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蜂蜜样品中磺胺类药物的环保测定方法:基于疏水性天然深共熔溶剂的微萃取-高效液相色谱法及基质匹配校准技术

Environmentally friendly determination of sulfonamides in honey samples: Hydrophobic natural deep eutectic solvent-based microextraction prior to high-performance liquid chromatography by matrix matching calibration techniques.

作者信息

Erim Ümit Can

机构信息

Istanbul Medipol University, School of Pharmacy, Department of Analytical Chemistry, 34810 Istanbul, Turkey.

出版信息

Food Chem. 2025 Oct 15;489:144996. doi: 10.1016/j.foodchem.2025.144996. Epub 2025 Jun 1.

Abstract

Hydrophobic natural deep eutectic solvent-based microextraction (H-NADES-ME) combined with high-performance liquid chromatography UV-visible (HPLC-UV) was developed to determine two common sulfonamides; sulfadiazine (SDZ) and sulfamethoxazole (SMX). The analytes were pre-concentrated using DES to ensure eco-friendly extraction. H-NADES and HPLC-UV parameters were optimized, and robustness tests were performed. For SDZ and SMX, the detection limits were 13.7 ng/mL and 3.5 ng/mL; RSD% values were 1.5 and 9.1 and the linear dynamic ranges were 40-5000 ng/mL and 30-5000 ng/mL, respectively. Intraday and interday precision values (RSD%) were below 10 % for both analytes. Matrix-matched calibration was employed to ensure an accurate quantification in two different honey types from Artvin and Kırklareli, yielding recoveries between 90.1 % and 113.9 %. To assess the method's sustainability, greenness evaluation tools AGREE, ComplexMoGAPI, and BAGI were used. Overall, the proposed H-NADES-ME-HPLC-UV strategy offers a selective, reproducible, and sustainable alternative to routine sulfonamide analysis in food safety applications.

摘要

开发了基于疏水型天然深共熔溶剂的微萃取(H-NADES-ME)结合高效液相色谱紫外可见检测法(HPLC-UV)来测定两种常见的磺胺类药物:磺胺嘧啶(SDZ)和磺胺甲恶唑(SMX)。使用深共熔溶剂对分析物进行预浓缩,以确保萃取过程环保。对H-NADES和HPLC-UV参数进行了优化,并进行了稳健性测试。对于SDZ和SMX,检测限分别为13.7 ng/mL和3.5 ng/mL;相对标准偏差(RSD%)值分别为1.5和9.1,线性动态范围分别为40 - 5000 ng/mL和30 - 5000 ng/mL。两种分析物的日内和日间精密度值(RSD%)均低于10%。采用基质匹配校准以确保对来自阿尔特温省和克尔克拉雷利省的两种不同蜂蜜类型进行准确定量,回收率在90.1%至113.9%之间。为评估该方法的可持续性,使用了绿色度评估工具AGREE、ComplexMoGAPI和BAGI。总体而言,所提出的H-NADES-ME-HPLC-UV策略为食品安全应用中常规磺胺类药物分析提供了一种选择性、可重现且可持续的替代方法。

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