华中农业大学食品科学技术学院/环境食品学教育部重点实验室/ 果蔬加工与品质调控湖北省重点实验室，武汉 430070
崔瑞霞，E-mail： 2678598308@qq.com.
李秀娟，E-mail： lixiujuan@mail.hzau.edu.cn.
O657.3;TS207.5+3
海南省科技厅重点研发计划项目（ZDYF2021XDNY304）；中央高校基本科研业务费专项（2662020SPPY015）；湖北省农业科技创新中心项目（2019-620-000-001-31）
College of Food Science and Technology，Huazhong Agricultural University/ Key Laboratory of Environment Correlative Dietology， Ministry of Education/Hubei Key Laboratory of Fruit & Vegetable Processing & Quality Control，Wuhan 430070，China
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为满足豇豆中极性农药的检测需求，在MCM-41介孔硅表面聚合二乙烯基苯（DVB）、N-乙烯基吡咯烷酮（NVP）和4-丙烯酰吗啉（ACMO），得到ACMO-co-DVB-co-NVP@MCM-41材料；采用扫描电子显微镜、傅立叶变换红外光谱仪、热重分析仪、N2-物理吸附脱附等手段对材料进行了表征；以该材料制得固相微萃取萃取头，采用直接固相微萃取与气相色谱-氮磷检测器联用，建立了豇豆（Vigna unguiculata （L.） Walp.）中灭多威、克百威和灭蝇胺3种极性农药的检测方法。结果显示：在优化的条件下，3种农药的线性关系良好，决定系数均大于0.99，检出限为1.71~18.79 μg/kg，定量限为5.71~62.63 μg/kg。3种农药的加标回收率为84.4%~116.1%，相对标准偏差为2.2%~7.5%。结果表明，该方法具有较好的灵敏度、准确性和可靠性，可以满足国家规定豇豆中农药的最大残留限量检测。
ACMO-co-DVB-co-NVP@MCM-41 material was obtained by polymerizing divinylbenzene （DVB）， N-vinylpyrrolidone （NVP） and 4-acryloylmorpholine （ACMO） on MCM-41 mesoporous microspheres to meet the requirements of detecting polar pesticides in cowpea. The material was characterized with scanning electron microscope， Fourier transform infrared spectrometer， thermogravimetric analyzer and N2 adsorption-desorption. Solid-phase microextraction （SPME） fibers were prepared from this material. A method for determining methomyl， carbofuranandcyromazine in cowpea was established by direct immersion-SPME combined with gas chromatography-nitrogen phosphorus detector. Under the optimized extraction conditions， the linear relationship of the three pesticides was good， the coefficients of determination were all greater than 0.99， with the detection limits of 1.71-18.79 μg/kg and the quantification limits of 5.71-62.63 μg/kg. The recoveries of 3 pesticides ranged from 84.4% to 116.1%， and the relative standard deviations ranged from 2.2%-7.5%. It is indicated that the method established has good sensitivity， accuracy and reliability， and can satisfy the maximum residue limit （MRL） of pesticide in cowpea. Compared with the popular coating made from hydrophilic-lipophilic balance particles， it has a large extraction capacity and a stronger extraction performance for strong polar substances， which will have a good application prospect in the extraction of non-targeted analytes.
引用本文
崔瑞霞,向孝哲,孙鑫,张小帆,李秀娟. ACMO-co-DVB-co-NVP@MCM-41的制备及其在豇豆农药固相微萃取中的应用[J].华中农业大学学报,2022,41(5):257-265
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- 收稿日期:2022-06-24
- 在线发布日期: 2022-10-11
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