分子印迹磁固相萃取/气相色谱法分析环境水样中5种酰胺类除草剂残留
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摘要
以丁草胺为假模板分子,丙烯酰胺为功能单体,利用四氧化三铁磁性纳米微球成功制备了具有特异性识别能力的磁性分子印迹聚合物。采用透射电子显微镜、红外光谱和振动样品磁强计对印迹聚合物进行表征,结果显示,分子印迹聚合物成功包裹在四氧化三铁表面。印迹聚合物对5种酰胺类除草剂均有特异性识别作用。以磁性分子印迹聚合物为基础,建立了酰胺类除草剂的气相色谱检测方法。方法学验证表明该方法具有良好的回收率(85.0%~99.5%)和精密度(RSD为2.8%~5.0%,n=5),线性范围为0.1~500μg·L~(-1),检出限为0.02~0.05μg·L~(-1)。该方法能够应用于农田灌溉用水等环境水样的测定。
Magnetic molecularly imprinted polymers( MMIPs) with specific recognition ability were successfully synthesized by using butachlor as template molecule and acrylamide( AM) as functional monomer. MMIPs were characterized by transmission electron microscopy( TEM),infrared spectroscopy( FT-IR) and vibrating sample magnetometry( VSM). The results showed that molecularly imprinted layer was successfully wrapped on the surface of Fe3O4. MMIPs showed a specific recognition for five chloroacetamide herbicides. The developed magnetic molecular imprinted solid phase extraction coupled with gas chromatography( MMISPE/GC) method exhibited a good recovery( 85. 0%-99. 5%),a good precision( RSD: 2. 8%-5. 0%,n = 5),a good linearity( 0. 1-500 μg·L~(-1)) and a low limit of detection( 0. 02-0. 05 μg · L~(-1)) under the optimized conditions. The introduced MMISPE/GC method was successfully used to analyze five chloroacetamide herbicides in environmental water samples.
Magnetic molecularly imprinted polymers( MMIPs) with specific recognition ability were successfully synthesized by using butachlor as template molecule and acrylamide( AM) as functional monomer. MMIPs were characterized by transmission electron microscopy( TEM),infrared spectroscopy( FT-IR) and vibrating sample magnetometry( VSM). The results showed that molecularly imprinted layer was successfully wrapped on the surface of Fe3O4. MMIPs showed a specific recognition for five chloroacetamide herbicides. The developed magnetic molecular imprinted solid phase extraction coupled with gas chromatography( MMISPE/GC) method exhibited a good recovery( 85. 0%-99. 5%),a good precision( RSD: 2. 8%-5. 0%,n = 5),a good linearity( 0. 1-500 μg·L~(-1)) and a low limit of detection( 0. 02-0. 05 μg · L~(-1)) under the optimized conditions. The introduced MMISPE/GC method was successfully used to analyze five chloroacetamide herbicides in environmental water samples.
引文
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[2]Konda L N,Pásztor Z.J.Agric.Food Chem.,2001,49(8):3859-3863.
[3]Hu X G,Dai G M,Huang J J,Ye T T,Fan H J,Youwen T,Yu Y,Liang Y.J.Chromatogr.A,2010,1217(38):5875-5882.
[4]Li J Z,Chu X G,Cai H X,An J,Yang Q.Chin.J.Chromatogr.(李建中,储晓刚,蔡会霞,安娟,杨强.色谱),2006,24(6):585-588.
[5]Yang M,Ma Y A,Lin Z S,Yao Z W.J.Instrum.Anal.(杨梅,马永安,林忠胜,姚子伟.分析测试学报),2008,27(1):38-41.
[6]Lin Z,Chen J,Li J,Hui M X,Lan J C,Jang J B,Yang F.Chin.Agric.Sci.Bull.(林真,陈健,李捷,惠美星,蓝锦昌,江锦彬,杨方.中国农学通报),2015,31(11):162-165.
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[8]Xie L Q,Lan F,Lin L,Zhao Q H,Jin B H,Wu W D,Cai Y N.J.Instrum.Anal.(谢丽琪,蓝芳,林黎,赵琼晖,靳保辉,吴卫东,蔡伊娜.分析测试学报),2007,26(3):365-367.
[9]Tan W,Hu X X,Yang M,Barrow C J,Yang W,Wang H B.Desalin.Water Treat.,2014,52(4/6):1177-1182.
[10]Hegedus G,Krikunova V,Belai I,Eremin S,Székács A.Int.J.Environ.Anal.Chem.,2002,82(11/12):879-891.
[11]Chen J,Lin Y X,Jia L.J.Chromatogr.A,2015,1388:43-51.
[12]Tan C J,Chua H G,Ker K H,Ker K H,Tong Y W.Anal.Chem.,2008,80(3):683-692.
[13]Ji Y S,Yin J J,Xu Z G,Zhao C M,Huang H Y,Zhang H X,Wang C M.Anal.Bioanal.Chem.,2009,395(4):1125-1133.
[14]Wang X X,Yang J,Xie S Y,Chen Y,Liu F L,Shen H Y,Xia Q H.J.Instrum.Anal.(王新鑫,杨军,谢晟瑜,陈扬,刘芳伶,沈昊宇,夏清华.分析测试学报),2015,34(11):1213-1219.
[15]Ma J,Huang J,Zeng Y B,Zhang Z L,Zhang J,Chen Z D,Li L.J.Instrum.Anal.(马洁,黄静,曾延波,张祖磊,张剑,陈智栋,李蕾.分析测试学报),2013,32(6):726-731.
[16]Huang C N,Duan X J,Ma H P,Yu Y H,Chen L G.J.Instrum.Anal.(黄超囡,段西健,麻海鹏,于嫣涵,陈立钢.分析测试学报),2013,32(3):275-280.
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[19]Chen L X,Wang X Y,Lu W H,Wu X Q,Li J H.Chem.Soc.Rev.,2016,45:2137-2211.
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[22]Ji W H,Zhang M M,Liu W,Wang X M,Duan W J,Xie H K,Wang X.RSC Adv.,2016,6:50487-50496.