摘要
采用真菌毒素多功能净化柱(Mycotoxin multifunctional purification column,MFC)对样品进行前处理,建立了高效液相色谱-串联质谱法测定油菜籽和亚麻籽中16种真菌毒素及其代谢产物的检测方法。以50%乙腈水溶液对样品中目标物进行震荡提取,经MycoSpin TM 400多功能净化柱净化处理,采用EclipsePlus C18色谱柱分离,11种毒素采用电喷雾多反应离子监测正模式分析,5种毒素采用负模式分析,同位素内标法定量。16种真菌毒素在各自浓度范围内线性关系良好(R 2>0.988),在二种基质中进行3个水平添加实验(n=6),回收率为65.0%~97.3%,相对标准偏差为5.1%~10.9%,方法检出限为0.2~11.5μg/kg,定量限为0.5~30.0μg/kg。本方法操作简单、准确性和灵敏度高,可用于油菜籽和亚麻籽中16种真菌毒素残留的检测分析。
The samples were treated with mycotoxin multifunctional purification column to establish an analytical method for simultaneous determination of 16 mycotoxins and their metabolites in rapeseed and flaxseed by high performance liquid chromatography-tandem mass spectrometry.50%acetonitrile in water was selected as extraction solvent to extract sample via shaking and treated with MycoSpin TM 400 multifunctional purification column,and then filtrated.11 mycotoxins were separated by EclipsePlus C18 chromatographic column and analyzed by electrospray reaction positive mode.5 mycotoxins were analyzed by electrospray reaction negative mode,and quantitated by isotope internal stand method.Good linear relationships of 16 kinds of mycotoxins in rapeseed and flaxseed were obtained in respective linear ranges,their correlation coefficients(R 2)were all greater than 0.988 and recoveries of 16 kinds of mycotoxins in rapeseed and flaxseed at 3 spiked levels were ranged from 65.0%to 97.3%,with precisions in a range of 5.1%~10.9%.The limits of detection are ranged from 0.2 to 11.5μg/kg,and the limits of quantification were ranged from 0.5 to 30.0μg/kg in different matrices,respectively.This method is simple to operate,of high accuracy and sensitivity,which is instantly available for the needs of quantitative analysis of 16 mycotoxins in rapeseed and flaxseed.
作者
孙利东
王震
刘贺
鲁婷婷
娄婷婷
SUN Li-dong;WANG Zhen;LIU He;LU Ting-ting;LOU Ting-ting(Technology Center of Manzhouli Customs,Manzhouli 021400,China;Animal,Plant and Foodstuffs Inspection Center of Tianjin Customs,Tianjin 300461,China)
出处
《化学试剂》
CAS
北大核心
2023年第4期136-143,共8页
Chemical Reagents
基金
海关总署科研项目(2020HK204)。
关键词
真菌毒素
多功能净化柱
高效液相色谱串联质谱法
油菜籽
亚麻籽
mycotoxins
multifunctional purification column
high performance liquid chromatography-tandem mass spectrometry
rapeseed
flaxseed
作者简介
孙利东(1983-),女,满族,内蒙古满洲里人,硕士,工程师,主要研究方向为食品安全检测。;通讯作者:娄婷婷,E-mail:loutingtinggucas@126.com。
