摘要
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。
A simple and novel sample pretreatment method for determination of eight kinds of mycotoxin in juice samples has been developed using acid-assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography-tandem mass spectrometry.The factors effecting extraction efficiency were investigated including the type and volume of extraction solvent,the volume of dispersive solvent and pH of the equilibrium system.Under the optimum extraction conditions including 60μL of trichloroaniline as extraction solvent,1500μL of hydrochloric acid solution as dispersive solvent and pH 5 as the acidity of equilibrium system,the method showed a good linearity for these mycotoxins within the concentration range from 1 to 500μg/L with correlation coefficients higher than 0.994.The detection limits were 0.15-17.71ng/L,0.09-7.08ng/L and 0.40-14.29ng/L in fruit juice of mango,pineapple and dragon,respectively.The average recoveries of eight kinds of mycotoxins ranged from 75.6% to 110.0% at three spiked concentrations of 0.2μg/L,1.0μg/L and 10.0μg/L,with the relative standard deviation of lower than 15.5%.The proposed method is simple,fast with less consumption of organic solvent,and has high sensitivity and repeatability,which is suitable for the detection of mycotoxins residues in fruit juice.
作者
韩艺烨
邓年
谢建军
刘承兰
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)
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2019年第3期455-462,共8页
Chinese Journal of Analytical Chemistry
基金
广东省省级科技项目(No.2016A040403102)资助~~
关键词
酸辅助-分散液液微萃取
高效液相色谱-串联质谱法
真菌毒素
果汁
Acid-assisted dispersive liquid-liquid microextraction
High performance liquid chromatography-tandem mass spectrometry
Mycotoxins
Juice
