Simultaneous determination of cortisol, dexamethasone, methylprednisolone, prednisone, prednisolone, mycophenolic acid and mycophenolic acid glucuronide, in human plasma utilizing liquid chromatography-tandem mass spectrometry
Simultaneous determination of cortisol, dexamethasone, methylprednisolone, prednisone, prednisolone, mycophenolic acid and mycophenolic acid glucuronide, in human plasma utilizing liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/j.jchromb.2007.09.003
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发表时间：
2007-11-01
影响因子：
3
通讯作者：
Tornatore, Kathleen M.
中科院分区：
文献类型：
--
作者：
DiFrancesco, Robin;Frerichs, Valerie;Tornatore, Kathleen M.
慢性联合免疫抑制方案通常用于肾移植受者。为了建立一种用于多种免疫抑制剂药代动力学研究和治疗药物监测的分析方法，研究了同时分析几种糖皮质激素麦考酚酸（MPA）和麦考酚酸葡糖苷酸（MPAG）的液相色谱-串联质谱（LC/MS/MS）方法。所得方法利用在pH 3.5下使用乙酸铵-甲醇移动的相的Symmetry C18柱上的梯度反相分离。通过电喷雾将色谱系统耦合到三重四极杆质谱仪来检测分析物。负离子多反应监测使用（MH-/产物），选择MPA为319.1/190.9，MPAG为495.1/191.0，地塞米松为391.0/361.0，氢化可的松为361.1/331.1，甲泼尼龙为373.1/343.1，泼尼松为357.1/327.2，泼尼松龙组为359.1/329.1。校准曲线浓度范围为3.60 ng/mL至50 μ g/mL，皮质类固醇的最低定量限分别为3.60-7.20 ng/mL和0.656-6.75 μ g/mL（MPA和MPAG）。所有分析物的质控品日内变异和日间变异的相对标准偏差在0.76%和9.57%之间。该检测试剂盒为联合免疫抑制期间的多分析物免疫抑制测定提供了一种通用、独特的方法。(C)2007 Elsevier B. V.保留所有权利。
Chronic combination immunosuppressive regimens are commonly prescribed to renal transplant recipients. To develop an assay method for pharmacokinetic studies and therapeutic drug monitoring of multiple inummosuppressives, a liquid chromatography-tandem mass spectrometry (LC/MS/MS) approach for the simultaneous analysis of several glucocorticoids, mycophenolic acid (MPA) and mycophenolic acid glucuronide (MPAG) was investigated. The resultant method utilized a gradient reverse phase separation over a Symmetry C 18 column using an ammonium acetate-methanol mobile phase at pH 3.5. The analytes were detected by coupling the chromatography system via electrospray to a triple quadrupole mass spectrometer. Multiple-reaction monitoring in the negative mode ion (MH-/product) was employed selecting MPA at 319.1/190.9, MPAG at 495.1/191.0, dexamethasone at 391.0/361.0, hydrocortisone at 361.1/331.1, methylprednisolone at 373.1/343.1, prednisone at 357.1/327.2, and prednisolone at 359.1/329.1. The calibration curve concentrations ranged from 3.60 ng/mL to 50 mu g/mL with the lowest limit of quantitation for corticosteroids being 3.60-7.20 ng/mL and 0.656-6.75 mu g/mL for MPA and MPAG, respectively. The relative standard deviation for quality control intraday variation and interday variation was between 0.76% and 9.57% for all analytes. This assay offers a versatile, unique method for multi-analyte immunosuppressive determinations during combination immunosuppression. (C) 2007 Elsevier B.V. All rights reserved.