色谱

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离子对高效液相色谱法同时测定鱼类中四种喹诺酮类药物的残留

郭根和,潘葳,苏德森,陈涵贞   

  1. Central Laboratory, Fujian Academy of Agricultural Sciences, Fuzhou 350003, China
  • 收稿日期:2004-07-25 修回日期:1900-01-01 出版日期:2005-07-30 发布日期:1988-06-25
  • 通讯作者: 潘葳
  • 基金资助:

Simultaneous Determination of Four Fluoroquinolone Residues in Fish by Ion-Pair High Performance Liquid Chromatography

GUO Genhe, PAN Wei, SU Desen, CHEN Hanzhen   

  1. Central Laboratory, Fujian Academy of Agricultural Sciences, Fuzhou 350003, China
  • Received:2004-07-25 Revised:1900-01-01 Online:2005-07-30 Published:1988-06-25

摘要: 采用离子对高效液相色谱法同时测定了鱼类中4种喹诺酮类药物(FQS)的残留。检测条件为:采用Waters μBondapakTM C18柱,以11 mmol/L的四丁基溴化铵溶液-乙腈(体积比为94∶6)为流动相(用冰乙酸调pH为3.0,流速1.0 mL/min),柱温40 ℃;采用荧光检测器检测,激发波长280 nm,发射波长460 nm。测定结果表明,该方法对FQS的最低检测限为1 μg/kg,在6~100 μg/kg线性范围内,溶液含量与峰面积的相关系数达0.9995以上。在高、中、低3种含量水平下对所测鱼组织中4种喹诺酮类药物进行回收率测定,结果为76%~100%,相对标准偏差小于7%。该法简便、准确,灵敏度高,符合痕量测定的要求。

关键词: 恩诺沙星, 环丙沙星, 离子对高效液相色谱法, 诺氟沙星, 氧氟沙星,

Abstract: An ion-pair high performance liquid chromatographic method with a fluorescence detector was established to determine four fluoroquinolone residues in fish. The chromatographic conditions were as follows: Waters μBondapakTM C18 column (3.9 mm i.d.×300 mm, 10 μm) was used at 40 ℃ with 11 mmol/L tetrabutylammonium bromide solution (pH 3.0)-acetonitrile (94∶6, v/v) as the mobile phase with a flow rate of 1.0 mL/min, at the excitation wavelength of 280 nm and emission wavelength of 460 nm. The detection limit for fish was 1 μg/kg. The linear range was from 6-100 μg/kg, and correlation coefficients were more than 0.9995. At the levels of 10, 50 and 100 μg/kg, the recoveries were 76%-100% with relative standard deviations of less than 7%. The method developed can meet the requirement for residue analysis.

Key words: ciprofloxacin, enrofloxacin, fish , norfloxacin, ofloxacin, ion-pair high performance liquid chromatography