中国药物警戒 ›› 2025, Vol. 22 ›› Issue (4): 368-371.
DOI: 10.19803/j.1672-8629.20240820

• 细菌内毒素检测技术研究专栏 • 上一篇    下一篇

药用辅料三甲基间苯三酚的细菌内毒素检查方法研究

赵雨歆1, 蔡彤2,△, 孙会敏2, 刘涛3, 裴宇盛2#, 许华容1,*   

  1. 1沈阳药科大学药学院,辽宁 沈阳 110016;
    2中国食品药品检定研究院化学药品检定研究所,北京 102629;
    3中国科学院苏州生物医学工程技术研究所,江苏 苏州 215163
  • 收稿日期:2024-10-24 发布日期:2025-04-17
  • 通讯作者: *许华容,男,博士,副教授,药物分析。E-mail: xuh@syphu.edu.cn #为共同通信作者。
  • 作者简介:赵雨歆,女,硕士,药物分析。△为并列第一作者。
  • 基金资助:
    国家重点研发计划（2023YFC2606100）

Testing Methods for Bacterial Endotoxin in a Pharmaceutical Excipient of Trimethyl-Phloroglucinol

ZHAO Yuxin1, CAI Tong2,△, SUN Huimin2, LIU Tao3, PEI Yusheng2#, XU Huarong1,*   

  1. 1Shenyang Pharmaceutical University, School of Pharmacy, Shenyang Liaoning 110016, China;
    2National Institute for Food and Drug Control, Institute for Chemical Drug Control, Beijing 102629, China;
    3Suzhou Institute of Biomedical Engineering and Technology, Chinese Academy of Sciences, Suzhou Jiangsu 215163, China
  • Received:2024-10-24 Published:2025-04-17

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摘要： 目的 为难溶性药用辅料三甲基间苯三酚建立细菌内毒素检测方法。方法 根据《中华人民共和国药典》（2020年版）通则1143细菌内毒素检查法项,使用3种方法建立三甲基间苯三酚药用辅料的细菌内毒素检查方法。①二甲基亚砜溶解供试品至10 mg·mL-1后,用细菌内毒素检查用水稀释200倍,使用凝胶法、灵敏度为0.03 EU·mL-1的鲎试剂进行检测;②70%乙醇溶液溶解供试品至5 mg·mL-1后,用细菌内毒素检查用水稀释30倍,使用凝胶法、灵敏度为0.25 EU·mL-1的鲎试剂进行检测;③甲醇溶解供试品至100 mg·mL-1,再用20%的吐温80溶液将供试品溶液稀释至10 mg·mL-1后,用细菌内毒素检查用水稀释40倍,使用凝胶法、灵敏度为0.03 EU·mL-1的鲎试剂进行细菌内毒素检测。结果 3种溶解方法溶解供试品后采用检查用水稀释的方法,均可排除溶剂和供试品对细菌内毒素检测的干扰,干扰试验结果符合规定,且供试品细菌内毒素含量均低于限值,符合《中华人民共和国药典》（2020 年版）规定。结论 建立了3种三甲基间苯三酚的细菌内毒素检查方法,为难溶性样品建立细菌内毒素检查方法提供参考。

关键词: 三甲基间苯三酚, 药用辅料, 细菌内毒素, 凝胶法, 二甲基亚砜, 难溶性

Abstract: Objective To establish a detection method for bacterial endotoxin in trimethyl-phloroglucinol. Methods According to the General Requirements of the Chinese Pharmacopoeia(2020 Edition),three methods were adopted to establish one for detection of bacterial endotoxin.①The test sample was dissolved in dimethyl sulfoxide(DMSO) to a concentration of 10 mg·mL-1, diluted 200-fold with BET water, and tested using the gel method with Limulus amebocyte lysate at a sensitivity of 0.03 EU·mL-1.②The test sample was dissolved in 70% ethanol to a concentration of 5 mg·mL-1, diluted 30-fold with BET water, and tested using the gel method with Limulus amebocyte lysate at a sensitivity of 0.25 EU·mL-1. ③The test sample was dissolved in methanol to a concentration of 100 mg·mL-1. The test solution was diluted to 10 mg·mL-1 with 20% Tween 80 solution before being diluted 40-fold with BET water and tested using the gel method with Limulus amebocyte lysate at a sensitivity of 0.03 EU·mL-1. Results After the tested products were dissolved with the three methods, the interference of the solvent and test sample with endotoxin detection was eliminated. The results of the interference test met the requirements. Conclusion Three test methods for bacterial endotoxin in trimethyl-phloroglucinol have been established, which can provide a reference for the establishment of detection methods for bacterial endotoxin in insolvable samples.

Key words: Trimethyl-Phloroglucinol, Pharmaceutical Excipients, Bacterial Endotoxin, Gel Method, Dimethyl Sulfoxide, Insolubility

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