亲水-亲油聚合物型固相萃取材料的制备及其在除草剂残留萃取分析中的应用  

Preparation of hydrophile lipophile polymer solid phase extraction filler and its application for determining herbicide

作　　者：申书昌[1] 吕伟超[1] 戴建华[2] 

机构地区：[1]齐齐哈尔大学分析测试中心,黑龙江齐齐哈尔161006 [2]齐齐哈尔市疾病预防控制中心,黑龙江齐齐哈尔161000

出　　处：《化学研究与应用》2017年第9期1295-1300,共6页Chemical Research and Application

基　　金：黑龙江省自然科学基金项目(B201101)资助

摘　　要：本文以甲基丙烯酸甲酯(MMA)和苯乙烯(St)为原料,二乙烯基苯(DVB)为交联剂,聚乙烯吡咯烷酮(PVP)为分散剂,偶氮二异丁腈(AIBN)为引发剂,采用分散聚合法制备了亲水-亲油聚合物型固相萃取填料。采用红外光谱和扫描电子显微镜分别表征了聚合物微球的结构、形貌及粒径。用该填料和聚丙烯管制成固相萃取小柱,分别萃取水溶液中烟嘧磺隆、吡嘧磺隆、苄嘧磺隆、利谷隆、戊炔草胺,用甲醇洗脱后经超高效液相色谱分析。考察了固相萃取填料对5种除草剂的吸附量,分别为55.7mg·g^(-1)、46.8mg·g^(-1)、70.8mg·g^(-1)、93.2mg·g^(-1)、61.5mg·g^(-1)。在1μg·L^(-1)~20μg·L^(-1)浓度范围内,5种组分的峰面积与浓度呈良好的线性关系,烟嘧磺隆、吡嘧磺隆、苄嘧磺隆、利谷隆、戊炔草胺的检出限分别为0.067μg·L^(-1)、0.091μg·L^(-1)、0.114μg·L^(-1)、0.076μg·L^(-1)、0.117μg·L^(-1)。In the paper,use methyl methacrylate and styrene as raw materials,divinylbenzene as crosslinking agent,polyvinyl pyrro- lidone as dispersing agent,2,2-azobisisobutyronitrile as initiator,the hydrophile lipophile polymer solid phase extraction packing was prepared by dispersion polymerization. The structure, morphology and particle size of polymer microspheres were characterized by in-frared spectroscopy and scanning electron microscopy. The solid phase extraction column was made by the polymer filler and the polypropylene tube,then extract nicosulfuron,pyrazosulfuron,bensulfuron methyl,linuron and propyzamide in water. The pesticides were eluted by methanol,and detected by ultra performance liquid chromatography. The adsorption capacities of the solid phase ex-traction packing for 5 herbicides were 55. 7mg · g^- 1 ,46. 8mg · g^- 1,70. 8mg · g^- 1,93. 2mg· g^- 1 ,61. 5mg · g^- 1 Respectively. There was good linearity between the peak area and concentration of 5 herbicide residues within 1 μg · L^-12 0 μg · L^-1. T h e detection limits of 5 herbicides were 0. 067 （μg · L^-1、 0. 09 1 （μg · L^-1、 0. 11 4 μg · L^-1、 0. 0 7 6 （μg · L^-1、 0. 117 （μg · L^-1, respectively.

关 键 词：固相萃取填料 分散聚合 甲基丙烯酸甲酯-苯乙烯共聚物微球 超高效液相色谱 除草剂 

分 类 号：O657.7[理学—分析化学]