自组装成环荧光显微成像技术在抗生素残留量检测中的应用

提出了一种基于溶剂毛细流效应的微波加热自组装成环荧光显微成像技术，并应用于内蒙古乳都乳中抗生素残留量检测。在六氢吡啶反应介质和聚乙烯醇-124(PVA-124) 存在下，将米诺环素液滴滴在疏水性玻璃表面上，当液滴受热挥发时，形成直径约为1.54 mm，环带宽为 22.6 μm的自组装环。当点样体积为0.30 μL时，线性范围为4.2×10-12～1.8×10-11 mol·ring-1(1.4×10-6～0.60×10-5 mol·L-1)，方法的检测限(3σ)为4.2×10-13 mol·ring-1(1.4×10-7 mol·L-1)。应用于内蒙古乳都乳中残留米诺环素和米诺环素胶囊中米诺环素含量的检测，回收率分别为97.2%～103%和99.4%～102%，相对标准偏差(RSD)小于1.2%。该方法建立了高灵敏、高选择性的痕量药物污染物分析新方法，为内蒙古地方优势资源产品——乳品中抗生素类药物残留量的定量检测提供理论依据，同时对不同地区乳品中抗生素的来源、残留情况的系统动态研究及对乳品行业的管理、监督等具有重要的现实意义和更广泛的应用前景。

Application of Fluorescence Microscopic Imaging Technique with Self-Ordered Ring to Residues Detection of Antibiotics

Fluorescence microscopic self-ordered ring (SOR) technique with microwave heating is proposed for minocycline based on the capillary flow of solvent on the surface of hydrophobic glass slide and applied to residues detection of the antibiotics in milks of Inner Mongolia. In the reaction medium of hexahydropyridine containing polyvinyl alcohol-124 (PVA-124), a SOR of minocycline with the outer diameter of 1.54 mm and the ring belt width of 22.6 μm can be formed. When a 0.30 μL droplet of minocycline mixture was spotted on the solid surface, minocycline in the range of 4.2×10-12-1.8×10-11 mol·ring-1 (1.4×10-6-0.60×10-5 mol·L-1) can be detected, the maximum fluorescence intensity was found to be proportional to the minocycline concentration, and the limit of detection can reach 4.2×10-13 mol·ring-1 (1.4×10-7 mol·L-1) with three times of signal to noise ratio. With the present method, the contents of minocycline in milk samples of Inner Mongolia and minocycline hydrochloride capsule sample were satisfactorily determined with recoveries of 97.2%-103% and 99.4%-102%, respectively, and RSD lower than 1.2%, correspondingly. Therefore, a highly sensitive and selective analysis method for detecting content of trace drug contaminations was established. The method provided theory basis to quantificational analysis of the residues of the antibiotics in milks which was Inner Mongolia’ preponderant resource products. It has important realistic meaning and broad application prospect