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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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作者单位
施琦,杨嘉丽,王雅玲,廖建萌,郑景娇,孙力军 1.广东省湛江市质量计量监督检测所国家海产品质量监督检验中心(湛江)2.广东海洋大学食品科技学院广东省水产品加工与安全重点实验室广东普通高等学校水产品深加工重点实验室3.湛江市食品药品检验所 
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)
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
 
Determination of 7 Mycotoxins in Shrimp Feed by Liquid Chromatography-Tandem Mass Spectrometry
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,(3):334-338.
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