A novel Py-GC-MS method was developed for the quantification of microplastics in environmental samples, addressing the need for reliable analytical techniques to assess microplastic pollution in terrestrial and freshwater ecosystems. A multi-ion approach using one quantification ion and two confirmation ions for each of 12 common polymer types was developed and validated according to the NF T 90-210 standard. Rigorous sampling and pretreatment protocols were implemented. The method was demonstrated to be applicable in quantifying microplastics in complex environmental sample. Five polymers were quantified in the compost sample with a total concentration of 300 µg/kg, polyethylene accounting for 80% besi. The developed Py-GC-MS method provides a robust analytical approach for the identification and quantification of microplastics in complex environmental matrices.