色谱

色谱 ›› 2012, Vol. 30 ›› Issue (12): 1241-1245.DOI: 10.3724/SP.J.1123.2012.08020

• 研究论文 • 上一篇    下一篇

超声辅助萃取-气相色谱-负化学电离源质谱法测定室内灰尘样品中8种常见多溴联苯醚

张晓玲1, 王炳玲2*, 陆晓梅1, 张琦2, 张正东2   

  1. 1. 南京医科大学公共卫生学院卫生检验学系, 江苏 南京 210029; 2. 南京医科大学公共卫生学院职业医学与环境卫生学系, 江苏 南京 210029
  • 收稿日期:2012-08-14 修回日期:2012-11-08 出版日期:2012-12-28 发布日期:2012-12-19
  • 通讯作者: 王炳玲,博士,讲师. Tel: (025)86862748, E-mail: blwang@njmu.edu.cn.
  • 基金资助:

    国家自然科学基金面上项目(81072268)、江苏省自然科学基金面上项目(BK2010535)、江苏省博士后基金项目(1001017C)和江苏高校优势学科建设工程资助项目.

Determination of polybrominated diphenyl ethers in indoor dust using ultrasonic-assisted extraction and gas chromatography-negative chemical ionization mass spectrometry

ZHANG Xiaoling1, WANG Bingling2*, LU Xiaomei1, ZHANG Qi2, ZHANG Zhengdong2   

  1. 1. Department of Hygienic Analysis and Detection, School of Public Health, Nanjing Medical University, Nanjing 210029, China; 2. Department of Occupational Medicine and Environmental Health, School of Public Health, Nanjing Medical University, Nanjing 210029, China
  • Received:2012-08-14 Revised:2012-11-08 Online:2012-12-28 Published:2012-12-19

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351

被引次数

16

摘要： 建立了室内灰尘样品中8种常见多溴联苯醚(PBDEs: BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)的气相色谱-负化学电离源质谱(GC-NCI/MS)分析方法。样品经吸尘器采集、正己烷超声萃取、浓缩后,采用GC-NCI/MS测定。结果表明,方法的加标回收率为53.2%～107.6%,日内测定的相对标准偏差(RSD)为2.8%～16.5%,日间测定的RSD为6.4%～22.6%。除了BDE-209的检出限(信噪比为3)为0.15 ng/g外,其他多溴联苯醚的检出限为0.003～0.015 ng/g。该方法灵敏度高,准确度和精密度好,简便快速,溶剂消耗量少,适用于灰尘中三溴～十溴联苯醚的测定。

关键词: 超声辅助萃取, 多溴联苯醚, 气相色谱-负化学电离源质谱, 室内灰尘

Abstract: A method for the determination of eight polybrominated diphenyl ethers (PBDEs) in indoor dust was developed. A vacuum cleaner was used for gathering the house dust, and n-hexane was added and the extraction was performed in an ultrasonic bath. The supernatant was concentrated and then n-hexane was added to 0.1 mL. Gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS) has been investigated for the determination of the eight PBDE congeners in indoor dust. The eight PBDEs were separated within 20 min. The absolute recoveries were 53.2%~107.6%. The relative standard deviations (RSDs) of intra-day were between 2.8% and 16.5%, while the RSDs of inter-day were between 6.4% and 22.6%. The limits of detection (LOD, S/N=3) were in the range of 0.003~0.015 ng/g except the LOD of BDE-209 was 0.15 ng/g. The results indicated that the proposed method is sensitive, accurate, fast, simple, low solvent consumption and suitable for the determination of tri- to deca-BDEs in indoor dust.

Key words: gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS), indoor dust, polybrominated diphenyl ethers (PBDEs), ultrasonic-assisted extraction