固相支撑液液萃取-液相色谱-串联质谱法检验生物样本中的地高辛及其代谢物  

Determination of digoxin and its metabolites in biological samples by solid-phase supported liquid-liquid extraction-liquid chromatography-tandem mass spectrometry

作　　者：孙一健 邹波 王爱华[2] 王瑞花[2] 李佳宜 侯小平[2] 王继芬[1] 常靖[2] SUN Yijian;ZOU Bo;WANG Aihua;WANG Ruihua;LI Jiayi;HOU Xiaoping;WANG Jifen;CHANG Jing(Investigation Institute,People's Public Security University of China,Beijing 100038,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]公安部物证鉴定中心,北京100038

出　　处：《分析试验室》2023年第5期665-670,共6页Chinese Journal of Analysis Laboratory

基　　金：公安部物证鉴定中心基科费项目(2020JB010)资助。

摘　　要：采用固相支撑液液萃取-超高效液相色谱-串联质谱(SLE-UPLC-MS/MS)技术建立了生物样本血液、尿液和肝组织中地高辛(DG)及其3种代谢物的分析方法。生物样本经匀浆、蛋白沉淀后,通过含有硅藻土的固相支撑液液萃取(SLE)柱净化富集,经洗脱、定容后进行LC-MS/MS分析。结果表明,血液基质中,地高辛在0.1~100 ng/mL浓度范围内线性关系良好;肝脏和尿液基质中,地高辛在0.2~100 ng/mL浓度范围内线性关系良好,地高辛的3种代谢物在0.5~100 ng/mL浓度范围内线性关系良好,3个浓度水平(10, 50和100 ng/mL)的加标回收率为60.5%~95.6%,基质效应80.7%~113.6%,日内、日间相对标准偏差(RSD)均小于13%,检出限为0.1~0.5 ng/mL。所建立的方法可用于生物样本中地高辛及其代谢物的定性定量分析。A method by solid-phase supported liquid-liquid extraction-liquid chromatography-tandem mass spectrometry(SLE-LC-MS/MS)for the analysis of digoxin(DG),digoxin-bis-digitoxosid(DGbis),digoxin-monodigitoxosid(DGmono)and dihydrodigoxin(H_(2)DG)in biological samples,including blood,urine and liver tissue was established.The biological samples were loaded on the solid supported liquid-liquid extraction column after protein precipitation and homogenization for purification and enrichment.In the blood matrix,there was a good linearity for the detection of DG in the range of 0.1-100 ng/mL.In the liver and urine matrix,there were good linearities for the detection of DG in the range of 0.2-100 ng/mL.Three metabolites of DG exhibited good linearities in the range of 0.5-100 ng/mL.The average recoveries for the analyte at three spiked levels ranged from 60.5%to 95.6%and the matrix effects ranged from 80.7%to 113.6%,with the intra-day and inter-day RSD less than 13%.The detection limits were 0.1-0.5 ng/mL.This method can be used for the qualitative and quantitative analysis of DG and its metabolites in biological samples.

关 键 词：固相支撑液液萃取 生物样本 超高效液相色谱-串联质谱 地高辛及其代谢物 

分 类 号：O657.63[理学—分析化学]