Ji Hye Young, Park Eun Jeong, Lee Kang Choon, Lee Hye Suk
Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy, Wonkwang University, Iksan, Republic of Korea.
J Sep Sci. 2008 May;31(9):1628-33. doi: 10.1002/jssc.200700662.
Hydrophilic interaction LC with MS/MS (HILIC-MS/MS) was described as a rapid, sensitive, and selective method for the quantification of doxazosin in human plasma. Doxazosin and cisapride (internal standard) were extracted from human plasma with ethyl acetate at alkaline pH and analyzed on an Atlantis HILIC Silica column with the mobile phase of ACN/ammonium formate (100 mM, pH 4.5) (93:7 v/v). The analytes were detected using an ESI MS/MS in the selective-reaction-monitoring mode. The standard curve was linear (r = 0.9994) over the concentration range of 0.2-50 ng/mL. The LOQ for doxazosin was 0.2 ng/mL using 100 microL plasma sample. The CV and relative error for intra- and interassay at four QC levels were 3.7-8.7% and 0.0-9.8%, respectively. The matrix effect for doxazosin and cisapride were practically absent. The recoveries of doxazosin and cisapride were 67.4 and 61.7%, respectively. This method was successfully applied to the pharmacokinetic study of doxazosin in humans.
亲水作用液相色谱-串联质谱法（HILIC-MS/MS）被描述为一种快速、灵敏且具有选择性的定量人血浆中多沙唑嗪的方法。多沙唑嗪和顺阿曲库铵（内标）在碱性pH条件下用乙酸乙酯从人血浆中提取，并在Atlantis HILIC硅胶柱上进行分析，流动相为乙腈/甲酸铵（100 mM，pH 4.5）（93:7 v/v）。使用电喷雾串联质谱仪在选择性反应监测模式下检测分析物。在0.2 - 50 ng/mL的浓度范围内，标准曲线呈线性（r = 0.9994）。使用100 μL血浆样本时，多沙唑嗪的定量下限为0.2 ng/mL。四个质量控制水平下的批内和批间变异系数及相对误差分别为3.7 - 8.7%和0.0 - 9.8%。多沙唑嗪和顺阿曲库铵的基质效应几乎不存在。多沙唑嗪和顺阿曲库铵的回收率分别为67.4%和61.7%。该方法成功应用于多沙唑嗪在人体内的药代动力学研究。
