液相色谱串联质谱测定人血清中多黏菌素E1、E2的血药浓度

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中文摘要：目的:建立液相色谱串联质谱(LC-MS/MS)法测定人血清中多黏菌素E1、E2的血药浓度.方法:以多黏菌素B1为内标、乙腈溶液蛋白沉淀处理样品.色谱柱为Kinetex C18(3mm×100mm,2.6 μm),流动相A为含0.1%甲酸和5 mmol·L-1乙酸铵的水溶液,流动相B为含0.1%甲酸的甲醇溶液,梯度洗脱,流速0.5 mL·min-1.选用电喷雾离子源(ESI),正离子多反应监测扫描检测(MRM),用于定量分析的离子对分别为:m/z 585.6→241.1(多黏菌素E1),m/z 578.6→227.2(多黏菌素E2),m/z 602.6→101.2(多黏菌素B1),考察多黏菌素E的方法学,并测定使用硫酸黏菌素的患者血清中多黏菌素E1、E2的血药浓度.结果:多黏菌素E1、E2分别在0.0193～3.86 μg·mL-1、0.0283～5.65 μg·mL-1与测定值线性关系良好,多黏菌素E1、E2的定量下限分别为0.0193 μg·mL-1、0.0283 μg·mL-1.多黏菌素E1、E2日内与日间精密度、准确度、提取回收率、基质效应、稳定性均符合方法学要求,应用本方法测定接受硫酸黏菌素的15例患者的稳态血药谷浓度为(1.84±0.85)μg·mL-1.结论:本方法准确、灵敏、快速,稳定性良好,可用于检测人血清中多黏菌素E1、E2的血药浓度.

外文标题：Determining Plasma Concentrations of Polymyxin E1 and E2 in Human Serum with LC-MS/MS

外文摘要：Objective:To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining the concentrations of polymyxin E1 and E2 in human serum.Methods:Polymyxin B1 was used as an internal standard,and the samples were treated with acetonitrile solution for protein precipitation.The chromatographic column was Kinetex C18(3 mm×100 mm,2.6 μm).The mobile phase A was water solution containing 0.1%formic acid and 5 mmol·L-1 ammonium acetate,and the mobile phase B was methanol solution containing 0.1%formic acid.The flow rate was 0.5 mL·min-1 for gradient elution.Electrospray ionization(ESI)source and positive ion multiple reaction monitoring(MRM)scan detection were used.The ion pairs used for quantification were:m/z 585.6→241.1(Polymyxin E1),m/z 578.6→227.2(Polymyxin E2),and m/z 602.6→101.2(Polymyxin B1).The methodology of polymyxin E was investigated,and the serum concentrations of polymyxin E1 and E2 in patients treated with colistin sulfate were deter-mined.Results:The linear relationship between the determined values and the polymyxin E1 and E2 were good in the ranges of 0.0193-3.86 μg·mL-1 and 0.028 3-5.65 μg·mL-1,respectively.The lower limits of quantitation of polymyxin E1 and E2 were 0.0193 μg·mL-1 and 0.0283 μg·mL-1,respectively.The results of intra-day and inter-day precision,accuracy,extraction recovery,matrix effect and stability of Polymyxin E1 and E2 met the methodological requirements.The mean steady-state blood trough concentration of polymyxin E in 15 patients receiving colistin sulfate was(1.84±0.85)μg·mL-1.Conclusion:The method is accurate,sensitive,rapid and stable,and can be used to detect the serum concentrations of polymyxin E1 and E2.

外文关键词：

Liquid chromatography-tandem mass spectrometryColistin sulfatePolymyxin E1Polymyx-in E2Serum concentration

作者：

张淑婷、杨旭萍、左李安、薛晓燕、陈荣、胡楠、王莉英

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作者单位：

苏州大学附属第三医院,常州市第一人民医院药学部,常州 213003

苏州大学药学院,苏州 215000

关键词：

液相色谱-串联质谱硫酸黏菌素多黏菌素E1 多黏菌素E2 血药浓度

基金：

常州市科技基础设施建设计划—常州市临床药学重点实验室基金资助项目江苏省药学会—恒瑞医院药学科研项目常州市第十四批科技计划(应用基础研究指导性)项目江苏省药学会医院药学基金项目

项目编号：

CM20223005H202301CJ20219031H202146

出版年：

2024

药学与临床研究

江苏省药学会

药学与临床研究

CSTPCD

影响因子：0.95

ISSN：1673-7806

年,卷(期)：2024.32(4)