超高效液相色谱-质谱联用快速测定玉米及其产品中11种生物毒素  

Rapid determination of 11 biotoxins in maize and its products by ultra-performance liquid chromatography-mass spectrometry

作　　者：李彩虹 王永宏[2] 赵如浪[2] 张维军[2] 赵健[2] 刘霞 赵子丹 LI Caihong;WANG Yonghong;ZHAO Rulang;ZHANG Weijun;ZHAO Jian;LIU Xia;ZHAO Zidan(Institute of Quality Standard and Testing Technology for Agro-Products of Ningxia,Yinchuan 750002,China;The Crop Research Institute,Ningxia Academy of Agriculture and Forestry Science,Yinchuan 750002,China;Key Laboratory of Agricultural Product Quality Standard Research and Evaluation of Ningxia Hui Autonomous Region,Yinchuan 750002,China)

机构地区：[1]宁夏农产品质量标准与检测技术研究所,宁夏银川750002 [2]宁夏农林科学院农作物研究所,宁夏银川750002 [3]宁夏回族自治区农产品质量标准研究与评价重点实验室,宁夏银川750002

出　　处：《食品与发酵工业》2023年第9期304-309,共6页Food and Fermentation Industries

基　　金：宁夏农林科学院农业高质量发展和生态保护科技创新示范项目(NGSB-2021-3-02,NGSB-2021-5-05);宁夏农林科学院科技创新引导项目(NKYZZ-J-22-01)。

摘　　要：采用超高效液相色谱-三重四极杆质谱联用法,建立玉米籽粒中11种生物毒素的快速检测方法。样品用体积分数80%乙腈提取,HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,以体积分数0.1%甲酸甲醇-5 mmol/L乙酸铵体积分数0.1%甲酸水为流动相梯度洗脱,质谱采用电喷雾离子源(electrospray ionization,ESI),正、负离子模式下,多重反应监测(multiple reaction monitoring,MRM),外标法定量。11种生物毒素在一定的浓度范围内均具有良好的线性关系,相关系数r值均大于0.9995,定量限均小于0.001 mg/kg。在0.001~2.0 mg/kg添加水平下,每个添加水平做5个重复,平均回收率为72%~88%,相对标准偏差在0.8%~13.4%。该方法测定玉米籽粒中11种生物毒素定量准确,快速高效,具备较强实用性。To establish a rapid method for determining 11 mycotoxins in corn kernels using ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry.Samples were extracted with 80%acetonitrile,separated on an HSS T3 chromatographic column(2.1 mm×100 mm,1.8μm),and gradient eluted with 0.1%methanol containing formic acid-5 mmol/L ammonium acetate using 0.1%formic acid in water as mobile phase.Electrospray ionization(ESI),multiple reaction monitoring(MRM)in positive and negative ion modes and the external standard method were used for mass spectrometry.The 11 mycotoxins showed a good linear relationship in a certain concentration range,with the correlation coefficient r>0.9995,and the limit of quantitation<0.001 mg/kg.At the addition level of 0.001-2.0 mg/kg,each addition level was repeated for 5 times,revealing that the mean recovery was 72%-88%and the relative standard deviation was 0.8%-13.4%.This method is accurate,rapid and efficient for quantifying the 11 mycotoxins in corn kernels,with high practicability.

关 键 词：玉米 玉米产品 超高效液相色谱-质谱/质谱法 生物毒素 快速检测 

分 类 号：TS213.4[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]