Pressurized Liquid Extraction and Microwave-Assisted Extraction in the Determination of Organochlorine Pesticides in Fish Muscle Samples

Abstract

This paper describes a comparative study of 2 extraction methods, pressurized liquid extraction (PLE) and microwave-assisted extraction (MAE), for the determination of organochlorine pesticides (OCPs) in fish muscle samples. In both cases, samples were extracted with hexaneacetone (50 + 50), and the extracts were purified by solid-phase extraction using a carbon cartridge as the adsorbent. Pesticides were eluted with hexaneethyl acetate (80 + 20) and determined by gas chromatography with electron-capture detection. Both methods demonstrated good linearity over the range studied (0.0050.100 g/mL). Detection limits ranged from 0.029 to 0.295 mg/kg for PLE and from 0.003 to 0.054 mg/kg for MAE. For most of the pesticides, analytical recoveries with both methods were between 80 and 120, and the relative standard deviations were <10. The proposed methods were shown to be powerful techniques for the extraction of OCPs from fish muscle samples. Although good recovery rates were obtained with both extraction methods, MAE provided advantages with regard to sample handling, cost, analysis time, and solvent consumption. Acceptable validation parameters were obtained although MAE was shown to be more sensitive than PLE.

Occurrence of Organochlorine Pesticides Residues in Animal Feed and Fatty Bovine Tissue

“…In addition, several standardised methods, including AOAC 970.52, EN 1528 and EN 12393, have employed such solid-liquid or liquid-liquid extraction techniques for the determination of OCPs in both fatty and non-fatty foods. [43,44,45] In some occasions, sonication or Polytron was also applied to improve the extraction efficiency and recoveries.…”