HPLC检测柳氮磺吡啶原料药有关物质

目的: 建立了高效液相色谱(HPLC)法检查柳氮磺吡啶原料药有关物质检查的方法。 方法: 用C₁₈硅胶色谱柱(250 mm×4.6 mm,5 μm),采用梯度洗脱程序,以无水乙酸钠2.5 g和磷酸二氢钠1.13 g,溶于900 mL水中,用醋酸调pH为4.9,定容至1000 mL 为流动相A,另取流动相A-甲醇(1∶ 4)为流动相B,检测波长320 nm,流速1.0 mL·mim^-1。 结果: 柳氮磺吡啶线性关系良好,可用于其有关物质总杂质的检测。 方法: 同时建立了高效液相色谱法对其磺胺吡啶和水杨酸进行了检查,以流动相A-流动相B(71∶ 29)为流动相,调节pH为4.4,检测波长300 nm。 结果: 磺胺吡啶和水杨酸线性关系良好,可用于柳氮磺吡啶原料杂质的检查。 结论: 方法简便、快速、准确可靠,为柳氮磺吡啶原料药质量控制提供了新的测定方法。

Objectives: To establish an HPLC method to examine related substances in sulfasalazine . Methods: The column was Inertsil ODS column (250 mm×4.6 mm,5 μm) .In a 1000 mL volumetric flask dissolve 1.13 g of sodium dihydrogen phosphate and 2.5 g of sodium acetate in 900 mL of water R.Adjust to pH 4.8 with glacial acetic acid R and adjust the volume to 1000 mL with water R,was used as the mobile phase A and Mix 1 volume of mobile phase A with 4 volumes of methanol methanol as mobile phase B with the flow rate of 1.0 mL·min^-1,and gradient was 40%-100% in 60 min.The detection wavelength was 320 nm. Results: The linear range for sulfasalazine was excellent . Methods: At the same time,the HPLC method to examine salicylic acid and sulfapyridine was estabkished.with the same column,mobile phase at a flow rate of 1 mL·min^-1 a mixture of 71volumes of mobile phase A and 29 volumes of mobile phase B with the pH 4.4,the detection wavelength was 300 nm. Results: The linear range for salicylic acid and sulfapyridine were excellent.The methods are simple,quick and reliable. Conclusion: It can be used to examine related substances and salicylic acid and sulfapyridine in sulfasalazine.