Multiplug filtration clean-up with multiwalled carbon nanotubes in the analysis of pesticide residues using LC-ESI-MS/MS.

A novel design for a rapid clean-up method was developed for the analysis of pesticide residues in fruit and vegetables followed by LC-ESI-MS/MS. The acetonitrile-based sample extraction technique was used to obtain the extracts, and further clean-up was carried out by applying the streamlined procedure on a multiplug filtration clean-up column coupled with a syringe. The sorbent used for clean-up in this research is multiwalled carbon nanotubes, which was mixed with anhydrous magnesium sulfate to remove water from the extracts. This method was validated on 40 representative pesticides and apple, cabbage, and potato sample matrices spiked at two concentration levels of 10 and 100 μg/kg. It exhibited recoveries between 71 and 117% for most pesticides with RSDs < 15%. Matrix-matched calibrations were performed with the coefficients of determination >0.995 for most studied pesticides between concentration levels of 10-500 μg/L. The LOQs for 40 pesticides ranged from 2 to 50 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market fruit and vegetable samples.