摘要
建立用高效液相色谱-串联质谱法测定水产品中19喹诺酮类药物——氟甲喹、噁喹酸、诺氟沙星、依诺沙星、环丙沙星、培氟沙星、洛美沙星、丹诺沙星、恩诺沙星、氧氟沙星、沙拉沙星、司帕沙星、双氟沙星、西诺沙星、奥比沙星、麻保沙星、萘啶酸、氟罗沙星和吡哌酸残留量的方法。用酸化乙腈提取水产品中喹诺酮类药物,正己烷脱脂。采用电喷雾电离源(ESI),正离子扫描模式,选择反应监测模式(SRM)监测,外标法定量。该方法对19种喹诺酮类药物标准曲线的线性回归系数均在0.99以上,线性范围为2～200ng/mL,氟罗沙星和吡哌酸检出限为1.0μg/kg、定量限为2.0μg/kg,其余17种喹诺酮的检出限为0.5μg/kg、定量限为1.0μg/kg。19种喹诺酮类药物回收率在76.3%～108%之间,相对标准偏差为0.743%～13.1%。该方法简单、灵敏,结果可靠,可满足实验室批量样品分析的需求。
A method has been developed for detecting nineteen quinolones including oxolinic acid, flumequine, norfloxaein, enoxacin, ciprofloxaein, pefloxaein, lomefloxacin, danofloxacin, enrofloxacin, ofloxacin, sarafloxacin , sparfloxaein, difloxacin, cinoxaein, orbifloxacin, marbofloxaein, nalidixic acid, fleroxacin and pipemidie acid by high performance liquid chromatographytandem mass spectrometry. Samples were extracted with acidified acetonitrile, cleaned up with hexane. Analyte identification and quantification were performed using selected reaction monito- ring （SRM） with one precursor ion and two product ions as identifiers and electrospray ionization in positive mode. There are good linear correlations between the peak areas and concentrations of quinolones （ the calibration coefficients are above 0.99） , the dynamic linear range is 2 - 200 ng/mL . The limits of detection are 0.5 μg/kg for quinolones and the limits of quantification is 1.0μg/kg. The average recoveries ranged from 76.3% to 108% and their relative standard deviations were between 0.743 % and 13.1%. The method can be used to identify and quantify the metabolites of quinolones in aquatic products with satisfactory sensitivity, accuracy and precision. [ Chinese Fishery Quality and Standards, 2012,2（3）：68 -76]
出处
《中国渔业质量与标准》
2012年第3期68-76,共9页
Chinese Fishery Quality and Standards
基金
福建省海洋与渔业厅重点项目(闽海渔合同[2009]1-17号)
关键词
高效液相色谱-串联质谱法
喹诺酮
水产品
残留
high performance liquid chromatography - tandem mass spectrometry
quinolones
fishery products
residues
