采用固相萃取法对水样中的溴酚(BPs)进行富集纯化,以乙酸酐为衍生化试剂,气相色谱-质谱联用仪为检测仪器,建立适于水中痕量BPs的分析方法,并通过以市政供水为测试水样的加标回收实验对该方法进行评价. 在优化后的实验条件下,BPs衍生后具有较好的色谱响应信号和色谱行为,定性检出限为0.8~17.7 ng/mL,空白加标回收率为93.2%~114.5%,以市政供水为水样加标回收率为68.3%~110.1%(其中仅2,4,6-三溴苯酚加标回收率相对较低,为68.3%~73.0%),相对标准偏差均小于20%. 所建立的分析方法灵敏度、回收率和重复性均较好,可以用于实际水样中BPs的测定.
In this work, bromophenols(BPs)in water samples were enriched by solid phase extraction, with acetic anhydride as derivative reagent and gas chromatography-mass spectrometer as detection instrument and an analysis method suitable for trace BPs in water was established. The method was evaluated by the standard recovery experiment of municipal water sample. After derivatization, BPs showed good chromatographic response signal. The detection limits were 0.8—17.7 ng/mL. The addition recoveries of blank water and municipal water ranged from 93.2% to 114.5%, 68.3% to 110.1%, and only the addition recoveries of 2,4,6-tribromophenol(2,4,6-TBP)was low, ranged from 68.3% to 73.0%. The relative standard deviations were less than 20%. This method was proved to have good sensitivity, recovery and repeatability, and can be applied for the determination of BPs in actual water samples.
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