Assessment of benzothiazoles, benzotriazoles and benzenesulfonamides in environmental waters using an optimized combination of microextraction by packed sorbent with programmed temperature vaporization-gas chromatography tandem-mass spectrometry

This work proposes a new method for the quantification of benzothiazoles (BTs), benzotriazoles (BTRs), and benzenesulfonamides (BSAs) in tap water, river water, and wastewater. The protocol involved the use of microextraction by packed sorbent (MEPS), applied for the first time for the extraction of the target analytes, combined with programmed temperature vaporization-gas chromatography-triple quadrupole mass spectrometry (PTV-GC-QqQ-MS). Considering the synergism between MEPS extraction and PTV injection, the experimental variables affecting their performance were simultaneously optimized by experimental design, while principal component analysis (PCA) was used to find the overall optimal working conditions. Response surface methodology was used to gain a comprehensive understanding of the effects of working variables on method performance. The developed method achieved very good linearities and satisfactory intra- and inter-day accuracies and precisions. The protocol permitted the detection of the target molecules with limit of detection (LODs) values between 0.005 and 0.85 mu g/L. The green character of the procedure was evaluated using three metrics: Analytical Eco-Scale, Green Analytical Procedure Index (GAPI), and Analytical Greenness metric for sample preparation (AGREEprep). The satisfactory results obtained with real water samples demonstrate the applicability of the method for monitoring campaigns and exposome studies.

Automated summary

This study proposes a new method for quantifying BTs, BTRs, and BSAs in tap water, river water, and wastewater. The method combines microextraction by packed sorbent (MEPS) and programmed temperature vaporization-gas chromatography-triple quadrupole mass spectrometry (PTV-GC-QqQ-MS). Experimental design and principal component analysis (PCA) were used to optimize the variables affecting the performance of MEPS and PTV injection. The method achieved good linearity, accuracy, and precision, with LODs between 0.005 and 0.85 μg/L. The greenness of the procedure was assessed using Analytical Eco-Scale, GAPI, and AGREEprep metrics. The satisfactory results obtained with real water samples demonstrate the method's applicability for monitoring campaigns and exposome studies.