LC-MS／MS同时测定人血浆中对乙酰氨基酚和右氯苯那敏浓度

目的高效液相色谱·串联质谱联用法（LC—MS／MS）同时测定人血浆中对乙酰氨基酚和右氯苯那敏浓度。方法样品用甲醇进行沉淀蛋白后进样，Zorbax Eclipse TC—C18色谱柱，以甲醇旬．1％甲酸的1mmol·L^-1甲酸铵溶液，采用梯度洗脱进行分离，3200QTRAP型质谱仪的多重反应监测（MRM）扫描方式进行检测。结果对乙酰氨基酚线性范围为：0．05-20μg·mL^-1，定量下限为0．05μg·mL^-1，准确度与精密度结果显示对乙酰氨基酚日间、日内RSD均≤5．50％，相对偏差一8．08％～5．73％，方法提取回收率92．0％～99．0％，稳定性测定值与添加值的相对偏差均〈15％；右氯苯那敏线性范围为：0．05～20ng·mL^-1，定量下限为0．05ng·mL^-1，准确度与精密度结果显示右氯苯那敏日间、日内RSD均≤13．71％，相对偏差-1．29％～1．71％，方法提取回收率89．8％～101．4％，稳定性测定值与添加值的相对偏差均〈15％。结论本研究所建立的方法快速、灵敏、专属性强、重复性高，可用于同时测定人血浆中对乙酰氨基酚和右氯苯那敏浓度。

Simultaneous Determination of Paracetamol and Dextrochlorpheniramine in Human Plasma by LC-MS/MS

Aim To develop an LC-MS/MS method for simultaneous determination of paracetamol and dextrochlorpheniramine in human plasma. Methods Paracetamol, dextrochlorpheniramine and the internal standard were extracted from plasma by methanol which was used as a deproteinated solvent, and separated on a Zorbax Eclipse TC-C18 column using methanol and 1 mmol·L^-1 ammonium formate （containing 0. 1% formic acid） as the mobile phase by gradient elution. Detection was carried out by multiple reaction monitoring on a 3200QTRAP LC-MS/MS system. Results The assay for paracetamol was linear over the range 0.05 - 20.0μg·mL^-1 with a limit of quantitation of 0.05μg·mL^-1. Intra- and inter-day precision was less than 5.5%. The relative deviation was in the range - 8.08% - 5.73%. The recovery of paracetamol was 92.0% - 99.0% and relative deviation of stability was less than 15%. The assay for dextrochlorpheniramine was linear over the range 0.05 -20.0ng·mL^-1 with a limit of quantitation of 0.05ng·mL^-1. Intra- and inter-day precision was less than 13.71%. The relative deviation was in the range - 1.29% - 1.71%. The recovery of paracetamol was 89.8% - 101.4% and relative deviation of stability was less than 15%. Conclusion The method we found was a rapid, sensitive, selective and reliable method for the simultaneous determination of paracetamol and dextrochlorpheniramine in human plasma. The assay was applied to a pharmacokinetic study on healthy volunteers.