Simultaneous determination of enrofloxacin and its primary metabolite ciprofloxacin in meat and fish by HPLC
Simultaneous determination of enrofloxacin and its primary metabolite ciprofloxacin in meat and fish by HPLC
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高效液相色谱法同时测定肉、鱼中恩诺沙星及其主要代谢物环丙沙星
DOI：
10.3358/shokueishi.38.5_329
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发表时间：
1997
期刊：
影响因子：
--
通讯作者：
H. Nakazawa
中科院分区：
文献类型：
--
作者：
M. Horie;Koichi Saito;Youji Hoshino;H. Terada;H. Nakazawa
开发了一种简单、可靠、灵敏的高效液相色谱法同时测定肉和鱼中残留恩诺沙星及其主要代谢物环丙沙星的方法。用0.3%偏磷酸-乙腈(6:4)提取药物，提取物在Oasis HLB柱上净化。 HPLC分离采用TSK-GEL Super ODS柱(100×4.6mm i.d.)，以含1.0mmol/L十二烷基硫酸钠(SDS)的0.05mol/L磷酸盐缓冲液(pH 2.5)-乙腈(70:30)为流动相，流速0.5mL/min。荧光检测器在278nm的激发波长和445nm的发射波长下操作。两种药物的校准图在 0.5 至 20 ng 范围内呈直线。 0.2μg/g浓度下组织中药物的回收率均大于80%，检出限均为0.005μg/g。研究了烘烤对比目鱼中恩诺沙星和环丙沙星残留的影响。两种药物均表现出优异的热稳定性。
A simple, reliable and sensitive method for the simultaneous determination of residual enrofloxacin and its primary metabolite, ciprofloxacin, in meat and fish by HPLC has been developed. The drugs were extracted with 0.3% metaphosphoric acid-acetonitrile (6:4), and the extracts were cleaned up on an Oasis HLB cartridge. The HPLC separation was carried out on a TSK-GEL Super ODS column (100×4.6mm i. d.) with 0.05mol/L phosphate buffer (pH 2.5)-acetonitrile (70:30) containing 1.0mmol/L sodium dodecyl sulfate (SDS) as the mobile phase at a flow rate of 0.5mL/min. A fluorescence detector was operated at an excitation wavelength of 278nm and an emission wavelength of 445nm. The calibration graphs were rectilinear from 0.5 to 20ng for both drugs. The recoveries of the drugs from tissues fortified at the level of 0.2μg/g were greater than 80%, and the detection limits were 0.005μg/g for both drugs. The influence of baking on enrofloxacin and ciprofloxacin residues in flatfish was investigated. Both drugs showed excellent thermal stability.