液相色谱-串联质谱法测定蜂蜜和鱼肉中烟曲霉素残留量  

Determination of fumagillin in honey and fish muscle by liquid chromatography tandem mass spectrometric

作　　者：艾连峰[1] 段文仲[1] 马育松[1] 苏萌[1] 哈婧[2] 

机构地区：[1]河北出入境检验检疫局,石家庄050051 [2]河北科技大学化学与制药工程学院,石家庄050051

出　　处：《分析试验室》2012年第10期63-66,共4页Chinese Journal of Analysis Laboratory

基　　金：河北出入境检验检疫局科研项目(HE2011K005)资助

摘　　要：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 performance liquid developed for the determination of chromatography-tandem mass spectrometry method （HPLC-MS/MS） was fumagillin in honey and fish product. Honey and fish product samples were extracted with phosphate buffer and acetonitrile respectively and cleaned up by Oasis MAX solid phase extraction cartridge. The analyte was separated on a Kinetex C18 （2. 6 p,m ×2. 1 mmx 100 mm）column using the mobile phase of acetonitrile - 0. 1% formic acid aqueous solution （70 ＋ 30） and detected by tandem mass spectrometry with multiple reaction monitoring（MRM） mode under positive-ion electrospray ionization. The calibration curves were linear in the range of 2 - 100 μg/L with correlation coefficients no less than 0. 9997. The limits of quantitation （10S/N） were 2 p,g/kg for honey and 5 p,g/kg for fish product. The spiked recoveries at three different spiked levels were in the range of 75. 4% -79. 6% with relative standard deviations of 6. 4 -8. 4%. The method is suitable for the determination of fumagillin in honey and fish product.

关 键 词：液相色谱-串联质谱 烟曲霉素 残留 蜂蜜 鱼肉 

分 类 号：O657.63[理学—分析化学]