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液相色谱法快速测定鸡肉中氧氟沙星手性对映体残留量

Determination of Residual Ofloxacin Enantiomers in Chicken Muscle by Liquid Chromatography
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摘要 建立了鸡肉样品中氧氟沙星对映体液相色谱荧光检测(liquid chromatography fluorescence detector,LC-FLD)残留量快速分析方法。鸡肉样品经磷酸盐缓冲液提取后,用C18固相萃取小柱净化,洗脱液吹干后用流动相复溶即可进行液相色谱分析。分析时采用LeapsilTM C18色谱柱,以水相(含2 mmol/L硫酸铜和2.5 mmol/L异亮氨酸,pH3.5)和甲醇作为流动相进行梯度分析,荧光检测器检测,其中激发波长为297 nm,发射波长为487 nm,外标法定量。本方法在5.0、50、100μg/kg和150μg/kg 4个添加水平下,左氧氟沙星对映体平均添加回收率在75.5%~86.1%之间,批内变异系数在1.97%~4.42%之间,批间变异系数在3.02%~6.02%之间;右氧氟沙星对映体平均添加回收率在77.3%~84.9%之间,批内变异系数在2.15%~4.21%之间,批间变异系数在3.87%~5.84%之间。方法对两种对映体的检测限均为1.5μg/kg,定量限均为5.0μg/kg。 A method was developed for determining residual ofloxacin enantiomers in chicken muscle by liquid chromatography with fluorescence detection. Samples were extracted with phosphate buffer solution. The extract was purified by solid phase extraction (SPE) using a C18 cartridge and the eluent was then dried by nitrogen blowing and dissolved in mobile phase. The analytes were separated on a LeapsilTM C18 column using a mobile phase composed of a mixture of methanol and aqueous solution of (pH 3.5) 2 mmol/L copper sulfate and 2.5 mmol/L isoleucine. Excitation wavelength was 297 nm and emission wavelength was 487 nm. Quantitation was performed by using the external standard calibration method. The average recoveries for the two enantiomers in spiked chicken muscle were 75.5%-86.1%at four fortiifed levels ranging from 5 to 150μg/kg, and the intra-and inter-batch coefifcients of variation (CVs) were 2.15%-4.21%and 3.87%-5.84%, respectively. The limits of detection (LOD) and quantitation (LOQ) were 1.5 and 5.0μg/kg for the two enantiomers of olfoxacin, respectively.
出处 《肉类研究》 2014年第5期25-28,共4页 Meat Research
基金 宁波市重大科技攻关项目(2013C11003)
关键词 氧氟沙星 手性对映体 液相色谱法 固相萃取 ofloxacin enantiomers liquid chromatography solid phase extraction
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  • 1GARCIA M A, SOLANS C, CALVO A, et al. HPLC separation and quantification of ofloxacin enantiomers in rabbit plasma, application to pharmacokinetic studies[J]. Chromatographia, 2002, 56: 39-42.
  • 2姜金庆,杨雪峰,王自良,常新耀,王三虎,刘兴友.氟喹诺酮类药物多残留间接竞争ELISA检测方法的建立[J].中国预防兽医学报,2011,33(11):887-892. 被引量:11
  • 3HUET A C, CHARLIER C, TITTLEMIER S A, et al. Simultaneous determination of (fluoro) quinolone antibiotics in kidney, marine products, eggs, and muscle by enzyme-linked immunosorbent assay (ELISA)[J]. Journal of Agricultural Food Chemistry, 2006, 54(8): 2822-2827.
  • 4刘媛,谢孟峡,丁岚,单吉浩,杨清峰,刘素英.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. 被引量:103
  • 5PENA A, SILVA L J G, PEREIRA A, et al. Determination of fluoroquinolone residues in poultry muscle in portugal[J]. Analytical and Bionanalytical Chemistry, 2010, 397(6): 2615-2621.
  • 6MOEMA D, NINDI MM, DUBE S. Development of a dispersive liquid-liquid microextraction method for the determination of fluoroquinolones in chicken liver by high performance liquid chromatography[J]. Analytical Chimica Acta. 2012, 730: 80-86.
  • 7HUANG Jingfang, LIN Bo, YU Qiongwei. Determination of fluoroquinolones in eggs using in-tube solid phase microextraction coupled to high-performance liquid chromatography[J]. Analytical Chimica Acta. 2006, 384: 1228-1235.
  • 8李雅丽,郝晓蕾,冀宝庆,胥传来,沈崇钰,丁涛.HPLC-ESI-MS/MS测定动物性食品中19种喹诺酮类药物残留的研究[J].食品科学,2008,29(8):502-506. 被引量:26
  • 9SHEN J Z, GUO L M, XU F, et al. Simultaneous determination of fluoroquinolones, tetracyclines and sulfonamides in chicken muscle by UPLC-MS-MS[J]. Chromatographia, 2010, 71(5/6): 383-388.
  • 10曾苏,章立,刘志强.RP-HPLC手性流动相添加剂法分析尿中氧氟沙星对映体[J].药学学报,1994,29(3):223-227. 被引量:24

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