塞来昔布关键中间体HPLC含量测定方法的建立
Establishment of HPLC content determination method for key intermediates of celecoxib
刘晓莲1
作者信息
- 1. 河北冀衡药业股份有限公司,河北衡水 053400
- 折叠
摘要
为建立合成塞来昔布关键中间体对肼基苯磺酰胺盐酸盐的质量标准,测定对肼基苯磺酰胺盐酸盐的含量.采用高效液相色谱法,色谱柱:Agilent ZORBAX SB-C18柱(4.6×250 mm,5 µm);流动相:缓冲液(1.65 g庚烷磺酸钠置于1000 mL容量瓶中,用水溶解并稀释至刻度,用三氟乙酸调pH值至2.5)∶乙腈=88∶12;流速为1.0 mL/min;进样量为20 μL;检测波长为233 nm;柱温为25 ℃.结果显示:该中间体的峰面积与浓度呈良好的线性关系,加样平均回收率为99.77％,相对标准偏差RSD为0.40％.结果表明,该方法方便、准确、可靠,可用于测定对肼基苯磺酰胺盐酸盐的含量.
Abstract
In order to establish the quality standard for the synthesis of the key intermediate of celecoxib,and determine the content of 4-Hydrazinobenzene-1-sulfonamide hydrochloride.HPLC was performed on Agilent ZORBAX SB-C18 column(4.6×250 mm,5 μ m).Mobile phase:buffer(1.65 g sodium heptane sulfonate in 1 000 mL volumetric bottle,dissolved with water and diluted to the scale,adjusted to pH 2.5 with trifluoroacetic acid):acetonitrile=88:12;The flow rate was 1.0mL/min.The sample size was 20 µ L.The detection wavelength was 233 nm;The column temperature was 25℃.The results showed that the peak area of the intermediate had a good linear relationship with the concentration.The average recovery was 99.77％and the RSD was 0.40％.The results show that the method is convenient,accurate and reliable,and can be used to determine the content of 4-Hydrazinobenzene-1-sulfonamide hydrochloride.
关键词
塞来昔布/对肼基苯磺酰胺盐酸盐/高效液相色谱/含量测定Key words
celecoxib/4-Hydrazinobenzene-1-sulfonamide hydrochloridel/High performance liquid chromatography/content determination引用本文复制引用
基金项目
河北省省级科技计划资助(199676234H)
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据