WO2017185291A1

WO2017185291A1 - Method for preparing natural composite antioxidant of lycium ruthenicum murr

Info

Publication number: WO2017185291A1
Application number: PCT/CN2016/080487
Authority: WO
Inventors: 金英花
Original assignee: 金英花
Priority date: 2016-04-28
Filing date: 2016-04-28
Publication date: 2017-11-02

Abstract

A method for preparing a natural composite antioxidant of lycium ruthenicum murr comprises the following steps: pulverizing lycium ruthenicum murr, liquoric roots, rosemary and fresh ginger, drying the them to a constant weight, and placing them into petroleum ether to make them soaked and allowing them to be subjected to degreasing; adding alcohol solution to allow the flow back to be carried out 10 h to 20 h; carrying out filtering, adding water into the filtrate to evenly mix; feeding the product into macroporous resin to carry out refinement, the refinement conditions comprising: the PH of the liquid fed up to a cylinder ranging 6.1 to 6.8, the temperature of the liquid fed up to the cylinder ranging 50ºC to 58ºC, and flow speed ranging from 1 mL/min to 2 mL/min in the adsorption stage; using deionized water in a washing stage, the speed of the deionized water passing through the cylinder ranging from 1 mL/min to 3 mL/min; using 70-80wt％ alcohol solution in a desorption stage, the speed of the deionized water passing through the cylinder ranging from 2 mL/min to 5 mL/min; and drying the desorbed extract liquid to a constant weight, adding lecithin, vitamin C, citric acid and tea polyphenol to carrying out compounding, drying the product to a constant weight, and carrying sterilization, so as to obtain the natural composite antioxidant of lycium ruthenicum murr. The prepared product has a high oxidative activity, a simple process and low costs.

Description

Preparation method of black fruit 枸杞 natural composite antioxidant

Technical field

The invention relates to the technical field of natural composite antioxidants, in particular to a preparation method of natural composite antioxidants of black berry.

Background technique

With the continuous advancement of the food industry, food antioxidants have also been greatly developed. For a long time, synthetic antioxidants such as dibutylhydroxytoluene, butylhydroxyanisole, butyl hydroquinone, propyl gallate, etc. have been used, which are easy to decompose, low in efficacy and irritating, and animal experiments have shown that synthesis Antioxidants also have toxic and carcinogenic effects. Synthetic antioxidants cause people to feel uneasy. Now people have turned their research focus to natural antioxidants and have achieved many research results. However, a single natural antioxidant has low activity, a complicated process, and low cost.

Summary of the invention

The invention provides a preparation method of natural compound antioxidant of black berry, which has high oxidation activity, simple process and low cost.

The preparation method of the black fruit 枸杞 natural composite antioxidant proposed by the invention comprises the following steps:

S1, 40-60 parts of black berry, 5-15 parts of licorice, 1-5 parts of rosemary, 2-6 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 2-3 hours Air drying

S3, adding 100-200 parts of a 60-70 wt% ethanol solution to the air-dried material of S1 for 10-20 h, filtering, adding 50-100 parts of water to the filtrate, mixing uniformly, and feeding into a macroporous resin column for purification. The purification conditions are as follows: the pH of the upper column liquid is 6.1-6.8, the temperature of the upper column is 50-58 ° C, the flow rate of the adsorption stage is 1-2 mL/min; the water washing stage uses deionized water, and the flow rate of the deionized water is 1 -3mL / min, the desorption stage using 70-80wt% ethanol solution, ethanol solution column flow rate of 2-5mL / min;

S3, drying the desorbed extract to constant weight, adding 1-5 parts of lecithin, 2-10 parts of vitamin C, 1-5 parts of citric acid, 1-5 parts of tea polyphenols, compounding, drying to constant weight , sterilization, get the natural complex antioxidant of black fruit.

Further, in S1, the weight ratio of black berry, licorice, rosemary and ginger is 50-55:8-12:2-3.5:3-5 parts.

Further, in S2, the purification conditions are: the pH of the upper column liquid is 6.2-6.5, the temperature of the upper column is 52-56 ° C, the flow rate of the adsorption stage is 1.2-1.6 mL/min; and the water washing stage uses deionized water. The flow rate of deionized water through the column was 2-2.5 mL/min, and the desorption stage used 72-76 wt% ethanol solution, and the flow rate of the ethanol solution was 3.5-4.2 mL/min.

Further, in S3, the weight ratio of lecithin, vitamin C, citric acid, and tea polyphenol is 2-4.5:5-8:2-4:2-4.

Further, the method for preparing the black fruit 枸杞 natural composite antioxidant comprises the following steps:

S1, 50-55 parts of black berry, 8-12 parts of licorice, 2-3.5 parts of rosemary, 3-5 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 2-3 hours Air drying

S3, adding 120-156 parts of a 62-64 wt% ethanol solution to the air-dried material of S1 for 12-16 hours, filtering, adding 80-95 parts of water to the filtrate, uniformly mixing, and feeding into a macroporous resin column for purification. The purification conditions are as follows: the pH of the upper column liquid is 6.2-6.5, the temperature of the upper column is 52-56 ° C, the flow rate of the adsorption stage is 1.2-1.6 mL/min; the water washing stage uses deionized water, and the flow rate of the deionized water is 2-2.5mL / min, desorption stage using 72-76wt% ethanol solution, ethanol solution column flow rate of 3.5-4.2mL / min;

S3, drying the desorbed extract to constant weight, adding 2-4.5 parts of lecithin, 5-8 parts of vitamin C, 2-4 parts of citric acid, 2-4 parts of tea polyphenols, and drying to constant weight , sterilization, get the natural complex antioxidant of black fruit.

In the present invention, the natural composite antioxidant of the black berry prepared by the above process maximizes the effectiveness of the active ingredient, and the synergistic effect of lecithin, vitamin C and citric acid is added, and on the one hand, the single oxidant function is overcome. On the other hand, synergy not only has a synergistic effect, but also has higher antioxidant activity, and can play its own functions among different components, and has a multi-purpose function; added tea polyphenols and black berry, licorice extract Synergistic action not only can greatly improve the anti-oxidation performance, but also can effectively extend the shelf life of the product and improve food safety; the product has no pollution to the environment during the preparation process, and the production process is simple and convenient for practical operation.

detailed description

Hereinafter, the technical solution of the present invention will be described in detail through specific embodiments.

Example 1

A method for preparing a natural composite antioxidant of black berry, comprising the following steps:

S1, 40 parts by weight of black quince, 15 parts of licorice, 1 part of rosemary, 6 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 2h, air dried;

S3, adding 200 parts of a 60% by weight ethanol solution to the air-dried material of S1 for 20 hours, filtering, adding 50 parts of water to the filtrate, mixing uniformly, and feeding into a macroporous resin column for purification, the purification condition is: upper column liquid The pH value is 6.8, the upper column temperature is 50 °C, the adsorption phase flow rate is 2 mL/min; the water washing stage uses deionized water, the deionized water cross column flow rate is 1 mL/min, and the desorption stage uses 80 wt% ethanol solution, ethanol solution The column flow rate is 2 mL/min;

S3, drying the desorbed extract to constant weight, adding 5 parts of lecithin, 2 parts of vitamin C, 5 parts of citric acid, 1 part of tea polyphenols, compounding, drying to constant weight, sterilizing, obtaining black berry natural Compound antioxidant.

Example 2

S1, 60 parts by weight of black quince, 5 parts of licorice, 5 parts of rosemary, 2 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 3 hours, air-dried;

S3, adding 100 parts of 70% by weight ethanol solution to the air-dried material of S1, refluxing for 10 hours, filtering, adding 100 parts of water to the filtrate, mixing uniformly, and feeding into a macroporous resin column for purification, the purification condition is: upper column liquid The pH value is 6.1, the upper column temperature is 58 ° C, the adsorption phase flow rate is 1 mL/min; the water washing stage uses deionized water, the deionized water cross column flow rate is 3 mL/min, and the desorption stage uses 70 wt% ethanol solution, ethanol solution The column flow rate is 5 mL/min;

S3, drying the desorbed extract to a constant weight, adding 1 part of lecithin, 10 parts of vitamin C, 1 part of citric acid, 5 parts of tea polyphenols, compounding, drying to constant weight, sterilizing, obtaining black berry natural Compound antioxidant.

Example 3

S1, 50 parts by weight of black quince, 12 parts of licorice, 2 parts of rosemary, 3-5 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 2h, air dried;

S3, adding 156 parts of a 62% by weight ethanol solution to the air-dried material of S1 for 16 hours. Filtration, adding 80 parts of water to the filtrate and mixing well, and feeding it into a macroporous resin column for purification. The purification conditions are as follows: the pH of the upper column liquid is 6.5, the temperature of the upper column is 52 ° C, and the flow rate of the adsorption stage is 1.6 mL/min. The water washing stage uses deionized water, the deionized water flow rate is 2 mL/min, the desorption stage uses 76 wt% ethanol solution, and the ethanol solution cross column flow rate is 3.5 mL/min;

S3, drying the desorbed extract to a constant weight, adding 4.5 parts of lecithin, 5 parts of vitamin C, 4 parts of citric acid, 2 parts of tea polyphenols, compounding, drying to constant weight, sterilizing, obtaining black berry natural Compound antioxidant.

Example 4

S1, 55 parts of black berry, 8 parts of licorice, 3.5 parts of rosemary, 3 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 3 hours, air-dried;

S3, adding 120 parts of a 64% by weight ethanol solution to the air-dried material of S1 for 12 hours, filtering, adding 95 parts of water to the filtrate, mixing uniformly, and feeding into a macroporous resin column for purification, the purification condition is: upper column liquid The pH value is 6.2, the upper column temperature is 56 ° C, the adsorption phase flow rate is 1.2 mL / min; the water washing stage uses deionized water, the deionized water cross column flow rate is 2.5 mL / min, and the desorption stage uses 72 wt% ethanol solution, ethanol The flow rate of the solution through the column was 4.2 mL/min;

S3, drying the desorbed extract to constant weight, adding 2 parts of lecithin, 8 parts of vitamin C, 2 parts of citric acid, 4 parts of tea polyphenols, compounding, drying to constant weight, sterilizing, obtaining black berry natural Compound antioxidant.

Example 5

S1, 53 parts of black berry, 10.6 parts of licorice, 3.2 parts of rosemary, 4.5 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 2.5 hours, air-dried;

S3, adding 152 parts of the 65% by weight ethanol solution to the air-dried material of S1 for 14 hours, filtering, adding 92 parts of water to the filtrate, mixing uniformly, and feeding into a macroporous resin column for purification, the purification condition is: upper column liquid The pH value is 6.4, the upper column temperature is 53 ° C, the adsorption phase flow rate is 1.4 mL / min; the water washing stage uses deionized water, the deionized water cross column flow rate is 2.2 mL / min, and the desorption stage uses 74 wt% ethanol solution, The flow rate of the ethanol solution was 3.8 mL/min;

S3, drying the desorbed extract to a constant weight, adding 3.6 parts of lecithin, 7.5 parts of vitamin C, 3.5 parts of citric acid and 3.6 parts of tea polyphenols were compounded, dried to constant weight, and sterilized to obtain a natural composite antioxidant of black berry.

The above is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any technical person skilled in the art within the technical scope disclosed by the present invention, the technical solution according to the present invention Equivalent substitutions or modifications of the inventive concept are intended to be included within the scope of the invention.

Claims

A method for preparing a natural composite antioxidant of black berry, which comprises the following steps:

S1, 40-60 parts of black berry, 5-15 parts of licorice, 1-5 parts of rosemary, 2-6 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 2-3 hours Air drying

S3, adding 100-200 parts of a 60-70 wt% ethanol solution to the air-dried material of S1 for 10-20 h, filtering, adding 50-100 parts of water to the filtrate, mixing uniformly, and feeding into a macroporous resin column for purification. The purification conditions are as follows: the pH of the upper column liquid is 6.1-6.8, the temperature of the upper column is 50-58 ° C, the flow rate of the adsorption stage is 1-2 mL/min; the water washing stage uses deionized water, and the flow rate of the deionized water is 1 -3mL / min, the desorption stage using 70-80wt% ethanol solution, ethanol solution column flow rate of 2-5mL / min;

S3, drying the desorbed extract to constant weight, adding 1-5 parts of lecithin, 2-10 parts of vitamin C, 1-5 parts of citric acid, 1-5 parts of tea polyphenols, compounding, drying to constant weight , sterilization, get the natural complex antioxidant of black fruit.
The method for preparing a black berry natural composite antioxidant according to claim 1, wherein in S1, the weight ratio of black berry, licorice, rosemary and ginger is 50-55:8-12:2-3.5. : 3-5 servings.
The method for preparing a natural composite antioxidant of black berry according to claim 1, wherein in S2, the purification condition is: the pH of the upper column liquid is 6.2-6.5, the temperature of the upper column is 52-56 ° C, and the adsorption stage The flow rate is 1.2-1.6mL/min; the water washing stage uses deionized water, the deionized water cross-column flow rate is 2-2.5mL/min, the desorption stage uses 72-76wt% ethanol solution, and the ethanol solution cross-column flow rate is 3.5-4.2 mL/min.
The method for preparing a black berry natural composite antioxidant according to claim 1, wherein the weight ratio of lecithin, vitamin C, citric acid and tea polyphenol in S3 is 2-4.5:5-8:2- 4:2-4.
A method for preparing a natural composite antioxidant of black berry, which comprises the following steps:

S1, 50-55 parts of black berry, 8-12 parts of licorice, 2-3.5 parts of rosemary, 3-5 parts of ginger, crushed, dried to constant weight, placed in petroleum ether soaked for 2-3 hours Air drying

S3, adding 120-156 parts of a 62-64 wt% ethanol solution to the air-dried material of S1 for 12-16 hours, filtering, adding 80-95 parts of water to the filtrate, uniformly mixing, and feeding into a macroporous resin column for purification. The purification conditions are as follows: the pH of the upper column liquid is 6.2-6.5, the temperature of the upper column is 52-56 ° C, and the flow in the adsorption stage The speed is 1.2-1.6mL/min; the deionized water is used in the water washing stage, the flow rate of the deionized water is 2-2.5mL/min, the 72-76wt% ethanol solution is used in the desorption stage, and the flow rate of the ethanol solution is 3.5-4.2mL. /min;

S3, drying the desorbed extract to constant weight, adding 2-4.5 parts of lecithin, 5-8 parts of vitamin C, 2-4 parts of citric acid, 2-4 parts of tea polyphenols, and drying to constant weight , sterilization, get the natural complex antioxidant of black fruit.