[关键词]
[摘要]
建立液相色谱 -质谱联用法同时测定禽蛋中金刚烷胺和恩诺沙星、环丙沙星、达氟沙星、沙拉沙星 4种氟喹诺酮类药物的分析方法,为快速简便测定禽蛋中的兽药残留提供参考。以鸡蛋为供试材料,样品经过 Na2EDTA溶液、甲酸乙腈水溶液提取,涡旋振荡和高速离心,上清液用 Agilent Captiva EMR -Lipid萃取柱萃取后,用氮气吹扫浓缩后,将含 1 g/kg甲酸水溶液和 1 g/kg甲酸乙腈水溶液分别作为流动相,测定鸡蛋中的金刚烷胺和恩诺沙星、环丙沙星、达氟沙星、沙拉沙星 4种氟喹诺酮类药物残留。结果表明,在 1~50 μg/kg的线性范围内,金刚烷胺和氟喹诺酮类兽药的线性相关系数均在 0.99以上,其中金刚烷胺相对标准偏差为 0.20%~0.58%,氟喹诺酮类的相对标准偏差为 0.06%~0.55%;5种药物的平均加标回收率为 89.3%~111.0%。色谱图进一步证明所采用的色谱条件能准确检测出鸡蛋中金刚烷胺和 4种氟喹诺酮类药物,该方法操作简单、快速、精确、复现度高,适合于禽蛋样品的测定,可作为实验室禽蛋常规检测方法。
[Key word]
[Abstract]
A liquid chromatography-mass spectrometry method was established for the simultaneous determination of amanta.dine and 4 fluoroquinolone drugs, namely enrofloxacin, ciprofloxacin, danofloxacin, and sarafloxacin, in poultry eggs, providing a refer.ence for the rapid and convenient determination of veterinary drug residues in poultry eggs. Hen egg samples were extracted withNa2EDTA solution and formic acid-acetonitrile aqueous solution, followed by vortexing and high-speed centrifugation. The superna.tant was purified using a Agilent Captiva EMR-Lipid extraction cartridge, concentrated under nitrogen, and then analyzed using anaqueous solution containing 1 g/kg formic acid and a 1 g/kg formic acid-acetonitrile aqueous solution as mobile phases to determineresidues of amantadine and the 4 fluoroquinolone drugs in eggs. Results showed that within the linear range of 1 to 50 μg/kg, the lin.ear correlation coefficients of amantadine and the fluoroquinolone veterinary drugs were all above 0.99. The relative standard deviationof amantadine ranged from 0.20% to 0.58%, while that of the fluoroquinolones ranged from 0.06% to 0.55%. The average spiked recov.eries of the 5 drugs ranged from 89.3% to 111.0%. The chromatograms further confirmed that the adopted chromatographic conditionscould accurately detect amantadine and the 4 fluoroquinolone drugs in eggs. This method is simple, rapid, accurate, and highly repro.ducible, making it suitable for the determination of poultry egg samples and applicable as a routine laboratory method for poultry egg testing.
[中图分类号]
S873;TS207.5
[基金项目]
武威市市级科技计划 B类项目( WW25Z01NY033)。