Combination of a cost-effective glass density separator followed by quantitative 1H-Nuclear Magnetic Resonance spectroscopy for the determination of microplastics in marine sediments

This work presents a method for determining the presence of microplastics in marine sediments. The method comprises a portable and cost-effective setup for separating microplastics using the principle of density floatation, followed by solubilization and quantitative qNMR spectroscopy. This method h...

Full description

Bibliographic Details
Authors: López Vázquez, Javier, Montes Goyanes, Rosa, Sánchez Pedregal, Víctor Manuel, Quintana Álvarez, José Benito, Rodil Rodríguez, María del Rosario
Format: article
Publication Date:2026
Country:España
Institution:Universidad de Santiago de Compostela (USC)
Repository:Minerva. Repositorio Institucional de la Universidad de Santiago de Compostela
Language:English
OAI Identifier:oai:dnet:minerva_____::88070cb33d649303f3dc7dd85c15e8bc
Online Access:https://hdl.handle.net/10347/47468
Access Level:Open access
Keyword:Density separation
Microplastics
Quantitative Nuclear Magnetic Resonance (qNMR)
Beach sand
Description
Summary:This work presents a method for determining the presence of microplastics in marine sediments. The method comprises a portable and cost-effective setup for separating microplastics using the principle of density floatation, followed by solubilization and quantitative qNMR spectroscopy. This method has been tested with polyethylene terephthalate (PET), polyvinyl chloride (PVC) and low-density polyethylene (LDPE) microplastics. The separation was carried out by using a novel home-made three-part glass setup and a separating solution of zinc chloride with a density of 1.6 g/cm3. Following Fenton clean-up, the supernatants were solubilized in suitable deuterated solvents and quantified by qNMR spectroscopy. The methodology was validated by the analysis of artificially spiked sediments at two levels, achieving recoveries between 71% and 105%, with relative standard deviation (RSD) below 22%. Method limits of quantification (MQLs) range from 15 to 245 ng/g. As a proof-of-principle application, sediment samples from three locations along the Galician coast (Northwest Spain) were analysed using the developed methodology. The concentrations of MP found in the marine sediments ranged from 62 to 186 ng/g of PET and from 192 to 229 ng/g of LDPE, with RSD ≤26%, whereas PVC was below the MQLs. This method allows for the estimation of the three polymer distribution and abundance in marine sediments in a swift, accurate and inexpensive way.