超高效液相色谱-串联质谱法同时测定鸡肉中四环素类和喹诺酮类抗生素含量

Simultaneous determination of tetracyclines and quinolones antibiotics in chicken by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  四环素  喹诺酮  鸡肉

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  tetracyclines  quinolones  chicken

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定鸡肉中2种四环素类和6种喹诺酮类抗生素含量的分析方法。方法 样品采用EDTA-Mcllvaine缓冲溶液(pH=4)提取, HLB固相萃取柱净化, Waters Acquility UPLC BEH C18色谱柱分离, 以乙腈-甲醇(1:1, V:V, 含0.2%甲酸)和0.2%甲酸水体系作为流动相进行梯度洗脱, 利用串联三重四级杆质谱多反应模式, 正离子监测方式检测, 外标法定量。结果 8种抗生素在1~20 μg/kg范围内具有良好线性, 相关系数均大于0.999, 检出限为0.1~0.6 μg/kg, 加标回收率为84.3%~115.8%, 相对标准偏差为0.63%~14.68%。结论 该方法回收率高, 灵敏度高, 重复性好, 有效缩短检测时间, 适用于鸡肉中8种抗生素的同时测定。

英文摘要:

      Objective To establish a method for simultaneous determination of 2 tetracyclines and 6 quinolones antibiotics in chicken by ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with EDTA-Mcllvaine buffered solution (pH=4), purified by HLB solid phase extraction column column, separated with Waters Acquility UPLC BEH C18 by gradient elution using acetonitrile-methanol (1:1, V:V, containing 0.2% formic acid) and 0.2% formic acid water systems as mobile phase. Then the sample was detected with a series of triple quadrupole mass spectrometry multiple reaction mode, positive ion monitoring mode. The content was quantitatively analyzed by external standard method. Results The 8 kinds of antibiotics had good linear relationships in the range of 1?20 μg/kg, and the correlation coefficients were larger than 0.999. The limits of detection were 0.1?0.6 μg/kg. The standard recoveries were 84.3%?115.8%, and the relative standard deviations were 0.63%?14.68%. Conclusion This method has the advantages of high recovery, high sensitivity, good repeatability and short detection time. It is suitable for simultaneous determination of 8 kinds of antibiotics in chicken.