| 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 |
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| 基金项目:国家重点研发计划项目子课题（2016YFD0400102-03） |
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| 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 |
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| Determination of Aflatoxins in Aquatic Feeds Samples by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Multi component Immunoaffinity Column Purification |
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| 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,2019,38(3):323-327. |
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