CN101665482B - Method for purifying proanthocyanidins in peanut coat - Google Patents
Method for purifying proanthocyanidins in peanut coat Download PDFInfo
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- CN101665482B CN101665482B CN2009101784157A CN200910178415A CN101665482B CN 101665482 B CN101665482 B CN 101665482B CN 2009101784157 A CN2009101784157 A CN 2009101784157A CN 200910178415 A CN200910178415 A CN 200910178415A CN 101665482 B CN101665482 B CN 101665482B
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- proanthocyanidin
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- proanthocyanidins
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- arachidis hypogaeae
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Abstract
The invention discloses a method for purifying the proanthocyanidins in peanut coat, comprising the steps of: (1) adding the degreased peanut coat into alcohol solution, microwave extracting and then leaching; concentrating filtrate, and obtaining crude product of the proanthocyanidins by vacuum freezing and drying; (2) preparing the crude product obtained in the step (1) into the proanthocyanidins solution, and passing through HPD-826 macroporous absorption resin filled column; then, eluting by using distilled water for removing impurities and eluting by using alcohol; and (3) concentrating, freezing and drying the obtained eluent of the alcohol, and obtaining the fine finished product of the proanthocyanidins in the peanut coat. The method has high absorption quantity for the proanthocyanidins and purity of the product, and ensures the resin to easily regenerate, thus being applicable to large-scale industrialized production.
Description
Technical field
The present invention relates to a kind of purification process, specifically, relate to proanthocyanidin purification process in a kind of Testa arachidis hypogaeae.
Background technology
Proanthocyanidin (Proanthocyanidins) is a big class polyphenolic compound that extensively exists in the vegitabilia, is the general name of flavan-3-alcohol derivative.It is to be polymerized by catechin, l-Epicatechol, comprises dimer, tripolymer, the tetramer, until ten aggressiveness.Proanthocyanidin has very strong biological activity, can remove superfluous free radical in the human body, and has a stronger resistance of oxidation, can be used as the main effective constituent of anti-cancer, anti-mutation, control cardiovascular disease medicine, and can suppress microbial growth, can be used as the new type natural antioxidant and the sanitas of safety non-toxic.
Contain abundant proanthocyanidin in the Testa arachidis hypogaeae, content accounts for 17% of Testa arachidis hypogaeae dry weight, but
The thick product of the proanthocyanidin that extracts from Testa arachidis hypogaeae is lower with purity, in order to make its due effect of performance, must carry out purifying to crude product.At present, to the separation and purification of proanthocyanidin, the industrial chromatography that adopt more, macroporous adsorbent resin is cheap and easy to get in the chromatography, and has that absorption is fast, desorb is fast, loading capacity is big, be easy to advantages such as regeneration, long service life.
Summary of the invention
The objective of the invention is to disclose a kind of can purifying Testa arachidis hypogaeae proanthocyanidin novel method, utilize this novel method to carry out separation and purification, the product purity height, be easy to regeneration.
For achieving the above object, the present invention adopts following steps:
(1) the defatted peanut clothing is joined ethanolic soln, suction filtration behind the microwave extracting, filtrate concentrates, 20Pa ,-4 ℃ of vacuum lyophilizations get the proanthocyanidin crude product
(2) the resulting crude product with step (1) is mixed with proanthocyanidin solution, by HPD-826 macroporous adsorbent resin packed column; The distilled water wash-out is removed impurity then, uses ethanol elution again.
(3) ethanol eluate of gained is concentrated, 20Pa ,-4 ℃ of lyophilizes get Testa arachidis hypogaeae proanthocyanidin highly finished product.
The purity that detects the proanthocyanidin of this sample with Vanillin-salt acid system is 92.05%.
(m: ratio v) added in 40% ethanolic soln defatted peanut clothing described in the step (1) in 1: 25; Described microwave extracting is that setting power is that 600W, temperature are 40 ℃, stirs extraction 90S.
The described proanthocyanidin concentration of step (2) is 10-12mg/ml; Flow velocity by HPD-826 macroporous adsorbent resin packed column is 0.5-1ml/min; Described distilled water wash-out 4BV; Described ethanol elution is the ethanol elution 2BV with 5%, and elution flow rate is 0.5-1ml/min.
The method of not listing in detail among the present invention is and well known to a person skilled in the art ordinary method as suction filtration, Vanillin-salt acid system etc.
The invention provides a kind of novel method of Testa arachidis hypogaeae proanthocyanidin purifying, utilize macroporous adsorbent resin that the proanthocyanidin in the Testa arachidis hypogaeae is carried out specific adsorption, again according to the difference of Different concentrations of alcohol, thereby reach the purpose of proanthocyanidin purifying to the analytic ability of adsorption sample.The advantage of present method is that absorption is fast, desorb is fast, loading capacity is big, products obtained therefrom purity height, be easy to advantage such as regeneration.
Embodiment
The invention will be further described below in conjunction with specific embodiment, to help understanding content of the present invention.Confirm that through the contriver step of the present invention and parameter all can realize purpose of the present invention.
Embodiment 1
(1) (m: ratio v) added 40% ethanolic soln, and setting power is that 600W, temperature are 40 ℃ in the microwave extracting instrument, stirs extraction 90S in 1: 25 with the defatted peanut clothing, extraction finishes the back suction filtration, and filtrate concentrates, 20Pa,-4 ℃ of vacuum lyophilizations get the proanthocyanidin crude product
(2) the resulting crude product of step (1) is mixed with proanthocyanidin concentration be the solution of 10mg/ml with the flow velocity of 0.5ml/min by HPD-826 macroporous adsorbent resin packed column; Use distilled water wash-out 4BV then, remove impurity, use 5% ethanol elution 2BV again, elution flow rate is 0.5ml/min.
(3) 5% ethanol eluate with step (2) gained concentrate, 20Pa ,-4 ℃ of vacuum lyophilizations, Testa arachidis hypogaeae proanthocyanidin highly finished product, the purity of the proanthocyanidin of this sample is 92.05% after testing.
Embodiment 2
(1) (m: ratio v) added 40% ethanolic soln, and setting power is that 600W, temperature are 40 ℃ in the microwave extracting instrument, stirs extraction 90S in 1: 25 with the defatted peanut clothing, extraction finishes the back suction filtration, and filtrate concentrates, 20Pa,-4 ℃ of vacuum lyophilizations get the proanthocyanidin crude product
(2) the resulting crude product of step (1) is mixed with proanthocyanidin concentration be the solution of 12mg/ml with the flow velocity of 1ml/min by HPD-826 macroporous adsorbent resin packed column; Use distilled water wash-out 4BV then, remove impurity, use 5% ethanol elution 2BV again, elution flow rate is 1ml/min.
(3) 5% ethanol eluate with step (2) gained concentrate, 20Pa ,-4 ℃ of vacuum lyophilizations, Testa arachidis hypogaeae proanthocyanidin highly finished product, the purity of the proanthocyanidin of this sample is 94.25% after testing.
Embodiment 3
(1) (m: ratio v) added 40% ethanolic soln, and setting power is that 600W, temperature are 40 ℃ in the microwave extracting instrument, stirs extraction 90S in 1: 25 with the defatted peanut clothing, extraction finishes the back suction filtration, and filtrate concentrates, 20Pa,-4 ℃ of vacuum lyophilizations get the proanthocyanidin crude product
(2) the resulting crude product of step (1) is mixed with proanthocyanidin concentration be the solution of 11mg/ml with the flow velocity of 0.8ml/min by HPD-826 macroporous adsorbent resin packed column; Use distilled water wash-out 4BV then, remove impurity, use 5% ethanol elution 2BV again, elution flow rate is 0.8ml/min.
(3) 5% ethanol eluate with step (2) gained concentrate, 20Pa ,-4 ℃ of vacuum lyophilizations, Testa arachidis hypogaeae proanthocyanidin highly finished product, the purity of the proanthocyanidin of this sample is 93.0% after testing.
Embodiment 4
(1) (m: ratio v) added 40% ethanolic soln, and setting power is that 600W, temperature are 40 ℃ in the microwave extracting instrument, stirs extraction 90S in 1: 25 with the defatted peanut clothing, extraction finishes the back suction filtration, and filtrate concentrates, 20Pa,-4 ℃ of vacuum lyophilizations get the proanthocyanidin crude product
(2) the resulting crude product of step (1) is mixed with proanthocyanidin concentration be the solution of 10.5mg/ml with the flow velocity of 0.6ml/min by HPD-826 macroporous adsorbent resin packed column; Use distilled water wash-out 4BV then, remove impurity, use 5% ethanol elution 2BV again, elution flow rate is 0.6ml/min.
(3) 5% ethanol eluate with step (2) gained concentrate, 20Pa ,-4 ℃ of vacuum lyophilizations, Testa arachidis hypogaeae proanthocyanidin highly finished product, the purity of the proanthocyanidin of this sample is 91.14% after testing.
Embodiment 5
(1) (m: ratio v) added 40% ethanolic soln, and setting power is that 600W, temperature are 40 ℃ in the microwave extracting instrument, stirs extraction 90S in 1: 25 with the defatted peanut clothing, extraction finishes the back suction filtration, and filtrate concentrates, 20Pa,-4 ℃ of vacuum lyophilizations get the proanthocyanidin crude product
(2) the resulting crude product of step (1) is mixed with proanthocyanidin concentration be the solution of 12mg/ml with the flow velocity of 0.9ml/min by HPD-826 macroporous adsorbent resin packed column; Use distilled water wash-out 4BV then, remove impurity, use 5% ethanol elution 2BV again, elution flow rate is 0.7ml/min.
(3) 5% ethanol eluate with step (2) gained concentrate, 20Pa ,-4 ℃ of vacuum lyophilizations, Testa arachidis hypogaeae proanthocyanidin highly finished product, the purity of the proanthocyanidin of this sample is 92.21% after testing.
Embodiment 6
(1) (m: ratio v) added 40% ethanolic soln, and setting power is that 600W, temperature are 40 ℃ in the microwave extracting instrument, stirs extraction 90S in 1: 25 with the defatted peanut clothing, extraction finishes the back suction filtration, and filtrate concentrates, 20Pa,-4 ℃ of vacuum lyophilizations get the proanthocyanidin crude product
(2) the resulting crude product of step (1) is mixed with proanthocyanidin concentration be the solution of 10mg/ml with the flow velocity of 0.7ml/min by HPD-826 macroporous adsorbent resin packed column; Use distilled water wash-out 4BV then, remove impurity, use 5% ethanol elution 2BV again, elution flow rate is 0.9ml/min.
(3) 5% ethanol eluate with step (2) gained concentrate, 20Pa ,-4 ℃ of vacuum lyophilizations, Testa arachidis hypogaeae proanthocyanidin highly finished product, the purity of the proanthocyanidin of this sample is 94.11% after testing.
Claims (1)
1. proanthocyanidin purification process in the Testa arachidis hypogaeae may further comprise the steps:
(1) the defatted peanut clothing is joined ethanolic soln, suction filtration behind the microwave extracting, filtrate concentrates, and vacuum lyophilization gets the proanthocyanidin crude product;
(2) the resulting crude product with step (1) is mixed with proanthocyanidin solution, by HPD-826 macroporous adsorbent resin packed column; The distilled water wash-out is removed impurity then, uses ethanol elution again;
(3) ethanol eluate of gained is concentrated, lyophilize gets Testa arachidis hypogaeae proanthocyanidin highly finished product;
Defatted peanut clothing mass volume ratio described in the step (1) adds in 40% ethanolic soln at 1: 25; Described microwave extracting is that setting power is that 600W, temperature are 40 ℃, stirs extraction 90S;
Proanthocyanidin concentration described in the step (2) is 10-12mg/ml; Described flow velocity by HPD-826 macroporous adsorbent resin packed column is 0.5-1ml/min; Described distilled water wash-out 4BV; Described ethanol elution is the ethanol elution 2BV with 5%, and elution flow rate is 0.5-1ml/min;
Lyophilize condition in the step 3 is 20Pa ,-4 ℃ of vacuum lyophilizations.
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| CN2009101784157A CN101665482B (en) | 2009-09-24 | 2009-09-24 | Method for purifying proanthocyanidins in peanut coat |
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| CN2009101784157A CN101665482B (en) | 2009-09-24 | 2009-09-24 | Method for purifying proanthocyanidins in peanut coat |
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| CN101665482A CN101665482A (en) | 2010-03-10 |
| CN101665482B true CN101665482B (en) | 2011-10-05 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214448A (en) * | 2013-03-29 | 2013-07-24 | 刘治国 | Method for extracting procyanidine from peanut skin |
| CN103194089A (en) * | 2013-04-22 | 2013-07-10 | 青岛春明调味品有限公司 | Microwave-assisted method for extracting peanut coat haematochrome |
| CN104277025A (en) * | 2013-07-08 | 2015-01-14 | 山东省高唐蓝山集团总公司 | Method for extraction of proanthocyanidins from peanut red skin |
| CN103622135A (en) * | 2013-11-26 | 2014-03-12 | 山东鲁花集团有限公司 | Method for extracting polyphenols from peanut skins |
| CN104327540A (en) * | 2014-10-23 | 2015-02-04 | 青岛宝泉花生制品有限公司 | Method for extracting haematochrome or proanthocyanidin from peanut skin |
| CN105061381B (en) * | 2015-08-06 | 2017-05-10 | 山东鲁花集团有限公司 | Method for removal of aflatoxin from peanut skin |
| CN105418572B (en) * | 2015-11-06 | 2019-02-12 | 大兴安岭林格贝寒带生物科技股份有限公司 | It is extracted using microwave counter current, the method for macroporous absorbent resin adsorption and purification whortle anthocyanidin |
| CN108720009A (en) * | 2017-04-21 | 2018-11-02 | 大江生医股份有限公司 | Using peanut membrane extraction object in the application for preparing the composition for promoting the performance of PTPRD genes |
| CN109620857B (en) * | 2019-01-16 | 2021-05-25 | 浙江大学 | Peanut coat active component and application thereof in preparation of anti-obesity and anti-diabetic drugs |
| CN111454242B (en) * | 2020-05-14 | 2021-12-14 | 湖南华诚生物资源股份有限公司 | Method for separating multiple active ingredients from peanut coat |
-
2009
- 2009-09-24 CN CN2009101784157A patent/CN101665482B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
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| 刘大川 等.花生红衣中白藜芦醇和原花色素的提取分离工艺.《中国粮油学会油脂专业分会第十四届学术年会论文选集》.2005,第92-97页. * |
| 张红梅 等.花生衣红色素微波提取工艺研究.《安徽农业科学》.2005,第33卷(第2期),第297-299页. * |
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Owner name: QINGDAO BAOQUAN PEANUTS PRODUCTS CO., LTD. Free format text: FORMER OWNER: SHANDONG PEANUT INST. Effective date: 20120504 |
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Free format text: CORRECT: ADDRESS; FROM: 266100 QINGDAO, SHANDONG PROVINCE TO: 266000 QINGDAO, SHANDONG PROVINCE |
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Effective date of registration: 20120504 Address after: 266000, No. 12, water road, Laixi industry and Trade Development Zone, Shandong, Qingdao Patentee after: Qingdao Baoquan Peanuts Products Co., Ltd. Address before: 266100 Peanut Research Institute, No. 126 floating mountain road, Licang District, Shandong, Qingdao, Shandong Patentee before: Shandong Peanut Inst. |
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