A combined method of multi-plug filtration cleanup (m-PFC) and liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was established to simultaneously detect 14 pesticides in tea. The pesticides in water-soaked tea were extracted with acetonitrile. Cleanup of tea extract was performed using an m-PFC column packed with multiple cleanup materials: multi-walled carbon nano-tubes (MWCNTs), primary secondary amine (PSA) and anhydrous magnesium sulfate (MgSO4). The cleanup effect of the column was evaluated based on the rates of removal of tea components that interfered with pesticide recovery, henceforth referred to as interference components. Results showed that 14 pesticides had strong linearity in the range of 5-500 μg L-1 (r2 > 0.99). The quantitative limits were within the range of 3-50 μg kg-1. The average recoveries of 14 pesticides spiked into three different blank tea samples (green tea, black tea, oolong tea) at three levels of 0.05, 0.50 and 2.00 mg kg-1 were in the range of 62.3-108.8% with relative standard deviations of 0.2-13.6%. The m-PFC method can greatly improve the efficiency of sample pretreatment. Furthermore, this work provides methodological guidance on how to select cleanup materials and allocate their proportions.
Keywords: Liquid chromatography-tandem mass spectrometry; multi-plug filtration cleanup; selection of cleanup materials.