HPLC测定厄贝沙坦片有关物质及其稳定性考察.doc

此论文已发表于《食品与药品》2015年第4期 HPLC测定厄贝沙坦片有关物质梁艳芬，许，黎，李( （广东药学院 药科学院，广东 广州 510006） 摘 要：目的 建立HPLC测定厄贝沙坦片有关物质含量的。方法 采用Agilent ，10 μm，-0.025 mol/L KH2PO4 溶液（35:65用三乙胺调pH至6.0）为流动相，流速1.0 mLmin，柱温30 ℃，检测波长220 nm用外标法有关物质A的含量，以峰面积归一化法其他杂质的含量。结果 主成分与有关物质A的分离度大于2.0，有关物质A的质量浓度与峰面积在0.1~0.6 μgmL范围内线性良好r=0.9981）；平均回收率98.9 %（n=9）。结论 方法简便、快速、准确可靠，适用于厄贝沙坦有关物质检查。 关键字：厄贝沙坦；有关物质；含量测定；高效液相色谱法列出中图分类号：文献标识码：A 文章编号：1672-979X（2015）00-0000-00 Determination of Irbesartan Related Substances by HPLC LIANG Yan-fen, XU Xx-xxxx, LI Xxxx-xxxx, LI Xxxx (School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006, China) Abstract: Objective To establish a high performance liquid chromatography method for the determination of related substance of irbesartan. Methods The Agilent Pursuit C18 (4.6 mm×250 mm, 10 μm) was adopted. The mobile phase consisted of acetonitrile-0.025 mol/L of potassium dihydrogen phosphate buffer (65:35, the pH was adjusted to 6.0 with triethylamine), with the flow rate of 1 mL/min; the detection wavelength was 220 nm and the column temperature was 30 ℃. The content of related substance A was calculated by external standard method; other related substances were calculated by peak area normalization method. Results Irbesartan could be completely separated with related substance A under this chromatographic condition. A good linear correlation was observed within the range of 0.1-0.6 μg/mL (r=0.9981) for irbesartan related substance A. The average recovery (n=9) was 98.9 %, with RSD of 2.1 %. Conclusion The method was simple, efficient and accurate for the analysis of the related substances of irbesartan. Key Words: irbesartan; related substance; determination; HPLC 厄贝沙坦irbesartan）是一种长效的血管紧张素ⅡAngⅡ）受体拮抗剂，能抑制AngⅠ转化为AngⅡ，特异性地拮抗血管紧张素Ⅱ受体AT1）[1]，通过选择性地阻断AngⅡ与AT1受体的结合，抑制血管收缩和醛固酮的释放，产生降压作用[2-3]，临床上主要用于高血压的治疗，具有口服有效，降压作用持久，药物不良反应小等特点[4]。目前，国家试行标准[5]和美国药典等[67]采用峰面积归一化法计算杂质含量。另有文献报道[8-10]采用主成分自身稀释对照法，误差均较外标法大。此外，经预试验发现已有标准的色谱条件下，磷酸盐易堵塞色谱柱导致拖尾峰及保留时间重现性差。因此，参考厄贝沙坦含量测定的报道[8-10]，优化色谱