Prakash Katakam, Adiki Shanta K, Kalakuntla Rama Rao
Nirmala College of Pharmacy, Mangalagiri, Guntur 522503, AP, India.
Department of Biotechnology, Acharya Nagarjuna University, Guntur, AP, India.
Sci Pharm. 2014 Mar 26;82(3):571-83. doi: 10.3797/scipharm.1402-19. Print 2014 Jul-Sep.
A selective and sensitive liquid chromatography-tandem mass spectrometric method (LC-MS/MS) has been developed and validated for the quantification of zileuton in human plasma. Deuterated internal standard (zileuton D4) was used as the internal standard (ISTD). Zileuton was extracted by liquid-liquid extraction using methyl tert-butyl ether and separated by isocratic elution on a C18 column (100 × 4.6 mm, 5 μm, Discovery C18) with the mobile phase consisting of 1 mM ammonium acetate buffer and methanol in the ratio of 10:90. A flow rate of 1.0 ml/min was used with isocratic elution. Multiple reaction monitoring transitions in positive mode for zileuton and the internal standard were 237.3/161.2 and 241.2/161.1, respectively. The method was validated within the linearity range of 50.5-10,012.7 ng/ml for the bioanalytical method validation parameters like selectivity, accuracy, precision, recovery, stability, and matrix effect.
已开发并验证了一种选择性和灵敏的液相色谱-串联质谱法（LC-MS/MS），用于定量测定人血浆中的齐留通。使用氘代内标（齐留通D4）作为内标（ISTD）。齐留通通过液-液萃取法，用甲基叔丁基醚进行萃取，并在C18柱（100×4.6 mm，5μm，Discovery C18）上通过等度洗脱进行分离，流动相由1 mM醋酸铵缓冲液和甲醇按10:90的比例组成。等度洗脱时流速为1.0 ml/min。齐留通和内标的正模式下的多反应监测跃迁分别为237.3/161.2和241.2/161.1。该方法在50.5-10,012.7 ng/ml的线性范围内针对选择性、准确性、精密度、回收率、稳定性和基质效应等生物分析方法验证参数进行了验证。
