箭型顶空固相微萃取-气相色谱串联质谱法测定水中4种嗅味物质

    Determination of four odor substances in water by HS-SPME arrow-GC-MS/MS

    • 摘要:
      目的 建立全自动箭型固相微萃取-气相色谱串联质谱法(headspace solid-phase microextraction arrow combined with gas chromatography-tandem mass spectrometry, HS-SPME arrow-GC-MS/MS)同时测定水中土臭素、二甲基异莰醇、β-紫罗兰酮和2, 4, 6三氯苯甲醚的分析方法。
      方法 水样经全自动固相微萃取进行富集, 经HP-5MS柱分离, 在GC-MS/MS的多反应监测模式进行分析, 外标法定量。
      结果 4种物质在1~200 ng/L范围内决定系数(R2)>0.997; 方法检出限0.41~0.85 ng/L; 3个浓度(5、50和150 ng/L)加标回收率分别为88.9%~108%、80.0%~98.4%和69.4%~81.5%;相对标准偏差分别为5.6%~10.5%、6.9%~12.1%和1.5%~4.2%。采用本方法对水源水、出厂水和末梢水中4种物质进行检测, 土臭素和二甲基异莰醇均有检出, 检出值为 < 0.49~7.4ng/L和 < 0.41~4.7ng/L; β-紫罗兰酮只在水源水中检出, 检出值为 < 0.85~4.5ng/L; 未检出2, 4, 6三氯苯甲醚。同时结果也表明β-紫罗兰酮受到水样中余氯的干扰。
      结论 该方法具有污染少、操作步骤简单、灵敏度高、精密度好等特点, 适用于水源水和饮用水中4种嗅味物质的快速测定。

       

      Abstract:
      Objective To establish a fully automatic headspace solid-phase microextraction arrow combined with gas chromatography-tandem mass spectrometry (HS-SPME arrow-GC-MS/MS) for simultaneous determination of geosmin, 2-methylisoborneol, β-ionone, and 2, 4, 6-trichloroanisole in water.
      Methods Water samples were enriched by fully automatic solid-phase microextraction, separated by HP-5MS columns, and analyzed in the multiple reaction monitoring mode of GC-MS/MS, with the external standard method for quantification.
      Results Thecontent of the four substances ranged from 1 to 200 ng/L, and thecorrelation coefficient (R2) of the 4 substances in the range of 1-200 ng/L was greater than 0.997. The detection limit of the method was 0.41-0.85 ng/L. The spike recovery rates at three concentrations (5, 50, and 150 ng/L) were 88.9%-108%, 80.0%-98.4%, and 69.4%-81.5%, respectively, and the relative standard deviations were 5.6%-10.5%, 6.9%-12.1%, and 1.5%-4.2%, respectively. Determination of the four substances in source water, finished water, and terminal water by this method showed that, geosmin and 2-methylisoborneol were detected with values ranging from < 0.49 to 7.4 ng/L and < 0.41 to 4.7 ng/L, respectively; β-ionone was only detected in source water with values ranging from < 0.85 to 4.5 ng/L; and 2, 4, 6-trichloroanisole was not detected.
      Conclusion The method has the characteristics of less pollution, simple operation procedure, high sensitivity, and good precision. Therefore, it is suitable for rapid determination of the 4 odor substances in source water and drinking water.

       

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