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建立了云南普洱茶、湖南黑茶、广西六堡茶和湖北老青茶等发酵黑茶黄曲霉毒素B_1(AFB_1)、黄曲霉毒素B_2(AFB_2)、黄曲霉毒素G_1(AFG_1)、黄曲霉毒素G_2(AFG_2)、脱氧雪腐镰刀菌烯醇(DON)、3-乙酰基脱氧雪腐镰刀菌烯醇(3-AcDON)、玉米赤霉烯酮(ZEN)、T-2毒素(T-2)、HT-2毒素(HT-2)、赭曲霉毒素A(OTA)等10种真菌毒素的简单、快速、高灵敏度超高效液相色谱-串联质谱检测方法。样品采用乙腈/水溶液(84+16)提取试样、QuEChERS净化,试样以C18柱分离,多反应监测(MRM)模式进行定量与定性分析,采用外标法定量。结果表明,在优化的条件下,10种真菌毒素在各自的线性响应范围内线性关系良好,相关系数(r)均不小于0.9995,定量限(LOQ)为0.1~10μg/kg,在三个不同加标水平下平均回收率为61.9%~120.3%,相对标准偏差(RSD)为3.2%~16.1%。采用建立的方法对市面上销售的黑茶中的10种真菌毒素进行了筛查,数批产品检出真菌毒素。该方法简单、准确、可靠,可适用于发酵黑茶中多种真菌毒素的快速分析。
The fermented black tea such as aflatoxin B_1, aflatoxin B_2, aflatoxin G_1 (AFG_1), aflatoxin B (AFB_1), fermented black tea such as Yunnan Pu’er tea, Hunan black tea, Guangxi Liubao tea and Hubei old green tea were established. G_2, AFG_2, DON, 3-AcDON, ZEN and T-2 ), HT-2 toxin (OTA) and other 10 kinds of mycotoxins by simple, rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile / water (84 + 16), purified by QuEChERS, and separated by C18 column. Multiple reaction monitoring (MRM) mode was used for quantitative and qualitative analysis. The results showed that the 10 mycotoxins showed a good linear relationship in the linear response range under the optimized conditions with the correlation coefficients (r) of no less than 0.9995 and LOQ of 0.1 ~ 10μg / kg. The average recoveries at spiked levels ranged from 61.9% to 120.3% with relative standard deviations (RSDs) of 3.2% to 16.1%. Ten kinds of mycotoxins in the black tea sold on the market were screened by the established method, and mycotoxins were detected in several batches of products. The method is simple, accurate and reliable and can be applied to the rapid analysis of various mycotoxins in fermented black tea.