Microplastics (MPs) have emerged as pervasive contaminants in aquatic ecosystems, presenting severe risks to environmental and public health. Conventional analytical techniques, although accurate, often involve environmentally hazardous reagents and energy-intensive protocols. This review critically assesses the evolution of analytical methodologies used to detect and quantify MPs, with particular focus on green analytical chemistry (GAC) principles. The paper evaluates sample preparation, extraction, and detection methods aligned with sustainable practices and introduces recent innovations in green solvents, enzymatic digestion, and spectroscopic analysis. Future trends in eco-friendly analytical instrumentation and data integration tools are also discussed. This work provides researchers and policy-makers with a comprehensive perspective on sustainable microplastic quantification strategies, vital for long-term environmental monitoring and pollution mitigation.