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采用GC-MS/SIM联用技术,结合固相萃取柱浓缩净化法,以目标化合物β-苯乙醇特征碎片离子m/z 91为定量离子,m/z 122分子离子为定性离子,采用“Xcalibur”软件处理数据,建立了β-苯乙醇的定性分析和外标定量分析方法。该方法在0.005 mg/L~100 mg/L浓度范围内线性关系良好,相关系数R2为0.9994。在3个加标水平平均回收率为83.6%~103.8%,相对标准偏差小于7.6%;β-苯乙醇分析方法的LOD及LOQ分别为0.0006和0.005 mg/L,日内和日间重复性实验的相对标准偏差小于5.3%~8.0%;该方法灵敏度高、选择性好,用于实际酒类样品中β-苯乙醇的快速测定,得到满意的结果。
The GC-MS / SIM combined with solid-phase extraction column concentration purification method, the target compound β-phenyl ethanol characteristic fragment ions m / z 91 as a quantitative ion, m / z 122 molecular ions as a qualitative ion, using “ Xcalibur ”software processing data, the establishment of β-phenyl ethanol qualitative analysis and external standard quantitative analysis method. The method has good linearity in the concentration range of 0.005 mg / L ~ 100 mg / L with a correlation coefficient R2 of 0.9994. The average recoveries at three spiked levels ranged from 83.6% to 103.8% with relative standard deviations less than 7.6%. The LOD and LOQ of the β-phenylethanol assay were 0.0006 and 0.005 mg / L, respectively. The intra- and inter-day reproducibility The relative standard deviation (RSD) was less than 5.3% ~ 8.0%. The method has high sensitivity and good selectivity and is used for the rapid determination of β-phenylethanol in real alcohol samples. The results are satisfactory.