液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量
Journal of Instrumental Analysis(2015)
Abstract
建立了同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物残留量的液相色谱-串联质谱分析方法.样品用2 mol/L氢氧化钠溶液水解,盐酸调节pH值后,以乙腈作为提取溶剂,经C18固相萃取柱净化.各待测物分别经0.1%甲酸甲醇溶液和氨化甲醇(0.1%氨水)洗脱,Phe-nomenex Kinetex C1s(100 mm×4.6 mm,2.6 μm)色谱柱进行分离,采用0.1%甲酸(含5 mmol/L乙酸铵)-甲醇作流动相,梯度洗脱,串联质谱法对5种药物含量进行测定.结果表明,5种药物在2 ~ 100 μg/L范围内线性关系良好,相关系数为0.996 2 ~0.999 8.在加标浓度为5~50 μg/kg的禽肉组织中,这5种药物的加标回收率为73.7% ~92.3%,相对标准偏差(n=5)为3.9% ~ 16.6%,检出限为0.2~ 3.0 μg,/kg,定量下限为0.7~ 10 μg/kg.方法快速、简便、经济实用,符合法规要求,可满足日常检测的需要.
MoreKey words
amantadine hydrochloride,rimantadine hydrochloride,dexamethasone,tilmicosin,olaquindox metabolite,solid phase extraction(SPE),high performance liquid chromatography-tandem mass spectrometry
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