Validation of QuEChERS Method for the Analyses of Chlorpyrifos-methyl, Lambda-cyhalothrin, Tebuconazole Residues in Grapes

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Duman A., Tiryaki O.

7th International Conference on Engineering and Natural Sciences (ICENS 2021) , Sarajevo, Bosna-Hersek, Sarajevo, Bosnia And Herzegovina, 23 - 27 June 2021, vol.2021, pp.211-217

  • Publication Type: Conference Paper / Full Text
  • Volume: 2021
  • City: Sarajevo
  • Country: Bosnia And Herzegovina
  • Page Numbers: pp.211-217
  • Çanakkale Onsekiz Mart University Affiliated: Yes


Method validation (MV) is an important quality parameter in pesticide residue analyse and has a direct

impact on the quality of data. MV is the process of verifying that a method is fit for purpose All

methods used in pesticide residue analysis must be validated prior to original laboratory samples.

Working with validated methods is also a basic requirement in ISO 17025 and OECD - GLP quality

systems. This study was carried out to validate QuEChERS Official Method 2007.01 method using

grapes spiked at 0.1 x maximum residue limit (MRL) 0.1 x MRL and 10 x MRL levels of the three

(,chlorpyrifos-methyl, lambda-cyhalohtrin and tebuconazole) pesticides. For the extraction and

cleanup, QuEChERS 2007.1 version was followed, then the samples were subjected to LC-MS/MS for

chromatography. For the quantification represenative (apple) matrix-matched calibration (MC) was

used to compansate matrix effect. Detection limit of three pesticides blow the EU-MRLs. The recovery

ranges were 91.3%-131.4% (mean 114.80%), 85.8%-133.2% (mean 108.05%), 90.3%-111.6% (mean

102.96) for chlorpyrifos-methyl, lambda-cyhalohtrin and tebuconazole, respectively. The overall

recovery of the QuEChERS method was 108.6% with a relative standard deviation (RSD) of 11.8% (n=

108). These figures are within the recovery limits (60-140%) and the values specified for the

Precision, accuracy and linearity were also within the required limits. All the required method

validation criteria were met in this study. QuEChERS method was found suitable for the analyses of

chlorpyrifos-methyl, lambda-cyhalohtrin and tebuconazole residues in grape under our laboratory