CN102659872B - Preparation method of high purity scutellarin - Google Patents
Preparation method of high purity scutellarin Download PDFInfo
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- CN102659872B CN102659872B CN201210103239.2A CN201210103239A CN102659872B CN 102659872 B CN102659872 B CN 102659872B CN 201210103239 A CN201210103239 A CN 201210103239A CN 102659872 B CN102659872 B CN 102659872B
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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 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 the ground such as Yunnan, Sichuan, Guizhou, Guangxi, Hunan.Herba Erigerontis prime system is isolated flavonoids effective constituent from Herba Erigerontis, wherein be mainly lamp-dish flower acetic and (have another name called scutellarin, scutellarin), chemistry is by name 4 ' 5,6-trihydroxyflavone-7-O-glucuronide, the breviscapine active pharmaceutical ingredient of buying from the market is at present analyzed through HPLC, lamp-dish flower acetic content, in 90% left and right, is widely used in treatment cardiovascular and cerebrovascular diseases, determined curative effect clinically.But its injection liquid poor stability, the storage time is short, and indivedual patients have the phenomenon generations such as caloric response, skin pruritus, fash when rear clinically, and the appearance of these phenomenons is mainly due to due to some not removed impurity in bulk drug.
Breviscapine active pharmaceutical ingredient process for purification not can solve always for many years, is therefore necessary to study new preparation method and solves the technological problems of high-purity scutellarin.About the technological problems of high-purity scutellarin, Chinese patent 200510010723 proposes a kind of method of preparing high-purity scutellarin, Breviscarpine is dissolved in alkali lye, then add a large amount of organic solvents to precipitate, after throw out is dissolved, acid adding is separated out precipitation, filtration, the dry lamp-dish flower acetic that obtains, its purity can reach more than 99%, but the method need to be used soda acid and a large amount of organic solvent, brings very large pollution to environment, and yield is not high, difficulty is amplified in industrialization.
Summary of the invention
For addressing the above problem, disclosure object is to provide a kind of reversed phase chromatography filler, this filler is all grain microballoons of CARBOPOL, and it is not only beneficial to the aqueous solution and reaches high purity and high yield as moving phase separation and purification lamp-dish flower acetic as column chromatography bed of packings
For achieving the above object, technical scheme of the present invention is to adopt Suzhou to receive the monodisperse cross-linked polymethacrylate microballoon resin of Uni PMM series that microorganism scientific & technical corporation produces as chromatographic stuffing.Its process comprises that packing this resin into chromatographic column as filler becomes stationary phase.Containing to be separated or analyzing containing the Herba Erigerontis crude product of lamp-dish flower acetic and flow through this chromatographic column, and then the lamp-dish flower acetic to be separated or that analyze being adsorbed on Uni PMM Series Stationary Phases is eluted,
Concrete technical scheme is as follows:
A preparation method for high-purity scutellarin, carries out according to following step:
(1) chromatographic column balance: after dress post completes, the flow velocity balance chromatographic column with ultrapure water with 1 ~ 4 times of column volume per hour;
(2) sample preparation: take lamp-dish flower acetic crude product and join boiling water, stir, slowly drip arginine solution, control pH be between 6.0 ~ 9.0, make sample dissolution complete, after constant volume while hot with for subsequent use after filter paper filtering;
(3) loading: the sample liquid that step (2) is obtained, cross resin column with the flow velocity Continuous Flow of 1 ~ 4 times of column volume per hour
, the weight (g) of resin volume used (L) and lamp-dish flower acetic crude product is than being 100:1 ~ 100:3;
(4) wash-out: continue to spend ionized water wash-out after end of the sample, then, with the speed wash-out of 1 ~ 4 times of column volume per hour, be in charge of collection according to UV detection case, detect purity; Collection liquid qualified purity is merged, obtain collecting liquid, concentrating under reduced pressure obtains medicinal extract;
(5) dry: the lyophilize of gained medicinal extract is obtained to lamp-dish flower acetic, and its purity is greater than 99%.
Wherein in step (1), be preferably the flow velocity balance chromatographic column of 2 times of column volume flow velocitys hourly;
Wherein in step (2), preferably pH value is 8.0,
The wherein lamp-dish flower acetic crude product purity 80 ~ 92% described in step (2),
Wherein the concentration of the lamp-dish flower acetic crude product described in step (2) is 10 ~ 100mg/ml,
Wherein in step (2), be preferably 2 times of column volume flow velocity Continuous Flow hourly and cross resin column;
Wherein the resin described in step (3) is all grain microballoon resins of Uni PMM series CARBOPOL;
Wherein in step (4), be preferably 2 times of column volume speed wash-outs hourly;
Adopt the beneficial effect of the technical program 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 column chromatography filler, without the need for machine solvent, and there is fabulous selectivity, single job just can obtain the lamp-dish flower acetic of 99% above purity, compared with the prior art, has simple to operate, efficiency is high, favorable reproducibility, easily suitability for industrialized production, the advantage such as environmental pollution is little.
Embodiment
Illustrate in greater detail the present invention below by embodiment.But scope of the present invention is not limited to these embodiment.
Embodiment 1
Breviscarpine sample solution preparation: 12g arginine is dissolved in 50mL boiling water for adjusting pH.Take 30g Breviscarpine crude product (purity 90.1%), add 400mL boiling water, stir, slowly drip arginine solution, controlling pH is 8.0, makes sample dissolution complete, is settled to 600mL, for subsequent use after 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 chromatographic stuffing, dress column volume 867 mL, the flow velocity balance chromatographic column with 3 times of column volume ultrapure waters with 1 times of column volume per hour.Get Breviscarpine sample solution 520 mL of preparation, flow velocity Continuous Flow with 1 times of column volume per hour is crossed resin column loading, continues to spend ionized water wash-out after end of the sample, then with the speed wash-out of 1 times of column volume per hour, be in charge of collection according to UV detection case, detect purity.Collection liquid qualified purity is merged, obtain collecting liquid 300mL altogether, it is 99.18% that HPLC detects purity, and this test scutellarin rate of recovery is 67.9%.
Embodiment 2
Breviscarpine sample solution preparation: 6g arginine is dissolved in 20mL boiling water for adjusting pH.Take 15g Breviscarpine crude product (purity 80%), add 600mL boiling water, stir, slowly drip arginine solution, controlling pH is 8.0, makes sample dissolution complete, is settled to 750mL, for subsequent use after 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 chromatographic stuffing, dress column volume 867mL, the flow velocity balance chromatographic column with the ultrapure water of 3 times of column volumes with 4 times of column volumes per hour.Get by Breviscarpine sample solution 433 mL of preparation, flow velocity Continuous Flow with 4 times of column volumes per hour is crossed resin column loading, continues to spend ionized water wash-out after end of the sample, then with 4 times of column volume speed wash-outs hourly, be in charge of collection according to UV detection case, detect purity.Collection liquid qualified purity is merged, obtain collecting liquid 285mL altogether, add Glacial acetic acid, making to collect liquid pH is 2-3, quiescent setting, filters, and filter cake is dried at 60 DEG C, obtain scutellarin dry product 5.7g, it is 99.51% that HPLC detects purity, and this test scutellarin rate of recovery is 70%.
Claims (3)
1. a preparation method for high-purity scutellarin, is characterized in that carrying out according to following step:
(1) chromatographic column balance: after dress post completes, use ultrapure water with 1 ~ 4 times of column volume flow velocity balance hourly chromatographic column;
(2) sample preparation: take lamp-dish flower acetic crude product and join boiling water, stir, slowly drip arginine solution, control pH be between 6.0 ~ 9.0, make sample dissolution complete, after constant volume while hot with for subsequent use after filter paper filtering; The wherein lamp-dish flower acetic crude product purity 80 ~ 92% described in step (2), wherein the concentration of the lamp-dish flower acetic crude product described in step (2) is 10 ~ 100mg/ml,
(3) loading: the sample liquid that step (2) is obtained, cross resin column with 2 times of column volume flow velocity Continuous Flow hourly
, resin volume used, unit is L; With the weight of sample, unit is g; Its ratio is 100:1 ~ 100:3; Wherein the resin described in step (3) is all grain microballoon resins of Uni PMM series CARBOPOL;
(4) wash-out: continue to spend ionized water wash-out after end of the sample, then, with 1 ~ 4 times of column volume speed wash-out hourly, be in charge of collection according to UV detection case, detect purity; Collection liquid qualified purity is merged, obtain collecting liquid, concentrating under reduced pressure obtains medicinal extract;
(5) dry: the lyophilize of gained medicinal extract is obtained to lamp-dish flower acetic, and its purity is greater than 99%; Wherein said lamp-dish flower acetic is the arginic acid salt of lamp-dish flower acetic.
2. 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.
3. the preparation method of a kind of high-purity scutellarin according to claim 1, is characterized in that wherein in step (4) with 2 times of column volume speed wash-outs hourly.
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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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| 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 |
| CN101580527A (en) * | 2009-04-29 | 2009-11-18 | 南开大学 | Adsorption resin method separation technology of scutellarin in fleabane flower extract |
| CN101683332A (en) * | 2008-09-26 | 2010-03-31 | 樊献俄 | high purity scutellarin salt bulk drug and preparation method thereof |
| 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
- 2012-04-11 CN CN201210103239.2A patent/CN102659872B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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| 楼云雁，等.静态吸附法选择纯化灯盏花素的大孔树脂.《中医药学刊》.2006,第24卷(第6期),第1129-1131页. * |
| 赵艳，等.大孔吸附树脂分离纯化灯盏花提取物中灯盏花甲素和灯盏花乙素的研究.《中草药》.2009,第40卷第153-155页. * |
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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 |
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