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
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。
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.
标题：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
英文标题：Determination of 4 kinds of tetracycline drugs residues in food of animal origin by ultra performance liquid chromatography-tandem mass spectrometry
作者：
石春红 上海市松江食品药品检验所
曹向英 上海市松江区食用农产品安全监督检测中心
曹美萍 上海市松江食品药品检验所
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,
发表日期：2019-03-28
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