van Vyncht Géry, Jànosi Amaya, Bordin Guy, Toussaint Brigitte, Maghuin-Rogister Guy, De Pauw Edwin, Rodriguez Adela Rosa
European Commission, Joint Research Center, Institute for Reference Materials and Measurements Geel, Retieseweg, Belgium.
J Chromatogr A. 2002 Apr 5;952(1-2):121-9. doi: 10.1016/s0021-9673(02)00092-4.
New antibiotics were recently developed, among which are the (fluoro)quinolones. This paper presents an analytical method which allows the determination of 11 (fluoro)quinolones in swine kidneys: norfloxacin, ofloxacin, cinoxacin, oxolinic acid, nalidixic acid, flumequine, enrofloxacin, enoxacin, ciprofloxacin, danofloxacin and marbofloxacin. The procedure involves a rapid and efficient pre-treatment by solid-phase extraction (recoveries 83-98%), followed by the sensitive and selective determination of all compounds in a single run using LC-ESI-MS-MS. Multiple reaction monitoring (MRM) was used for selective detection of each (fluoro)quinolone. Quinine was selected as internal standard. The accuracy of the method, expressed as recovery, was between 89 and 109%; the repeatability had a maximum RSD lower than 15%. The limits of detection (LOD) were much lower than the respective Maximum Residue Limits (MRL)/4.
最近开发了新型抗生素,其中包括(氟)喹诺酮类。本文介绍了一种分析方法,可用于测定猪肾中的11种(氟)喹诺酮类药物:诺氟沙星、氧氟沙星、西诺沙星、恶喹酸、萘啶酸、氟甲喹、恩诺沙星、依诺沙星、环丙沙星、达氟沙星和马波沙星。该方法包括通过固相萃取进行快速有效的预处理(回收率83-98%),随后使用LC-ESI-MS-MS在一次运行中灵敏且选择性地测定所有化合物。采用多反应监测(MRM)对每种(氟)喹诺酮类进行选择性检测。选择奎宁作为内标。该方法的准确度以回收率表示,在89%至109%之间;重复性的最大相对标准偏差低于15%。检测限(LOD)远低于各自的最大残留限量(MRL)/4。