Chemistry Department, Yasouj University, Yasouj, 75918-74831, Iran.
Chemistry Department, Yasouj University, Yasouj, 75918-74831, Iran.
J Chromatogr A. 2019 Jun 7;1594:13-22. doi: 10.1016/j.chroma.2019.02.015. Epub 2019 Feb 7.
This paper reports a new variant of sample clean-up procedure based on miniaturized matrix solid phase dispersion (MSPD) combining with water compatible magnetic molecularly imprinted polymers (MMIP) for preconcentration of melamine from milk samples prior high-performance liquid chromatography with UV detection. By employing MMIP as dispersant sorbent matrix interferences could be eliminated completely and the column packing step was interestingly omitted that decreasing in glassware expenditure, labor effort and extraction time which cause improvement of the method performance. In order to investigate the functionality, morphology and magnetic properties of the prepared MMIP, it was fully characterized by FT-IR, VSM, SEM, and TEM. Multivariate optimization was applied as a versatile statistical approach for evaluating the influence of the main variables and their interactions on extraction efficiency. Under optimized conditions, the proposed method exhibited a wide linear response in the concentration range of 250.0-5000.0 μg L, satisfactory recoveries for all samples (86.6% ≤), and supreme repeatability (RSD less than 6.3%) were achieved as well. The low limit of detection close to 67.0 μg L implied high ability of proposed method for isolation of melamine from complicate milk sample. These befitting results demonstrated that the developed method is unique in terms of the facility, rapidly and least solvent consumption as well as accurate analysis of melamine at trace levels.
本文报道了一种基于微型基质固相分散（MSPD）的新型样品净化方法，结合水相溶性磁性分子印迹聚合物（MMIP），用于在高效液相色谱-紫外检测之前从牛奶样品中预浓缩三聚氰胺。通过使用 MMIP 作为分散剂吸附剂基质，可以完全消除干扰，并且有趣的是省略了柱填充步骤，从而减少了玻璃器皿的支出、劳动力和提取时间，提高了方法的性能。为了研究制备的 MMIP 的功能、形态和磁性特性，对其进行了全面的傅里叶变换红外光谱（FT-IR）、振动样品磁强计（VSM）、扫描电子显微镜（SEM）和透射电子显微镜（TEM）的表征。多元优化被用作一种通用的统计方法，用于评估主要变量及其相互作用对萃取效率的影响。在优化条件下，该方法在 250.0-5000.0 μg L 的浓度范围内表现出宽的线性响应，对所有样品的回收率均令人满意（86.6%≤），并且具有极好的重复性（RSD 小于 6.3%）。接近 67.0 μg L 的低检测限表明，该方法具有从复杂牛奶样品中分离三聚氰胺的高能力。这些合适的结果表明，与传统方法相比，该方法具有操作简便、快速、溶剂消耗少、痕量分析三聚氰胺准确等优点。
