Abstract

Stir bar sorptive extraction with in-situ derivatization using 2,3-diaminonaphthalene (DAN) followed by liquid desorption and high performance liquid chromatography with diode array detection (SBSE(DAN) in-situ -LD-HPLC-DAD) was developed for the determination of glyoxal (Gly) and methylglyoxal (MGly) in environmental and biological matrices. DAN proved very good specificity as in-situ derivatising agent for Gly and MGly in aqueous media, allowing the formation of adducts with remarkable sensitivity, selectivity and the absence of photodegradation. Assays performed on spiked (1.0 μg L −1) water samples, under convenient experimental conditions, yielded recoveries of 96.2 ± 7.9% for Gly and 96.1 ± 6.4% for MGly. The analytical performance showed good accuracy, suitable precision (<12.0%), low detection limits (15 ng L −1 for Gly and 25 ng L −1 for MGly adducts) and excellent linear dynamic ranges ( r 2 > 0.99) from 0.1 to 120.0 μg L −1. By using the standard addition method, the application of the present method to tap and swimming-pool water, beer, yeast cells suspension and urine samples allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for routine quality control analysis, showing to be easy to implement, reliable, sensitive and with a low sample volume requirement to monitor Gly and MGly in environmental and biological matrices.

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