Zhao Sijun, Jiang Haiyang, Li Xuelian, Mi Tiejun, Li Cun, Shen Jianzhong
Department of Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100094, People's Republic of China.
J Agric Food Chem. 2007 May 16;55(10):3829-34. doi: 10.1021/jf0635309. Epub 2007 Apr 13.
A HPLC method using a modified sample preparation procedure was optimized and validated for the quantification of 10 quinolones (QNs), including marbofloxacin, ciprofloxacin, norfloxacin, lomefloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, and flumequine, in swine, chicken, and shrimp tissues. In this method, only a small mass (<or=2.0 g) of sample and a relatively small volume of organic reagent (<or=4.6 mL) of a nonchlorinated extraction solvent were required. The QNs were analyzed by liquid chromatography in a single run using a gradient elution program and with a programmable fluorescence detector to obtain optimum detection wavelengths. Mean recoveries of 10 drugs from edible animal tissues at a concentration range of 1-100 ng g-1 were 72.8-106.8% with relative standard deviations below 11.2%. The limits of quantification for each QN in different muscle tissues ranged from 0.3 to 1.0 ng g-1, which were below the lowest maximum residue limits (10 ng g-1) established in many countries. The method was also applied to the measurement of QN residues in commercial muscle samples. The results showed it was rapid, simple, sensitive, and suitable for use in food surveillance programs.
一种采用改良样品制备程序的高效液相色谱（HPLC）方法，针对猪、鸡和虾组织中10种喹诺酮类药物（QNs）进行了优化和验证，这些药物包括马波沙星、环丙沙星、诺氟沙星、洛美沙星、达氟沙星、恩诺沙星、沙拉沙星、二氟沙星、恶喹酸和氟甲喹。在该方法中，仅需少量样品（≤2.0 g）和相对少量（≤4.6 mL）的非氯化萃取溶剂有机试剂。使用梯度洗脱程序并通过可编程荧光检测器对QNs进行单次液相色谱分析，以获得最佳检测波长。在1 - 100 ng g⁻¹浓度范围内，10种药物在可食用动物组织中的平均回收率为72.8% - 106.8%，相对标准偏差低于11.2%。不同肌肉组织中各QN的定量限为0.3至1.0 ng g⁻¹，低于许多国家规定的最低最大残留限量（10 ng g⁻¹）。该方法还应用于商业肌肉样品中QN残留量的测定。结果表明，该方法快速、简便、灵敏，适用于食品监测计划。
