应用固载表面毛细流自组装环荧光显微成像技术,建立了Ca2+增敏米诺环素荧光体系测定牛奶中米诺环残留量的分析方法.将米诺环素溶液与一定量的氯化钙溶液,pH 8.50的氨性缓冲溶液及PVA-124溶液充分混合均匀.反应10 min后,滴在疏水性载玻片表面上,微波加热,溶剂受热挥发后,形成直径约为1.7 mm,环带宽约为45.3 μm的自组装环.当点样体积为0.3 μL时,线性范围为5.6×10-13~1.8×10-11mol,方法的检出限(3σ)为5.6×10-14mol.应用于米诺环素胶囊中米诺环素和牛奶中残留米诺环素的检测,回收率分别为104.3%~105.0%和96.0%~105.9%,相对标准偏差(n=5)小于3.5%.

By applying the fluorescence microscopic imagery and using the Ca2+-ion sensitized minocycline fluorescence reaction system,a method for determination of residual amount of minocycline in milk was proposed.The fluorescence reaction mixture was prepared by mixing the minocycline solution with definite amounts of CaCl2 solution,pH 8.50 ammoniacal buffer solution and PVA-124 solution.After reacting for 10 min,a drop of the mixed solution was dropped onto the hydrophobic glass slide,and after volatilization of the solvent by microwave heating,a capillary fluent self-ordered ring with its diameter of 1.7 mm and ring belt width of 45.3 μm was formed.When the volume of sample droplet taken was 0.3 μL,the linearity range of minocycline found was between 5.6×10-13-1.8×10-11mol,and the detection limit (3σ) found was 5.6×10-14mol.The proposed method was applied to the determination of minocycline in minocycline capsules and of residual amounts of minocycline in milk,giving values of recovery in the ranges of 104.3%-105.0% and 96.0%-105.9% with RSD′s (n=5) less than 3.5%.