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J4 ›› 2013, Vol. 48 ›› Issue (05): 34-38.

• 前沿进展 • 上一篇    下一篇

稳定性同位素稀释气相色谱-质谱法测定金枪鱼中多氯联苯的不确定度评定

申中兰1,袁东2,王茂森1, 脱英英3,张红霞1,盛建伟1,张卉1,祝建华1   

  1. 1. 山东省产品质量监督检验研究院, 山东 济南 250100;  2. 齐鲁师范学院化学系, 山东 济南 250013;
    3. 山东轻工业学院学生处, 山东 济南 250353
  • 收稿日期:2012-10-09 出版日期:2013-05-20 发布日期:2013-05-10
  • 作者简介:申中兰(1978- ),女,高级工程师,博士,研究方向为色谱技术与食品安全.Email:zlshen-sdqi@163.com
  • 基金资助:

    山东省质量技术监督局项目(2009KY13)

Uncertainty estimation in determination of polychlorinated biphenyls in  tuna by stable isotope dilution gas chromatographymass spectrometry

SHEN Zhong-lan1, YUAN Dong2, WANG Mao-sen1, TUO Ying-ying3, ZHANG Hong-xia1, SHENG Jian-wei1, ZHANG Hui1, ZHU Jian-hua1   

  1. 1. Shandong Supervision and Inspection Institute for Product Quality, Jinan 250100, Shandong, China;
    2. Chemistry Department, Qilu Normal University, Jinan 250013, Shandong, China;
    3. Student Affairs Office of Shandong Polytechnic University, Jinan 250353, Shandong, China
  • Received:2012-10-09 Online:2013-05-20 Published:2013-05-10

摘要:

鱼肉制品中多氯联苯的测定步骤复杂,分析结果与真实值之间往往存在一定的出入。本文采用稳定性同位素稀释气相色谱-质谱法对金枪鱼中多氯联苯的含量进行测定,并对整个测试过程的不确定度来源进行系统分析。以PCB28(Polychlorinated Biphenyl 28)为分析对象,对测试过程中引入的不确定的各个分量进行评定与合成,当PCB28测定结果为17.7ng/g时,扩展不确定度为1.9ng/g, k=2, p=95%。较为全面地评定了测量结果不确定度的影响因素,并提出了金枪鱼中多氯联苯测定质量控制的改进方法。

关键词: 气相色谱-质谱法;金枪鱼;多氯联苯;不确定度

Abstract:

Existing methods for analyzing PCBs in animal muscle require multiple and laborious steps prior to quantitation. In this paper, a method for determination of Polychlorinated Biphenyls(PCBs) in tuna by Stable Isotope Dilution Gas Chromatography-Mass Spectrometry(GCMS) has been proposed. Uncertainty source of the method has been analyzed systematically. By analyzing of standard material PCB28, the uncertainty factors of testing process were evaluated and synthesized. When the result for the determination of PCB28 was 17.7ng/g, the expanded uncertainty was 1.9ng/g, k=2, p=95%. This paper evaluated comprehensively the predominant influences on the uncertainty, some methods used to improve the quality control were also discussed.

Key words: Gas Chromatography-Mass Spectrometry (GCMS); tuna; polychlorinated biphenyls(PCBs); uncertainty

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