中国药品标准2024,Vol.25Issue(6) :618-623.DOI:10.19778/j.chp.2024.06.015

SPE-UV法快速测定蟾酥鲜浆中蟾毒灵、华蟾酥毒基、脂蟾毒配基的总含量

Rapid determination of total content of bufalin,cinobufotalin and lipobufotalin in Bufonis Venenum pulp by solid phase extraction(SPE)-UV spectrometry

孔瑶 姜鹏 詹常森
中国药品标准2024,Vol.25Issue(6) :618-623.DOI:10.19778/j.chp.2024.06.015

SPE-UV法快速测定蟾酥鲜浆中蟾毒灵、华蟾酥毒基、脂蟾毒配基的总含量

Rapid determination of total content of bufalin,cinobufotalin and lipobufotalin in Bufonis Venenum pulp by solid phase extraction(SPE)-UV spectrometry

孔瑶 1姜鹏 1詹常森1
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作者信息

  • 1. 上海和黄药业,上海 201400;上海中药固体制剂创新工程技术研究中心,上海 201400
  • 折叠

摘要

目的:建立固相萃取(SPE)紫外分光光度法(UV)快速检测蟾酥鲜浆中蟾毒灵、华蟾酥毒基、脂蟾毒配基总含量的方法.方法:采用Waters Oasis HLB固相萃取小柱纯化蟾酥鲜浆样品,清洗液为29%乙腈,清洗体积为5 mL,洗脱液为95%乙腈,洗脱体积为6 mL,洗脱液采用紫外分光光度法检测,检测波长为295 nm.结果:建立了 HLB SPE-UV法快速测定蟾酥鲜浆中蟾毒灵、华蟾酥毒基、脂蟾毒配基总含量的方法,该方法线性关系良好(r>0.999),精密度高(RSD<5%),重复性好(RSD<5%),样品回收率在96.34%~104.76%范围内,均符合要求.结论:该方法样品处理简单,检测快速简便,重复性好,准确度高,精密度高.作为蟾酥药材中间体的质量控制,填补了蟾酥鲜浆快速检测方法的空白.

Abstract

Objective:To establish a method for SPE purification of Bufonis Venenum pulp and determination of total content of bufalin,cinobufotalin and lipobufotalin in Bufonis Venenum pulp by UV spectrophotometry.Methods:Using Waters Oasis HLB solid-phase extraction small column to purify Bufonis Venenum pulp,the cleaning solution was 29%acetonitrile,the cleaning volume was 5 mL,the eluent was 95%acetonitrile,the elution volume was 6 mL,the elution was detected by UV spectrophotometer and the detection wavelength was 295 nm.Results:The method has good linear relationship(r>0.999),high precision(RSD<5%),good repeatability(RSD<5%),and the sample recovery rate within in the ranges of 96.34%-104.76%,which meets the requirements.Conclusion:The sample processing method was rapid and simple,with good repeatabili-ty,high accuracy and high precision.As the quality control of Bufonis Venenum medicinal material intermediate,it fills the gap in the detection method of Bufonis Venenum pulp.

关键词

固相萃取/紫外分光光度法/蟾酥鲜浆/蟾毒灵/华蟾酥毒基/脂蟾毒配基

Key words

solid phase extraction/UV spectrophotometry/Bufonis Venenum pulp/bufalin/cinobufotalin/lipobufotalin

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出版年

2024
中国药品标准
国家药典委员会

中国药品标准

影响因子:0.372
ISSN:1009-3656
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