An eco-friendly approach developed for the microextraction of N-nitrosamines in water and beverage samples with deep eutectic solvent and multivariate optimization
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引用次数: 0
Abstract
N-nitrosamines are a class of environmental and beverage contaminants known for their carcinogenic potential in humans. In this study, a deep eutectic solvent was employed in hollow fiber microporous membrane liquid-liquid extraction for the determination and quantification of six nitrosamines (N-nitrosopyrrolidine, N-nitrosomethylethylamine, N-nitrosopiperidine, N-nitrosodiethylamine, N-nitrosodi-n-propylamine, and N-nitrosodi-n-butylamine) in water and beverages by high-performance liquid chromatography and diode array detection. The deep eutectic solvent was selected using a univariate strategy, while the subsequent steps were optimized through multivariate approaches. A simplex-centroid design with a process variable was employed to optimize the solvent mixture and desorption time, whereas a Box-Behnken design was used to optimize pH, NaCl concentration, and extraction time. The optimized conditions were comprised of levulinic acid: thymol (1:1) as extractor solvent; a mixture of 45 μL of methanol, 111 μL of ultrapure water, and 144 μL of ethanol was used as desorption solvent, and the desorption time was fixed at 20.4 min; and extraction time last 31.5 min, at pH 3.9 and 8.5 % (w/v) of NaCl. For all curves in ultrapure water, ANOVA values were statistically validated. LODs and LOQs were 3.3 and 10 μg L−1 for all analytes. Intraday and interday precision ranged from 2.3 % to 18.3 % and 5.2 % to 19.7 %, respectively. The relative recoveries were obtained in vinegar samples, and the range was 74.2 % to 119.2 %. Five samples, collected from a river, a lagoon, and three beverages, were analyzed using the proposed methodology. The analyte concentrations were not detected in these samples or were lower than the LOQ.
期刊介绍:
The Microchemical Journal is a peer reviewed journal devoted to all aspects and phases of analytical chemistry and chemical analysis. The Microchemical Journal publishes articles which are at the forefront of modern analytical chemistry and cover innovations in the techniques to the finest possible limits. This includes fundamental aspects, instrumentation, new developments, innovative and novel methods and applications including environmental and clinical field.
Traditional classical analytical methods such as spectrophotometry and titrimetry as well as established instrumentation methods such as flame and graphite furnace atomic absorption spectrometry, gas chromatography, and modified glassy or carbon electrode electrochemical methods will be considered, provided they show significant improvements and novelty compared to the established methods.