Development of automated online gel permeation chromatography–gas chromatograph mass spectrometry for measuring multiresidual pesticides in agricultural products

An automated online gel permeation chromatography–gas chromatograph mass spectrometer (GPC–GC/MS) was developed for the rapid determination of residual pesticides in agricultural products. Pesticides were extracted from homogenized food samples with acetonitrile and decontaminated via the matrix solid-phase dispersion (MSPD) technique, using a primary secondary amine as sorbent prior to GPC–GC/MS analysis. A slightly modified preparation method and automated GPC step proved useful in minimizing matrix interference. To evaluate the performance of the system, 97 target pesticides were spiked at a concentration of 0.1 mg/kg into a range of food types, including potato, cabbage, carrot, apple, orange, cucumber, and rice. A low flow rate of 0.1 mL/min in GPC resulted in a 40-fold reduction in solvent consumption compared with conventional GPC column applications. The combination of MSPD technique and GPC–GC/MS for the analysis of the 97 pesticides can be accomplished within 90 min. Most pesticides were recovered in the range of 70–120%, with relative standard deviation generally less than 10%. The results demonstrate that the method can be successfully applied with acceptable recoveries to a broad range of target pesticides within a diverse range of food types.