高效液相色谱-串联质谱法测定动物源食品中粘杆菌素、多粘菌素B的残留量

Determination of colistin and polymyxin B residues in animal derived foods by high performance liquid chromatography tandem mass spectrometry

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.