饲料中16种霉菌毒素液相色谱-三重四级杆/线性离子阱串联质谱法的条件优化  

Optimizing conditions for determination of mycotoxins in feeds by UPLC-Quadrupole/Orbitrap High resolution Mass Spectrometry

作　　者：符金华 杨琳芬 董泽民 徐国茂 姜文娟 邢磊 黄艳清 李瑾瑾 周仁丹 叶金[3] 吴宇[3] 廖丰 

机构地区：[1]江西省兽药饲料监察所,江西南昌330029 [2]南昌大学分析测试中心,江西南昌330047 [3]国家粮食局科学研究院,北京西城100037 [4]双胞胎(集团)股份有限公司,江西南昌330096

出　　处：《中国饲料》2017年第21期25-30,共6页China Feed

基　　金：江西省重点研发计划项目(20161BBF60115)

摘　　要：本文优化并建立了饲料中16种霉菌毒素的多残留提取、净化及液相色谱-三重四级杆/线性离子阱串联质谱(Qtrap-LC-MS/MS)的检测方法。样品经20 m L乙腈/水/乙酸(V∶V∶V,70∶29∶1)溶液提取、稀释和上机检测。采用0.1%甲酸的1 mmol/L NH4Ac的水相作为弱洗脱流动相梯度洗脱程序,离子源温度为500℃,采用分段MRM扫描模式,100ms的驻留时间,16种霉菌毒素分离理想、基线平稳、选择离子信号强度高、干扰离子信号弱;同时,得到了与理论计算值非常接近的所有选择离子精确质量数。完成了16种毒素的Qtrap-LC-MS/MS方法条件优化,成功的实现饲料中16种霉菌毒素的快速定性、定量分析。The residue extraction,purification and liquid chromatography-triple level 4 bar/linear ion trap tandem mass spectrometry（Qtrap-LC-MS/MS） detection method of 16 kinds of mycotoxins in feed were optimized and established in this paper.Mycotoxins were extracted by 20 m L of acetonitrile/water/acetic acid（V∶V∶V,70∶29∶1） solution,diluted and detected.The gradient elution procedure was used with 0.1% formic acid and 1 mmol/L NH4 Ac as weak elution mobile phase.The ion source temperature was 500 ℃ and dwell time was 100 ms,using segmented MRM scan mode.Mycotoxins were well separated with smooth baseline,high select ion signal intensity and the weak signal interference.All select ion mass numbers of mycotoxins were also obtained,which was very close to the theoretical calculation value.The optimization conditions for Qtrap-LC-MS/MS method of mycotoxins were found.It realized both qualitative and quantitative analysis of16 kinds of mycotoxins in feed.

关 键 词：霉菌毒素 液相色谱-三重四级杆/线性离子阱串联质谱法 同位素内标 优化 

分 类 号：S816.17[农业科学—饲料科学]