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    改进的QuEChERS方法结合在线凝胶色谱-气相色谱-串联质谱法测定茶叶中39种有机磷农药的含量

    Determination of 39 Organophosphorus Pesticides in Tea by Online Gel Permeation Chromatography-Gas Chromatography Tandem Mass Spectrometry Coupled with Modified QuEChERS Method

    • 摘要: 将茶叶样品4.000 0 g、乙腈10.0 mL和4.00 mg·L-1环氧七氯内标溶液400 μL涡漩混合1 min,超声提取15 min,离心后取上清液1.0 mL,加入甲苯1 mL,经含N-丙基乙二胺(PSA)30 mg、C18 30 mg、石墨化炭黑(GCB)15 mg和无水硫酸镁150 mg的分散固相萃取吸附剂净化后,采用在线凝胶色谱-气相色谱-串联质谱法(Online GPC-GC-MS/MS)测定净化溶液中39种有机磷农药残留量。结果表明:39种有机磷农药在一定范围内呈线性关系,检出限(3S/N)为0.5~4.3 μg·kg-1。按标准加入法进行回收试验,回收率为83.1%~105%,相对标准偏差(n=6)均小于9.0%。

       

      Abstract: The tea sample of 4.000 0 g, acetonitrile of 10.0 mL and 4.00 mg·L-1 heptachlor epoxide internal standard solution of 400 μL were swirled for 1 min, and extracted ultrasonically for 15 min. After centrifugation, the supernatant of 1.0 mL was taken and toluene of 1 mL was added. The mixture was purified with dispersive solid phase extraction adsorbents containing PSA of 30 mg, C18 of 30 mg, GCB of 15 mg, and anhydrous magnesium sulfate of 150 mg, and 39 organophosphorus pesticides in the purified solution were determined by online gel permeation chromatography-gas chromatography tandem mass spectrometry (Online GPC-GC-MS/MS). As shown by the results, linear relationships of 39 organophosphorus pesticides were found in definite ranges, with detection limits (3S/N) in the range of 0.5-4.3 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 83.1%-105%, with RSDs (n=6) all less than 9.0%.

       

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