中国药物警戒 ›› 2025, Vol. 22 ›› Issue (7): 749-754.
DOI: 10.19803/j.1672-8629.20250061

• 基础与临床研究 • 上一篇    下一篇

基于高效液相色谱-三重四极杆质谱联用技术的依非韦伦片有关物质研究

刘毅1, 吴静芳2#, 覃玲1, 陈俊苗3, 章娟2, 陈华1,*, 宁霄1, 曹进1   

  1. 1中国食品药品检定研究院化学药品检定所,北京 102629;
    2广州市药品检验所,广东 广州 510160;
    3上海爱博才思分析仪器贸易有限公司,北京 100015
  • 收稿日期:2025-01-26 出版日期:2025-07-15 发布日期:2025-07-17
  • 通讯作者: *陈华,男,硕士,主任药师,化学药品质量分析。E-mail: chenhua@nifdc.org.cn
  • 作者简介:刘毅,男,博士,主任药师,化学药品质量分析。#为并列第一作者。
  • 基金资助:
    国家重点研发计划（2021YFC2401100）

Related Substances in Efavirenz Tablets Based on HPLC-TRIPLE QUAD-MS/MS Technology

LIU Yi1, WU Jingfang2#, QIN Lin1, CHEN Junmiao3, ZHANG Juan2, CHEN Hua1,*, NING Xiao1, CAO Jin1   

  1. 1Institute for Chemical Drug Control, National Institutes for Food and Drug Control, Beijing 102629, China;
    2Guangzhou Institute for Drug Control, Guangzhou Guangdong 510160, China;
    3SCIEX China, Beijing 100015, China
  • Received:2025-01-26 Online:2025-07-15 Published:2025-07-17

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摘要： 目的 建立测定依非韦伦片中有关物质的高效液相色谱-三重四极杆质谱联用（HPLC-TRIPLE QUAD-MS/MS）法,并推导质谱裂解途径。方法 以十八烷基键合相硅胶为填料的色谱柱（4.6 mm×100 mm, 3 μm）;流动相为0.1%甲酸（含2 mmol·L-1甲酸铵）-甲醇（梯度洗脱）;质谱采用电喷雾离子源（ESI）,以正离子模式、多反应监测方式（MRM）进行定量分析。结果 对依非韦伦和4种杂质的质谱图进行解析并推导其裂解途径。对检测方法进行了方法学验证,依非韦伦杂质A、杂质B和杂质C在1~500 ng·mL-1内线性关系良好,杂质D在5~500 ng·mL-1内线性关系良好;定量限在1.0~5.0 ng·mL-1;4种杂质的加样回收率在89.5%~95.3%。结论 该方法专属性强、灵敏度高且准确度好,适用于依非韦伦片中有关物质的检查与控制。

关键词: 依非韦伦片, 有关物质, 高效液相色谱-三重四极杆质谱联用, 质谱定量

Abstract: Objective To establish an HPLC-TRIPLE QUAD-MS/MS method for determination of related substances in efavirenz tablets and to deduce their mass spectrometry fragmentation pathways. Methods The separation was carried out on a C18 column (4.6 mm×100 mm, 3 μm). The mobile phase was 0.1% formic acid (containing 2 mmol·L-1 ammonium formate)-methanol (gradient elution). An ion source ESI was used and quantification was in a positive ion mode in a multi-reaction monitoring mode (MRM). Results The mass spectra of efavirenz and four of its impurities were analyzed before the fragmentation pathways were deduced. The determination method was validified methodologically. Impurities A, B, and C had good linear relationships within the range of 1-500 ng·mL-1, while impurity D had a good linear relationship within the range of 5-500 ng·mL-1. The limits of quantification ranged from 1.0 to 5.0 ng·mL-1, while the average recovery ranged from 89.5% to 95.3%. Conclusion The established HPLC-TRIPLE QUAD-MS/MS method has a strong specificity, high sensitivity, and good accuracy. It is suitable for simultaneous quantitative determination of related substances in efavirenz tablets.

Key words: Efavirenz Tablets, Related Substances, HPLC-TRIPLE QUAD-MS/MS, Mass Spectrometry Quantification

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