Paek In Bok, Moon Ya, Ji Hye Young, Kim Hui-Hyun, Lee Hye Won, Lee Yong-Bok, Lee Hye Suk
Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy and Phytofermentation Research Center, Wonkwang University, Shinyongdong, Iksan 570-749, Republic of Korea.
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Oct 5;809(2):345-50. doi: 10.1016/j.jchromb.2004.07.005.
A rapid, sensitive and selective hydrophilic interaction liquid chromatography-tandem mass spectrometric (HILIC-MS/MS) method for the determination of levosulpiride in human plasma was developed. Levosulpiride and internal standard, tiapride were extracted from human plasma with ethyl acetate at pH 11 and analyzed on an Atlantis HILIC silica column with the mobile phase of acetonitrile-ammonium formate (190 mM, pH 3.0) (94:6, v/v). The analytes were detected using an electrospray ionization tandem mass spectrometry in the multiple-reaction-monitoring mode. The standard curve was linear (r = 0.999) over the concentration range of 1.00-200 ng/ml. The lower limit of quantification for levosulpiride was 1.00 ng/ml using 100 microl plasma sample. The coefficient of variation and relative error for intra- and inter-assay at three quality control (QC) levels were 3.8-9.1 and -2.9 to -0.1%, respectively. The recoveries of levosulpiride ranged from 80.5 to 87.4%, with that of tiapride (internal standard) being 84.6%. This method was successfully applied to the pharmacokinetic study of levosulpiride in humans.
建立了一种快速、灵敏且选择性的亲水作用液相色谱-串联质谱法（HILIC-MS/MS）用于测定人血浆中的左舒必利。左舒必利和内标替加色罗在pH 11条件下用乙酸乙酯从人血浆中提取，然后在Atlantis HILIC硅胶柱上进行分析，流动相为乙腈-甲酸铵（190 mM，pH 3.0）（94:6，v/v）。采用电喷雾电离串联质谱在多反应监测模式下检测分析物。标准曲线在1.00 - 200 ng/ml浓度范围内呈线性（r = 0.999）。使用100微升血浆样品时，左舒必利的定量下限为1.00 ng/ml。在三个质量控制（QC）水平下，批内和批间变异系数及相对误差分别为3.8 - 9.1%和 -2.9%至 -0.1%。左舒必利的回收率在80.5%至87.4%之间，替加色罗（内标）的回收率为84.6%。该方法成功应用于左舒必利在人体内的药代动力学研究。
