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    顶空-固相微萃取-气相色谱串联质谱法测定饮水中7种异味物质

    Determination of seven odorous compounds in drinking water by headspace solid-phase microextraction-gas chromatography-tandem mass spectrometry

      摘要
    • 摘要:
      目的  建立顶空-固相微萃取(headspace solid-phase microextraction, HS-SPME)气相色谱串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定饮水中包括2-异丙基-3-甲氧基吡嗪(IPMB)、2-异丁基-3-甲氧基吡嗪(IBMB)、二甲基异莰醇(2-MIB)、2, 4, 6-三氯苯甲醚(2, 4, 6-TCA)、2, 3, 6-三氯苯甲醚(2, 3, 6-TCA)、土臭素(GSM)和2, 3, 4-三氯苯甲醚(2, 3, 4-TCA)在内7种异味物质含量的检测方法。
      方法  通过优化含盐量、萃取温度和时间、解析时间和温度、气相条件和质谱条件, 实现饮水中上述7种异味物质的分析。
      结果  7种异味物质的线性范围为0.50~100 ng/L, 相关系数(R2)在0.997 1~0.999 0之间, 检出限(limits of detection, LOD)和定量限(limits of quantitation, LOQ)范围分别为0.04~0.15 ng/L和0.14~0.50 ng/L, 三个浓度水平(1.00、10.0和50.0 ng/L)加标平均回收率分别为85.0%~119%、103%~116%和92.3%~107%, 相对标准偏差(n=6)分别为6.58%~14.1%、3.87%~9.01%和1.86%~8.98%。
      结论  本方法操作、简便, 选择性好、灵敏度高、准确度好, 可用于饮水中7种异味物质的检测。

       

      Abstract:
      Objective  To establish a method for the determination of seven odorous compounds including 2-isopropyl-3-methoxypyrazine (IPMB), 2-isobutyl-3-methoxypyrazine (IBMB), dimethyl isoborneol (2-MIB), 2, 4, 6-trichloroanisole (2, 4, 6-TCA), 2, 3, 6-trichloroanisole (2, 3, 6-TCA), geosmin (GSM) and 2, 3, 4-trichloroanisole (2, 3, 4-TCA) in drinking water using headspace solid-phase microextraction (HS-SPME)-gas chromatography-tandem mass spectrometry (GC-MS/MS).
      Methods  Analyses of the aforementioned seven odorous compounds in drinking water were performed by optimizing salt content, extraction temperature, extraction time, desorption temperature, desorption time, and gas chromatography and mass spectrometry conditions.
      Results  The seven odorous compounds exhibited linearity over the range of 0.50 ng/L to 100 ng/L, with correlation coefficients (R2) of 0.997 1 to 0.999 0, limits of detection of 0.04 ng/L to 0.15 ng/L, and limits of quantitation of 0.14 ng/L to 0.50 ng/L. At three concentration levels (1.00, 10.0, and 50.0 ng/L), the mean spiked recoveries were in the ranges of 85.0% to 119%, 103% to 116%, and 92.3% to 107%, respectively, with relative standard deviations (RSD, n=6) within the ranges of 6.58% to 14.1%, 3.87% to 9.01%, and 1.86% to 8.98%, respectively.
      Conclusion  This proposed method is simple to operate, offers good selectivity, high sensitivity, and excellent accuracy, making it suitable for the determination of the seven odorous compounds in drinking water.

       

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