摘要
目的:建立高效液相色谱法测定塞来昔布原料药的有关物质。方法:采用SUPELCOSIL LC-DP(4.6 mm×250 mm,5μm)色谱柱,以20 mmol·L^(-1)磷酸二氢钾水溶液(磷酸调pH为3.0)-甲醇-乙腈(60∶30∶10)为流动相,流速1.5 mL·min^(-1),柱温60℃,检测波长215 nm。结果:塞来昔布与6个已知杂质A～F色谱峰之间的分离度良好,其中杂质E、F在各自的线性范围内线性关系良好(r^2>0.999,n=6)。3批塞来昔布样品测定结果显示,已知杂质及其他最大单个杂质均小于0.01%,杂质总含量小于0.05%。结论:经方法学验证,本法灵敏度高,专属性好,可用于塞来昔布原料药有关物质的测定。
Objective:To establish an HPLC method for the determination of related substances in celecoxib raw material. Methods:HPLC was adopted on a SUPELCOSIL LC-DP column(4.6 mm×250 mm,5 μm)with a gradient elution system of 20 mmol·L-1 potassium dihydrogen phosphate solution(pH was adjusted to 3.0 with phosphate acid)-methanol-acetonitrile(60∶30∶10). The flow rate was 1.5 mL·min-1,and the column temperature was maintained at 60 ℃,the detection wavelength was set at 215 nm. Results:The resolutions between the peaks of celecoxib and six known impurities(including impurities A-F)were good. The calibration curves of impurities E and F were linear in their respective concentration ranges(r2>0.999,n=6). The determination results of the three batches of celecoxib samples showed that the known impurities were less than 0.01%,the maximum single unknown impurity was less than 0.01%,the total impurities were less than 0.05%. Conclusion:The method is proved that it has good sensitivity and specificity,and it is suitable for the quality control of celecoxib.
作者
杨浩天
宋浩静
吴茵
董占军
YANG Hao-tian;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
2019年第1期164-170,共7页
Chinese Journal of Pharmaceutical Analysis
