高效液相色谱-电喷雾串联质谱法同时测定鸡肉中残留的磺胺类和氟喹诺酮类兽药

建立了一种同时测定鸡肉中两类共10种兽药(3种磺胺和7种氟喹诺酮类药物)残留量的高效液相色谱-电喷雾串联质谱方法(HPLC -ESI-MS2)。样品经2%醋酸-乙腈提取,正己烷脱脂,过ENVI-18固相萃取柱净化,经氮气吹干后,残余物用流动相定容到1 mL。以乙腈和 0.05%甲酸溶液作为流动相,采用梯度洗脱程序进行液相色谱分离,用质谱检测器进行定性和定量分析,并对10种药物的二级质谱碎裂方 式进行分析。10种药物在0.02～2.0 mg/L范围内线性良好,相关系数均大于0.9988。检出限(LOD)为1.10～6.85 μg/kg,定量限(LOQ) 为3.68～22.85 μg/kg,样品的平均加标回收率为68.9%～102.6%,相对标准偏差均小于8.6%(n=3)。实验结果表明,该方法灵敏度高,重 现性好,确证能力强,分析时间短,可满足动物源性食品中磺胺和氟喹诺酮类药物的残留分析。

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.