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Abstract: A method for determining the volatile organic compounds (VOCs) in textiles was developed, by the use of high capacity headspace, solid phase micro extraction (SPME) and gas chromatography–mass spectrometry (GC/MS). The detection targets contained total organic compounds (TVOCs) and six specific substances (toluene, vinylcyclohexene, styrene, 4-phenylcyclohexene, vinylchloride and butadiene), according to Oeko-Tex Standard 100. A designed experiment was used to optimize the headspace–SPME–GC/MS operation, and the method was validated in terms of linearity, limit of detection (LOD) and method precision. It was found that at a loading ratio of 10m2/m3, the LODs for toluene, vinylcyclohexene, styrene and 4-phenylcyclohexene were 0.0002mg/m2, 0.01mg/m2, 0.01mg/m2 and 0.0001mg/m2 respectively, while for vinylchloride and butadiene they were both 0.08mg/m2. SPME exhibited better adsorption performance for toluene, vinylcyclohexene, styrene and 4-phenylcyclohexene, for which the extraction fractions were 10 times of those for vinylchloride and butadiene. The method developed was successfully applied to analyze several commercial textiles, and would be a simple, efficient and promising technique for the analysis of volatile compounds from textiles or other samples (such as polymer materials). [Copyright &y& Elsevier]