Liu Qiutao, Kong Weijun, Guo Weiying, Yang Meihua
Pharmacy College, Liaoning Medical University, Jinzhou, Liaoning 121001, China; Institute of Medicinal Plant Development, Chinese Academy of Medicinal Sciences & Peking Union Medical College, Beijing 100193, China.
Institute of Medicinal Plant Development, Chinese Academy of Medicinal Sciences & Peking Union Medical College, Beijing 100193, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Apr 15;988:175-81. doi: 10.1016/j.jchromb.2015.02.022. Epub 2015 Feb 23.
An ultra fast liquid chromatography coupled with tandem mass spectrometry (UFLC-MS/MS) method was developed and validated for simultaneous analysis of multi-class mycotoxins including aflatoxins (AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), fumonisins (FB1 and FB2) and zearalanone (ZEN) in 20 batches of Angelica sinensis samples collected from different markets and stores in China. The eight mycotoxins were extracted and cleaned up by using QuEChERS-based procedure, and then were quantified under the multiple reaction monitoring (MRM) together with positive and negative ionization modes. Focusing on the optimization of extraction and clean-up conditions, as well as UFLC separation and MS/MS parameters of targeted analytes, the developed method expressed good linearity for the eight mycotoxins within their respective linear ranges with correlation coefficients all higher than 0.9974. The limits of detection (LODs) and quantification (LOQs) ranged from 0.005 to 0.125 μg/kg and from 0.0625 to 0.25 μg/kg, respectively. Recoveries for spiked A. sinensis sample at three different levels were all above 78.9% with relative standard deviations (RSDs) below 6.36% for all analytes. Analysis of real samples demonstrated that two visibly moldy A. sinensis samples were detected with AFB1 of 2.07 and 2.92 μg/kg, and AFG1 of 2.84 and 1.53 μg/kg. The proposed quantitative method with significant advantages including simple pretreatment, rapid determination and high sensitivity would be the preferred candidate for the determination and quantification of multi-class mycotoxin contaminants in complex matrixes, which well fulfilled the maximum residue limits (MRLs) from various countries.
建立了一种超快速液相色谱-串联质谱（UFLC-MS/MS）方法，并对其进行了验证，用于同时分析从中国不同市场和商店采集的20批当归样品中的多类霉菌毒素，包括黄曲霉毒素（AFB1、AFB2、AFG1和AFG2）、赭曲霉毒素A（OTA）、伏马毒素（FB1和FB2）和玉米赤霉烯酮（ZEN）。采用基于QuEChERS的方法对8种霉菌毒素进行提取和净化，然后在多反应监测（MRM）模式下，分别在正离子和负离子模式下进行定量分析。该方法着重优化了提取和净化条件以及目标分析物的UFLC分离和MS/MS参数，在各自线性范围内对8种霉菌毒素表现出良好的线性关系，相关系数均高于0.9974。检测限（LOD）和定量限（LOQ）分别为0.005至0.125 μg/kg和0.0625至0.25 μg/kg。在三个不同加标水平下，加标当归样品的回收率均高于78.9%，所有分析物的相对标准偏差（RSD）均低于6.36%。实际样品分析表明，检测到两个明显发霉的当归样品，其AFB1含量分别为2.07和2.92 μg/kg，AFG1含量分别为2.84和1.53 μg/kg。所提出的定量方法具有预处理简单、测定快速、灵敏度高等显著优点，是复杂基质中多类霉菌毒素污染物测定和定量的首选方法，该方法很好地满足了各国的最大残留限量（MRL）要求。
