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
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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 pyrrolidone 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 infrared 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 extraction 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 1μg·L~(-1)~ 20μg·L~(-1). The detection limits of 5herbicides were 0. 067 μg·L~(-1)、0. 091 μg·L~(-1)、0. 114 μg·L~(-1)、0. 076 μg·L~(-1)、0. 117 μg·L~(-1),respectively.
In the paper,use methyl methacrylate and styrene as raw materials,divinylbenzene as crosslinking agent,polyvinyl pyrrolidone 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 infrared 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 extraction 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 1μg·L~(-1)~ 20μg·L~(-1). The detection limits of 5herbicides were 0. 067 μg·L~(-1)、0. 091 μg·L~(-1)、0. 114 μg·L~(-1)、0. 076 μg·L~(-1)、0. 117 μg·L~(-1),respectively.
引文
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[4]吴春英,白鹭,谷风.固相萃取-超高效液相色谱-串联质谱法同时测定地表水中的18种酰胺类除草剂[J].理化检验:化学分册,2016,52(5):602-606.
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[7]陈冬东,侯士聪,代汉慧,等.固相萃取/超高效液相色谱-串联质谱法测定食品中涕灭威及其代谢产物涕灭威亚砜与涕灭威砜残留量[J].分析测试学报,2011,30(12):1367-1371.
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[10]傅若农.用于色谱分析固相萃取(SPE)技术的演变和现状[J].化学试剂,2007,21(1):15-22.
[11]张海霞,朱彭龄.固相萃取[J].分析化学,2000,28(9):1172-1180.
[12]王萍.固相萃取新技术研究进展[J].水质监测,2015,(1):44-45.
[13]彭媛,范云鸽,马建标.固相萃取中使用的聚合物载体[J].高分子材料科学与工程,2007,23(4):1-4.
[14]Tsyurupa M P,Ilyin M M,Andreeva A I,et al.Use of the hyper crosslinked polystyrene sorbents"Styrosorb"for solid phase extraction of phenols from water[J].Fresenius J Anal Chem,1995,352:565-571.
[15]Mohamed G Mahfouz,Hamada M Killa,Mohamed E Sheta,et al.Synthesis,characterization,and application of polystyrene adsorbents containing tri-n-butylphosphate for solid-phase extraction of uranium(VI)from aqueous nitrate solutionsr[J].J Radioanal Nucl Chem,2014,301:739-749.
[16]包建民,谢丹,孙超慧,等.一种亲水-亲油复合固相萃取填料的制备及其在食品安全检测中的应用[J].色谱,2013,31(9):825-830.
[17]申书昌,徐雅雯,马柏凤.弱酸型聚合物微球固相萃取填料的制备及水中杀虫剂的测定[J].化学研究与应用,2015,27(9):1289-1294.
[18]陆馨,辛忠,杨海.分散聚合法制备甲基丙烯酸甲酯-苯乙烯共聚物微球[J].功能高分子学报,2005,18(2):310-315.
[19]刘兰珍,金顺子,张宪宗,等.苯乙烯/甲基丙烯酸甲醋共聚物组分的测定[J].分析化学,1982,10(6):371-373.
[2]马又娥,刘宝峰.环境水中7种酰胺类和磺酰脲类除草剂残留检测方法研究[J].现代农药,2011,10(4):44-46.
[3]杨丽华,龚道新,唐晶.高效液相色谱法同时测定稻田中苄嘧磺隆和苯噻酰草胺残留[J].色谱,2012,30(1):71-75.
[4]吴春英,白鹭,谷风.固相萃取-超高效液相色谱-串联质谱法同时测定地表水中的18种酰胺类除草剂[J].理化检验:化学分册,2016,52(5):602-606.
[5]姜莲华,马继平,侯丽玮.固相萃取-高效液相色谱法测定地表水中10种磺酰脲类除草剂[J].青岛理工大学学报.2015,36(5):73-79.
[6]易盛国,杨晓凤,侯雪,等.GC/MS方法分析豇豆中水胺硫磷等37种农药残留[J].化学研究与应用,2011,23(1):96-101.
[7]陈冬东,侯士聪,代汉慧,等.固相萃取/超高效液相色谱-串联质谱法测定食品中涕灭威及其代谢产物涕灭威亚砜与涕灭威砜残留量[J].分析测试学报,2011,30(12):1367-1371.
[8]Uitema A D,Reinders C,Tibben M M,et al.Sensitive gas chromatographic determineation of the cyclophosphamide metabolite 2-dechloroethyl cyclophosphamide in human plasma[J].J Chromatogr Biomed Appl,2001,757(2):349-357.
[9]孙海红,钱叶苗,宋相丽,等.固相萃取技术的应用与研究新进展[J].现代化工,2011,31(2):21-26.
[10]傅若农.用于色谱分析固相萃取(SPE)技术的演变和现状[J].化学试剂,2007,21(1):15-22.
[11]张海霞,朱彭龄.固相萃取[J].分析化学,2000,28(9):1172-1180.
[12]王萍.固相萃取新技术研究进展[J].水质监测,2015,(1):44-45.
[13]彭媛,范云鸽,马建标.固相萃取中使用的聚合物载体[J].高分子材料科学与工程,2007,23(4):1-4.
[14]Tsyurupa M P,Ilyin M M,Andreeva A I,et al.Use of the hyper crosslinked polystyrene sorbents"Styrosorb"for solid phase extraction of phenols from water[J].Fresenius J Anal Chem,1995,352:565-571.
[15]Mohamed G Mahfouz,Hamada M Killa,Mohamed E Sheta,et al.Synthesis,characterization,and application of polystyrene adsorbents containing tri-n-butylphosphate for solid-phase extraction of uranium(VI)from aqueous nitrate solutionsr[J].J Radioanal Nucl Chem,2014,301:739-749.
[16]包建民,谢丹,孙超慧,等.一种亲水-亲油复合固相萃取填料的制备及其在食品安全检测中的应用[J].色谱,2013,31(9):825-830.
[17]申书昌,徐雅雯,马柏凤.弱酸型聚合物微球固相萃取填料的制备及水中杀虫剂的测定[J].化学研究与应用,2015,27(9):1289-1294.
[18]陆馨,辛忠,杨海.分散聚合法制备甲基丙烯酸甲酯-苯乙烯共聚物微球[J].功能高分子学报,2005,18(2):310-315.
[19]刘兰珍,金顺子,张宪宗,等.苯乙烯/甲基丙烯酸甲醋共聚物组分的测定[J].分析化学,1982,10(6):371-373.