高效液相色谱法测定蔬菜中异菌脲残留量的不确定度分析
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摘要
采用高效液相色谱法对蔬菜中异菌脲残留量的不确定度进行评估。根据JJF 1135—2005《化学分析测量不确定度评定》和JJF 1059.1—2012《测量不确定度评定与表示》中的有关规定,建立测定蔬菜中异菌脲残留量不确定度的数学模型,逐层对不确定度来源进行分析。通过对不确定度分量进行量化和合成,得出当蔬菜中异菌脲残留量为5.31 mg/kg时,其扩展不确定度为0.40 mg/kg(k=2)。结果表明,影响检测结果的主要因素为标准溶液配制、标准曲线拟合和测量重复性等。
The uncertainty of measurement in the determination of iprodione residues in vegetables by high performance liquid chromatography(HPLC) was evaluated.According to the national metrology technical specifications JJF 1135-2005(Evaluation of Uncertainty in Chemical Analysis Measurement) and JJF 1059.1-1999(Evaluation and Expression of Uncertainty in Measurement),a mathematical model was established to evaluate the uncertainty for determining iprodione residues in vegetables.The sources of uncertainty that may be introduced were analyzed and each component of uncertainty was quantified and used to calculate combined uncertainty.The results showed that an expended uncertainty of 5.31 mg/kg(k=2) was obtained for the determination of 0.40 mg/kg of iprodione in vegetables,and the preparation of standard solution,calibration curve fitting and measurement repeatability were the main sources of uncertainty.
The uncertainty of measurement in the determination of iprodione residues in vegetables by high performance liquid chromatography(HPLC) was evaluated.According to the national metrology technical specifications JJF 1135-2005(Evaluation of Uncertainty in Chemical Analysis Measurement) and JJF 1059.1-1999(Evaluation and Expression of Uncertainty in Measurement),a mathematical model was established to evaluate the uncertainty for determining iprodione residues in vegetables.The sources of uncertainty that may be introduced were analyzed and each component of uncertainty was quantified and used to calculate combined uncertainty.The results showed that an expended uncertainty of 5.31 mg/kg(k=2) was obtained for the determination of 0.40 mg/kg of iprodione in vegetables,and the preparation of standard solution,calibration curve fitting and measurement repeatability were the main sources of uncertainty.
引文
[1]宋国春,于建垒,张君亭,等.异菌脲在苹果和土壤中的残留消解动态研究[J].农药,2004,43(4):184-185;180.DOI:10.3969/j.issn.1006-0413.2004.04.014.
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[7]郭藤,李娜,张洋,等.固相萃取-高效液相色谱法测定果蔬中异菌脲残留量[J].分析试验室,2014,33(7):860-863.
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[11]徐秋生,刘俊,贺慧琳,等.SPE-HPLC测定黄瓜、番茄中敌菌灵和异菌脲残留量[J].食品研究与开发,2017,38(3):157-161.DOI:10.3969/j.issn.1005-6521.2017.03.034.
[12]戚向阳.果蔬中6种杀真菌剂残留的固相分散气相色谱检测及基质效应[J].中国食品学报,2012,12(7):178-185.DOI:10.3969/j.issn.1009-7848.2012.07.026.
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[14]王朝杰,李倩,胡玉,等.固相萃取-毛细管气相色谱法测定蔬菜中14种有机氯类农药残留量分析[J].现代农业科技,2016(5):137-139.DOI:10.3969/j.issn.1007-5739.2016.05.079.
[15]赵子丹,牛艳,姜瑞,等.黄瓜及土壤中异菌脲残留量的气相色谱分析[J].湖北农业科学,2015(10):2483-2485.DOI:10.14088/j.cnki.issn0439-8114.2015.10.048.
[16]BLETSOU A A,HANAFI A H,DASENAKI M E,et al.Development of specific LC-ESI-MS/MS methods to determine bifenthrin,lufenuron,and iprodione residue levels in green beans,peas,and chili peppers under egyptian field conditions[J].Food Science and Technology,2013,6(4):1099-1112.
[17]OZGUR G,BULENT K.Evaluation of Qu ECh ERS sample preparation and liquid chromatography-triple-quadrupole mass spectrometry method for the determination of 109 pesticide residues in tomatoes[J].Food Chemistry,2015,176:319-332.DOI:10.1016/j.foodchem.2014.12.083.
[18]关秋艳,方菁,杨万群,等.超高效液相色谱-串联质谱法检测元谋县村民尿液中农药残留[J].中国卫生检验杂志,2016,26(23):3350-3356.
[19]丁葵英,高彦,于金玲,等.凝胶渗透色谱净化高效液相色谱-串联质谱法检测辛辣蔬菜中咪鲜胺等7种农药残留[J].检验检疫学刊,2013,23(5):38-43.DOI:10.3969/j.issn.1674-5354.2013.05.012.
[20]梁林,张爱娟,潘金菊,等.高效液相色谱-串联质谱法测定黄瓜及番茄中异菌脲残留[J].农药科学与管理,2014,35(4):45-48.DOI:10.3969/j.issn.1002-5480.2014.04.010.
[21]蒋永祥,谈金辉,涂红艳,等.气相色谱-质谱法同时测定菠菜中4种二缩甲酰亚胺类杀菌剂的残留量[J].理化检验:化学分册,2011,47(7):813-815.
[22]程志,张蓉,刘韦华,等.气相色谱-串联质谱法快速筛查测定中药材中144种农药残留[J].色谱,2014,32(1):57-68.DOI:10.3724/SP.J.1123.2013.09043.
[23]甘静妮,程雪梅,莫晓君,等.分散固相萃取/气相色谱-三重四极杆串联质谱测定蔬菜和水果中67种农药残留[J].分析测试学报,2016,35(12):1528-1534.
[24]褚能明,孟霞,康月琼,等.分散固相萃取-气相色谱-串联质谱法测定茉莉花茶中86种农药残留[J].食品科学,2016,37(24):239-246.DOI:10.7506/spkx1002-6630-201624038.
[25]胡珅,杨长志,魏冬旭,等.气相色谱-质谱法测定植物源食品中异菌脲残留量[J].检验检疫学刊,2013(4):57-60.DOI:10.3969/j.issn.1674-5354.2013.04.015.
[26]MARTINS J,ESTEVES C,LIMPO-FARIA A,et al.Analysis of six fungicides and one acaricide in still and fortified wines using solid-phase microextraction-gas chromatography/tandem mass spectrometry[J].Food Chemistry,2012,132(1):630-636.DOI:10.1016/j.foodchem.2011.10.102.
[27]CELEIRO M,LLOMPART M,LAMAS J P,et al.Determination of fungicides in white grape bagasse by pressurized liquid extraction and gas chromatography tandem mass spectrometry[J].Journal of Chromatography A,2014,1343:18-25.DOI:10.1016/j.chroma.2014.03.057.
[28]HERRMANN S S,POULSEN M E.Clean-up of cereal extracts for gas chromatography-tandem quadrupole mass spectrometry pesticide residues analysis using primary secondary amine and C18[J].Journal of Chromatography A,2015,1423:47-53.DOI:10.1016/j.chroma.2015.10.086.
[29]中国实验室国家认可委员会.化学分析中不确定度的评估指南:CNAS-GL06:2006[S].北京:中国计量出版社,2006.
[30]国家质量技术监督局.化学分析测量不确定度评定:JJF 1135—2005[S].北京:中国计量出版社,2005.
[31]国家质量技术监督局.测量不确定度评定与表示:JJF 1059.1—2012[S].北京:中国计量出版社,2012.
[32]国家质量技术监督局.蔬菜中异菌脲残留量的测定高效液相色谱法:NY/T 1277—2007[S].北京:中国计量出版社,2007.
[33]国家质量技术监督局.常用玻璃量器检定规程:JJG 196—2006[S].北京:中国计量出版社,2006.
[2]沈群超,陈华才,陆宏,等.异菌脲在不同栽培模式下的降解动态[J].农药,2008,47(1):59-60;63.DOI:10.3969/j.issn.1006-0413.2008.01.020.
[3]国家卫生和计划生育委员会,农业部.食品中农药最大残留限量:GB 2763—2014[S].北京:中国标准出版社,2014.
[4]GIUSEPPE C,DORINA D P,FABRIZIO R,et al.Determination and validation of a simple high-performance liquid chromatographic method for simultaneous assay of iprodione and vinclozolin in human urine[J].Journal of Chromatography B,2005,828(1/2):108-112.DOI:10.1016/j.jchromb.2005.08.025.
[5]D'ARCHIVIO A A,FANELLI M,MAZZEO P,et al.Comparison of different sorbents for multiresidue solid-phase extraction of 16pesticides from groundwater coupled with high-performance liquid chromatography[J].Talanta,2007,71(1):25-30.DOI:10.1016/j.talanta.2006.03.016.
[6]徐秋生,贺慧琳,朱吕,等.高效液相色谱法测定番茄中腐霉利和异菌脲的残留量[J].食品安全质量检测学报,2017,8(2):486-490.DOI:10.3969/j.issn.2095-0381.2017.02.020.
[7]郭藤,李娜,张洋,等.固相萃取-高效液相色谱法测定果蔬中异菌脲残留量[J].分析试验室,2014,33(7):860-863.
[8]潘静,徐妍,马超,等.40%嘧霉·异菌脲悬浮剂的高效液相色谱分析[J].现代农药,2016,15(2):36-38.DOI:10.3969/j.issn.1671-5284.2016.05.012.
[9]成妙金.40%烯酰·异菌脲悬浮剂液相色谱定量分析[J].世界农药,2013,35(2):56-57.DOI:10.3969/j.issn.1009-6485.2013.02.011.
[10]李月茹,孙亮,许煊炜.人参和土壤中异菌脲残留分析[J].安徽农业科学,2012(19):10359-10360.DOI:10.3969/j.issn.0517-6611.2012.19.133.
[11]徐秋生,刘俊,贺慧琳,等.SPE-HPLC测定黄瓜、番茄中敌菌灵和异菌脲残留量[J].食品研究与开发,2017,38(3):157-161.DOI:10.3969/j.issn.1005-6521.2017.03.034.
[12]戚向阳.果蔬中6种杀真菌剂残留的固相分散气相色谱检测及基质效应[J].中国食品学报,2012,12(7):178-185.DOI:10.3969/j.issn.1009-7848.2012.07.026.
[13]ANGIONI A,PORCU L,DEDOLA F.Determination of famoxadone,fenamidone,fenhexamid and iprodione residues in greenhouse tomatoes[J].Pest Management Science,2012,68(4):543-547.DOI:10.1002/ps.2287.
[14]王朝杰,李倩,胡玉,等.固相萃取-毛细管气相色谱法测定蔬菜中14种有机氯类农药残留量分析[J].现代农业科技,2016(5):137-139.DOI:10.3969/j.issn.1007-5739.2016.05.079.
[15]赵子丹,牛艳,姜瑞,等.黄瓜及土壤中异菌脲残留量的气相色谱分析[J].湖北农业科学,2015(10):2483-2485.DOI:10.14088/j.cnki.issn0439-8114.2015.10.048.
[16]BLETSOU A A,HANAFI A H,DASENAKI M E,et al.Development of specific LC-ESI-MS/MS methods to determine bifenthrin,lufenuron,and iprodione residue levels in green beans,peas,and chili peppers under egyptian field conditions[J].Food Science and Technology,2013,6(4):1099-1112.
[17]OZGUR G,BULENT K.Evaluation of Qu ECh ERS sample preparation and liquid chromatography-triple-quadrupole mass spectrometry method for the determination of 109 pesticide residues in tomatoes[J].Food Chemistry,2015,176:319-332.DOI:10.1016/j.foodchem.2014.12.083.
[18]关秋艳,方菁,杨万群,等.超高效液相色谱-串联质谱法检测元谋县村民尿液中农药残留[J].中国卫生检验杂志,2016,26(23):3350-3356.
[19]丁葵英,高彦,于金玲,等.凝胶渗透色谱净化高效液相色谱-串联质谱法检测辛辣蔬菜中咪鲜胺等7种农药残留[J].检验检疫学刊,2013,23(5):38-43.DOI:10.3969/j.issn.1674-5354.2013.05.012.
[20]梁林,张爱娟,潘金菊,等.高效液相色谱-串联质谱法测定黄瓜及番茄中异菌脲残留[J].农药科学与管理,2014,35(4):45-48.DOI:10.3969/j.issn.1002-5480.2014.04.010.
[21]蒋永祥,谈金辉,涂红艳,等.气相色谱-质谱法同时测定菠菜中4种二缩甲酰亚胺类杀菌剂的残留量[J].理化检验:化学分册,2011,47(7):813-815.
[22]程志,张蓉,刘韦华,等.气相色谱-串联质谱法快速筛查测定中药材中144种农药残留[J].色谱,2014,32(1):57-68.DOI:10.3724/SP.J.1123.2013.09043.
[23]甘静妮,程雪梅,莫晓君,等.分散固相萃取/气相色谱-三重四极杆串联质谱测定蔬菜和水果中67种农药残留[J].分析测试学报,2016,35(12):1528-1534.
[24]褚能明,孟霞,康月琼,等.分散固相萃取-气相色谱-串联质谱法测定茉莉花茶中86种农药残留[J].食品科学,2016,37(24):239-246.DOI:10.7506/spkx1002-6630-201624038.
[25]胡珅,杨长志,魏冬旭,等.气相色谱-质谱法测定植物源食品中异菌脲残留量[J].检验检疫学刊,2013(4):57-60.DOI:10.3969/j.issn.1674-5354.2013.04.015.
[26]MARTINS J,ESTEVES C,LIMPO-FARIA A,et al.Analysis of six fungicides and one acaricide in still and fortified wines using solid-phase microextraction-gas chromatography/tandem mass spectrometry[J].Food Chemistry,2012,132(1):630-636.DOI:10.1016/j.foodchem.2011.10.102.
[27]CELEIRO M,LLOMPART M,LAMAS J P,et al.Determination of fungicides in white grape bagasse by pressurized liquid extraction and gas chromatography tandem mass spectrometry[J].Journal of Chromatography A,2014,1343:18-25.DOI:10.1016/j.chroma.2014.03.057.
[28]HERRMANN S S,POULSEN M E.Clean-up of cereal extracts for gas chromatography-tandem quadrupole mass spectrometry pesticide residues analysis using primary secondary amine and C18[J].Journal of Chromatography A,2015,1423:47-53.DOI:10.1016/j.chroma.2015.10.086.
[29]中国实验室国家认可委员会.化学分析中不确定度的评估指南:CNAS-GL06:2006[S].北京:中国计量出版社,2006.
[30]国家质量技术监督局.化学分析测量不确定度评定:JJF 1135—2005[S].北京:中国计量出版社,2005.
[31]国家质量技术监督局.测量不确定度评定与表示:JJF 1059.1—2012[S].北京:中国计量出版社,2012.
[32]国家质量技术监督局.蔬菜中异菌脲残留量的测定高效液相色谱法:NY/T 1277—2007[S].北京:中国计量出版社,2007.
[33]国家质量技术监督局.常用玻璃量器检定规程:JJG 196—2006[S].北京:中国计量出版社,2006.