High sensitivity in quantitative analysis of mixed-size polystyrene micro/nanoplastics in one step

As emerging environmental pollutants, microplastics (MPs) and nanoplastics (NPs) pose a serious threat to human health. Owing to the lack of feasible and reliable analytical methods, the separation and identification of MPs and NPs of different sizes remains a challenge. In this study, a hyphenated method involving filtration and surface-enhanced Raman spectroscopy (SERS) for the separation and identification of MPs and NPs is reported. This method not only avoids the loss of MPs and NPs during the transfer process but also provides an excellent SERS substrate. The SERS substrate was fabricated by electrochemically depositing silver particles onto the reduced graphene oxide layer coated on stainless steel mesh. Results show that polystyrene (PS) MPs and NPs are efficiently separated on the SERS substrate via vacuum filtration, resulting in high retention rates (74.26 % ± 1.58 % for 100 nm, 81.06 % ± 1.49 % for 500 nm, and 97.73 % ±0.11 % for 5 μm) and low limit of detection (LOD). The LOD values of 100 nm, 500 nm, and 5 μm PS are 8.89 × 10^-5, 3.39 × 10^-5, and 1.57 × 10^-4 μg/mL, respectively. More importantly, a linear relationship for uniform quantification of 100 nm, 500 nm, 3 μm and 5 μm PS was established, and the relationship is Y = 225.61 lgX + 1076.36 with R² = 0.980. The method was validated for the quantitative analysis of a mixture of 100 nm, 500 nm PS NPs, 3 μm and 5 μm PS MPs in a ratio of 1:1:1:1, which successfully approaches the evaluation of evaluated PS NPs in the range of 10^-4-10 μg/mL with an LOD value of approximately 7.82 × 10^-5 μg/mL. Moreover, this method successfully detected (3.87 ± 0.06) × 10^-5 μg MPs and NPs per gram of oyster tissue.