College of Pharmacy, Ewha Womans University, Seoul, South Korea.
J Sep Sci. 2012 Sep;35(17):2219-22. doi: 10.1002/jssc.201200367. Epub 2012 Jul 17.
We developed a method for the simultaneous quantification of aceclofenac and its three major metabolites in rat plasma. After protein precipitation with acetonitrile including flufenamic acid as an internal standard (IS), aceclofenac, diclofenac, 4'-hydroxyaceclofenac, 4'-hydroxydiclofenac, and the IS were chromatographed on a reverse-phase C18 analytical column. The isocratic mobile phase of acetonitrile/0.1% formic acid (aq; 9:1 [v/v]) was eluted at 0.3 mL/min. Quantification was performed on a triple-quadrupole mass spectrometer using electrospray ionization, and the ion transitions were monitored in selective reaction-monitoring mode. The coefficient of variation in the assay precision was less than 8%, and the accuracy was 92-103%. This method was successfully used to measure the concentrations of aceclofenac and its three major metabolites in rat plasma following the oral administration of a single 20 mg/kg oral dose of aceclofenac.
我们开发了一种同时定量测定大鼠血浆中醋氯芬酸及其三种主要代谢物的方法。采用含氟芬那酸（作为内标，IS）的乙腈进行蛋白沉淀后，醋氯芬酸、双氯芬酸、4'-羟基醋氯芬酸、4'-羟基双氯芬酸和 IS 在反相 C18 分析柱上进行色谱分离。以乙腈/0.1%甲酸（水）（9:1[v/v]）为等度流动相，流速为 0.3 mL/min。采用电喷雾电离源，在选择反应监测模式下进行三重四极杆质谱检测。该测定方法的精密度变异系数小于 8%，准确度为 92-103%。该方法成功用于测定大鼠口服单剂量 20mg/kg 醋氯芬酸后血浆中醋氯芬酸及其三种主要代谢物的浓度。
