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液相色谱-质谱联用法检测鸡蛋中8种氟喹诺酮类药物残留 被引量:16

An improved method for determination of eight fluoroquinolones antibiotics in eggs by liquid chromatography tandem mass spectrometry
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摘要 建立了一种液相色谱-质谱联用法(LC-MS/MS)快速测定鸡蛋中8种氟喹诺酮类药物残留的方法.样品经磷酸-乙腈提取,冷冻离心,旋转蒸发浓缩,初始流动相溶解,然后用正己烷脱脂,有效地去除杂质,随后进行LC-MS/MS定性定量分析.8种氟喹诺酮类药物含量在2~50μg/kg线性关系良好,相关系数R均大于0.9956;添加量在5,10和20μg/kg时,该方法的加标回收率为65.4% ~119.6%,相对标准偏差均小于7.52%.该方法的检出限为0.0005~0.22μg/kg,定量限为0.02~0.74μg/kg,适用于鸡蛋中8种氟喹诺酮类药物残留的定性和定量检测. A method was established for the determination of eight fluoroquinolones antibiotics in egg sample by liquid chromatography tandem mass spectrometry.The sample was extracted with phosphoric acid and ace-tonitrile.After separated with high speed frozen centrifugation and concentrated with a rotary evaporator, the residue was dissolved with the mobile phase and then defatted with n-hexane.It was then analyzed with LC-MS.The linear ranges were from 2 to 50 μg/kg with the correlation coefficients above 0.995 6 μg/kg for all the 8 fluoroquinolones.The average recoveries of 8 fluoroquinolones were 65.4% ~119.6% at three spiked level:5, 10, 20μg/kg with the RSD lower than 7.52%.The limit of detection was of 0.000 5μg/kg to 0.22 μg/kg.The limit of quantification was of 0.02μg/kg to 0.74μg/kg.The method could be applied to accurate qualitative and quantitative detection of the eight fluoroquinolones in the eggs.
出处 《浙江师范大学学报(自然科学版)》 CAS 2016年第1期53-59,共7页 Journal of Zhejiang Normal University:Natural Sciences
基金 国家自然科学基金资助项目(KYZKY11132) 金华市科技局项目(2014-3-030)
关键词 液相色谱-质谱联用 鸡蛋 氟喹诺酮 残留 liquid chromatography tandem mass spectrometry egg fluoroquinolone residues
作者简介 杨朝琳(1991-),女,山东青岛人,硕士研究生.研究方向:地理环境与污染控制. 洪华嫦.E-mail:huachang2002@163.com
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