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In the present study, a new extraction method using microwave-assisted extraction (MAE) combined with Py\u2013GC\/MS was developed to extract and quantify a wide range of plastic polymers, and the method was validated using different environmental matrices. This new extraction method was able to extract polyethylene, polystyrene, polypropylene, poly(methyl-methacrylate) (PMMA), polyvinylchloride (PVC), and polycarbonate in dichloromethane with good recoveries (92.9\u2013119.7%). The limit of detection and limit of quantification (LOQ) of the method ranged from 0.002 to 0.18\u2009\u00b5g and from 1.2 to 5.8\u2009\u00b5g, respectively. Intra- and interday repeatability values with coefficients of variation less than 25% for all polymers were obtained. Method validation also included a spike and recovery using all polymers from clean water, dirty water, and shrimp and salmon fillet samples, with recoveries of 85 to 111, 87 to 138, 81 to 122, and 50 to 151%, respectively. Finally, the method was tested on unspiked wild mussels and bottled water for proof-of-concept. Both polyethylene and PVC were detected and quantified in mussels, and polycarbonate and polypropylene were detected below the LOQ. For bottled water, polypropylene, polystyrene, and polycarbonate were all detected below the LOQ. We introduce a method combining MAE and Py\u2013GC\/MS as a tool for mass quantification of microplastics. This method can be used as a stand-alone, or as a complementary method to spectroscopic techniques. Environ Toxicol Chem 2021;40:2733\u20132741. \u00a9 2021 SETAC<\/jats:p>\n               <jats:p>Abstract<\/jats:p>\n               <jats:p>Microwave-assisted extraction (MAE) of microplastics and their analysis by pyrolysis\u2013gas chromatography\/mass spectrometry (Py\u2013GC\/MS). Sample extraction and analysis are done at the same time as external calibration curves, allowing the quantification of six polymer types in various sample matrices. 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