[1]张海霞,杨静,刘畅,等.QuEChERS-超高效液相色谱-串联质谱法快速检测玉米中7种真菌毒素[J].黑龙江农业科学,2017,(07):61-65.[doi:10.11942/j.issn1002-2767.2017.07.0061]
　ZHANG Hai-xia,YANG Jing,LIU Chang,et al.Rapid Detection of Seven Mycotoxins in Maize by QuEChERS with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].HEILONGJIANG AGRICULTURAL SCIENCES,2017,(07):61-65.[doi:10.11942/j.issn1002-2767.2017.07.0061]
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QuEChERS-超高效液相色谱-串联质谱法快速检测玉米中7种真菌毒素

《黑龙江农业科学》[ISSN:1002-2767/CN:23-1204/S] 卷: 期数: 2017年07期 页码: 61-65 栏目: 出版日期: 2017-07-10
Title:
Rapid Detection of Seven Mycotoxins in Maize by QuEChERS with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
文章编号:
1002-2767（2017）07-0061-05
作者:
张海霞; 杨静; 刘畅; 刘志鹏
哈尔滨市农产品质量安全检验检测中心，黑龙江 哈尔滨 150070
Author(s):
ZHANG Hai-xia; YANG Jing; LIU Chang; LIU Zhi-peng
Harbin Examing and Inspection Center for Agricultural Products Safety and Quality,Harbin,Heilognjiang 150070
关键词:
QuEChERS; 超高效液相色谱-串联质谱; 玉米; 真菌毒素
Keywords:
QuEChERS;  ultra-high performance liquid chromatography-tandem mass spectrometry;  maize;  mycotoxins
分类号:
O657.63;TS210.7
DOI:
10.11942/j.issn1002-2767.2017.07.0061
文献标志码:
A
摘要:
建立了QuEChERS结合超高效液相色谱-串联质谱(UPLC-MS/MS)对玉米中的真菌毒素进行检测的方法。样品用20 mL乙腈∶水∶甲酸（50∶49∶1）震荡提取，离心后取上清液4 mL经无水硫酸镁、PSA、C18分散固相萃取净化，离心，取2 mL净化液氮吹至近干。残渣用流动相溶解，以Waters BEH C18色谱柱分离，采用多反应检测模式进行检测，外标法定量。根据各个化合物的响应值和限量标准，选择3个不同水平添加浓度，回收率在89.7%～112.9%，相对标准偏差小于8.7%。7种真菌毒素在0.5～1 200.0 μg?kg-1时相关系数均大于0.99。方法的定性限为0.06～10.00 μg?kg-1,定量限为0.30～32.00 μg?kg-1。表明，该方法具有提取效率高，净化效果好，回收率高，准确灵敏等优点，适用于玉米中7种真菌毒素的快速检测。
Abstract:
A method for detection of mycotoxins in maize was established using the ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Samples were extracted with 20 mL of acetonitrile∶water∶formic acid (50∶49∶1) .The 4 mL upper cleaning fluid obtained from centrifuge was purified with anhydrous magnesium sulfate,PSA and C18.Once again centrifuge,2 mL purifying fluid was blown by nitrogen.The residue was dissolved by flow phase,separated by the Waters BEH C18 column,and the multi-reaction detection mode was used for detection with super area-external standard method.According to the response value and the limited standard of each compound,the concentration of 3 different levels was selected.The recovery rate was between 89.7%~112.9% and the relative standard deviation was less than 8.7%.The correlation coefficients of 7 mycotoxins were greater than 0.99 in the range of 0.5~1 200.0 μg?kg-1.The qualitative limit of the method was 0.06~10.00 μg?kg-1,and the quantitative limit was 0.3~32.0 μg?kg-1.The results showed that the method had high efficiency,good purification effect,high recovery rate and accurate sensitivity,which was suitable for rapid detection of 7 kinds of mycotoxins in maize.

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备注/Memo

收稿日期：2017-05-30

基金项目：哈尔滨市科技攻关计划资助项目（2016AB3BS063）
第一作者简介：张海霞（1980-），女，黑龙江省大庆市人，硕士，高级农艺师，从事药残检测研究。E-mail: xdsun65@yahoo.com。

更新日期/Last Update: 2017-09-19