关键词: Antibiotic Extraction method Food sample Natural adsorbent Sample preconcentration

Mesh : Animals Tetracyclines / analysis Chromatography, High Pressure Liquid / methods Ocimum basilicum Tetracycline / analysis Milk / chemistry Anti-Bacterial Agents / analysis Solid Phase Extraction / methods

来  源:   DOI:10.1016/j.talanta.2024.125645

Abstract:
Unmodified hairy basil seed mucilage (Ocimum basilicum L.), with attractive features as structural functionality and adsorption capacity, was employed as a green biosorbent for dispersive solid phase extraction and enrichment of oxytetracycline, tetracycline, and doxycycline before quantitation by HPLC-UV for the first time. Hairy basil crushed seed increased the contacting surface area and was completely dispersed in the sample solution to extract tetracyclines under acidic condition with the assistance of ultrasonic waves. The analytes in the extraction phase were separated on a C18 column under isocratic condition with a mobile phase consisted of acetonitrile and trifluoroacetic acid. Influence of chemical and physical variables on the extraction efficiency of the developed method was investigated and optimized systematically. Under the optimal condition of all experimental parameters, good linear ranges were obtained at 15.0-500 μg L-1 for tetracyclines with determination coefficients more than 0.9994. Limits of detection (LODs) and limits of quantitation (LOQs) ranged 5.0-7.0 and 15.0 μg L-1, respectively. Relative standard deviations (RSDs) of the proposed method at 100 and 300 μg L-1 for TCs were less than 13 % and 10 %, respectively with percentage TC recoveries from spiked standard ranging 83.1-109.9 %. This simple, reliable, cost-effective, and environmentally friendly method was successfully applied for the analysis of tetracycline residues in milk. The greenness of the proposed method was assessed using the Analytical Eco-Scale and AGREE protocol.
摘要:
未修饰的毛状罗勒种子粘液(OcimumbasilicumL.),具有结构功能和吸附能力等有吸引力的特征,被用作分散固相萃取和富集土霉素的绿色生物吸附剂,四环素,和多西环素,然后通过HPLC-UV首次定量。毛状罗勒压碎的种子增加了接触表面积,并在超声波辅助下在酸性条件下完全分散在样品溶液中提取四环素。萃取相中的分析物在等度条件下在C18柱上分离,流动相由乙腈和三氟乙酸组成。研究了化学和物理变量对所开发方法提取效率的影响并进行了系统优化。在所有实验参数的最佳条件下,四环素在15.0-500μgL-1时获得了良好的线性范围,测定系数大于0.9994。检测限(LODs)和定量限(LOQs)分别为5.0-7.0和15.0μgL-1。提出的方法在100和300μgL-1时对TC的相对标准偏差(RSD)小于13%和10%,来自加标标准的TC回收率分别为83.1-109.9%。这个简单的,可靠,成本效益高,该方法成功应用于牛奶中四环素残留的分析。使用分析生态尺度和AGREE协议评估了所提出方法的绿色性。
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