基于Myco净化柱建立快速测定饲料中真菌毒素的UPLC-MS/MS法
Establishment of a rapid UPLC-MS/MS method for determination of mycotoxins in feed based on Myco purification column
胡剑 1郑百芹 1谷守国 1丛倩倩 1裴小亮 1刘宇奇 1李梁 1张建雄1
作者信息
- 1. 唐山市食品药品综合检验检测中心,河北唐山 063000;农业农村部农产品品质评价与营养健康重点实验室,河北唐山 063000;河北省农产品质量安全检测技术创新中心,河北唐山 063000;唐山市功能性农产品产业技术研究院,河北唐山 063000
- 折叠
摘要
试验旨在建立一种便捷、快速的通用型快速净化柱作为前处理方法,通过优化提取、净化等步骤缩短前处理时间,对饲料中常见的真菌毒素进行快速定量分析.试验建立了基于碳骨架(MOFS)材料填充的Myco净化柱,快速测定饲料中7种真菌毒素的超高效液相色谱-质谱/质谱法(UPLC-MS/MS)方法.饲料样品经乙腈-水提取,涡旋振荡,经Myco净化柱上样净化,以5 mmol/L甲酸铵-甲醇为流动相,采用UPLC-MS/MS测定,外标法定量.结果显示,7种真菌毒素在0.5～50.0 μg/L范围内线性关系良好,相关系数(R2)＞0.99.方法检测限为0.5～2.0 μg/kg,定量限为2.0～5.0μg/kg.7种毒素在空白样品加标的低、中、高3个水平添加量下样品回收率为82.3％～96.8％,相对标准偏差在2.1％～9.3％.研究表明,基于Myco净化柱建立的UPLC-MS/MS法快速测定饲料中真菌毒素的试验方法处理简单,结果可靠,适合大部分饲料中7种真菌毒素的定量测定.
Abstract
The experiment aims to establish a convenient and rapid universal quick purification column as a pre-treatment method,shortening the pre-treatment time by optimizing steps such as extraction and purification,and conducting rapid quantitative analysis of common mycotoxins in feed.The experiment has established an UPLC-MS/MS method for the rapid determination of seven mycotoxins in feed based on the Myco purification column filled with MOFS materials.The feed sample is extracted with acetonitrile-water,vortexed,loaded and purified through the Myco purification column,with 5 mmol/L ammonium formate-methanol as the mobile phase,and quantified by the external standard method using UPLC-MS/MS.The results show that the seven mycotoxins have a good linear relationship in the range of 0.5～500 μg/L,with a correlation coefficient(R2)＞0.99.The method detection limit is 0.5～2.0 μg/kg,and the quantification limit is 2.0～5.0 μg/kg.The recovery rates of the seven toxins at low,medium,and high levels of spiking in blank samples are 82.3％～96.8％,with relative standard deviations of 2.1％～9.3％.The results indicate that the UPLC-MS/MS method established based on the Myco purification column for the rapid determination of mycotoxins in feed is simple to handle and reliable,suitable for the quantitative determination of the seven mycotoxins in most feeds.
关键词
UPLC-MS/MS/真菌毒素/饲料/快速测定Key words
UPLC-MS/MS/toxin/feed/rapid detection引用本文复制引用
基金项目
河北省现代农业产业技术体系奶牛创新团队三期建设项目()
河北省第四批高端人才项目()
院士合作重点单位项目()
河北省现代农业产业技术体系建设专项资金(HBCT2024280206)
出版年
2024
国家科技期刊平台
NSTL
万方数据