| 摘要: |
| 建立了同时测定鱼肉中氧氟沙星(Ofloxacin，OFL)、诺氟沙星(Norflxacin，NOR)、环丙沙星(Ciprofloxacin，CIP)、恩诺沙星(Enrofloxacin，ENR) 4种喹诺酮类药物残留量的高效液相色谱方法 (HPLC) ,并对样品提取条件和色谱条件进行了优化分析。确定使用四丁基溴化铵溶液提取，固相萃取净化、高效液相色谱-荧光检测器检测、外标法定量的分析方法。本方法对氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星标准曲线的线性回归系数均在0.999以上，线性范围为0.002～0.5μg/mL，检出限为1.5μg/kg，定量限为4μg/kg。在草鱼、鳙鱼、大黄鱼中进行这4种喹诺酮类药物加标回收率的验证实验，回收率在68.5%~106.6%之间，相对标准偏差为0.80%~9.16%，说明本方法简单、灵敏，结果可靠。 |
| 关键词: 高效液相色谱 荧光检测 喹诺酮类药物 鱼肉 |
| DOI： |
| 投稿时间：2012-06-29修订日期：2012-08-06 |
| 基金项目: |
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| High Performance Liquid Chromatographic Method for Simultaneous Determination of Four Quinolone Residues in Fish Muscle Tissues |
|
| (Changsha Livestock Poultry and Aquatic Animals Products Quality Inspection Center) |
| Abstract: |
| A high performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of 4 quinolone residues (enrofloxacin, ciprofloxacin, norfloxacin, ofloxacin) in n fish muscle tissues. The conditions of extraction and chromatography parameters were optimized and discussed. Extracted by tetrabutyl ammonium bromide solution, cleanup on a solid phase extraction cartilage, HPLC with a flurorescence detector was used for analyzing 4 quinolones, and their quantification was achieved by external standard method. Four quinolones exhibited good linearity within the range of 0.002－0.5 μg/mL and the regression coefficients were all over 0.99. The limit of quanification (LOQ) was 4.5μg/kg, the limit of detection (LOD) was 1.5μg/kg. This method was suitable for analysis of grass carp, bighead carp, and Yellow croaker samples, and the recoveries were within 68.5%~106.6%, with RSD range of 0.80%~9.16%. This method is simple, sensitive and reliable, has good suitability for the simultaneous determination of 4 quinolone residues in fish muscle tissues. |
| Key words: high performance liquid chromatography (HPLC) fluorescence detection quinolones fish muscle tissues |
