顶空-气相色谱-串联质谱法测定血浆中甲醇含量

目的 建立测定血浆中甲醇含量的顶空-气相色谱-串联质谱法。方法 设计L₉(3⁴)正交实验对顶空条件进行优化,样品在选择反应监测模式下检测,外标法定量。结果 通过正交实验,确定最优顶空条件为平衡温度80 ℃、平衡时间30 min、盐析剂1.5 g MgSO₄。该方法的线性范围为1.0～80 mg/L,线性方程为Y=82 670X+45 930,r=0.9998,检出限为0.2 mg/L,样品加标回收率为80.9%～90.5%,精密度为2.7%～3.3%。结论 本方法前处理简单、灵敏、准确,可用于血浆中甲醇含量的快速检测。

Determination of methanol in plasma by headspace gas chromatography-mass spectrometry

Objective To establish a headspace gas chromatography-mass spectrometry(HS-GC-MS/MS)method to determine methanol in plasma.Methods We designed a L9(34)orthogonal experiment to optimize the process conditions of headspace.Samples were determined in the selected reaction monitoring mode,and external standard method was used in the quantification.Results Through the orthogonal experiment,the optimum headspace conditions were determined as follows:equilibrium temperature 80℃,equilibrium time 30 min and salting-out agent 1.5 g MgSO4.The linear range of the method was 1.0 mg/L-80 mg/L.The linear equation was as follows:Y=82670X+45930,r=0.9998.The detection limit of the method was 0.2 mg/L.The recovery rates ranged from 80.9%to 90.5%,and the precision was between 2.7%and 3.3%.Conclusions The sample pre-processing of the established method is simple,sensitive and accurate,and it can be applied to the rapid determination of methanol in plasma.