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[利用同位素稀释-高分辨率质谱法制备和认证用于有机氯农药和多氯联苯分析的贻贝参考物质]

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

作者信息

Lu Xianbo, Chen Jiping, Wang Shuqiu, Zou Lili, Tian Yuzeng, Ni Yuwen, Su Fan

机构信息

Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China.

出版信息

Se Pu. 2012 Sep;30(9):915-21. doi: 10.3724/sp.j.1123.2012.04035.

DOI:10.3724/sp.j.1123.2012.04035
PMID:23285973
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.

摘要

描述了一种贻贝组织中有机氯农药(OCPs)和多氯联苯(PCBs)标准物质的制备及定值方法。依次对大连湾贻贝组织进行冷冻干燥、粉碎、过筛、匀浆、包装,并通过60Co辐射灭菌。采用同位素稀释和内标定量技术,通过高分辨率气相色谱/高分辨率质谱(HRGC/HRMS)测定18种OCPs和16种PCBs的认定值。认定值基于7个认可实验室进行验证并给出,这些值通过重量法制备的具有既定纯度的标准物质和测量比对可溯源至国际单位制(SI)。贻贝中PCBs和OCPs的认定值跨越4个数量级,相对不确定度约为10%。该物质是一种经确认具有良好均匀性和稳定性的天然生物物质,于2012年6月在中国被批准为“一级标准物质”(GBW10069)。该标准物质为我国实施《关于持久性有机污染物的斯德哥尔摩公约》中持久性有机污染物(POPs)监测提供了必要的质量控制物质。该物质旨在用于生物样品中OCPs和PCBs测定的方法验证和质量控制。

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