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目的建立测定人全血中羟氯喹浓度的液相色谱-串联质谱(LC-MS/MS)法。方法全血样品经特丁基甲醚提取,采用同位素内标(氘4-羟氯喹)进行测定。以Thermo Syncronis C18(50 mm×2.1 mm,5μm)为色谱柱,流动相A为含10 mmol·L-1乙酸铵、0.1%甲酸的10%乙腈水溶液,流动相B为95%乙腈水溶液,梯度洗脱,洗脱条件为0~1.2 min:0%B,1.3~2.3min:100%B;2.4~5.5 min:0%B,流速为0.4 m L·min-1。电喷雾离子源,正离子MRM扫描分析。结果羟氯喹血浓度测定的线性范围为1~500μg·L-1,定量下限为1μg·L-1,批内、批间RSD均<9%,提取回收率57.6%~69.2%。结论本方法灵敏度高、专属性好,可检测人全血中羟氯喹的浓度,并用于羟氯喹的药动学研究。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for determination of hydroxychloroquine in human whole blood. Methods Whole blood samples were extracted with tert-butyl methyl ether and subjected to isotope internal standard (deuterium 4-hydroxychloroquine). On a Thermo Syncronis C18 (50 mm × 2.1 mm, 5 μm) column, mobile phase A was a 10% acetonitrile in water containing 10 mmol·L -1 ammonium acetate, 0.1% formic acid and 95% acetonitrile in water. The gradient The elution conditions were 0-1.2 min: 0% B, 1.3-2.3 min: 100% B; 2.4-5.5 min: 0% B at a flow rate of 0.4 m L · min-1. Electrospray ionization, positive ion MRM scan analysis. Results The linear range of hydroxychloroquine concentration was 1 ~ 500μg · L-1, and the lower limit of quantification was 1μg · L-1. The RSDs within and between batches were all less than 9% and the recovery rates were between 57.6% and 69.2%. Conclusion The method is sensitive and specific, and can detect the concentration of hydroxychloroquine in human whole blood and is used to study the pharmacokinetics of hydroxychloroquine.