高效液相色谱-质谱联用法检测免疫抑制剂及其合并用药

引用本文: 李鹏飞, 王燕, 张征, 童卫杭, 吴华, 马萍, 王静, 刘丽宏. 高效液相色谱-质谱联用法检测免疫抑制剂及其合并用药[J]. 分析化学, 2012, 40(10): 1573-1578. doi: 10.3724/SP.J.1096.2012.11135 shu

Citation: LI Peng-Fei, WANG Yan, ZHANG Zheng, TONG Wei-Hang, WU Hua, MA Ping, WANG Jing, LIU Li-Hong. Determination of Immunodepressants and Combined Drugs by Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(10): 1573-1578. doi: 10.3724/SP.J.1096.2012.11135 shu

高效液相色谱-质谱联用法检测免疫抑制剂及其合并用药

李鹏飞 ^1, ,
王燕 ^2, ,
张征 ^1, ,
童卫杭 ^2, ,
吴华 ^1, ,
马萍 ^2, ,
王静 ^2, ,
刘丽宏 ^{1,
,}

通讯作者: 刘丽宏

基金项目:
本文系首都医学发展科研基金(No.2007-1016)资助 (No.2007-1016)

摘要: 建立高效液相色谱-质谱联用法同时测定人血浆中免疫抑制剂及合并用药12种药物浓度的方法。选用Kromasil-C₁₈色谱柱(50 mm×4.6 mm×5 μm),以甲醇-乙腈-1 mmol/L乙酸铵溶液为流动相,采用梯度洗脱进行分离,样本用甲醇沉淀蛋白后进样,流速:1.1 mL/min;柱温: 35 ℃;进样量:20 μL。选用3200QTrap型液相色谱-串联质谱仪的多反应监测(MRM)扫描方式进行检测。12种药物的线性范围为0.2-1000 μg/L;定量下限为0.2 μg/L。准确度与精密度结果显示方法日间、日内RSD均小于15%;相对偏差-13%-9.33%,稳定性较好。本方法快速、灵敏,专属性强、重现性好,可用于人体血浆中免疫抑制剂及其常用合并用药共12种药物浓度的测定。

关键词:

English

Determination of Immunodepressants and Combined Drugs by Liquid Chromatography-Tandem Mass Spectrometry

LI Peng-Fei ^1, ,
WANG Yan ^2, ,
ZHANG Zheng ^1, ,
TONG Wei-Hang ^2, ,
WU Hua ^1, ,
MA Ping ^2, ,
WANG Jing ^2, ,
LIU Li-Hong ^{1,
,}

1.
¹ Pharmacy Department of Beijing Chao-Yang Hospital, Beijing 100043, China;

Corresponding author: 刘丽宏

Received Date: 09 October 2011
Fund Project:
本文系首都医学发展科研基金(No.2007-1016)资助

Abstract: This study aims to develop an LC-MS/MS method for the determination of drugs contained immunodepressants and other drugs in human plasma. The drugs and the internal standard were treated by methanol precipitation to remove protein component from human plasma, and then separated on a Kromasil-C₁₈ column (5 μm, 50 mm×4.6 mm) with a gradient elution. The mobile phase consisted of methanol-acetonitrile-1 mmol/L ammonium acetate was maintained at 35 ℃. The flow rate was 1.1 mL/min and 20 μL aliquot of residues was injected into the LC-MS/MS system. Detection was carried out by multiple reaction monitoring on a 3200 QTrap LC-MS/MS system. The assay was linear over the range of 0.2-1000 μg/L with a lower limit of quantitation of 0.2 μg/L. Intra-and inter-day precisions were both less than 15%. The relative deviation was in the range of -13%-9.33%. The stabilities of the method were good. It is a rapid, sensitive, selective and reliable method for the determination of the drugs which contain immunodepressants and other drugs in human plasma. The assay can be applied for the determination of these drugs in human plasma.

Key words:

Liquid chromatography tandem mass spectrometry
/ Immunodepressants
/ Drug combination

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

高效液相色谱-质谱联用法检测免疫抑制剂及其合并用药

通讯作者: 刘丽宏

English

Determination of Immunodepressants and Combined Drugs by Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: 刘丽宏

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高效液相色谱-质谱联用法检测免疫抑制剂及其合并用药

通讯作者: 刘丽宏

English

Determination of Immunodepressants and Combined Drugs by Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: 刘丽宏

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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