Determination of organochlorine compounds in fish liver by ultrasound-assisted dispersive liquid–liquid microextraction based on solidification of organic droplet coupled with gas chromatography-electron capture detection

Abstract

A simple and rapid method for the extraction of organochlorine compounds (OCs) including poly-chlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in fish liver using ultrasound assisted dispersive liquid–liquid microextraction based on the solidification of floating organic droplet (US-DLLME-SFO) was developed. For reducing the complexity of the matrix, the sample was pre-treated prior to microextraction. Factors affecting US-DLLME-SFO were optimized by using statistical design of experiment (DoE). The analysis was carried out by Gas Chromatography (GC) equipped with micro electron capture detector (μ-ECD). The optimized parameters were 4.8 min of ultrasound, 3.0 mL of Milli-Q and 24 μL of 1-undecanol as an extraction solvent as determined by DoE. US-DLLME-SFO was validated in terms of limit of detection, limit of quantification, dynamic linearity range, coefficient of determination (linearity) and extraction recovery in fish liver for OCs, and the respective values were (1.06-3.84 ng g−1), (3.50-12.67 ng g−1), (1.0–500 ng g−1), (R2 = 0.994-0.999), (88.5-108.4%). Interday and intraday precisions were evaluated as relative standard deviation (% RSD) and the values were ≤10%.