2.7 重复性试验.pdfVIP

RP-HPLC 测定盐酸地芬尼多原料的有关物质 曹凤习，姜建国，刘红莉 (河北省药品检验所，石家庄 050011) 摘要：目的 建立高效液相色谱法测定盐酸地芬尼多原料有关物质的方法。方法 采用 VP-ODS C18 色谱柱(250 mm ×4.6 mm ，5 µm) ，以0.5%三乙胺溶液(用磷酸调 pH 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，重复性及稳定性良好。最低检出限为 1 ng。结论 该 方法操作简便、专属性强、灵敏度高、结果准确，可用于盐酸地芬尼多原料有关物质的检查。 关键词：高效液相色谱法；盐酸地芬尼多原料；有关物质 中图分类号：R927.1; R917.101 文献标志码：B 文章编号：1007-7693(2009)08-0661-04 作者简介：曹凤习，女，副主任技师 Tel ：(03118038 E-mail ：caofengxi2008@163.com 中国现代应用药学杂志2009 年 8 月第 26 卷第 8 期 Chin JMAP, 2009 August, Vol.26 No.8 ·661 · Determination of the Related Substances of Difenidol Hydrochloride by RP-HPLC CAO Fengxi, JIANG Jianguo, LIU Hongli (Hebei Province Institute for Drug Control, Shijiazhuang 050011,China) ABSTRACT: OBJECTIVE To establish an HPLC method for determination of related substances of difenidol hydrochloride. METHODS VP-ODS C18 column (250 mm ×4.6 mm, 5 µm) was adopted. 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 method was good repeatability and stability. The LOD was 1 ng. CONCLUSION The method was selective, sensitive, accurate, and it is suitable for determination of related substances in difenidol hydrochloride. KEY WORDS: HPLC; difenidol hydrochloride; related substances 盐酸地芬尼多(difenidol hydrochloride)是临床 上常用的抗晕止吐药，用于治疗高血压、美尼尔氏 综合征等引起的眩晕症，口服吸收迅速，疗效确切。 其质量标准收录在中国药典 2005 年版二部[1]，但 质量标准中未收载有关物质的检查方法，为使该药 品的质量标准更加科学、有效，笔者参考文献[2] 图 1 盐酸地芬尼多有关物质测定色谱图 对盐酸地芬尼多原料的有关物质检查方法进行了