Development of a gas chromatographic method for the determination of Chlorpyrifos and its metabolite Chlorpyrifos-oxon in wine matrix

A reliable method has been developed for the determination of Chlorpyrifos (CP) and its metabolite Chlorpyrifos-oxon (CPO) in wine sample using pulsed splitless technique coupled with gas chromatography by using electron capture detector. In this study, a quick, easy and cheap sample preparation method (QuEChERS) based on liquid extraction with acetonitrile, followed by dispersive solid phase extraction using primary secondary amine was tested for the separation and quantification of CP and CPO in wine samples. The accuracy of the developed method was tested upon recovery studies and it was calculated as (92.3 ± 18.2)% for CP and (96.6 ± 16.1)% for CPO. LOD and LOQ values of CP were found as 0.04 and 0.15 ng/mL and 0.49 and 1.62 ng/mL for CPO respectively. By using the pulsed splitless injection mode, the sensitivity of the determination of CP and its metabolite CPO in wine samples was improved compared to splitless technique. CP content of analyzed wine sample was found as 2.05 ± 0.15 ng/mL with a RSD of 7.6% and CPO content was found as 4.99 ± 0.15 ng/mL with a RSD of 3.0% (n = 3). The expanded measurement uncertainties were calculated as 17% and 6% for CP and CPO, respectively.

► Monitoring of pesticides with their metabolites is essential in food quality.
► This method is the first validated method to quantify CP and CPO in wine sample.
► The signal of CP and CPO was improved by pulsed splitless technique.
► Low detection limit for CPO compared to the literature.
► QuEChERS method was tested for the separation of CP and CPO.