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Simultaneous distillation-extraction (SDE) is routinely used by analysts for sample preparation prior to gas chromatography analysis. In this work, a new process design and operation for microwave assisted simultaneous distillation-solvent extraction (MW-SDE) of volatile compounds was developed. Using the proposed method, isolation, extraction and concentration of volatile compounds can be carried out in a single step. To demonstrate its feasibility, MW-SIDE was compared with the conventional technique, SDE, for gas chromatography-mass Spectrometry (GC-MS) analysis of volatile compounds in a fresh aromatic herb, Zygophyllum album L., a wild salty desert herb belonging to the family Zygophyllaceae. SDE method required a long time (3 h) to isolate the volatile compounds, and large amounts of organic solvent (200 mL of hexane) for further extraction, while MW-SDE needed shorter time (only 30 min) to prepare the sample, and less amount of organic solvent (10 mL of hexane). These results show that MW-SDE-GC-MS is a simple, rapid and solvent-less method for the determination of volatile compounds from aromatic plants.