气相色谱/三重四极杆质谱法测定动物组织中五氯酚的不确定度评定
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摘要
目的建立气质联用法测定动物组织中五氯酚含量的不确定度评定方法,通过对样品前处理过程中不确定度的分析及讨论等提高对检测过程中不确定度的控制。方法分析气质联用—内标衍生法测定动物组织中五氯酚浓度的整个过程,确定不确定度的来源和大小,最后进行合成并扩展。结果动物组织中五氯酚浓度为5.21μg/kg,其扩展不确定度为0.86μg/kg (P=95%,k=2)。结论气相色谱质谱联用法测定动物组织中五氯酚浓度的不确定度,主要由重复性、内标加入量、标准曲线的拟合引入。
Objectives To evaluate the uncertainty of determination of Pentachlorophenol in animal tissues by GC-MS, through the analysis of uncertainty in the processes of sample preparation and discussion to improve control of uncertainty in the testing process. Methods The whole process during the determination of Pentachlorophenol was analyzed to determine the uncertainty sources and to calculate the combined and expanded uncertainty.Result The expanded uncertainty with 5.21 μg/kg levels of Pentachlorophenol in animal tissues was 0.86 μg/kg(P=95%,k=2). Conclusions The uncertainty evaluation for the determination of Pentachlorophenol in animal tissues by GC-MS was mainly caused by repeatability, the Internal standard addition, and the Fitting Standard.
Objectives To evaluate the uncertainty of determination of Pentachlorophenol in animal tissues by GC-MS, through the analysis of uncertainty in the processes of sample preparation and discussion to improve control of uncertainty in the testing process. Methods The whole process during the determination of Pentachlorophenol was analyzed to determine the uncertainty sources and to calculate the combined and expanded uncertainty.Result The expanded uncertainty with 5.21 μg/kg levels of Pentachlorophenol in animal tissues was 0.86 μg/kg(P=95%,k=2). Conclusions The uncertainty evaluation for the determination of Pentachlorophenol in animal tissues by GC-MS was mainly caused by repeatability, the Internal standard addition, and the Fitting Standard.
引文
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[9] 韩嘉艺,李晓明,钱乐,等.微量分光光度法测定饮用水中亚硝酸盐氮检测结果的有效性评估[J].环境卫生学杂志,2016,6(5):360-364.Han JY,Li XM,Qian Y,et al.Assessment on validity nitrite-nitrogen results in drinking-water by micro-spectro photometry[J].J Environ Hyg,2016,6(5):360-364.
[10] 中国合格评定国家认可委员会.CNAS-CL01 检测和校准实验室能力认可准则[S].北京:中国计量出版社,2018.(In English:China National Accreditation Service for Conformity Assessment.CNAS-CL01 Accreditation criteria for the competency of testing and calibration laboratories[S].Beijing:China Metrology Publishing House,2018)
[11] 中华人民共和国国家质量监督检验检疫总局.JJG 646-2006 移液器检定规程[S].北京:中国计量出版社,2007.(In English:General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China.JJG 646-2006 Verification regulation of locomotive pipette[S].Beijing:China Metrology Publishing House,2007.)
[12] 中华人民共和国国家质量监督检验检疫总局.JJG 196-2006 常用玻璃量器检定规程[S].北京:中国计量出版社,2007.(In English:General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China.JJG 196-2006 Verification regulation of working glass container[S].Beijing:China Metrology Publishing House,2007)
[13] 刘芳芳,魏秋宁,丁亚磊.氢化物原子荧光法测定尿中砷的不确定度分析[J].环境卫生学杂志,2018,8(4):350-354.(Liu FF,Wei QN,Ding YL.Uncertainty evaluation on the determination of arsenic in urine by hydride generation atomic fluorescence spectrometry[J].J Environ Hyg,2018,8(4):350-354.)
[2] 许文青,樊柏林,陈明,等.五氯苯酚和五氯苯酚钠毒性作用研究进展[J].中国药理学与毒理学杂志,2011,25(6):596-600.(In English:Xu WQ,Fan BL,Chen M,et al.Progress in toxicity of pentachlorophenol and sodium pentachlorophenol[J].Chin J Pharmacol Toxicol,2011,25(6):596-600.)
[3] 国家卫生和计划生育委员会.GB 23200.92-2016 动物源性食品中五氯酚残留量的测定液相色谱—质谱法[S].北京:中国标准出版社,2017.(In English:National Health and Family Planning Commission of PRC.GB 23200.92-2016 National food safety standards—Determination of pentachlorophenol residue in animal-derived foods[S].Beijing:Standards Press of China,2017.)
[4] 农业部.GB 29708-2013 动物性食品中五氯酚钠残留量的测定气相色谱-质谱法.[S].北京:中国标准出版社,2014.(In English:Ministry of Agriculture GB 29708-2013 Determination of sodium pentachlorophenol residue in animal derived food by Gas Chromatography-mass spectrometry method Beijing:Stand Press of China,2014).
[5] 中华人民共和国国家质量监督检验检疫总局.JJF 1059.1-2012 测量不确定度评定与表示[S].北京:中国标准出版社,2013.(In English:General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China.JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement[S].Beijing:Standards Press of China,2013.)
[6] 中华人民共和国国家质量监督检验检疫总局.JJF 1135-2005 化学分析测量不确定度评定[S].北京:中国计量出版社,2005.(In English:General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China.JJF 1135-2005 Evaluation of uncertainty in chemical analysis measurement[S].Beijing:China Metrology Publishing House,2005.)
[7] 中华人民共和国国家质量监督检验检疫总局.GB/T 27418-2017 测量不确定度评定和表示[S].北京:中国标准出版社,2018.(In English:General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China.GB/T 27418-2017 Guide to the evaluation and expression of uncertainty in measurement[S].Beijing:Standards Press of China,2018.)
[8] 中国合格评定国家认可委员会.CNAS-GL06-2006 化学分析中不确定度的评估指南[S].北京:中国计量出版社,2006.(In English:China National Accreditation Service for Conformity Assessment.CNAS-GL06-2006 Guidance on evaluating the uncertainty in chemical analysis[S].Beijing:China Metrology Publishing House,2006.)
[9] 韩嘉艺,李晓明,钱乐,等.微量分光光度法测定饮用水中亚硝酸盐氮检测结果的有效性评估[J].环境卫生学杂志,2016,6(5):360-364.Han JY,Li XM,Qian Y,et al.Assessment on validity nitrite-nitrogen results in drinking-water by micro-spectro photometry[J].J Environ Hyg,2016,6(5):360-364.
[10] 中国合格评定国家认可委员会.CNAS-CL01 检测和校准实验室能力认可准则[S].北京:中国计量出版社,2018.(In English:China National Accreditation Service for Conformity Assessment.CNAS-CL01 Accreditation criteria for the competency of testing and calibration laboratories[S].Beijing:China Metrology Publishing House,2018)
[11] 中华人民共和国国家质量监督检验检疫总局.JJG 646-2006 移液器检定规程[S].北京:中国计量出版社,2007.(In English:General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China.JJG 646-2006 Verification regulation of locomotive pipette[S].Beijing:China Metrology Publishing House,2007.)
[12] 中华人民共和国国家质量监督检验检疫总局.JJG 196-2006 常用玻璃量器检定规程[S].北京:中国计量出版社,2007.(In English:General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China.JJG 196-2006 Verification regulation of working glass container[S].Beijing:China Metrology Publishing House,2007)
[13] 刘芳芳,魏秋宁,丁亚磊.氢化物原子荧光法测定尿中砷的不确定度分析[J].环境卫生学杂志,2018,8(4):350-354.(Liu FF,Wei QN,Ding YL.Uncertainty evaluation on the determination of arsenic in urine by hydride generation atomic fluorescence spectrometry[J].J Environ Hyg,2018,8(4):350-354.)