超高效液相色谱-三重四级杆串联质谱法测定多种动物源性食品中11种喹诺酮类药物残留

Determination of 11 quinolones residues in animal derived foods by UPLC-MS/MS

目的建立多种动物源性食品中11种喹诺酮类药物残留的超高效液相色谱-三重四级杆串联质谱法。方法样品经提取后,提取液经HLB固相萃取柱进行净化。以C18色谱柱(3.0 mm×10 mm,1.7μm)为分离柱,甲醇-乙腈(1∶1,V/V)和0.1%甲酸水溶液为流动相梯度洗脱,串联四级杆质谱仪检测,外标法定量。结果本法在0.25μg/kg^5.0μg/kg呈良好线性关系,相关系数>0.99,平均回收率在78.0%~110.0%,最低检出限为0.2μg/kg^0.3μg/kg,相对标准差<15%。结论本法操作简单、灵敏度高、重现性好,能满足多种动物源性食品中11种喹诺酮类药物痕量残留的检测。

Objective To establish a method for the determination of 11 quinolones residues in animal derived foods by ultra high performance liquid chromatography-triple quadrupole mass spectrometry （UPLC-MS/MS）. Methods After the samples were extracted, the extract was purified with HLB solid phase extraction column and separated with a C18 column （3.0 mm×10 mm, 1.7 μm）. The methanol-aeetonitrile（ 1 ： 1, V/V） and 0.1% formic acid aqueous solution were used as mobile phase. The analytes were detected with triple quadrupole mass spectrometer and quantified by the external standard method. Results The method showed a good linear relationship within 0.25 g/kg-5 g/kg, with the correlation coefficient（r） greater than 0.99. The average recovery rates was within 78.0%-110.0%, and the lowest detection limit was within 0.2 μg/kg-0.3 μg/kg, with the relative standard deviation（RSD） less than 15%. Conclusion The method is simple, sensitive, repro-ducible, and selective. It can be used for the detection of trace residues of 11 quinolones in animal derived foods.