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Interaction of Pesticides with Clean-up Agents during QuEChERS Dispersive-SPE Clean-up


Affiliations
1 ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
 

A method was developed using liquid chromatography tandem mass spectroscopy for the identification and quantification of multi residues of pesticides. The present study is first of this kind, destined purely to understand the interaction between the clean-up agents with 103 pesticides. The QuEChERS clean-up, employing most commonly used clean-up agents like anhyd.MgSO4, PSA, C-18 and GCB in twelve combinations, was performed to assess their adsorption behavior with the pesticides. Recovery studies at 1μg∙mL−1 showed that anhyd.MgSO4 gave acceptable recovery for 100 pesticides (97.08%) in treatment T1. The PSA adsorbed some polar and acidic pesticides onto it and gave acceptable recovery for < 90% pesticides in T2 to T5 and C-18 with anhyd.MgSO4 & varying amount of PSA (T6, T7) gave a lower, but acceptable recovery of 83.49% pesticides. GCB with anhyd.MgSO4 & varying amount of PSA (T8, T9), adsorbed some planar pesticides like carbendazim, tricyclazole and gave a lower, but acceptable recovery for 74.75 – 77.66% pesticides. In T10 to T12, when all the adsorbents were used, adsorption of polar, acidic and planar pesticides (25.24%) was observed while rest of the pesticides (74.75%) gave acceptable recovery. The method also satisfied the single laboratory validation criteria for linearity, specificity, accuracy and precision.

Keywords

Anhydrous MgSO4, C-18, GCB, Pesticides, PSA
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  • Wilkowska A & Biziuk M, Determination of pesticide residues in food matrices using the QuEChERS methodology, Food Chem, 125(3) (2011) 803–812, https://doi.org/10.1016/j. foodchem.2010.09.094.

  • Souza-Silva E A, Jiang R, Rodríguez-Lafuente A, Gionfriddo E & Pawliszyn J, A critical review of the state of the art of solidphase microextraction of complex matrices I. environmental analysis, Trends Analyt Chem, 71 (2015) 224–235, https://doi.org/10.1016/j.trac.2015.04.016.

  • Akiyama Y, Yoshioka N, Mitsuhashi T, Takeda N & Tsuji M, Multi-pesticide screening method for agricultural products with an automated sample preparation instrument, J Food Hyg Saf, 38(5) (1997) 363–371, https://doi.org/10.3358/shokueishi. 38.5_363.

  • Lehotay S J & Eller K I, Development of a method of analysis for 46 pesticides in fruits and vegetables by supercritical fluid extraction and gas chromatography/ion TVap mass spectrometry, J AOAC Int, 78(3) (1995) 821–830, https://doi. org/10.1093/jaoac/78.3.821.

  • Anastassiades M, Lehotay S J, Štajnbaher D & Schenck F J, Fast and easy multi residue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce, J AOAC Int, 86(2) (2003) 412–431, https://doi.org/10.1093/jaoac/ 86.2.412.

  • Perestrelo R, Silva P, Porto-Figueira P, Pereira J A, Silva C, Medina S & Câmara J S, QuEChERS-Fundamentals, relevant improvements, applications and future trends, Anal Chim Acta, 1070 (2019) 1–28, https://doi.org/10.1016/j.aca. 2019.02.036.

  • Wang Y, Nie J, Yan Z, Li Z, Cheng Y & Chang W, Occurrence and co-occurrence of mycotoxins in nuts and dried fruits from China, Food Control, 88 (2018) 181–189, https://doi.org/10.1016/j.aca.2019.02.036.

  • Rutkowska E, Łozowicka B & Kaczyński P, Modification of multi residue QuEChERS protocol to minimize matrix effect and improve recoveries for determination of pesticide residues in dried herbs followed by GC-MS/MS, Food Anal Methods, 11(3) (2018) 709–724, https://doi.org/10.1007/s12161-017-1047-3.

  • Sell B, Sniegocki T, Zmudzki J & Posyniak A, Development of an analytical procedure for the determination of multiclass compounds for forensic veterinary toxicology, J Anal Toxicol, 42(3) (2018) 183–191, https://doi.org/10.1093/jat/bkx093.

  • Luke M A, Froberg J E & Masumoto H T, Extraction and cleanup of organochlorine, organophosphate, organonitrogen, and hydrocarbon pesticides in produce for determination by gasliquid chromatography, J AOAC Int, 58(5) (1975) 1020–1026, https://doi.org/10.1093/jaoac/58.5.1020.

  • Cook J, Beckett M P, Reliford B, Hammock W & Engel M, Multi residue analysis of pesticides in fresh fruits and vegetables using procedures developed by the florida department of agriculture and consumer Services, J AOAC Int, 82(6) (1995) 1419–1435, https://doi.org/10.1093/jaoac/82.6.1419.

  • Lehotay S J, Quick, easy, cheap, effective, rugged, and safe approach for determining pesticide residues. in Methods in Biotechnology-Pesticide Protocols, edited by J L M Vidal & A G Frenich (Humana Press, Totowa, New Jersey, USA) 19 (2006) 239–261, https://doi.org/10.1385/1-59259-929-X:239-261.

  • Rejczak T & Tuzimski T, A review of recent developments and trends in the QuEChERS sample preparation approach, Open Chem, 13(1) (2015) 980–1010, dx.doi.org/10.1021/ jf304648h.

  • Lehotay S J, Anastassiades M & Majors R E, The QuEChERS revolution, LcGc Eur, 23(9) (2010) 418–428.

  • Majors R E, Modern techniques for the extraction of solid materials-an update, LC GC North America, 20(2) (2007), 71–81.

  • Zhao L & Stevens J, Optimizing recoveries of planar pesticides in spinach using toluene and the AOAC QuEChERS kits with graphitized carbon, In 123rd AOAC Int Ann Meet, (2008) 141.

  • SANTE guidelines, Analytical quality control and method validation procedures for pesticide residues analysis in food and feed, SANTE 11312/2021 (European Commission) 2021, 155, [https://www.accredia.it/app/uploads/2021/02/ SANTE_11312_2021.pdf, Accessed on 30.08.2023]

  • Damale R D, Dutta A, Shaikh N, Pardeshi A, Shinde R, Babu K D & Banerjee K, Multi residue analysis of pesticides in four different pomegranate cultivars: Investigating matrix effect variability by GC-MS/MS and LC-MS/MS, Food Chem, 407 (2023) 135179, https://doi.org/10.1016/j.foodchem.2022. 135179.

  • Jankar J, Taynath B, Hingmire S, Patil R & Banerjee K, Method development and validation in the curry leaf matrix employing advanced mass spectrometry: Quantitative screening of 490 multiclass pesticides by buffered ethyl acetate technique, J Env Sci Health, Part B, 58(5) (2023) 1–17, https://doi.org/

  • 1080/03601234.2023.2221994. 20 Varela-Martinez D A, Gonzalez-Curbelo M A, Gonzalez- Salamo J & Hernandez-Borges J, Analysis of multiclass pesticides in dried fruits using QuEChERS-gas chromatography tandem mass spectrometry, Food Chem, 297 (2019) 124961, https://doi.org/10.1016/j.foodchem.2019.124961.

  • Lehotay S J, Kok A D, Hiemstra M & Bodegraven P V, Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection, J AOAC Int, 88(2) (2005) 595–614, https://doi.org/10.1093/ jaoac/88.2.595.

  • He Y & Liu Y H, Assessment of primary and secondary amine adsorbents and elution solvents with or without graphitized carbon for the SPE clean-up of food extracts in pesticide residue analysis, Chromatographia, 65 (2007) 581–590, https://doi. org/10.1365/s10337-007-0198-6.

  • Koesukwiwat U, Lehotay S J, Mastovska K, Dorweiler K J & Leepipatpiboon N, Extension of the QuEChERS method for pesticide residues in cereals to flaxseeds, peanuts, and doughs, J Agric Food Chem, 58(10) (2010) 5950–5958, https://doi.org/ 10.1021/jf902988b.

  • Lehotay S J, 2011). QuEChERS Sample Preparation Approach for Mass Spectrometric Analysis of Pesticide Residues in Foods, In Mass Spectrometry in Food Safety-Methods in Molecular Biology edited by J Zweigenbaum (Humana Press) 2011, 747, https://doi.org/10.1007/978-1-61779-136-9_4

  • Mol H G, Rooseboom A, Van D R, Roding M, Arondeus K & Sunarto S, Modification and re-validation of the ethyl acetatebased multi-residue method for pesticides in produce, Anal Bioanal Chem, 389 (2007) 1715–1754, https://doi.org/10.1007/ s00216-007-1357-1.


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  • Interaction of Pesticides with Clean-up Agents during QuEChERS Dispersive-SPE Clean-up

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Authors

Madhu Tippannanavar
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
Tirthankar Banerjee
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
Sumit Shekhar
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
Harshang Talaviya
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
Sudama Sahu
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
Neethu Narayanan
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
Suman Gupta
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India
Anupama Singh
ICAR-Indian Agricultural Research Institute, New Delhi 110 012, India

Abstract


A method was developed using liquid chromatography tandem mass spectroscopy for the identification and quantification of multi residues of pesticides. The present study is first of this kind, destined purely to understand the interaction between the clean-up agents with 103 pesticides. The QuEChERS clean-up, employing most commonly used clean-up agents like anhyd.MgSO4, PSA, C-18 and GCB in twelve combinations, was performed to assess their adsorption behavior with the pesticides. Recovery studies at 1μg∙mL−1 showed that anhyd.MgSO4 gave acceptable recovery for 100 pesticides (97.08%) in treatment T1. The PSA adsorbed some polar and acidic pesticides onto it and gave acceptable recovery for < 90% pesticides in T2 to T5 and C-18 with anhyd.MgSO4 & varying amount of PSA (T6, T7) gave a lower, but acceptable recovery of 83.49% pesticides. GCB with anhyd.MgSO4 & varying amount of PSA (T8, T9), adsorbed some planar pesticides like carbendazim, tricyclazole and gave a lower, but acceptable recovery for 74.75 – 77.66% pesticides. In T10 to T12, when all the adsorbents were used, adsorption of polar, acidic and planar pesticides (25.24%) was observed while rest of the pesticides (74.75%) gave acceptable recovery. The method also satisfied the single laboratory validation criteria for linearity, specificity, accuracy and precision.

Keywords


Anhydrous MgSO4, C-18, GCB, Pesticides, PSA

References