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 C_(18)(100 mm×2.1 mm,1.8μm)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B_(1)(aflatoxin B_(1),AFB_(1))和黄曲霉毒素B_(2)(aflatoxin B_(2),AFB_(2))外,还在中药样本中发现了伏马毒素B_(2)(fumonisin B_(2),FB_(2))、柄曲霉素(sterigmatocystin,ST)、白僵菌素(beauvericin,BEA)、恩镰孢菌素B_(1)(enniatin B_(1),ENNB_(1))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。
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 C_(18)(100 mm×2.1 mm,1.8μm)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 B_(1)and aflatoxin B_(2)that are restricted in the Chinese pharmacopoeia(2020 edition),potential mycotoxins and fungal metabolites such as fumonisin B_(2),sterigmatocystin,beauvericin,enniatin Br,and fumigaclavine C were also detected.Conclusions: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.
作者
徐晓艳
俞飞洋
马伶俐
王怜星
李雪
杨文志
XU Xiao-yan;YU Fei-yang;MA Ling-li;WANG Lian-xing;LI Xue;YANG Wen-zhi(State Key Laboratory of Component-based Chinese Medicine,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China)
出处
《药物分析杂志》
北大核心
2025年第6期1041-1055,共15页
Chinese Journal of Pharmaceutical Analysis
基金
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)。
关键词
真菌毒素
中药
超高效液相色谱/离子淌度四极杆飞行时间质谱
自建数据库
非靶向筛查
mycotoxin
traditional Chinese medicine
ultra-high performance liquid chromatography/ion mobility time-of-flight mass spectrometry
in-house library
untargeted screening
