Fast gas chromatography with solid phase extraction clean-up for ultratrace analysis of pesticide residues in baby food

Abstract

A sample preparation method based on single solvent phase extraction and solid-phase extraction (SPE-NH 2) clean-up is studied in combination with fast capillary gas chromatography (GC) to determine 18 selected pesticides belonging to various chemical classes in apples, the common raw material for baby food production and baby food, at the concentration level ≤10 μg/kg maximum residual limit (MRL). Possibilities of mass spectrometry (MS) detector and electron capture detector (ECD) in fast gas chromatography (GC) of samples with complex matrice at ultra trace levels of pesticide residues were studied and compared. MS detection in single ion monitoring (SIM) mode provided higher selectivity compared to ECD. Optimisation of extraction as well as the simplifying of the whole process of sample preparation was carried out. Recoveries obtained at concentration level of 5 μg/kg (the required value for limit of quantification (LOQ) in baby food) were >90%, except of dimethoate (77.7%) and captan (46.4%) with MS detection. The obtained LOQs were at least 1 order lower than 5 μg/kg for the majority of compounds. The repeatability of gas chromatography–mass spectrometry (GC–MS) measurements of the matrix matched standards expressed as relative standard deviation was <11% except of captan and cypermethrin.