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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

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【作者】 蒋黎艳赵其阳龚蕾刘雁雨张耀海马良焦必宁

【Author】 JIANG Li-Yan;ZHAO Qi-Yang;GONG Lei;LIU Yan-Yu;ZHANG Yao-Hai;MA Liang;JIAO Bi-Ning;College of Food Science,Southwest University;Citrus Research Institute,Southwest University/Laboratory of Citrus Quality and Safety Risk Assessment,Ministry of Agriculture;Supervision and Testing Centre for Citrus and Seedling Quality,Ministry of Agriculture;National Center for Citrus Engineering;

【机构】 西南大学食品科学学院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农业部柑桔及苗木质量监督检验测试中心国家柑桔工程技术研究中心

【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MgSO4和NaCl盐析,以ACQUITY UPLC BEH C18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(R2>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。

【Abstract】 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 C18 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 R2>0.9922,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.

【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
  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2015年12期
  • 【分类号】O657.63;TS255.7
  • 【被引频次】44
  • 【下载频次】809
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