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Advanced Spectroscopic and Thermoanalytical Quantification of LLDPE in Mealworm Frass: A Multitechnique Approach
Summary
This study presented the first proof-of-concept application of a multitechnique analytical framework including TGA, TGA-FTIR-MS, and solid-state ¹³C CP-MAS NMR for quantifying linear low-density polyethylene (LLDPE) in Tenebrio molitor mealworm frass. CP-MAS NMR provided matrix-independent quantification with a detection limit of 0.173% w/w and a quantification limit of 0.525% w/w, lying within the reported ingestion range for mealworms, establishing NMR as the most robust tool for quantifying polyethylene residues in complex biological matrices.
Plastic pollution from polyethylene-based materials is a critical environmental concern due to their high persistence. Here, we report the first proof-of-concept application of a multitechnique analytical framework for quantifying linear low-density polyethylene (LLDPE) in Tenebrio molitor frass. Artificially enriched frass–LLDPE mixtures were analyzed using thermogravimetric analysis (TGA), TGA coupled with Fourier-Transform Infrared Spectroscopy (FTIR) and Mass Spectrometry (MS), TGA under inert atmosphere, and solid-state 13C nuclear magnetic resonance spectroscopy with Cross-Polarization and Magic Angle Spinning (CP-MAS NMR) 13C CP-MAS NMR combined with interval Partial Least Squares (iPLS) modeling. Thermal methods provided insight into decomposition pathways but showed reduced specificity at <1% w/w due to matrix interference. CP-MAS NMR offered matrix-independent quantification, with characteristic signals in the 10–45 ppm region and a calculated LOD and LOQ of 0.173% and 0.525% w/w, respectively. The LOQ lies within the reported ingestion range for T. molitor (0.8–3.2% w/w in frass), confirming biological relevance. This validated workflow establishes CP-MAS NMR as the most robust tool for quantifying polyethylene residues in complex matrices and provides a foundation for in vivo biodegradation studies and environmental monitoring.