摘要
目的:建立高效液相色谱法测定盐酸西那卡塞原料药的有关物质。方法:采用Venusil XBP-C_(18)色谱柱(4.6 mm×150 mm,5μm),以含0.5%三乙胺的30 mmol·L^(-1)磷酸二氢钾水溶液(磷酸调pH 2.5)-甲醇-乙腈-异丙醇(60∶15∶15∶10)为流动相等度洗脱,流速为1.3 mL·min^(-1),柱温为35℃,检测波长为220nm。结果:盐酸西那卡塞与各杂质峰之间的分离度良好,10个已知杂质在各自的线性范围内线性关系良好(r^2>0.999,n=6);3批盐酸西那卡塞样品测定结果显示,已知杂质及最大未知单杂均小于0.1%,杂质总含量小于0.5%。结论:经方法学验证,本法灵敏度高,专属性好,可用于盐酸西那卡塞原料药有关物质的测定。
Objective：To establish an HPLC method for the determination of related substances in cinacalcet hydrochlorid raw material.Methods：HPLC was adopted on a Venusil XBP-C（18） column（4.6 mm×150 mm,5μm）with the mobile phase of 30 mmol·L^（-1） potassium dihydrogen phosphate solution containing 0.5%triethylamine（p H was adjusted to 2.5 with phosphate acid）-methanol-acetonitrile-isopropanol（60∶15∶15∶10）.The flow rate was 1.3 mL·min^（-1）,and the column temperature was maintained at 35℃,the detection wavelength was set at 220 nm.Results：The resolutions between cinacalcet hydrochlorid and known impurities were greater than those of the requirements.The calibration curves of 10 known impurities were linear in the self-concentration range（r20.999,n=6）.The determination results of the three batches of cinacalcet hydrochlorid samples showed that the known impurities were less than 0.1%,the maximum single unknown impurity was less than 0.1%,and the total impurities were less than 0.5%.Conclusion：The method showed good sensitivity and specificity,and it is suitable for the quality control of cinacalcet hydrochlorid.
作者
杨浩天
马银玲
宋浩静
吴茵
董占军
YANG Hao-tian;MA Yin-ling;SONG Hao-jing;WU Yin;DONG Zhan-jun(Department of Pharmacy, Hebei General Hospital, Shijiazhuang 050051, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第5期844-850,共7页
Chinese Journal of Pharmaceutical Analysis
