RP-HPLC 测定盐酸地芬尼多片的含量与有关物质

 摘要：目的 建立高效液相色谱法测定盐酸地芬尼多片的含量与有关物质的方法。方法 采用VP-ODS C18色谱柱 （4.6 mm×250 mm，5 μm），以0.5%三乙胺溶液（用磷酸调节pH值至4.0）-甲醇（44∶56）为流动相；流速为0.8 mL·min-1；检测波长为210 nm，柱温：30 ℃。结果 盐酸地芬尼多与有关物质及各降解成分完全分离；盐酸地芬尼多浓度在3.158~63.15 mg·L-1内与峰面积呈良好线性关系，r=1.000 0(n=7)；最低检出限为1 ng，最低定量限为3 ng；低、中、高3种浓度的回收率(n=3)分别为100.4%(RSD=0.4%)，99.5%(RSD=0.8%)，99.8%(RSD=0.4%)。结论 该方法操作简便、快速、准确，灵敏度高，可用于盐酸地芬尼多片含量及有关物质的测定。

Determination of Content and Related Substances in Difenidol Hydrochloride Tablets by RP-HPLC

ABSTRACTOBJECTIVE To establish a HPLC method for the determination of content and related substances in difenidol hydrochloride tablets. METHODS The separation was performed on a VP-ODS C18 column (4.6 mm×250 mm, 5 μm). The mobile phase consisted of 0.5% triethylamine solution (adjusted to pH 4.0 with phosphoric acid )- methanol (44∶56) and the flow rate was 0.8 mL·min-1. The detection wavelength was 210 nm and the column temperature was 30 ℃. RESULTS Related substances and degraded substances were completely separated from difenidol hydrochloride . The linear range of determination was 3.158～63.15 mg·L-1 with the correlation coefficient of 1.000 0 (n=7), and the LOD was 1 ng. LOQ was 3 ng. The average recoveries (n=3) of low, middle and high concentration were 100.4% (RSD=0.4%), 99.5% (RSD=0.8%) and 99.8% (RSD=0.4%). CONCLUSION The method is simple, rapid, accurate, sensitive and it is suitable for the determination of the content and related substances in difenidol hydrochloride tablets.