9-芴甲氧羰酰氯柱前衍生高效液相色谱法测定克拉霉素血药浓度

目的 采用柱前衍生高效液相色谱法测定克拉霉素血药浓度.方法 克拉霉素血浆样品以正己烷-正丁醇混合溶液萃取后,与9-芴甲氧羰酰氯（FMOC-CL）衍生化后进样.色谱柱为Hypersil TMODS2柱（4.6mm×250mm,5μm）,柱温：62℃;流动相：0.05mol/L NH4H2PO4缓冲液（PH6.72）-乙腈=38：62 （v/v）,流速2.5 mL/min;激发波长：265nm,发射波长：315nm.结果 克拉霉素血药浓度在50～3000ng/mL范围内,浓度与峰面积比有良好的线性关系,最低检测浓度为30ng/mL,平均回收率为97.9～100.2％,日内RSD≤4.1％,日间RSD≤6.8％.结论 本方法简单、快速、准确,可用于克拉霉素临床药动学研究.

Determination of Clarithromycin in Human Plasma by HPLC with Pre-column Derivatization FMOC-CL

Objective To establish a HPLC method with pre-column derivatization to measure the plasma concentration of clarithromycin. Methods A n-hexane and n-butanol extract of plasma was treated with FMOC-CL and chromatographed on a HypersilTM ODS2 column （4.6mm×250mm, 5μm） using an eluent composed of acetonitrile- 0.05mol/L phosphate buffer （PH6.72） （62：38）. The column temperature was at 62~C and flow rate of eluent was 2.5mL/min. The exciation and emission wavelength were 265nm and 315nm, respectively. Results The assay procedure was shown to produce linear calibration curves over the range 50ng/mL to 3000ng/mL of clarithromycin in plasma. The limit of detection was 30ng/mL. The recovery rate was 97.9～100.2%. The coefficients of variation within a day and between days did not exceed 4.1%, 6.8%, respectively. Conclusion This method is found to be easy, convenient and precise for clinical pharmacokinetics study of clarithromycin.