Hebei Jiheng Pharmaceutical Corporation Ltd.

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1 000 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。

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 μm). 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 μL. 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.

刘晓莲. 塞来昔布关键中间体HPLC含量测定方法的建立[J]. 煤炭与化工, 2024, 47(3): 146-150.

Liu Xiaolian. Establishment of HPLC content determination method for key intermediates of celecoxib. CCI, 2024, 47(3): 146-150.