关键词: &alpha, -硫丹；&beta, -硫丹；硫丹硫酸酯；残留；气相色谱法；水产品

Abstract:

A gas chromatography method was established to analyze residues of α-endosulfan, β-endosulfan and endosulfan
sulfate in aquatic products. Samples were extracted with acetonitrile and ethyl acetate (4:1, V/V), frozen-degreased, purified
with tandem SPE columns (carbon-florisil followed by neutral alumina), and analyzed by gas chromatography with
electron capture detector (GC-ECD) and quantified by an external standard method. Each compound showed a good linear
relationship over the concentration range of 0.001–0.2 μg/mL. The recovery rates for shrimp, grass carp, oyster and eel
spiked with three different levels of endosulfan at 1, 10 μg/kg and 20 μg/kg ranged from 74.1% to 106%, with RSD between
1.22% and 7.79%. The limits of detection (LOD) for α-endosulfan, β-endosulfan and endosulfan sulfate were 0.035, 0.06
μg/kg and 0.06 μg/kg, respectively, and the limit of quantitation (LOQ) for all of them was 1.00 μg/kg. The method can be
applied in the detection of residues of endosulfan and its metabolites in fish, crustacean and shellfish.

Key words: &alpha, -endosulfan；&beta, -endosulfan；endosulfan sulfate；residue；gas chromatography；aquatic product