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目的建立快速测定人尿中美沙酮的超高效液相色谱串联质谱测定方法。方法尿样采用0.10 mol/L氢氧化钠溶液碱化后,经乙醚漩涡提取、离心,吸取上清液浓缩吹干,用80%甲醇定容后进液相色谱-质谱系统分析,同位素内标法定量。色谱柱采用Waters ACQUITY UPLC BEH C18柱(2.1 mm×100 mm,1.7μm),流动相为乙腈-0.1%甲酸,流速为0.4 ml/min,柱温为35℃,进行梯度洗脱;质谱采用电喷雾离子源,在正离子多反应监测模式(MRM)下进行检测。结果美沙酮在1 ng/ml~100 ng/ml时线性关系良好(r>0.999);检测限(LOD)和定量限(LOQ)分别为0.003 mg/L和0.01 mg/L;低、中、高3个浓度(2 ng/ml、10 ng/ml、50 ng/ml)的回收率分别为99.8%、100.1%、100.3%,精密度(RSD)分别为1.51%、2.72%、2.25%。结论该方法简便、灵敏、准确、稳定,适用于人尿中美沙酮的测定,可满足美沙酮临床研究尿样监测的要求。
OBJECTIVE To establish a method for the rapid determination of methadone in human urine by ultra performance liquid chromatography-tandem mass spectrometry. Methods Urine samples were alkalized with 0.10 mol / L sodium hydroxide solution, extracted by ether vortex and centrifuged. The supernatant was concentrated and dried. The samples were determined by liquid chromatography - mass spectrometry with 80% methanol and isotope internal standard method Quantitative. The column was eluted with a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) using a mobile phase of acetonitrile-0.1% formic acid at a flow rate of 0.4 ml / min and a column temperature of 35 ° C. Spray ion source for detection in positive ion multiple reaction monitoring mode (MRM). Results The linear range of methadone was between 1 ng / ml and 100 ng / ml (r> 0.999). The limit of detection (LOD) and limit of quantification (LOQ) were 0.003 mg / L and 0.01 mg / The recoveries of three concentrations (2 ng / ml, 10 ng / ml and 50 ng / ml) were 99.8%, 100.1% and 100.3%, respectively. The RSDs were 1.51%, 2.72% and 2.25%, respectively. Conclusion The method is simple, sensitive, accurate and stable. It is suitable for the determination of methadone in human urine, and can meet the requirements of urine sample monitoring in clinical research of methadone.