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机构地区:[1]河北科技大学化学与制药工程学院,石家庄050051 [2]河北出入境检验检疫局,石家庄050051
出 处:《分析试验室》2012年第3期73-77,共5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:建立了动物源食品中粘杆菌素和多粘菌素B残留的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品用V(10%三氯乙酸水溶液):V(乙腈)=30:70提取,Oasis WCX SPE柱净化,LC-MS/MS电喷雾正离子多反应监测模式(ESI+-MRM)检测。分析物在0~250μg/kg的浓度范围内呈良好线性,线性相关系数>0.995。方法的定量限为10μg/kg。方法在三个添加水平的平均回收率在71.6%~78.9%之间,相对标准偏差在6.2%~12%之间。方法适用于动物源食品中粘杆菌素和多粘菌素B的定量及确证检测。A sensitive liquid chromatography-tandem mass spectrometric method (LC-MS/MS) was developed to determine colistin and polymyxin B residues in animal derived foods. Samples were extracted with V (10% trichloroacetic acid solution) : V (acetonitrile) = 30:70 and purified by an Oasis WCX SPE column. LC-MS/MS analysis was performed on multiple reaction monitoring mode under positive ion electrospray ionization. The linearity is satisfactory with a correlation coefficient of 〉 0. 995 at concentrations ranging from 0 to 250 μg/kg. The limit of quantization (LOQ) is 10 μg/kg. Average recoveries of the analytes fortified at three level ranged from 71.6% to 78.9%, and the relative standard deviations ranged from 6. 2% to 12%. It showed to be suitable for quantitative analysis and confirmation of t colistin and polymyxin B residues in animal derived foods.
关 键 词:高效液相色谱-串联质谱法 粘杆菌素 多粘菌素B 动物源食品
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