摘要
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-0.1%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-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。
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.
出处
《解放军药学学报》
CAS
2009年第1期33-37,共5页
Pharmaceutical Journal of Chinese People's Liberation Army
