Liu Hongmei, Luo Jiaoyang, Kong Weijun, Liu Qiutao, Hu Yichen, Yang Meihua
Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing, 100193, China.
Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing, 100193, China; Liaoning Medical University Pharmacy College, Jinzhou, 121000, China.
Chemosphere. 2016 May;150:176-183. doi: 10.1016/j.chemosphere.2016.02.032. Epub 2016 Feb 20.
A robust, sensitive and reliable ultra fast liquid chromatography combined with electrospray ionization tandem mass spectrometry (UFLC-ESI-MS/MS) was optimized and validated for simultaneous identification and quantification of eleven mycotoxins in medicinal and edible Areca catechu, based on one-step extraction without any further clean-up. Separation and quantification were performed in both positive and negative modes under multiple reaction monitoring (MRM) in a single run with zearalanone (ZAN) as internal standard. The chromatographic conditions and MS/MS parameters were carefully optimized. Matrix-matched calibration was recommended to reduce matrix effects and improve accuracy, showing good linearity within wide concentration ranges. Limits of quantification (LOQ) were lower than 50 μg kg(-1), while limits of detection (LOD) were in the range of 0.1-20 μg kg(-1). The accuracy of the developed method was validated for recoveries, ranging from 85% to 115% with relative standard deviation (RSD) ≤14.87% at low level, from 75% to 119% with RSD ≤ 14.43% at medium level and from 61% to 120% with RSD ≤ 13.18% at high level, respectively. Finally, the developed multi-mycotoxin method was applied for screening of these mycotoxins in 24 commercial samples. Only aflatoxin B2 and zearalenone were found in 2 samples. This is the first report on the application of UFLC-ESI(+/-)-MS/MS for multi-class mycotoxins in A. catechu. The developed method with many advantages of simple pretreatment, rapid determination and high sensitivity is a proposed candidate for large-scale detection and quantification of multiple mycotoxins in other complex matrixes.
建立了一种快速、灵敏、可靠的超快速液相色谱-电喷雾串联质谱法(UFLC-ESI-MS/MS),该方法基于一步萃取无需进一步净化处理,可同时鉴定和定量药用和食用槟榔中的11种霉菌毒素。以玉米赤霉烯酮(ZAN)为内标,在多反应监测(MRM)模式下,于正、负离子模式下单次进样实现分离和定量。对色谱条件和MS/MS参数进行了仔细优化。建议采用基质匹配校准以减少基质效应并提高准确性,在宽浓度范围内显示出良好的线性关系。定量限(LOQ)低于50 μg kg⁻¹,检测限(LOD)在0.1 - 20 μg kg⁻¹范围内。所建立方法的准确性通过回收率验证,低水平下回收率为85%至115%,相对标准偏差(RSD)≤14.87%;中等水平下回收率为75%至119%,RSD≤14.43%;高水平下回收率为61%至120%,RSD≤13.18%。最后,将所建立的多霉菌毒素方法应用于24个商业样品中这些霉菌毒素的筛查。仅在2个样品中检测到黄曲霉毒素B2和玉米赤霉烯酮。这是首次关于UFLC-ESI(+/-)-MS/MS应用于槟榔中多类霉菌毒素检测的报道。所建立的方法具有预处理简单、测定快速、灵敏度高的诸多优点,是用于其他复杂基质中多种霉菌毒素大规模检测和定量的理想方法。