液质联用法对饲料中真菌毒素的检测方法研究  

Simultaneous Determination of Mycotoxins in Feed by Liquid Chromatography-Tandem Mass Spectrometric

作　　者：周秀莹 上官国莲 黎小鹏 林小贞 曾建勇 何丽红 贾晓菲 林簇 Zhou Xiuying;Shangguan Guolian;Li Xiaopeng;Lin Xiaozhen;Zeng Jianyong;He Lihong;Jia Xiaofei;Lin Cu(Zhongshan Quality Safety&Inspection Institute of Agricultural Products,Zhongshan 528400,Guangdong,China;Foshan University,Foshan 528231,Guangdong,China)

机构地区：[1]中山市农产品质量安全检验所,广东中山528400 [2]佛山大学,广东佛山528231

出　　处：《绿色科技》2025年第2期159-167,共9页Journal of Green Science and Technology

基　　金：中山市社会公益科技研究项目(编号:2023B2054)。

摘　　要：建立一种饲料中真菌毒素高通量检测方法,使用含水酸化乙腈提取、通过式小柱的净化,配合液相色谱-串联质谱仪(6495 Triple Quadrupole LC/MS System)检测37种真菌毒素及其相关化合物。样品加入含有水和甲酸的乙腈(乙腈∶水∶甲酸V∶V∶V=840∶159∶1),摇床振荡提取30 min,离心分层,上清液过PRiME HLB固相萃取小柱净化,待测。液质联用仪采用甲酸-甲酸铵水溶液(A)和甲醇溶液(B)作为流动相进行梯度洗脱,质谱(ESI离子源)采用多离子动态检测模式(dMRM)对37种真菌毒素的定量离子和定性离子进行监测。结果表明:在12 min内完成37种目标化合物的分离和定量分析。37种真菌毒素在4、8、40μg/kg(B组40、80、400μg/kg,C组200、400、2000μg/kg)添加水平的回收率为:83%~110%,相对标准偏差:1.25%~16.23%,相对标准偏差小于20.0%(n=6),方法检出限在0.05~52μg/kg。该方法快速、准确、灵敏,适合测定饲料中真菌毒素残留量。This paper aims to determination of 37 mycotoxins in feed by liquid chromatography-tandem mass spectrometric(6495 Triple Quadrupole LC/MS System)and with identical pretreatment.Feed samples were extracted with extraction solution(acetonitrile,water and formic acid V∶V∶V=840∶159∶1),shake for 30 minutes,separated by centrifuging and cleaned up by PRiME HLB SPE.And then the 37 mycotoxins were separated on a reversed phase using a gradient elution program of formic acid aqueous solution(A)and methanol solution(B).LC–MS/MS(ESI)was used to detect the quantitative and qualitative ions of 37 mycotoxins using multiple reactions monitoring(dMRM).The results show that the 37 target compounds were completely separated and quantified within 12 minutes.The recoveries were ranged from 83%to 110%for the 37 mycotoxins residues with 3 spiked levels of 4,8 and 40μg/kg(group B 40,80 and 400μg/kg;group C 200,400 and 2000μg/kg).The relative standard deviations(RSDs)were 1.25%to 16.23%,less than 20%(n=6),and the limits of detection(LOD)for the 37 kinds of mycotoxins were 0.05 to 52μg/kg.The proposed method is fast,accurate and sensitive,which is suitable for detecting 37 mycotoxins in feed.

关 键 词：饲料 液相色谱-串联质谱法 真菌毒素残留 

分 类 号：S831.5[农业科学—畜牧学]