鸡肉中金刚烷胺超高效液相色谱-电喷雾串联质谱检测方法的建立及阳性样品的制备

被引:3
作者
常平平 [1 ]
许春南 [1 ]
张立新 [2 ]
郝小妹 [1 ]
高兴 [1 ]
陈超 [1 ]
机构
[1] 北京勤邦生物技术有限公司
[2] 北京市优质农产品产销服务站
关键词
超高效液相色谱—电喷雾串联质谱; 金刚烷胺; 鸡肉; 阳性样品;
D O I
10.16431/j.cnki.1671-7236.2015.09.009
中图分类号
S859.84 [动物性食品中化学物残留];
学科分类号
0906 ;
摘要
本试验建立了一种超高效液相色谱—电喷雾串联质谱测定鸡肉中金刚烷胺的分析方法。以甲醇-1%三氯乙酸作提取剂,采用超声波辅助溶剂萃取法萃取鸡肉中金刚烷胺,萃取液用MCX固相萃取柱进行净化浓缩。以BEH C18色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。对质谱和色谱条件、提取剂的种类、超声提取时间、固相萃取柱及洗脱液的种类进行了优化,在0.1~20.0ng/mL范围内线性关系良好(r=0.9998)。样品在5.0、10.0和20.0μg/kg添加水平的回收率为89.7%101.4%,相对标准偏差(RSD)小于7.0%;方法的检测限为0.07μg/kg,定量限为0.23μg/kg。本方法灵敏度高、准确度高,能满足公司及相应鸡肉行业的客户进行鸡肉中金刚烷胺残留量的快速、高灵敏检测分析。本试验还根据金刚烷胺在动物体内的代谢动力学成功制备了浓度为11.16和7.18mg/kg的金刚烷胺阳性鸡肉样品,为研发金刚烷胺ELISA试剂盒提供了相应的阳性样品。
引用
收藏
页码:2278 / 2285
页数:8
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