自动固相微萃取-气相色谱-串联质谱测定生活饮用水中2-甲基异莰醇和土臭素

    Determination of 2-methylisoborneol and geosmin in drinking water by automated solid-phase microextraction-gas chromatography-tandem mass spectrometry

    • 摘要:
      目的 建立自动固相微萃取气相色谱-串联质谱法, 测定生活饮用水中痕量2-甲基异莰醇(2-methylisoborneol, 2-MIB)和土臭素(geosmin, GSM)。
      方法 优化气相色谱条件和质谱参数提升仪器检测灵敏度, 通过对比不同盐析条件、萃取温度、萃取时间获得最佳前处理及固相微萃取条件, 并对加标回收率、精密度、方法检出限及定量限等方法性能进行评估。
      结果 本研究建立的方法可准确测定5 mL生活饮用水中痕量2-MIB和GSM。在2.0~100 ng/L浓度范围内, 2-MIB和GSM的线性关系良好, 相关系数(r)均大于0.999。2-MIB和GSM的检出限分别为0.56和0.71 ng/L, 定量限分别为1.84和2.36 ng/L, 加标回收率范围分别为89.7%~115%和83.3%~110.3%, 日内相对标准偏差范围分别为2.4%~3.1%和2.3%~4.7%, 日间相对标准偏差范围分别为4.2%~9.4%和3.2%~7.5%。应用本方法对5份生活饮用水进行分析, 两种目标物均有检出, 检出范围分别为1.6~4.6和2.2~2.5 ng/L, 均低于《生活饮用水卫生标准》(GB/T 5749-2022)中规定的限值(10 ng/L)。
      结论 本方法操作简单, 能够实现对生活饮用水中2-MIB和GSM的准确、高效、高灵敏度检测。

       

      Abstract:
      Objective To establish a method using automated solid-phase microextraction-gas chromatography-tandem mass spectrometry for the determination of trace levels of 2-methylisoborneol (2-MIB) and geosmin (GSM) in drinking water.
      Methods The sensitivity of the instrument was enhanced by optimizing gas chromatography conditions and mass spectrometry parameters.Various salting-out conditions, extraction temperatures, and extraction times were compared to identify the optimal pretreatment and solid-phase microextraction conditions.The performance was evaluated based on spiked recovery, precision, limit of detection, and limit of quantification.
      Results The established method enabled the accurate determination of trace 2-MIB and GSM in 5 mL drinking water samples.The method demonstrated excellent linearity for both 2-MIB and GSM within the concentration range of 2.0 to 100 ng/L, with correlation coefficients (r) exceeding 0.999.The limits of detection for 2-MIB and GSM were 0.56 and 0.71 ng/L, respectively, and their limits of quantitation were 1.84 and 2.36 ng/L, respectively.The spiked recoveries ranged from 89.7% to 115% for 2-MIB and from 83.3% to 110.3% for GSM.The intra-day relative standard deviations for 2-MIB and GSM ranged from 2.4% to 3.1% and from 2.3% to 4.7%, respectively.The inter-day relative standard deviations ranged from 4.2% to 9.4% and from 3.2% to 7.5%, respectively.This method was applied to analyze five drinking water samples and both target compounds were detected.Their concentrations ranged from 1.6 to 4.6 ng/L (2-MIB) and from 2.2 to 2.5 ng/L (GSM).These concentrations were below the limit of 10 ng/L as specified in the Standards for Drinking Water Quality(GB/T 5749-2022).
      Conclusion This method is simple, accurate, efficient, and highly sensitive for the determination of 2-MIB and GSM in drinking water.

       

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