| 液相色谱-串联质谱法测定虾饲料中7种真菌毒素 |
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| 基金项目:广东省质量技术监督局科技项目（2016zz04）；国家自然科学基金面上项目（31371777，31871898） |
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| 中文摘要:建立了虾饲料中黄曲霉毒素B1(AFB1)、黄曲霉毒素M1(AFM1)、T-2毒素(T-2)、HT-2毒素(HT-2)、脱氧雪腐镰刀菌烯醇(DON)、赭曲霉毒素A(OTA)和玉米赤霉烯酮(ZEN)的液相色谱-串联质谱（LC-MS/MS）同时检测方法。样品中加入15 mL乙腈-水（体积比4∶1）和10 mL乙腈饱和正己烷，涡旋混匀，超声提取，MycoSpinTM400多毒素净化柱净化后上机测定。采用Hypersil Gold （150 mm×2.1 mm,5 μm）色谱柱进行分离，以甲醇-水（含0.03%氨水）为流动相梯度洗脱，在电喷雾电离模式下正、负离子同时扫描检测，基质匹配外标法定量。在优化条件下，7种真菌毒素的线性相关系数（r2）均大于0.991，检出限为1.83~12.63 μg/kg。在高、中、低3个加标水平下，各目标毒素的回收率为87.5%~116%，相对标准偏差为2.4%~18%。该法可为水产饲料中多种真菌毒素的同时检测提供参考。 |
| 中文关键词:真菌毒素 液相色谱-串联质谱（LC-MS/MS） 饲料 |
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| Determination of 7 Mycotoxins in Shrimp Feed by Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A liquid chromatography-tandem mass spectrometric（LC-MS/MS） method was developed for the quantitative determination of aflatoxin B1（AFB1）,aflatoxin M1（AFM1）,T-2 toxin（T-2）,HT-2 toxin（HT-2）,deoxynivalenol（DON）,ochratoxin A （OTA） and zearalenone（ZEN） in shrimp feed.Samples were extracted with 15 mL acetonitrile-water（4∶1,by volume）,and degreased with 10 mL acetonitrile saturated hexane.The extract was cleaned up with a MycoSpinTM400 multitoxin LC-MS/MS clean-up column.The target compounds were separated on an Hypersil Gold（150 mm×2.1 mm,5 μm）chromatographic column by gradient elution with methanol-water containing 0.03%ammonia as mobile phase,and analyzed simultaneously by electron spray ionization mass spectrometry in positive or negative ion mode,and quantified by the matrix-matched external standard method.Under the optimized conditions,there were good linearities for the analytes in corresponding concentration range with their correlation coefficients（r2） more than 0.991.The limits of detection（LOD）ranged from 1.83 μg/kg to 12.63 μg/kg.Average recoveries for the target mycotoxins at high,medium and low spiked levels ranged from 87.5%to 116%with relative standard deviations of 2.4%-18%.The developed method could provide a reference for the simultaneous determination of mycotoxins in aquatic feeds. |
| Key Words:mycotoxin liquid chromatography-tandem mass spectrometry（LC-MS/MS） feed |
| 引用本文：施琦，杨嘉丽,王雅玲，廖建萌，郑景娇，孙力军.液相色谱-串联质谱法测定虾饲料中7种真菌毒素[J].分析测试学报,2019,38(3):334-338. |
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