[Simultaneous determination of sulfonamides and fluoroquinolones residues in chicken by high performance liquid chromatography-electrospray tandem mass spectrometry].
A method was developed for the simultaneous determination of 10 residual antibiotics--three sulfonamides (sulfadiazine, sulfamethazine and sulfamethoxydiazine) and seven fluoroquinolones (enoxacin, norfloxacin, enrofloxacin, fleroxacin, levofloxacin, lomefloxacin and ciprofloxacin) in chicken by high performance liquid chromatography-electrospray tandem mass spectrometry (HPLC-ESI-MS2). The sample was extracted with 2% acetic acid-acetonitrile for three times and defatted with n-hexane, then purified by an ENVI-18 solid-phase extraction column. After evaporation, the residue was dissolved in the mobile phase of 1 mL. The HPLC separation was performed with a gradient elution program of acetonitrile and water (containing 0.05% formic acid) as the mobile phase. The identification and quantification were done with mass spectrometry. MS2 fragmentation pathways of the ten antibiotics were also analyzed. Good linearities were observed in the range from 0.02 to 2.0 mg/L with correlation coefficients above 0.998 8. The limits of detection (LOD) were 1.10 -6.85 microg/kg and the limits of quantification (LOQ) were 3.68 -22.85 microg/kg. The average recoveries of 10 antibiotics ranged from 68.9% to 102.6% with relative standard deviations below 8.6% (n = 3). The experimental results show that this method is of high sensitivity, good reproducibility, better determination capacity and shorter analysis time. The method can be used for the multi-residue analysis of sulfonamides and fluoroquinolones in animal foods.
Liu
Pengyan
P
College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China. pyliu01@yahoo.com.cn
Jiang
Ning
N
Wang
Yingfeng
Y
Yan
Lizhi
L
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis / Q000302:isolation & purification; D002138:Calibration; D002645:Chickens; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D024841:Fluoroquinolones / Q000032:analysis* / Q000302:isolation & purification; D005506:Food Contamination / Q000032:analysis*; D057230:Limit of Detection; D012997:Solvents / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013449:Sulfonamides / Q000032:analysis* / Q000302:isolation & purification; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013997:Time Factors
D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D012997:Solvents; D013449:Sulfonamides