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牛奶中黄曲霉毒素M1残留固相萃取-液相色谱质谱检测方法研究
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摘要
建立了牛奶中黄曲霉毒素M_1(AFM;)残留的固相萃取-超高效液相色谱(UPLC)和超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。样品经乙腈提取,Plexa固相萃取柱净化,UPLC荧光检测器或UPLC-MS/MS电喷雾正离子多反应监测(MRM)模式检测。AFM_1在0.5~50μg/L的系列浓度范围呈线性相关,牛奶中AFM_1的检测限为0.1μg/kg,定量限为0.2μg/kg。在0.1~0.5μg/kg的添加浓度范围内平均回收均为90%~110%,变异系数均小于10%。结果表明该方法简单快速、灵敏度高、重复性好,适用于牛奶中AFM_1残留检测。
An ultra performance liquid chromatography(UPLC) and ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was established for the determination of aflatoxin M_1(AFM_1) residues in milk.The samples were extracted by acetonitrile,and was cleaned up by the Plexa SPE,AFM_1 was detected by HPLC Fluorescence detector or HPLC-MS/MS electrospray ionization in the positive ion multiple reaction mode.The calibration curves of the AFM_1 was linear over the concentration ranges of 0.5~50 μg/L.The limit of detection of AFM_1 was 0.1 μg/kg,and the limit of quantification was 0.2 μg/kg.The control samples were spiked in 0.1~0.5 μg/kg,and the average recoveries ranged from 90%to 110%.The coefficient of variation was less than 10%.This method can be applied for the determination of AFM_1 residues in milk.
引文
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