气相色谱-质谱法测定鞋用橡胶中的1,1,2,2-四氯乙烷和六氯丁二烯

Determination of 1,1,2,2-tetrachloroethane and Hexachlorobutadiene in Rubber for Shoes by Gas Chromatography-Mass Spectrometry

建立了鞋用橡胶中两种卤代烃(1,1,2,2-四氯乙烷和六氯丁二烯)的气相色谱-质谱检测方法。样品采用乙酸乙酯超声提取,采用气相色谱-质谱联用仪对提取液进行定性定量分析,定性采用全扫描,定量采用选择离子扫描方式,外标法定量。结果表明:当1,1,2,2-四氯乙烷和六氯丁二烯质量浓度在0. 20～5. 0 mg·L^(-1)范围内时,线性关系良好,相关因数大于0. 999;1,1,2,2-四氯乙烷和六氯丁二烯的检出限(3倍信噪比)分别为1. 0和0. 25 mg·kg^(-1),定量限(10倍信噪比)分别为2. 5和1. 0 mg·kg^(-1);平均加标回收率分别为85. 6%～91. 6%和89. 2%～94. 5%。该方法检出限低,灵敏度高,准确度和精密度高,操作简便,可用于鞋用橡胶中两种卤代烃的定性定量检测。

A gas chromatography-mass spectrometric method was established for the determination of two halohydrocarbons(1,1,2,2-tetrachloroethane and hexachlorobutadiene) in the rubber materials for shoes.The halohydrocarbons were firstly extracted out by using ethyl acetate with ultrasound,the obtained solution was then analyzed by gas chromatography-mass spectrometry under full scan and selected ion monitoring mode,and the results were quantified by the external standard method.The results showed that,when the mass concentration of 1,1,2,2-tetrachloroethane and hexachlorobutadiene was in range of 0.2~5.0 mg·L^-1,the calibration curves were linear with good correlation coefficients(>0.999),the limits of detection(signal-to-noise ratio=3) were 1 mg·kg^-1 and 0.25 mg·kg^-1 respectively,the limits of quantitation(signal-to-noise ratio=10) were 2.5 mg·kg^-1 and 1 mg·kg^-1 respectively,and the average recoveries were 85.6%~91.6% and 89.2%~94.5% respectively.The method featured low detection limit,good accuracy,high sensitivity,and simple operation.It could be used for the identification and quantification of the two halohydrocarbons in rubber for shoes.