HPLC法测定塞来昔布原料药有关物质

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，5 μm）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（r²>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. 

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