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

关键词:  氟苯尼考粉  喹诺酮类药物  高效液相色谱法

Key words:  florfenicol Powder  quinolones  HPLC

摘要:

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,以流动相A(磷酸3.0mL加水至1000mL,用三乙胺调pH值至3.0?0.1,加乙腈50mL)-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,分辨率为1.2nm,记录光谱图和283nm波长处的色谱图,流速1.0mL/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0.5mg/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。

Abstract:

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 3ml Phosphoric acid to 1000ml with water, adjusted the pH value with triethylamine to 3.0?0.1,then added acetonitrile 50ml)-methol(88:12),the flow rate was 1.0mL/min and the column worked at 30℃,the wavelength range was 200~400nm.The result show that the standard cures for ribavirin were in good linearity within a concentration range of 0.5~200μg/mL, the recoveries for quinolones in florfenicol Powder ranged between 98% and 100.5% with the RSD from 0.1% to 0.8%.The limits of detection(LOD) was 0.5mg/g. The method was fast and accurately, and could be used for identification and determination the quinolones in florfenicol Powder.