Microplastics are fragments less than 1 μm in size that are tiny enough to bypass wastewater treatment facilities, eventually accumulating in aquatic life and posing a serious threat to the food chain. Owing to their hydrophobic nature, microplastics can adsorb or accumulate PFAS and act as carriers of organic pollutants such as polyfluoroalkyl substances. Microplastic concentrations found in aquatic matrices range from 1 to 26 particles/L, which is crucial for the development of detection methods and the measurement of new microplastic concentrations down to ppb. The ideal method for detection should be convenient, allow for onsite monitoring, be highly sensitive, have a low detection limit, avoid pretreatment, be economical, and be environmentally friendly. This chapter highlights the prevalence of MPs and PFASs and their co-occurrence as secondary pollutants. The current challenges and costs associated with adopting new detection technology and sustainable MPS removal are examined to ensure water safety.