摘要
目的:采用高效液相色谱法,使用氢化可的松琥珀酸单酯对照品,建立氢化可的松琥珀酸钠及制剂含量测定方法。方法:考察氢化可的松琥珀酸钠及氢化可的松琥珀酸单酯引湿性、稳定性等理化性质;参照2020年版《中华人民共和国药典》二部氢化可的松琥珀酸钠各论项下方法建立氢化可的松琥珀酸单酯国家标准品;建立氢化可的松琥珀酸钠及制剂含量测定方法,采用反相高效液相色谱法,使用Waters Xbridge C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈-水-磷酸(330∶670∶1)作为流动相,流速为1.0 mL·min^(-1),柱温为30℃,检测波长为254 nm,进样体积20μL。结果:氢化可的松琥珀酸钠极具引湿性,热不稳定,而氢化可的松琥珀酸单酯引湿性小,稳定性好,适合作为含量测定用对照品;研制了氢化可的松琥珀酸单酯国家标准品,以质量平衡法定值,含量为99.6%;建立了以氢化可的松琥珀酸单酯为外标对照品的专属性、耐用性、精密度良好的氢化可的松琥珀酸钠及制剂含量测定方法,采用建立的方法与原标准方法同时测定多批原料及制剂含量,测定结果没有显著性差异。结论:氢化可的松琥珀酸单酯可作为氢化可的松琥珀酸钠含量测定用对照品,稳定性更好,该方法适用于氢化可的松琥珀酸钠及制剂的含量测定。
Objective:To establish a high-performance liquid chromatography(HPLC)method for the determination of the content of sodium hydrocortisone succinate and its preparations using hydrocortisone hemisuccinate as the reference standard.Methods:The hygroscopicity,stability,and other physical and chemical properties of sodium hydrocortisone succinate and hydrocortisone hemisuccinate were investigated.The national reference standard of hydrocortisone hemisuccinate was calibrated according to the method specified in the 2020 edition of the second part of the Chinese Pharmacopoeia for sodium hydrocortisone succinate.A HPLC method for the determination of the content of sodium hydrocortisone succinate and its preparations was developed using a Waters Xbridge C_(18) column(4.6 mm×250 mm,5μm)with a mobile phase consisting of acetonitrile-water-phosphoric acid(330∶670∶1)at a flow rate of 1.0 mL·min^(-1),column temperature of 30℃,detection wavelength of 254 nm,and injection volume of 20μL.Results:Sodium hydrocortisone succinate exhibits strong hygroscopicity and thermal instability,whereas hydrocortisone hemisuccinate demonstrates low hygroscopicity and excellent stability,making it suitable as a reference standard for content determination.A national reference standard for hydrocortisone hemisuccinate was developed and calibrated using the mass balance method,with a determined content of 99.6%.A specific,robust,and precise method for the determination of the content of sodium hydrocortisone succinate and its preparations was established using hydrocortisone hemisuccinate as an external reference standard.The method was validated for specificity,robustness,and precision.The method was also validated by simultaneous analysis of the content of multiple batches of raw materials and formulations using the newly established method and the standard method,and there was no significant differences in the results.Conclusion:Hydrocortisone hemisuccinate can be used as a reference standard for the determination of sodium hydrocortisone succinate content,with better stability.The developed method is suitable for the quantitative analysis of sodium hydrocortisone succinate and its preparations.
作者
孙悦
罗淑青
胡馨月
周征
蔡怡
李晶
Sun Yue;Luo Shuqing;Hu Xinyue;Zhou Zheng;Cai Yi;Li Jing(National Institutes for Food and Drug Control,NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,Beijing 102629,China;Ningbo Institute for Drug Control,Ningbo 315040,China;Zhejiang Pharmaceutical University,Ningbo 315500,China)
出处
《中国药事》
2025年第11期1272-1281,共10页
Chinese Pharmaceutical Affairs
基金
中国食品药品检定研究院化学药品检定所重点实验室项目(编号2024HYZX38)。
关键词
氢化可的松琥珀酸钠
氢化可的松琥珀酸单酯
对照品
含量测定
高效液相色谱法
sodium hydrocortisone succinate
hydrocortisone hemisuccinate
reference standard
content determination
high-performance liquid chromatography method
