高效液相色谱法测定人血浆中扎来普隆的浓度

Determination of zaleplon in blood plasma by RP-HPLC with fluorescence detection

目的 :建立测定人血浆中扎来普隆浓度的高效液相色谱法。方法 :以美国迪马公司钻石C1 8反相柱 ( 15 0mm× 4.6mm ,5μm)为色谱柱 ,流动相为 ψ(乙腈 ∶冰乙酸∶三乙胺 ∶水 ) =5 0 ∶ 0 .2 5∶ 0 .0 2 5 ∶49.72 5 ,流速为 1.0mL/min ,荧光激发波长 3 45nm ,发射波长 460nm ,以乙酸乙酯为提取剂。结果 :扎来普隆高 ( 10 0 .0ng/mL)、中 ( 5 0 .0ng/mL)、低 ( 5 .0ng/mL)三种浓度的平均回收率分别为 96.9%、95 .4%、96.0 %,日内、日间差RSD均低于 8%;分析方法的最低检测浓度为 0 .5ng/mL。线性范围为 :1.0～ 10 0 .0ng/mL。结论 :该方法灵敏、准确、简单、快速 ,可用于临床血浓监测和药动学研究。

Objective:To develop an HPLC method for quantitative determination of zaleplon in blood plasma . Methods: Blood plasma samples were extracted with hexane to remove lipid and interfering substances,then extracted with ethyl acetate. The residue was analyzed with a reverse phase HPLC system (C 18 column,4.6 mm × 150 mm,5μm; Mobile phase, ψ (MeOH ∶acetic acid∶riethylamine∶H 2O )=50∶0.25∶0.025∶ 49.725; fluorescence detection was conducted with excitation at 345 nm and emission at 460 nm) . Results:The average recoveries for three concentration of zaleplon (100.0 ng/mL,50.0ng/mL,and 5.0 ng/mL) were 96.9%,95.4% and 96.0%,respectively. The within day and day to day relative standard deviations were lower than 8%. The calibration curves had good linearity (r = 0.9999) within a concentration range of 1.0～100.0 ng/mL . The limit of quantitation for zaleplon was 0.5 ng/mL . Conclusions:The method provides a sensitive,accurate,and reliable analytical procedure for clinical monitoring of zaleplon blood plasma and its phamacokinetic studies.