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UPLC-MS/MS法测定鸡肉组织中金刚烷胺残留
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摘要
建立了鸡肉组织中金刚烷胺残留检测的UPLC-MS/MS方法。采用三氯乙酸:乙腈(1:1,V/V)提取试样中残留的金刚烷胺,SPE净化浓缩,ACQUITY UPLCTMBEH C_(18)色谱柱为分离柱,正离子扫描上机测定。结果显示,金刚烷胺在1~20 ng/mL的范围内线性关系良好(R~2=0.997);样品检出限为1 ng/g,定量限为2 ng/g。在2、5、10 ng/g添加水平的回收率为85%~125%,批内批间变异系数均小于20%。本方法快速、灵敏、重现性好,适用于鸡肉中金刚烷胺的残留检测。
A mothod was established for determination of amantadine residues in chicken tissue by UPLC-MS/MS.Samples were extracted by acetocaustin- acetonitrile(1:1,V/V),Sample purification and concentration were performed by SPE with watersoasis mcx column.Then the reconstituted sample solution was analyzed by UPLC-MS/MS under positive ion mode,with ACQUITY UPLCTMBEH C_(18) as the analytical column.The results showed that the good linear range was 1.0~20 ng/mL(R~2=0.997).The detection limit was 1 ng/g,and the quantitation limit was 2 ng/g.The recoveries ranged from 85%~125%and the relative standard deviations were below 20%following analysis of spiked at concentrations 2,5,10 ng/g.The mothod was reliable,sensitive and reproducibility,adapts to the determination of amantadine residues in chiken tissue.
引文
[1]戴晓健,陈笑艳,张勇,等.液相色谱-串联质谱法同时测定人血浆中金刚烷胺和氯苯那敏[J].药物分析杂志,2006,06:17-21.
    [2].李云巍,周小淳,秦焕杰.同时测定人血浆中金刚烷胺、马来酸氯苯那敏的分析方法[J].中国医药指南,2012,10(26):450-452.
    [3].云环,张朝晖,罗生亮,等.固相萃取/LC-MS-MS法检测动物源性食品中的金刚烷胺[J].现代仪器,2009,06:42-45.
    [4].中华人民共和国农业部公告第560号[Z].2005.
    [5].农业部文件农医发[2005]33号关于清查金刚烷胺等抗病毒药物的紧急通知[Z].2005.

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