In Korea, Eighty three maximum residue levels (MRL) are established for livestock. The aim of this study was the development of rapid, effective multi-residues analytical method for those pesticides in egg and milk using gas chromatography-ECD/NPD for routine analysis. Eighty three compounds were screened with Agilent 7890B Gas Chromatograph to find suitable detectors, resulting that 65 compounds were found to be GC amenable (two groups of NPD compounds and two groups of ECD compounds). Through various optimization procedures for clean-up, partitioning, extraction, final sample treatment method was established. The target analytes were extracted with acidified acetonitrile and partitioned with aid of magnesium sulfate and sodium chloride. Florisil SPE cartridge was used for clean-up of extracts before the analysis of GC-ECD/NPD. Quantification of each analytes was performed by plotting standard calibration curves of 65 compounds at concentration ranging from 0.005 to 1.0 mg/kg. Correlation coefficients (R<sup>2</sup>) of calibration curves were &gt;0.99 for all of target compounds. Limit of detection and limit of quantitation were determined by signal to noise ratio of 3 and 10, respectively. Method limit of quantitation was 0.005 mg/kg, considering 10 times concentration. To evaluate validity of the method developed in this study, recovery tests were carried out with untreated organic samples at spiking levels of 0.005 and 0.05 mg/kg (n=3). Most of the compounds satisfied the recovery criteria of 70-120% (RSD ≤20%). As a result, the optimized method in this study was proved to be efficient and suitable for analyzing GC amendable pesticide multi-residues in egg and milk.

Development of analytical method for pesticide multi-residues in egg and milk using GC-ECD/NPD

253rd National Meeting (2017)

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