高效液相色谱-串联质谱法测定肝组织中华蟾酥毒基和酯蟾毒配基  

Determination of Cinobufagin and Resibufogenin in Liver Tissue by HPLC-MS/MS

作　　者：王薇[1] 刘明东[2] 颜有仪[1] 叶懿[1] 赵俊红[2] 熊卉[1] 肖敏[1] 廖林川[1] 

机构地区：[1]四川大学华西基础医学与法医学院,四川成都610041 [2]四川大学华西药学院,四川成都610041

出　　处：《法医学杂志》2013年第4期268-272,共5页Journal of Forensic Medicine

摘　　要：目的建立灵敏、准确的高效液相色谱-串联质谱法（HPLC-MS/MS）测定肝组织中华蟾酥毒基和酯蟾毒配基含量的方法。方法肝组织匀浆液中加入内标地塞米松,用二氯甲烷提取后挥干,残渣加入甲醇溶液溶解并上样到ProElut C18固相萃取柱上分离净化,应用HPLC-MS/MS正离子多反应监测模式测定。结果肝组织中华蟾酥毒基和酯蟾毒配基分别在1~204 ng/g和1~206 ng/g范围内线性关系良好。检测限（S/N≥3）均为0.3 ng/g。基质效应为96.5%~126.7%。萃取回收率为70.0%~82.3%。日内及日间精密度均小于10%。结论所建方法灵敏、可靠,能满足法医毒物分析的鉴定需要。Objective To develop a sensitive and accurate assay for detecting cinobufagin and resibufogenin in liver tissue using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.Methods The homogenization of liver tissue with internal standard dexamethasone was extracted with dichloromethane.The extracts with methanol were purified through ProElut C18 solid phase extraction and tested in positive electrospray ionization with multiple reaction monitoring of HPLC-MS/MS.Results The good linear relationship of cinobufagin and resibufogenin in liver tissue were 1-204 ng/g and 1-206 ng/g,respectively.The minimal detection threshold（S/N≥3） of this method was 0.3 ng/g for both cinobufagin and resibufogenin.The matrix effect was 96.5%-126.7%.The extraction recovery coefficient was 70.0%-82.3%.The precision of intra-day and inter-day was less than 10%.Conclusion This method is sensitive and reliable,and can be used in forensic toxicological analysis.

关 键 词：法医毒理学 串联质谱法 高效液相色谱法 华蟾酥毒基 酯蟾毒配基 

分 类 号：R969.1[医药卫生—药理学]