高效液相色谱-串联质谱法测定能力验证肉粉中四环素类抗生素残留量

Determination of 4 kinds of tetracycline antibiotics in meat powder samples from food analysis performance assessment scheme by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  四环素类抗生素  高效液相色谱-串联质谱法  残留量

英文关键词:tetracycline antibiotics  high performance liquid chromatography-tandem mass spectrometry  residues

中文摘要:

      目的 优化肉粉样品中四环素类药物的高效液相色谱-串联质谱检测方法。方法 采用80%乙腈-水溶液提取肉粉样品中的四环素类药物, Prime HLB固相萃取小柱净化, 洗脱液用氮气吹至近干, 用10%乙腈水溶液(含0.2%甲酸)溶解, 采用多反应监测正离子模式(multiple reaction monitoring, MRM)进行高效液相色谱-串联质谱仪测定。结果 与国标方法GB/T 21317-2007(HLB固相小柱萃取法)相比, 4种药物的线性范围均在5~200 μg/L时线性良好(r＞0.99), 回收率差异不显著(P>0.05)。实验室方法测得的含量分别为: 四环素113.93 μg/kg, 金霉素68.16 μg/kg, 多西环素155.73 μg/kg, 土霉素未检出; 回收率为四环素94.5%, 金霉素95.2%, 多西环素104.7%, 土霉素97.8%。测得四环素、金霉素、多西环素、土霉素线性相关系数r分别为: 0.9995、0.9998、0.9989、0.9997。结论 本实验室方法简单快速, 回收率高, 重现性好, 适用于熟肉制品中四环素类药物的多残留检测。

英文摘要:

      Objective To optimize the high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for determination of tetracycline in meat powder samples. Methods The samples were extracted by the solution of 80% acetonitrile 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 the solution of 10% acetonitrile (include 0.2% formic acid). Finally, the samples were detected by HPLC-MS/MS with multiple reaction monitoring (MRM) mode. Results Compared to GB/T 21317-2007 (HLB solid phase extraction column method), the results showed that 4 kinds of tetracyclines had good linear relationships in the range of 5-200 μg/L with correlation coefficients were better than 0.99. The recovery difference was not significant (P>0.05). The residues of tetracycline, chlortetracycline, and doxycycline were 113.93, 68.16, and 155.73 μg/kg, and oxytetracycline was not detected. The recoveries of tetracycline, chlortetracycline, doxycycline and oxytetracycline were 94.5%, 95.2%, 104.7%, 97.8%, respectively. The correlation coefficients of tetracycline, chlortetracycline, doxycycline, and oxytetracycline were 0.9995, 0.9998, 0.9989, and 0.9997, respectively. Conclusion The established methods is simple and rapid, which can be used as the detection method of tetracycline antibiotics in meat products.