安全监测

基于超高效液相色谱/离子淌度四极杆飞行时间质谱母离子列表数据依赖采集技术非靶向筛查和鉴定中药中真菌毒素*

  • 徐晓艳 ,
  • 俞飞洋 ,
  • 马伶俐 ,
  • 王怜星 ,
  • 李雪 ,
  • 杨文志
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  • 天津中医药大学, 组分中药国家重点实验室, 天津 301617
第一作者 Tel:15703410192;E-mail:xxy_0421@163.com
**李雪 Tel:13752329580;E-mail:tjdxsyx@163.com; 杨文志 Tel:17602666784;E-mail:wzyang0504@tjutcm.edu.cn

收稿日期: 2024-12-30

  网络出版日期: 2025-11-13

基金资助

*现代中药新质生产力科技创新工程专项(24ZXZKSY00010); 国家自然科学基金项目(82304884)

Non-targeted screening and identification of mycotoxins in traditional Chinese medicine by UHPLC/IM-QTOF-MS with HDDDA-PIL acquisition technology*

  • XU Xiao-yan ,
  • YU Fei-yang ,
  • MA Ling-li ,
  • WANG Lian-xing ,
  • LI Xue ,
  • YANG Wen-zhi
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  • State Key Laboratory of Component-based Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China

Received date: 2024-12-30

  Online published: 2025-11-13

摘要

目的: 采用超高效液相色谱/离子淌度四极杆飞行时间质谱(UPLC/IM-QTOF-MS)结合自建的584种真菌毒素及真菌代谢物数据库广谱筛查和鉴定中药中的真菌毒素。方法: 使用ACQUITY UPLC HSS C18(100 mm×2.1 mm,1.8 μm)色谱柱、以0.1%甲酸-3 mmol · L-1乙酸铵水溶液(A)和乙腈(B)为流动相,通过梯度洗脱,采用电喷雾离子源,正负离子模式下数据依赖采集母离子列表(HDDDA-PIL)方法扫描。结果: 从果实种子类中药中筛查鉴定出9种真菌毒素及真菌代谢物,发现14个被真菌毒素及真菌代谢物污染的阳性样本。除《中国药典》 (2020年版)规定的黄曲霉毒素B1(aflatoxin B1,AFB1)和黄曲霉毒素B2(aflatoxin B2,AFB2)外,还在中药样本中发现了伏马毒素B2(fumonisin B2,FB2)、柄曲霉素(sterigmatocystin,ST)、白僵菌素(beauvericin,BEA)、恩镰孢菌素B1(enniatin B1,ENNB1)和fumigaclavine C等真菌毒素和可能的真菌代谢物。结论: 该方法可实现对中药中可能受污染的真菌毒素的快速筛查,为中药中真菌毒素和真菌代谢物的检测提供了一种高通量的广谱筛查和鉴定策略。

本文引用格式

徐晓艳 , 俞飞洋 , 马伶俐 , 王怜星 , 李雪 , 杨文志 . 基于超高效液相色谱/离子淌度四极杆飞行时间质谱母离子列表数据依赖采集技术非靶向筛查和鉴定中药中真菌毒素*[J]. 药物分析杂志, 2025 , 45(6) : 1041 -1055 . DOI: 10.16155/j.0254-1793.2024-1380

Abstract

Objective: To establish a method for universal screening and identification of mycotoxins in traditional Chinese medicines (TCM) by ultra-high performance liquid chromatography/ion mobility quadrupole time-of-flight mass spectrometry (UHPLC/IM-QTOF-MS) combined with an in-house library containing 584 mycotoxins and fungal metabolites. Methods: The samples were separated on an ACQUITY UPLC HSS C18 (100 mm×2.1 mm,1.8 μm) column with a mobile phase of water containing ammonium formate (3 mmol · L-1), formic acid (0.1%) (A) and acetonitrile (B) by gradient elution. The acquisition strategy was high-definition data dependent acquisition with precursor ion list (HDDDA-PIL) and electrospray ion source operating both in positive and negative mode. Results: A total of 14 TCM samples were found to be contaminated by mycotoxins and fungal metabolites, and nine types of mycotoxins or fungal metabolites that were screened and identified. In addition to aflatoxin B1 and aflatoxin B2 that are restricted in the Chinese pharmacopoeia (2020 edition), potential mycotoxins and fungal metabolites such as fumonisin B2, sterigmatocystin, beauvericin, enniatin B1, and fumigaclavine C were also detected. Conclusion: The method can realize the rapid screening of mycotoxins that may be contaminated in TCM and provides a universe and high-throughput screening and identification strategy for the detection of mycotoxins and fungal metabolites.

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