Establishment of HPLC content determination method for key intermediates of celecoxib
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.
国家科技期刊平台
NSTL
万方数据
维普
