花生及其制品中16种真菌毒素的超高效液相色谱串联质谱测定法  

Rapid determination of 16 mycotoxins in peanut and its products by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：李俊玲[1] 王冬梅[1] 张宇 王书舟[1] LI Jun-ling;WANG Dong-mei;ZHANG Yu;WANG Shu-zhou(Anyang Center for Disease Control and Prevention,Anyang,Henan 455000,China)

机构地区：[1]安阳市疾病预防控制中心,河南455000

出　　处：《现代预防医学》2022年第19期3590-3597,共8页Modern Preventive Medicine

基　　金：安阳市科技攻关项目(2018-78)。

摘　　要：目的建立花生及其制品中16种真菌毒素包括黄曲霉毒素(AF)、伏马菌素(FB)、赭曲霉毒素A(OTA)等的超高效液相色谱串联质谱测定法。方法样品经研磨粉碎后酸性乙腈溶液提取,10000r/min离心后用水稀释,再经2℃低温10000r/min离心后加入同位素内标,多反应离子监测模式(MRM)检测,内标法定量。结果16种待测物线性关系良好,相关系数均大于0.9900,方法定量限为0.3μg/kg~45.0μg/kg,加标回收率在72.7%~126.3%之间,相对标准偏差为1.3%~5.0%。采用优化后方法对60份花生及其制品包括花生油、花生酱、生花生和熟花生进行检测,AFB_(1)、AFB_(2)和AFG_(1)的总检出率分别为35%(21/60)、18.3%(11/60)、5.0%(3/60),含量范围分别为0.1μg/kg~57.5μg/kg,0.1μg/kg~18.4μg/kg,0.1μg/kg~3.3μg/kg。结论该法前处理快速、简捷、灵敏度高、准确度好,适合于花生及其制品中16种真菌毒素快速检测。Objective To establish a method for the determination of 16 mycotoxins in peanut and its products,including aflatoxin(AF),fumonisins(FB),ochratoxin A(OTA)by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC).Methods The samples were extracted with acidic acetonitrile solution after grinding,then diluted with water after centrifugation at 10000r/min.After centrifugation at 2℃10000r/min,internal standards were added in the sample solution,and detected by multiple reaction ion monitoring mode(MRM),and quantified by internal standard method.Results The correlation coefficients(r)of 16 species were all greater than 0.9900.The limits of quantitation were 0.3μg/kg-45.0μg/kg.The recoveries were in the range of 72.7%-126.3%with RSDS of 1.3%-5.0%.Sixty peanuts and their products,including peanut oil,peanut butter,raw peanuts and cooked peanuts,were detected by the optimized method.The total detection rates of AFB_(1),AFB_(2) and AFG_(1) were 35%(21/60),18.3%(11/60)and 5.0%(3/60)respectively.The contents of 16 mycotoxins were 0.1μg/kg-57.5μg/kg,0.1μg/kg-18.4μg/kg,0.1μg/kg-3.3μg/kg.Conclusion The method is rapid,simple,sensitive and accurate for the rapid detection of 16 mycotoxins in peanut and its products.

关 键 词：花生及其制品 真菌毒素 超高效液相色谱串联质谱法 

分 类 号：R379[医药卫生—病原生物学]