首页|期刊导航|分析测试学报|超高效液相色谱-质谱联用法检测血中丁咪酯、仲丁咪酯及依托咪酯酸

超高效液相色谱-质谱联用法检测血中丁咪酯、仲丁咪酯及依托咪酯酸OA

Determination of Butomidate,Secbutomidate and Etomidate Acid in Blood by UPLC-MS/MS

中文摘要英文摘要

该研究建立了超高效液相色谱-质谱联用(UPLC-MS/MS)测定血中丁咪酯、仲丁咪酯及其主要代谢物的分析方法.样品经甲醇-乙腈(1∶3)混合溶液沉淀蛋白法提取后,采用XSelect HSS T3色谱柱(100 mm× 2.1mm,2.5 μm),以0.1%甲酸水溶液-0.1%甲酸乙腈为流动相进行梯度洗脱,在电喷雾离子源(ESI)和多反应监测(MRM)模式下进行检测.结果表明,丁咪酯、仲丁咪酯和依托咪酯酸在0.1~100 ng/mL范围内线性关系良好,相关系数(r2)均不小于0.999 1,检出限(LOD)为0.001~0.01 ng/mL,定量下限(LOQ)为0.004~0.03 ng/mL,基质效应为80.1%~120%,回收率为90.1%~96.9%,日内相对标准偏差(RSD)均不大于8.3%,日间RSD均不大于9.7%.该方法具有操作简便、选择性好、线性范围宽、灵敏度高的特点,可用于法庭科学血样中丁咪酯、仲丁咪酯和依托咪酯酸的检验鉴定.

A method of ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the detection of butomidate,secbutomidate,and major metabo-lites in blood.The blood samples were extracted by precipitation protein using a mixed solution of methanol-acetonitrile(1∶3),then separated on a XSelect HSS T3 column(100 mm×2.1 mm,2.5μm)by gradient elution,with 0.1%formic acid water and 0.1%formic acid acetonitrile as mobile phases,and electrospray ion source(ESI)in multi-response monitoring(MRM)mode.The results indicated that the linear relationship of butomidate,secbutomidate,and etomidate acid was good in the range of 0.1-100 ng/mL,with correlation coefficients(r2)not less than 0.999 1.The limits of de-tection(LODs)and the limits of quantitation(LOQs)were in the range of 0.001-0.01 ng/mL and 0.004-0.03 ng/mL,respectively.The matrix effects ranged from 80.1%-120%,and the recoveries ranged from 90.1%-96.9%,with the intra-day relative standard deviations(RSDs)not more than 8.3%and inter-day RSDs not more than 9.7%.The method has the advantages of simple operation,good selectivity,wide linear range,high sensitivity,and it is suitable for the identification of bu-tomidate,secbutomidate,and etomidate acid in blood.

李想;张睿文;宋辉;夏鑫鑫;朱昱;易梓琛

中国刑事警察学院 刑事科学技术学院,辽宁 沈阳 110854沈阳市公安局 禁毒支队,辽宁 沈阳 110084中国刑事警察学院 刑事科学技术学院,辽宁 沈阳 110854中国刑事警察学院 刑事科学技术学院,辽宁 沈阳 110854中国刑事警察学院 刑事科学技术学院,辽宁 沈阳 110854中国刑事警察学院 刑事科学技术学院,辽宁 沈阳 110854

化学化工

超高效液相色谱-质谱联用丁咪酯仲丁咪酯依托咪酯酸裂解规律定性定量分析

UPLC-MS/MSbutomidatesecbutomidateetomidate acidfragmentation rulequalitative and quantitative analysis

《分析测试学报》 2026 (2)

414-419,6

辽宁省教育厅高校基本科研项目(LJ212510175005,LJ212410175012)公安部技术研究计划项目(2024JSYJC08)辽宁省科技厅重点研发项目(民生科技类)(2024JH2/102500083)

10.12452/j.fxcsxb.25072002

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