液相色谱-串联质谱负离子模式数据库的构建及对水产品中多种兽药的筛查检测

Development of veterinary drugs data library and screening method of negative mode by liquid chromatography-tandem mass spectrometry in aquatic products

建立水产品中兽药的液相色谱-串联质谱复合线性离子阱系统EPI扫描方式的数据库及筛查分析方法.7种兽药的最低检出限（LOD,S/N≥3）5 μg/kg,最低定量限（LOQ,S/N≥10）10 μg/kg.每种兽药添加10 μg/kg、50 μg/kg、100 μg/kg 3个水平到空白基质中（n=6）,回收率为83.2％～105.8％,相对标准偏差（RSD）为4.9％～10.2％.方法除两对离子对、保留时间外,利用子离子比对进行化合物的真伪鉴定,可以有效的排除假阳性.数据库建立过程简单快捷,借助离子阱的富集功能,实现对水产品样本中多种兽药残留的定性定量分析,且具有灵敏、准确的特点.

A liquid chromatography tandem triple-quadrupole linear ion trap mass spectrometric （QTrap LC-MS/MS） EPI mode was developed for the data library and simultaneous screening of veterinary drugs residual in aquatic products. The results showed that the limits of detection （LOD, S/N≥3） were 5μg/kg and the limits of quantity（LOQ, S/N≥10） was 10 μg/kg for the veterinary drugs. The average recoveries （n= 6） of the veterinary drugs in aquatic product samples at three levels 10 μg/kg,50μg/kg,100μg/kg were from 83.2% to 105.8% with the relative standard deviations （RSD） between 4. 9% and 10. 2%. Besides using two transitions and retention time, product ions were matched with the data libraries to identification the compounds. This process is proved to exclude the false positive samples effectively. The setting of the data library is quick and easy, and the ion-trap will help to apply the qualitative and quantitative determination of veterinary drugs in aquatic products with sensitive and accurate characteristics.