气相色谱法探究果蔬中有机氯和拟除虫菊酯类农药残留的基质效应
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摘要
[目的]应用农业标准方法NY/T 761—2008,考察气相色谱法(GC-ECD)同时测定水果和蔬菜基质中有机氯和拟除虫菊酯类农药残留的基质效应。[方法]选用15种水果和蔬菜上机液作为溶剂,将20种有机氯和拟除虫菊酯类农药配制成4个不同质量浓度水平的混合标准溶液,与同等质量浓度水平下的溶剂标准溶液进行比较,得出各种农药在不同浓度水平下不同基质中的绝对基质效应。[结果] 15种水果和蔬菜对20种有机氯和拟除虫菊酯类农药均存在不同程度的基质效应,梨、香蕉、黄瓜中各农药的基质效应与农药的浓度和种类没有很强的关联性,表现为弱基质效应;有机氯类农药受基质效应的影响显著高于拟除虫菊酯类农药;基质效应的强弱和待测物的质量浓度之间存在着一定的相关性,在低浓度水平更易产生显著的基质效应。[结论]检测水果和蔬菜中有机氯和拟除虫菊酯类农药残留时,建议采用基质配制的标准品进行定量检测,从而保证检测结果的准确性。
[Aims] Application of agricultural standard method NY/T 761—2008, matrix effects of organochlorine and pyrethroid pesticides have been studied by GC-ECD. [Methods] 15 Kinds of vegetables determined to have no pesticides by GC-ECD were selected, and 20 kinds of organochlorine and pyrethroid pesticides standard were mixed in the 15 kinds of vegetables matrix at 4 different concentrations levels. And they were compared with the same concentration levels of pesticide standard solution with pure acetone as solvent. [Results] 15 Kinds of fruits and vegetables had different degree of matrix effects on 20 organochlorine and pyrethroid pesticides residues, different types of pesticides in pear, banana and cucumber have week matrix effects with concentration, and the matrix effect of organochlorine was much more significant. There was relevance between the strength of matrix effects and the concentration of determinand. [Conclusions] It is recommendable to apply the matrix-matched external standard method on the determination of organochlorine and pyrethroid pesticides in real samples, so as to ensure the accuracy of the detection results.
[Aims] Application of agricultural standard method NY/T 761—2008, matrix effects of organochlorine and pyrethroid pesticides have been studied by GC-ECD. [Methods] 15 Kinds of vegetables determined to have no pesticides by GC-ECD were selected, and 20 kinds of organochlorine and pyrethroid pesticides standard were mixed in the 15 kinds of vegetables matrix at 4 different concentrations levels. And they were compared with the same concentration levels of pesticide standard solution with pure acetone as solvent. [Results] 15 Kinds of fruits and vegetables had different degree of matrix effects on 20 organochlorine and pyrethroid pesticides residues, different types of pesticides in pear, banana and cucumber have week matrix effects with concentration, and the matrix effect of organochlorine was much more significant. There was relevance between the strength of matrix effects and the concentration of determinand. [Conclusions] It is recommendable to apply the matrix-matched external standard method on the determination of organochlorine and pyrethroid pesticides in real samples, so as to ensure the accuracy of the detection results.
引文
[1] ERNEY D R, GILLESPIE A M, GILVYDIS D M, et al.Explanation of the Matrix-induced Chromatographic Response Enhancement of Organophosphorus Pesticides During Open Tubular Column Gas Chromatography with Splitless or Hot on-Column Injection and Flame Photometric Detection[J].J Chromatogr, 1993, 638(1):57-63.
[2]王贵双,高丽华,孙晶,等.基质效应对气相色谱-质谱法测定粮谷中17种有机氯和拟除虫菊酯农药残留影响的研究[J].中国酿造, 2012, 31(11):169-172.
[3]宋春满,和智君,田丽梅,等.有机氯农药残留气相色谱法测定中的基质效应[J].农药, 2013, 52(10):745-746.
[4]罗俊霞,符建伟,李德瑜,等. 14种有机磷农药在9种蔬菜中的基质效应研究[J].湖北农业科学, 2013(23):5858-5862.
[5]刘莉,袁名安,盛仙俏,等.基质效应对黄瓜中4种有机磷农药残留检测的影响[J].浙江农业学报, 2014, 26(6):1564-1567.
[6]陈韵贤,吴春梅,梁志刚,等. 30种有机磷农药残留在5种蔬菜中的基质效应比较[J].现代农业科技, 2015(13):147-150.
[7]叶宇飞,许秀琴,王立君,等.气相色谱法测定蔬菜水果中农药残留的基质效应研究[J].安徽农学通报, 2015, 21(5):114-117.
[8]吴姻如,汤旭东,孙超斌,等.基质效应对瓜类蔬菜中有机磷农药残留测定的影响研究[J].农产品质量与安全, 2016(4):62-64.
[9]叶倩,邓义才,路大海,等.气相色谱法测定蔬菜水果中氟虫腈等6种农药残留[J].农药, 2016, 55(1):51-54.
[10]姚勇,刘全科.多种蔬菜基质对有机磷农药残留检测的基质效应的研究[J].湖北植保, 2016(2):14-17.
[11]张利强,程盛华,李琪,等.气相色谱法测定谷物中9种有机磷农药残留量的基质效应[J].理化检验(化学分册), 2016, 52(2):136-140.
[12]顾亚萍,乔方,林慧纯,等. 4种蔬菜中20种农药残留的基质效应的研究[J].食品研究与开发, 2017, 38(22):148-152.
[13]范君,刘腾飞,杨代凤,等.不同基质效应对蔬菜中有机磷农药残留检测的影响[J].食品安全质量检测学报, 2017, 8(9):3543-3548.
[14]李丽春,刘书贵,尹怡,等.气相色谱法检测水产品中拟除虫菊酯类农药的基质效应研究[J].现代食品科技, 2018, 34(4):270-280.
[15]罗贵文,郭儒敏,牙家璇,等.不同芒果品种中基质效应对16种有机磷农药残留检测的影响[J].农业科技通讯, 2018(3):129-132.
[16]王圆圆.基质效应对六种蔬菜中啶虫脒和吡虫啉检测的影响[J].农业开发与装备, 2018(4):87-89.
[17]黄宝勇.果蔬中农药多残留的气相色谱-质谱方法与基质效应的研究(硕士论文)[D].北京:中国农业大学, 2005.
[18]贺利民,刘祥国,曾振灵.气相色谱分析农药残留的基质效应及其解决方法[J].色谱, 2008, 26(1):98-104.
[19]杨旭,汤佳峰,巢文君.基质效应对有机磷农药测定的影响及解决方法[J].分析测试学报, 2009, 28(12):1368-1372.
[20]刘莉,罗军.基质效应对气相色谱分析有机磷农药残留的影响和解决方法[J].江西农业学报, 2009, 21(7):146-148.
[21]商鲁宁.农药残留检测过程中基质效应的研究进展[J].安徽农业科学, 2017, 45(12):73-75.
[22]于建华,朱梅华,吉绍长,等.色谱法测定多种农药残留的基质效应研究进展[J].广东化工, 2017, 44(3):101-104.
[23]张艳丽,韩木先. NY/T 761—2008.标准方法中蔬菜样品前处理过程应注意的问题[J].理化检验-化学分析, 2015, 51(8):1130-1132.
[24]鲍忠赞.基质效应在农药残留检测中的研究现状及进展[J].食品安全导刊, 2018(1):88-89.
[25]中华人民共和国农业部. NY/T 761—2008.蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].北京:中国农业出版社, 2008.
[26] LEHOTAY STEVEN J, KATERINA M. Evaluation of Two Fast and Easy Methods for Pesticide Residue Analysis in Fatty Food Matrixes[J]. J AOAC Inter, 2005, 88(2):615-629.
[27] MARTINEZ-VIDAL J L, ARREBOLA F J, GARRIDO F A.Validation of a Gas Chromatographic-tandem Mass Spectrometric Method for Analysis of Pesticide Residues in Six Food Commodities Selection of a Reference Matrix for Calibration[J].Chromatographia, 2004, 59:321-327.
[2]王贵双,高丽华,孙晶,等.基质效应对气相色谱-质谱法测定粮谷中17种有机氯和拟除虫菊酯农药残留影响的研究[J].中国酿造, 2012, 31(11):169-172.
[3]宋春满,和智君,田丽梅,等.有机氯农药残留气相色谱法测定中的基质效应[J].农药, 2013, 52(10):745-746.
[4]罗俊霞,符建伟,李德瑜,等. 14种有机磷农药在9种蔬菜中的基质效应研究[J].湖北农业科学, 2013(23):5858-5862.
[5]刘莉,袁名安,盛仙俏,等.基质效应对黄瓜中4种有机磷农药残留检测的影响[J].浙江农业学报, 2014, 26(6):1564-1567.
[6]陈韵贤,吴春梅,梁志刚,等. 30种有机磷农药残留在5种蔬菜中的基质效应比较[J].现代农业科技, 2015(13):147-150.
[7]叶宇飞,许秀琴,王立君,等.气相色谱法测定蔬菜水果中农药残留的基质效应研究[J].安徽农学通报, 2015, 21(5):114-117.
[8]吴姻如,汤旭东,孙超斌,等.基质效应对瓜类蔬菜中有机磷农药残留测定的影响研究[J].农产品质量与安全, 2016(4):62-64.
[9]叶倩,邓义才,路大海,等.气相色谱法测定蔬菜水果中氟虫腈等6种农药残留[J].农药, 2016, 55(1):51-54.
[10]姚勇,刘全科.多种蔬菜基质对有机磷农药残留检测的基质效应的研究[J].湖北植保, 2016(2):14-17.
[11]张利强,程盛华,李琪,等.气相色谱法测定谷物中9种有机磷农药残留量的基质效应[J].理化检验(化学分册), 2016, 52(2):136-140.
[12]顾亚萍,乔方,林慧纯,等. 4种蔬菜中20种农药残留的基质效应的研究[J].食品研究与开发, 2017, 38(22):148-152.
[13]范君,刘腾飞,杨代凤,等.不同基质效应对蔬菜中有机磷农药残留检测的影响[J].食品安全质量检测学报, 2017, 8(9):3543-3548.
[14]李丽春,刘书贵,尹怡,等.气相色谱法检测水产品中拟除虫菊酯类农药的基质效应研究[J].现代食品科技, 2018, 34(4):270-280.
[15]罗贵文,郭儒敏,牙家璇,等.不同芒果品种中基质效应对16种有机磷农药残留检测的影响[J].农业科技通讯, 2018(3):129-132.
[16]王圆圆.基质效应对六种蔬菜中啶虫脒和吡虫啉检测的影响[J].农业开发与装备, 2018(4):87-89.
[17]黄宝勇.果蔬中农药多残留的气相色谱-质谱方法与基质效应的研究(硕士论文)[D].北京:中国农业大学, 2005.
[18]贺利民,刘祥国,曾振灵.气相色谱分析农药残留的基质效应及其解决方法[J].色谱, 2008, 26(1):98-104.
[19]杨旭,汤佳峰,巢文君.基质效应对有机磷农药测定的影响及解决方法[J].分析测试学报, 2009, 28(12):1368-1372.
[20]刘莉,罗军.基质效应对气相色谱分析有机磷农药残留的影响和解决方法[J].江西农业学报, 2009, 21(7):146-148.
[21]商鲁宁.农药残留检测过程中基质效应的研究进展[J].安徽农业科学, 2017, 45(12):73-75.
[22]于建华,朱梅华,吉绍长,等.色谱法测定多种农药残留的基质效应研究进展[J].广东化工, 2017, 44(3):101-104.
[23]张艳丽,韩木先. NY/T 761—2008.标准方法中蔬菜样品前处理过程应注意的问题[J].理化检验-化学分析, 2015, 51(8):1130-1132.
[24]鲍忠赞.基质效应在农药残留检测中的研究现状及进展[J].食品安全导刊, 2018(1):88-89.
[25]中华人民共和国农业部. NY/T 761—2008.蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].北京:中国农业出版社, 2008.
[26] LEHOTAY STEVEN J, KATERINA M. Evaluation of Two Fast and Easy Methods for Pesticide Residue Analysis in Fatty Food Matrixes[J]. J AOAC Inter, 2005, 88(2):615-629.
[27] MARTINEZ-VIDAL J L, ARREBOLA F J, GARRIDO F A.Validation of a Gas Chromatographic-tandem Mass Spectrometric Method for Analysis of Pesticide Residues in Six Food Commodities Selection of a Reference Matrix for Calibration[J].Chromatographia, 2004, 59:321-327.