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分散液液微萃取-氣相色譜-質(zhì)譜法測(cè)定魚(yú)塘水中24種農(nóng)藥

發(fā)布時(shí)間:2018-04-17 15:05

  本文選題:分散液液微萃取 + 氣相色譜-質(zhì)譜法 ; 參考:《理化檢驗(yàn)(化學(xué)分冊(cè))》2017年12期


【摘要】:采用分散液液微萃取結(jié)合氣相色譜-質(zhì)譜法同時(shí)快速測(cè)定魚(yú)塘水中24種常見(jiàn)農(nóng)藥。在水樣5.00mL中快速加入乙醇1.0mL、四氯乙烯30μL,形成乳濁液,靜置5min后,以4 000r·min~(-1)轉(zhuǎn)速離心5min,有機(jī)相在VF-5MS毛細(xì)管色譜柱上分離,質(zhì)譜分析中選擇電子轟擊離子源和選擇離子監(jiān)測(cè)模式。24種農(nóng)藥的質(zhì)量濃度在一定范圍內(nèi)與峰面積呈線性關(guān)系,檢出限(3S/N)在0.33~7.45μg·L~(-1)之間。加標(biāo)回收率在72.4%~103%之間,測(cè)定值的相對(duì)標(biāo)準(zhǔn)偏差(n=6)在1.7%~13%之間。該方法成功應(yīng)用于魚(yú)塘投毒案件中硫丹α、硫丹β和甲氰菊酯的檢測(cè)。
[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 偽, endosulfan 尾 and cypermethrin in fish pond poisoning cases.
【作者單位】: 江蘇省江陰市公安局;江蘇省無(wú)錫市公安局;
【分類號(hào)】:O657.63;X839.2
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本文編號(hào):1764101

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