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提出了液相色谱串联质谱测定蜂蜜和鱼肉中烟曲霉素残留量的分析方法。蜂蜜样品和鱼肉样品分别用磷酸盐缓冲液和乙腈提取,经Oasis MAX固相萃取柱净化后,在Kinetex C18(2.6μm×2.1 mm×100 mm)反相色谱柱上以乙腈-0.1%甲酸酸水溶液(70+30)为流动相色谱分离,采用电喷雾正离子扫描、多反应监测模式(ESI+-MRM)进行质谱检测,外标法定量。方法的测定下限(10S/N)蜂蜜为2μg/kg,鱼肉为5μg/kg。在2～100μg/L的浓度范围内呈良好线性,线性相关系数>0.9997。方法在3个水平的添加回收率在75.4%～79.6%之间,相对标准偏差在6.4%～8.4%之间。方法适用于蜂产品和鱼肉中烟曲霉素残留的定量及确证检测。
A method for the determination of fumagillin residues in honey and fish by liquid chromatography tandem mass spectrometry was proposed. Samples of honey and fish were extracted with phosphate buffer and acetonitrile, respectively. After purification with Oasis MAX solid phase extraction column, acetonitrile and 0.1% formic acid were applied to a Kinetex C18 (2.6 μm × 2.1 mm × 100 mm) The aqueous solution (70 + 30) was separated by mobile phase chromatography. Electrospray positive ion scan (ESI-MS) and multi-reaction monitoring mode (ESI + -MRM) were used for mass spectrometry. The lower limit of the method (10S / N) was 2μg / kg for honey and 5μg / kg for fish. In the concentration range of 2 ~ 100μg / L showed a good linearity, linear correlation coefficient> 0.9997. The recoveries of the methods at three levels ranged from 75.4% to 79.6% with relative standard deviations between 6.4% and 8.4%. The method is suitable for quantitative and confirmatory detection of fumagillin residues in bee products and fish.