盐酸法舒地尔中杂质和二聚体HPLC法测定.PDF

• 538 • 现代药物与临床 Drugs Clinic 第 28 卷 第 4 期 2013 年 7 月 盐酸法舒地尔中杂质和二聚体的 HPLC 法测定 * 郝全文，孙国祥 ，殷瑞娟，豆小文 沈阳药科大学 药学院，辽宁 沈阳 110016 摘 要：目的 采用高效液相色谱法建立盐酸法舒地尔中杂质检查和二聚体的测定。方法 用Venusil XBP C18 柱（250 mm ×4.6 mm ，5 μm ），甲醇–水（50 ∶50，含 10 mmol/L 庚烷磺酸钠和 5 mmol/L 磷酸二氢钠，用磷酸调 pH 3.0 ）为流动相；紫外检 测波长为 275 nm ；进样量 10 μL ；体积流量 1.0 mL/min。采用自身对照法测定杂质，标准曲线法测定二聚体。结果 盐酸法 舒地尔中 4 个单一杂质量的均值不大于 1.34%，之和的均值不大于 1.38%。盐酸法舒地尔二聚体在 0.63～41.60 μg/mL 线性 关系良好，r ＝0.999 9 ；平均回收率为99.5%，RSD 值为 1.3%。结论 本方法简便、准确、专属性强，可作为盐酸法舒地尔 中杂质检查及二聚体的测定方法。 关键词：盐酸法舒地尔；杂质；二聚体；高效液相色谱 中图分类号：R927.1 文献标志码：A 文章编号：1674 - 5515(2013)004 - 0538 - 04 DOI: 10.7501/j.issn.1674-5515.2013.04.017 Determination of impurities and dimers in fasudil hydrochloride by HPLC HAO Quan-wen, SUN Guo-xiang, YIN Rui-juan, DOU Xiao-wen School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China Abstract: Objective To develop an RP-HPLC method for determination of the impurities and dimers in fasudil hydrochloride. Methods Venusil XBP C column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase was composed of methanol-H O (50 ∶50, 18 2 including 10 mmol/L sodium heptane-1-sulphonate and 5 mmol/L sodium dihydrogen phosphate, pH 3.0). The flow rate was 1.0 mL/min, and the determination wavelength was set at 275 nm with the injection volume of 10 μL. The total impurities were determined by the principal self contrast method, at the same time the dimmer contents in the sample were determined by standard curve method. Results Each and total contents of four impurities in fasudil hydrochloride were below 1.34% and 1.38%. A linearity between peak areas and dimer content was achieved in the range of 0.63—41.60 μg/mL(r = 0. 999 9), and the average recov