大米中16种真菌毒素同时检测分析

Simultaneous detection and analysis of 16 mycotoxins in rice

目的建立大米中黄曲霉毒素、伏马毒素、雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇类毒素、玉米赤霉烯酮、赭曲霉毒素A、T-2毒素、HT-2毒素以及杂色曲霉毒素等16种真菌毒素便捷准确的液相色谱-串联质谱法。方法大米样品经粉碎均质后采用70%甲醇水溶液浸泡提取,通过PriboFastRM226多功能净化柱净化,利用液相色谱串联质谱的多反应监测模式进行测定分析,采用内标法定量。结果 16种真菌毒素均具有良好的线性关系(r>0.99),3个加标水平回收率为85.2%~102.8%,相对标准偏差范围为2.05%~4.75%。在61件大米检测中,共有5件样品检出真菌毒素,检测到的真菌毒素有5种,其中雪腐镰刀菌烯醇、伏马毒素B1、伏马毒素B2、15-乙酰基脱氧雪腐镰刀菌烯醇各有1件样品检出,黄曲霉毒素B1有3件检出,检出率为8.33%,检出的5种真菌毒素含量在0.69~71.47μg/kg,均未超过国家食品安全标准规定的真菌毒素限量标准。结论大米中真菌毒素的检出率低,含量符合国家标准要求,该检测方法准确、可靠、便捷,可适用于大米中多种真菌毒素的检测。

Objective To establish a convenient and accurate method for the determination of 16 mycotoxins,including aflatoxin,fumonisin,nivalenol,deoxynivalenol,zearalenone,ochratoxin A,T-2 toxin,HT-2 toxin and sterigmatocystin by liquid chromatography-tandem mass spectrometry.Methods Rice samples were extracted by 70%methanol aqueous solution after homogenization,purified by PriboFastRM226 multifunctional purification column,determined and analyzed by multi-reaction monitoring mode of liquid chromatography-tandem mass spectrometry,and quantified by internal standard method.Results The regression equations of 16 mycotoxins had good linear relationships(r>0.99).The recoveries of the 3 spiked levels ranged from 85.2%to 102.8%,and the relative standard deviations ranged from 2.05%to 4.75%.In tests of 61 rice samples,5 samples were found to detect mycotoxins,and 5 species of mycotoxins were detected.Among them,nivalenol,fumonisin B1,fumonisin B2,15-acetyl deoxynivalenol were detected in one sample,and aflatoxin B1 was detected in 3 samples.The detection rate was 8.33%,and the five mycotoxins were detected in the range of 0.69-71.47μg/kg,which did not exceed the limit of mycotoxin limit specified by the national food safety standards.Conclusion The detection rates of mycotoxins in rice are low,and the contents meet the requirements of national standards.The detection method is accurate,reliable and convenient,and can be applied to the detection of multiple mycotoxins in rice.