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Advanced Spectroscopic and Thermoanalytical Quantification of LLDPE in Mealworm Frass: A Multitechnique Approach
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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.
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Advanced Spectroscopic and Thermoanalytical Quantification of LLDPE in Mealworm Frass: A Multitechnique Approach
AI summary Read the abstract
This study applied a multitechnique analytical approach including thermal decomposition-FTIR-MS, TGA under inert atmosphere, and solid-state ¹³C CP-MAS NMR with chemometric iPLS modeling to detect and quantify LLDPE in Tenebrio molitor mealworm frass. CP-MAS NMR provided the highest sensitivity, detecting polyethylene signals at concentrations as low as 0.096% w/w, supporting its application as the most robust method for quantifying plastic residues in biological matrices in insect-mediated biodegradation studies.
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Researchers investigated whether measurement methods could distinguish between Tenebrio molitor mealworm larvae fed plastic substrates versus conventional diets, testing larvae on flour-carrot, polystyrene foam, and mixed diets. The study sought to identify industrially viable detection approaches to verify plastic biodegradation by larvae and their gut microbiota, supporting their potential use in plastic waste management.
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