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一种液相色谱-电喷雾串联质谱法测定法医全血样品中的抗心律失常药物及其代谢物。

A liquid chromatography-electrospray tandem mass spectrometry method for the determination of antiarrhythmic drugs and their metabolites in forensic whole blood samples.

机构信息

Section for Toxicology and Drug Analysis, Department of Forensic Medicine, Aarhus University, Brendstrupgaardsvej 100, 8200 Aarhus N, Denmark.

出版信息

J Anal Toxicol. 2012 Mar;36(2):116-22. doi: 10.1093/jat/bkr021.

DOI:10.1093/jat/bkr021
PMID:22337781
Abstract

A liquid chromatography-tandem mass spectrometry method, using pneumatically assisted electrospray ionization was developed for the determination of amiodarone, desethylamiodarone, propafenone, N-depropylpropafenone, 5-OH-propafenone, flecainide, and sotalol in human antemortem and postmortem whole blood. A mixture of methanol and acetonitrile was used to extract the samples, and the clear extracts obtained from the protein precipitation were injected directly onto an ethyl-linked phenyl LC column. The isotope dilution technique was applied for quantitative analysis. The relative intralaboratory reproducibility standard deviations were 5-9% at a concentration range of 1-5 mg/L and 9-12% at a concentration of 0.1 mg/L. The mean true recoveries were greater than 91% in the concentration range of 0.05-5 mg/L. The detection limits were in the range of 8-18 µg/L.

摘要

建立了一种采用气动辅助电喷雾电离的液相色谱-串联质谱法,用于检测人死后全血中的胺碘酮、去乙基胺碘酮、普罗帕酮、N-去丙基普罗帕酮、5-OH-普罗帕酮、氟卡尼和索他洛尔。甲醇和乙腈的混合物用于提取样品,从蛋白沉淀中得到的澄清提取物直接注入乙基键合苯基 LC 柱。同位素稀释技术用于定量分析。在浓度范围为 1-5 mg/L 时,相对实验室内重现性标准偏差为 5-9%,在浓度为 0.1 mg/L 时为 9-12%。在 0.05-5 mg/L 的浓度范围内,平均真实回收率大于 91%。检测限在 8-18 µg/L 范围内。

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