摘要
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.
作者
葛嘉雨
梁海燕
刘冬
李春灵
张丰泉
赵茜
GE Jiayu;LIANG Haiyan;LIU Dong;LI Chunling;ZHANG Fengquan;ZHAO Qian(School of Public Health,Xinxiang Medical University,Xinxiang 453003,China)
出处
《河北大学学报（自然科学版）》
CAS
北大核心
2022年第4期395-402,共8页
Journal of Hebei University(Natural Science Edition)
基金
国家自然科学基金资助项目(21707115)
河南省科技攻关项目(212102311076,212102210121)
新乡医学院博士科研启动基金资助项目(XYBSKYZZ201518)。
关键词
溴代苯酚
柱前衍生
固相萃取法
气相色谱-质谱法
bromophenols
precolumn derivation
solid phase extraction
gas chromatography-mass spectrometry
