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固相支持液-液萃取/液相色谱-串联质谱法测定人全血中环孢素A
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作者单位
利利,贾叶青,张倩影,张爱国,王曼曼,李冬梅,王学生 1.华北理工大学公共卫生学院2.华北理工大学附属医院3.华北理工大学药学院 
基金项目:国家自然科学基金(21305028);河北省自然科学基金(H2017209232,H2016209018);河北省教育厅重点项目(ZD2018014);华北理工大学培育基金项目(JQ201717)
中文摘要:采用固相支持液-液萃取/液相色谱-串联质谱(LC-MS/MS)技术建立了人全血中环孢素A的分析方法。全血样品经蛋白沉淀后,上样至固相支持液-液萃取柱,经甲基叔丁基醚洗脱,Shim-pack XR-ODS色谱柱(75 mm×3.0 mm i.d.,2.2 μm)分离,电喷雾电离源、正离子模式和多反应监测模式下采集数据,以环孢素D为内标物定量。结果表明,环孢素A在 1.5~500 μg/L范围内呈良好的线性关系,相关系数(r)为0.998,检出限和定量下限分别为0.5 μg/L和1.5 μg/L,在50、100、400 μg/L 3个加标浓度下的平均回收率为78.6%~83.5%,日内和日间相对标准偏差(n=3)分别为3.1%~5.6%和4.5%~8.3%。该方法操作简便、灵敏度高,可用于全血中环孢素A的分析。
中文关键词:环孢素A  全血  固相支持液-液萃取  液相色谱-串联质谱法
 
Determination of Cyclosporin A in Human Whole Blood Using Liquid Chromatography-Tandem Mass Spectrometry with Solid Supported Liquid-Liquid Extraction
Abstract:A method based on liquid chromatography-tandem mass spectrometry(LC-MS/MS) with solid supported liquid-liquid extraction was developed for the determination of cyclosporin A in human whole blood.The whole blood sample was loaded on the solid supported liquid-liquid extraction column after protein precipitation,and then eluted with methyl tert butyl ether.The extract was injected into a Shim pack XR-ODS(75 mm×3.0 mm i.d.,2.2 μm) column for separation,followed by detection of mass spectrometry in multiple reaction monitoring mode via an electrospray ionization interface.The quantitation was achieved using cyclosporin D as the internal standard.There was a good linearity for the method toward cyclosporin A in the range of 1.5-500 μg/L with a correlation coefficient(r) of 0.998.The limits of detection and quantitation were down to 0.5 μg/L and 1.5 μg/L,respectively.The average recoveries for the analyte at three spiked levels ranged from 78.6% to 83.5% with the intra day and inter day relative standard deviations of 3.1%-5.6% and 4.5%-8.3%,respectively.This method is suitable for the determination of cyclosporin A in whole blood sample due to its advantages of simplicity,rapidness,accuracy and reliability.
Key Words:cyclosporin A  whole blood  solid supported liquid-liquid extraction  liquid chromatography-tandem mass spectrometry(LC-MS/MS)
引用本文:利利,贾叶青,张倩影,张爱国,王曼曼,李冬梅,王学生.固相支持液-液萃取/液相色谱-串联质谱法测定人全血中环孢素A[J].分析测试学报,2018,37(11):1371-1375.
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