采用超高效液相色谱串联质谱法(UPLC-MS/MS)对鸡蛋中金刚乙胺的含量残留进行研究.样品由1％乙酸乙腈提取后,通过PCX阳离子交换固相萃取柱净化,使用Eclipse Plus C18反相色谱柱(2.1 mm × 50 mm,1.8 μm)进行分离,以0.1％甲酸水和甲醇溶液作为流动相进行梯度洗脱,使用超高效液相色谱-三重四极杆串联质谱联用仪,选择正离子多反应监测模式进行定性定量测定.金刚乙胺在1.0～20.0 ng/mL质量浓度下呈良好线性关系,相关系数(R2)大于0.999,分别添加质量分数1,2和10 μg/kg这3个水平的标准品,加标回收率为84.2％～91.8％,方法定量限为1.0μg/kg.该方法的建立对于监控鸡蛋中的金刚乙胺残留具有积极作用.
Determination of Rimantadine Residues in Eggs by Ultra High Phase Liquid Chromatography Tandem Mass Spectrometry
The contents of rimantadine in eggs were studied by ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).After the sample was extracted from 1％acetonitrile,it was purified by PCX Cation-exchange solid phase extraction column,separated by Eclipse Plus C18 reverse phase column(2.1 mm×50 mm,1.8 μm),and gradient elution was performed with 0.1％formic acid water and methanol solution as mobile phase.Using ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry,the positive ion multi-reaction monitoring mode was selected for qualitative and quantitative determination.Rimanantine showed a good linear relationship at the concentration of 1.0-20.0 ng/mL,and the correlation coefficient(R2)was greater than 0.999.The standard substances with mass concentrations of 1,2 and 10 μg/kg were added,respectively.The recoveries were 84.2％-91.8％,and the limits of quantitation were 1.0 μg/kg.The establishment of this method had a positive effect on the monitoring of rimantadine residues in eggs.
万方数据
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