高效液相色谱串联质谱法测定普洱茶中51种农药残留
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- 英文论文题名：An quantificational method for 51 pesticide residues determination in Pu'er tea by LC-MS/MS
- 论文作者：伍旭东 ; 罗发美 ; 罗正刚 ; 满红平 ; 车涛 ; 吕生
- 英文论文作者：Wu Xu-dong ; Luo Fa-mei ; Luo Zheng-gang ; Man Hong-ping ; Che Tao ; Lv Sheng ; National Center for Pu'er tea Product Quality Supervision and Inspection
- 年：2017
- 作者机构：国家普洱茶产品质量监督检验中心;
- 论文关键词：多农药残留 ; 普洱茶 ; 液相色谱串联质谱
- 英文论文关键词：multi-pesticide residue determination ; Pu'er tea ; LC-MS/MS
- 会议召开时间：2017-09-25
- 会议录名称：第七届云南省科协学术年会论文集——专题一：科普助力精准扶贫
- 语种：中文
- 分类号：O657.63;TS272.7
- 学会代码：SSAD
- 会议名称：第七届云南省科协学术年会
- 会议地点：中国云南普洱
- 主办单位：云南省科学技术协会、中共普洱市委、普洱市人民政府
- 学会名称：云南省机械工程学会
- 页数：11
- 文件大小：131k
- 原文格式：D
- 会议级别：地方
摘要
茶叶农药残留是一个普遍性问题,从保护消费者的角度出发,建立一种高效的检测方法时很有必要的。本研究建立了一种成熟有效的方法,可以同时测定普洱茶中的51中农药残留。茶叶样品首先用乙腈进行提取,再经过固相萃取TPT小柱进行净化,最后通过液相色谱串联质谱的多反应检测模式进行检测,方法通过线性、精密度和添加三个不同浓度的农药的添加回收率对其有效性进行评价。标准曲线的范围为10 ng/m L到100 ng/m L,相关系数大于0.995,三个添加浓度为0.01 mg/kg、0.05 mg/kg、0.11 mg/kg,回收率在72%到89%之间,相关系数小于19%,检出限在0.001 mg/kg到0.01 mg/kg之间。
Pesticide residues in tea is a major issue due to their widely used in tea cultivation.Thus,to protect consumers,an appropriate method for determination of their residues in tea should be done.In this study,a method for the simultaneous determination of 51 pesticides in tea was developed and validated.The tea sample was extracted by acetonitrile and purified SPE clearnet TPT column followed by liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS) with multi-reaction monitoring(MRM) mode.The method was validated according to the linearity,limit of detention,precision,and the percentage of recovery at three different spike levels.The linear concentration range used was 10-100ng/m L,the square of Correlation coefficient r2 was more than >0.995.Recoveries were adequate being in the acceptable range of 72-89% and RSD of <19 % for all the analytes at three level of 0.01,0.05 and 0.11mg/kg,the LOD of all chemicals from 0.001 mg/kg to 0.01 mg/kg.The method was applied for the determination for 400 tea samples collected from Pu'er which contain green tea and black tea.Among the analyzed samples,36 % samples had Imidacloprid and 25% samples contain Acetamiprid,which were at a level below the European Union maximum residue levels(EU-MRLs).The information would be beneficial for Pu'er tea exporters.
Pesticide residues in tea is a major issue due to their widely used in tea cultivation.Thus,to protect consumers,an appropriate method for determination of their residues in tea should be done.In this study,a method for the simultaneous determination of 51 pesticides in tea was developed and validated.The tea sample was extracted by acetonitrile and purified SPE clearnet TPT column followed by liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS) with multi-reaction monitoring(MRM) mode.The method was validated according to the linearity,limit of detention,precision,and the percentage of recovery at three different spike levels.The linear concentration range used was 10-100ng/m L,the square of Correlation coefficient r2 was more than >0.995.Recoveries were adequate being in the acceptable range of 72-89% and RSD of <19 % for all the analytes at three level of 0.01,0.05 and 0.11mg/kg,the LOD of all chemicals from 0.001 mg/kg to 0.01 mg/kg.The method was applied for the determination for 400 tea samples collected from Pu'er which contain green tea and black tea.Among the analyzed samples,36 % samples had Imidacloprid and 25% samples contain Acetamiprid,which were at a level below the European Union maximum residue levels(EU-MRLs).The information would be beneficial for Pu'er tea exporters.
引文
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[3]Cynthia K.Colapinto,Tye E.Arbuckle,Lise Dubois.Tea consumption in pregnancy as a predictor of pesticide exposure and adverse birth outcomes:The MIREC Study.Environmental Research 2015,142:77–83.
[4]H Chen,M Pan,X Liu.Evaluation of transfer rates of multiple pesticides from green tea into infusion using water as pressurized liquid extraction solvent and ultra-performance.Food Chemistry,2017,216:1.
[5]A.Niaz,R.A.Sial1,M.Yaseen,G.A.Mand.Determination of Imidacloprid residues in rice from various districts of Punjab using high performance liquid chromatography.The Journal of Animal&Plant Sciences,2016,26(1):170-176.
[6]Lou Zhenyun,Chen Zongmao,Luo Fengjian.Determination of 92 pesticide residues in tea by gas chromatography with solid-phase extraction.Chinese journal of chromatography,2008,26(5):568-576.
[7]Lu Xiao lei,Zhou Wei long.Overview of Chinese determination standards of pesticides residues in tea.Journal of Food Safety and Quality,2015,6(5):1548-1553.
[8]Hongping Chen,Guanwei Gao,Pingxiang Liu.Determination of 16 Polycyclic Aromatic Hydrocarbons in Tea by Simultaneous Dispersive Solid-Phase Extraction and Liquid–Liquid Extraction Coupled with gas Chromatography-Tandem Mass Spectrometry.Food analytical methods,2016,9:2374-2384.
[9]Chia Chang Wu,Chun Chu,Yei Shung Wang.Multi residue method for high-performance liquid chromatography determination of carbamate pesticides residues in tea samples.Journal of Environmental Science and Health Part B(2009)44,58-68.2374-2384.
[10]Xin Li,Zhaowei Zhang,Peiwu Li.Determination for major chemical contaminants in tea(Camellia sinensis)matrices.Food Research International.2013,53:649-658.
[11]Cai,L.S,Xing,J,Dong,L.Application of polyphenylmethylsiloxane coated fiber for solid-phase microextraction combined with microwave-assisted extraction for the determination of organochlorine pesticides in Chinese teas.Journal of Chromatography.A,1015(1-2),11-21.
[12]Chen G,Cao P,Liu R.A multi-residue method for fast determination of pesticides in tea by ultra performance liquid chromatography-electrospray tandem mass spectrometry combined with modified Qu ECh ERS sample preparation procedure.Food Chemistry,125(4),1406–1411.
[13]XX Zeng,YQ Wan,MY Xie.Simultaneous Determination of Organochlorine and Pyrethroid Pesticide Residues in Tea of Jiangxi Province by GC-ECD.Journal of Analytical Science,2008,24(6):636-640.
[14]Z Lou,Z Chen,F Luo.Determination of 92 pesticide residues in tea by gas chromatography with solid-phase extraction.Chinese Journal of Chromatography,2008,26(5):568-576
[15]B Li,F Zeng,Q Dong.Rapid Determination Method for 12 Pyrethroid Pesticide Residues in Tea by Stir Bar Sorptive Extraction-Thermal Desorption-Gas Chromatography.Physics Procedia,2012,25(22):1776-1780
[16]Cho,S.K,Abd El-Aty,A.M,Choi.Effectiveness of pressurized liquid extraction and solvent extraction for the simultaneous quantification of 14 pesticide residues in green tea using GC.Journal of Separation Science,31(10),1750-1760.
[17]Zhiqiang Huang,Ying Zhang,Libing Wang.Simultaneous determination of 103 pesticide residues in tea samples by LC-MS/MS.J.Sep.Sci.2009,32,1294-1301.
[18]S Liu,Z Zheng,Wei.Simultaneous Determination of Seven Neonicotinoid Pesticide Residues in Food by Ultraperformance Liquid Chromatography Tandem Mass Spectrometry.Journal of Agricultural&Food Chemistry,2017,58(6):3271-3278.
[19]M.D.H.Prodhan,Emmanouil-N,Papadakis,Euphemia Papadopoulou-Mourkidou.Analysis of Pesticide Residues and Their Variability in Cabbage Using Qu ECh ERS Extraction in Combination with LC-MS/MS.Food Anal.Methods.2016.5.
[2]H Chen,Z Hao,Q Wang.Occurrence and risk assessment of organophosphorus pesticide residues in Chinese tea.Human&Ecological Risk Assessment,2016,22(1):28-38.
[3]Cynthia K.Colapinto,Tye E.Arbuckle,Lise Dubois.Tea consumption in pregnancy as a predictor of pesticide exposure and adverse birth outcomes:The MIREC Study.Environmental Research 2015,142:77–83.
[4]H Chen,M Pan,X Liu.Evaluation of transfer rates of multiple pesticides from green tea into infusion using water as pressurized liquid extraction solvent and ultra-performance.Food Chemistry,2017,216:1.
[5]A.Niaz,R.A.Sial1,M.Yaseen,G.A.Mand.Determination of Imidacloprid residues in rice from various districts of Punjab using high performance liquid chromatography.The Journal of Animal&Plant Sciences,2016,26(1):170-176.
[6]Lou Zhenyun,Chen Zongmao,Luo Fengjian.Determination of 92 pesticide residues in tea by gas chromatography with solid-phase extraction.Chinese journal of chromatography,2008,26(5):568-576.
[7]Lu Xiao lei,Zhou Wei long.Overview of Chinese determination standards of pesticides residues in tea.Journal of Food Safety and Quality,2015,6(5):1548-1553.
[8]Hongping Chen,Guanwei Gao,Pingxiang Liu.Determination of 16 Polycyclic Aromatic Hydrocarbons in Tea by Simultaneous Dispersive Solid-Phase Extraction and Liquid–Liquid Extraction Coupled with gas Chromatography-Tandem Mass Spectrometry.Food analytical methods,2016,9:2374-2384.
[9]Chia Chang Wu,Chun Chu,Yei Shung Wang.Multi residue method for high-performance liquid chromatography determination of carbamate pesticides residues in tea samples.Journal of Environmental Science and Health Part B(2009)44,58-68.2374-2384.
[10]Xin Li,Zhaowei Zhang,Peiwu Li.Determination for major chemical contaminants in tea(Camellia sinensis)matrices.Food Research International.2013,53:649-658.
[11]Cai,L.S,Xing,J,Dong,L.Application of polyphenylmethylsiloxane coated fiber for solid-phase microextraction combined with microwave-assisted extraction for the determination of organochlorine pesticides in Chinese teas.Journal of Chromatography.A,1015(1-2),11-21.
[12]Chen G,Cao P,Liu R.A multi-residue method for fast determination of pesticides in tea by ultra performance liquid chromatography-electrospray tandem mass spectrometry combined with modified Qu ECh ERS sample preparation procedure.Food Chemistry,125(4),1406–1411.
[13]XX Zeng,YQ Wan,MY Xie.Simultaneous Determination of Organochlorine and Pyrethroid Pesticide Residues in Tea of Jiangxi Province by GC-ECD.Journal of Analytical Science,2008,24(6):636-640.
[14]Z Lou,Z Chen,F Luo.Determination of 92 pesticide residues in tea by gas chromatography with solid-phase extraction.Chinese Journal of Chromatography,2008,26(5):568-576
[15]B Li,F Zeng,Q Dong.Rapid Determination Method for 12 Pyrethroid Pesticide Residues in Tea by Stir Bar Sorptive Extraction-Thermal Desorption-Gas Chromatography.Physics Procedia,2012,25(22):1776-1780
[16]Cho,S.K,Abd El-Aty,A.M,Choi.Effectiveness of pressurized liquid extraction and solvent extraction for the simultaneous quantification of 14 pesticide residues in green tea using GC.Journal of Separation Science,31(10),1750-1760.
[17]Zhiqiang Huang,Ying Zhang,Libing Wang.Simultaneous determination of 103 pesticide residues in tea samples by LC-MS/MS.J.Sep.Sci.2009,32,1294-1301.
[18]S Liu,Z Zheng,Wei.Simultaneous Determination of Seven Neonicotinoid Pesticide Residues in Food by Ultraperformance Liquid Chromatography Tandem Mass Spectrometry.Journal of Agricultural&Food Chemistry,2017,58(6):3271-3278.
[19]M.D.H.Prodhan,Emmanouil-N,Papadakis,Euphemia Papadopoulou-Mourkidou.Analysis of Pesticide Residues and Their Variability in Cabbage Using Qu ECh ERS Extraction in Combination with LC-MS/MS.Food Anal.Methods.2016.5.