多壁碳纳米管净化-液相色谱串联质谱法测定瓜菜中双酰胺类杀虫剂
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摘要
目的建立多壁碳纳米管净化,超高效液相色谱串联质谱技术同时测定瓜菜中3种双酰胺类杀虫剂残留的分析方法。方法瓜菜样品用乙腈提取后,经多壁碳纳米管净化,超高效液相色谱-电喷雾电离串联质谱法测定。结果3种双酰胺类杀虫剂在0.005～0.1 mg/L范围内线性良好,相关系数均大于0.99,定量限均为5μg/kg,平均加标回收率在71.7%～99.1%之间,相对标准偏差在0.6%～3.5%之间。与N-丙基乙二胺和石墨化炭黑吸附剂相比,多壁碳纳米管具有更好的净化性能。结论该方法具有简单灵敏、定量准确等优点,可用于瓜菜中3种双酰胺类杀虫剂残留的检测。
Objective To establish a multi-residue method for the simultaneous determination of 3 diamide insecticide residues in melons and vegetables by multiwalled carbon nanotubes purification coupled with ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods The melon and vegetable samples were extracted with acetonitrile and cleaned up with multiwalled carbon nanotubes, then determined by UPLC-MS/MS. Results Three kinds of diamide insecticide had good linear relationships in the range of 0.005-0.1 mg/L, and the correlation coefficients were larger than 0.99. The limits of quantitation for 3 diamide insecticide were all 5 μg/kg. Calibration curves exhibited good linearity over the concentration range from 0.005 to0.1 mg/L. Average recoveries for 3 diamide insecticide were 71.7%-99.1%, with relative standard deviations ranged of 0.6%-3.5%. Compared with primary secondary amine and graphited carbon black sorbent, the multiwalled carbon nanotube had better purification performance. Conclusion The developed method is simple, sensitive, and accurate,which can be used for determination of 3 diamide insecticide residues in melons and vegetables.
Objective To establish a multi-residue method for the simultaneous determination of 3 diamide insecticide residues in melons and vegetables by multiwalled carbon nanotubes purification coupled with ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods The melon and vegetable samples were extracted with acetonitrile and cleaned up with multiwalled carbon nanotubes, then determined by UPLC-MS/MS. Results Three kinds of diamide insecticide had good linear relationships in the range of 0.005-0.1 mg/L, and the correlation coefficients were larger than 0.99. The limits of quantitation for 3 diamide insecticide were all 5 μg/kg. Calibration curves exhibited good linearity over the concentration range from 0.005 to0.1 mg/L. Average recoveries for 3 diamide insecticide were 71.7%-99.1%, with relative standard deviations ranged of 0.6%-3.5%. Compared with primary secondary amine and graphited carbon black sorbent, the multiwalled carbon nanotube had better purification performance. Conclusion The developed method is simple, sensitive, and accurate,which can be used for determination of 3 diamide insecticide residues in melons and vegetables.
引文
[1]刘子记,贺滉,杨衍,等.海南冬季瓜菜播种面积变化趋势分析[J].中国蔬菜,2016, 4:6-8.Liu ZJ, He H, Yang Y, et al. Analysis of variation trend of seeding area of winter melons and vegetables in Hainan[J]. China Veg, 2016,(4):6-8.
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[3]赵平,严秋旭,李新,等.双酰胺类杀虫剂的现状与展望[J].农药科学与管理,2015, 36(11):23-29.Zhao P, Yan QX, Li X, et al. Status and perspective of diamide insecticides[J]. Pestic Sci Adm,2015, 36(11):23-29.
[4]GB 2763-2016食品安全国家标准食品中农药残留最大限量[S].GB 2763-2016 National food safety standard-Maximum residue limits for pesticides in food[S].
[5] Anastassuade M, Lehotay SJ, Stajnbaher D, et al. Fast and easy multi-residue method employing acetonitrile extraction/partitioning an"dispersive solid-phase extraction"for the determination of pesticide residues in produce[J]. J AO AC Int, 2003, 86(2):412-431.
[6] Ozgur G, Bulent K. Evaluation of QuEChERS sample preparation and liquid chromatography-triple-quadrupole mass spectrometry method for the determination of 109 pesticide residues in tomatoes[J]. Food Chem,2015,(176):319-332.
[7] Wu CC. Multiresidue method for the determination of pesticides in Oolong tea using QuEChERS by gas chromatography-triple quadrupole tandem mass spectrometry[J]. Food Chem, 2017,(229):580-587.
[8]Han Y, Zou N, Song L, et al. Simultaneous determination of 70 pesticide residues in leek, leaf lettuce and garland chrysanthemum using modified QuEChERS method with multi-walled carbon nanotubes as reversed-dispersive solid-phase extraction materials[J]. J Chromatogr B,2015, 1005:56-64.
[9] Zou N, Han YT, Li YJ, et al. Multiresidue method for determination of183 pesticide residues inleeks by rapid multiplug filtration cleanup and gas chromatography-tandem mass spectrometry[J]. J Agric Food Chem, 2016,64(31):6061-6070.
[10] Lehoty SJ, Mary ON, Jose T, et al. Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate[J]. J AO AC Int, 2007, 90(2):485-520.
[11] European Standard EN 15662:Foods of plant origin-Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by Dispersive SPEQuEChERS-method[S].
[12]田海英,韦风杰,张东豫,等.RP-HPLC法测定烟草中的质体色素[J].烟草科技,2009,49(7):32-36.Tian HY, Wei FJ, Zhang DY, et al. Determination of plastid pigments in tobacco leaf by reversed-phase high performance liquid chromatography[J]. Tob Sci Technol, 2009, 49(7):32-36.
[13] NY/T 788-2004农药残留试验准则[S].NY/T 788-2004 Guideline on pesticide residue trials[S].
[14] Rutkowska E, Lozowicka B, Kaczynski P. Modification of multiresidue QuEChERS protocol to minimize matrix effect and improve recoveries for determination of pesticide residues in dried herbs followed by GC-MS/MS[J]. Food Anal Methods, 2018, 11(3):709-724.
[15] Kim YA, El-Aty AMA, Rahman MM, et al. Method development, matrix effect, and risk assessment of 49 multiclass pesticides in kiwifruit using liquid chromatography coupled to tandem mass spectrometry[J]. J Chromatogr B, 2018, 1076:130-138.
[16] Pavel S, Daniel S, Katerina P, et al. Development of matrix effect-free MISPE UHPLC-MS/MS method for determination of lovastatin in Pu-erh tea, oyster mushroom, and red yeast rice[J]. J Pharm Biomed Anal, 2017,140:367-376.
[2]侯媛媛.海南省冬季瓜菜产业发展及价格形成研究[J].世界热带农业信息,2016.(8):9-15.Hou YY. Industry development and price formation of winter vegetables in Hainan[J]. World Trop Agric Inf, 2016,(8):9-15.
[3]赵平,严秋旭,李新,等.双酰胺类杀虫剂的现状与展望[J].农药科学与管理,2015, 36(11):23-29.Zhao P, Yan QX, Li X, et al. Status and perspective of diamide insecticides[J]. Pestic Sci Adm,2015, 36(11):23-29.
[4]GB 2763-2016食品安全国家标准食品中农药残留最大限量[S].GB 2763-2016 National food safety standard-Maximum residue limits for pesticides in food[S].
[5] Anastassuade M, Lehotay SJ, Stajnbaher D, et al. Fast and easy multi-residue method employing acetonitrile extraction/partitioning an"dispersive solid-phase extraction"for the determination of pesticide residues in produce[J]. J AO AC Int, 2003, 86(2):412-431.
[6] Ozgur G, Bulent K. Evaluation of QuEChERS sample preparation and liquid chromatography-triple-quadrupole mass spectrometry method for the determination of 109 pesticide residues in tomatoes[J]. Food Chem,2015,(176):319-332.
[7] Wu CC. Multiresidue method for the determination of pesticides in Oolong tea using QuEChERS by gas chromatography-triple quadrupole tandem mass spectrometry[J]. Food Chem, 2017,(229):580-587.
[8]Han Y, Zou N, Song L, et al. Simultaneous determination of 70 pesticide residues in leek, leaf lettuce and garland chrysanthemum using modified QuEChERS method with multi-walled carbon nanotubes as reversed-dispersive solid-phase extraction materials[J]. J Chromatogr B,2015, 1005:56-64.
[9] Zou N, Han YT, Li YJ, et al. Multiresidue method for determination of183 pesticide residues inleeks by rapid multiplug filtration cleanup and gas chromatography-tandem mass spectrometry[J]. J Agric Food Chem, 2016,64(31):6061-6070.
[10] Lehoty SJ, Mary ON, Jose T, et al. Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate[J]. J AO AC Int, 2007, 90(2):485-520.
[11] European Standard EN 15662:Foods of plant origin-Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by Dispersive SPEQuEChERS-method[S].
[12]田海英,韦风杰,张东豫,等.RP-HPLC法测定烟草中的质体色素[J].烟草科技,2009,49(7):32-36.Tian HY, Wei FJ, Zhang DY, et al. Determination of plastid pigments in tobacco leaf by reversed-phase high performance liquid chromatography[J]. Tob Sci Technol, 2009, 49(7):32-36.
[13] NY/T 788-2004农药残留试验准则[S].NY/T 788-2004 Guideline on pesticide residue trials[S].
[14] Rutkowska E, Lozowicka B, Kaczynski P. Modification of multiresidue QuEChERS protocol to minimize matrix effect and improve recoveries for determination of pesticide residues in dried herbs followed by GC-MS/MS[J]. Food Anal Methods, 2018, 11(3):709-724.
[15] Kim YA, El-Aty AMA, Rahman MM, et al. Method development, matrix effect, and risk assessment of 49 multiclass pesticides in kiwifruit using liquid chromatography coupled to tandem mass spectrometry[J]. J Chromatogr B, 2018, 1076:130-138.
[16] Pavel S, Daniel S, Katerina P, et al. Development of matrix effect-free MISPE UHPLC-MS/MS method for determination of lovastatin in Pu-erh tea, oyster mushroom, and red yeast rice[J]. J Pharm Biomed Anal, 2017,140:367-376.