Division of Clinical Pharmacology, University of Cape Town, Medical School, Observatory, 7925 Cape Town, South Africa.
J Pharm Biomed Anal. 2012 Jan 25;58:177-81. doi: 10.1016/j.jpba.2011.09.030. Epub 2011 Oct 1.
A sensitive and selective liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of ofloxacin in 20 μl human plasma over the concentration range of 0.078-20 μg/ml. Sample preparation was achieved by protein precipitation with acetonitrile and methanol containing the internal standard (Gatifloxacin). Chromatographic separation was achieved on a Luna 5 μm PFP (110 A, 50 × 2 mm) column with acetonitrile and water containing 0.1% formic acid (50:50, v/v) as the mobile phase, at a flow rate of 400 μl/ml. The within-day and between-day precision determinations for ofloxacin, expressed as the percentage coefficient of variation, were lower than 7% at all test concentrations. Recovery of ofloxacin was greater than 70% and reproducible at the low, medium and high end of the dynamic range. No significant matrix effects were observed for the analyte or internal standard. The assay was successfully used to examine the pharmacokinetics of ofloxacin as part of a study to characterize the pharmacokinetics of a number of anti-tuberculosis drugs utilized in the treatment of multi-drug resistant tuberculosis (MDR-TB).
建立并验证了一种灵敏、专属性的液相色谱-串联质谱法，用于测定人血浆中浓度范围为 0.078-20μg/ml 的氧氟沙星。样品制备采用含内标（加替沙星）的乙腈和甲醇进行蛋白沉淀。采用 Luna 5μm PFP（110A，50×2mm）柱进行色谱分离，以含 0.1%甲酸的乙腈和水（50:50，v/v）为流动相，流速为 400μl/ml。在所有测试浓度下，氧氟沙星日内和日间精密度（以变异系数的百分比表示）均低于 7%。在低、中、高浓度范围内，氧氟沙星的回收率大于 70%且重现性良好。分析物和内标均无明显基质效应。该测定法成功用于考察氧氟沙星的药代动力学，作为研究多种用于治疗耐多药结核病（MDR-TB）的抗结核药物药代动力学的一部分。
