LC-MS/MS法测定大鼠血浆中青蒿素与羟氯喹
Traditional Chinese Drug Research and Clinical Pharmacology(2018)
Abstract
目的 建立一种快速可靠地测定大鼠血浆中青蒿素和羟氯喹浓度的LC-MS/MS法.方法 青蒿素用液-液萃取法提取,采用Synergi Hydro-RP C18柱(30 mm×2.0 mm,4μm,80?)分析;羟氯喹用蛋白沉淀法提取,采用Agilent Zorbax Bonus-RP柱(100 mm×4.6 mm,3.5μm,80?)分析;两者均以0.6%甲酸甲醇和5 mmol·L-1醋酸铵水溶液为流动相进行梯度洗脱,流速0.6 mL·min-1.质谱采用电喷雾电离(ESI)源,正离子扫描,多反应监测(MRM)方式进行检测.结果青蒿素在0.4~1000 ng·mL-1,羟氯喹在1~1000 ng·mL-1范围内线性关系良好(r>0.995);青蒿素与羟氯喹的批内、批间精密度和准确度均符合生物样品分析的相关要求;两者提取回收率分别为67.2%~77.0%和73.5%~81.3%.结论 该方法快速灵敏、 准确可靠, 可用于大鼠血浆中青蒿素和羟氯喹浓度的测定.
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Key words
Artemisinin,hydroxychloroquine,LC-MS/MS
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