摘要
建立一种可同时测定僵蚕和土鳖虫药材中多种真菌毒素检测方法,为该类药材的监测和质量控制提供技术支撑。以易霉变的僵蚕、土鳖虫为研究对象,采用UPLC-MS/MS技术进行检测,并对色谱、质谱条件,供试品制备方法和QuEChERS净化参数进行优化,在多反应监测模式(MRM)下扫描,基质标准曲线法定量分析。所检14种真菌毒素在0.04~500 ng·mL^(-1)线性关系良好,相关系数(r)≥0.99,检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.01~0.648、0.022~1.435μg·kg^(-1);在高、中、低3个添加水平下,所测毒素平均回收率为70.99%~124.7%,相对标准偏差(RSD)为0.44%~8.5%,均符合2020年版《中国药典》的规定。将方法应用于20批次僵蚕、土鳖虫药材中真菌毒素的检测,共检测出脱氧雪腐镰刀菌烯醇(DON)、黄曲霉毒素B_(1)(AFB_(1))、杂色曲霉素(ST)、黄曲霉毒素G_(1)(AFG_(1))、赭曲霉毒素A(OTA)5种毒素。其中,10批僵蚕样本中,有OTA、AFB_(1)、AFG_(1)3种毒素被检出,AFs存在10.0%的超标;10份土鳖虫样本中检出AFB_(1)、AFG_(1)、ST、DON 4种毒素,AFB_(1)、AFs均存在10.0%的超标,存在一定的风险,应重点关注。该研究成功建立了一种适用于僵蚕和土鳖虫等动物类中药材中多种真菌毒素的检测方法,该方法适用范围广,解决了现有真菌毒素检测方法适用性窄的问题,可为其他易霉变中药材真菌毒素检测方法的开发提供参考。
A method for simultaneous determination of multiple mycotoxins in Bombyx Batryticatus and Eupolyphaga Steleophaga was established to provide technical support for monitoring and quality control of such medicinal materials.The mildew-prone Bombyx Batryticatus and Eupolyphaga Steleophaga were detected by UPLC-MS/MS technology,and the chromatographic conditions,mass spectrometry conditions,test sample preparation methods,and QuEChERS purification parameters were optimized.Scanning was conducted under multiple reaction monitoring mode(MRM),and quantitative analysis was performed by matrix standard curve method.The detected 14 mycotoxins had good linear relationships in the range of 0.04-500 ng·mL^(-1),with correlation coefficients(r)≥0.99.The limits of detection(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)were 0.01-0.648μg·kg^(-1)and 0.022-1.435μg·kg^(-1).At the high,medium,and low addition levels,the average recovery of the detected toxins was 70.99%-124.7%,and the relative standard deviation(RSD)was 0.44%-8.5%,all of which were in line with the requirements of the 2020 edition of the Chinese Pharmacopoeia.The method was applied to the detection of mycotoxins in 20 batches of Bombyx Batryticatus and Eupolyphaga Steleophaga,and five kinds of toxins including DON,AFB_(1),ST,AFG_(1),and OTA were detected.Among them,OTA,AFB_(1),and AFG_(1)were detected in 10 batches of Bombyx Batryticatus samples,and 10.0%of AFs exceeded the standard.Four toxins of AFB_(1),AFG_(1),ST,and DON were detected in 10 samples of Eupolyphaga Steleophaga,and 10.0%of AFB_(1)and AFs exceeded the standard,indicating certain risks and requiring more attention.In this paper,a detection method for multiple mycotoxins in Bombyx Batryticatus,Eupolyphaga Steleophaga,and other animal Chinese herbal medicines was successfully established.This method had a wide range of applications and expanded the narrow application range of existing mycotoxin detection methods.This research can provide a reference for the development of mycotoxin detection methods for other mildew-prone Chinese herbal medicines.
作者
朱贵红
杨昌贵
江维克
郭兰萍
康传志
袁青松
吴小凤
周涛
ZHU Gui-hong;YANG Chang-gui;JIANG Wei-ke;GUO Lan-ping;KANG Chuan-zhi;YUAN Qing-song;WU Xiao-feng;ZHOU Tao(Guizhou University of Traditional Chinese Medicine,Guiyang 550025,China;State Key Laboratory for Quality Ensurance and Sustainable Use of Dao-di Herbs,National Resource Center for Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2024年第18期4905-4912,共8页
China Journal of Chinese Materia Medica
基金
国家重点研发计划项目(2023YFC3503803)
中央本级重大增减支项目(2060302)。
