Skip to main content
SpringerLink
Log in

Validation of Analytical Methods Used for Pesticide Residue Detection in Fruits and Vegetables

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

Injudicious and ever-increasing use of pesticides has made consumers more aware and critical about quality control and quality assurance in fruits and vegetables. Presence of pesticide residues in food commodities is one of the most indispensable parameters in quality control and quality assurance. To meet out the demand of acceptable or no residues in crops, different agencies viz. Codex Alimentarius Commission, European Union, FSSAI etc. have assigned maximum residue limits for different pesticides on different crops. As these residues are present in very small quantities, their extraction and quantification involve the use of very effective and sensitive analytical methods and instruments. Different accreditation bodies have fixed analytical parameters to be met out by the pesticide residue laboratories so as to detect the pesticide residues with high precision and accuracy. Some of these parameters are linearity, accuracy, precision, limit of detection, limit of quantitation, and specificity etc. Validation of analytical methods is one such essential parameter in establishing the analytical quality control for detection of pesticide residues and also an essential component to meet out the requirements of different accreditation bodies. In the present paper, an attempt has been made to make an overview of the validation of analytical methods employed in pesticide residue analysis globally. The present review focuses on methods validated by different workers for residue detection along with each analytical parameter covered for validating the analytical methods. This compilation will be a useful tool to the analysts working on pesticide residue analysis in fruits and vegetables.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

Data Availability

As it is a review paper, hence, the data and material were not a part of paper. The literature used in the paper is collected from sources like Cera and e-journals in the University Library.

References

  • Anastassiades M, Lehotay SJ, Stajbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid phase extraction of the determination of pesticide residues in produce. J AOAC Int 86:412–431

    Article  CAS  Google Scholar 

  • AOAC Peer verified methods program (1993) Manual on policies and procedures, Arlington, V.A.

  • Bhagyasree T, Injeti N, Azhakesan A, Rao UMV (2014) A review on analytical method development and validation. Int J Pharm Res & Analysis 4:444–448

    Google Scholar 

  • Chai LK, Zaidel ND, Hans CBH (2012) A rapid multi residue method for the determination of pesticide residues in choi sum, yardlong beans and aubergines. Food Chem 131:611–616

    Article  CAS  Google Scholar 

  • Chandran S, Singh RSP (2007) Comparison of various international guidelines for analytical method validation. Pharmazie 62:4–14

    CAS  PubMed  Google Scholar 

  • Chowdhury MAZ, Fakhruddin ANM, Islam MN, Moniruzzaman M, Gan SH, Alam MK (2013) Detection of the residues of nineteen pesticides in fresh vegetable samples using gas chromatography mass spectrometry. Food Control 34:457–465

    Article  Google Scholar 

  • Commission Regulation (EC) (2005) 396/2005 on maximum residue levels of pesticides in or on foods and feed of plant and animal origin. J Eur Union L70/1

  • CXG-90 (2017) Guidelines on performance criteria for methods of analysis for the determination of pesticide residues in food and feed. http://www.fao.org/fao-who-codexalimentarius/sh-proxy/en/?lnk=1&url=https%253A%252F%252Fworkspace.fao.org%252Fsites%252Fcodex%252FStandards%252FCXG%2B90-2017%252FCXG_090e.pdf.

  • Drouillet-Pinard P, Boisset M, Periquet A, Lecerf JM, Casse F, Catteau M (2010) Realistic approach of pesticide residues and French consumer exposure within fruit and vegetable intake. J Environ Sci Health B 46:84–91

    Article  Google Scholar 

  • Dubey JK, Patyal SK, Sharma A (2018) Validation of QuEChERS analytical technique for organochlorines and synthetic pyrethroids in fruits and vegetables using GC-ECD. Environ Monit Assess 190:231

    Article  CAS  Google Scholar 

  • Fenik J, Tankiewicz M, Biziuk M (2011) Properties and determination of pesticides in fruits and vegetables. Trends Anal Chem 30:814–826

    Article  CAS  Google Scholar 

  • Green JM (1996) A practical guide to analytical method validation. Anal Chem 68:305A–309A

    Article  CAS  Google Scholar 

  • Grimalt S, Dehouck P (2016) Review of analytical methods for the determination of pesticide residues in grapes. J Chromatogr A 1433:1–23

    Article  CAS  Google Scholar 

  • Guedes JAC, Silva RO, Lima CG, MAL M, Nascimento RF (2016) Matrix effect in guava multiresidue analysis by QuEChERS method and gas chromatography coupled to quadropole mass spectrometry. Food Chem 199:280–286

    Article  Google Scholar 

  • Hill ARC, Reynolds SL (1999) Guidelines for in-house validation of analytical methods for pesticide residues in food and animal feed. Analyst 124:953–995

    Article  CAS  Google Scholar 

  • Hubner L (1998) Validation and qualification in analytical laboratories. Taylor and Francis. 336p

  • IUPAC (2006) Compandeium of chemical terminology 2nd ed. (the “Gold Book”) compiled by A.D Mc Naught and A. Wilkinson Blackwell. Scientific publications oxford. XML. Online corrected verison: http://goldbook.iupac.org

  • Kruve A, Rebane R, Kipper K, Oldekop ML, Evard H, Herodes K, Ravio P, Leito I (2015) Tutorial review on validation of liquid chromatography-mass spectrometry methods: part II. Anal Chim Acta 870:8–28

    Article  CAS  Google Scholar 

  • Kumar V, Bhardwaj R, Kumar GGS (2015) An overview on HPLC method development, optimization and validation process for drug analysis. Pharm Chem J 2:30–40

    CAS  Google Scholar 

  • Lawal A, Wond RCS, Tan GH, Abdrula’uf LB, Alsharif AMA (2018) Recent modifications and validation of QuEChERS-dSPE coupled to LCMS and GCMS instruments and determination of pesticides/agrochemical residues in fruits and vegetables: review. J Chromatogr Sci 56:656–669

    Article  CAS  Google Scholar 

  • Lawal A, Wong RCS, Tan GH, Abdulra’uf LB (2019) Determination of pesticide residues in fruit and vegetables by high performance liquid chromatography-tandem mass spectrometry with multivariate response surface methodology. Anal Lett 52:231–248

    Article  CAS  Google Scholar 

  • Lehotay SJ (2007) Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: Collaborative study. J AOAC Int 90:485–520

    Article  CAS  Google Scholar 

  • Lehotay SJ, Kok AD, Himestra M, Bodegraven PV (2005a) 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 88:595–614

    Article  CAS  Google Scholar 

  • Lehotay SJ, Mastovska K, Lightfield AR (2005b) Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables. J AOAC Int 88:615–629

    Article  CAS  Google Scholar 

  • Leito I, Kruve A, Rebane R, Oldekopp ML, Evard H, Herodes K, Kipper K, Helm I (2016) Validation of liquid chromatography mass spectrometry (LC-MS) methods (analytical chemistry) course. http://www.utv.ee/naita?id=23245

  • Lopes RP, Freitas EE, Filho JFA, Vargas EA, Augusti DV, Augusti R (2012) Development and validation of a method for determination of sulfomide in animal feed by modified QuEChERS and LCeMS/MS analysis. Food Control 28:192–198

    Article  CAS  Google Scholar 

  • Magnusson B,(2014) Ornemark (eds) Eurachem Guide The fitness of purpose of analytical methods. A laboratory guide to method validation and related topics. 2nd edition

  • Mishra S, Saini MK, Alam S, Thakur LK, Raza SK (2015) Method validation and uncertainty measurement for determination of 25 pesticides by GC-ECD and MSD in banana using modified QuEChERS. Int Res J Environ Sci 4:21–27

    CAS  Google Scholar 

  • Nash RA, Wachter AH (1993) In Pharmaceutical process validation. Third edition; revised and expanded, Marcel Dekker Inc., New York.

  • Pay P, Anastassiades M, Mack D, Sigalova I, Tasdelen B, Oliva J, Barba A (2007) Analysis of pesticide residues using the quick easy cheap effective rugged and safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Anal Bioanal Chem 389:1697–1714

    Article  Google Scholar 

  • Raju MB, Rao CN, Kumar RGV, Rao BT, Krishna PM, Sreenivasulu V, Prasad K, Venkateswarlu P (2012) Method for determination of organophosphorus pesticides in okra (Ablemoschus esculentus) by liquid chromatography tandem mass spectrometry. J Liq Chromatogr Relat Technol 35:375–384

    Article  CAS  Google Scholar 

  • Ramadan G, Al Jabir M, Alabdulmalik M, Mohammed A (2016) Validation of method for determination of120 pesticide residues in apples and cucumbers by LC-MS/MS. Drug Test Anal 8:498–510

    Article  CAS  Google Scholar 

  • Raphaella PC, Fabiano AS, Fernando DM, Gilsara S, Wesley R, Renata PL (2013) Development and method validation for determination of 128 pesticides in bananas by modified QuEChERS and UHPLCeMS/MS analysis. Food Control 33:413–423

    Article  Google Scholar 

  • Ravichandran V, Shalini S, Sundaram KM, Rajak H (2010) Validation of analytical methods- strategies and importance. Int J Pharm Pharm Sci 2:18–22

    Google Scholar 

  • Rizzeti TM, Kemmerich M, Martins ML, Prestes OD, Adaime MB, Zanella R (2016) Optimization of QuEChERS based method by means of central composite design for pesticide multiresidue determination in orange juice by UHPLC-MSMS. Food Chem 196:25–33

    Article  Google Scholar 

  • Sahoo CK, Sudhakar M, Ramana DV, Satyanarayana K, Panda KC (2018) Validation of analytical procedure- a review. Asian J Pharm Ana 8:109–116

    Article  Google Scholar 

  • SANCO (2019) Analytical quality control and validation procedures for pesticide residue analysis in food and feed. Document No SANTE/12682/2019

  • Shrivastava A, Gupta VB (2012) Isocratic or gradient elution and assessment linearity in analytical methods. J Advan Sci Res 3:12–20

    CAS  Google Scholar 

  • Szepesi MG, Mihalyfi K (1989) Selection of HPLC methods in pharmaceutical analysis-III method validation. J Chromatogr 46:265–278

    Google Scholar 

  • Thompson M, Ellison SLR, Wood R (2002) Harmonize guidelines for single-laboratory method for analyses (IUPAC Technical Report). Pure Appl Chem 74:835–855

    Article  CAS  Google Scholar 

  • Tiryaki O (2016) Validation of QuEChERS method for determination of some pesticide residues in two apple varieties. J Environ Sci Health B 51:722–729

    Article  CAS  Google Scholar 

  • Tiwari G, Tiwari R (2010) Bioanalytical method validation: an updated review. Pharm methods 1:25–38

    Article  Google Scholar 

  • UNODC (2009) Guidance for the validation of analytical methodology and calibration of equipment used for testing of illicit drugs in seized materials and biological specimens. United Nations Publication. https://www.unodc.org/documents/scientific/validation_E.pdf

  • US FDA Guidance of industry- bioanalytical method validation (2001), # 5600, Fishers Lane, Rockville, MD 20857

Download references

Acknowledgements

The authors are thankful to Indian Council of Agricultural Research (ICAR), New Delhi, India, for providing necessary facilities to the authors in preparing the manuscript.

Code Availability

Not applicable

Author information

Authors and Affiliations

  1. Pesticide Residue Laboratory, Department of Entomology, Dr Y S Parmar University of Horticulture and Forestry, Nauni, Solan, HP, 173230, India

    Ajay Sharma, Jatiender Kumar Dubey, Sapna Katna, Deepika Shandil, Gaganpreet Singh Brar & Shubhra Singh

Authors
  1. Ajay Sharma
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Jatiender Kumar Dubey
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Sapna Katna
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Deepika Shandil
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Gaganpreet Singh Brar
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Shubhra Singh
    View author publications

    You can also search for this author in PubMed Google Scholar

Contributions

All the authors have contributed towards the preparation of this manuscript. Dr Ajay Sharma and Dr Sapna Katna were instrumental in writing the manuscript, compiling the literature, and preparing the original draft. Dr Gagandeep and Ms Shubhra Singh helped by collecting the required papers and downloading literature from different sources. Dr Deepika Shandil recompiled the matter in the format of your esteemed journal and typed the references as per the format. Dr JK Dubey reviewed and checked the paper for its language, matter, technical appropriateness, and finalized the manuscript.

Corresponding author

Correspondence to Jatiender Kumar Dubey.

Ethics declarations

Ethical Approval

Not applicable

Informed Consent

Informed consent not applicable

Conflict of Interest

Ajay Sharma declares that he has no conflict of interest. Jatiender Kumar Dubey declares that he has no conflict of interest. Sapna Katna declares that she has no conflict of interest. Deepika Shandil declares that she has no conflict of interest. Gaganpreet Singh Brar declares that he has no conflict of interest. Shubhra Singh declares that she has no conflict of interest.

Additional information

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Sharma, A., Dubey, J.K., Katna, S. et al. Validation of Analytical Methods Used for Pesticide Residue Detection in Fruits and Vegetables. Food Anal. Methods 14, 1919–1926 (2021). https://doi.org/10.1007/s12161-021-02027-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-021-02027-y

Keywords

Search

Navigation