坎地沙坦酯片有关物质测定方法考察  

Determination of Related Substances in Candesartan Cilexetil Tablets

作　　者：马超[1] 苏慕君[1] 臧可昕[1] 

机构地区：[1]天津药物研究院释药技术与药代动力学国家重点实验室,300193

出　　处：《医药导报》2013年第2期208-212,共5页Herald of Medicine

基　　金：国家重点基础研究发展计划(973计划)资助项目(2012CB724002)

摘　　要：目的建立测定坎地沙坦酯片有关物质的高效液相色谱法。方法参照国家食品药品监督管理局发布的坎地沙坦酯片标准,采用Hypersil C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-乙腈-0.05 mol.L-1磷酸二氢钠(用磷酸调节pH至3.2)(55∶30∶20)为流动相,流速0.9 mL.min-1,检测波长254 nm。参照第16版《日本药局方》中坎地沙坦酯片的质量标准,采用Waters C18色谱柱(150 mm×4.6 mm,5μm),以流动相A-B[A:乙腈-水-醋酸(57∶43∶1);B:乙腈-水-醋酸(90∶10∶1)]梯度洗脱,流速0.9 mL.min-1,检测波长254 nm。结果参照国家食品药品监督管理局发布的标准建立的方法,能分离和检测坎地沙坦酯的5种有关物质,在0.25～25.00μg.mL-1范围内线性关系良好,最低检测限1 ng;参照《日本药局方》质量标准建立的方法,能分离和检测坎地沙坦酯的8种有关物质,在0.40～40.00μg.mL-1范围内线性关系良好,最低检测限0.8 ng。结论两种方法均能检测坎地沙坦酯片有关物质。参照《日本药局方》建立的方法检测灵敏度更高,专属性更强,更准确。Objective To establish high performance liquid chromatography （HPLC） methods for determination of related substances in candesartan cilexetil tablets. Methods According to the quality standard of candesartan cilexetil tablets announced by State Food and Drug Administration （SFDA）, the related substances were determined on a Hypersil C18 column （250 mm×4.6 mm, 5μm） with the mobile phase of Methanol-acetonitrile-0.05 mol·L^-1 sodium dihydrogen phosphate solution （adjusted to pH 3.2 with phosphoric acid） （55 ： 30 ： 20） at a flow rate of 0.9 mL ·min^-1, detected at 254 nm wavelength. According to the standard of candesartan cilexetil tablets established by the Japanese Pharmacopoeia 16th Edition, the related substances were determined on a Waters Cls column （150 mm×4.6 mm, 5μm） with gradient elution of mobile phase A and B [A： acetonitrile-water-acetic acid （57 ： 43 ： 1 ）, B： acetonitrile-water-acetic acid （90 ： 10 ：1 ）] at a flow rate of 0.9 mL·min^-1 , detected at 254 nm. Results Five related substances of candesartan cilexetil could be determined by the method referred to SFDA. A good linear relationship was observed in the concentration range of 0.25-25.00 μg· mL^-1 The detection limit was 1 ng. Eight related substances of candesartan cilexetil could be determined by the method referred to Japanese Pharmacopoeia. A good linear relationship was observed in the concentration range of O. 40-40.00μg ·mL^-1. The detection limit was 0.8 ng. Conclusion Both of the determination methods could be used for the determination of related substances in candesartan cilexetil tablets. The method referred to Japanese Pharmacopoeia was proved to be more sensitive, specific, and accurate.

关 键 词：坎地沙坦酯片 有关物质 色谱法 高效液相 

分 类 号：R972.6[医药卫生—药品] R927.1[医药卫生—药学]