【摘要】 目的:建立人血浆中克林霉素浓度的高效液相色谱-质谱法。方法:血浆冷冻干燥后以甲醇提取,进行 HPLC-MS 检测。色谱柱为 Intersil ODS-3（150mm×4.6mm,5μm）,流动相为甲醇-水（40%磷酸调 pH=3.0）（30:70）,流速0.3mL·min^-1,用 HPLC-ESI⁺-MS 法,选择离子检测方式。18名健康志愿者随机分成2组,分别服用供试胶囊和参比胶囊,临床实验方案采用双周期交叉实验设计法。结果:盐酸克林霉素的线性范围为60～10000ng·mL^-1,最低检测浓度为60ng·mL^-1,日内精密度的 RSD<2%,日间精密度的 RSD<3%。用本法测定了18名志愿者随机交叉口服单剂量600mg 后血浆中药物的浓度经时变化过程,并对其药动学参数进行估算。测得的两种胶囊的主要药代动力学参数无显著性差异。结论:该法简便,准确,灵敏度高。可用于盐酸克林霉素的药代动力学研究。更多还原

【Abstract】 Objective:To develop a high performance liquid chromatograph（HPLC）-mass spectrometry（MS） method for the determination of clindamycin hydrochloride in human plasma.Methods:The plasma was extracted with methanol after freeze drying and determined by HPLC-MS.The separation was performed on an Intersil ODS -3（150 nun×4.6 mm,5 μm）.The mobile phase was methanol-water（30:70,pH adjusted to 3 with 40% phos- phoric acid）,and was set at a flow rate of 0.3 mL·min^-1.The analytes were detected by the positive electrospray ionization（ESI⁺）-MS method under selected-ion monitoring（SIM）mode.The plasma concentration of clindamy- cin hydrochloride was determined by this LC-MS method following two formulations given to each 18 volunteers in an open randomized two-way crossover design.Results:The linear range of the plasma concentration of clindamy- cin hydrochloride was 60-10000 ng·mL^-1,and the limit of detection was 60 ng·mL^-1.The RSDs of intra-day and inter-day were less than 2% and 3%,respectively.Conclusions :The method has high sensitivity and good se- lectivity,it can be used for the pharmacokinetic research of clindamycin hydrochloride.更多还原