摘要
建立了分散固相萃取-高效液相色谱-串联质谱(QuEChERS-HPLC-MS/MS)测定鱼血浆中喹烯酮残留的分析方法。血浆样品经乙腈萃取,采用乙二胺-N-丙基硅烷(PSA)与石墨化炭黑(GCB)为吸附剂进行固相分散净化。用Xtrerra C18(3.5μm,4.6 mm i.d.×150 mm)色谱柱分离,电喷雾正离子(ESI+)模式电离,多反应监测模式检测,外标法定量。方法在5～100μg/L范围内有较好的线性关系,相关系数大于0.998,方法检出限为1.5μg/L,定量限为5μg/L。采用该方法对空白血浆检测并进行加标回收实验,在5和25μg/L两个添加水平下,加标回收率大于90%,相对标准偏差(n=3)低于7.2%。
method for the determination of quinocetone （QCT） in fish plasma by quick, easy, cheap, rugged and safe （QuEChERS） extraction coupled with high performance liquid chromatography-tandem mass spectromety （HPLC-MS/MS） has been established. The plasma sample was extracted with acetonitrile, and purified by the mix of PSA and GCB, the separation was carried out on a Xtrerra C18 column（3.5 μm,4. 6 mm i. d.×150 mm）, the identification and quantification were achieved by using electrospray ionization in positive ion mode （ESI ＋ ） with multiple reaction monitoring （MRM）. The calibration graph of the proposed method was linear in the range of 5 - 100 μg/L. The limit of detection was 1.5μg/L and the limit of quantification was 5 μg/L. The method was applied to analyze the Tilapia plasma samples, and the spike recoveries at the levels of 5μg/L and 25 μg/L were more than 90% with the relative standard deviation （ n = 3 ） less than 7.2%.
出处
《分析试验室》
CAS
CSCD
北大核心
2013年第6期79-82,共4页
Chinese Journal of Analysis Laboratory
基金
中国水产科学研究院基本科研业务费专项(2012A1006)资助
