| 聚合物整体柱在线固相萃取/高效液相色谱法测定水果中敌灭灵与伏虫灵 |
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| 基金项目:国家自然科学基金（21305028）；河北省自然科学基金（H2017209232，H2016209018）；河北省教育厅重点项目（ZD2018014）；华北理工大学培育基金项目（JQ201717） |
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| 中文摘要:构筑了以甲基丙烯酸异辛酯（EHMA）为单体，乙二醇二甲基丙烯酸酯（EDMA）为交联剂的聚合物整体柱（10 mm × 46 mm，id.）作为在线固相萃取吸附剂，结合高效液相色谱紫外检测器，建立了水果中苯甲酰类农药敌灭灵和伏虫灵的分析方法。构筑的聚合物整体柱结构多孔，比表面积为16401 m2·g-1，将其作为在线固相萃取净化柱，样品在01 mL·min-1流速下经5 mmol·L-1乙酸铵溶液上样，10 mL·min-1条件下以乙腈-水（65∶35，体积比）洗脱后，进入C18柱分析。该方法在01~500 mg·L-1范围内线性关系良好（r≥0998），对敌灭灵和伏虫灵的检出限分别为0007 2、0009 mg·kg-1，定量下限分别为0024、0030 mg·kg-1。在003、03、15 mg·kg-13个加标水平下的回收率为895%~102%，日内和日间相对标准偏差不大于68%。 |
| 中文关键词:苯甲酰类农药 聚合物整体柱 在线固相萃取 高效液相色谱（HPLC） 水果 |
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| Determination of Diflubenzuron and Hexaflumuron in Fruits by High Performance Liquid Chromatography with Online Polymeric Monolithic Column Solid phase Extraction |
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| Abstract:A method based on high performance liquid chromatography（HPLC） with online monolithic column solid phase extraction was developed for the determination of diflubenzuron and hexa flumuron in fruits. The polymer（poly（2 ethylhexyl methacrylate co ethylene dimethacrylate）） monolithic column（10 mm×46 mm，id.） was prepared by using 2 ethylhexyl methacrylate（EHMA） as monomer and ethylene dimethacrylate（EDMA） as crosslinker，which exhibited a porous structure with a specific surface area of 16401 m2·g-1. Using polymer monolithic column as online solid phase extraction sorbent，the extracted fruit sample solution was loaded into the monolithic column using 5 mmol·L-1 NH4OAc at a flow rate of 01 mL·min-1. The adsorbed analytes were transferred from monolithic column to the analytical column using acetonitrile-water（65∶35，by volume） as mobile phase at a flow rate of 10 mL·min-1. Under the optimized conditions，there was a good linearty for the method in the range of 01-500 mg·L-1（r≥0998）. The limits of detection and quantitation for diflubenzuron and hexaflumuron were 0007 2 mg·kg-1 and 0009 mg·kg-1，and 0024 mg·kg-1 and 0030 mg·kg-1，respectively. The recoveries at three spiked levels of 003，03 and 15 mg·kg-1 were in the range of 895%-102% with intra day and inter day relative standard deviations not more than 68%. |
| Key Words:benzoylurea insecticides polymer based monolithic column online solid phase extraction high performance liquid chromatography（HPLC） fruit |
| 引用本文：念琪循，李娜，贾叶青，利利，李冬梅，王阳，王曼曼，王学生.聚合物整体柱在线固相萃取/高效液相色谱法测定水果中敌灭灵与伏虫灵[J].分析测试学报,2018,37(8):900-905. |
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