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B1（AFB1）、黄曲霉毒素B2（AFB2）、黄曲霉毒素G1（AFG1）、黄曲霉毒素G2（AFG2）、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0.1~10 μg/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。

A method was established for the determination of ten mycotoxins (aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1), aflatoxin G2 (AFG2), deoxynivalenol (DON), 3-acetyldeoxynivalenol (3-AcDON), zearalenone (ZEN), T-2 mycotoxin (T-2), HT-2 toxin (HT-2), and ochratoxin A (OTA)) in fermented dark tea (Pu'er tea, Hunan dark tea, Guangxi Liupu tea, and Hubei old green tea) using (QuEChERS) ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with acetonitrile-water (84:16, V/V), and the extracted solutions were purified using the QuEChERS approach. The mycotoxins were then separated on an Agilent Zorbax Rrhd SB-C18 column (2.1 mm×100 mm, 1.8 μm) using (0.1% formic acid-5 mM ammonium acetate-water)/methanol as the mobile phase and detected by MS/MS under multiple reaction monitoring (MRM) mode. The mass spectrometry measurement was conducted using positive (ESI+) and negative (ESI-) electrospray ionization with an external standard. The results showed that ten mycotoxins had a good linear relationship within their own linear response ranges, with correlation coefficients (r) all >0.9995. The limits of quantitation (LOQ) (S/N≥10) were 0.1~1.0 μg/kg, and the average recoveries at three spike levels of ten mycotoxins ranged from 61.9% to 120.3%, with a relative standard deviation (RSD, n=3) of 3.2%~16.1%. This newly developed method was successfully applied for the assessment of 61 commercial black tea samples, and mycotoxins were detected in several batches of samples. Based on these results, the developed method is reliable, simple, and accurate, and is suitable for the rapid analysis of multiple mycotoxin contaminants in fermented dark tea.

广东省高等学校优秀青年教师培养计划资助项目（Yq2013196）；国家质检总局科技计划项目（2014QK051）；广东省食药局科技计划项目（2015ZX07）；中山市科技计划项目（2014A2FC247、2015B2297）