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超分子溶剂的制备与表征及其萃取牛奶中磺胺类抗生素的性能分析
Preparation and Characterization of Supramolecular Solvent and Its Extraction of Sulfonamide Antibiotics from Milk
【摘要】 磺胺类抗生素(SAs)作为一种廉价且有效的抗菌药物,常用于畜牧养殖中,但其残留于动物源性食品中会威胁人体健康。本研究采用三丁基辛基膦四氟硼酸盐([P4448]BF4)和四氢呋喃(THF)制备的超分子溶剂作为萃取溶剂,通过分散液液微萃取(Dispersive liquid-liquid microextraction, DLLME)方法分离富集样品中的SAs,采用高效液相色谱(HPLC)法进行分析检测。采用相图、傅里叶红外光谱(FT-IR)、扫描电镜(SEM)和荧光倒置显微镜等对超分子溶剂的组成和微观形貌进行了表征,并测定了其密度和pH值,通过单因素实验优化了萃取条件。结果表明,在最优的萃取条件下,磺胺氯哒嗪、磺胺甲噁唑、磺胺甲氧哒嗪和磺胺二甲氧嘧啶4种SAs在其各自的检测范围内均呈现良好的线性关系(R2≥0.9998),检出限(LOD, S/N=3)为0.67~1.45μg/L。与文献报道的其它方法相比,本方法具有操作简便、试剂消耗少等优点,可用于牛奶样品中SAs残留的分析检测。本研究不仅为食品安全监管提供了技术支撑,也为超分子溶剂在萃取分离领域的应用开辟了新路径。
【Abstract】 As a cheap and effective antibiotic, sulfonamides are often used in animal husbandry. However, their residues in animal-derived foodstuffs will threaten human health. Consequently, a high-performance liquid chromatography(HPLC) method integrated with supramolecular solvent microextraction was successfully established for simultaneous quantification of sulfonamide residues sulfachlorpyridazine, sulfamethoxazole,sulfamethoxypyridazine and sulfadimethoxine in milk matrices. This approach exhibited prominent characteristics of operational simplicity, environmental sustainability, and high extraction efficiency. The supramolecular solvents prepared by tributyl octylphosphine tetrafluoroborate and tetrahydrofuran were employed as extraction solvents.The analytes underwent isolation and concentration via dispersive liquid-liquid microextraction(DLLME) prior to quantitative determination using high-performance liquid chromatography(HPLC). The composition and microscopic morphology of the supramolecular solvent were characterized through a series of analytical techniques, including phase diagram, Fourier transform infrared spectroscopy, scanning electron microscopy, and inverted fluorescence microscopy and so on. The density and p H value of supramolecular solvents were determined. The extraction conditions were optimized through the one-factor experiments. The experimental results demonstrated that under the optimal extraction conditions, the four kinds of sulfonamide antibiotics exhibited excellent linearity within respective detection range(R~2≥0.9998) and the limits of detection(LOD) were0.67–1.45μg/L. Compared with literature methods, this approach offered some advantages such as simplicity of operation and less reagent consumption, and could be used for analysis and detection of sulfonamide antibiotic residues in milk samples. The present method provided technical support for food safety regulation and paved a new way for the application of supramolecular solvents in the field of extraction and separation.
【Key words】 Sulfonamide antibiotics; Dispersive liquid-liquid microextraction; Supramolecular solvents; High performance liquid chromatography; Milk;
- 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2025年06期
- 【分类号】TQ413;TS252.7;O657.72
- 【下载频次】30