The global methods approved and reliable for the analysis of dioxins in food and feed, which take a lot of time, money and effort in addition to that, take many harmful solvents. A simple and rapid method for sample preparation and extraction of dioxins from food developed using freeze-drying (FD) and accelerated solvent extraction (ASE) techniques, respectively. Average recoveries of dioxins extracted from the food obtained by a conventional soxhlet extraction and the ASE almost equal, when the data compared by both methods. Moreover, decrease the time of tissue extraction from 24 hours using soxhlet to only 35 minutes using ASE technique. Development of dioxin analysis in food and feed samples by entire method of fat extraction based on ASE for determination of dioxin compounds with high-resolution gas chromatography-high resolution mass spectrometry (HRGC/HRMS) from food and feed samples was developed. Optimization conditions for ASE method are effective and reliable by using Dionex ASE 350 as follows oven temperature: 150 °C, static cycle time: 5 minute, cycle'sno.: 4, flush volume: 100%, purge time: 90 sec, cell pressure: 1590 psi (nitrogen gas) and total extraction time: 35 min per sample.Extraction solvents used for fatty-food samples such as fish, meat and liver were Hexane: DCM (1:1 v,v). While toluene used for extraction of Non-fatty food samples. Quality assurance for ASE extraction method such as precision and recovery as well as robustness and natural contaminated samples evaluated through certified reference materials (CRM) analysis. Accuracy of PCDD/Fs estimated with CRM for Trout sample was below 4% for both ASE and soxhlet, (complying with EU requirement ≤ 20%). This study was to compare efficiency of various extraction tools to determine the content of dioxins in food and feed samples by using accelerated solvent extraction technique (ASE) with those prepared by extraction in soxhlet technique.