Food and Fermentation Industries >

2022 , Vol. 48 >Issue 17: 282 - 290

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.029524

Determination of 50 pesticide residues in fruits and vegetables by QuEChERS extraction with multi-walled carbon nanotubes (MWCNTs) coupled to UPLC-MS/MS

  • HUANG Hua ,
  • XIE Wendong ,
  • GU Yu ,
  • MENG Zhaoqi ,
  • SUN Yuanjie ,
  • DU Hongmiao ,
  • SUN Yana ,
  • KANG Shuai ,
  • LI Mengyun
Expand
  • (Beijing Products Quality Supervision and Inspection Institute, Beijing 101300, China)

Received date: 2021-09-27

  Revised date: 2021-11-16

  Online published: 2022-10-01

Fold

Abstract

This study intended to develop a method for the determination of 50 pesticide residues in fruits and vegetables by sample purification with QuEChERS of combing multi-walled carbon nanotube and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Because of its unique hollow structure and large specific surface area, multi-walled carbon nanotube has excellent adsorption properties, which make it shows superior purification efficiency in the sample pre-treatment process of pesticide residue analysis of fruits and vegetables. This paper selected and determined the type and usage of multi-walled carbon nanotubes through optimization experiments. Based on the QuEChERS method, this paper improved the sample purification effect. This paper extracted fruit and vegetable samples with 0.1% formic acid acetonitrile solution. Meanwhile, this paper detected 50 pesticide residues in fruits and vegetables through ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The results demonstrated that they were 0.002-0.010mg/kg for the limits of quantification (LOQs) for 50 compounds, 71%-105% recoveries of low, medium and high supplemental levels within the linear range and 3.1%-11.2% relative standard deviation (RSD). Good linearity of the Matrix matching standard curve was observed for all calibration curves with correlation coefficients (r) > 0.99. This method was rapid, high sensitivity and accuracy. It is suitable for rapid detection and analysis of pesticide residues in fruit and vegetable samples.

Key words： multi-walled carbon nanotube (MWCNTs); ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS); fruits and vegetables; pesticides

Cite this article

HUANG Hua , XIE Wendong , GU Yu , MENG Zhaoqi , SUN Yuanjie , DU Hongmiao , SUN Yana , KANG Shuai , LI Mengyun . Determination of 50 pesticide residues in fruits and vegetables by QuEChERS extraction with multi-walled carbon nanotubes (MWCNTs) coupled to UPLC-MS/MS[J]. Food and Fermentation Industries, 2022 , 48(17) : 282 -290 . DOI: 10.13995/j.cnki.11-1802/ts.029524

References

[1] 王慧君, 薛亚薇, 康健, 等.SPE和QuEChERS前处理方法结合LC-Q-TOF/MS检测苹果和番茄中282种农药残留对比研究[J].分析试验室, 2015, 34(4):383-387.
WANG H J, XUE Y W, KANG J, et al.Comparison of SPE and QuEChERS combined with LC-Q-TOF/MS for determination of 282 pesticide residues in apple and tomato[J].Chinese Journal of Analysis Laboratory, 2015, 34(4):383-387.
[2] 李凌云, 许晓敏, 林桓, 等.超高效液相色谱-串联质谱法快速检测蔬菜中248种农药残留[J].色谱, 2016, 34(9):835-849.
LI L Y, XU X M, LIN H, et al.Rapid detection of 248 pesticide residues in vegetables by ultra high performance liquid chromatographytandem mass spectrometry[J].Chinese Journal of Chromatography, 2016, 34(9):835-849.
[3] 曹静, 庞国芳, 王明林, 等.液相色谱-电喷雾串联质谱法测定生姜中的215种农药残留[J].色谱, 2010, 28(6):579-589.
CAO J, PANG G F, WANG M L, et al.Determination of 215 pesticide residues in ginger using liquid chromatography coupled with electrospray ionization tandem mass spectrometry[J].Chinese Journal of Chromatography, 2010, 28(6):579-589.
[4] 李岩, 郑锋, 王明林, 等.液相色谱-串联质谱法快速筛查测定浓缩果蔬汁中的156种农药残留[J].色谱, 2009, 27(2):127-137.
LI Y, ZHENG F, WANG M L, et al.Rapid screening and confirmation of 156 pesticide residues in concentrated fruit and vegetable juices using liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography, 2009, 27(2):127-137.
[5] 徐娟, 陈捷, 王岚, 等.QuEChERS提取与超高效液相色谱-电喷雾电离串联质谱联用法检测果蔬中的230种农药残留[J].分析测试学报, 2013, 32(3):293-301.
XU J, CHEN J, WANG L, et al.Large-scale analysis of pesticides in fruits and vegetables by liquid chromatography-electrospray tandem mass spectrometry with QuEChERS as cleanup step[J].Journal of Instrumental Analysis, 2013, 32(3):293-301.
[6] 刘宝峰, 刘罡一, 马又娥, 等.高效液相色谱-串联质谱法检测蔬菜水果中65种农药残留方法研究[J].科技通报, 2010, 26(1):93-99.
LIU B F, LIU G Y, MA Y E, et al.Study on determination of multi-residues for 65 pesticides in vegetables and fruits using liquid chromatography coupled with mass spectrometry[J].Bulletin of Science and Technology, 2010, 26(1):93-99.
[7] 闫震, 聂继云, 徐国锋, 等.超高效液相色谱-串联质谱法对比4种净化方式对不同色素含量基质中19种农药残留检测的影响[J].分析测试学报, 2014, 33(9):1 000-1 009.
YAN Z, NIE J Y, XU G F, et al.Effects of four kinds of purification methods for determination of 19 pesticide residues in substrates of different pigments analyzed by ultra performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis, 2014, 33(9):1 000-1 009.
[8] 曹慧, 朱岩, 李祖光, 等.磁性多壁碳纳米管净化技术快速测定甘蓝中10种农药残留[J].分析试验室, 2015, 34(12):1 480-1 484.
CAO H, ZHU Y, LI Z G, et al.Simultaneous determination of ten pesticide residues in ball cabbage by ultra performance liquid chromatography-tandem mass spectrometry and magnetic multiwalled carbon nanotubes cleaning[J].Chinese Journal of Analysis Laboratory, 2015, 34(12):1 480-1 484.
[9] 帖金鑫, 余斐, 廖付, 等.多壁碳纳米管在农药残留检测中的应用进展[J].农产品加工, 2017(8):61-65.
TIE J X, YU F, LIAO F, et al.Progress in applications of multi-walled carbon nanotubes in pesticide residue detection[J].Farm Products Processing, 2017(8):61-65.
[10] 张爱芝, 王全林, 曹丽丽, 等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留[J].色谱, 2016, 34(2):158-164.
ZHANG A Z, WANG Q L, CAO L L, et al.Determination of 250 pesticide residues in vegetables using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography, 2016, 34(2):158-164.
[11] 刘炎, 欧阳迪庆, 叶玉凤, 等.QuEChERS结合超高效液相色谱-串联质谱法同时测定番茄中噻虫嗪、噻虫胺、螺虫乙酯及其代谢物残留[J].分析测试学报, 2017, 36(12):1 431-1 438.
LIU Y, OUYANG D Q, YE Y F, et al.Analysis of thiamethoxam, clothianidin and spirotetramat and their metabolites residues in tomato using QuEChERS method with ultra performance liquid chromatography-mass spectrometry[J].Journal of Instrumental Analysis, 2017, 36(12):1 431-1 438.
[12] 董亚蕾, 刘文婧, 曹进, 等.QuEChERS-超高效液相色谱-串联质谱法测定坚果中38种农药残留[J].分析化学, 2017, 45(9):1 397-1 404.
DONG Y L, LIU W J, CAO J, et al.Determination of 38 kinds of pesticide residues in nuts by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry, 2017, 45(9):1 397-1 404.
[13] 陈跃, 王金花, 卢晓宇, 等.超高效液相色谱-串联质谱法快速测定农产品中残留的种衣剂农药[J].色谱, 2008, 26(6):720-725.
CHEN Y, WANG J H, LU X Y, et al.Determination of pesticide residues from seed coating reagent in agricultural products using ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography, 2008, 26(6):720-725.
[14] 苏明伟, 郑言波, 杨海, 等.果蔬农药残留检测的预处理和检测条件优化研究[J].食品科学, 2006, 27(5):199-201.
SU M W, ZHENG Y B, YANG H, et al.Study on opitimization of sample preparation and determination for pesticide residues in fruits and vegetables[J].Food Science, 2006, 27(5):199-201.
[15] 朱俊杰, 陆利霞, 熊晓辉.食品中农残检测及预处理新技术进展[J].食品研究与开发, 2008, 29(2):129-132.
ZHU J J, LU L X, XIONG X H.New technologies of pre-disposal treatment and detection of pesticide residues in food[J].Food Research and Development, 2008, 29(2):129-132.
[16] 彭晓俊, 温绮靖, 庞晋山, 等.改性多壁碳纳米管固相萃取测定农产品中苯氧羧酸类除草剂残留[J].分析测试学报, 2012, 31(11):1 373-1 378.
PENG X J, WEN Q J, PANG J S, et al.Determination of phenoxyacid herbicides in agricultural products by solid phase extraction using modified multi-walled carbon nanotubes as adsorbent[J].Journal of Instrumental Analysis, 2012, 31(11):1 373-1 378.
Options
Outlines

/

〈 〉

Powered by Beijing Magtech Co. Ltd,.