CAJ | 학술논문

建立了蜂蜜样品中15种喹诺酮类兽药残留的超高效液相色谱-串联质谱检测方法. 蜂蜜样品用磷酸盐缓冲溶液溶解提取后,用Oasis HLB固相萃取柱净化,超高效液相-电喷雾串联四级杆质谱检测,外标法定量. 测定时用AcquityUPLC BEH C_(18)色谱柱(50 mm×2.1 mm,1.7 μm)分离,体积分数 0.1%甲酸溶液-乙腈系统梯度洗脱,质谱测定采用多重反应监测(MRM)模式. 15种喹诺酮类兽药的检出限均低于或等于1.0 ng/mL,回收率均在78.6%～112.9%范围内,相对标准偏差均在10%范围内. 该方法各项指标均能满足国内外各项法规的要求,可用于蜂蜜样品中喹诺酮类药物残留的定量和定性检测.
건립료봉밀양품중15충규낙동류수약잔류적초고효액상색보-천련질보검측방법. 봉밀양품용린산염완충용액용해제취후,용Oasis HLB고상췌취주정화,초고효액상-전분무천련사급간질보검측,외표법정량. 측정시용AcquityUPLC BEH C_(18)색보주(50 mm×2.1 mm,1.7 μm)분리,체적분수 0.1%갑산용액-을정계통제도세탈,질보측정채용다중반응감측(MRM)모식. 15충규낙동류수약적검출한균저우혹등우1.0 ng/mL,회수솔균재78.6%～112.9%범위내,상대표준편차균재10%범위내. 해방법각항지표균능만족국내외각항법규적요구,가용우봉밀양품중규낙동류약물잔류적정량화정성검측.
An ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method was developed for the determination of fifteen quinolones residues in honey. Honey samples were diluted with phosphate buffer solution, then cleaned up with Oasis HLB columns and detected by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometric detection. Quantitation was carried out using an external standard method. Separation of the samples was performed on an acquity UPLC BEH C_18column (50 mm×2.1 mm,1.7 μm) using a gradient solvent system (acetonitrile -0.1% formic acid). MS/MS was performed with multiple reaction monitoring (MRM) mode. The detection limit of all the 15 quinolones could reach 1.0 ng/mL. The recoveries ranged from 78.6% to 112.9% with relative standard deviations less than 10%. The method is fast, sensitive, with good ruggedness, and all indexes can meet various law and regulation of China and other countries. It's suitable for quantitative and qualitative analysis of quinolones residues in honey.