kg of glucose are dissolved in 130 kg of water at 70° C., to form a 49% gelatin and glucose aqueous phase solution.

(14) The coenzyme Q10 oil is poured into the 49% gelatin and glucose aqueous phase solution and emulsified under high-speed shear condition, and then degassed and homogenized to obtain a stable emulsion, and then the stable emulsion is delivered into a starch bed to conduct a pray granulation, and then fluidized dried and crosslinked under high temperature to obtain 218 kg of water-repellent coenzyme Q10 microcapsule. The content of coenzyme Q10 is 52% and the microencapsulated yield is 95%, by the HPLC analysis. The coenzyme Q10 microcapsules are placed in a sample bottle and sealed away from light, stored at 40° C. for 6 weeks, and the content of coenzyme Q10 is 49%, and the content retention rate is 94.2%.

Examples 5-11

(15) The experiment method is the same as that of Example 1. Preparing different fat-soluble active ingredient oil and the retention rate is determined in the Table 5.

(16) TABLE-US-00005 TABLE 5 Retention rate of fat-soluble Fat-soluble Tocopherol active ingredient active Weight VC 0 1 2 3 Example ingredient Type ratio palmitate week week weeks weeks 5 Vitamin K α 5.0% 2.5% 100% 98.3% 97.6% 97.0% 6 Xanthin β 6.0% 2.0% 100% 98.6% 97.9% 97.0% 7 Astaxanthin γ 8.0% 2.0% 100% 98.7% 97.8% 96.5% 8 Lycopene Synthetic 10.0% 2.0% 100% 98.1% 96.5% 95.1% 9 DHA Natural 9.6% 1.6% 100% 98.5% 97.8% 96.3% Acetate 10 Linoleic Mixted 10.0% 1.4% 100% 97.8% 96.6% 96.4% acid glyceride 11 Linolenic Mixted 10.0% 1.2% 100% 98.0% 96.3% 95.2% acid phosphate

(17) It may be obviously seen from Table 5 that the content retention rate of the fat-soluble active ingredient is higher in the range of formula ratio of the present invention.

(18) Although the present invention has been described in connection with the above embodiments, it should be understood that the present invention is not limited to such preferred embodiments and procedures set forth above. The embodiments and procedures were chosen and described in order to best explain the principles of the invention and its practical application, to thereby enable others skilled in the art to best utilize the invention. It will be apparent to those skilled in the art that various substitution, modifications and changes may be thereto without departing from the scope and spirit of the invention. Therefore, the intention is intended to cover all alternative constructions and equivalents falling within the spirit and scope of the invention as defined only by the appended claims and equivalents thereto.