Determination of Cinobufagin and Resibufogenin in Liver Tissue by HPLC-MS/MS
Author(s): WANG Zuo, LIU Mingdong, YAN Youyi, YE Zuo, ZHAO Junhong, XIONG Hui, XIAO Min, LIAO Linchuan
Pages: 268-272
Year: 2013 Issue: 4
Journal: Journal of Forensic Medicine
Keyword: forensic toxicology; tandem mass spectrometry; high performance liquid chromatography-tandem mass spectrometry; cinobufagin; resibufogenin;
Abstract: 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.
Pages: 268-272
Year: 2013 Issue: 4
Journal: Journal of Forensic Medicine
Keyword: forensic toxicology; tandem mass spectrometry; high performance liquid chromatography-tandem mass spectrometry; cinobufagin; resibufogenin;
Abstract: 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.
Related Articles