Determination Of Veterinary Drug Residues And Sudan Red In Food By Ultra Performance Liquid Chromatography-Trandem Mass Spectrum

Ultra performance liquid chromatography(UPLC)is a new HPLC technique which is of high peak capacities,high resolving power,and short separation times with the column packed with 1.7μm particles.Multiple reaction monitoring(MRM)scan mode of the tandem quadrupole mass spectrometer were used as identification as well as confirmation method for MS/MS,which effectively improved the selectivity and sensitivity for samples with complex martrix.Ultra-performance liquid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS)provided an excellent flat for the high throughput determination samples of food safety analysis for its high selectivity,extremely short analysis time and strong identification capability. This paper developed the identification and quantitation method of fluoroquinolones and tetracyclines residues in bovine muscle,as well as Sudan Red in duck egg yolk and ketchup performed by UPLC-MS/MS.This paper included three parts as follows.1.The method of simultaneous analysis of three fluoroquinolones (Ciprofloxacin,Enrofloxacin and Sarafloxacin)in bovine muscle was developed with an UPLC-MS/MS.Acetonitrile was used to extract the residues from bovine muscle in an ultrasonic barth,and the acetonitrile solution was concentrated and dried by the rotary evaporator.The residues were dissolved with mobile phase after cleaned with hexane.The lower layer was detected by the UPLC-MS/MS.The sample was separated on a UPLC apparatus,and detected by the MRM mode of the mass spectrum.The Calibration curves showed good linear relations in the concentration range of 1～50ng·mL^-1(R＞0.998).The average recoveries of 20,50 and 100μg·kg^-1 three spiked concentration levels were between 72.13～89.07%and the RSD values were less than 10.4%.The limit of detection(LOD)in bovine muscle were 5,2,5μg·kg^-1of Ciprofloxacin,Enrofloxacin and Sarafloxacin, respectively.2.The method of simultaneous analysis of five tetracyclines(Tetracycline, Oxytetracycline,Chlortetracycline,Doxycycline and Minocycline)in bovine muscle was developed with an UPLC-MS/MS.Analytes were extracted with Mcllvaine buffer-EDTA(pH4.0)and concentrated by solid-phase extraction on Oasis HLB cartridges.The sample was separated on a UPLC apparatus,and detected by the MRM mode of the mass spectrum.The Calibration curves showed good linear relations in the concentration range of 1～100ng·mL^-1 (R＞0.994).The average recoveries of 20,50 and 100μg·kg^-1three spiked concentration levels were between 69.36～94.82%and the RSD were less than 19.8%.The LOD was 0.1μg·kg^-1of the five substances in brovie tousle.3.The methods of simultaneous analysis of Sudan RedⅠ～Ⅳin duck egg yolk and ketchup were developed with an UPLC-MS/MS.Acetonitrile was used to extract the analytes from the two matrixs.The extraction was detected by UPLC-MS/MS after centrifuge and filtration.The sample was separated on a UPLC apparatus,and detected by the MRM mode of the mass spectrum.The Calibration curves showed good linear relations in the concentration range of 1～50ng·mL^-1(R＞0.994).The average recoveries were between 50.20～101.3%(RSD＜17.50%)and 67.42～84.59%(RSD＜9.57%)of 100,200 and 300μg·kg^-1three spiked concentration levels for duck egg yolk and ketchup,respectively.The LOD was 10μg·kg^-1in the spiked samples all of the four substances.