法医学杂志

法医学杂志 ›› 2013, Vol. 29 ›› Issue (4): 268-272.DOI: 10.3969/j.issn.1004-5619.2013.04.008

• 论著 • 上一篇    下一篇

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

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   

  1. （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）
  • 发布日期:2013-08-25 出版日期:2013-08-28
  • 通讯作者: 廖林川，男，博士，教授，主要从事法医毒物分析教学及科研工作；E-mail：linchuanliao@scu.edu.cn
  • 作者简介:王薇（1986—），女，四川泸州人，硕士研究生，主要从事法医毒物分析研究；E-mail：freja_v@163.com

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

WANG WEI1, LIU MING-DONG2, YAN YOU-YI1, YE YI1, ZHAO JUN-HONG2, XIONG HUI1, XIAO MIN1, LIAO LIN-CHUAN1   

  1. （1. West China School of Preclinical and Forensic Medicine, Sichuan University, Chengdu 610041, China; 2. West China School of Pharmacy, Sichuan University, Chengdu 610041, China）
  • Online:2013-08-25 Published:2013-08-28

被引次数

2

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。

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

Abstract: 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.

Key words: forensic toxicology, tandem mass spectrometry, high performance liquid chromatography-tandem mass spectrometry, cinobufagin, resibufogenin

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