摘要
目的研究7种喹诺酮类抗生素的电喷雾质谱裂解规律。方法采用超高效液相串联-四极杆飞行时间质谱对农业部公告限用的7种喹诺酮类抗生素进行分析,Acquity HSS T3UPLC色谱柱(2.1 mm×100 mm,1.8μm),柱温:30℃,流速:0.2ml·min^(-1),进样量:2μl,采用流动相梯度对样品进行分析,质谱离子源为电喷雾电离源,在正离子模式下进行检测,碰撞气为氮气,干燥气温度:350℃,干燥气流速:10L·min^(-1),毛细管出口电压:125V,锥孔电压:65V。结果正离子模式下,喹诺酮类化合物易获得质子形成[M+H]+的母离子,碰撞诱导解离后产生特征碎片离子,根据各子离子的精确质量数可确证其结构,对各喹诺酮类化合物的质谱裂解规律进行分析。结论本文提出的喹诺酮类抗生素的质谱裂解规律可为动物源食品中喹诺酮类化合物的筛查及结构鉴定提供依据。
Objective To study the patterns of fragmentation of seven types of quinolones.Methods Ultra high performance liquid chromatography-quadrupole time of flight mass spectrometry was applied.Based on the structure,the veterinary drugs of quinolones were determined in a positive ion mode by electrospray ionization.The column was a T3 UPLC（2.1 mm×100 mm,1.8μm）from Waters,the column temperature was 30 ℃,and the injection volume was 2μl.The total time was 18 min by gradient elution,and flow rate was 0.2 ml·min-1.Nitrogen was used as the collision gas,and the gas temperature was 350 ℃ at a flow rate of 10 L·min-1.The fagmentor was 125 V,and skimmer was 65 V.Results An H＋was easily obtainable from quinolones to form [M ＋ H]＋,on which collision induced dissociation was performed to obtain fragment ions.The structure of each quinolone was analyzed with the help of accurate mass.Conclusion The fragmentation mechanism of quinolones is explained,which provides reference for the supervision of animal derived foods.
作者
王聪
苗贝贝
钮正睿
曹进
WANG Cong;MIAO Bei-bei;NIU Zheng-rui;CAO Jin(National Institutes for Food and Drug Control,Institute for Food Control,Beijing 100050,China)
出处
《解放军药学学报》
CAS
CSCD
2018年第4期317-321,共5页
Pharmaceutical Journal of Chinese People's Liberation Army
关键词
喹诺酮
电喷雾
质谱
裂解规律
quinolones
electrospray ionization
mass spectrometry
fragmentation mechanism
