Determination of three natural pesticides in processed fruit and vegetables using high-performance liquid...

This paper describes a method for the sensitive and selective determination of two macrocyclic lactones (abamectin and spinosad) and azadirachtin in apple purée, concentrated lemon juice, tomato purée and canned peas. The general sample extraction-partitioning method for our gas chromatography and liquid chromatography multiresidue methods has been used. The analytical procedure involves an extraction with acetone and liquid-liquid partitioning with ethyl acetate/cyclohexane combined in one step. The extracts are analyzed by liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) without any further clean-up step. The pesticides are separated on a reversed-phase C12 column using a gradient elution. Thirteen simultaneous MS/MS transitions of precursor ions were monitored. Studies at fortification levels of 2.5-10 microg/kg and 25-100 microg/kg gave mean recoveries ranging from 70-100% for all compounds with satisfactory precision (relative standard deviation (RSD) from 3-20%). The excellent selectivity and sensitivity allows quantification and identification of low levels of pesticides in canned peas, tomato and apple purées (limits of quantitation (LOQs) 1-5 microg/kg) and in concentrated lemon juice (LOQs 2-10 microg/kg). The quantification of analytes was carried out using the most sensitive transition for every compound and by 'matrix-matched' standards calibration.