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表面活性剂改性二氧化硅在环境水样和蜂蜜样品中磺胺类残留的提取和预浓缩中的绿色应用。

Green application of surfactant modified silica as effective sorbent for extraction and preconcentration of sulfonamide residues in environmental water and honey samples.

机构信息

Creative Chemistry and Innovation Research Unit, Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahasarakham University, Maha Sarakham 44150, Thailand.

Creative Chemistry and Innovation Research Unit, Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahasarakham University, Maha Sarakham 44150, Thailand; Multidisciplinary Research Unit of Pure and Applied Chemistry (MRUPAC), Department of Chemistry and Center of Excellent for Innovation in Chemistry, Faculty of Science, Mahasarakham University, Maha Sarakham 44150, Thailand.

出版信息

J Chromatogr A. 2024 Mar 15;1718:464720. doi: 10.1016/j.chroma.2024.464720. Epub 2024 Feb 6.

Abstract

Micro-solid phase extraction (µ-SPE) using surfactant coated silica for extraction and preconcentration of sulfonamide residues at trace levels in environmental water and honey samples prior their analysis by high performance liquid chronatography coupled with photodiode array detector (HPLC-PDA). The sample solution were dispersed in a small amounts of solid sorbent by vacuum manifold for sample preparation, and extraction occurred by adsorption in a short time. Finally, the analytes were subsequently desorbed using an appropriate solvent. The pure and coated silica were physicochemically and morphologically characterized by nittrogen (N) sorptions analyses, and transmission electron microscopy (TEM). Parameters influencing extraction efficiency, such as amount of sorbent, kind, concentration and volume of surfactant, and kind and volume of desorption solvent, were investigated. The optimum conditions of the proposed method, were mixed standard/sample solution (10 mL), 0.4 g silica, 0.03 M CTAB (150 µL), and 500 μL methanol (as elution solvent). The proposed method, under optimal conditions, showed excellent linearity in different ranges (9-300 μg L, the a coefficient of determination (R) of greater than 0.99), good repeatability (RSD < 6.72 %), good sensitivity (LODs in the range of 1 to 3 µg L), high enrichment factor (5.63-13.33), and acceptable relative recoveries (61.0-121.4 %). The developed µ-SPE method was applied to analyze sulfonamide residues in water and honey samples with relative recoveries of 60.9-119.4 % were obtained. This alternative method is simple and is also environmentally friendly which assessed using Analytical Eco-scale and Analytical GREEnness metric (AGREE).

摘要

采用表面活性剂修饰的硅胶固相微萃取(µ-SPE),结合高效液相色谱-光电二极管阵列检测(HPLC-PDA),用于痕量环境水样和蜂蜜样品中磺胺类残留的提取和预浓缩。在进行分析之前,将样品溶液分散在少量固体吸附剂中,通过真空多管阀进行样品制备,然后在短时间内通过吸附进行萃取。最后,使用适当的溶剂将分析物洗脱。通过氮(N)吸附分析和透射电子显微镜(TEM)对纯硅胶和修饰硅胶进行了物理化学和形态学表征。考察了影响萃取效率的参数,如吸附剂的用量、种类、表面活性剂的浓度和体积,以及洗脱溶剂的种类和体积。在所提出方法的最佳条件下,混合标准/样品溶液(10 mL)、0.4 g 硅胶、0.03 M CTAB(150 µL)和 500 µL 甲醇(作为洗脱溶剂)。在所提出的方法的最佳条件下,在不同范围内(9-300 µg L)显示出极好的线性,相关系数(R)大于 0.99,具有良好的重复性(RSD < 6.72 %),良好的灵敏度(LOD 范围为 1-3 µg L),高富集因子(5.63-13.33)和可接受的相对回收率(61.0-121.4 %)。该开发的µ-SPE 方法用于分析水样和蜂蜜样品中的磺胺类残留,相对回收率为 60.9-119.4 %。这种替代方法简单,对环境友好,通过分析生态规模和分析绿色度指标(AGREE)进行了评估。

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