吹扫捕集与固相微萃取结合气相色谱-质谱法测定饮用水中4种嗅味物质的比较研究

    Determination of four odorants in drinking water by P&T-GC-MS versus SPME-GC-MS

    • 摘要:
      目的 建立和比较吹扫捕集(purge and trap, P&T)-气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)和固相微萃取(solid-phase microextraction, SPME)气相色谱-质谱法(GC-MS)同时测定饮用水中2-甲基异莰醇、土臭素、二甲基二硫醚和二甲基三硫醚4种嗅味物质的方法。
      方法 P&T法: 水样中的待测物在吹扫管中被氮气吹脱后, 被捕集阱捕获, 捕集阱瞬间加热将待测物解吸; SPME法: 采用固相微萃取纤维将水样中的待测物富集后, 于GC进样口解吸; 待测物解吸后经HP-5 MS色谱柱分离, GC-MS检测, 以保留时间和特征离子定性, 内标法定量。
      结果 P&T-GC-MS法: 取样量为25 mL, 4种嗅味物质的线性范围为10~100 ng/L, 方法最低检测质量浓度为1.8~3.5 ng/L, 回收率84.4%~108.3%, 相对标准偏差为2.0%~9.8%;SPME-GC-MS法: 取样量为10 mL, 二甲基二硫醚和二甲基三硫醚的线性范围为10~100 ng/L, 2-甲基异莰醇和土臭素的线性范围为5.0~100 ng/L, 方法最低检测质量浓度为1.8~ 6.0 ng/L, 回收率81.7%~114.0%, 相对标准偏差为3.7%~13.4%。
      结论 两种方法的检出限均达到ng/L级别, 回收率及精密度均满足检测要求, 适用于同时测定饮用水中的4种嗅味物质和不同实验室条件的需求。

       

      Abstract:
      Objective To develop the method of simultaneous determination of four odorants in drinking water (2-methylisoborneol, geosmin, dimethyl disulfide, and dimethyl trisulfide) using purge and trap-gas chromatography-mass spectrometry (P&T-GC-MS) versus solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS).
      Methods In P&T-GC-MS, the analytes in water sample were purged with nitrogen in a purge tube and captured by a trap, and the trap was quickly heated to desorb the analytes. In SPME-GC-MS, the analytes in water sample were enriched by a solid-phase microextraction fiber and then desorbed in the GC injection port. The desorbed analytes were separated on a HP-5 MS column and detected by GC-MS. A qualitative analysis was performed based on retention time and characteristic ions, and a quantitative analysis was conducted using the internal standard method.
      Results For the P&T-GC-MS method, the sample volume was 25 mL, the linear range for all four odorants was 10-100 ng/L, the limits of detection were 1.8-3.5 ng/L, the recovery rates were 84.4%-108.3%, and the relative standard deviations were 2.0%-9.8%. For the SPME-GC-MS method, the sample volume was 10 mL, the linear range of dimethyl disulfide and dimethyl trisulfide was 10-100 ng/L, the range of 2-methylisoborneol and geosmin was 5.0-100 ng/L, the limits of detection were 1.8-6.0 ng/L, the recovery rates were 81.7%-114.0%, and the relative standard deviations were 3.7%-13.4%.
      Conclusion Both method achieved detection limits at the ng/L level, the recovery rates and precision met the detection requirements, and these method were suitable for simultaneous determination of the four odorants in drinking water.

       

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