分散液液微萃取-气相色谱-质谱法测定鱼塘水中24种农药
发布时间:2018-04-17 15:05
本文选题:分散液液微萃取 + 气相色谱-质谱法 ; 参考:《理化检验(化学分册)》2017年12期
【摘要】:采用分散液液微萃取结合气相色谱-质谱法同时快速测定鱼塘水中24种常见农药。在水样5.00mL中快速加入乙醇1.0mL、四氯乙烯30μL,形成乳浊液,静置5min后,以4 000r·min~(-1)转速离心5min,有机相在VF-5MS毛细管色谱柱上分离,质谱分析中选择电子轰击离子源和选择离子监测模式。24种农药的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在0.33~7.45μg·L~(-1)之间。加标回收率在72.4%~103%之间,测定值的相对标准偏差(n=6)在1.7%~13%之间。该方法成功应用于鱼塘投毒案件中硫丹α、硫丹β和甲氰菊酯的检测。
[Abstract]:Dispersion liquid microextraction combined with gas chromatography-mass spectrometry (GC-MS) was used to determine 24 common pesticides in fish pond water.Ethanol 1.0 mL and tetrachloroethylene 30 渭 L were rapidly added to the water sample 5.00mL to form emulsion. After 5min was still set up, the organic phase was separated on VF-5MS capillary column for 5 min at 4 000 r / min ~ (-1) rotating speed.In mass spectrometry, the mass concentration of electron bombardment ion source and ion monitoring mode .24 pesticides showed a linear relationship with the peak area in a certain range, and the detection limit of 3s / N was between 0.33 ~ 7.45 渭 g / L ~ (-1)).The recoveries were between 72.4% and 103%, and the relative standard deviations of the determination values were between 1.7and 13%.The method has been successfully applied to the detection of endosulfan 伪, endosulfan 尾 and cypermethrin in fish pond poisoning cases.
【作者单位】: 江苏省江阴市公安局;江苏省无锡市公安局;
【分类号】:O657.63;X839.2
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本文编号:1764101
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