超高效液相色谱-串联质谱法测定莲雾中多菌灵、噻菌灵和甲霜灵残留
投稿时间：2015-04-11      点此下载全文 HTML
引用本文：李春丽,乐渊,尹桂豪,等.超高效液相色谱-串联质谱法测定莲雾中多菌灵、噻菌灵和甲霜灵残留[J].农药学学报,2015,17(5):579-584.
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作者单位E-mail
李春丽 中国热带农业科学院 分析测试中心, 海口 571101  
乐渊 中国热带农业科学院 分析测试中心, 海口 571101  
尹桂豪 中国热带农业科学院 分析测试中心, 海口 571101  
阳辛凤 中国热带农业科学院 分析测试中心, 海口 571101  
黎舒怀 中国热带农业科学院 分析测试中心, 海口 571101  
刘春华 中国热带农业科学院 分析测试中心, 海口 571101 chunhualiu111@126.com 
中文摘要:建立了莲雾中多菌灵、噻菌灵和甲霜灵残留的超高效液相色谱-串联质谱(UPLC-MS/MS)的快速检测方法。样品直接用乙腈匀浆提取,过0.22 μm滤膜后,在电喷雾正离子模式下以多反应监测(MRM)模式测定,基质匹配标准溶液外标法定量。结果表明:方法的线性范围为0.01~0.5 μg/mL,决定系数(R2)>0.99;在0.04、0.4和2 mg/kg 3个添加水平下,方法的平均回收率为75%~107%,相对标准偏差为2.0%~8.9%(n=5),定量限均为0.04 mg/kg。该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求。
中文关键词:超高效液相色谱-串联质谱(UPLC-MS/MS)  莲雾  多菌灵  噻菌灵  甲霜灵  残留
 
Determination of carbendazim,thiabendazole and metalaxyl residues in wax-apple by ultra performance liquid chromatography-tandem mass spectrometry
Abstract:A rapid method for determining carbendazim, thiabendazole and metalaxyl residue in wax-apples was developed with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) detection. The samples were extracted with acetonitrile. The samples were detected by UPLC-MS/MS under positive electrospray ionization and multiple reaction monitoring mode. The matrix-matched external standard calibration curves were used for the quantitative analysis. It was shown that the calibration curves were linear in the range of 0.01-0.5 μg/mL and coefficient of determination R2>0.99.The limits of quantitation were 0.04 mg/kg. The average recoveries of the three pesticides were 75%-107% at spiked levels of 0.04, 0.4 and 2 mg/kg, with relative standard deviations in the range of 2.0%-8.9% (n=5). The sample pretreatment of the method is simple and time-saving. The method is applied for detection of carbendazim, thiabendazole and metalaxyl residues in market wax-apples.
Key words:ultra performance liquid chromatography-tandem mass spectrometry  wax-apple  carbendazim  thiabendazole  metalaxyl  residue
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