色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 915-921.DOI: 10.3724/SP.J.1123.2012.04035

• 研究论文 • 上一篇    下一篇

贻贝中有机氯农药和多氯联苯标准物质的研制及同位素稀释高分辨质谱法定值

卢宪波, 陈吉平*, 王淑秋, 邹黎黎, 田玉增, 倪余文, 苏凡   

  1. 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2012-04-25 修回日期:2012-05-21 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 陈吉平,博士,研究员,主要研究方向为生态环境评价与分析. Tel: (0411)84379562, E-mail: chenjp@dicp.ac.cn.
  • 基金资助:

    国家“863”计划项目(2009AA061603)和国家“973”计划项目(2009CB421602).

Preparation and certification of mussel reference material for organochlorine pesticides and polychlorinated biphenyls using isotope dilution-high resolution mass spectrometry

LU Xianbo, CHEN Jiping*, WANG Shuqiu, ZOU Lili, TIAN Yuzeng, NI Yuwen, SU Fan   

  1. (Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2012-04-25 Revised:2012-05-21 Online:2012-09-28 Published:2012-09-20

PDF

454

被引次数

30

摘要： 建立了贻贝中有机氯农药(OCPs)和多氯联苯(PCBs)标准物质的研制和定值方法,该研究对我国开展环境生物标准物质的研制具有重要的方法学借鉴价值。该标准物质样品为采自大连湾海域的贻贝,其定值目标物包括18种OCPs和16种PCBs,采用的定值测量方法是目前世界上最权威、最准确的同位素稀释-高分辨气相色谱/高分辨质谱联用法(ID-HRGC/HRMS)。所研制的标准物质具有定值目标物种类多、不确定度较小(约10%)等特点。该标准物质是目前国际上唯一一种采用同位素稀释高分辨质谱法进行定值的底栖生物中OCPs标准物质,于2012年3月通过了国家一级标准物质的终审,并于2012年6月被国家质量监督检验检疫总局批准为国家一级标准物质(GBW10069)。该标准物质可用于食品安全控制、环境监测、质量检测等领域相关分析方法的评价、测量质量控制及技术仲裁检验等。

关键词: 多氯联苯, 高分辨气相色谱/高分辨质谱, 环境标准物质, 同位素稀释质谱法, 贻贝, 有机氯农药

Abstract: A method for the preparation and certification of the reference material of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in mussel tissue is described. The mussel tissue from Dalian Bay was frozen-dried, comminuted, sieved, homogenized, packaged, and sterilized by 60Co radiation sterilization in turn. The certified values for 18 OCPs and 16 PCBs were determined by high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) using isotope dilution and internal standard quantitation techniques. The certified values were validated and given based on seven accredited laboratories, and these values are traceable to the SI (international system of units) through gravimetrically prepared standards of established purity and measurement intercomparisons. The certified values of PCBs and OCPs in mussel span 4 orders of magnitude with a relative uncertainty of about 10%. This material is a natural biological material with confirmed good homogeneity and stability, and it was approved as the grade “primary reference material” (GBW10069) in June 2012 in China. This reference material provided necessary quality control products for our country to implement the Stockholm Treaty on the monitoring of persistent organic pollutants (POPs). The material is intended to be used for the method validation and quality control in the determination of OCPs and PCBs in biota samples.

Key words: environmental reference material, isotope dilution mass spectrometry (IDMS), mussel, organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs), high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS)