Validation of QuEChERS analytical technique for organochlorines and synthetic pyrethroids in fruits and vegetables using GC-ECD
In the present day scenario of increasing awareness and concern about the pesticides, it is very important to ensure the quality of data being generated in pesticide residue analysis. To impart confidence in the products, terms like quality assurance and quality control are used as an integral part of quality management. In order to ensure better quality of results in pesticide residue analysis, validation of analytical methods to be used is extremely important. Keeping in view the importance of validation of method, the validation of QuEChERS (quick, easy, cheap, effective, rugged, and safe) a multiresidue method for extraction of 13 organochlorines and seven synthetic pyrethroids in fruits and vegetables followed by GC ECD for quantification was done so as to use this method for analysis of samples received in the laboratory. The method has been validated as per the Guidelines issued by SANCO (French words Sante for Health and Consommateurs for Consumers) in accordance with their document SANCO/XXXX/2013. Various parameters analyzed, viz., linearity, specificity, repeatability, reproducibility, and ruggedness were found to have acceptable values with a per cent RSD of less than 10%. Limit of quantification (LOQ) for the organochlorines was established to be 0.01 and 0.05 mg kg−1 for the synthetic pyrethroids. The uncertainty of the measurement (MU) for all these compounds ranged between 1 and 10%. The matrix-match calibration was used to compensate the matrix effect on the quantification of the compounds. The overall recovery of the method ranged between 80 and 120%. These results demonstrate the applicability and acceptability of this method in routine estimation of pesticide residues of these 20 pesticides in the fruits and vegetables by the laboratory.
KeywordsOrganochlorines Synthetic pyrethroids QuEChERS GC-ECD Fruits Vegetables
- Anastassiades, M., Lehotay, S. J., & Stajnbaher, F. J. (2003). Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. Journal of AOAC International, 86(2), 412–443.Google Scholar
- EURACHEM. (2000). Quantifying uncertainty in analytical measurement (2nd ed.).Google Scholar
- EURACHEM GUIDE. (1998). The fitness for purpose of analytical methods. A laboratory guide to method validation and related topics. Available athttps://www.eurachem.org/images/stories/Guides/pdf/MV_guide_1998_ EN.Pdf. Accessed June 2016).
- Lehotay, S. J. (2007). Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: Collaborative study. Journal of AOAC International, 90(2), 485–520.Google Scholar
- Lehotay, S. J., Kok, A. D., Hiemstra, M., & Bodegraven, P. V. (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. Journal of AOAC International, 88(2), 595–614.Google Scholar
- Lehotay, S. J., Mastovská, K., & Lightfield, A. R. (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. Journal of AOAC International, 88(2), 615–629.Google Scholar
- 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 multiresiduemethod in combination with gas and liquid chromatography and tandem mass spectrometric detection. Analytical and Bioanalytical Chemistry, 389, 1697–1714.CrossRefGoogle Scholar
- SANCO. (2014). Guidance Document on Analytical Quality Control and Validation Procedures for Pesticide Residues Analysis in Food and Feed. Document No. SANCO/XXXX/2013, EC, Health & Consumer Protection Directorate-General, Almeria Spain, 1–42.Thompson, M., Wood, R.(1995) Harmonized guidelines for international quality control in analytical chemistry laboratories. Pure and Applied Chemistry, 67(4), 649–666.Google Scholar
- United States Pharmacopeia, (2007)Validation of compendial methods, 30, National Formulary 25, Rockville, Md., USA, The United States Pharmacopeial Convention, Inc., General Chapter 1225, 729.Google Scholar