Determination of polar pesticide residues in vegetable and fruit by supercritical fluid chromatography­Q­Orbitrap

Abstract

ObjectiveTo establish a method for determination of 12 polar pesticide residues in vegetables and fruits by supercritical fluid chromatography­Q­Orbitrap （SFC­Q­Orbitrap）.MethodsThe samples were extracted with 1% acidified methanol，and the extract was purified by dispersed solid phase extraction， separated by ultra silica column （150 mm× 2.1 mm， 3 μm） and obelisc r column （150 mm× 2.1 mm， 5 μm）， determined by SFC­Q­Orbitrap， scanned by segmented mixed product ions， and quantified by isotope internal standard calibration curve.ResultsThe calibration curves for 12 pesticides exhibited good linearity in the range of 20.0­500 μg/L， with the correlation coefficients（R2） above 0.997. The average recoveries at 0.05 and 0.20 mg/kg spiked levels were in the range of 80.2%­120% and the relative standard deviations （RSD，n＝6） were in the range of 2.14%­14.6%. The limits of detection and the limits of quantification were 0.010 1­0.016 2 mg/kg and 0.050 mg/kg.ConclusionThe method has the advantages of simple operation， accurate quantification and high efficiency. It can meet the requirements determination of high polar pesticide residues in vegetables and fruits.

Keywords

• polar pesticide residues
• supercritical fluid chromatography
• q­orbitrap