色谱

色谱 ›› 2012, Vol. 30 ›› Issue (05): 468-473.DOI: 10.3724/SP.J.1123.2011.11055

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定人血清中多溴联苯

刘潇1,2, 李敬光1,2*, 黄飞飞2,3, 吴永宁2   

  1. 1. 南昌大学食品科学与技术国家重点实验室, 江西 南昌 330047; 2. 中国疾病预防控制中心营养与食品安全所, 北京 100050; 3. 苏州市疾病预防控制中心, 江苏 苏州 215004
  • 收稿日期:2011-11-30 修回日期:2012-01-12 出版日期:2012-05-28 发布日期:2012-06-07
  • 通讯作者: 李敬光,博士,研究员,主要从事食品安全研究. E-mail: lichrom@yahoo.com.cn. 基金项目: 科技部支撑计划课题(2007BAC27B02)和卫生部行业公益科研项目(200902009).
  • 基金资助:

    科技部支撑计划课题(2007BAC27B02)和卫生部行业公益科研项目(200902009).

Simultaneous determination of 8 polybrominated biphenyls in human serum using gas chromatography-mass spectrometry

LIU Xiao1,2, LI Jingguang1,2*, HUANG Feifei2,3, WU Yongning2   

  1. 1. State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330047, China; 2. National Institute of Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China; 3. Suzhou Center for Disease Control and Prevention, Suzhou 215004, China
  • Received:2011-11-30 Revised:2012-01-12 Online:2012-05-28 Published:2012-06-07

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摘要： 建立了血清中8种多溴联苯(PBBs,包括BB-15、18、52、101、153、180、194和206)的气相色谱-质谱检测方法。采用Oasis HLB固相萃取柱对血清样品中的多溴联苯进行萃取和初步净化,再使用自制的硅胶/酸化硅胶固相萃取柱(Sep-Pak silica/acidified silica)进行进一步的净化,并以正己烷为洗脱溶剂洗脱,氮吹洗脱液浓缩至100 μL后上样分析。以DB-5ms色谱柱(15 m×0.25 mm×0.1 μm)分离样品,在选择离子监测(SIM)模式下进行质谱检测,使用同位素内标法对8种目标物进行准确定量。结果显示,8种多溴联苯单体的方法检出限(LOD,以3.14倍标准偏差计)为0.002～0.029 ng/mL,方法定量限(LOQ,以10倍标准偏差计)为0.008～0.092 ng/mL;低、中、高3个加标水平的平均回收率为74.24%～119.49%,相对标准偏差(RSD)为1.23%～12.02%。采用本方法测定标准参考物质SRM1957和SRM1958中的BB-153含量,结果在参考值范围内。本方法准确、灵敏、操作简便,适用于血清中多溴联苯的测定。

关键词: 多溴联苯, 固相萃取, 气相色谱-质谱, 人血清

Abstract: A comprehensive analytical method based on gas chromatography-mass spectrometry (GC-MS) has been developed for the simultaneous determination of 8 polybrominated biphenyl congeners (PBBs: BB-15, 18, 52, 101, 153, 180, 194 and 206) in human serum. After the protein was removed, the sample was cleaned-up by an Oasis HLB solid-phase extraction (SPE) cartridge, then purified further by a two-layer cartridge containing activated silica gel and a mixture of silica gel and sulfuric acid, in which elution solvent was optimized. The eluent was evaporated to about 100 μL by a gentle nitrogen stream for GC-MS analysis. The separation was performed on a DB-5ms column (15 m×0.25 mm×0.1 μm) and the qualitative and quantitative analyses were carried out in electron impact (EI) selected ion monitoring (SIM) mode, in which isotope was used as internal standard. The limits of detection (LODs, 3.14 times of standard deviation) and the limits of quantification (LOQs, 10 times of standard deviation) were 0.002~0.029 ng/mL and 0.008~0.092 ng/mL respectively for the 8 PBBs. The average recoveries for all PBBs at three spiked levels were 74.24%~119.49% with the relative standard deviations in the range of 1.23%~12.02%. The method was verified by accurate analysis of BB-153 in organic contaminant standard reference materials (SRM) 1957 and 1958. This method is simple, rapid, accurate, precise and fit for the determination of PBBs in human serum.

Key words: gas chromatography-mass spectrometry (GC-MS), human serum, polybrominated biphenyls (PBBs), solid-phase extraction (SPE)

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