中欧蔬菜农药残留检测方法差异及应对
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摘要
近年来,我国对欧盟出口蔬菜产品屡受欧盟技术性贸易措施的制约。农药残留检测方法方面的差异是主要因素之一。本文通过分析我国出口蔬菜受阻的案例,对比了中欧农药残留检测方法数量、方法标准结构、蔬菜样品检测技术内容和农药残留检测质量控制方面的差异,分析了我国典型出口蔬菜中农药残留检测方法方面与欧盟的差异。在此基础上,提出整合方法标准、提高方法前处理效率、提高方法精密度和灵敏度以及进一步规范检测质量控制4个方面的具体对策。
In recent years, China's export of vegetable products to the European Union(EU) has been affected by technical measures to trade due to the differences between the methods and standards used for the determination of pesticide residues in China and the EU. In this paper, we analyze China's export stumble cases, aiming to find the differences in the number of methods used for pesticide residue determination, the technical details of vegetable detection and the quality control of the standard methods between the country and the EU. Our focus is on the differences between the analytical methods used for typical exported vegetable products in China and the EU. Furthermore, we put forward some countermeasures including integrating the current methods and standards, improving the efficiency of sample pretreatment as well as the precision and sensitivity of the methods, and further standardizing the quality control of the methods.
In recent years, China's export of vegetable products to the European Union(EU) has been affected by technical measures to trade due to the differences between the methods and standards used for the determination of pesticide residues in China and the EU. In this paper, we analyze China's export stumble cases, aiming to find the differences in the number of methods used for pesticide residue determination, the technical details of vegetable detection and the quality control of the standard methods between the country and the EU. Our focus is on the differences between the analytical methods used for typical exported vegetable products in China and the EU. Furthermore, we put forward some countermeasures including integrating the current methods and standards, improving the efficiency of sample pretreatment as well as the precision and sensitivity of the methods, and further standardizing the quality control of the methods.
引文
[1]徐克,李辉尚,马娟娟,等.2015年中国蔬菜进出口贸易状况及展望[J].农业展望,2016,12(5):72-76.DOI:10.3969/j.issn.1673-3908.2016.05.017.
[2]汪漫.2015年国外扣留(召回)我国产品情况分析报告[EB/OL].(2016-04-07)[2016-04-04].http://www.tbtsps.cn/page/tradez/W detainereport content.acti on?id=3 6&lm=008002.
[3]王文君,陈琼.欧盟最新食品农药残留限量标准研究[J].WTO经济导刊,2015(2):90-92.DOI:10.3969/j.issn.1672-1160.2015.02.037.
[4]蒋玉宝,周科清,刘莹,等.中国与欧盟苹果农药残留限量标准概况[J].中国农学通报,2013,29(4):195-199.DOI:10.3969/j.issn.1000-6850.2013.04.037.
[5]王涛,廖炯峰,张毅,等.蓝莓农药残留限量标准比较分析[J].世界农业,2015(10):118-123.DOI:10.13856/j.cnll-1097/s.2015.10.027.
[6]焦知岳,赵凌云.欧盟茶叶农药残留限量措施对中国茶叶出口的影响及对策[J].世界农业,2015(6):132-136.DOI:10.13856/j.cnll-1097/s.2015.06.028.
[7]中国技术性贸易措施网.欧盟召回我国食品数据[EB/OL].(2016-12-31)[2014-02-06].http://www.tbtsps.cn/page/tradez/Wdetainderecall.action.
[8]农业部.食品安全国家标准食品中农药最大残留限量:GB/T2763-2016[S].北京:中国标准出版社,2016:1-9.
[9]EU Reference Laboratories for Residues of Pesticides.EURLDataPool(NEW)[EB/OL].(2017-03-02)[2014-01-01].http://www.eurl-pesticides.eu/docs/public/tmplt_article.asp?CntID=629&LabID=100&Lang=EN.
[10]农业部.农药残留检测方法国家标准编制指南:农业部2386号公告[EB/OL].(2016-04-14)[2016-04-11].http://www.moa.gov.cn/govpublic/ZZYGLS/201604/t20160413_5093548.htm.
[11]国家质量监督检验检疫总局.水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法:GB/T20769-2008[S].北京:中国标准出版社,2008:1-73.
[12]国家质量监督检验检疫总局.食品安全国家标准水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法:GB 23200.8—2016[S].北京:中国标准出版社,2016:1-60.
[13]农业部.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:NY/T761-2008[S].北京:中国标准出版社,2008:1-30.
[14]卫生部.植物性食品中二嗉磷残留量的测定:GB/T 5009.107-2003[S].北京:中国标准出版社,2013:1-34.
[15]卫生部.水果和蔬菜中多种农药残留量的测定:GB/T 5009.218—2008[S].北京:中国标准出版社,2008:1-44.
[16]农业部.食品安全国家标准食品中苯醚甲环唑残留量的测定气相色谱-质谱法:GB 23200.49-2016[S].北京:中国标准出版社,2016:1-2.
[17]农业部.蔬菜中334种农药多残留的测定气相色谱质谱法和液相色谱质谱法:NY/T 1379—2007[S].北京:中国标准出版社,2007:1-21.
[18]DG SANCO European Commission.Pesticide analysis in fruits and vegetables by microflow liquid chromatography coupled to mass spectrometry:EURL-FV(2014-M15)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-16.
[19]DG SANCO European Commission.Multiresidue method using QuEChERS followed by GC-QqQ-MS/MS and LC-QqQ-MS/MS for fruits and vegetables:EURL-FV(2010-M1)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-18.
[20]DG SANCO European Commission.Validation data for the analysis of chlorotalonil in leek using Mini-Luke method followed by GCQqQ-MS/MS:EURL-FV(2010-M2)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-6.
[21]DG SANCO European Commission.Multiresidue method using Mini-Luke followed by GC-QqQ-MS-MS for fruits and vegetables:EURL-FV(2010-M3)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-10.
[22]DG SANCO European Commission.Analysis of pesticide residues in fruit and vegetables with ethyl acetate extraction using gas and liquid chromatography with tandem mass spectrometric detection:EURL-FV(2010-M4)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-33.
[23]DG SANCO European Commission.Validation data of 127 pesticides using a multiresidue method by LC-MS/MS and GC-MS/MS in olive oil:EURL-FV(2012-M6)[S].European Union Reference Laboratory in Pesticide Residue,2012:1-16.
[24]DG SANCO European Commission.Accurate mass pesticide database by LC-HRMS:EURL-FV(2012-M7)[S].European Union Reference Laboratory in Pesticide Residue,2012:1-21.
[25]DG SANCO European Commission.Pesticide analysis in teas and chamomile by liquid chromatography and gas chromatography tandem mass spectrormetry:EURL-FV(2013-M8)[S].European Union Reference Laboratory in Pesticide Residue,2013:1-19.
[26]DG SANCO European Commission.Validation data of five selected pesticides using QuEChERS by linquid chromatography tandem massspectrometry:EURL-FV(2013-M9)[S].European Union Reference Laboratory in Pesticide Residue,2013:1-10.
[27]DG SANCO European Commission.Determination of pesticide residues in avocado and almond by liquid and gas chromatography tandem mass spectrometry:EURL-FV(2014-M11)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-32.
[28]DG SANCO European Commission.Dutch Mini-Luke("NL-")extraction method followed by LC and GC-MS/MS for multi-residue analysis of pesticides in fruits and vegetables:EURL-FV(2014-M12)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-19.
[29]DG SANCO European Commission.Evaluation of extract backgrounds for MRM-pes tic ides(QuECHERS)in fruits and vegetables:EURL-FV(2014-M13)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-5.
[30]DG SANCO European Commission.High-resolution accuracy-mass method for the screening of a wide range of pesticides in different fruit and vegetable matrices:EURL-FV(2014-M16)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-5.
[31]DG SANCO European Commission.Accurate mass pesticide database by GC-HRMS:EURL-FV(2015-M17)[S].European Union Reference Laboratory in Pesticide Residue,2015:1-12.
[32]DG SANCO European Commission.Evaluation of interferences between matrix-analyte for the correct identification of the pesticides by GC-QqQMS/MS and LC-QqQ-MS/MS:EURL-FV(2015-M18)[S].European Union Reference Laboratory in Pesticide Residue,2015:1-21.
[33]DG SANCO European Commission.LC-QTOF-MS/MS method for the simultaneous full scan and MS/MS analysis of pesticides in fruit and vegetables:EURL-FV(2015-M19)[S].European Union Reference Laboratory in Pesticide Residue,2015:1-10.
[34]马琳,唐伟,陈建波,等.QuEchERS-液相色谱串联质谱法测定复杂基质蔬菜中四聚乙醛残留量[J].上海农业学报,2015,31(4):40-45.DOI:10.15955/j.issn1000-3924.2015.04.08.
[35]贺泽英,刘潇威.农产品中农药残留分析技术研究进展[J].农业资源与环境学报,2016,33(4):310-319.DOI:10.13254/j.jare.2016.0076.
[36]European Commission.Guidance document on analytical quality control and method validation procedures for pesticide residues analysis in food and feed:DG SANCO/110945/2015[S].Sweden,2015:1-42.
[2]汪漫.2015年国外扣留(召回)我国产品情况分析报告[EB/OL].(2016-04-07)[2016-04-04].http://www.tbtsps.cn/page/tradez/W detainereport content.acti on?id=3 6&lm=008002.
[3]王文君,陈琼.欧盟最新食品农药残留限量标准研究[J].WTO经济导刊,2015(2):90-92.DOI:10.3969/j.issn.1672-1160.2015.02.037.
[4]蒋玉宝,周科清,刘莹,等.中国与欧盟苹果农药残留限量标准概况[J].中国农学通报,2013,29(4):195-199.DOI:10.3969/j.issn.1000-6850.2013.04.037.
[5]王涛,廖炯峰,张毅,等.蓝莓农药残留限量标准比较分析[J].世界农业,2015(10):118-123.DOI:10.13856/j.cnll-1097/s.2015.10.027.
[6]焦知岳,赵凌云.欧盟茶叶农药残留限量措施对中国茶叶出口的影响及对策[J].世界农业,2015(6):132-136.DOI:10.13856/j.cnll-1097/s.2015.06.028.
[7]中国技术性贸易措施网.欧盟召回我国食品数据[EB/OL].(2016-12-31)[2014-02-06].http://www.tbtsps.cn/page/tradez/Wdetainderecall.action.
[8]农业部.食品安全国家标准食品中农药最大残留限量:GB/T2763-2016[S].北京:中国标准出版社,2016:1-9.
[9]EU Reference Laboratories for Residues of Pesticides.EURLDataPool(NEW)[EB/OL].(2017-03-02)[2014-01-01].http://www.eurl-pesticides.eu/docs/public/tmplt_article.asp?CntID=629&LabID=100&Lang=EN.
[10]农业部.农药残留检测方法国家标准编制指南:农业部2386号公告[EB/OL].(2016-04-14)[2016-04-11].http://www.moa.gov.cn/govpublic/ZZYGLS/201604/t20160413_5093548.htm.
[11]国家质量监督检验检疫总局.水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法:GB/T20769-2008[S].北京:中国标准出版社,2008:1-73.
[12]国家质量监督检验检疫总局.食品安全国家标准水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法:GB 23200.8—2016[S].北京:中国标准出版社,2016:1-60.
[13]农业部.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:NY/T761-2008[S].北京:中国标准出版社,2008:1-30.
[14]卫生部.植物性食品中二嗉磷残留量的测定:GB/T 5009.107-2003[S].北京:中国标准出版社,2013:1-34.
[15]卫生部.水果和蔬菜中多种农药残留量的测定:GB/T 5009.218—2008[S].北京:中国标准出版社,2008:1-44.
[16]农业部.食品安全国家标准食品中苯醚甲环唑残留量的测定气相色谱-质谱法:GB 23200.49-2016[S].北京:中国标准出版社,2016:1-2.
[17]农业部.蔬菜中334种农药多残留的测定气相色谱质谱法和液相色谱质谱法:NY/T 1379—2007[S].北京:中国标准出版社,2007:1-21.
[18]DG SANCO European Commission.Pesticide analysis in fruits and vegetables by microflow liquid chromatography coupled to mass spectrometry:EURL-FV(2014-M15)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-16.
[19]DG SANCO European Commission.Multiresidue method using QuEChERS followed by GC-QqQ-MS/MS and LC-QqQ-MS/MS for fruits and vegetables:EURL-FV(2010-M1)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-18.
[20]DG SANCO European Commission.Validation data for the analysis of chlorotalonil in leek using Mini-Luke method followed by GCQqQ-MS/MS:EURL-FV(2010-M2)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-6.
[21]DG SANCO European Commission.Multiresidue method using Mini-Luke followed by GC-QqQ-MS-MS for fruits and vegetables:EURL-FV(2010-M3)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-10.
[22]DG SANCO European Commission.Analysis of pesticide residues in fruit and vegetables with ethyl acetate extraction using gas and liquid chromatography with tandem mass spectrometric detection:EURL-FV(2010-M4)[S].European Union Reference Laboratory in Pesticide Residue,2010:1-33.
[23]DG SANCO European Commission.Validation data of 127 pesticides using a multiresidue method by LC-MS/MS and GC-MS/MS in olive oil:EURL-FV(2012-M6)[S].European Union Reference Laboratory in Pesticide Residue,2012:1-16.
[24]DG SANCO European Commission.Accurate mass pesticide database by LC-HRMS:EURL-FV(2012-M7)[S].European Union Reference Laboratory in Pesticide Residue,2012:1-21.
[25]DG SANCO European Commission.Pesticide analysis in teas and chamomile by liquid chromatography and gas chromatography tandem mass spectrormetry:EURL-FV(2013-M8)[S].European Union Reference Laboratory in Pesticide Residue,2013:1-19.
[26]DG SANCO European Commission.Validation data of five selected pesticides using QuEChERS by linquid chromatography tandem massspectrometry:EURL-FV(2013-M9)[S].European Union Reference Laboratory in Pesticide Residue,2013:1-10.
[27]DG SANCO European Commission.Determination of pesticide residues in avocado and almond by liquid and gas chromatography tandem mass spectrometry:EURL-FV(2014-M11)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-32.
[28]DG SANCO European Commission.Dutch Mini-Luke("NL-")extraction method followed by LC and GC-MS/MS for multi-residue analysis of pesticides in fruits and vegetables:EURL-FV(2014-M12)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-19.
[29]DG SANCO European Commission.Evaluation of extract backgrounds for MRM-pes tic ides(QuECHERS)in fruits and vegetables:EURL-FV(2014-M13)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-5.
[30]DG SANCO European Commission.High-resolution accuracy-mass method for the screening of a wide range of pesticides in different fruit and vegetable matrices:EURL-FV(2014-M16)[S].European Union Reference Laboratory in Pesticide Residue,2014:1-5.
[31]DG SANCO European Commission.Accurate mass pesticide database by GC-HRMS:EURL-FV(2015-M17)[S].European Union Reference Laboratory in Pesticide Residue,2015:1-12.
[32]DG SANCO European Commission.Evaluation of interferences between matrix-analyte for the correct identification of the pesticides by GC-QqQMS/MS and LC-QqQ-MS/MS:EURL-FV(2015-M18)[S].European Union Reference Laboratory in Pesticide Residue,2015:1-21.
[33]DG SANCO European Commission.LC-QTOF-MS/MS method for the simultaneous full scan and MS/MS analysis of pesticides in fruit and vegetables:EURL-FV(2015-M19)[S].European Union Reference Laboratory in Pesticide Residue,2015:1-10.
[34]马琳,唐伟,陈建波,等.QuEchERS-液相色谱串联质谱法测定复杂基质蔬菜中四聚乙醛残留量[J].上海农业学报,2015,31(4):40-45.DOI:10.15955/j.issn1000-3924.2015.04.08.
[35]贺泽英,刘潇威.农产品中农药残留分析技术研究进展[J].农业资源与环境学报,2016,33(4):310-319.DOI:10.13254/j.jare.2016.0076.
[36]European Commission.Guidance document on analytical quality control and method validation procedures for pesticide residues analysis in food and feed:DG SANCO/110945/2015[S].Sweden,2015:1-42.