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This study describes the optimization and application of a method for quantitative analysis of flavor volatiles in beer using headspace solid-phase microextraction and gas chromatography–flame ionization detection (HS-SPME-GC-FID). These flavor volatiles can be divided into three groups: esters, alcohols, and organic acids. The fiber used was 85 µm polyacrylate. The parameters affecting the extraction of all these analytes were studied: sampling volume, extraction time, extraction temperature, and the dosage of NaCl. The optimized headspace extraction was carried out at 40°C for 30 min by adding 3 g of NaCl to 10-mL samples of beer in a 20-mL headspace vial. The optimized method was validated for linearity, precision, sensitivity, and accuracy, and results showed that the performance of the optimized method was good. The contents of 18 volatiles in nine domestic beer samples were analyzed with the optimized HS-SPME-GC-FID. Keywords: Headspace, Solid-phase microextraction (SPME), Beer, Flavor, Volatile