Automatic Multi-Plug Filtration Cleanup Tip-Filtration with Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry Detection For 22 Pesticide Residues in Typical Vegetables.

An automatic multi-plug filtration cleanup (m-PFC) tip-filtration method was developed to reduce the manual operation workload in sample preparation. In this work, m-PFC was based on multi-walled carbon nanotubes mixed with primary secondary amines and anhydrous magnesium sulfate (MgSO4) in a packed column for analysis of pesticide residues followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry. Method validation was performed on 22 pesticide residues in carrot, spinach and leek, at spiked levels of 5, 10 and 50 μg/kg, respectively. The average recoveries were between 70.1 and 119.5% with associated relative standard deviations <20% (n = 6) indicating satisfactory accuracy and repeatability. Matrix-matched calibration curves were performed with the correlation coefficients (R2) higher than 0.9903 within a linearity range of 5-100 ng/mL. The limits of quantification were 5 μg/kg for all the pesticides in carrot, spinach and leek matrices. The developed method was successfully used to determine pesticide residues in market samples.