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目的建立环境水体中致嗅物质甲硫醚和二甲基三硫醚的吹扫-捕集-气相色谱-质谱测定方法。方法采用吹扫-捕集法对水样进行富集,热解吸后导入HP-5MS毛细色谱柱(30 m×0.25 mm,0.25μm)进行气相色谱分离,利用质谱全扫描及选择离子模式进行定性及定量分析。结果甲硫醚和二甲基三硫醚分别在0.1～10和0.4～10μg/L的线性范围内,所得回归方程均呈较好的线性关系(r≥0.999);所得方法的检出限分别为0.02、0.1μg/L,定量下限分别为0.08、0.4μg/L;平均回收率为94.0%～96.4%,RSD为1.46%～2.63%。结论该方法具有操作简便、快速的优点,检测的灵敏度较高,适用于环境水体中微量甚至痕量致嗅物甲硫醚和二甲基三硫醚的一次性定性、定量分析。
Objective To establish a purge-trap-gas chromatography-mass spectrometry (MS-MS) method for the determination of the olfactory substances methyl sulfide and dimethyl trisulfide in environmental water. Methods Purified water samples were collected by purge-trap method. After thermal desorption, HP-5MS capillary column (30 m × 0.25 mm, 0.25 μm) was used for gas chromatographic separation and mass spectrometry scan and selected ion mode Qualitative and quantitative analysis. Results The linear regression equations of methyl sulfide and dimethyl trisulfide were obtained in the linear range of 0.1-10 and 0.4-10 μg / L, respectively (r ≥ 0.999). The detection limits of the obtained methods were respectively 0.02μg / L, the lower limit of quantification was 0.08,0.4μg / L, the average recovery was 94.0% ~ 96.4%, RSD was 1.46% ~ 2.63%. Conclusion The method has the advantages of simple and rapid operation, high detection sensitivity, and is suitable for the qualitative and quantitative analysis of trace amounts of methyl sulfide and dimethyl trisulfide caused by trace or even traces of trace amounts in environmental water.