CN100545157C - The method of simulated moving bed chromatography method separating and purifying flavone from the reed wormwood artemisia - Google Patents
The method of simulated moving bed chromatography method separating and purifying flavone from the reed wormwood artemisia Download PDFInfo
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- CN100545157C CN100545157C CNB200710022903XA CN200710022903A CN100545157C CN 100545157 C CN100545157 C CN 100545157C CN B200710022903X A CNB200710022903X A CN B200710022903XA CN 200710022903 A CN200710022903 A CN 200710022903A CN 100545157 C CN100545157 C CN 100545157C
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Abstract
The invention discloses the method for simulated moving bed chromatography method separating and purifying flavone from the reed wormwood artemisia, the reed wormwood artemisia that at first takes by weighing the 0.7-1.0kg drying and crushing carries out the water-bath refluxing extraction in 80% ethanol that 85-95 ℃ of constant temperature adds 10-15kg down, filtration, merging filtrate; Extract twice repeatedly, the washing residue merges washings, and with petroleum ether degreasing, concentrating under reduced pressure gets reed wormwood artemisia flavone gruff bring up substance; Reed wormwood artemisia flavone gruff bring up substance is made sample introduction liquid to simulation moving-bed separation and purification; Dissolve with methanol reed wormwood artemisia flavone gruff bring up substance, 0.45 μ m organic system membrane filtration gets the simulation moving-bed feeding liquid of concentration 100-300mg/ml; Elutriant is the mixture of methyl alcohol and water, and the volume ratio of methyl alcohol and water is 40: 60; With simulation moving-bed extraction liquid be concentrated into saturated after, be cooled to subzero 4-10 ℃ gradually, crystallization 5-6 hour, filter, the washing crystal, crystallization twice, vacuum drying gets the pure product of reed wormwood artemisia flavones.The inventive method has improved the automatization level of producing, and working efficiency, production environment are improved greatly.
Description
Technical field
The present invention relates to the separating and purifying method of natural drug, be specifically related to the method for a kind of simulated moving bed chromatography method separating and purifying flavone from the reed wormwood artemisia.
Background technology
The reed wormwood artemisia has another name called lamb's-quarters wormwood artemisia, water wormwood artemisia, beach wormwood wormwood artemisia etc., for all there is distribution the perennial perennial root herbaceous plant of composite family, all parts of the country, is a flavour potherb.The pharmaceutical use of reed wormwood artemisia is just on the books as far back as Ancient Times in China, and medicinal have effects such as heat-clearing, curing rheumatism, appetizing, contains compositions such as volatile oil, flavones, and the acute and chronic infectious hepatitis of among the people also useful treatment, effect are fine.The method of extracting at present flavones in the reed wormwood artemisia is to soak, filter, extract and obtain thick product, but will reach medicinal requirements must be further purified, and purification process commonly used at present is with the column chromatography of neutral alumina as filler.Column chromatography is refining means commonly used in medicine and the foodstuffs industry, and the simple cost of equipment is low, but the isolating efficient of this method low, yield poorly, the cost height, be not suitable for separating for the complicated material of composition.
Since the seventies, American UOP company has developed the chromatographic technique of simulation moving-bed (SMB) principle, this technology is not moving after making the absorbent particles filling, by the method that raw material is imported and exported and product liquid flow inlet and outlet constantly switches, the formation absorbent particles flows relative to countercurrent movement with liquid simulates moving of stationary phase.Utilize simulated moving bed chromatography separate drug technology to obtain development fast in recent years.Some patent documentations of the U.S. have been reported simulated moving bed chromatography separating chiral medicine such as optical isomer, racemize material and enantiomorph, and the separation of petroleum chemicals.But, for using simulated moving bed chromatography that the method that flavones in the reed wormwood artemisia separates purification is not seen open report yet.
Summary of the invention
The objective of the invention is to: the method for a kind of simulated moving bed chromatography method separating and purifying flavone from the reed wormwood artemisia is provided, the technology continuous production, the purity and the yield of raising product, reduction manufactures a finished product.
The realization of purpose of the present invention may further comprise the steps:
A, the reed wormwood artemisia that takes by weighing the 0.7-1kg drying and crushing carry out the water-bath refluxing extraction in 80% ethanol that 85-95 ℃ of constant temperature adds 10-15kg down, filter, merging filtrate;
B, extract twice repeatedly, the washing residue merges washings, and with petroleum ether degreasing, concentrating under reduced pressure, reed wormwood artemisia flavone gruff bring up substance;
C, reed wormwood artemisia flavone gruff bring up substance is made sample introduction liquid to simulation moving-bed separation and purification; Dissolve with methanol reed wormwood artemisia flavone gruff bring up substance, 0.45 μ m organic system membrane filtration gets the simulation moving-bed feeding liquid of concentration 100-300mg/ml; Elutriant is the mixture of methyl alcohol and water, and the volume ratio of methyl alcohol and water is 40: 60;
D, with simulation moving-bed extraction liquid be concentrated into saturated after, be cooled to subzero 4-10 ℃ gradually, crystallization 5-6 hour, filter, the washing crystal, crystallization twice, vacuum drying gets the pure product of reed wormwood artemisia flavones.
Simulated moving bed chromatography in the inventive method (SMBC) separation system is connected to form by wash-out pump, sampling pump, extraction pump, chromatographic column, magnetic valve, signal picker, central controller and computer, wash-out pumping capacity 10-1000ml/min, pressure 2-10Mpa; Sampling pump flow 1-50ml/min, pressure 2-10Mpa; Extraction pumping capacity 10-500ml/min, pressure 2-10Mpa; Working temperature 15-25 ℃; Chromatographic column filler is an octadecylsilane key silica gel, filler granularity 10-50 μ m.
Simulation moving-bed in the inventive method props up chromatographic column by 4-16 to be formed, and switches through magnetic valve and changes opening for feed, discharge port position, and chromatographic column is divided 4 zones, and prop up chromatographic column by 1-4 and is composed in series in every district; The sample introduction flow velocity is 1-50ml/min, and eluent flow rate is 10-1000ml/min, and the extraction liquid flow velocity is 10-500ml/min, and the raffinate flow velocity is 10-300ml/min; Valve switching time is 4-30min.
The inventive method compares with the column chromatography that present essence is carried reed wormwood artemisia flavones, the yield height, produce every kilogram of reed wormwood artemisia flavones product and can save solvent 16050L, save filler 680.6Kg, product purity reaches more than 96%, and simulation moving-bed is serialization production, column chromatography method is intermittently, the introducing of simulated moving bed chromatography has improved the automatization level of producing, and working efficiency, production environment are improved greatly, have realized cleaner production.
Embodiment
Example 1: according to simulated moving bed chromatography method from the reed wormwood artemisia separating and purifying flavone of following steps in Hanbon Sci. ﹠ Tech. Co., Ltd.:
A, the reed wormwood artemisia that takes by weighing the 0.7kg drying and crushing carry out the water-bath refluxing extraction in 80% ethanol that 85 ℃ of constant temperature add 10kg down, filter, merging filtrate;
B, extract twice repeatedly, the washing residue merges washings, and with petroleum ether degreasing, concentrating under reduced pressure, reed wormwood artemisia flavone gruff bring up substance;
C, reed wormwood artemisia flavone gruff bring up substance is made sample introduction liquid to simulation moving-bed separation and purification; Dissolve with methanol reed wormwood artemisia flavone gruff bring up substance, 0.45 μ m organic system membrane filtration gets the simulation moving-bed feeding liquid of concentration 100mg/ml; Elutriant is the mixture of methyl alcohol and water, and the volume ratio of methyl alcohol and water is 40: 60;
D, with simulation moving-bed extraction liquid be concentrated into saturated after, be cooled to subzero 4 ℃ gradually, crystallization 5 hours is filtered, the washing crystal, crystallization twice, vacuum drying gets the pure product of reed wormwood artemisia flavones.
Simulated moving bed chromatography in the inventive method (SMBC) separation system is connected to form by wash-out pump, sampling pump, extraction pump, chromatographic column, magnetic valve, signal picker, central controller and computer, wash-out pumping capacity 10ml/min, pressure 2Mpa; Sampling pump flow 1ml/min, pressure 2Mpa extraction pumping capacity 10ml/min, pressure 2Mpa; 15 ℃ of moving-bed working temperatures; Chromatographic column filler is an octadecylsilane key silica gel, filler granularity 10 μ m.
Simulation moving-bed in the inventive method is made up of 4 chromatographic columns, switches through magnetic valve and changes opening for feed, discharge port position, and 4 chromatographic columns are divided 4 zones; The sample introduction flow velocity is 1ml/min, and eluent flow rate is 10ml/min, and the extraction liquid flow velocity is 10ml/min, and the raffinate flow velocity is 10ml/min; Valve switching time is 4min.
Finished product HPLC method detects: PerkinElmer Series 200 highly effective liquid phase chromatographic systems, diode-array detector, Hedera ODS-3 4.6mm * 250mm analytical column, packing material size 5 μ m, mobile phase methanol/0.2% phosphate aqueous solution (v/v)=80/20, flow velocity 1ml/mim, sample introduction concentration 0.500mg/ml, sample size 20 μ l, 25 ℃ of detected temperatures are used external standard method finished product reed wormwood artemisia flavones content 96%.
Example 2:
According to simulated moving bed chromatography method from the reed wormwood artemisia separating and purifying flavone of following steps in Hanbon Sci. ﹠ Tech. Co., Ltd.:
A, the reed wormwood artemisia that takes by weighing the 0.9kg drying and crushing carry out the water-bath refluxing extraction in 80% ethanol that 90 ℃ of constant temperature add 12kg down, filter, merging filtrate;
B, extract twice repeatedly, the washing residue merges washings, and with petroleum ether degreasing, concentrating under reduced pressure, reed wormwood artemisia flavone gruff bring up substance;
C, reed wormwood artemisia flavone gruff bring up substance is made sample introduction liquid to simulation moving-bed separation and purification; Dissolve with methanol reed wormwood artemisia flavone gruff bring up substance, 0.45 μ m organic system membrane filtration gets the simulation moving-bed feeding liquid of concentration 200mg/ml; Elutriant is the mixture of methyl alcohol and water, and the volume ratio of methyl alcohol and water is 40: 60;
D, with simulation moving-bed extraction liquid be concentrated into saturated after, be cooled to subzero 7 ℃ gradually, crystallization 5.5 hours is filtered, the washing crystal, crystallization twice, vacuum drying gets the pure product of reed wormwood artemisia flavones.
Simulated moving bed chromatography in the inventive method (SMBC) separation system is connected to form by wash-out pump, sampling pump, extraction pump, chromatographic column, magnetic valve, signal picker, central controller and computer, wash-out pumping capacity 500ml/min, pressure 5Mpa; Sampling pump flow 30ml/min, pressure 5Mpa; Extraction pumping capacity 250ml/min, pressure 5Mpa; 20 ℃ of moving-bed working temperatures; Chromatographic column filler is an octadecylsilane key silica gel, filler granularity 30 μ m.
Simulation moving-bed in the inventive method is made up of 12 chromatographic columns, switches through magnetic valve and changes opening for feed, discharge port position, and 12 chromatographic columns are divided 4 zones, and every district is composed in series by 3 identical chromatographic columns; The sample introduction flow velocity is 30ml/min, and eluent flow rate is 500ml/min, and the extraction liquid flow velocity is 250ml/min, and the raffinate flow velocity is 250ml/min; Valve switching time is 18min.
Finished product HPLC method detects: PerkinElmer Series 200 highly effective liquid phase chromatographic systems, diode-array detector, Hedera ODS-34.6mm * 250mm analytical column, packing material size 5 μ m, mobile phase methanol/0.2% phosphate aqueous solution (v/v)=80/20, flow velocity 1ml/mim, sample introduction concentration 0.500mg/ml, sample size 20 μ l, 25 ℃ of detected temperatures are used external standard method finished product reed wormwood artemisia flavones content 97%.
Example 3:
According to simulated moving bed chromatography method from the reed wormwood artemisia separating and purifying flavone of following steps in Hanbon Sci. ﹠ Tech. Co., Ltd.:
A, the reed wormwood artemisia that takes by weighing the 1kg drying and crushing carry out the water-bath refluxing extraction in 80% ethanol that 95 ℃ of constant temperature add 15kg down, filter, merging filtrate;
B, extract twice repeatedly, the washing residue merges washings, and with petroleum ether degreasing, concentrating under reduced pressure, reed wormwood artemisia flavone gruff bring up substance;
C, reed wormwood artemisia flavone gruff bring up substance is made sample introduction liquid to simulation moving-bed separation and purification; Dissolve with methanol reed wormwood artemisia flavone gruff bring up substance, 0.45 μ m organic system membrane filtration gets the simulation moving-bed feeding liquid of concentration 100-300mg/ml; Elutriant is the mixture of methyl alcohol and water, and the volume ratio of methyl alcohol and water is 40: 60;
D, with simulation moving-bed extracting solution be concentrated into saturated after, be cooled to subzero 10 ℃ gradually, crystallization 6 hours is filtered, the washing crystal, crystallization twice, vacuum drying gets the pure product of reed wormwood artemisia flavones.
Simulated moving bed chromatography in the inventive method (SMBC) separation system is connected to form by wash-out pump, sampling pump, extraction pump, chromatographic column, magnetic valve, signal picker, central controller and computer, wash-out pumping capacity 1000ml/min, pressure 10Mpa; Sampling pump flow 50ml/min, pressure 10Mpa; Extraction pumping capacity 500ml/min, pressure 10Mpa; 25 ℃ of working temperatures; Chromatographic column filler is an octadecylsilane key silica gel, filler granularity 50 μ m.
Simulation moving-bed in the inventive method is made up of 16 chromatographic columns, switches through magnetic valve and changes opening for feed, discharge port position, and 16 chromatographic columns are divided 4 zones, and prop up identical chromatographic column by 1-4 and is composed in series in every district; The sample introduction flow velocity is 50ml/min, and eluent flow rate is 1000ml/min, and the extraction liquid flow velocity is 500ml/min, and the raffinate flow velocity is 300ml/min; Valve switching time is 30min.
Finished product HPLC method detects: PerkinElmer Series 200 highly effective liquid phase chromatographic systems, diode-array detector, Hedera ODS-34.6mm * 250mm analytical column, packing material size 5 μ m, mobile phase methanol/0.2% phosphate aqueous solution (v/v)=80/20, flow velocity 1ml/mim, sample introduction concentration 0.500mg/ml, sample size 20 μ l, 25 ℃ of detected temperatures are used external standard method finished product reed wormwood artemisia flavones content 98%.
Claims (1)
1. the method for simulated moving bed chromatography method separating and purifying flavone from the reed wormwood artemisia, concrete steps:
A, the reed wormwood artemisia that takes by weighing the 0.7kg-1kg drying and crushing carry out the water-bath refluxing extraction in 80% ethanol that 85-95 ℃ of constant temperature adds 10-15kg down, filter, merging filtrate;
B, extract twice repeatedly, the washing residue merges washings, and with petroleum ether degreasing, concentrating under reduced pressure, reed wormwood artemisia flavone gruff bring up substance;
C, reed wormwood artemisia flavone gruff bring up substance is made sample introduction liquid to simulation moving-bed separation and purification; Dissolve with methanol reed wormwood artemisia flavone gruff bring up substance, 0.45 μ m organic system membrane filtration gets the simulation moving-bed feeding liquid of concentration 100-300mg/ml; Elutriant is the mixture of methyl alcohol and water, and the volume ratio of methyl alcohol and water is 40: 60;
D, with simulation moving-bed extraction liquid be concentrated into saturated after, be cooled to subzero 4-10 ℃ gradually, crystallization 5-6 hour, filter, the washing crystal, crystallization twice, vacuum drying gets the pure product of reed wormwood artemisia flavones.
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| CN102688266A (en) * | 2012-06-15 | 2012-09-26 | 通化师范学院 | Method for separating and purifying Chinese actinidia root flavone by simulated moving bed chromatography |
| CN103508991A (en) * | 2012-06-27 | 2014-01-15 | 江苏汉邦科技有限公司 | Method for separating and purifying quercetin by virtue of simulated moving bed chromatography |
| CN106350545B (en) * | 2016-10-20 | 2019-07-30 | 南京工业大学 | A kind of method that reed wormwood artemisia stalk full constituent utilizes |
| CN108239059B (en) * | 2018-01-29 | 2020-01-03 | 扬州工业职业技术学院 | Method for separating flavonoid compounds from ginkgo leaf extract by using simulated moving bed |
| CN113485494B (en) * | 2021-07-01 | 2022-04-15 | 安徽普冈电子材料有限公司 | Mixed acid process system for anode aluminum foil production |
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Non-Patent Citations (6)
| Title |
|---|
| 模拟移动床色谱技术及其应用. 蔡宇杰等.色谱，第22卷第2期. 2004 |
| 模拟移动床色谱技术及其应用. 蔡宇杰等.色谱，第22卷第2期. 2004 * |
| 纯化银杏总内酯的新工艺. 高丽娟等.化学世界，第12期. 2005 |
| 纯化银杏总内酯的新工艺. 高丽娟等.化学世界，第12期. 2005 * |
| 芦蒿中黄酮类化合物提取工艺研究. 吕丽爽等.食品工业科技，第23卷第9期. 2002 |
| 芦蒿中黄酮类化合物提取工艺研究. 吕丽爽等.食品工业科技，第23卷第9期. 2002 * |
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Address after: 223005 No. 1-9, Jixian Road, Huaian economic and Technological Development Zone, Jiangsu Patentee after: JIANGSU HANBON SCIENCE & TECHNOLOGY Co.,Ltd. Address before: 223001, 116 Health East Road, Qinghe District, Jiangsu, Huaian Patentee before: JIANGSU HANBON SCIENCE & TECHNOLOGY Co.,Ltd. |
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Address after: 223005 no.1-9 Jixian Road, Huai'an Economic and Technological Development Zone, Jiangsu Province Patentee after: Jiangsu Hanbang Technology Co.,Ltd. Address before: 223005 no.1-9 Jixian Road, Huai'an Economic and Technological Development Zone, Jiangsu Province Patentee before: JIANGSU HANBON SCIENCE & TECHNOLOGY Co.,Ltd. |