超高效液相色谱-四极杆串联离子阱质谱法同时检测动物源性食品中26种新型抗病毒药物

Simultaneous determination of 26 kinds of antiviral drugs in animal derived foods by ultra performance liquid chromatography quadrupole tandem ion trap-mass spectrometry

目的建立一种超高效液相色谱-四极杆串联离子阱质谱法(ultra performance liquid chromatography quadrupole tandem ion trap-mass spectrometry,UPLC-MS/MS)同时检测动物源性食品中多种抗病毒药物的方法。方法样品经三氯乙酸-乙腈(20:80,V:V)溶液提取,Captive EMR-Lipid净化柱净化,采用Waters BEH C18色谱柱分离,UPLC-MS/MS检测,多反应监测-信息关联扫描-增强子离子扫描(multiple response monitoring-information dependent acquisition-enhanced product ion,MRM-IDA-EPI)确证,外标法定量。结果26种抗病毒药物定量限为0.1~5.0μg/kg,相关系数均高于0.99,回收率范围为71%~97%,相对标准偏差为1.3%~10.7%。结论采用新型通过型净化技术及四极杆串联离子阱质谱法,可同时对26种抗病毒药物进行定性、定量检测;采用二级全扫描谱图与谱库检索比对,实现了化合物的确证分析。

Objective To establish a method for the simultaneous determination of multiple antiviral drugs in animal derived foods by ultra performance liquid chromatography quadrupole tandem ion trap-mass spectrometry(UPLC-MS/MS).Methods The sample was extracted with a solution of trichloroacetic acid acetonitrile(20:80,V:V),purified with Captive EMR Lipid,separated using a Waters BEH C18 chromatographic column,detected by UPLC-MS/MS,confirmed by multiple response monitoring-information dependent acquisition-enhanced product ion(MRM-IDA-EPI),and quantified by external standard method.Results The limits of quantitative of 26 kinds of antiviral drugs were 0.1–5.0μg/kg,with correlation coefficients higher than 0.99.The recovery rates were 71%–97%,and the relative standard deviations were 1.3%–10.7%.Conclusion Using a new type of purification technology and quadrupole tandem ion trap mass spectrometry,26 kinds of antiviral drugs can be qualitatively and quantitatively detected simultaneously;by using a second level full scan spectrogram and comparing it with the spectral library retrieval,the confirmation analysis of compounds can be achieved.