饲料和饲料原料等25种样品中16种真菌毒素超高效液相色谱-三重四级杆/线性离子阱串联质谱法基质效应的研究  

The matrix effect research of determination of 16 mycotoxins by UPLC-Quadrupole/Qtrap mass spectrometry in 25 kinds of feed and feedstuff samples

作　　者：符金华 杨琳芬 董泽民 徐国茂 姜文娟 叶金[2] 吴宇[2] 邢磊 刘国花 樊晶 周仁丹 廖丰 FU Jinhua;YANG Linfen;DONG Zemin;XU Guomao;JIANG Wenjuan;YE Jin;WU Yu;XING Lei;LIU Guohua;FAN Jing;ZHOU Rendan;LIAO Feng(Jiangxi Institute of Veterinary and Feed Control,Nanchang,Jiangxi Province 330029,China;Academy of State Administration of Grain,Beijing 100037,China;Analysis and testing center of NanChang University,Nanchang,Jiangxi Province 330047,China;Twins(group)co.,LTD.,Nanchang,Jiangxi Province 330096,China)

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

出　　处：《中国饲料》2019年第21期66-71,共6页China Feed

基　　金：江西省重点研发计划项目(20161BBF60115)

摘　　要：利用已建立的饲料及饲料原料中16种真菌毒素多残留提取、净化及液相色谱-三重四级杆/线性离子阱串联质谱(Qtrap-UPLC-MS/MS)检测方法及同位素稀释技术,探究常见的5大类配合饲料(鱼、猪、鸭、鸡和牛)和5种饲料原料(豆粕、鱼粉、菜籽粕、菜粕及DDGS)等25种样品的基质效应。结果表明:16种真菌毒素在鱼饲料中的基质效应为48.6%~145.4%,在猪饲料中绝大部分毒素的基质效应为41.8%~146.4%,在鸭饲料中的基质效应为43.2%~148.1%,在不同种类鸡饲料中的基质效应为42.1%~148.3%,在犊牛饲料中的基质效应为50.3%~140.8%,5大类饲料中均存在不同程度的基质增强或抑制效应。在5种常见饲料原料中的基质效应为30.7%~148.6%,豆粕和鱼粉的基质效应较弱,其他三种原料的基质效应严重,且16种真菌毒素的基质效应基本上呈现一致规律性变化。采用稳定同位素稀释技术对基质效应产生的影响进行校正与消除;定量结果表明,在一定的线性范围内,16种真菌毒素线性关系良好,相关系数良好,高、中、低3个浓度添加水平的回收率和RSD均符合相关法规的检测要求,说明本研究能提高饲料及饲料原料中真菌毒素检测结果的准确度与精密度。Qtrap-UPLC-MS/MS and stable isotope dilution technique were used to explore the matrix effect of the determination of 16 mycotoxins in common 5 kinds of feed(fish,pig,duck,chicken and cow)and 5 kinds of feedstuff(soybean meal,fish meal,meal,rapeseed meal and DDGS)samples.The results showed that the matrix effects in the fish feed was 48.6%~145.4%,41.8%~146.4%for the pig feed,43.2%~148.1%for the duck feed,42.1%~148.3%for chicken feed and 50.3%~140.8%for the calf feed.The matrix effect was 30.7%~148.6%in the five kinds of common feedstuffs and matrix effects of 16 kinds of mycotoxins present regular change consistent basically.The stable isotope dilution technique was used to correct and eliminate the impact of the matrix effect.Quantitative results showed that under certain linear range,16 kinds of mycotoxins linear relationship was good,the good correlation coefficient,high,medium and low add three concentration levels of the detection requirements for recovery and RSD were in accordance with relevant laws and regulations.The study provided a scientific reference for improving the accuracy and precision of the 16 kinds of mycotoxins detection result in feed and feedstuffs.

关 键 词：真菌毒素 超高效液相色谱-三重四级杆/线性离子阱串联质谱法 同位素稀释 基质效应 

分 类 号：S816.17[农业科学—饲料科学]