•  
  •  
  •  
  •  
  •  
  •  
  •  
  •  
  •  
期刊检索


检索
检索项:
检索词:
总目录
  • WCSB9︱2019(第九届)世界采样和混样大会 查看全文>>
  • 关于召开第十五届全国青年分析测试学术报告会的通知 查看全文>>
友情链接
多组分免疫亲和柱净化/超高效液相色谱-串联质谱检测水产饲料中的黄曲霉毒素
    点此下载全文
作者单位
刘文静,余海霞,严忠雍,张小军,丁国芳 1.浙江海洋大学食品与医药学院2.浙江省海洋水产研究所3.浙江大学舟山海洋研究中心 
基金项目:国家重点研发计划项目子课题(2016YFD0400102-03)
中文摘要:建立了多组分免疫亲和柱净化/超高效液相色谱-串联质谱(UPLC-MS/MS)测定水产饲料中黄曲霉毒素AFB1、AFB2、AFG1及AFG2含量的方法。饲料样品用80%乙腈水超声提取后,经多组分免疫亲和柱净化,采用UPLC-MS/MS测定,外标法定量。以0.1%甲酸-乙腈为流动相,梯度洗脱分离,电喷雾正离子多反应监测模式检测。结果表明,AFB1、AFG1和AFB2、AFG2分别在2.25~22.5 ng/mL和0.75~7.5 ng/mL质量浓度范围内呈良好线性,相关系数大于0.997;AFB1、AFG1的定量下限均为0.7 μg/kg,AFB2、AFG2的定量下限均为0.2 μg/kg。AFB1、AFG1在1.5 μg/kg,AFB2、AFG2在0.5 μg/kg加标水平下的回收率为78.7%~85.5%,日内相对标准偏差(RSD)为6.0%~6.5%,日间RSD为6.6%~7.0%。该法操作简单,耗时少,重复性好,灵敏度高,适用于水产饲料中黄曲霉毒素的测定。
中文关键词:多组分免疫亲和柱  超高效液相色谱-串联质谱  饲料  黄曲霉毒素
 
Determination of Aflatoxins in Aquatic Feeds Samples by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Multi component Immunoaffinity Column Purification
Abstract:An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of aflatoxins(AFB1,AFB2,AFG1 and AFG2)in aquatic feeds based on multi-component immunoaffinity column purification.The samples were ultrasonically extracted with 80%acetonitrile aqueous solution,then purified with a multi-component immunoaffinity column,finally analyzed by UPLC-MS/MS with electrospray ionization in positive ion mode(ESI+)under multiple reaction monitoring(MRM)mode and quantified by the external standard method.The separation was performed on an Acquity UPLC BEH C18 column by gradient elution with 0.1%formic acid-acetonitrile as mobile phases.Good linear responses were obtained in the concentration ranges of 2.25-22.5 ng/mL for AFB1 and AFG1,and 0.75-7.5 ng/mL for AFB2 and AFG2,with their correlation coefficients larger than 0.997,respectively.The limits of quantitation(LOQs) were 0.7 μg/kg for AFB1 and AFG1,and 0.2 μg/kg for AFB2 and AFG2,respectively.The average recoveries for AFB1 and AFG1 at a spiked level of 1.5 μg/kg,and AFB2 and AFG2 at a spiked level of 0.5 μg/kg ranged from 78.7%to 85.5%,with intra-day and inter-day relative standard deviations of 6.0%-6.5%and 6.6%-7.0%,respectively.The method was simple,rapid,sensitive and reliable,and was suitable for the determination of aflatoxins residues in aquatic feed samples.
Key Words:multi-component immunoaffinity column  ultra performance liquid chromatography-tandem mass spectrometry  feeds  aflatoxins
引用本文:刘文静,余海霞,严忠雍,张小军,丁国芳.多组分免疫亲和柱净化/超高效液相色谱-串联质谱检测水产饲料中的黄曲霉毒素[J].分析测试学报,2019,(3):323-327.
摘要点击次数: 84
全文下载次数: 133
查看全文  查看/发表评论  下载PDF阅读器