中国药物警戒 ›› 2023, Vol. 20 ›› Issue (11): 1238-1242.
DOI: 10.19803/j.1672-8629.20230129

• 基础与临床研究 • 上一篇    下一篇

高效液相色谱法测定环酯红霉素片的含量

侯金凤1, 李珉1, 黄晓春1, 寇晋萍1, 车宝泉1, 刘海涛1,*, 姚尚辰2#   

  1. 1北京市药品检验研究院,国家药品监督管理局仿制药研究与评价重点实验室,中药成分分析与生物评价北京市重点实验室,北京 102206;
    2中国食品药品检定研究院,北京 100050
  • 收稿日期:2023-03-07 出版日期:2023-11-15 发布日期:2023-11-13
  • 通讯作者: *刘海涛,男,硕士,副主任药师,抗生素类药物分析及质量控制。E-mail：livaerduo@sina.com,#为共同通信作者。
  • 作者简介:侯金凤,女,博士,副主任药师,抗生素类药物分析及质量控制。
  • 基金资助:
    国家重点研发计划（2022YFC3401205）

Determination of contents of erythromycin cyclocarbonate tablets using HPLC method

HOU Jinfeng1, LI Min1, HUANG Xiaochun1, KOU Jinping1, CHE Baoquan1, LIU Haitao1,*, YAO Shangchen2#   

  1. 1Beijing Institute for Drug Control, NMPA Key Laboratory for Research and Evaluation of Generic Drugs, Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine, Beijing 102206, China;
    2National Institutes for Food and Drug Control, Beijing 100050,China
  • Received:2023-03-07 Online:2023-11-15 Published:2023-11-13

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摘要： 目的 建立高效液相色谱法测定环酯红霉素片的含量。方法 将环酯红霉素片研细后,经乙腈提取,采用Waters XBridge C18（250 mm×4.6 mm,5μm）色谱柱,以0.02 mol·L-1磷酸氢二钾溶液（用5 mol·L-1氢氧化钾试液调节pH至11.4）-乙腈（35∶65）为流动相进行洗脱,流速为1.0 mL·min-1,在204 nm波长下测定。结果 环酯红霉素在浓度0.51~1.52 mg·mL-1范围内线性关系良好（r=0.999 9）,回收率在99.0%~100.5%（RSD为0.5%,n=9）,重复性试验RSD为0.8%（n=6）,中间精密度试验RSD为0.9%（n=12）,供试品和对照品溶液5℃放置10 h内均保持稳定,方法耐用性良好。3批供试品含量测定结果分别为102.3%、102.0%和103.5%,均在现行质量标准93.0%~107.0%限度范围内,符合规定。结论 本方法操作简便、快速、准确、专属性好,适用于环酯红霉素片的含量测定,为该品种的深入研究提供了方法参考,为存在互变异构反应的化合物的液相色谱分析提供了研究思路。

关键词: 环酯红霉素, 互变异构, 含量测定, 高效液相色谱法

Abstract: Objective To establish an HPLC method for determination of the content of erythromycin cyclocarbonate (EMC) tablets. Methods EMC tablets were grinded and extracted with acetonitrile. The chromatographic separation was performed on a Waters Xbridge C18 column (250 mm×4.6 mm, 5μm) with an isocratic elution system composed of 0.02 mol·L-1 potassium hydrogen phosphate solution (adjust pH to 11.4 with 5 mol·L-1 potassium hydroxide solution)-acetonitrile (35 : 65) at a flow rate of 1.0 mL·min-1. The elutes were detected at the wavelength of 204 nm. Results A good linearity (r=0.9999) was observed within the range of 0.51 to 1.52 mg·mL-1. The recovery was between 99.0% and 100.5% (RSD=0.5%, n=9), the repeatability was 0.8% (n=6), and the intermediate precision was 0.9% (n=12). The test and standard sample solution remained stable for 10 hours at 5℃, and the method showed good durability. The contents of the three batches of EMC tablets were 102.3%, 102.0% and 103.5% respectively, which were within the current standard limit range of 93.0% to 107.0%. Conclusion This method is simple, rapid, accurate and specific, and is workable for the content determination of EMC tablets. A reference method has become available for the in-depth study of EMC and for the analysis of compounds with tautomeric structure by liquid chromatography.

Key words: erythromycin cyclocarbonate, tautomerism, assay, HPLC

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