中国药物警戒 ›› 2025, Vol. 22 ›› Issue (10): 1100-1103.
DOI: 10.19803/j.1672-8629.20250392

• 基础与临床研究 • 上一篇    下一篇

醋酸去氨加压素中聚合物测定方法研究

孙悦1, 罗淑青2△, 潘笑然3, 胡馨月1, 丁晓丽1, 李晶1,*   

  1. 1中国食品药品检定研究院化学药品检定所,国家药品监督管理局化学药品质量研究与评价重点实验室,北京 102629;
    2宁波市药品检验所化学药品检验室,浙江 宁波 315048;
    3北京石油化工学院新材料与化工学院,北京 102600
  • 收稿日期:2025-06-16 出版日期:2025-10-15 发布日期:2025-10-20
  • 通讯作者: *李晶,女,博士,研究员,激素与生物技术药物质量控制研究。E-mail: li_jing@nifdc.org.cn
  • 作者简介:孙悦,女,硕士,助理研究员,激素类药物质量控制研究。△为并列第一作者。
  • 基金资助:
    国家重点研发计划（2021YFF0600804）; 中国食品药品检定研究院中青年发展研究基金课题（2024A2）

A Method for Determination of Polymers in Desmopressin Acetate

SUN Yue1, LUO Shuqing2△, PAN Xiaoran3, HU Xinyue1, DING Xiaoli1, LI Jing1,*   

  1. 1Institute for Chemical Drug Control, National Institutes for Food and Drug Control, NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs, Beijing 102629, China;
    2Chemical Drug Analysis Laboratory, Ningbo Institute for Drug Control, Ningbo Zhejiang 315040, China;
    3College of New Materials and Chemical Engineering, Beijing Institute of Petrochemical Technology, Beijing 102600, China
  • Received:2025-06-16 Online:2025-10-15 Published:2025-10-20

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摘要： 目的 采用分子排阻色谱法建立醋酸去氨加压素中聚合物检查方法,进行方法学验证。方法 采用分子排阻高效液相色谱法,使用TSKgel G2000SWXL色谱柱（7.8 mm×300 mm,5μm）,以磷酸-乙腈-甲醇-水（0.2∶15∶5∶80）（用磷酸氢二钠溶液调节pH值至2.5）为流动相;流速为0.3 mL·min-1;柱温25℃;检测波长为210 nm;进样量50μL。结果 平行二聚体与醋酸去氨加压素峰之间分离良好;专属性、耐用性、精密度良好;平行二聚体、交叉二聚体和醋酸去氨加压素分别在0.01~21.6、0.01~22.9、0.01~25.6μg·mL-1浓度范围内呈良好的线性关系（r均大于0.99）;平行二聚体、交叉二聚体和醋酸去氨加压素检出限分别为0.14、0.31、0.17 ng,定量限分别为0.43、0.46、0.51 ng;平行二聚体和交叉二聚体平均加标回收率（n=9）均在95%~105%内,准确度良好。结论 该方法可操作性强、准确、灵敏度高,适用于醋酸去氨加压素中聚合物的测定。

关键词: 醋酸去氨加压素, 分子排阻色谱法, 聚合物, 平行二聚体, 交叉二聚体

Abstract: Objective To establish a method for the determination of polymers in desmopressin acetate using size exclusion chromatography. Methods A size exclusion chromatography method was employed, using a TSKgel G2000SWXL column (TSKgel G2000SWXL, 7.8 mm×300 mm, 5μm) with a mobile phase consisting of phosphoric acid-acetonitrile-methanol-water (0.2∶15∶5∶80) (with pH adjusted to 2.5 by disodium hydrigenphosphate buffer) at the flow rate of 0.3 mL·min-1. The column temperature was 25℃, the detection wavelength 210 nm, and the injection volume was 50 µL. Results The peaks of the parallel-dimer and desmopressin acetate were well separated with a good specificity, durability and precision. The parallel-dimer, cross-dimer and desmopressin acetate showed a good linear relationship within the concentration ranges of 0.01-21.6 μg·mL-1, 0.01-22.9 μg·mL-1 and 0.01-25.6 μg·mL-1, respectively (r>0.99). The limits of detection and quantification for the parallel-dimer, cross-dimer and desmopressin acetate were 0.14, 0.31, 0.17ng and 0.43, 0.46, 0.51 ng, respectively. The average recovery (n=9) of the parallel-dimer and cross-dimer ranged from 95% to 105%, indicating good accuracy. Conclusion This method is operable, accurate and sensitive, making it desirable for the determination of polymers in desmopressin acetate.

Key words: Desmopressin Acetate, Size Exclusion Chromatography, Polymers, Parallel-Dimers, Cross-Dimers

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