摘要
基于液液萃取一酸化甲醇衍生化处理和气相色谱-三重四级杆质谱联用仪（GC-EI—MS／MS），建立了可用于检测水中10种卤乙酸（HAAs）的方法。本研究采用EI-MS／MS鉴别了10种HAAs衍生物的前级离子和产物离子，优化了质谱运行参数，同时以USEPA方法552．3为基础对样品预处理程序进行了部分优化。采用优化后的预处理程序建立标线，10种HAAs的线性范围为0．5～100μg／L（r=0．9976～0．9999，n=8），检出限为0．012～0．079μg／L，日内和日间相对标准偏差分别为1．0％～6．9％和1．6％～8．2％。向地表水、地下水和污水处理厂出水中添加浓度为2．5和25μg／L的10种HAAs混合标准溶液，回收率分别为90．3％～100．2％，90．5％～107．5％，76．9％～100．4％。本方法能够满足自来水和污水处理厂出水中10种HAAs的检测要求。
A method for determining ten haloacetic acids （HAAs） in water has been developed based on liquid-liquid extraction followed by acidic methanol derivatization and gas chromatography-triple quadrupole mass spectrometry （GC-EI-MS/MS）. Precursor ions and product ions of the ten HAA esters were first identified based on the mass spectra of the EI-MS/MS, and the operating conditions of mass spectrometry were optimized. In addition, this study was based on the US EPA method 552.3, and some pretreatment procedures were partially optimized. The modified pretreatment procedure was used to establish calibration, the linear calibration range extended from 0.5 to 100 μg/L （ r = 0. 9976-0. 9999, n = 8 ） for all the ten HAAs, and limits of detection （LODs） were between 0.012 μg/L and 0. 079 μg/L. The intra-day and inter-day relative standard deviations （RSDs） were in the range of 1.0% -6.9% and 1.6% -8.2% , respectively. The method was validated by the analysis of surface water, ground water and waste water effluent samples spiked with 2.5 and 25 μg/L individual HAAs, with the relative analyte recoveries being in the ranges of 90.3% -100.2%, 90.5%-107.5% and 76.9%-100.4% , for the three kinds of water samples respectively. This method can meet the detection requirements for ten kinds of HAAs in tap water and wastewater effluents.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第1期77-82,共6页
Chinese Journal of Analytical Chemistry
基金
长江学者与创新团队发展计划(No.PCSIRT
IRT0853)
西安建筑科技大学科研基金项目(Nos.DB03087
DB03137)资助
关键词
卤乙酸
气相色谱-三重四级杆质谱
酸化甲醇
预处理
Haloaeetic acid
Gas chromatography-triple quadrupole mass spectrometry
Acidic methanol
Pretreatment
