亲水作用色谱-串联质谱法测定动物源食品中10种氨基糖苷类药物的残留量

Determination of Ten Kinds of Aminoglycosides Residues in Animal Original Food Using Hydrophilic Interaction Chromatography Tandem Mass Spectrometry

通过不同键合相亲水作用色谱柱的分离效果比较和分离条件优化,建立动物源性食品中10种氨基糖苷类药物残留量检测的亲水作用色谱-串联质谱法。样品经磷酸缓冲液提取,三氯乙酸沉淀蛋白质,C18固相萃取柱净化,SielcObeliscR色谱柱分离,在电喷雾正离子模式下用串联质谱检测。结果表明,丁胺卡那霉素、潮霉素B,链霉素、双氢链霉素、卡那霉素、庆大霉素、妥布霉素的定量检出限为20μg/kg,新霉素、奇霉素和安普霉素的定量检出限为100μg/kg,在猪肉、牛肉、猪肾、牛肝中的添加回收率为73.9%~103.6%,RSD为3.3%~14.8%,可以满足动物源食品中氨基糖苷类药物的检测需求。

The method was established to analyze ten aminoglycosides in animal original food using hydrophilic interaction chromatography-tandem mass spectrometry(HILIC-MS/MS), after the optimization of separation conditions and the compare of four hydrophilic interaction chromatography columns. Before the samples were extracted by phosphoric acid buffer, trichloroacetic acid was used to precipitating the protein in sample. The target compounds were cleaned up by C18 solid phase extraction (SPE) column and separated by Sielc Obelisc R column. The detection of HPLC-MS/MS was applied in the positive mode of electrospray ionization. The limits of quantitation of amikacin, hygromycin B, streptomycin, dihydrostreptomycin, kanamycin, gentamycin and tobramycin were 20 μg/kg, and the limits of quantitation of neomycin, apramycin and apramycin were 100 μg/kg.The recovery of pork, beef, kidney and ox liver spiking ten aminoglycosides was between 73.9 % and 103.6 %,and the RSD was between 3.3 % and 14.8 %. The method could meet the need of detection of aminoglycosides residues in food.