鱼腥草注射液中非法添加水杨酸和氧氟沙星HPLC-PDA检测方法的建立

Determination of Salicylic Acid and Ofloxacin in Houttuynia Injection by HPLC-PDA

关键词:  水杨酸  氧氟沙星  鱼腥草注射液  峰纯度检查  光谱相似度检查  HPLC-PDA

Key words:  salicylic acid  ofloxacin  houttuynia injection  peak purity test  spectrum similar test  HPLC-PDA

摘要:

为建立鱼腥草注射液中非法添加水杨酸和氧氟沙星的测定方法，采用十八烷基键合硅胶为填充剂，磷酸二氢钠溶液（取磷酸二氢钠3.0 g，加1000 mL水使溶解，加三乙胺0.5 mL，用氢氧化钠饱和溶液调节pH值至7.0）-甲醇为流动相，梯度洗脱，流速为1.0 mL/min，二极管阵列检测器，提取波长为293 nm。采用峰纯度检查和光谱相似度检查辅助对照品比对方法，对非法添加药物进行确证。在此液相色谱条件下，水杨酸、氧氟沙星与其他物质峰分离良好。按外标法以峰面积计算，水杨酸和氧氟沙星的平均回收率分别为99.3%和98.8%，RSD分别为0.6%和0.8%。结果表明该检测方法简便、准确、可靠，可用于同时测定鱼腥草注射液中非法添加的水杨酸和氧氟沙星。

Abstract:

A method for the determination of salicylic acid and ofloxacin in houttuynia injection was developed by the high performance liquid chromatography with photo-diode array detector (HPLC-PDA). It was tested with C18 column, using gradient elution with sodium dihydrogen phosphate solution (Taking the sodium dihydrogen phosphate 3.0 g, add 1000 mL water to dissolve, and add 0.5 mL triethylamine, adjusting pH to 7.0 by sodium hydroxide saturated solution) and methanol as the mobile phase, flow rate was 1 mL per minute. The extract wavelength was 293 nm. Peak purity test and spectrum similar test were help to determine the salicylic acid and ofloxacin except the method of comparison between sample and reference. Under the conditions of liquid chromatography, the separation of salicylic acid, ofloxacin and other peaks is required. The mean recovery of salicylic acid and ofloxacin were 99.3% and 98.8%, and RSD were 0.6% and 0.8%, respectively. In conclusion, the method is simple, accurate and reliable for the determination of salicylic acid and ofloxacin in houttuynia injection.