UPLC-MS/MS法对蜂蜜中金刚烷胺和金刚乙胺药物残留的测定
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摘要
建立了快速测定蜂蜜中金刚烷胺和金刚乙胺药物残留的超高效液相色谱-串联质谱分析方法。样品用1%甲酸乙腈提取,浓缩后利用超高效液相色谱分离,以乙腈和0.1%甲酸水为流动相进行梯度洗脱,MRM反应监测模式检测。结果表明,在0.1～100μg/L的系列浓度范围内均呈良好线性关系,相关系数大于0.999。金刚烷胺检测限为0.2μg/kg,定量限为0.5μg/kg,金刚乙胺检测限为0.5μg/kg,定量限为1.0μg/kg。在1～20μg/kg浓度范围内平均回收率为80%～110%,精密度小于20%。该方法方便快捷、定性准确,适用于蜂蜜中金刚烷胺、金刚乙胺药物残留检测。
A UPLC-MS/MS method was developed and established to raplidly determine amantadine and rimantadine in honey. The sample were extracted with acetonitrile with 1% formic acid. After enrichment,the sample was separated by UPLC,eluted with acetonitrile and 0.1% formic acid as the mobile phase and the MRM reaction was monitored. The results showed that there was a good linearity in the range of 0.1～100 μg/L, and the correlation coefficient were more than 0.999. The detection limit of the amantadine was 0.2 μg/kg, and the limit of quantification was 0.5 μg/kg;the detection limit of the rimantadine was 0.5 μg/kg, and the limit of quantification was 1.0 μg/kg. The average recoveries were 75%～110% in the range from 1～20 μg/kg,and the precision was less than 20%. The method was convenient, rapid, accurate and it was suitable for the detection of amantadine and rimantadine in honey.
A UPLC-MS/MS method was developed and established to raplidly determine amantadine and rimantadine in honey. The sample were extracted with acetonitrile with 1% formic acid. After enrichment,the sample was separated by UPLC,eluted with acetonitrile and 0.1% formic acid as the mobile phase and the MRM reaction was monitored. The results showed that there was a good linearity in the range of 0.1～100 μg/L, and the correlation coefficient were more than 0.999. The detection limit of the amantadine was 0.2 μg/kg, and the limit of quantification was 0.5 μg/kg;the detection limit of the rimantadine was 0.5 μg/kg, and the limit of quantification was 1.0 μg/kg. The average recoveries were 75%～110% in the range from 1～20 μg/kg,and the precision was less than 20%. The method was convenient, rapid, accurate and it was suitable for the detection of amantadine and rimantadine in honey.
引文
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[5]张鑫,吴剑平,严凤,等.基于双柱固相萃取-色质联用技木同时检测鸡肉中8种抗病毒药物残留[J].中国兽药杂志,2015,49(9):45-50.
[6]吴剑平,张鑫,李丹妮,等.分散固相萃取结合亲水作用色谱-串联质谱法检测预混合饲料中7种抗病毒药物含量[J].中国兽药杂,2016,50(3):49-55.
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