HPLC-PDA法同时测定硫酸新霉素可溶性粉中非法添加4种化学药物

Simultaneous Determination of Four Kinds of Illegally Added Chemical Drugs in Neomycin Sulfate Soluble Powder by HPLC-PDA

建立了同时测定硫酸新霉素可溶性粉中非法添加甲硝唑、水杨酸、乙酰甲喹、甲氧苄啶的HPLC-PDA方法。样品用甲醇提取,经C18柱分离,以磷酸盐缓冲液-甲醇为流动相洗脱,流速为1.0 m L/min,采用二极管阵列检测器进行全波长(200~400 nm)扫描,提取波长为230 nm。检查保留时间、峰纯度和光谱相似度,对非法添加化学药物进行确证。结果表明,4种化学药物在0.01~0.12 mg/m L范围内线性关系良好(r≥0.9998);回收率在98.0%~99.9%之间,RSD≤1.0%,检出限为1~5 g/kg。该检测方法专属性强、操作简便,可用于硫酸新霉素可溶性粉中非法添加4种化学药物的测定。

To establish a method for simultaneous determination of illegally adding metronidazole, salicylic acid,mequindox and trimethoprim in neomycin sulfate soluble powder by the high performance liquid chromatographywith photo-diode array detector （HPLC-PDA）, samples were extracted by methanol. C18 column was appliedwith mobile phase consisting of sodium dihydrogen phosphate buffer-methanol （70 ∶ 30） at a flow rate of 1.0 mL/ min.The extract wavelength was 230 nm from the scanning of 200～400 nm by photo-diode array detector. Retentiontime, peak purity test and spectral similarity were helped to identify the four kinds of target analytes. The linearityin the correlation range of 0.01 ～ 0.12 mg/ mL were good（r≥0.9998）. The recoveries ranged from 98.0% to99.9% with the relative stand deviations （RSDs） all below 1.0%. The limits of detection were from 1 to 5 g/ kg. Inconclusion, the method has good specifity and simple treatment,and can be used as a reliable way for detectingdrugs adulterated in neomycin sulfate soluble powder.