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• New extraction method of xenobiotics from human adipose tissue. • Good sensitivity was achieved by GC-MS and GC-FPD. • The LOD were between 4 to 9 ng/g for synthetic musks • The LOD were between 1 to 7 ng/g for organophosphorus pesticides • Galaxolide was found in all the analyzed human adipose tissue samples. Synthetic musks and organophosphorus pesticides represent a potential risk to the human health since exposure can lead to distinct types of carcinogenesis and endocrine disorders. These are lipophilic compounds as such, prone to deposit and persist in fat tissues, mainly in adipose tissue. Very few studies have reported on the occurrence and accumulation profile of these contaminants in human adipose tissue. Analytical methods for the detection and quantification of synthetic musks and organophosphorus pesticides in adipose tissue are lacking. In this study, the efficacy of different extraction with ultrasonic homogenizer and dispersive solid-phase extraction (d-SPE) clean-up methods were evaluated in human adipose tissue. The relative sample clean-up was assessed by measurement of total lipid content. The quantification of four synthetic musks and six organophosphorus pesticides were performed by gas chromatography (GC) mass spectrometry (MS) and flame photometric detection (FPD), respectively. The d-SPE clean-up with 50 mg PSA, 150 mg MgSO 4 , 100 mg C18EC and 50 mg Z-Sep provided the most effective clean-up, removing the greatest amount of interfering substances including lipids and simultaneously ensuring good chromatographic separation and recoveries. Method detection limits were between 4 to 9 ng/g for synthetic musk and 1 to 7 ng/g for organophosphorus pesticides in adipose tissue. The proposed method was applied to adipose tissue of obese patients and positive samples were confirmed with GC tandem mass spectrometry. Galaxolide was found in all the samples tested with concentrations ranging from 0.08 to 0.5 μg/g of adipose tissue. No other synthetic musk studied was detected. Organophosphorus pesticides were not found in the analysed samples. The developed analytical procedures were successful and can easily be applied to biomonitoring these compounds in human adipose tissue. [ABSTRACT FROM AUTHOR]