超高效液相色谱-串联质谱法分析动物源性食品中4种四环素类药物残留

Determination of 4 kinds of tetracycline drugs residues in food of animal origin by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱  固相萃取  四环素类  残留  动物源性食品

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  tetracyclines  residues  food of animal origin

中文摘要:

      目的 建立超高效液相色谱-质谱联用法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测动物源性食品中四环素类药物(四环素、土霉素、金霉素、强力霉素)残留量的方法。方法 样品经Na2EDTA-Mcllvaine缓冲液(pH=4.0)提取, HLB固相萃取柱净化。采用超高效液相色谱-串联三重四极杆质谱法多反应监测(multiple reaction monitoring, MRM)模式采集, 外标法进行定性和定量检测。色谱柱为Waters ACQUITY BEH C18(100 mm×2.1 mm, 1.7 μm), 以20 mmol/L草酸溶液-乙腈为流动相梯度洗脱, 流速0.3 mL/min。结果 四环素、土霉素、金霉素、强力霉素在5~200 μg/L浓度范围内均具有良好的线性关系(r＞0.995), 检出限均为2.5 μg/kg。四环素、土霉素、金霉素、强力霉素的平均回收率分别为100.8%~105.7%、93.1%~107.2%、94.1%~96.2%和92.7%~99.3%, 相对标准偏差(relative standard deviation, RSD)<8%。结论 本方法选择性强, 灵敏度高, 快速, 重现性好, 可用于动物源性食品中四环素类药物残留的快速测定。

英文摘要:

      Objective To establish an analytical method for simultaneous determination of tetracycline drugs (tetracycline, oxytetracycline, doxycycline, chlortetracycline) residues in food of animal origin by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted by Na2EDTA/Mcllvaine buffer solution (pH=4.0), and then solid-phase cleaned up on a HLB column. The compounds were detected and analyzed by UPLC-MS/MS under multiple reaction monitoring (MRM), and quantified by external standard solution. Waters ACQUITY BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used with the mobile phase of 20 mmol/L oxalic acid aqueous solution and acetonitrile by gradient elution. The flow rate was 0.3 mL/min. Results Tetracycline, oxytetracycline, doxycycline, chlortetracycline had good linear relationships in the range of 5?200 μg/L (r>0.995), the limits of detection for the analytes were 2.5 μg/kg. The average recoveries of 4 tetracyclines were 100.8%-105.7% (tetracycline), 93.1%-107.2% (oxytetracycline), 94.1%-96.2% (chlortetracycline) and 92.7%-99.3% (doxycycline), with relative standard deviation were less than 8%. Conclusion This method is selective, sensitive, rapid and with good reproducibility, which can be used for the rapid determination of tetracycline, oxytetracycline, doxycycline and chlortetracycline in food of animal origin.