高效液相色谱-荧光检测法同时测定鱼肉组织中的诺氟沙星、环丙沙星和恩诺沙星残留.pdfVIP

1296 中国卫生检验杂志2008年7月第l8卷第7期 Chinese Journal of Health Laboratory Technology，Jul 2008；Vol 18 No 7 【化学测定方法】 高效液相色谱一荧光检测法同时测定鱼肉组织中的 诺氟沙星、环丙沙星和恩诺沙星残留 刘丽贞，周婉苹，薛冰 (广东省顺德区农产品质量监督检验测试中心，广东佛山 528333) [摘要] 目的：应用高效液相色谱法(HPLC)，建立起同时测定鱼肉中诺氟沙星(NOR)、环丙沙星(CIP)和恩诺沙星 (ENR)残留量的方法。方法：改进前处理方法和优化色谱条件，确定了以丙酮一0．1 mol／L氢氧化钠(10+1)为提取液， 以MecN一20 mmol／L磷酸盐缓冲液(含12 mmol／L溴化四丁铵)(20+80)，pH=3．0 为流动相，用Waters XTerra。Phenyl 色谱柱分析，荧光检测器测定的最佳条件。结果：该方法线性关系和重复性良好，样品回收率在84．20％～101．55％之 间，变异系数在10％以内，最低检出限为0．005 mg／kg。结论：该法提取效果好，操作简便、快捷、灵敏度高、重现性好，能 够满足鱼肉中诺氟沙星、环丙沙星和恩诺沙星残留量检测的技术要求。 [关键词] 诺氟沙星；环丙沙星；恩诺沙星；残留；高效液相色谱法 [中图分类号] 0657．7 2 [文献标识码] A [文章编号] 1004—8685(2008)07—1296—03 Simultaneous determination of norfloxacin，ciprofloxacin and enrofloxacin in fish tissue using high performance liquid chromatography with fluorescence detection Liu Li—zheng，Zhou Wan~ing，Xue Ping (Shunde Agricultural Product Qualiu Supervision and Inspection Center，Fushan 528333，China) [Abstract] 0bjective：A simultaneous determination method for norfioxacin，ciprofloxacin and enrofloxacin in fish tissue using high performance liquid chromatography with fluorescence detection was established．Methods：Acetone一0．1 mol／L sodium hy— droxide(10+1)was used as extraction solvent．Good separation result on Waters XTerra0 Phenyl column was achieved using MeCN一20 mmol／L phosphate buffer solution(20+80，pH=3．0，containing 12 mmol／L tetra—butylamine bromide)as mobile phase．Results：Matrix spiked recoveries were between 84．20％ ～101。55％ with deviation coefficients less than 10％．Method de— teetion limit was 0．005 mg／kg for each．Conclusion：This method was simple，fast，highly sensitive and reproducible,and could meet the determination requirements for norfioxacin，ciprofloxacin and enrofloxacin residue in fish tissue． [Key words] Norfioxacin；Cipr