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作 者:范志影[1] 赵丙超[1] 刘庆生[1] 田园[1]
出 处:《现代科学仪器》2016年第5期97-103,共7页Modern Scientific Instruments
摘 要:本研究建立了高效液相色谱-串联质谱法测定饲料中的5种三嗪类抗球虫药,包括地克珠利(DIC)、妥曲珠利(TOL)和帕托珠利(PON)。样品经乙腈提取,HLBSPE柱净化,Unitary C18色谱柱分离,电喷雾串联四极杆质谱多反应监测方式测定。3种化合物溶液浓度在1μg/L至1000μg/L之间有良好的线性关系,相关系数(R2)〉0.999。6种空白饲料中分别添加3种三嗪类药物,添加水平为5μg/kg、20μg/kg、100μg/kg,回收率在74.66%~111.50%之间、相对标准偏差〈10%。方法定量限为地克珠利1μg/kg、妥曲珠利和帕托珠利5μg/kg。该方法稳定、可靠,适合饲料样品中地克珠利、妥曲珠利和帕托珠利含量的测定。A LC-MS/MS method for simultaneous determination of three triazine coccidiostats (diclazuril,toltrazuril and Ponazuril) in feed has been developed.The feed sample was extracted by acetonitrile, was cleaned up by HLB SPE column and was separated by Unitary C18 chromatographic column. And then the sample was measured by LC-MS/MS in multiple reaction monitoring (MRM) scan model. The technique allowed the determination of the compounds in the concentration range from 1 μg/L to 1000μg/L.Thecoefficient of linearity (RE) is higher than 0.999. The average recovery of the three compounds (spiked at the levels of 5μg/kg,20μg/kg,100μg/kg) ranges from 74.66% to 111.50%, and relative standard deviation is less than 10%. LOQ of diclazuril is 1μg/kg ,and LOQ of toltrazuril and ponazuril is 5μg/kg. The method is steady and reliable.It can meet the needs for the analysis of diclazuril,toltrazuril and ponazuril in feed.
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