塞来昔布关键中间体HPLC含量测定方法的建立  

Establishment of HPLC content determination methodfor key intermediates of celecoxib

作　　者：刘晓莲 Liu Xiaolian(Hebei Jiheng Pharmaceutical Corporation Ltd.,Hengshui 053400,China)

机构地区：[1]河北冀衡药业股份有限公司,河北衡水053400

出　　处：《煤炭与化工》2024年第3期146-150,共5页Coal and Chemical Industry

基　　金：河北省省级科技计划资助(199676234H)。

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(4.6×250mm,5μm);流动相:缓冲液(1.65 g庚烷磺酸钠置于1 000 m L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 m L/min;进样量为20μL;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。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,5μm).Mobile phase∶buffer(1.65 g sodium heptane sulfonate in 1000 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 20μL.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 

分 类 号：TQ465[化学工程—制药化工]