RESUMO
A new method has been developed to determine heptachlor and its metabolites heptachlor-exo-epoxide and heptachlor-endo-epoxide in pork. The pork samples were extracted with acetone-n-hexane (2:8, V:V) and cleaned up by gel permeation chromatography and florisil solid-phase extraction cartridge. The extract was then determined by gas chromatography equipped with electron capture detector (GC-ECD), followed by validation using gas chromatography-mass spectrometry (GC-MS) with negative chemical ionization. Linearity of calibration curves ranged from 0.01 to 0.5 mg L(-1), with correlation coefficients of more than 0.9980 for GC-ECD and GC-MS, respectively. At spiked concentrations of 0.01, 0.05, and 0.1 mg kg(-1), the average recovery and relative standard deviation values were 87.1-102.2 and 4.0-11.3%, respectively. The limit of quantification for each analyte was 0.01 mg kg(-1), which satisfied the current maximum residue limit permitted in pork. Our results showed that the method developed was successfully used to determine heptachlor and heptachlor epoxide residues in real pork samples.
