Roy Bikash, Choudhury Hira, Das Ayan, Das Anjan Kumar, Pal Tapan Kumar
Bioequivalence Study Centre, Department of Pharmaceutical Technology, Jadavpur University, Kolkata-700032, India.
Biomed Chromatogr. 2011 Aug;25(8):890-901. doi: 10.1002/bmc.1539. Epub 2010 Dec 10.
A simple, high-throughput and specific high-performance liquid chromatography-tandem mass spectrometry method has been developed and validated according to the FDA guidelines for quantification of ulifloxacin in rat and rabbit plasma. The analyte was separated on a Peerless basic C(18) column (33 × 4.6 mm, 3 µm) with an isocratic mobile phase of methanol-water containing formic acid (0.5%, v/v; 9:1, v/v) at a flow rate of 0.5 mL/min. The MS/MS detection was carried out by monitoring the fragmentation of m/z 350.500 → 248.500 for ulifloxacin and m/z 332.400 → 231.400 for ciprofloxacin (internal standard; IS) on a triple quadrupole mass spectrometer. The response to ulifloxacin was linear over the range 0.010-2.500 µg/mL in both plasma. The limit of detection and lower limit of quantification of ulifloxacin were determined in both species to be 0.0025 and 0.010 µg/mL, respectively. The method was successfully applied to quantitatively assess the toxicokinetics of ulifloxacin in rat and rabbit following a single 400 mg/kg (in rat) and 200 mg/kg (in rabbit) oral dose of the prulifloxacin.
根据美国食品药品监督管理局（FDA）的指导方针，已开发并验证了一种简单、高通量且特异的高效液相色谱-串联质谱法，用于定量测定大鼠和兔血浆中的乌利沙星。分析物在一款Peerless basic C(18)柱（33×4.6 mm，3 µm）上分离，流动相为含甲酸（0.5%，v/v；9:1，v/v）的甲醇-水等度洗脱液，流速为0.5 mL/min。在三重四极杆质谱仪上，通过监测乌利沙星的m/z 350.500→248.500和环丙沙星（内标；IS）的m/z 332.400→231.400的碎片进行MS/MS检测。在两种血浆中，乌利沙星的响应在0.010 - 2.500 µg/mL范围内呈线性。在两种动物中，乌利沙星的检测限和定量下限分别确定为0.0025和0.010 µg/mL。该方法成功应用于定量评估大鼠和兔单次口服400 mg/kg（大鼠）和200 mg/kg（兔）普卢利沙星后乌利沙星的毒代动力学。
