氟苯尼考粉中非法添加四种喹诺酮类药物的HPLC检测方法研究

Study on the Determination Method of Quinolones in Florfenicol Powder by HPLC

建立了高效液相色谱法检测氟苯尼考粉中非法添加氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星的方法。用十八烷基键合硅胶色谱柱,以A(磷酸3.0 mL加水至1000 mL,三乙胺调pH值至3.0±0.1,加乙腈50 mL)-甲醇(88∶12)为流动相,采用二极管阵列检测器,采集波长为200～400nm,分辨率1.2 nm,记录光谱图和283 nm波长处的色谱图,流速1.0 mL/min,柱温30℃。结果显示,4种喹诺酮类药物的浓度在0.5～200μg/mL范围内呈良好的线性关系,添加回收率在98.5%～100.9%之间,相对标准偏差在0.14%～0.74%之间,检测限0.5 mg/g。本方法快速、准确,可用于氟苯尼考粉中非法添加喹诺酮类药物的定性和定量检测。

A method of HPLC -PDA for determination of quinolones in florfenicol powder was developed. The liquid chromatography separation was carried on C18 column, the mobile phase was mobile phase A（ diluted 3 mL phosphoric acid to 1000 mL with water, adjusted the pH value with triethylamine to 3.0±0. 1, then added acetonitrile 50 mL） -methol （88 ： 12 ）, the flow rate was 1.0 mL/min and the column worked at 30 ℃, the wavelength range was 200 -400 nm. The result showed that the standard curves for four quinolones were in good linearity within a concentration range of 0.5 - 200 μg/mL, the recoveries for quinolones in florfenicol powder ranged between 98.5% and 100.9% with the RSD from 0.14% to 0.74%. The limits of detection（LOD） was 0.5 mg/g. The method was fast and accurate, and could be used for identification and determination of the quinolones in florfenicol powder.