CN102086186A - Method for preparing tea polyphenol rich in methylated catechin - Google Patents
Method for preparing tea polyphenol rich in methylated catechin Download PDFInfo
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- CN102086186A CN102086186A CN2011100072754A CN201110007275A CN102086186A CN 102086186 A CN102086186 A CN 102086186A CN 2011100072754 A CN2011100072754 A CN 2011100072754A CN 201110007275 A CN201110007275 A CN 201110007275A CN 102086186 A CN102086186 A CN 102086186A
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Abstract
The invention discloses a method for preparing tea polyphenol rich in methylated catechin from tea cultivated in China. The method comprises the following steps: taking the tea cultivated in China, with higher content of methylated catechin, as a raw material, extracting with hot water, and drying to obtain a crude extract; treating the crude extract with a macroporous resin A to obtain a tea polyphenol component I (with content of methylated catechin being about 18%) rich in methylated catechin; separating and purifying the tea polyphenol component I rich in methylated catechin with a Toyopearl HW-40S resin to obtain monomer components (with purity being more than 95%) of (-)-epigallocatechin3-O-(3-O-methyl) gallate (EGCG3''Me) and (-)-3-O-methyl-epicatechin gallate (ECG3' Me) respectively; and treating the tea polyphenol component I rich in methylated catechin with a macroporous resin B to obtain a tea polyphenol II (with content of methylated catechin being more than 60%) rich in methylated catechin. As a preparation process with the advantages of low cost, high efficiency and environment friendliness, the method is easy to implement industrial production and has broad application prospects.
Description
Technical field
The present invention relates to a kind of adsorption chromatography post method of utilizing, with in homemade tealeaves be raw material, utilize the specific adsorption of macroporous resin to functional ingredient in the tealeaves, the method for the catechin tea polyphenol that methylates is rich in preparation.
Background technology
For a long time, tealeaves is subjected to liking of people always, is only second to water, is the most very popular in the world beverage.Except the immensely popular color, smell and taste, also subdue the mankind with its effect that is of illnesses and fitness, and the local flavor of tea and nourishing function just the peculiar polyphenolic substance of tealeaves given.
Tea-polyphenol is the general name that catechin (flavanol compound), anthocyan (anthocyanidin and leucoanthocyanidin), anthoxanthins (flavones and flavonoid) etc. combine in a group polyphenol complex in the tealeaves.Wherein catechin accounts for 60%-80%, is divided into ester catechin and free type catechin, and ester catechin accounts for about 70% of catechin.Aldehydes matter is in the news for a long time and has multiple physiologically active, especially NVP-XAA 723 (EGCG).Discovered in recent years and contained another kind of catechin in the tealeaves, be the derivative that methylates of catechin, based on (-)-epigallocatechin 3-O (3-O-methyl) gallic acid ester (EGCG3 " Me) and (-)-epigallocatechin 3-O (4-O-methyl) gallic acid ester (EGCG4 " Me).Present research about the catechin physiological function that methylates mainly concentrates on the research aspect to the anti-allergic effects of the EGCG that methylates, especially modal pollen hypersensitivity is had significant prevention and restraining effect.
In Japan, the product that part is rich in the EGCG that methylates has entered the business development stage, and in food service industry, interpolations such as biscuit, chewing gum, the tea drink EGCG feeding product industry that methylates has been injected new attraction, has obtained more human consumers' favor.Therefore, the research of the catechin that methylates is most important, is all having very important significance aspect science, the biology.
At present, external synthetic the mainly contain chemical method and the biological enzyme of the catechin that methylates of research report.But, needing to use a large amount of organic solvents and various radical protection agent in the chemical synthesis, synthetic reaction condition is comparatively harsh, and specificity is poor, and by product is many, and therefore, chemosynthesis should not be as the external synthetic method of the catechin that methylates.Though the synthetic specificity of external enzyme process is strong, reaction conditions is gentle, safe, the vitro conversion research of the catechin that methylates at present all less than carrying out separation and purification and structure elucidation to synthesizing reactant, does not realize a large amount of preparations of enzyme process synthetic product.From tealeaves, directly extract the catechin that methylates,, security is preferably arranged because it derives from natural product.From the foodstuffs industry angle, as a kind of functional base-material of a large amount of uses, must consider the raw material abundance, convenient, be easy to get nontoxicity, problem such as production cost is low.Therefore, reasonable method is directly to extract the catechin that methylates from tealeaves.Measure through experimental analysis, the content of the catechin that relatively methylates in the homemade tealeaves in some, in the discovery in the homemade tealeaves catechin content that methylates of some tealeaves higher.Therefore can utilize these tealeaves to be raw material,, prepare the tea-polyphenol product that is rich in the catechin that methylates in conjunction with the technology of adsorpting column chromatography method.
Summary of the invention
The technical problem to be solved in the present invention be with in homemade tealeaves be raw material, provide a kind of preparation to be rich in the method for the catechin tea polyphenol that methylates, can guarantee that the product purity height, the cost that extract are low, efficient is high, environmental friendliness, and technology is easy to realize suitability for industrialized production.For addressing the above problem, the invention provides homemade tealeaves in a kind of utilize and be rich in the method for the catechin tea polyphenol that methylates as feedstock production, comprise following processing step:
1) tealeaves is through hot water extraction, and drying obtains the tea-polyphenol crude extract;
2) adopt specific macroporous resin A to handle tea-polyphenol phase extract, the abundant wash-out of first water is removed pigment and trimethyl-xanthine;
3) then with certain density ethanolic soln wash-out, collect elutriant,, obtain being rich in the tea-polyphenol component I (catechin content about 18% methylates) of catechin of methylating through concentrated and dry;
4) adopt Toyopearl HW-40S plastic resin treatment to be rich in the tea-polyphenol component I of the catechin that methylates, with certain density ethanolic soln wash-out, collect the elutriant of different time, through concentrating and dry, obtain respectively (-)-Biao do not have food to give the monomer component (purity is all greater than 95%) of catechin 3-O (3-O-methyl) gallic acid ester (EGCG3 " Me) and (-)-3-O-methyl-L-Epicatechin gallate (ECG3 ' Me);
5) adopt specific macroporous resin B to handle the tea-polyphenol component I that is rich in the catechin that methylates, with certain density ethanolic soln wash-out, collect the elutriant of specified time,, obtain being rich in the tea-polyphenol II (catechin content that methylates＞60%) of catechin of methylating through concentrating and dry.
" Me and ECG3 ' Me purity are all greater than 95%; methylate catechin content greater than 60% among the tea-polyphenol II that is rich in the catechin that methylates for preparing; the macroporous adsorbent resin regenerability is good; the recycling of can regenerating; eluent ethanol is nontoxic, also can reclaim repeatedly and utilize for the EGCG3 that technology of the present invention is extracted.This technology cost is low, efficient is high, environmental friendliness, is easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the HPLC collection of illustrative plates that is rich in the tea-polyphenol component I of the catechin that methylates (wherein 8.332min and 10.286min are respectively EGCG3 " Me and ECG3 ' Me)
Fig. 2 is EGCG3 " the HPLC collection of illustrative plates of Me
Fig. 3 is EGCG3 " the hydrogen nuclear magnetic resonance spectrogram of Me
Fig. 4 is the hydrogen nuclear magnetic resonance spectrogram of ECG3 ' Me
Specific implementation method
1) tea-polyphenol crude extract: tealeaves hot water bath lixiviate 30min, solid-liquid ratio 1: 20, bath temperature are 80 ℃, carry out concentrating under reduced pressure after the lixiviate under 40 ℃;
2) macroporous resin A handles: choose macroporous resin A, with pH3.0 damping fluid balance, sample solution also is adjusted to same pH, the abundant wash-out of water behind the last sample, and the elution flow rate of water is 2 column volumes per hour;
3) be rich in the tea-polyphenol component I of the catechin that methylates: use the ethanolic soln wash-out macroporous resin A of 80% concentration, flow velocity is 1 column volume per hour, collects elutriant, carries out concentrating under reduced pressure under 50 ℃;
4) Toyopearl HW-40S plastic resin treatment: choose Toyopearl HW-40S resin, be rich in the ethanolic soln wash-out resin that uses 40% concentration on the tea-polyphenol component I of the catechin that methylates behind the sample, flow velocity is 1 column volume per hour, collect the elutriant of different time respectively, with the different components collected in 40 ℃ of following concentrating under reduced pressure, drying;
5) macroporous resin B handles: choose macroporous resin B, be rich in the ethanolic soln wash-out resin that uses 70% concentration on the tea-polyphenol component I of the catechin that methylates behind the sample, flow velocity is 1 column volume per hour, collects the elutriant of specified time, in 40 ℃ of following concentrating under reduced pressure, drying.
Claims (6)
1. the method for the catechin tea polyphenol that methylates is rich in preparation, comprises the steps:
1) through hot water extraction, drying obtains the tea-polyphenol crude extract to tealeaves (catechin content that methylates higher in homemade tealeaves);
2) adopt specific macroporous resin A to handle the tea-polyphenol crude extract, the abundant wash-out of first water is removed pigment and trimethyl-xanthine;
3) then with certain density ethanolic soln wash-out, collect elutriant,, obtain being rich in the tea-polyphenol component I (catechin content about 18% methylates) of catechin of methylating through concentrated and dry;
4) adopt Toyopearl HW-40S plastic resin treatment to be rich in the tea-polyphenol component I of the catechin that methylates, with certain density ethanolic soln wash-out, collect the elutriant of different time, through concentrating and dry, obtain (-)-epigallocatechin 3-O the monomer component (purity is all greater than 95%) of (3-O-methyl) gallic acid ester (EGCG3 " Me) and (-)-3-O-methyl-L-Epicatechin gallate (ECG3 ' Me) respectively;
5) adopt specific macroporous resin B to handle the tea-polyphenol component I that is rich in the catechin that methylates, with certain density ethanolic soln wash-out, collect the elutriant of specified time,, obtain being rich in the tea-polyphenol II (catechin content that methylates＞60%) of catechin of methylating through concentrating and dry;
2. be rich in the method for the catechin tea polyphenol that methylates according to the preparation under the claim 1, it is characterized in that the solid-liquid ratio that tealeaves extracts in the step 1) is 1: 20, at 80 ℃ of following water-bath lixiviate 30min.
3. be rich in the method for the catechin tea polyphenol that methylates according to the preparation under the claim 1, it is characterized in that step 2) in the macroporous resin A that chooses, damping fluid balance with pH2.0-3.0, sample solution also is adjusted to identical pH value, the abundant wash-out of water behind the last sample, the elution flow rate of water is 1-2 column volume per hour.
4. be rich in the method for the catechin tea polyphenol that methylates according to the preparation under the claim 1, it is characterized in that using in the step 3) certain density ethanolic soln (30%-50%) wash-out macroporous resin A, flow velocity is 1-2 column volume per hour, collects elutriant, at 40-50 ℃ of following concentrating under reduced pressure.
5. be rich in the method for the catechin tea polyphenol that methylates according to a kind of preparation under the claim 1, it is characterized in that the Toyopearl HW-40S resin chosen in the step 4), be rich in and use certain density ethanolic soln (70%-80%) wash-out resin on the tea-polyphenol component I of the catechin that methylates after the sample, flow velocity is 1-2 column volume per hour, collect the elutriant of different time respectively, with the different components collected in 40-50 ℃ of following concentrating under reduced pressure, drying.
6. be rich in the method for the catechin tea polyphenol that methylates according to a kind of preparation under the claim 1, it is characterized in that the macroporous resin B that chooses in the step 5), be rich in and use certain density ethanolic soln (70%-80%) wash-out resin on the tea-polyphenol component I of the catechin that methylates after the sample, flow velocity is 1-2 column volume per hour, collect the elutriant of specified time, in 40-50 ℃ of following concentrating under reduced pressure, drying.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102240343A (en) * | 2011-05-23 | 2011-11-16 | 中国农业科学院茶叶研究所 | Environment-friendly preparation method for high-ester catechin tea polyphenol |
| CN102432577A (en) * | 2011-11-10 | 2012-05-02 | 湖南农业大学 | Method for separating and purifying epicatechin gallate (ECG) monomer |
| CN102702163A (en) * | 2012-06-01 | 2012-10-03 | 广西济康生物科技有限公司 | Method for preparing high-purity monomer epigallocatechin gallate from processed leftovers of tea leaves |
| CN102870926A (en) * | 2012-10-30 | 2013-01-16 | 广州牌牌生物科技有限公司 | Method for preparing instant tea without alkaloid components including caffeine and theophylline etc. |
| CN103462041A (en) * | 2013-08-06 | 2013-12-25 | 浙江省农业科学院 | Antiallergic citrus dietary fiber preparation method and product thereof |
| WO2015089684A1 (en) * | 2013-12-16 | 2015-06-25 | 刘登富 | Method for preparation of tea tannin extract by leaching |
| CN104820059A (en) * | 2015-04-22 | 2015-08-05 | 湖南农业大学 | Method for rapidly screening tea tree resource containing EGCG3''Me (Epigallocatechin Gallate) |
| CN105585550A (en) * | 2016-01-28 | 2016-05-18 | 南京农业大学 | Preparation method of serial methylated catechin monomers |
-
2011
- 2011-01-14 CN CN2011100072754A patent/CN102086186A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| BING HU,ET AL: "Efficient procedure for isolating methylated catechins from green tea and effective simultaneous analysis of ten catechins, three purine alkaloids,and gallic acid in tea by high-performance liquid chromatography with diode array detection", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 周蓓等: "茶叶中甲基化儿茶素的分离、纯化和高效液相色谱法分析", 《分析化学》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102240343A (en) * | 2011-05-23 | 2011-11-16 | 中国农业科学院茶叶研究所 | Environment-friendly preparation method for high-ester catechin tea polyphenol |
| CN102432577A (en) * | 2011-11-10 | 2012-05-02 | 湖南农业大学 | Method for separating and purifying epicatechin gallate (ECG) monomer |
| CN102432577B (en) * | 2011-11-10 | 2013-03-20 | 湖南农业大学 | Method for separating and purifying epicatechin gallate (ECG) monomer |
| CN102702163A (en) * | 2012-06-01 | 2012-10-03 | 广西济康生物科技有限公司 | Method for preparing high-purity monomer epigallocatechin gallate from processed leftovers of tea leaves |
| CN102702163B (en) * | 2012-06-01 | 2014-07-09 | 广西济康生物科技有限公司 | Method for preparing high-purity monomer epigallocatechin gallate from processed leftovers of tea leaves |
| CN102870926A (en) * | 2012-10-30 | 2013-01-16 | 广州牌牌生物科技有限公司 | Method for preparing instant tea without alkaloid components including caffeine and theophylline etc. |
| CN103462041A (en) * | 2013-08-06 | 2013-12-25 | 浙江省农业科学院 | Antiallergic citrus dietary fiber preparation method and product thereof |
| CN103462041B (en) * | 2013-08-06 | 2014-12-17 | 浙江省农业科学院 | Antiallergic citrus dietary fiber preparation method and product thereof |
| WO2015089684A1 (en) * | 2013-12-16 | 2015-06-25 | 刘登富 | Method for preparation of tea tannin extract by leaching |
| CN104820059A (en) * | 2015-04-22 | 2015-08-05 | 湖南农业大学 | Method for rapidly screening tea tree resource containing EGCG3''Me (Epigallocatechin Gallate) |
| CN105585550A (en) * | 2016-01-28 | 2016-05-18 | 南京农业大学 | Preparation method of serial methylated catechin monomers |
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Application publication date: 20110608 |