摘要
目的 建立超高效液相色谱串联质谱测定人全血中羟氯喹浓度的方法.方法 全血样品经乙腈蛋白沉淀后,上清液采用超高效液相色谱串联质谱仪测定.色谱柱为ACQUITY UPLCHSS T3色谱柱(2.1 ×50 mm,1.8 μm),流动相A为含0.3％甲酸、3 mmol·L-1甲酸铵的水溶液,流动相B为含0.3％甲酸、3 mmol·L-1甲酸铵的乙腈∶甲醇∶水(V∶V∶V,95∶95∶10)混合溶液,进行梯度洗脱,总流速为0.30 mL·min-1,使用电喷雾正离子模式,多反应离子监测.结果 在 1～500ng·mL-1范围内,羟氯喹具有良好的线性关系,批内、批间RSD均小于10％.结论 本试验所建立的分析方法准确、灵敏、方便,可用于羟氯喹的人体药动学研究.
Abstract
OBJECTIVE To establish the determination method of hydroxychloroquine in human whole blood with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).METHODS Whole blood samples were precipitated by acetonitrile,then the supernatant was determinated by UPLC-MS/MS.Column ACQUITY UPLCHSS T3(2.1 ×50 mm,1.8 μm)was used with mobile phase A of water(containing 0.3％formic and 3 mmol·L-1 ammonium formate)and mobile phase B of acetonitrile∶methanol∶water(V∶V∶V,95∶95∶10)(con-taining 0.3％formic and 3 mmol·L-1ammonium formate),with the gradient elution at a flow rate of 0.30 mL·min-1.Electrospray positive ion model and multiple reaction monitoring were used.RESULTS There was a good linerrelationship in the calibration curve of 1-500 ng·mL-1 for hydroxychloroquine,and the intra-day and inter-day relative standard deviations were less than 10％.CONCLUSION The UPLC-MS/MS method was accuracy,sensi-tive and simple,and can be applied to a pharmacokinetics of hydroxychloroquine in human.
维普
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