CN102659872A - Preparation method of high purity scutellarin - Google Patents
Preparation method of high purity scutellarin Download PDFInfo
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- CN102659872A CN102659872A CN2012101032392A CN201210103239A CN102659872A CN 102659872 A CN102659872 A CN 102659872A CN 2012101032392 A CN2012101032392 A CN 2012101032392A CN 201210103239 A CN201210103239 A CN 201210103239A CN 102659872 A CN102659872 A CN 102659872A
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Abstract
The invention which discloses a preparation method of high purity scutellarin belongs to the chemical field of natural products. The preparation method adopts a homogeneous-grain polymethacrylate series resin as a chromatography filler and deionized water as a mobile phase to purify the scutellarin, so the purity of final products is greater than 99%. The resin has the advantages of high mechanical strength, good separation effect and the like when it is used as the column chromatography filler, and the deionized water which is used as the mobile phase is more economic and environmentally-friendly than organic solvents used by routine column chromatography.
Description
Technical field
The invention belongs to the natural product chemistry field, be specifically related to a kind of preparation method of high-purity vegetable bulk drug lamp-dish flower acetic.
Background technology
Herba Erigerontis is the dry herb of feverfew Erigeron breviscapus (Vant.) Hand.-Mazz., has another name called Herba Erigerontis, is distributed in ground such as Yunnan, Sichuan, Guizhou, Guangxi, Hunan.The Herba Erigerontis prime system is isolated flavonoids effective constituent from Herba Erigerontis; Wherein be mainly lamp-dish flower acetic (having another name called scutellarin, scutellarin), by name 4 ' 5, the 6-trihydroxyflavone-7-O-glucuronide of chemistry; The Breviscarpine bulk drug of buying from market is at present analyzed through HPLC; Lamp-dish flower acetic content is widely used in the treatment cardiovascular and cerebrovascular diseases, determined curative effect clinically about 90%.But its injection liquid poor stability, the storage time is short, and phenomenons generations such as caloric response, skin pruritus, fash are arranged when individual patient is with the back clinically, and the appearance of these phenomenons is mainly due to due to some decons that do not eliminate in the bulk drug.
Breviscarpine bulk drug process for purification not can solve always for many years, therefore is necessary to study the technological problems that new preparation method solves high-purity scutellarin.About the technological problems of high-purity scutellarin, Chinese patent 200510010723 proposes a kind of method for preparing high-purity scutellarin, and Breviscarpine is dissolved in alkali lye; Add a large amount of organic solvents again and precipitate, go out deposition with adding acid out after the throw out dissolving, filtration, drying obtain lamp-dish flower acetic; Its purity can reach more than 99%, but this method need be used soda acid and a large amount of organic solvents, brings very big pollution to environment; And yield is not high, and difficulty is amplified in industriallization.
Summary of the invention
For addressing the above problem; Disclosure purpose is to provide a kind of reversed phase chromatography filler; This filler is all grain microballoons of cross-linked poly-methyl methacrylate ester, and it not only is beneficial to the aqueous solution as the column chromatography bed of packings and reaches high purity and high yield as moving phase separation and purification lamp-dish flower acetic
For achieving the above object, technical scheme of the present invention is to adopt Suzhou to receive the monodisperse cross-linked Rohm tech inc microballoon resin of Uni PMM series that mikrobe scientific & technical corporation produces as chromatographic stuffing.Its process comprises becomes stationary phase with this resin as the filler chromatographic column of packing into.Flow through this chromatographic column containing to remain to be separated or analyze the Herba Erigerontis bullion that contains lamp-dish flower acetic, and then treating on the Uni PMM series stationary phase separated or the lamp-dish flower acetic analyzed elutes being adsorbed on,
Concrete technical scheme is following:
A kind of preparation method of high-purity scutellarin, carry out according to following step:
(1) chromatographic column balance: after the dress post is accomplished, with ultrapure water with the flow velocity balance chromatographic column of 1 ~ 4 times of column volume per hour;
(2) specimen preparation: take by weighing the lamp-dish flower acetic bullion and join boiling water, stir, slowly drip arginine solution, control pH be between 6.0 ~ 9.0, make sample dissolution complete, behind the constant volume while hot with subsequent use behind the filter paper filtering;
(3) go up appearance: the sample liquid that step (2) is obtained, cross resin column with the flow velocity even flow of 1 ~ 4 times of column volume per hour
, the weight (g) of used resin volume (L) and lamp-dish flower acetic bullion is than being 100:1 ~ 100:3;
(4) wash-out: the end of the sample continued is used the deionized water wash-out, with the speed wash-out of 1 ~ 4 times of column volume per hour, is in charge of collection according to the UV detection case then, detects purity; The collection liquid that purity is qualified merges, and obtains collecting liquid, and concentrating under reduced pressure obtains medicinal extract;
(5) drying: the lyophilize of gained medicinal extract is obtained lamp-dish flower acetic, and its purity is greater than 99%.
Wherein be preferably the flow velocity balance chromatographic column of 2 times of column volume flow velocitys hourly in the step (1);
Wherein preferred pH value is 8.0 in the step (2),
The lamp-dish flower acetic bullion purity 80 ~ 92% described in the step (2) wherein,
Wherein the concentration of the lamp-dish flower acetic bullion described in the step (2) is 10 ~ 100mg/ml,
Wherein be preferably 2 times of column volume flow velocity even flow hourly in the step (2) and cross resin column;
Wherein the resin described in the step (3) is all grain microballoon resins of Uni PMM series cross-linked poly-methyl methacrylate ester;
Wherein be preferably 2 times of column volume speed wash-outs hourly in the step (4);
Adopt the beneficial effect of present technique scheme to be: the Uni PMM series plastics that Suzhou Nano-Micro Bio-technology Co., Ltd. produces can use deionized water to do moving phase sample is separated during as the column chromatography filler, does not need organic solvent, and has fabulous selectivity; Single job just can obtain the lamp-dish flower acetic of 99% above purity, compares with existing technology, has simple to operate; Efficient is high; Favorable reproducibility, easy for industrialized production, advantage such as environmental pollution is little.
Embodiment
Illustrate in greater detail the present invention through embodiment below.But scope of the present invention is not limited to these embodiment.
Embodiment 1
Breviscarpine sample solution preparation: the 12g l-arginine is dissolved in confession accent pH use in the 50mL boiling water.Take by weighing 30g Breviscarpine bullion (purity 90.1%), add 400mL boiling water, stir, slowly drip arginine solution, control pH is 8.0, makes sample dissolution complete, is settled to 600mL, and is subsequent use behind the membrane filtration while hot.
The purifying of lamp-dish flower acetic: adopt 49 * 460 mm glass columns; Uni PMM40-500 resin (Suzhou Nano-Micro Bio-technology Co., Ltd.) is a chromatographic stuffing; Dress column volume 867 mL, with 3 times of column volume ultrapure waters with the flow velocity balance chromatographic column of 1 times of column volume per hour.Get Breviscarpine sample solution 520 mL of preparation; Cross appearance on the resin column with the flow velocity even flow of 1 times of column volume per hour, the end of the sample continued is used the deionized water wash-out, then with the speed wash-out of 1 times of column volume per hour; Be in charge of collection according to the UV detection case, detect purity.The collection liquid that purity is qualified merges, and obtains collecting liquid 300mL altogether, and it is 99.18% that HPLC detects purity, and this test scutellarin recovery is 67.9%.
Embodiment 2
Breviscarpine sample solution preparation: the 6g l-arginine is dissolved in confession accent pH use in the 20mL boiling water.Take by weighing 15g Breviscarpine bullion (purity 80%), add 600mL boiling water, stir, slowly drip arginine solution, control pH is 8.0, makes sample dissolution complete, is settled to 750mL, and is subsequent use behind the membrane filtration while hot.
The purifying of lamp-dish flower acetic: adopt 49 * 460 mm glass columns; The Uni PMM40-500 resin that Suzhou Nano-Micro Bio-technology Co., Ltd. produces is a chromatographic stuffing; Dress column volume 867mL, with the ultrapure water of 3 times of column volumes with the flow velocity balance chromatographic column of 4 times of column volumes per hour.Get Breviscarpine sample solution 433 mL by preparation; Cross appearance on the resin column with the flow velocity even flow of 4 times of column volumes per hour, the end of the sample continued is used the deionized water wash-out, then with 4 times of column volume speed wash-outs hourly; Be in charge of collection according to the UV detection case, detect purity.The collection liquid that purity is qualified merges, and obtains collecting liquid 285mL altogether, adds Glacial acetic acid min. 99.5, and making and collecting liquid pH is 2-3; Quiescent setting filters, and filter cake is dried down at 60 ℃; Obtain scutellarin dry product 5.7g, it is 99.51% that HPLC detects purity, and this test scutellarin recovery is 70%.
Claims (6)
1. the preparation method of a high-purity scutellarin is characterized in that carrying out according to following step:
(1) chromatographic column balance: after the dress post is accomplished, with ultrapure water with 1 ~ 4 times of column volume flow velocity balance hourly chromatographic column;
(2) specimen preparation: take by weighing the lamp-dish flower acetic bullion and join boiling water, stir, slowly drip arginine solution, control pH be between 6.0 ~ 9.0, make sample dissolution complete, behind the constant volume while hot with subsequent use behind the filter paper filtering;
(3) go up appearance:, cross resin column with 1 ~ 4 times of column volume flow velocity even flow hourly with the sample liquid that step (2) obtains
, the weight (g) of used resin volume (L) and sample is than being 100:1 ~ 100:3;
(4) wash-out: the end of the sample continued is used the deionized water wash-out, with 1 ~ 4 times of column volume speed wash-out hourly, is in charge of collection according to the UV detection case then, detects purity; The collection liquid that purity is qualified merges, and obtains collecting liquid, and concentrating under reduced pressure obtains medicinal extract;
(5) drying: the lyophilize of gained medicinal extract is obtained lamp-dish flower acetic, and its purity is greater than 99%.
2. the preparation method of a kind of high-purity scutellarin according to claim 1 is characterized in that being preferably in the step (1) wherein the flow velocity balance chromatographic column of 2 times of column volume flow velocitys hourly.
3. the preparation method of a kind of high-purity scutellarin according to claim 1 is characterized in that wherein the middle pH value of step (2) is 8.0.
4. the preparation method of a kind of high-purity scutellarin according to claim 1; It is characterized in that the wherein lamp-dish flower acetic bullion purity 80 ~ 92% described in the step (2); Wherein the concentration of the lamp-dish flower acetic bullion described in the step (2) is 10 ~ 100mg/ml, wherein crosses resin column with 2 times of column volume flow velocity even flow hourly in the step (2).
5. the preparation method of a kind of high-purity scutellarin according to claim 1 is characterized in that wherein the resin described in the step (3) is all grain microballoon resins of Uni PMM series cross-linked poly-methyl methacrylate ester.
6. the preparation method of a kind of high-purity scutellarin according to claim 1 is characterized in that wherein in the step (4) with 2 times of column volume speed wash-outs hourly.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110478361A (en) * | 2018-05-14 | 2019-11-22 | 昆明龙津药业股份有限公司 | A kind of highly-safe lamp-dish flower acetic pharmaceutical composition and preparation method thereof |
| CN113788870A (en) * | 2021-11-01 | 2021-12-14 | 湖南恒生制药股份有限公司 | High-purity breviscapine raw material medicine and preparation process thereof |
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| US20030054050A1 (en) * | 2001-09-17 | 2003-03-20 | Wolfson Philip E. | Standardized extracts of scutellaria lateriflora |
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| CN101735291A (en) * | 2009-12-22 | 2010-06-16 | 樊献俄 | Process for preparing high-purity scutellarin bulk drug |
| CN101747395A (en) * | 2009-12-25 | 2010-06-23 | 中国医药集团总公司四川抗菌素工业研究所 | Method for preparing high-purity scutellarin |
| CN102276699A (en) * | 2011-06-19 | 2011-12-14 | 苏州纳微生物科技有限公司 | Application of monodisperse polymethacrylate microballoons in column chromatography purification of vancomycin |
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2012
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| US20030054050A1 (en) * | 2001-09-17 | 2003-03-20 | Wolfson Philip E. | Standardized extracts of scutellaria lateriflora |
| CN101376668A (en) * | 2007-08-31 | 2009-03-04 | 樊献俄 | Preparation technique of high-purity scutellarin raw medicine |
| CN101683332A (en) * | 2008-09-26 | 2010-03-31 | 樊献俄 | high purity scutellarin salt bulk drug and preparation method thereof |
| CN101580527A (en) * | 2009-04-29 | 2009-11-18 | 南开大学 | Adsorption resin method separation technology of scutellarin in fleabane flower extract |
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| CN101747395A (en) * | 2009-12-25 | 2010-06-23 | 中国医药集团总公司四川抗菌素工业研究所 | Method for preparing high-purity scutellarin |
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|---|---|---|---|---|
| CN110478361A (en) * | 2018-05-14 | 2019-11-22 | 昆明龙津药业股份有限公司 | A kind of highly-safe lamp-dish flower acetic pharmaceutical composition and preparation method thereof |
| CN113788870A (en) * | 2021-11-01 | 2021-12-14 | 湖南恒生制药股份有限公司 | High-purity breviscapine raw material medicine and preparation process thereof |
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| CN102659872B (en) | 2014-11-19 |
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Address after: Xinghu Street Industrial Park of Suzhou city in Jiangsu province 215125 No. 218 BioBAY building C1 Applicant after: SUZHOU NANOMICRO TECHNOLOGY COMPANY LIMITED Address before: Xinghu Street Industrial Park of Suzhou city in Jiangsu province 215125 No. 218 BioBAY building C1 Applicant before: Suzhou Nano-Micro Bio-technology Co., Ltd. |
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Address after: 215125 2 Industrial Park, Suzhou, Jiangsu. Patentee after: Suzhou Nanwei Polytron Technologies Inc Address before: 215125 C1 Biological Park, No. 218 Xing Hu Street, Suzhou Industrial Park, Jiangsu. Patentee before: SUZHOU NANOMICRO TECHNOLOGY COMPANY LIMITED |