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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。
A method for the determination of tris (2-chloroethyl) phosphate in toys by microwave-assisted extraction-gas chromatography-mass spectrometry (GC-MS) was established. The extraction efficiency of tris (2-chloroethyl) phosphate by six different extraction solvents was investigated. Ethyl acetate was chosen as the extraction solvent. The effects of microwave-assisted extraction temperature and time on the extraction efficiency were investigated. The optimum microwaves Auxiliary extraction conditions. The extracts were concentrated and qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry in a selective ion monitoring mode. The results showed that the detection limit of this method was 0.02 mg / kg. The spiked recoveries were 93.6% ~ 98.2% and the relative standard deviations were less than 4.8%. The method has the advantages of fastness, convenience, high sensitivity and accuracy, and is suitable for the rapid determination of the content of tris (2-chloroethyl) phosphate of the organophosphorus flame retardant in toys.