Department of Analytical Sciences, Faculty of Sciences, National University of Distance, 28040 Madrid, Spain.
Department of Analytical Sciences, Faculty of Sciences, National University of Distance, 28040 Madrid, Spain.
Food Chem. 2017 Apr 15;221:721-728. doi: 10.1016/j.foodchem.2016.11.114. Epub 2016 Nov 23.
A series of molecularly imprinted polymers (MIPs) comprising reactionary sites which are complementary to macrolide antibiotic spiramycin (SPI) were synthetized by noncovalent bulk polymerization technique. MIPs were synthesized under different polymerization process and their recognition efficiency was evaluated in binding studies in comparison with non-imprinted polymers. The best MIP was morphologically characterized and equilibrium assays were carried out. The MIP was evaluated as a sorbent for extraction and preconcentration of SPI from aqueous and sheep milk samples, and an off-line MISPE method followed by high-performance liquid chromatography with UV diode-array detection was established. Good linearity were obtained for SPI in a range of 24-965μgkg and the average recoveries at three spiked levels in milk samples were higher than 90% (RSD<5%). Limit of quantification was 24.1μgkg. Cross-reactivity studies from other macrolides with similar structure were tested. The optimum imprinted polymer showed a good selectivity and affinity for SPI, demonstrating the potential of the proposed MISPE for rapid, sensitive and effective sample pretreatment for selective determination of SPI in sheep milk samples.
通过非共价整体聚合技术，合成了一系列包含与大环内酯抗生素螺旋霉素（SPI）互补的反应性位点的分子印迹聚合物（MIP）。在不同的聚合工艺下合成了 MIP，并在结合研究中对其与非印迹聚合物的识别效率进行了评估。对最佳 MIP 进行了形态学表征，并进行了平衡测定。该 MIP 被评估为从水相和绵羊奶样品中提取和预浓缩 SPI 的吸附剂，并建立了离线 MISPE 方法，然后进行高效液相色谱-紫外二极管阵列检测。在 24-965μgkg 的范围内，SPI 具有良好的线性，在牛奶样品的三个加标水平下的平均回收率高于 90%（RSD<5%）。定量限为 24.1μgkg。还测试了与类似结构的其他大环内酯的交叉反应性。最佳印迹聚合物对 SPI 表现出良好的选择性和亲和力，表明所提出的 MISPE 具有用于快速、灵敏和有效地进行样品前处理，选择性测定绵羊奶样品中 SPI 的潜力。
