UPLC-MS/MS法同时检测血液中15种常见安眠镇静药物

Simultaneous Determination of 15 Soporific and Sedative Drugs in Blood by UPLC-MS/MS

建立一种超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)同时检验血液中15种常见安眠镇静药物的方法。采用快速便捷的乙腈沉淀蛋白法提取血液中安眠镇静药物,通过Acquity BEH C18(2.1 mm×100 mm,1.7μm)色谱柱分离,电喷雾离子源正离子模式(ESI+)下,多反应监控(MRM)模式检测。结果表明,血液中15种常见安眠镇静药物检出限在0.08ng/mL~0.29ng/mL之间,定量限在0.25 ng/m~0.96ng/mL之间;在1 ng/m~50 ng/mL范围内线性关系良好,R2均大于0.9979;在低、中、高(2 ng/mL、10ng/mL、50 ng/mL)三种添加浓度中基质效应在81.06%~100.72%之间,提取回收率在76.86%~102.0%之间,日内、日间精密度RSD均不大于7.68%。本方法专属性好、灵敏度高、准确性好,可用于快速检验血液中15种常见安眠镇静药物。

To establish a method for the simultaneous determination of 15 soporific and sedative drugs in blood by ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS).The sedative drugs in the blood were extracted by a rapid and convenient acetonitrile precipitation protein method,separated by an Acquity BEH C18(2.1 mm×100 mm,1.7μm)chromatographic column,and detected by multiple reaction monitoring(MRM)mode under electrospray ion source positive ion mode(ESI+).The results showed that the detection limits of 15 hypnotic sedative drugs in blood were between 0.08 ng/mL~0.29 ng/mL,and the quantitative limits were between 0.25 ng/mL~0.96 ng/mL;The linear relationship was good in the range of 1 ng/mL~50 ng/mL,and R2 was greater than 0.9979;In the low,medium and high(2 ng/mL,10 ng/mL,50 ng/mL)concentrations,the matrix effect was between 81.06%~100.72%,the extraction recovery was between 76.86%~102.0%,and the intra-day and inter-day precision RSD were not more than 7.68%.The method has good specificity,high sensitivity and good accuracy,and can be used for rapid detection of 15 soporific and sedative drugs.