Determination of Residual Diisocyanates and Related Diamines in Biodegradable Mulch Films Using N-Ethoxycarbonylation Derivatization and GC-MS

Abstract

Diisocyanates are highly reactive compounds with two functional isocyanate groups. The exposure of diisocyanates is associated with severely adverse health effects, such as asthma, inflammation in the respiratory tract, and cancer. The hydrolysis product from diisocyanates to related diamines is also a potential carcinogen. Here, we developed an effective, accurate, and precise method for simultaneous determination of residual diisocyanates and related diamines in biodegradable mulch films, based on N-ethoxycarbonylation derivatization and gas chromatography-mass spectrometry. The method development included the optimization of ultrasonic hydrolysis and extraction, screening of N-ethoxycarbonylation conditions with ethyl chloroformate, evaluation of the diamines degradation, and analysis of the fragmentation mechanisms. Under the optimum experimental conditions, good linearity was observed with R2 > 0.999. The extraction recoveries were found in the range of 93.9–101.2% with repeatabilities and reproducibilities in 0.89–8.12% and 2.12–10.56%, respectively. The limits of detection ranged from 0.0025 to 0.057 µg/mL. The developed method was applied to commercial polybutylene adipate co-terephthalate (PBAT) biodegradable mulch film samples for analysis of the diverse residual diisocyanates and related diamine additives. The components varied greatly among the sample from different origin. Overall, this study provides a reliable method for assessing safety in biodegradable mulch films.

Development and Application of Portable Reflectometric Spectroscopy Combined with Solid-Phase Extraction for Determination of Potassium in Flue-Cured Tobacco Leaves

“…It is evident that the proposed water extraction following the test strips and reflectometric spectroscopy method proved high accuracy and precision, which meets the requirements of the International Council for Harmonization (ICH) guidelines. 39 …”

“…which meets the requirements of the International Council for Harmonization (ICH) guidelines 39. 2.6.…”

Amine Switchable Hydrophilic Solvent Vortex-Assisted Homogeneous Liquid–Liquid Microextraction and GC-MS for the Enrichment and Determination of 2, 6-DIPA Additive in Biodegradable Film

“…Switchable hydrophilicity solvent homogeneous liquid-liquid microextraction (SHS-HLLME) has been receiving increasing attention as reflected by Extraction, cleanup, and enrichment are key steps in sample preparation for complex matrices. Currently, sample extraction methods for the analysis of additives in plastics include ultrasound-assisted extraction [11], Soxhlet extraction [12], microwave-assisted extraction [13], accelerated solvent extraction [14], and heating extraction [15]. Compared to others, the heating extraction method is relatively simple to operate.…”

A thermoanalytical insight into the composition of biodegradable polymers and commercial products by EGA-MS and Py-GC-MS

“…Additionally, 1,6-diisocyanato-hexane is identified at 14.7 min. This is often used as a chain extender during the polycondensation of PBAT[61]-[63].J o u r n a l P r e -p r o o fThe most intense peak featured in the Py-GC-MS chromatogram of PBS is related to the di(3-butenyl) ester of succinic acid (15.6 min). As for PBAT, the peak related to 1,3-butadiene is very intense, in agreement with the high relative abundance of ions at m/z 54 and 55 in the EGA profile.…”