Positive List System (PLS) which has been used for safety management of imported agricultural products is a negative regulation, allowing below 0.01 mg/kg for unregistered pesticides residues. For establishing the PLS into Korea, it is required to develop rapid and sensitive methods that can simultaneously analyze unregistered pesticides in imported agricultural products using LC-MS/MS. In this study, Korean Pesticide Residue Analysis (KOPRA) method was developed to analyze 121 unregistered pesticides for three agricultural products, such as brown rice, orange, and green pepper chosen as representatives of fatty, non-fatty, and high chlorophyll-containing samples, respectively. Acetonitrile was used for the extraction of pesticide residues in samples, and the dispersive solid phase extraction using primary secondary amine and anhydrous magnesium sulfate was employed for a clean-up. Concentrations of pesticide standards prepared for the matrix-matched calibration ranged from 0.002 to 0.5 mg/kg, and limits of quantification (LOQ) were below 0.01 mg/kg for all tested pesticides. Correlation coefficients of matrix-matched calibration curves were more than 0.9921. Recoveries of pesticides in fortification ranges of 0.05-0.5 mg/kg using the KOPRA method were between 70 and 130%, and relative standard deviations were below 30%. The number of pesticides amenable to the KOPRA method was more than 97. Therefore, these results show that the KOPRA method developed in this study could be used as a rapid and high-sensitive analysis method of pesticide residues for agricultural products with meeting the LOQ of below 0.01 mg/kg for the PLS in Korea.

Simultaneous determination of unregistered pesticides in Korea for agricultural products using LC-MS/MS

252nd National Meeting (2016)

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