College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China.
J Chromatogr A. 2012 Mar 2;1227:48-53. doi: 10.1016/j.chroma.2011.12.108. Epub 2012 Jan 11.
A novel molecularly imprinted organic-inorganic hybrid composite material (MIP-HCM) was developed based on molecular imprinting technique in combination with hybrid composite synthesis and sol-gel technology for selective solid-phase extraction (SPE) of tetracyclines residues in milk. The MIP-HCM was prepared using oxytetracycline as the template, methacrylic acid as organic functional monomer, tetraethoxysilane as inorganic precursor and methacryloxypropyltrimethoxysilane as the coupling agent. Synthesis conditions are optimized by changing some factors to obtain sorbent with the controllable adsorption capacity, selectivity, hardness and toughness. Binding study demonstrated that the imprinted hybrid composites showed excellent affinity and high selectivity to oxytetracycline. An enrichment factor of 18.8 along with a good sample clean-up was obtained under the optimized SPE conditions. The average recoveries of three tetracyclines antibiotics spiked milk at 0.1, 0.2 and 0.5 mg kg⁻¹ were in the range of 80.9-104.3% with the precision of 1.5-5.0%. The limits of detection and quantitation of the proposed method were in a range of 4.8-12.7 μg kg⁻¹ and 16.0-42.3 μg kg⁻¹, respectively.
基于分子印迹技术，结合杂化复合材料合成和溶胶-凝胶技术，开发了一种新型的分子印迹有机-无机杂化复合材料（MIP-HCM），用于选择性固相萃取牛奶中的四环素残留。MIP-HCM 以土霉素为模板，甲基丙烯酸为有机功能单体，四乙氧基硅烷为无机前体，甲基丙烯酰氧基丙基三甲氧基硅烷为偶联剂合成。通过改变一些因素优化合成条件，获得了具有可控吸附容量、选择性、硬度和韧性的吸附剂。结合研究表明，印迹杂化复合材料对土霉素具有优异的亲和力和高选择性。在优化的 SPE 条件下，可获得 18.8 的富集因子和良好的样品净化效果。在 0.1、0.2 和 0.5 mg kg⁻¹ 三个四环素抗生素添加牛奶中的平均回收率在 80.9-104.3%之间，精密度为 1.5-5.0%。该方法的检出限和定量限分别在 4.8-12.7 μg kg⁻¹ 和 16.0-42.3 μg kg⁻¹ 范围内。
