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
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摘要
本文制备了聚合物基质弱酸型阳离子交换固相萃取填料,以甲基丙烯酸和苯乙烯为原料,二乙烯基苯为交联剂,聚乙烯醇为分散剂,过氧化苯甲酰为引发剂,采用悬浮聚合法制备了具有亲脂和弱阳离子交换性能的球形固相萃取填料,并对其结构和形貌进行了表征。以该聚合物微球作为填料制备固相萃取小柱,萃取水中联硝氯酚、硫双二氯酚、吡喹酮和丙硫苯咪唑4种杀虫剂,乙腈为洗脱剂,洗脱液采用液相色谱分析。分别考察了样品的p H值和流速、洗脱剂的体积和流速对萃取回收率的影响,确定了最佳固相萃取条件。选择了最佳色谱分析条件。结果表明,该聚合物微球单分散性好,自制固相萃取小柱对水中4种杀虫剂的吸附性能好,与HPLC联用测定结果重现性好,联硝氯酚、硫双二氯酚、吡喹酮和丙硫苯咪唑的最低检测限分别为0.26μg·L-1、0.31μg·L-1、0.42和0.63μg·L-1。
The polymer microspheres with lipotropy and weak cation exchange performance were prepared through suspension polymerization method using styrene and divinyl benzene and methyl acrylate as monomers,PVA as dispersant,benzoyl peroxide as the initiator. The structure and morphology of microspheres were examined by infrared spectrum and scanning electron microscope. While observing the structure and morphology of the filler. The composite microspheres were used as solid-phase extraction( SPE) sorbents for selective extraction nitroclofene,bithionol,praziquantel and albendazole in the river water. Acetonitrile was used as eluent,and the eluate was determined by high performance liquid chromatography. The effects of the sample flow rate and p H,volume and flow rate of eluent on adsorption ratios were investigated,the best solid phase extraction conditions were obtained. The best HPLC condition was chosen. The results show that Si O2/ PS composite microspheres have a uniform monodispersity in particle size. The SPE sorbents have good adsorption performance to nitroclofene,bithionol,praziquantel and albendazole in water,and the method of SPE-HPLC for determining the four pesticides has good reproducibility,the detection limits for nitroclofene,bithionol,praziquantel and albendazole were 0. 26μg·L-1,0. 31μg·L-1,0. 42μg·L-1and 0. 63μg·L-1respectively
The polymer microspheres with lipotropy and weak cation exchange performance were prepared through suspension polymerization method using styrene and divinyl benzene and methyl acrylate as monomers,PVA as dispersant,benzoyl peroxide as the initiator. The structure and morphology of microspheres were examined by infrared spectrum and scanning electron microscope. While observing the structure and morphology of the filler. The composite microspheres were used as solid-phase extraction( SPE) sorbents for selective extraction nitroclofene,bithionol,praziquantel and albendazole in the river water. Acetonitrile was used as eluent,and the eluate was determined by high performance liquid chromatography. The effects of the sample flow rate and p H,volume and flow rate of eluent on adsorption ratios were investigated,the best solid phase extraction conditions were obtained. The best HPLC condition was chosen. The results show that Si O2/ PS composite microspheres have a uniform monodispersity in particle size. The SPE sorbents have good adsorption performance to nitroclofene,bithionol,praziquantel and albendazole in water,and the method of SPE-HPLC for determining the four pesticides has good reproducibility,the detection limits for nitroclofene,bithionol,praziquantel and albendazole were 0. 26μg·L-1,0. 31μg·L-1,0. 42μg·L-1and 0. 63μg·L-1respectively
引文
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[2]Michelle L Hladik,Kelly L Smalling,Kathryn M Kuivila.A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extractionand gas chromatography-ion trap mass spectrometry[J].Bull Environ Contam Toxicol,2008,80:139-44.
[3]Evangelia Terzopoulou,Dimitra Voutsa,George Kaklamanos.A multi-Residue method for determination of 70 organic micropollutants in surface waters by solid-phase extraction followed by gas chromatography coupled to tandem mass spectrometry[J].Evironmental Science and Pollution Research,2015,22:1095-1112.
[4]黄运瑞,周庆祥.固相萃取吸附剂的研究进展[J].冶金分析,2012,32(12):22-28.
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[7]Rezaei B,Mallakpour S,Rahmanian O.Application of molecularly imprinted polymer for solid phase extraction and preconcentration of hydrochlorothiazide in pharmaceutical and serum sampleanalysis[J].J Iran Chem Soc,2010,7(4):1004-1011.
[8]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.
[9]张洪涛,吕睿,陈敏.分散共聚合制备PSt-AA-EGDMA功能性单分散微米级交联微球的研究[J].高等学校化学学报,2004,25(2):366-371.
[10]熊颖辉,李红,李慧芝,等.悬浮共聚法合成功能性微米级单分散交联聚苯乙烯微球[J].石油化工,2008,37(5):502-506.
[11]Bo Fu,Han-Cheng Yu,Jin-Wang Huang,et al.Synthesis and catalytic activities in cyclohexane hydroxylation of metalloporphyrins supported on styrene-methylacrylic acid copolymer microspheres[J].Transition Met Chem,2008,33:803-807.
[12]王忠磊,寇景轩,胡颖新.阿苯达唑、吡喹酮联合应用治疗脑囊虫病临床研究[J].中国热带医学,2008,8(11):1873-1876
[13]倪泽成,刘辛赟,武占银.银川地区羊肝中阿苯达唑(丙硫苯咪唑)残留情况的调查[J].中国动物检疫,2004,21(9):29-30.
[14]任晋,黄翠玲,赵国栋,等.固相萃取-高效液相色谱-质谱联机在线分析水中痕量除草剂[J].分析化学,2001,29(8):876-880.
[2]Michelle L Hladik,Kelly L Smalling,Kathryn M Kuivila.A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extractionand gas chromatography-ion trap mass spectrometry[J].Bull Environ Contam Toxicol,2008,80:139-44.
[3]Evangelia Terzopoulou,Dimitra Voutsa,George Kaklamanos.A multi-Residue method for determination of 70 organic micropollutants in surface waters by solid-phase extraction followed by gas chromatography coupled to tandem mass spectrometry[J].Evironmental Science and Pollution Research,2015,22:1095-1112.
[4]黄运瑞,周庆祥.固相萃取吸附剂的研究进展[J].冶金分析,2012,32(12):22-28.
[5]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.
[6]Masque'N,Gali'M,Marce'R M,et al.Influence of chemical modification of polymeric resin on retention of polar compounds in solid-phase extraction[J].Chromatographia,1999,50(1/2):21-26.
[7]Rezaei B,Mallakpour S,Rahmanian O.Application of molecularly imprinted polymer for solid phase extraction and preconcentration of hydrochlorothiazide in pharmaceutical and serum sampleanalysis[J].J Iran Chem Soc,2010,7(4):1004-1011.
[8]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.
[9]张洪涛,吕睿,陈敏.分散共聚合制备PSt-AA-EGDMA功能性单分散微米级交联微球的研究[J].高等学校化学学报,2004,25(2):366-371.
[10]熊颖辉,李红,李慧芝,等.悬浮共聚法合成功能性微米级单分散交联聚苯乙烯微球[J].石油化工,2008,37(5):502-506.
[11]Bo Fu,Han-Cheng Yu,Jin-Wang Huang,et al.Synthesis and catalytic activities in cyclohexane hydroxylation of metalloporphyrins supported on styrene-methylacrylic acid copolymer microspheres[J].Transition Met Chem,2008,33:803-807.
[12]王忠磊,寇景轩,胡颖新.阿苯达唑、吡喹酮联合应用治疗脑囊虫病临床研究[J].中国热带医学,2008,8(11):1873-1876
[13]倪泽成,刘辛赟,武占银.银川地区羊肝中阿苯达唑(丙硫苯咪唑)残留情况的调查[J].中国动物检疫,2004,21(9):29-30.
[14]任晋,黄翠玲,赵国栋,等.固相萃取-高效液相色谱-质谱联机在线分析水中痕量除草剂[J].分析化学,2001,29(8):876-880.
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