色谱

色谱 ›› 2011, Vol. 29 ›› Issue (02): 168-171.DOI: 10.3724/SP.J.1123.2011.00168

• 技术与应用 • 上一篇    下一篇

气相色谱-质谱法测定电子产品中的四溴双酚-A

肖进进*, 富玉, 林舒, 张姝   

  1. 谱尼测试科技股份有限公司, 北京 100080
  • 收稿日期:2010-11-08 修回日期:2010-12-14 出版日期:2011-02-28 发布日期:2007-03-25
  • 通讯作者: 肖进进,硕士,研究方向为电子、食品、环境样品等分析方法的研发.

Determination of tetrabromobisphenol-A in electronic products by gas chromatography-mass spectrometry

XIAO Jinjin*, FU Yu, LIN Shu, ZHANG Shu   

  1. Pony Testing Co., Ltd., Beijing 100080, China
  • Received:2010-11-08 Revised:2010-12-14 Online:2011-02-28 Published:2007-03-25
  • Contact: Jin-Jin XIAO

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721

被引次数

17

摘要： 建立了电子产品中四溴双酚-A(TBBP-A)的气相色谱-质谱联用(GC-MS)检测方法。样品经丙酮提取后挥发至干,经二氯甲烷重新溶解后,用碳酸钾溶液反提取,反提取液与乙酸酐衍生化反应。衍生产物经正己烷提取后,采用GC-MS进行分析。结果表明,方法的线性范围为0.25～5.0 mg/L,相关系数为0.996;方法的检出限为0.05 mg/kg;平均回收率为87.3%～104.1%,相对标准偏差为5.6%～8.5%。该方法准确、灵敏,可用于实际电子产品中四溴双酚-A的分析。

关键词: 电子产品, 气相色谱-质谱联用, 四溴双酚-A, 乙酰化

Abstract: A method for the determination of tetrabromobisphenol-A (TBBP-A) in electronic products was developed by gas chromatography-mass spectrometry (GC-MS). The TBBP-A was extracted from electronic products by automatic digestion oven with acetone and concentrated by the evaporation of solvent. It was redissolved in methylene chloride, back-extracted by potassium carbonate solution and reacted with acetic anhydride. The derivative was extracted by hexane and determined by GC-MS. The linear calibration curve was obtained in the range of 0.25~5.0 mg/L with a correlation coefficient of 0.996. The detection limit of the method was 0.05 mg/kg. The recoveries were 87.3%~104.1% and the relative standard deviations were 5.6%~8.5%. The method is accurate and sensitive, and it is suitable for the analysis of tetrabromobisphenol-A in electronic products.

Key words: acetylation, electronic products, gas chromatography-mass spectrometry (GC-MS), tetrabromobisphenol-A (TBBP-A)