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液相色谱-电喷雾电离串联质谱法测定人血浆中的氯诺昔康

Liquid chromatography-electrospray ionization tandem mass spectrometric determination of lornoxicam in human plasma.

作者信息

Kim Young Hoon, Ji Hye Young, Park Eun-Seok, Chae Soo-Wan, Lee Hye Suk

机构信息

Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy, Wonkwang University, Iksan 570-749, Korea.

出版信息

Arch Pharm Res. 2007 Jul;30(7):905-10. doi: 10.1007/BF02978844.

Abstract

A rapid, sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometric (LC-ESI-MS/MS) method for the determination of lornoxicam in human plasma was developed. Lornoxicam and isoxicam (internal standard) were extracted from human plasma with ethyl acetate at acidic pH and analyzed on a Sunfire C18 column with the mobile phase of methanol:ammonium formate (10 mM, pH 3.0) (70:30, v/v). The analyte was detected using a mass spectrometer, equipped with electrospray ion source. The instrument was set in the multiple-reaction-monitoring mode. The standard curve was linear (r = 0.9998) over the concentration range of 0.50-500 ng/mL. The coefficient of variation and relative error for intra- and inter-assay at four QC levels were 0.7 to 4.2% and -4.5 to 5.0%, respectively. The recoveries of lornoxicam and isoxicam were 87.8% and 66.5%, respectively. The lower limit of quantification for lornoxicam was 0.50 ng/mL using a 200 pL plasma sample. This method was successfully applied to a pharmacokinetic study of lornoxicam after oral administration of lornoxicam (8 mg) to humans.

摘要

建立了一种快速、灵敏且选择性好的液相色谱-电喷雾电离串联质谱法(LC-ESI-MS/MS)用于测定人血浆中的氯诺昔康。氯诺昔康和异昔康(内标)在酸性pH条件下用乙酸乙酯从人血浆中萃取,并在Sunfire C18柱上进行分析,流动相为甲醇:甲酸铵(10 mM,pH 3.0)(70:30,v/v)。使用配备电喷雾离子源的质谱仪检测分析物。仪器设置为多反应监测模式。在0.50 - 500 ng/mL的浓度范围内,标准曲线呈线性(r = 0.9998)。四个质量控制水平下批内和批间的变异系数和相对误差分别为0.7%至4.2%和 -4.5%至5.0%。氯诺昔康和异昔康的回收率分别为87.8%和66.5%。使用200 pL血浆样品时,氯诺昔康的定量下限为0.50 ng/mL。该方法成功应用于人体口服氯诺昔康(8 mg)后的药代动力学研究。

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