Two sample pretreatment methods and their applications in the determination of 111 pesticides and related chemicals in aquatic products

Se pu = Chinese journal of chromatography
Jianfeng SuDonghu Chen

Abstract

Two sample pretreatment methods were developed and applied to determine 111 residues of pesticides in aquatic products. For Method I, the residues were extracted from homogenized tissue with acetone-ethylacetate-n-hexane (1 : 1 : 1, v/v/v), and then were redissolved in acetonitrile; for Method II, the residues were extracted from homogenized tissue with acetonitrile - water under ultrasonication, and then were separated by liquid-liquid partition. The supernatants were purified using solid phase extraction (Envi-18 and PSA columns) prior to the GC-MS analysis. The determination was performed in selected ion monitoring (SIM) mode with the external calibration for quantitative analysis. Under the optimal conditions, the detection limits (S/N = 3) for residues of pesticides were in the ranges of 0.001 -0.026 mg/kg. The recoveries of Method I for the spiked standards at concentration of 0.25 mg/kg were 72% - 113% with the relative standard deviations (RSDs) of 3.4% - 12.1%. The recoveries of Method II were 51% - 127%, among which the recoveries for 94% pesticides were between 70% and 120% with the RSDs of 3.2% - 13.8%.

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