摘要
建立了一种液相色谱-串联质谱法测定鸡蛋中7种氟喹诺酮类药物残留的方法。样品经EDTA-Mcllvaine缓冲液提取,冷冻离心,然后用正己烷脱脂,有效地去除杂质,HLB固相萃取柱净化,氮气吹干浓缩,流动相溶解,进行LC-MS/MS定性定量分析。其中5种氟喹诺酮类药物含量在2.5μg/kg^100μg/kg范围内,线性关系良好,环丙沙星和恶喹酸含量分别在6μg/kg^240μg/kg和0.25μg/kg^10μg/kg范围内,线性关系良好,相关系数均大于0.995 9;添加量在100、200、500μg/kg时,该方法的加标回收率为36.9%~81.2%,相对标准偏差均小于15.8%。该方法对环丙沙星和恶喹酸的检测限分别为1.2μg/kg和0.05μg/kg,定量限为24μg/kg和1μg/kg,其他5种氟喹诺酮类药物的检测限为0.5μg/kg,定量限为10μg/kg,表明所建立的方法适用于鸡蛋中7种氟喹诺酮类药物残留的定性和定量检测。
In this paper,a method for the determination of 7 fluoroquinolone residues in eggs by liquid chromatography-tandem mass spectrometry was established.The sample was extracted with EDTA-Mcllvaine buffer,centrifuged,degreased with n-hexane to effectively remove impurities,purified by HLB solid-phase extraction cartridge,dried with nitrogen and concentrated in vacuo,and dissolved in mobile phase.Qualitative and quantitative analyses were made by LC-MS/MS.The linearity of five fluoroquinolones was in the range of 2.5-100μg/kg.The linearities of ciprofloxacin and oxolinic acid were good at 6-240μg/kg and 0.25-10μg/kg respectively,and the relative coefficients were all higher than 0.995 9.The spiked recoveries of this method ranged from 36.9%to 81.2%at 100,200 and 500μg/kg with relative standard deviations less than 15.8%.The detection limits of ciprofloxacin and oxolinic acid in this method were 1.2μg/kg and 0.05μg/kg,respectively.The limits of quantification were 24μg/kg and 1μg/kg.The limits of detection of the other 5 fluoroquinolones were 0.5μg/kg,the limit of quantification is 10μg/kg,which is suitable for the qualitative and quantitative detection of 7 fluoroquinolone residues in eggs.
作者
张晶
王桂琴
ZHANG Jing;WANG Gui-qin(College of Agriculture,Ningxia University,Yinchuan,Ningxia,750021,China)
出处
《动物医学进展》
北大核心
2018年第8期64-70,共7页
Progress In Veterinary Medicine
