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

作　　者：孔瑶 姜鹏 詹常森 KONG Yao;JIANG Peng;ZHAN Changsen(Shanghai Hutchison Pharmaceuticals Co.,Ltd,Shanghai 201499,China;Shanghai Engineering Research Center for Innovation of Solid Preparation of TCM,Shanghai 201499,China)

机构地区：[1]上海和黄药业,上海201400 [2]上海中药固体制剂创新工程技术研究中心,上海201400

出　　处：《中国药品标准》2024年第6期618-623,共6页Drug Standards of China

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。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 repeatability,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 

分 类 号：R921.2[医药卫生—药学]