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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%。
A method for the determination of Quinocetone residues in fish plasma by dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry (QuEChERS-HPLC-MS / MS) was established. Plasma samples were extracted with acetonitrile and purified by solid phase dispersion using ethylenediamine-N-propylsilane (PSA) and graphitized carbon black (GCB) as adsorbents. Separation with Xtrerra C18 (3.5 μm, 4.6 mm i.d. × 150 mm) column, Electrospray positive ion (ESI +) mode ionization, Multiple reaction monitoring mode, External standard method. The method has a good linear relationship in the range of 5 ~ 100μg / L, the correlation coefficient is greater than 0.998, the detection limit is 1.5μg / L and the limit of quantification is 5μg / L. The blank plasma was tested by this method. The spiked recoveries were more than 90% and the relative standard deviations (n = 3) were lower than 7.2% at 5 and 25 μg / L spiked levels.