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目的:建立塞来昔布中基因毒性杂质对磺酰胺基苯肼盐酸盐的含量测定方法。方法:采用HPLC法,色谱柱:以100%多孔渗水石墨为填料的Hypercarb系列C18柱(150 mm×4.6 mm,3μm);流动相:10 mmol·L~(-1)乙酸铵水溶液-甲醇(50∶50)和甲醇,梯度洗脱;流速:0.8 ml·min~(-1);检测波长:220 nm;柱温:35℃;进样量:20μl。结果:对磺酰胺基苯肼盐酸盐在99.897~599.382 ng·ml~(-1)(r=0.998 2)浓度范围内与峰面积呈良好的线性关系。平均回收率为97.4%(RSD=3.0%,n=9)。结论:该方法简便、准确,可用于塞来昔布中对磺酰胺基苯肼盐酸盐的含量测定。
OBJECTIVE: To establish a method for the determination of sulfonamidophenylhydrazine hydrochloride in genotoxicity of celecoxib. Methods: The HPLC method was used. Hypercarb C18 column (150 mm × 4.6 mm, 3 μm) packed with 100% porous graphite was used as the mobile phase. The mobile phase consisted of 10 mmol·L -1 ammonium acetate in methanol 50:50) and methanol gradient elution; flow rate: 0.8 ml · min -1; detection wavelength: 220 nm; column temperature: 35 ℃; injection volume: 20μl. Results: There was a good linear relationship between the sulfonamidophenylhydrazine hydrochloride and the peak area in the concentration range of 99.897-599.382 ng · ml -1 (r = 0.998 2). The average recovery was 97.4% (RSD = 3.0%, n = 9). Conclusion: This method is simple and accurate and can be used for the determination of sulfonamide phenylhydrazine hydrochloride in celecoxib.