【作者】 倪永付； 朱莉萍； 王勇； 闫秋成； 高坤；

【Author】 NI Yong-fu *,ZHU Li-ping,WANG Yong,YAN Qiu-cheng,GAO Kun (Jining Entry-Exit Inspection and Quarantine Bureau,Jining 272000,China)

【机构】 济宁出入境检验检疫局；

【摘要】 建立了微波辅助萃取/液相色谱-三重四极杆串联质谱法同时检测猪肉中氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星4种氟喹诺酮类和四环素、土霉素、金霉素、强力霉素4种四环素类药物残留的方法。样品经微波辅助萃取,C18净化粉净化后,上机检测。采用HypersilGOLD(1.9μm,50mm×2.1mmi.d.)色谱柱分离,在多反应监测模式下检测,外标法定量。结果表明:8种药物在0～100μg/L浓度范围内线性关系良好,相关系数r=0.9936～0.9990,方法检出限为1.2μg/kg,定量下限为5μg/kg;平均回收率为81%～98%,RSD为4.2%～7.7%。更多还原

【Abstract】 A new method was established to determine the four fluoroquinolones ofloxacin,norfloxacin,ciprofloxacin,enrofloxacin and the four tetracyclines tetracycline,oxytetracycline,chlortetracycline,doxycycline residues in pork by microwave assisted extraction technique combined with liquid chromatography-tandem mass spectrometry.The sample was extracted with microwave assisted extraction equipment.After being cleaned by C 18 powder,the sample was separated on Hypersil GOLD(1.9μm,50 mm ×2.1 mm i.d.) column.The analysis was carried out in the multi-reaction monitoring mode,and the external standard method was used for quantification.The calibration curves of the four fluoroquinolones and the four tetracyclines were in good linearities from 0 to 100 μg/L with the correlation coefficients of 0.993 6-0.999 0,the detection limit for this method was 1.2 μg/kg and the quantitative limit was 5 μg/kg.The average recoveries of this method were between 81%-98% with the RSDs of 4.2%-7.7%.更多还原