Optimization of Purification Process of Total Alkaloid Extract of <italic style="font-style: italic">Berberis dictyophylla</italic> Cortex by Macroporous Resin and Investigation of Its Quality Standard

Hui FENG; Ya ZHAO; Xiao-yan WANG; Yu-nan XIANG; Lu HAO; Qi-en LI; Xian-jia LI; Xian-rong LAI

doi:10.13422/j.cnki.syfjx.20190555

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Optimization of Purification Process of Total Alkaloid Extract of Berberis dictyophylla Cortex by Macroporous Resin and Investigation of Its Quality Standard

Pharmacy and Processing | 更新时间：2021-02-09

- Optimization of Purification Process of Total Alkaloid Extract of Berberis dictyophylla Cortex by Macroporous Resin and Investigation of Its Quality Standard
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 25, Issue 16, Pages: 97-103(2019)
- 作者机构：
  
  1.成都中医药大学　民族医药学院，成都　 611137；
  2.青海大学　藏医学院，西宁　 810000
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20190555
  CLC： R22; R28; R9; C37
- Received：24 September 2018，
  
  Published Online：19 November 2018，
  
  Published：20 August 2019
- 稿件说明：
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Hui FENG, Ya ZHAO, Xiao-yan WANG, et al. Optimization of Purification Process of Total Alkaloid Extract of Berberis dictyophylla Cortex by Macroporous Resin and Investigation of Its Quality Standard[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(16): 97-103.
DOI：

Hui FENG, Ya ZHAO, Xiao-yan WANG, et al. Optimization of Purification Process of Total Alkaloid Extract of Berberis dictyophylla Cortex by Macroporous Resin and Investigation of Its Quality Standard[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(16): 97-103. DOI： 10.13422/j.cnki.syfjx.20190555.

摘要

目的：

优选小檗皮总生物碱提取物的大孔树脂纯化工艺，并建立其质量标准，为该有效部位的制剂开发提供参考。

方法：

采用酸性染料比色法考察小檗皮总生物碱提取物的纯化工艺，考察的工艺参数包括上样液质量浓度、上样速度、树脂柱径高比、水洗用量、洗脱剂体积分数及用量、洗脱流速等。采用HPLC测定小檗皮总生物碱提取物中4种生物碱类成分(木兰花碱、盐酸药根碱、盐酸巴马汀、盐酸小檗碱)的含量，流动相乙腈-0.1%磷酸水溶液梯度洗脱，检测波长270 nm，确定最佳纯化工艺。按2015年版《中国药典》的要求进行小檗皮总生物碱纯化物的薄层色谱鉴别、含量测定、特征图谱等质量标准研究。

结果：

小檗皮总生物碱提取物的最佳纯化条件为采用HPD100型大孔树脂10 g，树脂柱径高比1∶8，上样液质量浓度11 g·L

－1

，上样液体积50 mL，上样流速1 mL·min

－1

，加4 BV水洗脱(1 BV＝15 mL)，加30%乙醇9 BV洗脱；纯化后小檗皮总生物碱的转移率

80%，纯度

65%。建立了小檗皮总生物碱纯化物的质量标准，特征图谱中共有峰有19个，整体相似度均

0.99。

结论：

优选的纯化工艺稳定可行，建立的质量标准可靠，适用于小檗皮总生物碱提取物的纯化及质量控制。

Abstract

Objective:

To optimize purification process of total alkaloid extract of

Berberis dictyophylla

cortex by macroporous resin

and to establish its quality standard.

Method:

Acid dye colorimetry was used to investigate the purification process of total alkaloid extract of

dictyophylla

cortex

the process parameters included concentration of sample solution

speed of sampling

diameter-height ratio of resin column

water washing amount

concentration and dosage of eluent

flow rate of elution

etc.In order to determine the optimum process

HPLC was employed to determine the contents of four alkaloids(magnoflorine

jatrorrhizine hydrochloride

palmatine hydrochloride

and berberine hydrochloride) with mobile phase of acetonitrile-0.1% phosphoric acid aqueous solution for gradient elution and detection wavelength at 270 nm.After being purified

quality standard of total alkaloid extract of

dictyophylla

cortex was investigated according to the requirements in the 2015 edition of

Chinese Pharmacopoeia

Result:

Optimal purification conditions were as following: 10 g of HPD100 macroporous adsorption resin with a column diameter-height ratio of 1∶8

sampling solution concentration of 11 g·L

-1

the loading flow rate of 1 mL·min

-1

sampling solution volume of 50 mL

washed with 4 BV of water(1 BV=15 mL) and added 9 BV of 30% ethanol

after being purified

the transfer rate of total alkaloids was

80%

and its purity was

65%.The quality standard of total alkaloid extract of

dictyophylla

cortex was established

there were 19 common peaks in the characteristic chromatogram

and the overall similarity was

0.99.

Conclusion:

This optimized purification process is stable and feasible

and the established quality standard is controllable.

关键词

Keywords

references

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Optimization of Purification Process of Total Alkaloid Extract of Berberis dictyophylla Cortex by Macroporous Resin and Investigation of Its Quality Standard

DOI：10.13422/j.cnki.syfjx.20190555

摘要

Abstract

关键词

Keywords

references