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《化学分析计量》 2021年第04期
DOI:10.3969/j.issn.1008-6145.2021.04.004
高效液相色谱-质谱联用法同时测定果蔬中丁醚脲、氟吡菌胺、氟唑菌酰胺、螺虫乙酯
张思敏,梁跃,苏梅清,潘艳坤,江燕,黄艳洪,黄璐璐
广西壮族自治区分析测试研究中心,南宁 530022 
Simultaneous determination of diafenthiuron, fluopicolide, fluxapyroxad and spirotetramat in fruits and vegetables by high performance liquid chromatography-mass spectrometry
张思敏,梁跃,苏梅清,潘艳坤,江燕,黄艳洪,黄璐璐
Guangxi Zhuang Autonomous Region Research Center for Analysis and Test, Nanning 530022, China 
摘要: 建立高效液相色谱-质谱联用法同时测定果蔬中丁醚脲、氟吡菌胺、氟唑菌酰胺、螺虫乙酯4种农药残留的分析方法。样品经乙腈提取,QuEchERS原则净化,以5 mmol/L乙酸胺溶液(含0.1%甲酸)和乙腈体系为流动相,采用电喷雾离子源正离子方式、选择离子反应监测模式进行测定,用外标法定量。4种农药的质量浓度在2~500 μg/L范围内与色谱峰面积呈良好的线性关系,相关系数均大于0.991,方法检出限为0.02~1.25 μg/kg,定量限为0.05~5.0 μg/kg。在柑橘、菜心两种基质中的加 标回收率分别为71.6%~109%和82.0%~109%,测定结果的相对标准偏差均不大于14.4%(n=6)。该方法便捷、快速、准确、可靠,适用于蔬菜水果中丁醚脲、 氟吡菌胺、氟唑菌酰胺、螺虫乙酯的测定。  
Abstract:A high performance liquid chromatography-mass spectrometry(HPLC-MS) method was developed for the simultaneous determination of four kinds of pesticide residues such as diafenthiuron, fluopicolide, fluxapyroxad and spirotetramat in fruits and vegetables. The samples were extracted with acetonitrile and purified by QuEChERS principle, and then were detected by HPLC-MS with 5 mmol/L ammonium acetate solution (containing 0.1%formic acid)and acetonitrile system as the mobile phase, performed by electrospray ion source positive ion mode and select reaction monitoring(SRM)mode. The results showed that the good linear relationship between the chromatography peak area and the mass concentration of four pesticide residues in the range of 2-500 μg/L, the correlation coefficients were all more than 0.991, the detection limits were 0.02-1.25 μg/kg, and the quantitation limits were 0.05-5.0 μg/kg. In the two substrates of citrus and brassica campestris, the recoveries were 71.6%-109% and 82.0%-109%, respectively. The relative standard deviations were not more than 14.4% (n=6). The method is convenient, rapid, accurate and reliable. It is suitable for the determination of diafenthiuron, fluopicolide, fluxapyroxad and spirotetramat in vegetables and fruits. 
关键词:高效液相色谱-质谱联用法;果蔬;丁醚脲;氟吡菌胺;氟唑菌酰胺;螺虫乙酯 
Keywords:HPLC-MS; fruits and vegetables; diafenthiuron; fluopicolide; fluxapyroxad; spirotetramat 
基金:广西壮族自治区直属公益性科研院所基本科研业务费专项课题(2019ACZ03) 
本文引用格式:
张思敏,梁跃,苏梅清,等.高效液相色谱-质谱联用法同时测定果蔬中丁醚脲、氟吡菌胺、氟唑菌酰胺、螺虫乙酯[J].化学分析计量,2021,30(4):15.
Zhang Simin,Liang Yue,Su Meiqing,et al. Simultaneous determination of diafenthiuron,fluopicolide,fluxapyroxad and spirotetramat in fruits and vegetables by high performance liquid chromatography-mass spectrometry[J]. Chemical Analysis and Meterage,2021,30(4):15. 

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