超高效液相色谱-串联质谱法测定禽蛋类中4种四环素类抗生素残留量
目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定禽蛋类中4种四环素类(tetracyclines, TCs)抗生素残留量的分析方法。方法 样品经含50 μg/mL蛋白酶K—0.1 mol/L EDTA-Na2溶液提取, Prime HLB固相萃取小柱净化, 洗脱液用氮气吹至近干, 用含甲醇和0.1%甲酸水(4+6)溶液溶解, 采用多反应监测正离子模式, 定性和定量测定禽蛋类中的四环素、土霉素、金霉素、强力霉素等4种四环素类抗生素。结果 4种四环素类抗生素在5~200 μg/L范围内呈现良好的线性关系, 相关系数均大于0.999; 方法的检出限为0.3 μg/kg, 定量限为1.0 μg/kg; 添加水平为20.0~200 μg/kg时, 平均回收率为80.5%~124%, 相对标准偏差(relative standard deviation, RSD)为0.89%~ 6.8%。结论 该方法简单、快捷, 可作为禽蛋类中四环素类抗生素的检测方法。
Objective To establish a method for the determination of 4 tetracycline(TCs) kinds of antibiotics residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by the solution including 50 μg/mL proteinase K and 0.1 mol/L EDTA-Na2, and the extracts were cleaned-up on Prime HLB solid phase extraction column, and the eluent which got from above conditions was dried nearly by nitrogen-blow, and dissolved in methanol and 0.1% formic acid (4+6). Finally, the qualitative and quantitative determination of the target analytes were detected by UPLC-MS/MS in multiple reaction monitoring(MRM)mode. Results The results showed that 4 kinds of tetracyclines had good linear relationships in the range of 5-200 μg/L with correlation coefficients better than 0.999. The limits of detection were 0.3 μg/kg and the limits of quantitation were 1.0 μg/kg. The average recoveries of the method ranged from 80.5% to 124% at the spiked levels of 20.0-200 μg/kg for the 4 kinds of TCs, with the relative standard deviations (RSD) of 0.89%-6.8%. Conclusion This method is simple and quick, which can be used as the detection method of antibiotic residues in poultry eggs.
标题：超高效液相色谱-串联质谱法测定禽蛋类中4种四环素类抗生素残留量
英文标题：Determination of the residues of 4 kinds of tetracycline antibiotics in eggs by ultra performance liquid chromatography-tandem mass spectrometry
作者：
薛荣旋 中山市疾病预防控制中心
刘国平 中山市疾病预防控制中心
黄诚 中山市疾病预防控制中心
丘福保 中山市疾病预防控制中心
林胜军 中山市疾病预防控制中心
中文关键词:蛋白酶K,超高效液相色谱-串联质谱法,四环素类抗生素,禽蛋类,
英文关键词:proteinase K,ultra performance liquid chromatography-tandem mass spectrometry,tetracycline antibiotics,egg,
发表日期：2018-08-14
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