分子印迹固相萃取膜-高效液相色谱法检测粮谷中腈菌唑残留  

Determination of Myclobutanil in Grains by Molecularly Imprinted Solid Phase Extraction Membrane- High Performance Liquid Chromatography

作　　者：王姣姣[1] 庞军[1] 刘博[1] 高文惠[1] 

机构地区：[1]河北科技大学生物科学与工程学院河北省发酵工程技术研究中心,石家庄050000

出　　处：《中国粮油学报》2015年第5期133-137,142,共6页Journal of the Chinese Cereals and Oils Association

基　　金：河北省科技支撑计划(14227504D;14236602D-13)

摘　　要：以腈菌唑为模板分子,丙烯酰胺（AM）为功能单体,乙二醇二甲基丙烯酸酯（EDMA）为交联剂,模板分子与功能单体最佳浓度配比为1∶2,制备出对腈菌唑具有高选择性的分子印迹固相萃取膜。通过紫外光谱试验考察了制备印迹膜时致孔剂的选择和分子印迹膜印迹次数对液体通过性的影响。建立了基于分子印迹固相萃取膜-高效液相色谱法测定粮谷中腈菌唑残留的方法。样品经乙腈提取,固相萃取膜净化,经C18柱分离,紫外检测210 nm。结果表明,腈菌唑在0.3～20μg/m L浓度范围内有良好的线性关系（r=0.999 4）,平均回收率在80.2%～86.0%之间,相对标准偏差（RSD）≤3.3%（n=5）,检出限为1.2μg/g。该方法选择性强、灵敏、可靠,适用于粮谷等复杂基质中腈菌唑的残留检测。Molecularly imprinted sold phase extraction membrane with high selectivity to myclobutanil had been prepared with myclobutanil as template molecular, acrylamide （AM） as functional monomer and ethylene dimethacrylate （EDMA） as cross - linker. The optimal concentration ratio of myclobutanil and acrylamide （AM） was C （M） ： C （AM） = 1 ： 2. UV spectra were applied to study the selection of porogen in preparation of molecularly imprinted membrane. The influence of imprinted times on liquid passing nature had also been researched. A molecularly imprinted solid phase membrane - high＇ s performance liquid chromatographic method was developed for the determi- nation approach of myclobutanil residues in grains. The grain samples were extracted with acetonitrile, cleaned up by the sold phase extraction membrane, separated with C18 column and determined at 210 nm. The results showed that a favorable linear range of 0.3 ～ 20 μg/mL of myclobutanil with r = 0. 999 4 has been obtained with the average recoveries ranged from 80.2% to 86.0% , and the relative standard deviations （RSDs） were proved to be less than 3.3 % （ n = 5 ） ; the detection limit of myclobutanil was 1.2 μg/g. The method was selective, sensitive and reliable, and could be applied to determine myclobutanil residues in grain samples.

关 键 词：粮谷 腈菌唑 分子印迹固相萃取膜 高效液相色谱法 

分 类 号：O657.32[理学—分析化学]