Akademik Veri Yönetim Sistemi
7th International Conference on Engineering and Natural Sciences (ICENS 2021) , Sarajevo, Bosna-Hersek, Sarajevo, Bosna-Hersek, 23 - 27 Haziran 2021, cilt.2021, ss.211-217
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
conditions.