摘要
建立了同时测定蜂蜜中14种喹诺酮类药物残留的高效液相色谱-串联质谱分析方法。蜂蜜中喹诺酮类药物残留用0.05 mol/L磷酸盐缓冲溶液(pH=3.0)提取,样液过滤后,经Oasis HLB固相萃取柱净化,氢氧化铵-甲醇溶液(体积比1∶19)洗脱,蒸干定容后,用反相液相色谱分离,电喷雾正离子模式离子化,用多反应监测方式(MRM)监测,三重四极杆质谱测定。环丙沙星在0.4～100.0μg/kg,噁喹酸在0.4～50.0μg/kg,恩诺沙星、沙拉沙星、双氟沙星、依诺沙星、诺氟沙星在1.0～100.0μg/kg,氧氟沙星、单诺沙星、氟罗沙星、奥比沙星、麻保沙星在1.0～50.0μg/kg,司帕沙星、氟甲喹在2.0～100.0μg/kg范围内呈线性关系,相关系数r>0.997,在2.0、5.0、10.0、50.0μg/kg 4个添加水平,回收率为66%～111%,相对标准偏差(RSD)为1.3%～13.6%。该方法操作简便,稳定性好,选择性好,灵敏度高,其检出限达1.0μg/kg。
A high performance liquid chromatography- tandem mass spectrometry （HPLC -MS/MS） method was established for simultaneous determination of 14 quinolones residues in honey. The sam- ple were extracted with 0.05 mol/L phosphate buffer solution（ pH = 3.0）. After filtration, the extract was purified by Oasis HLB solid phase extraction column and eluted with methanol - ammonia solution （ 19：1 ,by volume） , and then it was evaporated to dry under nitrogen and redissolved in 1 mL dissolving solution. The solution was separated on a RP-HPLC column and detected by triple-quadrupole MS. The electrospray was operated in the positive ionization mode and the quinolones were identified by using multiple reaction monitoring（MRM） mode. Linear ranges for 14 quinolones were as follows： eiprofloxacin（0.4 - 100.0 μg/kg） ; oxolinic acid（0. 4 - 50.0 μg/kg） ; enrofloxacin, sarafloxacin, difloxaein, enoxacin and norfloxaein（ 1.0 -100.0 μg/kg） ; ofloxaein, danofloxacin, fleroxacin, orbi- floxacin and marbofloxacin（ 1.0 - 50. 0 μg/kg） ; sparfloxacin and flumequin（2.0 - 100. 0 μg/kg）. Correlation coefficients were more than 0. 997. Recoveries at the four spiked levels of 2. 0, 5.0, 10. 0 and 50. 0 μg/kg ranged from 66% - 111% , and relative standard deviations（RSDs） were in the range of 1.3% - 13.6% . The limits of detection for the method were 1.0 μg/kg. Owing the merits of sire-plicity, selectivity and sensitivity, the proposed method has been successfully applied to the determination of quinolones residues in honey.
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第11期1141-1146,共6页
Journal of Instrumental Analysis
基金
国家标准化管理委员会资助项目(20051870-T-326)
关键词
蜂蜜
喹诺酮类药物
固相萃取
液相色谱-串联质谱法
honey
quinolones
solid phase extraction
liquid chromatography -tandem mass spec- trometry
