期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1642, 期 -, 页码 -出版社
ELSEVIER
DOI: 10.1016/j.chroma.2021.462036
关键词
Deep eutectic solvent; Low transition temperature mixture; Pesticides; Urine; Liquid chromatography; Dispersive liquid-liquid microextraction
资金
- INAIL (Istituto Nazionale per l'Assicurazione contro gli Infortuni sul Lavoro)
- (National Institute for Insurance against Accidents at Work) [2019-2021 [BRIC 2019]]
Biomonitoring is an effective tool for controlling health risks in populations exposed to various chemicals. The study presents a new approach using dispersive liquid-liquid microextraction (DLLME) with a low transition temperature mixture as the extraction solvent for analyzing pesticides in urine samples. The method offers advantages in terms of rapidity, simplicity, efficiency, and cost-effectiveness compared to other methods, and has been successfully applied in analyzing urine samples from volunteers.
Biomonitoring is a potent tool to control the health risk of people occupationally and non-occupationally exposed. The latest trend in bioanalytical chemistry is to develop quick, cheap, easy, safe and reliable green analytical procedures to analyse a large number of chemicals in easily accessible biomatrices such as urine. In this paper, a new dispersive liquid-liquid microextraction (DLLME) procedure, conceived to treat urine samples and based on the use of a low transition temperature mixture (LTTM), was developed and validated to analyse twenty pesticides commonly used in farm practises. The LTTM was composed of choline chloride and sesamol in molar ratio 1:3 (ChC1:Ses 1:3); its characterization via differential scanning calorimetry identified it as an LTTM and not as a deep eutectic solvent due to the occurrence of a glass transition at -71 degrees C. The prepared mixture was used as the extraction solvent in the DLLME procedure, while ethyl acetate as the dispersing solvent. The salting out effect (50 mg mL(-1) of NaCl in a diluted urine sample) improved the separation phase and the analyte transfer to the extractant. Due to the high ionic strength and despite the density of ChCl:Ses 1:3 (1.25 g mL(-1)), the LTTM layer floated on the top of the sample solution after centrifugation. All extracts were analysed by high-performance liquid chromatography coupled to mass spectrometry. After optimization and validation of the whole method, lower limits of quantitation were in the range of 0.02 - 0.76 mu g L-1. Extraction recoveries spanned from 50 to 101 % depending on the spike level and analytes. Precision and accuracy ranges were 3-18% and 5-20%, respectively. The extraction procedure was also compared with other methods, showing to be advantageous for rapidity, simplicity, efficiency, and low cost. Finally, urine samples from ten volunteers were effectively analysed using the developed method. (C) 2021 Elsevier B.V. All rights reserved.
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