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Microplastics and nanoplastics are persistent, nonbiodegradable pollutants with potential toxic effects on aquatic ecosystems and human health. Their removal requires innovative technologies, and adsorption has emerged as a promising method for water purification. This study investigates the adsorption of 0.2 µm polystyrene nanoplastics using commercially available zeolites (H-USY, H-β, X, clinoptilolite). For the first time, quantitative UV-vis spectroscopy in transmission and diffuse reflectance (DR UV-vis) modes were employed to analyze the adsorption and desorption process. This novel method ensures precise, repeatable, and reliable quantification of polystyrene concentration in both solution and adsorbent, enabling an accurate assessment of sorption efficiency. With minimal sample preparation and real-time monitoring, it serves as an effective tool for evaluating sorbents in nanoplastic removal. H-USY and clinoptilolite demonstrated high adsorption performance at 100 and 200 mg·L⁻¹ , with a sorption time of 20 minutes. The adsorption capacity of H-USY ranged from 80–91 mg·L⁻¹ (100 mg·L⁻¹) and 160–166 mg·L⁻¹ (200 mg·L⁻¹), while clinoptilolite reached 80–92 mg·L⁻¹ and 170–190 mg·L⁻¹ , respectively, depending on the sorbent dose. Studies on the renewable efficiency of the zeolite adsorbents (burning off of plastic, ultrasound treatment) have shown that the material retains its high adsorption capacity after several regeneration cycles. These findings suggest that zeolite can be effectively reused, making it a sustainable option for long-term applications in nanoplastic removal. These findings highlight the potential of zeolites as efficient, regenerable adsorbents for nanoplastic removal, offering a sustainable approach to mitigating environmental pollution.