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Density separation-Raman spectroscopic quantification of microplastic-antibiotic co-contamination and transport in plastic-mulched agricultural soils.
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Scientists developed a highly accurate new method to measure tiny plastic pieces and antibiotic residues together in farm soils covered with plastic mulch film. They found that as these plastic fragments break down and weather over time, they become better at soaking up antibiotics and can actually help carry them further through soil, meaning old, weathered microplastics in farmland could be helping antibiotic pollution spread into groundwater and, potentially, our food and water supply.
Plastic-mulched soils contain mineral particles, organic matter and weathered polymer fragments that complicate the joint measurement of microplastics and co-occurring antibiotics. We developed a matrix-adaptive workflow combining sequential Fenton-enzymatic digestion, ZnCl/NaI cascade density separation, silver-membrane collection, µ-Raman chemical imaging and isotope-dilution LC-MS/MS. Performance was evaluated with four agricultural soils, four mulch-relevant polymers, two particle-size fractions, pristine and aged surfaces, and tetracycline, ciprofloxacin and sulfamethoxazole. Across 2304 independent particle-spike observations, mean microplastic recovery was 93.72 ± 3.17% (95% confidence interval, 93.59-93.85%), within-laboratory relative standard deviations were 2.5-3.4%, and Raman classification accuracy was 96.25%. Antibiotic recovery across 432 observations was 95.31 ± 3.61%; matrix effects ranged from -14.2 to 5.3%, while matrix-matched calibration gave values of 0.9995-0.9998. Pyrolysis GC-MS confirmed Raman-derived mass estimates ( = 0.9897), with a mean inter-platform bias of 0.022 mg. Aging increased XPS O/C ratios, AFM roughness and BET area and nearly doubled Langmuir capacities; aged polyamide reached 32.66 mg g for tetracycline. In saturated columns, pristine polyethylene slightly advanced breakthrough, whereas aged polyethylene and polyamide shifted the 50% breakthrough point from 2.34 pore volumes without microplastics to 2.86 and 3.22 pore volumes, respectively. Factorial and mixed-effects analyses, multiplicity-controlled contrasts, grouped cross-validation and an uncertainty budget supported the method's cross-matrix robustness. The workflow provides a quantitative basis for linking analytical recovery, particle surface chemistry and contaminant migration in complex agricultural soils.
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