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作 者:刘瑜 张柏瑀[2] 闫军霞 付海滨 万建春 李志远 LIU Yu;ZHANG Boyu;YAN Junxia;FU Haibin;WAN Jianchun;LI Zhiyuan(Technical Center of Shenyang Customs,Shenyang 110000;Shenyang Heping District Disease Prevention and ControlCenters,Shenyang 110000;Shenyang International Travel Healthcare Center,Shenyang 110000;Technical Center ofNanchang Customs,Nanchang 330000;Shanghai Aibo Caisi Technology Co.,Ltd.,Shanghai 200000)
机构地区:[1]沈阳海关技术中心,沈阳110000 [2]沈阳市和平区疾病预防控制中心,沈阳110000 [3]沈阳国际旅行卫生保健中心,沈阳110000 [4]南昌海关技术中心,南昌330000 [5]上海爱博才思科技有限公司,上海200000
出 处:《食品工业》2024年第12期290-294,共5页The Food Industry
基 金:海关总署科研项目(2022HK021);辽宁省自然科学基金项目(2022MS426)。
摘 要:采用超高效液相色谱-四极杆串联离子阱质谱,建立了水产品中23种抗病毒药物同时检测的方法及筛查方法。样品经1%三氯乙酸-乙腈(20∶80,V/V)溶液提取,采用Captive EMR-Lipid净化,经Waters BEH C18色谱柱分离,采用UPLC-MS/MS检测,MRM-IDA-EPI确证,外标法定量。23种抗病毒药物定量限为0.1~5μg/kg,标准曲线浓度范围为0.2~200 ng/mL,相关系数均高于0.9916,加标浓度为5,10和50μg/kg(n=6),回收率范围为74.6%~101.9%,相对标准偏差为1.2%~9.8%。采用新型通过型净化技术及四极杆串联离子阱质谱,可同时对23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,实现化合物的确证分析。Use ultra-high performance liquid chromatography quadrupole tandem ion trap mass spectrometry to establish a method for simultaneous detection and screening of 23 antiviral drugs in aquatic products.The sample is extracted with a solution of 1%trichloroacetic acid acetonitrile(20∶80,V/V),purified with Captive EMR Lipid,separated by a Waters BEH C18 chromatographic column,detected by UPLC-MS/MS,confirmed by MRM-IDA-EPI,and quantified by external standard method.The results show that the quantitative limit of antiviral drugs is 0.1-5μg/kg.The standard curve concentration range is 0.2-200 ng/mL,with correlation coefficients higher than 0.9916.When adding recycling concentrations of 5,10 and 50μg/kg(n=6),the recovery rate range is 74.6%-101.9%,and the relative standard deviation is 1.2%-9.8%.By adopting a new type of purification technology and quadrupole tandem ion trap mass spectrometer,qualitative and quantitative detection of 23 antiviral drugs can be carried out 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.
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