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目的:建立吡诺克辛钠含量及有关物质的测定方法。方法:采用高效液相色谱法,色谱柱为Kromasil C_(18)(250 mm×4.6 mm,5μm);以0.1 mol·L~(-1)磷酸二氢钠溶液(用氢氧化钠试液调节pH至6.0)-甲醇-乙睛(75:30:10)为流动相;检测波长为230 nm;流速为1.0 ml·min~(-1);柱温为40℃。结果:吡诺克辛钠与杂质峰良好分离,在0.5～50.0μg·ml~(-1)质量浓度范围内线性关系良好(r=0.999 9),检测限为0.05μg·ml~(-1);平均回收率为100.3%(RSD=0.90%,n=9)。结论:本方法专属性强、准确、灵敏,适用于吡诺克辛钠原料药中有关物质的限度检查。
Objective: To establish the determination of piroxicam sodium content and related substances. Methods: High performance liquid chromatography (HPLC) was used with Kromasil C18 (250 mm × 4.6 mm, 5 μm) column and 0.1 mol·L -1 sodium dihydrogen phosphate solution (adjusted with sodium hydroxide solution (pH = 6.0) -methanol-acetonitrile (75:30:10) was used as mobile phase. The detection wavelength was 230 nm. The flow rate was 1.0 ml · min -1. The column temperature was 40 ℃. Results: The pirenoxine sodium was separated from the impurity peak well. The linear range was 0.5 ~ 50.0μg · ml ~ (-1) (r = 0.999 9), and the detection limit was 0.05μg · ml ~ (-1) ); The average recovery was 100.3% (RSD = 0.90%, n = 9). Conclusion: The method is highly specific, accurate and sensitive and is suitable for the limit check of related substances in pirenoxine sodium APIs.