液液萃取-气相色谱/质谱法同时测定水样中3种三烷基硫代磷酸酯类化合物  

Simultaneous Determination of Three Trialkyl Phosphorothioates in Water Samples Using Liquid-liquid Exaction and Gas Chromatography-Mass Spectrometry

作　　者：付善良[1] 丁利[1] 肖家勇[1] 龚强[1] 朱绍华[1] 成婧[1] 王利兵[1] 

机构地区：[1]湖南出入境检验检疫局技术中心,食品安全科学技术湖南省重点实验室,湖南长沙410004

出　　处：《分析科学学报》2016年第2期193-197,共5页Journal of Analytical Science

基　　金：国家863计划(No.2012AA06A303)

摘　　要：本文建立了液液萃取-气相色谱/质谱同时测定水中O,O,S-三甲基硫代磷酸酯（TMPT）、O,O,S-三甲基二硫代磷酸酯（TMDTP）和O,O,O-三乙基硫代磷酸酯（TETP）3种三烷基硫代磷酸酯类化合物的分析方法。采用电子轰击（EI）-选择离子模式（SIM）进行定性与定量分析。考察了萃取剂种类、pH值以及盐度对萃取效率的影响。在优化的实验条件下,3种目标化合物的线性范围在0.01-2.0μg/mL之间,检出限（S/N=3）为0.26-1.1ng/L,定量限（S/N=10）为0.87-3.7ng/L。以该方法测定自来水、池塘水和湖水样品,3种目标化合物均未检出,不同加标水平（0.05、0.25和1.0μg/L）回收率在85.7%-104.2%之间,相对标准偏差在1.5%-12.2%之间。Trialkyl phosphorothioates are a class of toxic chemicals which usually exist in many kinds of organophosphorus pesticides as impurities.An analytical method was developed for the simultaneous determination of three trialkyl phosphorothioates（i.e.O,O,S-Trimethylthiophosphate（TMTP）,O,O,STrimethyldithiophosphate（TMDTP）and O,O,O-Triethylphosphorothioate（TEPT））in water samples using liquid-liquid extraction（LLE）and gas chromatography-mass spectrometry（GC-MS）.The qualitative and quantitative analysis of the three analytes was conducted by application of EI Mass spectra and selected ion monitoring（SIM）.Several impact factors including types of extractants,pH value and salinity were investigated to achieve optimum extraction efficiency.Under the optimized extraction conditions,good linear relationships of all the three analytes were obtained in the range of0.01-2.0μg/mL.The detection limits（S/N=3）were within 0.26-1.1ng/L and the quantification limits（S/N=10）were 0.87-3.7ng/L.The method was used to analyze real water samples induding tap water,pond water,and lake water.None of the three analytes in real water samples was detected,and their recoveries ranged from 85.7%to 104.2% with relative standard deviations（RSD）of 1.5%-12.2%at three different spiked concentrations（0.05,0.25 and 1.0μg/L）.

关 键 词：液液萃取 气相色谱/质谱法 水样 化学品 三烷基硫代磷酸酯类化合物 

分 类 号：O657.63[理学—分析化学]