摘要
目的建立固相微萃取气相色谱质谱联用测定饮用水中6个卤乙腈、7个卤代硝基甲烷及5个含碘三卤甲烷消毒副产物的方法,并了解本市饮用水中目标消毒副产物的浓度水平。方法优化固相微萃取参数,建立检测方法,并对100个饮用水样品进行检测。结果选择DVB/PDMS萃取头,以氯化钠为盐析试剂且加入浓度为40%(W/V),在萃取温度40℃萃取时间20 min、解吸温度170℃解吸时间2 min的操作条件下,目标消毒副产物具有良好的检测灵敏度,检出限为0.14 ng/L~18.00 ng/L,方法的线性相关系数>0.99,加标回收率为70%~121%,相对标准偏差为1%~15%。对本市100个饮用水进行检测,结果卤乙腈、含碘三卤甲烷、卤代硝基甲烷的中位值浓度分别为0.86μg/L、0.36μg/L、0.07μg/L,检出率分别为99%、89%、89%。结论本方法灵敏、简便、无干扰,适合饮用水中痕量浓度水平的卤乙腈、卤代硝基甲烷、含碘三卤甲烷的检测。
Objective To establish a method for the determination of 6 haloacetanitriles(HANs), 7 halonitromethanes(HNMs) and 5 iodinated thrihalomethanes(I-THMs) disinfection byproducts(DBPs) in drinking water using solid-phase microextraction/gas chromatography-mass spectrometry, and to survey the concentration level of target DBPs in drinking water in local city. Methods The solid-phase microextraction(SPME) parameters were optimized, and then the determination method was developed, which was then used to analyze 100 drinking water samples. Results Good detection sensitivity was obtained for the target DBPs with DVB/PDMS as the fiber and sodium chloride as salting out reagent(40%, W/V), when operated at extraction temperature of 40 ℃ for 20 minutes and desorption temperature of 170 ℃ for 2 minutes. Detection limit was within 0.14 ng/L-18.00 ng/L. The linear correlation coefficients were greater than 0.99. The recovery was within 70%-121%, and relative standard deviation was within 1%-15%. A survey of 100 drinking water samples showed the median concentrations of HANs, I-THMs and HNMs were 0.86 μg/L, 0.36 μg/L, 0.07 μg/L, and the detected ratios were 99%, 89%, 89% respectively. Conclusion This method is simple, sensitive and of no interferences. It is suitable for the determination of trace concentration level of HANs, HNMs and I-THMs in drinking water.
引文
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