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[液相色谱-串联质谱法测定人血液中的美西律]

[Determination of mexiletine in human blood by liquid chromatography-tandem mass spectrometry].

作者信息

Yan Hui, Xiang Ping, Bo Juni, Shen Min

机构信息

Institute of Forensic Sciences, Ministry of Justice, Shanghai 200063, China.

出版信息

Fa Yi Xue Za Zhi. 2007 Dec;23(6):441-3.

Abstract

OBJECTIVE

To establish a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for detection of mexiletine by liquid chromatography tandem mass spectrometry.

METHODS

After simple protein precipitation of the blood sample with acetonitrile, the organic solvent layer diluted with LC mobile solvent was separated by Allure PFP Propyl column, confirmed and quantified by MS/MS in the multi-reaction monitoring (MRM) mode via positive electrospray ionization.

RESULTS

Mexiletine and naloxone (internal standard) got ideal resolution under the selected analytical condition. The correlation coeficient of linear calibration curve was over 0.9999 within the mexiletine concentration range 0.02-10 microg/mL. The relative standard deviations were under 10% for intra-day and under 15% for inter-day, and the detection limit was 0.01 microg/mL.

CONCLUSION

The established LC-MS/MS method is simple, rapid, sensitive, unaffected by matrix effect and appropriate for detection of mexiletine in blood in the field of therapeutic drug monitoring and forensic toxicology.

摘要

目的

建立一种采用液相色谱-串联质谱法(LC-MS/MS)检测美西律的方法。

方法

血液样本用乙腈进行简单的蛋白沉淀后,用液相色谱流动相溶剂稀释的有机相层通过Allure PFP丙基柱进行分离,采用正电喷雾电离,在多反应监测(MRM)模式下通过串联质谱进行确证和定量。

结果

在选定的分析条件下,美西律和纳洛酮(内标)得到了理想的分离度。美西律浓度在0.02 - 10μg/mL范围内,线性校准曲线的相关系数超过0.9999。日内相对标准偏差低于10%,日间相对标准偏差低于15%,检测限为0.01μg/mL。

结论

所建立的LC-MS/MS方法简便、快速、灵敏,不受基质效应影响,适用于治疗药物监测和法医毒理学领域血液中美西律的检测。

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