Improvement of Quality Control Standard of Bufonis Venenum in Shexiang Baoxin Pills

Li-yao SHI; Yun-ge FANG; Liang-mian CHEN; Rui WANG; Zhi-min WANG; Hui-min GAO; Peng JIANG; Chang-sen ZHAN

doi:10.13422/j.cnki.syfjx.20211646

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Improvement of Quality Control Standard of Bufonis Venenum in Shexiang Baoxin Pills

更新时间：2021-12-14

- Improvement of Quality Control Standard of Bufonis Venenum in Shexiang Baoxin Pills
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 28, Issue 2, Pages: 159-165(2022)
- 作者机构：
  
  1.山西中医药大学，山西晋中 030619
  2.中国中医科学院中药研究所中药质量控制技术国家工程实验室，北京 100700
  3.上海和黄药业有限公司，上海 200201
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20211646
  CLC： R22;R28;R914;O657.7
- Published：20 January 2022，
  
  Published Online：10 May 2021，
  
  Received：07 April 2021，
- 稿件说明：
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石莉尧,房蕴歌,陈两绵等.麝香保心丸中蟾酥的质量控制标准提升[J].中国实验方剂学杂志,2022,28(02):159-165.

SHI Li-yao,FANG Yun-ge,CHEN Liang-mian,et al.Improvement of Quality Control Standard of Bufonis Venenum in Shexiang Baoxin Pills[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(02):159-165.
石莉尧,房蕴歌,陈两绵等.麝香保心丸中蟾酥的质量控制标准提升[J].中国实验方剂学杂志,2022,28(02):159-165. DOI： 10.13422/j.cnki.syfjx.20211646.

SHI Li-yao,FANG Yun-ge,CHEN Liang-mian,et al.Improvement of Quality Control Standard of Bufonis Venenum in Shexiang Baoxin Pills[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(02):159-165. DOI： 10.13422/j.cnki.syfjx.20211646.

摘要

目的

建立麝香保心丸中蟾毒灵、华蟾酥毒基和脂蟾毒配基含量测定的一测多评法，为完善麝香保心丸国家标准提供检测方法。

方法

采用高效液相色谱法（HPLC）建立麝香保心丸中3种蟾毒配基含量的同步测定方法，并进行方法学验证，色谱条件为Nucleosil 100-5 C

色谱柱（4.6 mm×250 mm，5 μm），流动相乙腈-0.1%磷酸二氢钾水溶液（磷酸调节pH 3.2）（48∶52），流速0.6 mL·min

-1

，检测波长296 nm，柱温35 ℃；以华蟾酥毒基为内参物，建立其对蟾毒灵和脂蟾毒配基的相对校正因子，并对相对校正因子的关键影响因素进行考察，采用相对保留时间进行待测色谱峰定位，结合在线紫外光谱和超高效液相色谱-四级杆飞行时间质谱法（UPLC-QTOF/MS）提供的精确相对分子质量辅助识别待测色谱峰；采用外标法验证一测多评法测定结果的准确性。

结果

建立了麝香保心丸中3种蟾毒配基的一测多评质量评价模式，华蟾酥毒基对蟾毒灵和脂蟾毒配基的相对校正因子分别为0.922和1.01；11批样品中三者总量范围33.7~36.0 µg/丸，外标法和一测多评法测定结果无显著性差异。

结论

建立的方法可用于麝香保心丸中蟾毒灵、华蟾酥毒基和脂蟾毒配基的质量控制，建议麝香保心丸国家标准含量测定项下蟾酥药材的质量控制新增蟾毒灵，并以这3种成分总量制定含量限度值。

Abstract

Objective

To develop a quantitative analysis of multi-components by single marker （QAMS） for determination of bufalin， cinobufagin and resibufogenin in Shexiang Baoxin pills， and to provide a method for improving the national standard of the pills.

Method

High performance liquid chromatography （HPLC） was developed for simultaneous determination of bufalin， cinobufagin and resibufogenin in Shexiang Baoxin pills and the methodology validation was carried out. The chromatographic separation was performed on a Nucleosil 100-5 C

column （4.6 mm×250 mm， 5 μm） with the mobile phase of acetonitrile -0.1% potassium dihydrogen phosphate aqueous solution （pH adjusted to 3.2 with phosphoric acid）（48∶52）， and the flow rate was 0.6 mL·min

-1

， the detection wavelength was set at 296 nm and the column temperature was 35 ℃. Taking cinobufagin as the internal standard， the relative correction factors （RCFs） of bufalin and resibufogenin were calculated， and the key influencing factors of RCFs were investigated. Relative retention time was used for the chromatographic peak location of the analyte， combining with the on-line ultraviolet spectroscopy and accurate relative molecular weight obtained by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry （UPLC-QTOF/MS）. The external standard method was used to verify the contents of three components obtained by QAMS.

Result

QAMS was established for the determination of bufalin， cinobufagin and resibufogenin in the samples， and RCFs of cinobufagin to bufalin and resibufogenin were 0.922 and 1.01， respectively. The total content of the three marker compounds in 11 batches of Shexiang Baoxin pills was 33.7-36.0 µg per pill. There was no significant difference between the quantitative results of QAMS and external standard method.

Conclusion

The established method can be used for the quality control of bufalin， cinobufagin and resibufogenin in Shexiang Baoxin pills. It is suggested that bufalin should be considered as one of three marker compounds， and the sum of bufalin， cinobufagin and resibufogenin should be used for the content limit of this preparation.

关键词

蟾酥麝香保心丸华蟾酥毒基蟾毒灵脂蟾毒配基一测多评法高效液相色谱法（HPLC）

Keywords

Bufonis VenenumShexiang Baoxin pillscinobufaginbufalinresibufogeninquantitative analysis of multi-components by single marker （QAMS）high performance liquid chromatography （HPLC）

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