Nektarin ve Şeftali Örneklerinde Bazı Pestisit Kalıntılarının Belirlenmesi İçin Etkin Bir Yöntemin Doğrulanması

Abstract

Method verification is an internal quality control procedure verifying the suitability of the method for specific purposes. All methods should be verified prior to analyses of real samples. LOQ, range of linearity, precision, accuracy and recovery criteria have to be taken into consideration while performing the method verification. This study was conducted to verify QuEChERS procedure for the analysis of boscalid, chlorpyrifos and tebuconazole in nectarine and peach. Samples spiked at 3 levels of 3 different pesticides. LC-MS/MS was used for chromatographic separation. Matrix calibration (MC) was used to compensate the matrix effect. QuEChERS method revealed that all pesticide LOQs were less than MRL. Recovered boscalid, chlorpyrifos and tebuconazole from matrices were recorded as 123.73% (RSD= 8.89%; n=52), 108.37% (RSD= 14.95%; n=52) and 110.34% (RSD= 15.22%; n=52), respectively. Overall recovery of the QuEChERS-AOAC 2007.01 method was 113.96 %, with RSD value of 14.52 % (n=156; SD=16.55). All recovery ranges were noted as 66.42-139.68%. These values were fit the SANTE recovery ranges (60–140%). MC curves 3 pesticides were linear (R2 ≤0.999). Some other verification criteria, such as accuracy, linearity, precision and recovery were within the specified limits. According to the results of this study, the QuEChERS method is suitable for the analyses of chlorpyrifos, tebuconazole and boscalid in case of nectarine and peachs.