RP-HPLC-UV波长切换法测定复方阿司匹林牛磺酸胶囊中咖啡因、阿司匹林及有关物质水杨酸的含量

目的: 建立同时测定复方阿司匹林牛磺酸胶囊中咖啡因、阿司匹林和有关物质游离水杨酸含量的方法。方法: 以十八烷基键合硅胶为填充剂(Apollo-C₁₈),甲醇-4%醋酸溶液(40:60)为流动相,柱温和流速分别为室温和1 mL·min^-1,波长切换,0~10 min在275 nm波长下测定咖啡因和阿司匹林含量,10~18 min在303 nm波长下测定有关物质游离水杨酸含量。结果: 咖啡因、阿司匹林和水杨酸能实现完全分离,并与其他成分均能达到良好的分离;阿司匹林、咖啡因、水杨酸分别在0.53~5.28 μg,49.54~495.36 ng和2.04~24.48 ng的浓度范围内,与色谱峰峰面积呈良好线性响应;咖啡因、阿司匹林和水杨酸的回收率分别为99.3%,100.1%,100.3%(n=9)。结论: 建立的RP-HPLC-UV波长切换法操作简便、专属性高、重复性好,能准确、快速地测定咖啡因和阿司匹林含量,同时也适用于游离水杨酸检查。

Objective: To establish a RP-HPLC-UV wavelength switching method for the determination of aspirin,cafein and related substance salicylic acid in compound aspirin and taurine capsules.Methods: RP-HPLC wavelength switching method was adopted.Aspirin,cafein and salicylic acid were separated and determined on a Apollo-ODS2(250 mm×4.6 mm,5 μm)column with a mobile phase of methol-4% glacia acetic acid solution(40:60)and a flow rate of 1.0 mL·min^-1 at room temperature.The detection wavelength was set at 275 nm in first 10 min for cafein and asprin determination,and then changed to 303 nm for related substance salicylic acid determination between 10-18 min.Results: Under the established chromatographic conditions,the linear ranges of aspirin,cafein and related substance salicylic acid were 0.53-5.28 μg,49.54-495.36 ng and 2.04-24.48 ng with a correlation coefficient of 0.9999.Their recoveries were 99.3%,100.1% and 100.3%(n=9).Conclusions: RP-HPLC-UV wavelength switching method is simple and accurate for the determination of aspirin,cafein and related substance salicylic acid in compound aspirin and taurine capsules.