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

摘要:

建立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 mL/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/mL的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。

Abstract:

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 chromatography with photo-diode array detector (HPLC-PDA). Samples were extracted by methanol. C18 column was applied with 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 200-400 nm by photo-diode array detector. Retention time, peak purity test and spectral similarity were helped to identify the four kinds of target analytes. The linearity in the correlation range of 0.01～0.12 mg/mL were good(r≥0.9998). The recoveries ranged from 98.0% to 99.9% with the relative stand deviations (RSDs) all below 1.0%. The limits of detection were 1 to 5 g/kg. In conclusion, the method has good specifity and simple treatment，and can be used as a provides a reliable way for detecting drugs adulterated in neomycin sulfate soluble powder.