液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量  

Simultaneous Determination of Amantadine Hydrochloride,Rimantadine Hydrochloride,Dexamethasone,Tilmicosin and Olaquindox Metabolite Residues in Poultry Tissues by High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

作　　者：易锡斌[1,2] 裘立群[3] 刘世琦[1] 黄晓琴[1] 

机构地区：[1]山东农业大学园艺科学与工程学院,山东泰安271018 [2]新希望六和股份有限公司,山东青岛266555 [3]山东农业大学化学材料与工程学院,山东泰安271018

出　　处：《分析测试学报》2015年第3期346-351,共6页Journal of Instrumental Analysis

摘　　要：建立了同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物残留量的液相色谱-串联质谱分析方法.样品用2 mol/L氢氧化钠溶液水解,盐酸调节pH值后,以乙腈作为提取溶剂,经C18固相萃取柱净化.各待测物分别经0.1％甲酸甲醇溶液和氨化甲醇（0.1％氨水）洗脱,Phe-nomenex Kinetex C1s（100 mm×4.6 mm,2.6 μm）色谱柱进行分离,采用0.1％甲酸（含5 mmol/L乙酸铵）-甲醇作流动相,梯度洗脱,串联质谱法对5种药物含量进行测定.结果表明,5种药物在2 ～ 100 μg/L范围内线性关系良好,相关系数为0.996 2 ～0.999 8.在加标浓度为5～50 μg/kg的禽肉组织中,这5种药物的加标回收率为73.7％ ～92.3％,相对标准偏差（n=5）为3.9％ ～ 16.6％,检出限为0.2～ 3.0 μg,/kg,定量下限为0.7～ 10 μg/kg.方法快速、简便、经济实用,符合法规要求,可满足日常检测的需要.A method was developed for the determination of amantadine hydrochloride, rimantadine hydrochloride, dexamethasone, tilmicosin and olaquindox metabolite residues in poultry tissues by high performance liquid chromatography coupled with tandem mass spectrometry. The samples were extracted with acetonitrile after hydrolyzed with 2 mol/L sodium hydroxide and adjusted to pH value with hydrochloric acid. The extract was purified with a C18 solid phase extraction（SPE） cartridge, and eluted with methanol （containing O. 1% tormic acid） and ammonia methanol （containing O. 1% ammonia）. The target compounds were separated with a Phenomenex Kinetex C18 （ 100 mm× 4.6 mm, 2.6 μm） by gradient elution using O. 1% formic acid containing 5 mmol/L ammonium acetate -methanol as mobile phase, and detected by liquid chromatography -tandem mass spectrometry in ES1 under positive ion mode. The calibration curves were linear in the range of 2 - 100μg/L for five drugs, with correlation coefficients of 0. 996 2 - 0. 999 8. The spiked recoveries of five drugs in poultry tissues at spiked levels of 5 - 50 μg/kg were in the range of 73.7% - 92. 3% with relative standard deviations（ RSD, n = 5） of 3.9% - 16.6% . The detection limits （S/N≥3） for five drugs were in the range of 0.2 - 3.0 μg/kg and the quantitation limits （ S/N≥ 10 ） were 0.7 - 10 μg/kg,respectively. The method is rapid, simple, economical and practical, and conforms to regulationsrequirement. Therefore, the method could meet the demand for routine analysis.

关 键 词：盐酸金刚烷胺 盐酸金刚乙胺 地塞米松 替米考星 喹乙醇代谢物 固相萃取 液相色谱-串联质谱 SOLID phase extraction(SPE) 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]