超高效液相色谱串联质谱法快速检测柑橘中的5种链格孢霉毒素  

Rapid Determination of Five Alternaria Mycotoxins in Citrus by Ultra-high Performance Liquid ChromatographyTandem Mass Spectrometry

作　　者：蒋黎艳 赵其阳[2,4] 龚蕾[2,4] 刘雁雨[2,4] 张耀海[2,4] 马良[1,2] 焦必宁[1,2,3,4] 

机构地区：[1]西南大学食品科学学院,重庆400715 [2]农业部柑桔产品质量安全风险评估实验室(重庆),西南大学柑桔研究所,重庆400712 [3]国家柑桔工程技术研究中心,重庆400712 [4]农业部柑桔及苗木质量监督检验测试中心,重庆400712

出　　处：《分析化学》2015年第12期1851-1858,共8页Chinese Journal of Analytical Chemistry

基　　金：国家重点基础研究发展计划(973计划)项目(No.2013CB127803);国家自然科学基金项目(No.31301476);农业部现代农业(柑桔)产业技术体系建设专项(CARS-27);2015年国家农产品质量安全风险评估重大专项(GJFP2015004);中央高校基本科研业务费专项(XDJK2013B035)资助项目

摘　　要：建立了超高效液相色谱-串联质谱法快速检测柑橘中腾毒素、链格孢酚、交链格孢酚单甲醚、交链孢烯和细交链格孢菌酮酸5种链格孢霉毒素的新方法。样品经改进的QuEChERS(快速、简单、廉价、高效、灵活和安全)方法一步完成萃取净化,采用乙腈-甲酸(1.5%)提取,无水MgSO_4和NaCl盐析,以ACQUITY UPLC BEH C_(18)柱为分离柱,用乙腈和0.1%甲酸溶液进行梯度洗脱,电喷雾正离子(ESI^+)多反应模式监测,超高效液相色谱-串联质谱(UPLC-MS/MS)测定。在本方法条件下,5种链格孢霉毒素在2.0-100μg/L浓度范围内均呈现良好的线性关系(R^2>0.9922),检出限在0.11-0.91μg/kg之间。在5.20和100μg/kg加标水平下,5种毒素的回收率在71%-112%之间,相对标准偏差为1.1%-9.9%,能满足柑橘中链格孢霉毒素检测的要求。A novel method was developed for the rapid determination of five alternaria mycotoxins,alternariol,alternariol monomethyl ether,altenuene,tentoxin and tenuazonic acid,in citrus using ultra-high performance liquid chromatography-tandem mass spectrometry.The sample was prepared using the modified QuEChERS（quick,easy,cheap,effective,rigged,and safe） method to complete the extraction and cleanup steps in one procedure.In this QuEChERS method,sample was extracted with acetonitrile（1.5% formic acid）,then salted out with anhydrous MgSO4 and NaCl,separated on an ACQUITY UPLC BEH C_（18） with gradient elution by using acetonitrile and 0.1% formic acid aqueous as eluant,and detected by UPLC-MS /MS under negative（ESI~＋） electrospray ionization and MRM models.Under these conditions,five alternaria mycotoxins made a good linearity in the concentration range of 2.0- 100 μg/L with R^20.9922,and the limits of detection of the instrument were in the range of 0.11-0.91 μg/kg.Three spiked levels of five altenaria mycotoxins at 5,20 and 100 μg/kg were investigated,and the recoveries ranged from 71% to 112% with the relative standard deviations（RSDs） varying from 1.1% to 9.9%,which met the requirement of mycotoxins determination.

关 键 词：链格孢霉毒素 超高效液相色谱-串联质谱法 柑橘 QuEChERS法 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]