微波辅助萃取-GC-MS法测定玩具中磷酸三(2-氯乙基)酯  

Determination of tris(2-chloroethyl phosphate)in toys by Gas Chromatography-Mass spectrometry with microwave assisted extraction

作　　者：蒋小良[1] 曾铭 郝雨 王洁泉[1] 黄钧[1] 徐正华[1] 陈凯[1] 

机构地区：[1]江门出入境检验检疫局,广东江门529000 [2]花都出入境检验检疫局,广东广州510800

出　　处：《化学试剂》2013年第12期1108-1110,共3页Chemical Reagents

基　　金：广东检验检疫局科技计划项目(2012GDK28;2012GDK42)

摘　　要：建立了微波辅助萃取-气相色谱-质谱法（GC-MS）测定玩具中磷酸三（2-氯乙基）酯含量的分析方法。考察了6种不同萃取溶剂对磷酸三（2-氯乙基）酯的萃取效率,选择乙酸乙酯为萃取溶剂,考察了微波辅助萃取温度与时间对萃取效果的影响,选择了最佳的微波辅助萃取条件。萃取液经浓缩后,用气相色谱-质谱仪进行选择离子监测模式下的定性及定量分析。结果表明,该方法的检出限为0.02 mg/kg,样品的加标回收率为93.6%~98.2%,相对标准偏差〈4.8%。该方法具有快速、方便、灵敏度高、定性准确等优点,适用于玩具中有机磷阻燃剂磷酸三（2-氯乙基）酯含量的快速测定。An effective method was established for the determination of tris（2-chloroethyl phosphate） （TCEP） in toys by gas chromatography-mass spectrometry with microwave assisted extraction. The condition of microwave assisted extraction temperature and time were optimized based on the extraction effciency of six different extraction solvents for the TCEP sampies, and ethyl acetate as extraction solvent. The extract was concentrated and injected into GC-MS,qualitative and quantitative analysis was conducted under selected ion monitoring （SIM） mode. The detection limit was 0. 02 mg/kg. The recoveries are at the range of 93.6% ～ 98.2% with relative standard deviation（RSD） below 4.8%. The results indicated that the method is simple, rapid, sensitive and accurate ,which could satisfy the demand of the analysis of banned organo- phosphorous flame retardants-TCEP in toys.

关 键 词：微波辅助萃取 磷酸三(2-氯乙基)酯 玩具 气相色谱-质谱法 

分 类 号：O656.32[理学—分析化学]