首页|气相色谱-串联质谱法测定小麦中氟嘧菌酯和戊唑醇的残留量

气相色谱-串联质谱法测定小麦中氟嘧菌酯和戊唑醇的残留量

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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0.02~10mg/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.
Determination of Fluoxastrobin and Tebuconazole Residues in Wheat Using Gas Chromatography Tandem Mass Spectrometry
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 the spiked level ranged from 0.02 to 10 mg/kg,the average recovery rates of fluoxastrobin,(Z)-fluoxastrobin and tebuconazole in wheat ranged from 92%to 104%,and the relative standard deviation(RSD)ranged from 1.1%to 15.3%;the average recovery rates of fluoxastrobin,(Z)-fluoxastrobin and tebuconazole in wheat straw ranged from 88%to 106%,and RSD ranged from 1.4%to 10.9%.The method was proved to meet the basic requirements of pesticide residue analysis on sensitivity,accuracy and precision,and to be suitable for analysis of fluoxastrobin and tebuconazole residues in the environmental matrix such as wheat.

fluoxastrobintebuconazoleGC-MS/MSwheatresidue

晏姣、梁骥、蒋利、欧将、马婧、曾利红、宋强勇、陈力华、梁贵平

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湖南化工研究院有限公司 国家农药创制工程技术研究中心,湖南长沙 410014

农用化学品湖南省重点实验室,湖南长沙 410014

湖南安全生产科学研究有限公司,湖南长沙 410014

氟嘧菌酯 戊唑醇 气相色谱-串联质谱 小麦 残留

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)

2024

精细化工中间体
湖南化工研究院

精细化工中间体

CSTPCD
影响因子:0.236
ISSN:1009-9212
年,卷(期):2024.54(2)
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