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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of sulfonamides in food samples by membrane-protected micro-solid phase extraction coupled with high performance liquid chromatography
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Determination of sulfonamides in food samples by membrane-protected micro-solid phase extraction coupled with high performance liquid chromatography

机译:膜保护微固相萃取-高效液相色谱法测定食品中的磺胺类药物

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摘要

In the present study, a simple and sensitive extraction method based on polypropylene membrane-protected micro-solid phase extraction (MP-μ-SPE) has been developed for analysis of sulfonamides in food samples. Poly (methacrylic acid-ethylene glycol dimethacrylate) (p-MAA-EDMA) was synthesized using orthogonal array experimental design, optimized with three factors at four levels and evaluated on yield, hydrophobic and cation-exchange properties. The optimized p-MAA-EDMA was then employed as the sorbent in the MP-μ-SPE for extraction of sulfonamides from milk and chicken muscle samples, followed by high performance liquid chromatographic analysis with ultraviolet detection. Under optimized extraction conditions, good linearities (0.010-1.0μgmL~(-1) with r~2>0.9900), low limits of detection (0.38-0.62ngmL~(-1)), and acceptable intra-day (2.7-13.7%) and inter-day (6.7-15.2%) relative standard deviations were obtained. It was demonstrated to be an effective approach to handle semi-solid/solid samples with good resistance to interference from " dirty" samples.
机译:在本研究中,已经开发了一种基于聚丙烯膜保护的微固相萃取(MP-μ-SPE)的简单而灵敏的萃取方法,用于分析食品样品中的磺酰胺。使用正交阵列实验设计合成了聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)(p-MAA-EDMA),并在三个水平上对三个因素进行了优化,并对收率,疏水性和阳离子交换性能进行了评估。然后将优化的p-MAA-EDMA用作MP-μ-SPE中的吸附剂,以从牛奶和鸡肌肉样品中提取磺酰胺,然后进行高效液相色谱分析和紫外检测。在优化的提取条件下,线性良好(0.010-1.0μgmL〜(-1),r〜2> 0.9900),低检测限(0.38-0.62ngmL〜(-1))和日内可接受的(2.7-13.7) %)和日间(6.7-15.2%)相对标准偏差。它被证明是一种处理半固体/固体样品的有效方法,具有良好的抗“脏”样品干扰的能力。

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