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目的建立超高效液相色谱-串联质谱联用仪同时检测鸡肉中16种磺胺类和15种喹诺酮类兽药残留。方法称取5.0 g样品加入酸化乙腈均质3 min后,超声提取5 min,正己烷去除油脂,0℃、10 000 r/min高速离心5 min,取中间提取液10.0 ml,氮气吹干,初始流动相定容到1.0 ml,过0.20μm滤膜,供超高效液相色谱-串联质谱仪分析,内标法定量。结果当浓度为10.0μg/L~500μg/L时,31种兽药的线性关系良好,相关系数(r)均≥0.999 0,当加标量为50.0μg/kg时,31种兽药的加标回收率为84.0%~94.7%,相对标准偏差(RSD)均<2.5%。31种兽药的检出限均为0.10μg/kg,定量限为0.30μg/kg。结论通过均质提取的办法,大大提高提取的效率。本方法专属性强,灵敏度高,操作简单,快捷,可作为鸡肉中磺胺和喹诺酮类兽药残留的检测。
OBJECTIVE To establish simultaneous determination of 16 sulfonamides and 15 quinolones residues in chicken meat by ultra performance liquid chromatography-tandem mass spectrometry. Methods Weigh 5.0 g sample and add acidified acetonitrile homogenized for 3 min. After ultrasonic extraction for 5 min, remove the fat by hexane, centrifuge at 10 000 r / min for 5 min at 0 ℃, take the intermediate extract 10.0 ml, dry with nitrogen, initial The mobile phase volume to 1.0 ml, 0.20μm filter for ultra-high performance liquid chromatography - tandem mass spectrometry analysis, internal standard method. Results The linear relationship of 31 veterinary drugs was good at the concentration of 10.0μg / L ~ 500μg / L with the correlation coefficient (r) ≥0.9990. The spiked recoveries of 31 veterinary drugs at the standard addition of 50.0μg / kg Was 84.0% ~ 94.7%, with relative standard deviation (RSD) <2.5%. The detection limits of the 31 veterinary drugs were 0.10μg / kg, the limit of quantification was 0.30μg / kg. Conclusion The method of homogeneous extraction greatly improves the efficiency of extraction. The method has the advantages of high specificity, high sensitivity, simple and quick operation, and can be used as the detection of residues of sulfonamides and quinolones in chicken meat.