摘要
建立了气相色谱-串联质谱(GC-MS/MS)测定小麦中氟嘧菌酯、氟嘧菌酯Z体和戊唑醇残留量的分析方法。样品中氟嘧菌酯、氟嘧菌酯Z体和戊唑醇用乙腈提取,提取液经分散固相萃取净化,以HP-5ms色谱柱分离,GC-MS/MS多反应监测(MRM)模式测定,外标法-溶剂标准曲线法定量。结果表明:5~500 ng/mL质量浓度范围内,氟嘧菌酯、氟嘧菌酯Z体和戊唑醇的峰面积与质量浓度之间呈现出良好线性关系;氟嘧菌酯、氟嘧菌酯Z体和戊唑醇在小麦籽粒、小麦秸秆中的最低检测浓度均为0.02 mg/kg。在添加浓度为0.02~10 mg/kg,氟嘧菌酯、氟嘧菌酯Z体和戊唑醇在小麦籽粒中的平均回收率为92%~104%,相对标准偏差为1.1%~15.3%;氟嘧菌酯、氟嘧菌酯Z体和戊唑醇在小麦秸秆中的平均回收率为88%~106%,相对标准偏差为1.4%~10.9%。该方法具有精密度好、灵敏度和准确度高、杂质干扰少等特点,符合农药残留检测分析的基本要求。
A determination method for fluoxastrobin,(Z)-fluoxastrobin and tebuconazole in wheat by gas chromatography tandem mass spectrometry(GC-MS/MS)was established.The fluoxastrobin,(Z)-fluoxastrobin and tebuconazole residues in wheat samples were extracted with acetonitrile,and the extraction solution was purified by dispersed solid phase extraction,then analyzed using GC-MS/MS multiple reaction monitoring(MRM)mode with Agilent HP-5ms column as the analytical column.All the analytes were quantified.The results showed that there were in good linearity between the concentrations of fluoxastrobin,(Z)-fluoxastrobin and tebuconazole and their corresponding response values within the concentration of 5~500 ng/mL,and the limit of quantification(LOQ)of fluoxastrobin, (Z)-fluoxastrobin and tebuconazole in wheat and wheat straw samples were 0.02 mg/kg. When thespiked level ranged from 0.02 to 10 mg/kg, the average recovery rates of fluoxastrobin, (Z)-fluoxastrobin andtebuconazole in wheat ranged from 92% to 104%, and the relative standard deviation (RSD) ranged from 1.1% to15.3%;the average recovery rates of fluoxastrobin, (Z)-fluoxastrobin and tebuconazole in wheat straw ranged from88% to 106%, and RSD ranged from 1.4% to 10.9%.The method was proved to meet the basic requirements ofpesticide residue analysis on sensitivity, accuracy and precision, and to be suitable for analysis of fluoxastrobin andtebuconazole residues in the environmental matrix such as wheat.
作者
晏姣
梁骥
蒋利
欧将
马婧
曾利红
宋强勇
陈力华
梁贵平
YAN Jiao;LIANG Ji;JIANG Li;OU Jiang;MA Jing;ZENG Li-hong;SONG Qiang-yong;CHEN Li-hua;LIANG Gui-ping(National Engineering Research Center for Agrochemicals,Hunan Research Institute of Chemical Industry Co.,Ltd.,Changsha 410014,China;Agrochemical Key Laboratory of Hunan Province,Changsha 410014,China;Hunan Safety Science and Technology Co.,Ltd.,Changsha 410014,China)
出处
《精细化工中间体》
CAS
2024年第2期69-74,共6页
Fine Chemical Intermediates
基金
芙蓉计划省企业科技创新创业团队项目(湖南海利化工新材料科技创新创业团队)。
作者简介
晏姣(1993—),女,湖南邵阳人,工程师,硕士,研究方向:农药残留化学研究(E-mail:1120969160@qq.com);联系人:梁贵平,高级工程师,研究方向:农药残留化学研究(E-mail:1579182522@qq.com)。
