血浆中对乙酰氨基酚测定的LC-MS/MS法

Rapid determination of acetaminophen in plasma by LC-MS/MS

目的建立一种快速测定人血浆中对乙酰氨基酚(APAP)含量的液相色谱-串联质谱(LC-MS/MS)方法。方法血浆样品经甲醇-乙腈溶液(V/V, 1∶1)沉淀蛋白后, 以甲醇(5 mmol/L乙酸铵)-水(5 mmol/L乙酸铵)为流动相, 经C18色谱柱分离。采用LC-MS/MS电喷雾正离子多反应监测(MRM)模式进行定性定量分析。结果本方法在0~10 mg/L范围内线性良好, 相关系数(r)>0.999 0, 批间、批内精密度均<10%, 加标回收率为96.8%~101.7%, 检出限为0.1 mg/L, 定量下限为0.3 mg/L。结论本方法特异性强, 灵敏度高, 测定结果可靠, 适用于临床血浆样品的快速分析。

Objective To establish a method for the rapid determination of acetaminophen(APAP)in human plasma by LC-MS/MS.Methods The plasma samples were extracted by methanol and acetonitrile(1:1)and purified directly.Cis column was used for sample separation.The mobile phase were methanol(5 mmol/L ammonium acetate)and water(5 mmol/L ammonium acetate).Samples were analyzed by LC MS/MS with the electrospray ionization multi reaction monitoring(MRM)mode.Results The calibration curves of APAP was linear in the concentration range of 0~10 mg/L,the correlation coefficient(r)was greater than 0.9990.The relative standard deviation within and between batches was less than 10%.The recovery rate were 96.81%~101.7%.The detection limit of the method was 0.1μg/L and the lower limit of quantification was 0.3μg/L.Conclusion This method has strong specificity,high sensitivity and reliable determination results.It is suitable for the rapid analysis of clinical plasma samples.