谷物及其制品中11种真菌毒素污染水平的测定与分析  

Determination and analysis of 11 mycotoxins contamination levels in cereals and its product

作　　者：侯广月 徐志娇 周莉莉 李大为 卞英芳 姚傲男 HOU Guang-yue;XU Zhi-jiao;ZHOU Li-li;LI Da-wei;BIAN Ying-fang;YAO Ao-nan(Shandong Institute for Product Quality Inspection,Jinan 250102,China;National Inspection and Testing Center for Processed Food(Shandong),Jinan 250102,China)

机构地区：[1]山东省产品质量检验研究院,山东济南250102 [2]国家加工食品质量检验检测中心(山东),山东济南250102

出　　处：《化学研究与应用》2025年第1期33-39,共7页Chemical Research and Application

基　　金：国家市场监督管理总局科技计划项目(2017QK077)资助。

摘　　要：建立了超高效液相色谱-串联质谱技术同时检测谷物及其制品中11种真菌毒素的方法。样品经84%乙腈水溶液振荡提取,离心、氮吹,复溶,选择0.1%甲酸水-甲醇为流动相梯度洗脱目标化合物,以反相色谱柱进行分离,采用电喷雾离子源正离子模式和多反应监测模式进行质谱分析。结果表明,11种真菌毒素在一定浓度范围内线性关系良好,方法检出限为0.1~2.0μg·kg^(-1),定量限为0.4~6.0μg·kg^(-1)。在三个添加水平下,平均回收率为94.5%~111.7%,相对标准偏差为0.85%~8.98%。应用本方法对小麦、玉米、大米、小麦粉等790批次典型谷物及其制品中11种真菌毒素污染水平进行研究,其中182批次谷物样品中检出真菌毒素,检出率为29%,具有一定的地域性和季节性;小麦粉有1批次样品检出玉米赤霉烯酮,检出率低于小麦样品的。A method for simultaneous determination of 11 mycotoxins in cereals and its products by ultra high performance liquid chromatography-tandem mass spectrometry was established.Samples were sequentially extracted with 84%acetonitrile,then the extracts were centrifuged,nitrogen blowing and redissolved.The target compounds were gradient eluted with 0.1%formic acid-methanol by gradient elution and chromatographically separated with reversed phase chromatography column.The mass spectrometer equipped with electrospray ionization ion source was operated in the multiple reaction monitoring mode for the accurate quantitative analysis in positive mode.The result revealed that 11 mycotoxins presented excellent linearity.The limits of detection were 0.1一2.0μg·kg^(-1),meanwhile the limits of quantification were 0.4~6.0μg·kg^(-1).The mean recoveries of mycotoxins in three spiked concentrations ranged from 94.5%to 111.7%and the relative standard deviation n were in the range of 0.85%~8.98%.The method was applied for the determination of the contamination levels of 11 mycotoxins in 790 batches of typical cereals and its products,including wheat,corn,rice and wheat flour.182 batches of cereals were detected have mycotoxins contamination with a detection rate of 29%,which was certain regional and seasonal.Zearalenone was detected in one batch of wheat flour sample,and the detection rate of mycotoxin was lower than that of wheat.

关 键 词：谷物及其制品 真菌毒素 超高效液相色谱-串联质谱法 污染调查分析 

分 类 号：O657.7[理学—分析化学]