超高效液相色谱-串联质谱法测定畜禽肉及其内脏中四环素类兽药残留量

Determination of tetracycline veterinary drug residues in livestock and poultry meat and its visceral 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  畜禽肉  内脏  四环素  土霉素  金霉素  多西环素

英文关键词:ultra performance liquid chromatography tandem mass spectrometry  livestock and poultry meat  viscus  tetracycline  oxytetracycline  chlortetracycline  doxycycline

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography tandem mass spectrometry, UPLC)检测畜禽肉及其内脏中的四环素类兽药残留量的分析方法。方法 样品经过0.1 mol/L的Na2EDTA-Mcllvaine溶液提取并同时用乙酸铅溶液沉淀蛋白质, 正己烷脱去脂肪, 经过Oasis HLB固相萃取柱净化后上机测试, 用Phenomenex Kinetex Biphenyl 100A(50 mm×2.1 mm, 2.6 μm)柱子分离, 以乙腈-0.5%甲酸水溶液作为流动相, 梯度洗脱, 采用电喷雾离子源(electron spray ionization, ESI), 正离子模式, 多反应监测(multiple reaction monitoring, MRM)模式, 用外标法峰面积法定量。结果 4种四环素类兽药(四环素、土霉素、金霉素、多西环素)在3~300 ng/mL浓度范围内均呈良好的线性关系, 最低检出浓度均为0.1 μg/kg, 样品的加样回收率均在90%~111%之间, 重复性较好, 回收及重复性的相对标准偏差(relative standard deviation, RSD)均少于5.0%。结论 该方法重复性较好、准确度较高、选择性好, 能够对畜禽肉类及其内脏的中四环素类兽药残留进行定性及定量分析。

英文摘要:

      Objective To establish a method for determination of tetracyclines residues in poultry tissues and viscus by ultra performance liquid chromatography tandem mass spectrometry. Methods The samples were extracted with 0.1mol/L Na2EDTA-Mcllvaine, precipitated the protein with lead acetate, and eluted the fat by hexane. The extract was purified by Oasis HLB solid phase extraction column and performed on a Phenomenex Kinetex Biphenyl 100A (50 mm×2.1 mm, 2.6 μm) with gradient elution of acetonitrile-0.5% formic acid aqueous. Electrospray ionization (ESI), positive ion mode, multiple reaction monitoring (MRM) mode were used and the sample was quantified by external standard solution. Results The 4 tetracycline veterinary drugs (tetracycline,oxytetracycline, chlortetracycline, and doxycycline) showed a good linear relationship in the concentration range of 3-300 ng/mL, and the minimum detection concentration was 0.1 μg/kg. The recovery rates of the samples were 90%-111%, the repeatability was good, and the relative standard deviation (RSD) of recovery and reproducibility was less than 5.0%. Conclusion This method has good reproducibility, high accuracy and good selectivity, which is suitable for qualitatively and quantitatively analysis of the residues of tetracycline veterinary drugs in livestock and poultry meat and their internal organs.