Rapid Determination of 36 Pesticide Residues in Fruits by Solid-phase Extraction-Gas Chromatography-Mass Spectrometry
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Abstract:
A gas chromatography-mass spectrometry (GC/MS) method for the determination of 36 pesticide residues in fruits was established on the basis of the selection of solid phase extraction column, extraction solvent and eluent volume. The fruit samples were extracted with acetonitrile, purified by graphitized carbon black/amino solid-phase column (PC/NH2) t, analyzed by GC/MS with the single ion monitoring scanning mode (SIM), and quantified by the matrix-matched method with external standards. All the targeted substances showed a good linear correlation in the range of 70.00 ng/mL~560.0 ng/mL, with the correlation coefficients (R2) not less than 0.990. The limit of detection (LOD) of the method ranged in 0.0001~0.0018 mg/kg when the signal/noise (S/N) ration =3, with the limit of quantification (LOQ) in the range of 0.0002~0.0060 mg/kg (S/N=10). The spiked recovery tests were carried out at low, medium and high levels of the extraction matrix. The average recovery of the method ranged in 60.6 %~116.5 % with the relative standard deviations (RSDs, n=6) in the range of 0.8%~9.5%.The results demonstrated that the method is simple and the outcome of purification of matrix by solid phase extraction was satisfactory. Owing to high specificity and broad range of application, this method is suitable for screening and verification of multicomponent pesticide residues in pome fruits and small climbing fruits.
