基于UPLC-QTOF/MS法快速靶向筛查与测定克氏原螯虾中的三环唑  

Rapid targeted screening and determination of tricyclazole in Procambarus clarkii based on UPLC-QTOF/MS

作　　者：陈建武[1] 彭婕[1] 甘金华[1] 杨总 张涛[1] 何力[1] CHEN Jianwu;PENG Jie;GAN Jinhua;YANG Zong;ZHANG Tao;HE Li(Fishery Quality Supervision and Testing Center, ministry of Agriculture and Rural affairs, Fishery Products Quality Safety Risk Assessment Laboratory(Wuhan) of Ministry of Agriculture and Rural Affairs,Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Wuhan 434223, China;SCIEX,Shanghai 200335, China)

机构地区：[1]农业农村部淡水鱼类种质监督检验测试中心,农业农村部水产品质量安全风险评估实验室(武汉),中国水产科学研究院长江水产研究所,湖北武汉430223 [2]上海爱博才思分析仪器贸易有限公司,上海200335

出　　处：《中国渔业质量与标准》2020年第5期25-30,共6页Chinese Fishery Quality and Standards

基　　金：中央级公益性科研院所基本科研业务费专项(2018JBF);现代农业技术产业体系专项(CARS-48);国家农产品质量安全风险评估项目(GJFP201800902).

摘　　要：建立了克氏原螯虾(Procambarus clarkii)中三环唑的快速筛查和定量检测的超高效液相色谱-四级杆/飞行时间质谱法(UPLC-QTOF/MS法)。筛查样品经酸化乙腈(0.1%甲酸)提取,减压旋蒸浓缩后,50%甲醇(0.1%甲酸)复溶测定。该方法采用全扫描方式采集,结合保留时间、精确分子量、同位素比与自建的二级标准谱库数据可进行快速准确的定性确证;对于阳性样品采用二级扫描模式(MRMHR)进行准确定量。采用QuEChERS法对克氏原螯虾肌肉样品中的三环唑进行测定,在0.5~100.0μg/L范围内,空白基质匹配标准曲线为Y=694.34X+29.16,r=0.9995,方法检测限(LOD)为0.5μg/kg,定量限(LOQ)为1.0μg/kg,平均回收率为65.15%~94.24%(n=6),相对标准偏差为5.31%~8.12%。结果表明,本筛查和测定方法具有快速、准确等优点,适用于克氏原螯虾中三环唑的快速筛查和定量测定,可为水产品中农药残留的快速筛查和定量测定提供参考。A method for rapid screening and determination of tricyclazole in Procambarus clarkii based on UPLC-QTOF/MS was established.For Procambarus clarkii muscle samples,acetonitrile(0.1%formic acid)was used for extraction of tricyclazole.With reduced pressure distillation,50%methanol(0.1%formic acid)was used for constant volume of samples.In this method,full scan analysis was carried out,as well as retention time,accurate mass numbers,isotope ratio,and secondary ion spectra library of tricyclazole were collected that used for rapid and accurate characterization.The positive samples were accurately quantified by using targeted ion secondary scanning mode(MRMHR).QuEChERS(quick,easy,cheap,effective,rugged,safe)method was used to analyze tricyclazole in Procambarus clarkii muscle.In the range of 0.5-100.0μg/L,the matrix-matched standard curve was Y=694.34X+29.16 and r=0.9995,the limit of detection(LOD)for this method was 0.5μg/kg,the limit of quantification(LOQ)was 1.0μg/kg,the average recovery rate was 65.15%-94.24%(n=6),and the relative standard deviation was 5.31%-8.12%.The results showed that the screening and determination method was suitable for rapid screening and quantitative determination of tricyclazole in Procambarus clarkii,which could be used as a reference for rapid screening and quantitative determination of some pesticide residues in aquatic products.

关 键 词：克氏原螯虾 三环唑 超高效液相色谱-四级杆/飞行时间质谱法 QUECHERS 快速筛查 定量 

分 类 号：S94[农业科学—水产养殖]