超高效液相色谱-质谱联用法检测青贮玉米中9种真菌毒素

Determination of nine mycotoxins in corn silage by UPLC-MS/MS

为了建立超高效液相色谱-串联质谱检测青贮玉米中黄曲霉毒素B_1(AFB_1)、B_2(AFB_2)、G1(AFG1)、G2(AFG2)、T-2毒素、HT-2毒素、脱氧雪腐镰刀烯醇(DON)、玉米赤霉烯酮(ZEN)、赭曲霉毒素A(OTA)的分析方法,样品采用乙腈提取,C18为分散净化剂的QuEChERS净化柱净化,超高效液相色谱分离,多反应离子监测模式检测,外标法定量。结果显示:青贮玉米中9种真菌毒素的线性关系良好,9种毒素的平均添加回收率为71.86%~110.00%之间,相对标准偏差为0.09%~8.94%。方法检出限(LOD)在0.05~7.5μg/kg之间,定量限(LOQ)在0.18~25μg/kg之间。该方法快速灵敏,准确可靠,适用于青贮玉米中9种真菌毒素的检测。

A method was established to determine aflatoxin B_1（AFB_1）,aflatoxin B_2（AFB_2）,aflatoxin G1（AFG1）,aflatoxin G2（AFG2）,T-2 toxin,HT-2 toxin,Deoxynivalenol（DON）,Zearalmone（ZEN）and ochratoxins A（OTA）in corn silage by UPLC-MS/MS.Homogenized samples were extracted with acetonitrile,cleaned up by QuEChERS cartridge with C18 as sorbent for cleaning up.Chromatographic separation was achieved by UPLC and the determination was performed by tandem mass spectrometry under the mode of multiple reaction monitoring,the quantification analysis of external standard calibration curves was used.There were good linear correlations between the concentrations of the nine mycotoxins in corn silage.The recoveries of 9 kinds of toxins were in range of 71.86%—110.00% with the relative standard deviations（RSDs）of 0.09%—8.94%.The detection limit（LOD）and the limit of quantification（LOQ）were in range of 0.05—7.5μg/kg and 0.18~25μg/L,respectively.This method is rapid,sensitive,accurate and reliable,and it is suitable for the detection of 9 kinds of toxins in corn silage.