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优化基于涡旋辅助疏水磁性深共晶溶剂的分散液相微萃取法,用于实际样品中氯硝柳胺的定量分析。

Optimization of vortex-assisted hydrophobic magnetic deep eutectic solvent-based dispersive liquid phase microextraction for quantification of niclosamide in real samples.

机构信息

Faculty of Science, Department of Chemistry, Sivas Cumhuriyet University, Sivas, Türkiye.

Gdansk University of Technology, Faculty of Civil and Environmental Engineering, Department of Sanitary Engineering, G. Narutowicza St. 11/12, Gdansk 80 - 233, Poland.

出版信息

Food Chem. 2023 Nov 15;426:136646. doi: 10.1016/j.foodchem.2023.136646. Epub 2023 Jun 19.

Abstract

In this manuscript, a green and fast vortex-assisted hydrophobic magnetic deep eutectic solvent-based dispersive liquid phase microextraction (VA-HMDES-DLPME) method was developed for the selective extraction and determination of niclosamide in read samples, including rice, medicine tablets, and water samples. Here, hydrophobic magnetic deep eutectic solvents were used as the extracting solvent without requiring any centrifugation step. In the light of preliminary experiments, important parameters, such as volume of extraction solvent, pH, acetonitrile volume and vortex time, affecting the extraction efficiency of niclosamide were optimized using a Box-Behnken design. The linear dynamic range (0.25-120 µg/L), the limit of detection (0.08 µg/L), the limit of quantitation (0.25 µg/L), preconcentration factor (180), and enrichment factor (130) of the method were determined using optimized data. In particular, the validation parameters of the optimized VA-HMDES-DLPME, including robustness, matrix effect accuracy, and precision, were investigated. In addition to this, intra- and inter-day precisions were determined as ≤3.5 % and ≤4.1%, respectively. Finally, the optimized method was successfully used for the extraction of niclosamide in the selected samples prior to spectrophotometric analysis.

摘要

在本手稿中,开发了一种绿色且快速的涡旋辅助疏水磁性深共晶溶剂分散液相微萃取(VA-HMDES-DLPME)方法,用于选择性提取和测定实际样品中的氯硝柳胺,包括大米、药片和水样。在这里,疏水磁性深共晶溶剂被用作萃取溶剂,而无需任何离心步骤。根据初步实验,使用 Box-Behnken 设计优化了影响氯硝柳胺萃取效率的重要参数,如萃取溶剂体积、pH 值、乙腈体积和涡旋时间。使用优化后的数据确定了该方法的线性动态范围(0.25-120μg/L)、检出限(0.08μg/L)、定量限(0.25μg/L)、浓缩因子(180)和富集因子(130)。特别是,还研究了优化后的 VA-HMDES-DLPME 的验证参数,包括稳健性、基质效应准确度和精密度。此外,日内和日间精密度分别确定为≤3.5%和≤4.1%。最后,该优化方法成功用于分光光度分析前选定样品中氯硝柳胺的提取。

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