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

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

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0.999 5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.

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 μBondapak^TM C18 column （3.9 mm i. d. ×300 mm,l0 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 1μg/kg. The linear range was from 6 - 100 μg/kg, and correlation coefficients were more than 0. 999 5. 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.