摘要
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.
作者
刘瑜
董鸿竺
王悦
耿庆华
李晓东
张彤
姜莉
万建春
李志远
LIU Yu;DONG Hong-Zhu;WANG Yue;GENG Qing-Hua;LI Xiao-Dong;ZHANG Tong;JIANG Li;WAN Jian-Chun;LI Zhi-Yuan(Technical Center of Shenyang Customs,Shenyang 110000,China;Technical Center of Jiangxi Customs,Jiangxi 330000,China;Shanghai AB Sciex Analytical Instrument Trading Co.,Ltd.,Beijing 100015,China)
出处
《食品安全质量检测学报》
CAS
2024年第17期101-107,共7页
Journal of Food Safety and Quality
基金
海关总署科研项目(2022HK021)
辽宁省自然科学基金项目(2022MS426)。