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Technology for producing low-caffeine catechin through non-solvent method

A low-caffeine, non-solvent technology, applied in organic chemistry and other directions, can solve the problems of complicated operation, great influence on product yield, toxic chloride, etc., and achieve the effects of simple and convenient operation, green and safe products, and easy industrialization.

Inactive Publication Date: 2011-04-13
福建绿叶茶业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. Using chlorides such as chloroform or dichloromethane to extract and remove caffeine from the tea extract, the removal rate is high, but due to the toxicity of chlorides, the product is affected as a raw material for medicinal or health care products;
[0004] 2. The extract of ethyl acetate is washed with acid or weak alkali to remove caffeine. The amount of acid or weak alkali used in this method is large, which has a great impact on the yield of the product, which limits its industrial application. Residues of organic solvents cause tea polyphenols or catechins to be imprisoned in the use of medicinal or health care raw materials;
[0005] 3. Use metal salt ions such as Ca 2+ 、Al 3+ , Zn 2+ Wait for the decomplexation of tea polyphenols, then use acid to dissolve the precipitate, and extract with ethyl acetate to remove caffeine. This method is similar to the second method. Due to the large use of metal salt ions and organic solvents, tea polyphenols or children Tea element is severely restricted in the use of medicinal or health product raw materials;
[0006] 4. Using supercritical CO 2 The extraction method extracts the caffeine in the tea leaves or the caffeine in the tea polyphenol products, the operation is complex, the equipment investment is large, the production cost is high, and it is difficult to promote in industrial production;
[0007] 5. The green tea extract or tea polyphenols were first enriched and decaffeinated and pigmented by two reagents of ethyl acetate and chloroform to obtain tea polyphenols with high content of catechins, and then passed through Sephadex LH-20 column Chromatographic purification to enrich EGCG. This process not only uses toxic organic solvents, but also uses Sephadex gel resin, which is expensive and has a long preparation cycle, which is difficult to promote in industrial production;
[0008] 6. High-purity EGCG can be separated and prepared by high-speed countercurrent chromatography using a two-phase solvent system consisting of alkanes, fatty esters, fatty alcohols and water, but the The process also uses a large amount of toxic organic solvents, and the production process is difficult to scale up, and industrial production is difficult

Method used

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  • Technology for producing low-caffeine catechin through non-solvent method
  • Technology for producing low-caffeine catechin through non-solvent method

Examples

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Effect test

example 1

[0025] 1) Weigh 1000.0g green tea, add 12L of deionized water at a solid-liquid ratio of 1:12, 45°C, ultrasonic frequency 28KHz, ultrasonic extraction for 30min, stop for 2min every 15min, filter the extract, repeat the extraction once, combine the two Filtrate, to obtain extract 17L;

[0026] 2) The filtrate was allowed to stand at 4°C for stratification, and the clarified liquid was separated with a ceramic membrane with a pore size of 100nm, the separation pressure was 0.1MPa, and the flow rate was 20ml / min, and the permeate was collected; the permeate was concentrated with a nanofiltration membrane (200dal) to 1 / 2 of the original volume;

[0027] 3) Load the concentrated solution onto a well-balanced lignocellulose resin chromatography column (the column specification is 20cm×1500mm), let it stand for 30min, and elute the four bed layers sequentially with 5% ethanol with a pH value of 5 (flow rate 1.9L / min), 35% ethanol with a pH value of 5 elutes 3 bed layers (flow rate ...

example 2

[0031] 1) Weigh 500.0g of green tea, add 7.5L of deionized water at a solid-to-liquid ratio of 1:15, 50°C, ultrasonic frequency 40KHz, ultrasonic extraction for 30min, stop for 2min every 15min, filter the extract, repeat the extraction once, combine Secondary filtrate to obtain 11L of extract;

[0032] 2) The filtrate was allowed to stand at 5°C for stratification, and the clarified liquid was separated with a ceramic membrane with a pore size of 200nm at a separation pressure of 0.1MPa and a flow rate of 20ml / min to collect the permeate; the permeate was concentrated with a nanofiltration membrane (400dal) to 1 / 2 of the original volume;

[0033] 3) Load the concentrated solution onto a well-balanced lignocellulose resin chromatographic column (the column specification is 20cm×1500mm), let it stand for 30min, and elute the four bed layers sequentially with 15% ethanol with a pH value of 3.5 (flow rate 2.0L / min), 45% ethanol with a pH value of 3.5 eluted 3 bed layers (flow ra...

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Abstract

The invention discloses technology for producing low-caffeine catechin through a non-solvent method, which comprises the following steps of: mixing broken green tea and deionized water according to a solid-liquid ratio of 1:10-1:15 and ultrasonically extracting; standing and demixing the filtrate, separating by using a ceramic film, concentrating permeating liquid by using a nanofiltration membrane, separating and purifying by using a natural lignocellulose resin, and collecting and eluting the fraction; and performing concentrating and spray drying on the eluted fraction by using the nanofiltration membrane. The technology is easy and convenient to operate, low in cost and investment, and pollution-free, ensures green and safe products and is easy for industrialization. Compared with the conventional production technology, the technology does not need to use a lot of production reagents which pollute the environment and are harmful to a human body, has the advantages of high product purity and short production cycle, and meets the requirements on environment friendliness and safety.

Description

technical field [0001] The invention relates to a process for producing low-caffeine catechins, in particular to a process for producing low-caffeine catechins by a non-solvent method. Background technique [0002] Since the medicinal and health functions of catechins or tea polyphenols have attracted more and more attention, the technological process of extracting tea polyphenols or catechins from tea has developed rapidly in recent years, but the obtained tea polyphenols or It is difficult to remove caffeine and enrich EGCG at the same time in catechin products, and the content of caffeine and EGCG in the product has a great influence on the application of the product. At present, in order to remove caffeine and enrich EGCG from tea polyphenols or catechin products in industry, there are mainly the following methods: [0003] 1. Using chlorides such as chloroform or dichloromethane to extract and remove caffeine from the tea extract, the removal rate is high, but due to t...

Claims

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Application Information

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IPC IPC(8): C07D311/62
Inventor 张星海许金伟
Owner 福建绿叶茶业股份有限公司
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