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建立了同步测定水产品中黄曲霉毒素B1(AFB1)、黄曲霉毒素B2(AFB2)、黄曲霉毒素G1(AFG1)、黄曲霉毒素G2(AFG2)、黄曲霉毒素M1(AFM1)、赭曲霉毒素A(OTA)、玉米赤霉烯酮(ZEN)、脱氧雪腐镰刀菌烯醇(DON)、3-乙酰基脱氧雪腐镰刀菌烯醇(3-Ac DON)、15-乙酰基脱氧雪腐镰刀菌烯醇(15-Ac DON)、镰刀菌烯酮(Fus-X)等11种真菌毒素的超高效液相色谱-串联质谱分析方法。试样样品以乙腈/水溶液(84+16)提取,Myco Spin 400多功能柱净化,Waters ACQUITY UPLCTM BEH C18柱分离,多反应监测(MRM)模式进行定量与定性分析,外标法定量。结果表明,11种目标物在各自的线性响应范围内线性关系良好,相关系数(r)≥0.9918,定量限(LOQ)为0.1~20.0μg/kg,加标平均回收率(n=3)为62.8%~115.3%,相对标准偏差(RSD)为2.6%~19.0%。该方法前处理简单、净化效果好、灵敏度高、重现性好,适合于水产品中痕量真菌毒素的多残留快速检测。
The simultaneous determination of aflatoxin B1 (AFB1), afB2 (AFB2), aflatoxin G1 (AFG1), aflatoxin G2 (AFG2), aflatoxin M1 (AFM1), ochratoxin A (OTA), zearalenone (ZEN), deoxynivalenol (DON), 3-Ac deoxynivalenol (3-Ac DON), 15-acetyl deoxynivalenol 11 mycotoxins such as Fusobacterium, Xanthomonas, Fusarium, Xanthomonas oryzae were studied by ultra performance liquid chromatography-tandem mass spectrometry. Sample samples were extracted with acetonitrile / water (84 + 16), purified with Myco Spin 400 multi-functional column, separated by Waters ACQUITY UPLC BEH C18 column, and analyzed by multiple reaction monitoring (MRM) mode. The results showed that there was a good linear relationship between the 11 targets in their respective linear response ranges. The correlation coefficient (r) ≥0.9918, the limit of quantification (LOQ) ranged from 0.1 to 20.0 μg / kg, and the spiked average recovery (n = 3) 62.8% ~ 115.3%, and the relative standard deviation (RSD) was 2.6% ~ 19.0%. The method has the advantages of simple pretreatment, good purification effect, high sensitivity and good reproducibility, and is suitable for the rapid detection of trace residues of mycotoxins in aquatic products.