Laboratory of Pharmacology and Toxicology, University Hospital, Saint-Etienne, France.
J Sep Sci. 2010 Jul;33(13):1968-72. doi: 10.1002/jssc.201000115.
A sensible ultra-performance LC-MS method was developed and validated for the quantification of clopidogrel active metabolite in human plasma, with clopidogrel D4 as internal standard. Plasma pretreatment involved a one-step protein precipitation with acetonitrile. The separation was performed by reverse-phase chromatography on a C8 column. The method was linear over the concentration range of 1-150 ng/mL. The intra- and inter-day precision values were below 17% and accuracy was from 1.7 to 7.5% at all quality control levels. The lower LOQ was 0.8 ng/mL. Sample analysis time was reduced to 5 min including sample preparation (limited to protein precipitation). The present method was successfully applied to a clopidogrel active metabolite pharmacokinetic study following oral administration to healthy volunteers.
建立并验证了灵敏的超高效液相色谱-串联质谱法，用于人血浆中氯吡格雷活性代谢物的定量分析，以氯吡格雷 D4 为内标。血浆预处理采用乙腈一步蛋白沉淀法。采用 C8 柱进行反相色谱分离。该方法在 1-150ng/mL 浓度范围内呈线性。所有质控水平的日内和日间精密度值均低于 17%，准确度为 1.7-7.5%。较低的定量下限为 0.8ng/mL。包括样品制备（仅限于蛋白沉淀）在内，样品分析时间缩短至 5 分钟。本方法成功应用于健康志愿者口服氯吡格雷活性代谢物的药代动力学研究。
