Department of Analytical Chemistry, Shenyang Pharmaceutical University, 103# Wenhua Road, Shenyang 110016, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Mar 1;878(7-8):689-94. doi: 10.1016/j.jchromb.2010.01.007. Epub 2010 Jan 18.
A rapid, selective and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed to simultaneously determine venlafaxine (VEN) and O-desmethylvenlafaxine (ODV) in human plasma. Sample pretreatment involved a one-step extraction with diethyl ether of 0.5 mL plasma. The separation was carried out on an ACQUITY UPLC BEH C(18) column with 10 mmol/L ammonium acetate and methanol as the mobile phase at a flow rate of 0.30 mL/min. The detection was performed on a triple-quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source. The linear calibration curves for VEN and ODV were both obtained in the concentration range of 0.200-200 ng/mL (r(2)> or =0.99) with the lower limit of quantification (LLOQ) of 0.200 ng/mL. The intra- and inter-day precision (relative standard deviation, R.S.D.) values were less than 13% and the accuracy (relative error, R.E.) was within +/-5.3% and +/-3.6% for VEN and ODV. The method herein described was superior to previous methods in sensitivity and sample throughput and successfully applied to clinical pharmacokinetic study of venlafaxine sustained-release capsule in healthy male volunteers after oral administration.
建立了一种同时测定人血浆中文拉法辛（VEN）和 O-去甲文拉法辛（ODV）的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。样品预处理采用一步乙醚提取 0.5 mL 血浆。采用 ACQUITY UPLC BEH C18 柱，以 10 mmol/L 乙酸铵和甲醇为流动相，流速为 0.30 mL/min，进行分离。采用电喷雾离子源（ESI），以多反应监测（MRM）模式进行检测。VEN 和 ODV 的线性校准曲线范围均为 0.200-200 ng/mL（r（2）≥0.99），定量下限（LLOQ）为 0.200 ng/mL。VEN 和 ODV 的日内和日间精密度（相对标准偏差，RSD）均小于 13%，准确度（相对误差，RE）在±5.3%和±3.6%范围内。与以往方法相比，该方法具有更高的灵敏度和样品通量，成功应用于健康男性志愿者口服文拉法辛缓释胶囊后的临床药代动力学研究。
