环境友好型方法快速检测牛奶中的六种喹诺酮残留

摘要

本文建立了一种环境友好型、同时分离检测牛奶中六种喹诺酮类药物的高效液相色谱分析法。方法采用反相Chromatorex C18色谱柱，二极管阵列检测器，检测波长为280 nm。实验表明，适当浓度的柠檬酸和硫酸铵溶液作为提取液时可使牛奶中的蛋白质发生缓慢而彻底的变性，释放出与其结合的喹诺酮类药物，从而提高了从牛奶中提取喹诺酮类药物的提取效率。然后通过对提取液进行加热沉淀蛋白质、加入PSA （ N-丙基乙二胺修饰的硅胶）净化，即可实现样品的快速前处理。该方法用于牛奶中六种喹诺酮类抗生素残留的测定，回收率均在82.0％～117.8％之间，方法检出限为34.5～85.0 ng· g-1。本文提出的样品前处理方法可靠、快速、环保、易于操作。%A kind of environment friendly method for simultaneous separation and determination of six quinolones in milk by high performance liquid chromatography was established in this paper.The quinolones were separated on a reversed-phase Chromatorex C18 column and detected by diode array detector with the wavelength of 280 nm.Experiment showed that protein denaturation was slow but full in the mixture solution of citric acid and ammonium sulfate with suitable concentrations.Meanwhile the quinolones combined with protein might be dissociated , which would result in a high efficiency on extraction of quinolones from milk sam-ple.Then the protein was precipitated quickly from the extracting solution by heating ,and the extracting solution was purified with PSA( primary secondary amine modified silica gel ) subsequently to complete the sample preparation procedure.This method has been applied to the determination of six quinolones in bovine milk samples.The spiked recoveries were all in the range of 82.0%~117.8%,and the limits of detection were in the range of 34.5~85.0 ng· g-1 .The pre-treatment method proposed in this paper was reliable,rapid and environment friendly .