酸辅助分散液液微萃取-高效液相色谱-串联质谱法测定果汁中多种真菌毒素

建立了酸辅助分散液液微萃取结合高效液相色谱-串联质谱法检测果汁中黄曲霉毒素B_1(AflatoxinB_1,AFB_1)、黄曲霉毒素B_2(Aflatoxin B_2,AFB_2)、黄曲霉毒素G_1(Aflatoxin G_1,AFG_1)、黄曲霉毒素G_2(Aflatoxin G_2,AFG_2)、赭曲霉毒素(Ochratoxin A,OTA)、桔霉素(Citrinin,CIT)、链格孢霉酚(Alternariol,AOH)和链格孢甲醚(Alternariol monomethyl Ether,AME)共8种真菌毒素的分析方法。考察了萃取剂的种类以及用量、分散剂用量、平衡体系pH值对萃取效率的影响,获得了最佳的分散液液微萃取(Dispersive liquid-liquid microextraction,DLLME)条件:萃取剂为三氯苯胺,用量为60μL;分散剂为HCl溶液,用量为1500μL;平衡体系pH=5。结果表明,8种真菌毒素在1～500μg/L范围内呈良好的线性关系,相关系数>0.994;在芒果、菠萝和火龙果果汁中的检出限分别为0.15～17.71 ng/L、0.09～7.08 ng/L和0.40～14.29 ng/L;当添加浓度为0.2、1.0和10.0μg/L时,回收率在75.6%～110.0%之间,相对标准偏差<15.5%。本方法简单、快速,有机溶剂用量少,灵敏度高,重现性好,可用于果汁中多种痕量真菌毒素的检测。

Acid-assisted Dispersive Liquid-Liquid MicroextractionHigh Performance Liquid ChromatographyTandem Mass Spectrometry for Determination of Mycotoxins in Fruit Juice

HAN Yi-Ye;DENG Nian;XIE Jian-Jun;LIU Cheng-Lan(Key Laboratory of Natural Pesticide and Chemical Biology,Ministry of Education/Key Laboratory of Bio-pesticide Innovation and Application of Guangdong Province/College of Agriculture,South China Agricultural University,Guangzhou 510642,China;Guangdong Entry-Exit Inspection and Quarantine Technology Center,Guangzhou 510623,China)