›› 2011, Vol. 38 ›› Issue (2): 187-190.

• 疾病防治 • 上一篇    下一篇

高效液相色谱法测定猪肝组织中3-甲基喹喔啉-2-羧酸

姚蕴珊,沈建忠,吴聪明,程林丽   

  1. (中国农业大学动物医学院药理与毒理研究组,北京 100193)
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2011-02-20 发布日期:2011-02-20
  • 通讯作者: 沈建忠

Determination of 3-methyl-quinoxaline-2-carboxylic Acid in Porcine Liver by High Performance Liquid Chromatography

YAO Yun-shan,SHEN Jian-zhong,WU Cong-ming,CHENG Lin-li   

  1. (Department of Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China)
  • Received:1900-01-01 Revised:1900-01-01 Online:2011-02-20 Published:2011-02-20
  • Contact: SHEN Jian-zhong

摘要: 本研究建立了猪肝组织中3-甲基喹喔啉-2羧酸(3-methyl-quinoxaline-2-carboxylic acid,MQCA)的高效液相色谱检测方法。采用0.3 mol/L盐酸提取猪肝组织中药物,经MAX柱净化,以乙腈∶甲醇∶0.5%甲酸水(15∶50∶35,V/V/V)为流动相,C18色谱柱进行药物分离,320 nm波长下紫外检测,结果当药物在猪肝组织中添加水平为20~250 μg/kg时,平均回收率为72.35%~85.00%,日内测定的相对标准偏差(RSD)(n=5)为5.56%~9.49%,日间RSD(n=3)为5.96%~9.63%。猪肝组织中MQCA的定量限为20 μg/kg,检出限为6.65 μg/kg,表明该方法灵敏度、准确度和精密度均符合兽药残留分析技术的要求,适用于猪肝组织中MQCA的检测。

关键词: 高效液相色谱法; 猪肝组织; 3-甲基喹喔啉-2-羧酸

Abstract: To develop a high performance liquid chromatography method for determination of 3-methyl-quinoxaline-2-carboxylic acid (MQCA) in porcine liver.MQCA was extracted from porcine liver with 0.3 mol/L hydrochloric acid. The extract was cleaned up on MAX Sep-Pak Silica solid-phase extraction cartridge. Then the eluate was collected and dried under a gentle stream of nitrogen gas and the dissolved residue was analyzed by HPLC. The HPLC separation was performed on a Symmetry Shield reversed phase C18 boned silica column, with mobile phase of acetonitrile-methanol-0.5% formic acid (15∶50∶35,V/V/V) and determination wave of 320 nm in an UV detector.The validation was carried out on spiked porcine liver(spiked at 20~250 μg/kg), and the average recoveries of target drug ranged from 72.35% to 85.00%, with intra-day relative standard deviations(RSD)(n=5) of 5.56% to 9.49%, and inter-day RSD(n=3) of 5.96% to 9.63%.The limits of quantification (LOQ) in porcine liver was 20 μg/kg and the limits of detection (LOD) was 6.65 μg/kg.The results demonstrated that the sensitivity, accuracy, and precision of this method meet the requirements of veterinary drug residue analysis. The method is applicable to detect MQCA in porcine liver.

Key words: high performance liquid chromatography(HPLC); porcine liver; MQCA

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