A kind of preparation method and application of high-purity breviscapine extract and preparation

A technology of breviscapine and extracts, which is applied in the field of preparation of high-purity scutellarin extracts and preparations, can solve the problems of high impurity content, roughness, and low purity of ingredients, and achieve large separation, fast separation speed, and adsorption A large amount of effect

Active Publication Date: 2019-02-26
黑龙江华弘成生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the existing extraction and separation process of breviscapine is too rough, resulting in low purity of the main components of the product and high content of impurities. After clinical use of some breviscapine injections, occasional chest tightness, fatigue, rash, and itching all over the body , heart palpitations and other adverse reactions

Method used

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  • A kind of preparation method and application of high-purity breviscapine extract and preparation
  • A kind of preparation method and application of high-purity breviscapine extract and preparation
  • A kind of preparation method and application of high-purity breviscapine extract and preparation

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Example 1 High-purity breviscapine extract was prepared by dynamic ultrasonic countercurrent extraction combined with macroporous adsorption resin column chromatography and dynamic axial compression industrial preparation chromatographic separation technology

[0022] Crush 10 kg of Erigeron breviscapus to 20-30 meshes, add 8 times the amount of ethanol with a concentration of 70% by volume, extract continuously at a frequency of 30 kHz, and ultrasonic power 20 kW for 3 times, each time for 40 min, filter, and combine the extracts , recover the extraction solvent under reduced pressure, properly concentrate to a concentration of 0.6 g crude drug / ml, add 1 mol / L hydrochloric acid to adjust the pH value to 4, and pass through the HPD650 macroporous adsorption resin chromatography column at a flow rate of 2BV / h. The ratio of solid matter to dry resin is 1:6, and the ratio of diameter to height is 1:8. First wash the resin column bed with 4 BV of distilled water, and the elu...

Embodiment 2

[0023] Example 2 Preparation of High Purity Breviscapine Extract by Heating Reflux Extraction Combined with Macroporous Adsorption Resin Column Chromatography and High Speed ​​Counter-Current Chromatography

[0024] Add 15 times the amount of ethanol with a volume percentage concentration of 80% to 2 kg of Erigeron breviscapus crushed to 20-30 mesh, heat and reflux for extraction 3 times, each time for 1.5 h, filter, combine the extracts, and concentrate to a concentration of 1.0 g Crude drug / ml, after filtering, add 1 mol / L hydrochloric acid to adjust the pH value to 4-5, pass through the HPD400 macroporous adsorption resin chromatography column at a flow rate of 3BV / h, and the ratio of the sample solution to the dry resin is 1 : 8, the diameter-to-height ratio is 1: 10, first wash the resin with 6 BV of water, the elution flow rate is 4 BV / h, discard the water eluent; then elute with 60% methanol by volume, and elute The flow rate is 3 BV / h, the eluent is decompressed to rec...

Embodiment 3

[0025] Example 3 Preparation of high-purity breviscapine extract by heating reflux extraction combined with macroporous adsorption resin column chromatography and dynamic axial compression industrial preparation chromatographic separation technology

[0026] 5 kg of Asarum breviscapus was moderately crushed, and 10 times the amount of 60% methanol was added, and the frequency was 30 kHz, the ultrasonic power was 20 kW, and the ultrasonic power was continuously ultrasonically countercurrently extracted 3 times, each time for 0.5 h, filtered, combined extracts, methanol was recovered under reduced pressure, and water was added to adjust Concentration to 1.5 g crude drug / ml, add 1 mol / L hydrochloric acid to adjust the pH value to 6, pass through the SP825 macroporous adsorption resin chromatography column twice at a flow rate of 2BV / h, and load the sample solution according to the ratio of solid content to dry resin 1:9, the ratio of diameter to height is 1:8, first wash the resin...

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Abstract

The invention provides a preparation method for high-purity breviscapine extract as well as preparations and application thereof. The method disclosed by the invention comprises the following steps: taking erigeron breviscapus as a raw material, performing dynamic ultrasonic countercurrent extraction or heating reflux extraction, filtering, centrifuging, adjusting the pH value to 2.0-7.0, performing macroporous resin column chromatography, preparing by using dynamic axial compression industrial chromatographic separation, or preparing by adopting high-speed counter-current chromatography, freezing or performing spray drying, thereby obtaining the high-purity breviscapine extract. According to the method disclosed by the invention, extraction can be completed in a short time at a low temperature, the separation cycle is short, the efficiency is high, the occupied volume for extraction is reduced, the production cost is lowered, the energy consumption and environmental pollution can be reduced, and the purity of the obtained breviscapine can be 95% or higher. Added with various added pharmaceutical adjuvants, the high-purity breviscapine extract can be prepared into ordinary tablets, thin membrane coated tablets, capsules, dispersible tablets, dropping pills, granules, sustained-release preparations and other solid oral preparations, as well as spray, aerosol, lyophilized powder for injection and injection, and the preparations can be used for treating cardiovascular and cerebrovascular diseases and are obvious in curative effects, safe and reliable.

Description

technical field [0001] The invention belongs to the field of plant and traditional Chinese medicine extracts, and in particular relates to a preparation method and application of a high-purity scutellarin extract and preparation. Background technique [0002] Cardiovascular and cerebrovascular disease is the number one killer that seriously endangers human health and life in the world today, and its morbidity and mortality have surpassed malignant tumors and ranked first in the world. According to the report of the World Health Organization (WHO), 17 million people die from cardiovascular and cerebrovascular diseases in the world every year, accounting for 30.3% of the death population. , Roger VL, Benjamin EJ, Berry JD, Borden WB, et al. Heart disease and stroke statistics--2013 update: a report from the American Heart Association. Circulation. 2013; 127(1):e6-e245]. According to statistics from the National Health and Family Planning Commission, cardiovascular and cerebro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08A61K31/7048A61P9/10A61P7/02A61P25/28
Inventor 刘欣陈曾贞石晨瑜曹晨谭超李云飞
Owner 黑龙江华弘成生物科技有限公司
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