食品科学

• 安全检测 • 上一篇    下一篇

气相色谱-质谱法测定水中多溴联苯醚残留量

杨 芳,张宪臣,卢俊文,闫爱国,陈丽斯,张朋杰,郑雷青   

  1. 1.中山出入境检验检疫局,广东 中山 528403;2.江门市农产品质量监督检验检测中心,广东 江门 529000
  • 出版日期:2016-08-25 发布日期:2016-08-30
  • 通讯作者: 张宪臣
  • 基金资助:

    国家质检总局科技计划项目(2015IK052);广东检验检疫局科技计划项目(2015GDK32)

Determination of Polybrominated Diphenyl Ethers Residues in Water by Gas Chromatography-Mass Spectrometry

YANG Fang, ZHANG Xianchen, LU Junwen, YAN Aiguo, CHEN Lisi, ZHANG Pengjie, ZHENG Leiqing   

  1. 1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528403, China;
    2. Jiangmen Quality Supervision and Inspection Center for Agricultural Products, Jiangmen 529000, China
  • Online:2016-08-25 Published:2016-08-30
  • Contact: ZHANG Xianchen

摘要:

建立一套准确、高效、快捷的水中多溴联苯醚(polybrominated diphenyl ethers,PBDEs)残留量的检测方法。样品采用二氯甲烷提取,氮吹浓缩,正己烷定容,然后以气相色谱-质谱测定。19 种PBDEs组分线性良好,相关系数R2均大于0.99,相对标准偏差(relative standard deviation,RSD)(n=6)为1.5%~5.6%,检出限为0.1~1.0 μg/L。PBDE-3和PBDE-209平均加标回收率为84.3%~93.2%,RSD为3.6%~10.1%。结果表明,该方法各项指标均能满足检测工作要求,适用于水中PBDEs残留量的日常检测。

关键词: 气相色谱-质谱, 水, 多溴联苯醚, 溴代阻燃剂

Abstract:

An accurate, efficient and fast method for the determination of residues of polybrominated diphenyl ethers
in water using gas chromatography-mass spectrometry (GC-MS) was developed. The sample was extracted using
dichloromethane, concentrated under nitrogen blow, dissolved in hexane, and then detected by GC-MS. The calibration
curves of all 19 polybrominated diphenyl ethers presented good linearity with correlation coefficients (R2) higher than 0.99.
The relative standard deviations (RSD, n = 6) for precision were between 1.5% and 5.6%, and the limits of detection (LOD)
were in the range from 0.1 to 1.0 μg/L. The recoveries of PBDE-3 and PBDE-209 were from 84.3% to 93.2%, with RSD
(n = 6) between 3.6% and 10.1%. These results displayed that all the evaluated figures of merit of the method could meet the
analytical requirements. Thus, the developed method could be applied in the routine analysis of polybrominated diphenyl
ethers residues in water.

Key words: gas chromatography-mass spectrometry (GC-MS), water, polybrominated diphenyl ethers (PBDEs), brominated flame retardants

中图分类号: