HPLC Determination of Several Residual Veterinary Medicines in Chicken
摘 要
建立了一种测定鸡肉中氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星兽药残留的高效液相色谱法.样品经乙腈提取,正己烷液-液分配去除蛋白和脂类物质,旋转蒸发除去乙腈,乙腈与水溶解残渣,过微孔滤膜,采用高效液相色谱荧光检测,外标法定量.氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星的质量浓度在0.05~1.2 mg·L-1范围内呈线性关系,相关系数为0.999 7~0.999 9.在0.05~1.00 mg·kg-1质量浓度范围内,平均加标回收率在78.3%~101.8%之间,相对标准偏差为3.89%~12.43%.方法的检出限氧氟沙星为0.003 7 mg·kg-1、诺氟沙星为0.003 7 mg·kg-1、环丙沙星为0.003 5 mg·kg-1、恩诺沙星为0.002 2 mg·kg-1.
Abstract
A HPLC method for the determination of 4 residual quinolone antimicrobials (ofloxacin,norfloxacin,ciprofloxacin and enrofloxacin) in chicken was proposed.The residual medicines in chicken sample were extracted with acetonitrile,protein and fatty substances in the acetonitrile extract were removed by liquid-liquid partition with n-hexane.The acetonitrile layer was collected and evaporated with a rotary evaporator.Finally the residue was taken up with acetonitrile-water (6+4) mixture and used for HPLC determination with fluorescence detector and external standard calibration curve method.Linear relationship between chromatographic peaks and mass concentrations of all the 4 antimicrobials were kept in the range of 0.05-1.2 mg·L-1,with correlation coefficients from 0.999 7 to 0.999 9.Average values of recovery tested in the concentration range of 0.05-1.00 mg·kg-1 were in range from 78.3% to 101.8%,with RSD′s (n=7) from 3.89% to 12.43%.Detection limits of this method were found to be 0.003 7 mg·kg-1 (for ofloxacin,norfloxacin),0.003 5 mg·kg-1 (for ciprofloxacin) and 0.002 2 mg·kg-1 (for enrofloxacin).
中图分类号 O657.37
所属栏目 工作简报
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收稿日期 2006/8/20
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备注李德良(1966-),男,江西丰城人,实验师,主要从事实验室检测.
引用该论文: LI De-liang. HPLC Determination of Several Residual Veterinary Medicines in Chicken[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(10): 838~840
李德良. 高效液相色谱法测定鸡肉中几种兽药残留量[J]. 理化检验-化学分册, 2007, 43(10): 838~840
被引情况:
【1】蒋施,赵颖,金雁,徐宜宏,刘瑜,钟钰, "超高效液相色谱-串联质谱法测定动物组织中19种兽药残留量",理化检验-化学分册 46, 1319-1322(2010)
【2】刘亚梅,闵盛, "高效液相色谱法同时测定禽蛋中环丙沙星、达氟沙星和恩诺沙星的残留量",理化检验-化学分册 52, 305-307(2016)
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参考文献
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【4】Ulrike Neckel,Christian Joukhadar,Martin Frossard,et al.Simultaneous determination of levofloxacin and ciprofloxacin in microdialysates and plasma by high-performance liquid chromatography[J].Anal Chim Acta,2002,463:199-206.
【5】Manceau J,Gicquel M,Laurentie M,et al.Simultaneous determination of enrofloxacin and ciprofloxacin in animal biological fluids by high-performance liquid chromatography Application in pharmacokinetic studies in pig and rabbit[J].Journal of Chromatography B,1999,726:175-184.
【6】Marilyn J Schneider,Dan J Donoghue.Multiresidue determination of fluoroquinolone antibiotics in eggs using liquid chromatography-fluorescence-mass spectrometry[J].Anal Chim Acta,2003,483:39-49.
【7】Gigosos P G,Revesado P R,Cadahia O,et al.Determination of quinolones in animal tissues and eggs by high-performance liquid chromatography with photodiode-array detection[J].Journal of Chromatography A,2000,871:31-36.
【8】杜黎明,卫洪清,张俊燕,等.反相高效液相色谱同时测定6种氟喹诺酮类药物[J].色谱,2003,21(5):503-506.
【9】刘媛,谢孟峡,丁岚,等.高效液相色谱同时测定鸡蛋中4种氟喹诺酮类药物残留[J].分析化学,2004,32(3):352-355.
【10】赵燕燕,杨更亮,闫宏远,等.胶束毛细管电泳在线推扫富集技术测定血液中环丙沙星含量[J].分析化学,2004,32(4):485-488.
【2】Pecorelli I,Galarini R,Bibi R,et al.Simultaneous determination of 13 quinolones from feeds using accelerated solvent extraction and liquid chromatography[J].Anal Chim Acta,2003,483:81-89.
【3】Chandra Immanuel,Hemanth Kumar A K.Simple and rapid high-performance liquid chromatography method for the determination of ofloxacin concentrations in plasma and urine[J].Journal of Chromatography B,2001,760:91-95.
【4】Ulrike Neckel,Christian Joukhadar,Martin Frossard,et al.Simultaneous determination of levofloxacin and ciprofloxacin in microdialysates and plasma by high-performance liquid chromatography[J].Anal Chim Acta,2002,463:199-206.
【5】Manceau J,Gicquel M,Laurentie M,et al.Simultaneous determination of enrofloxacin and ciprofloxacin in animal biological fluids by high-performance liquid chromatography Application in pharmacokinetic studies in pig and rabbit[J].Journal of Chromatography B,1999,726:175-184.
【6】Marilyn J Schneider,Dan J Donoghue.Multiresidue determination of fluoroquinolone antibiotics in eggs using liquid chromatography-fluorescence-mass spectrometry[J].Anal Chim Acta,2003,483:39-49.
【7】Gigosos P G,Revesado P R,Cadahia O,et al.Determination of quinolones in animal tissues and eggs by high-performance liquid chromatography with photodiode-array detection[J].Journal of Chromatography A,2000,871:31-36.
【8】杜黎明,卫洪清,张俊燕,等.反相高效液相色谱同时测定6种氟喹诺酮类药物[J].色谱,2003,21(5):503-506.
【9】刘媛,谢孟峡,丁岚,等.高效液相色谱同时测定鸡蛋中4种氟喹诺酮类药物残留[J].分析化学,2004,32(3):352-355.
【10】赵燕燕,杨更亮,闫宏远,等.胶束毛细管电泳在线推扫富集技术测定血液中环丙沙星含量[J].分析化学,2004,32(4):485-488.
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