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| 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 |
| Received:October 15, 2018 Revised:October 15, 2018 |
| DOI：10.12137/j.issn.2095-5448.2019.04.0220 |
| 中文关键词: 气相色谱-质谱联用法；鞋用橡胶；1，1，2，2-四氯乙烷；六氯丁二烯 |
| 英文关键词: gas chromatography-mass spectrometry；rubber for shoes；1，1，2，2-tetrachloroethane；hexachlorobutadiene |
| 基金项目:国家质检总局科技计划项目（No：2017QK051） |
| 中图分类号: |
| Author Name | Affiliation | E-mail | | Lin Ningting* | Fiber Inspection Bureau of Fujian | 491706210@qq.com |
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| 中文摘要: |
| 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。 |
| 英文摘要: |
| 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. |
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