Simultaneous Determination of Dechlorane‐Related Compounds in Fish Muscle by Microwave‐Assisted Extraction Combined With Enhanced Matrix Removal for Lipids Cleanup and Gas Chromatography–Tandem Mass Spectrometry

ABSTRACT A robust and efficient analytical method was developed for the simultaneous determination of eight dechlorane‐related compounds in fish muscle using microwave‐assisted extraction combined with enhanced matrix removal for lipids cleanup and gas chromatography–tandem mass spectrometry. The method enables effective extraction of hydrophobic analytes from lipid‐rich matrices and efficient removal of co‐extracted lipids, resulting in improved analytical performance in terms of recovery and reproducibility. Under optimized conditions, the method exhibited good linearity ( R 2 = 0.9976–0.9997), low detection limits (method detection limits: 0.021–0.078 ng/g; limits of quantification: 0.067–0.248 ng/g), and satisfactory recoveries (77.6%–90.1%) with satisfactory precision (relative standard deviations: 2.9%–8.5%). Matrix effects were effectively controlled using matrix‐matched calibration combined with isotope‐labeled internal standards. The method was successfully applied to real fish samples, demonstrating reliable quantification of trace‐level dechloranes. Owing to its simplified workflow and improved throughput, the proposed method provides a practical and reliable approach for the routine analysis of dechloranes in high‐lipid biological matrices.