Determination Of 27 Quinolones Residues In Aquatic Products By LC-MS/MS

A liquid chromatography electrospray ionization tandem mass spectrometry method to determenting the resid ues of 27 kinds ofquinolones in the edible tissues of mandarinfish,perch,eel and prawn was developed.And the 27 kinds of quinolones was included fleroxacin,ofloxacin,ciprofloxacin,enrofloxacin,lomefloxacin,danofloxacin,orbifloxacin,difloxacin,sarafloxacin,sparfloxacin,flumequine,oxolinic acid,nalidixic acid,cinoxacin,pipemidic acid,moxifloxacin,gatifloxacin,pazufloxaxin,enoxacin,norfloxacin,marbofloxacin,pefloxacin,antofloxacin,nadifloxacin,balofloxacin,gemifloxacin and tosuflo xacin.The samples were extracted twice by 2% formic acid-acetonitrile solution,then the supernatant which was extraceted twice was dropped pressure to reduece acetonitrile,and the concentrated solution was defatted by n-hexane which has been saturated by acetonitrile.The n-hexane was apartmented and abandoned,the eluent reduced was concentrated to dryness under a stream of nitrogen.Then the residue was dissolved in water with 0.1% formic acid-acetonitrile(95:5,V/V).Twice high-speed centrifuge to remove impurities,following filtrated by 0.22 ?m filterable membrane.Finally,the filtrate was analyzed by LC-MS/MS.In this study,the result showed a good linear relationship between the peak area and the concentration of 27 kinds of quinolones drugs during their linear ranges with correlation coefficient more than 0.99.The result of adding experiment with high,medium and low levels,the recovery rate of 27 kinds of quinolones drugs in tissues were higher than 60.0%,except ANT which got a low recovery rate in perch which respectively were 51.3%~64.0%.The intra-assay coefficient of variation between 0.7%~14.2%,inter-assay coefficients of variation between 2.1%~17.1%.Besides,the limit of detection(LOD)and the limit of quantification(LOQ)of the 27 kinds quinolones in the tissues of mandarinfish,perch,eel and prawn respectively were 0.2~2?g/kg and 0.5~4 ?g/kg.The results showed that the LC-MS/MS determination methods described in this invstigation was fasty,high sensitivity and specificity,while totally match the analysis on residus of quinolones in edible tissues of mandarinfish,perch,eel and prawn.