超高效液相色谱-串联质谱法检测鸡肉中抗病毒药物残留

目的建立鸡肉样品中4种抗病毒药物残留的超高效液相色谱-串联质谱方法。方法样品经甲醇-1%三氯乙酸(50∶50,V/V)溶液振荡提取,离心后,上清液过C18固相萃取柱净化,5%氨水-甲醇(15∶85,V/V)洗脱,洗脱液浓缩复溶后,经Waters Acquity UPLC BEH C18色谱柱分离,以甲醇和0. 01 mol/L乙酸铵水溶液(含0. 1%甲酸)为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,MRM扫描模式检测。结果经方法学验证,本方法的回收率、精密度均符合要求。结论本方法应用超高效液相色谱-串联质谱法建立了鸡肉样品中抗病毒药物同时检测的方法,实现了4种抗病毒药物同时定性、定量分析,方法具有灵敏度高,重现性好等特点。

Determination of antiviral drug residues in chicken by ultra-high performance liquid chromatography tandem mass spectrometry

Objective A method for the determination of four antiviral drugs residues in chicken samples by ultra-high performance liquid chromatography-tandem mass spectrometry was established. Methods The samples were extracted by oscillation with methanol and 1% acetocaustin( 50∶50,V/V) solution. After centrifugation,the supernatant was purified by C18 solid phase extraction column and eluted by 5% ammonia water-methanol( 15∶85,V/V). Eluent was concentrated and resolved,and then was separated by a Waters Acquity UPLC BEH C18 column. The mobile phases were methanol and 0. 01 mol/L ammonium acetate with 0. 1% formic acid in gradient elution. The electrospray was operated in the positive ionization mode,and the compounds were identified by MRM scan mode. Results It has been validated by methodology,recovery rate and precision meet are the requirements. Conclusion A method for simultaneous determination of antiviral drugs in chicken samples by ultra-high performance liquid chromatography tandem mass spectrometry was established. Qualitative and quantitative analysis of four antiviral drugs was achieved simultaneously. The method has the characteristics of high sensitivity and good reproducibility.