Department of Chemistry, Aristotle University, 54124 Thessaloniki, Greece.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Jan 15;881-882:90-5. doi: 10.1016/j.jchromb.2011.12.007. Epub 2011 Dec 15.
A sensitive and robust LC-APCI-MS/MS method has been developed for the unambiguous detection and quantitative determination of the antimicrobial agent Carbadox, its metabolite quinoxaline-2-carboxylic acid and methyl-3-quinoxaline-2-carboxylic acid the major metabolite of Olaquindox. The method was aimed for application in the assaying of muscle tissue so the developed sample preparation scheme subjected samples to enzymatic digestion prior to the application of solid phase extraction clean-up. Subsequently the purified extracts were analyzed by reversed-phase LC-MS/MS in positive APCI and multiple reaction monitoring mode. The method was validated at a level of 1 μg/kg. The decision limits CCα and detection capability CCβ ranged from 0.09 μg/kg to 0.24 μg/kg and from 0.12 μg/kg to 0.41 μg/kg, respectively. The accuracy and precision of the method were satisfactory. The recoveries ranged from 92% to 101% for the metabolites and from 60% to 62% for Carbadox, with coefficient of variances (CVs) less than 12%. The developed method proved efficient and straightforward allowing positive identification and quantitation of the target banned analytes and is thus suitable for application in residue control programmes and metabolism studies.
建立了一种灵敏且稳健的 LC-APCI-MS/MS 方法，用于明确检测和定量测定抗菌剂卡巴多及其代谢物喹喔啉-2-羧酸和甲基-3-喹喔啉-2-羧酸（奥拉喹多的主要代谢物）。该方法旨在应用于肌肉组织的测定，因此开发的样品制备方案在固相萃取净化前对样品进行酶解。随后，通过反相 LC-MS/MS 在正 APCI 和多反应监测模式下分析纯化提取物。该方法在 1 μg/kg 水平进行验证。决策限 CCα 和检测能力 CCβ 范围分别为 0.09 μg/kg 至 0.24 μg/kg 和 0.12 μg/kg 至 0.41 μg/kg。该方法的准确性和精密度令人满意。对于代谢物，回收率范围为 92%至 101%，对于卡巴多回收率范围为 60%至 62%，变异系数（CV）小于 12%。开发的方法证明是高效且直接的，允许对目标禁用分析物进行阳性识别和定量，因此适用于残留控制计划和代谢研究。
