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.
Abstract
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.
维普
万方数据