Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan, China.
J Chromatogr A. 2012 Jan 6;1219:66-74. doi: 10.1016/j.chroma.2011.11.026. Epub 2011 Nov 19.
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 (0.010-1.0 μg mL(-1) with r(2)>0.9900), low limits of detection (0.38-0.62 ng mL(-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.
在本研究中,开发了一种基于聚丙烯膜保护微固相萃取(MP-μ-SPE)的简单、灵敏的萃取方法,用于分析食品样品中的磺胺类药物。采用正交实验设计合成了聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)(p-MAA-EDMA),并采用三因素四水平优化,评价了其产率、疏水性和阳离子交换性能。优化后的 p-MAA-EDMA 用作 MP-μ-SPE 的吸附剂,从牛奶和鸡肉肌肉样品中萃取磺胺类药物,然后用高效液相色谱法分析,紫外检测。在优化的萃取条件下,得到了良好的线性关系(0.010-1.0μg mL(-1),r(2)>0.9900)、低检测限(0.38-0.62ng mL(-1))以及可接受的日内(2.7-13.7%)和日间(6.7-15.2%)相对标准偏差。该方法对于处理半固体/固体样品具有良好的效果,对“脏”样品的干扰有很好的抵抗力。