雌二醇分子印迹整体棒在类固醇雌激素分析中的应用
|
摘要
类固醇雌激素对生物体及环境的影响较大,在环境中含量低且易受基质干扰而难以检测。本文以雌二醇为模板分子、甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂,采用原位聚合法制备一种新型分子印迹聚合物整体棒,其中模板分子、功能单体、交联剂三者的摩尔比为1∶6∶30。采用扫描电镜对分子印迹聚合物进行了结构表征,对雌二醇分子印迹整体棒的萃取条件进行了优化,进一步研究其萃取性能,并联用高效液相色谱应用于环境水样中类固醇雌激素的萃取分析,线性范围在0.5~50μg·L-1之间,加标回收率在94.58%~103.72%之间,相对标准偏差在2.4%~4.9%之间(n=5)。该方法简便、易于操作,能实现水相样品中类固醇类雌激素的选择性萃取分析。
Steroid estrogens have a great influence to organisms and environment.It was difficult to be detected for its low levels and matrix interference.In this paper,a novelmolecularly imprinted monolithic bar was synthesized by situ-polymerization method.Estradiol,methacrylate and ethylene glycol dimethacrylate were used as template molecule,functional monomer and cross-linking agent,respectively.The ratio of template,functional monomer and cross-linking agent is 1: 6: 30. The morphological structure of the molecularly imprinted polymer monolithic bar was investigated via scanning electron microscopy. The extraction conditions were optimized and the extraction performance was further investigated.Finally,the molecularly imprinted monolithic bar was coupled with HPLC for the analysis of steroid estrogens in environmental water samples.The linear range was in 0. 5-5. 0 μg·L-1.The recovery of environmental sampleswas between 94. 58%and103. 72%,and the RSD was from 2. 4%to 4. 9%( n = 5). The developed method was simple and easy to operate.It can be used to selectively extracted steroids estrogens in water samples.
Steroid estrogens have a great influence to organisms and environment.It was difficult to be detected for its low levels and matrix interference.In this paper,a novelmolecularly imprinted monolithic bar was synthesized by situ-polymerization method.Estradiol,methacrylate and ethylene glycol dimethacrylate were used as template molecule,functional monomer and cross-linking agent,respectively.The ratio of template,functional monomer and cross-linking agent is 1: 6: 30. The morphological structure of the molecularly imprinted polymer monolithic bar was investigated via scanning electron microscopy. The extraction conditions were optimized and the extraction performance was further investigated.Finally,the molecularly imprinted monolithic bar was coupled with HPLC for the analysis of steroid estrogens in environmental water samples.The linear range was in 0. 5-5. 0 μg·L-1.The recovery of environmental sampleswas between 94. 58%and103. 72%,and the RSD was from 2. 4%to 4. 9%( n = 5). The developed method was simple and easy to operate.It can be used to selectively extracted steroids estrogens in water samples.
引文
[1]李攻科,胡玉玲,阮贵华.样品前处理仪器与装置[M].北京:化学工业出版社,2007:1-11.
[2]黄健祥,胡玉斐,潘加亮,等.分子印迹样品前处理技术的研究进展[J].中国科学,2009,39(8):733-746.
[3]Hu Y L,Pan J L,Zhang K G,et al.Novel applications of molecularly imprinted polymers in sample preparation[J].Tr Anal Chem,2013,43:37-52.
[4]Tan J,Jiang Z T,Li R,et al.Molecularly-imprinted monoliths for sample treatment and separation[J].Tr Anal Chem,2012,39:207-217.
[5]Martin-Esteban A.Molecularly-imprinted polymers as a versatile,highly selective tool in sample preparation[J].Tr Anal Chem,2013,45:169-181.
[6]刘蓉,钟桐生,刘石泉,等.电聚合分子印迹传感器测定黑茶中芦丁的含量[J].化学研究与应用,2015,27(8):1118-1122.
[7]姜忠义,吴洪.分子印迹技术[M].北京:化学工业出版社,2003:1-6.
[8]Chen Y,Guo Z P,Wang X Y,et al.Sample preparation[J].J Chromatogr A,2008,1184(1-2):191-219.
[9]Xu Z G,Feng F,Liu Z M,et al.Molecularly imprinted polymer microextraction techniques for sample preparation[J].昆明理工大学学报:自然科学版,2014,39(4):112-121.
[10]Turiel E,Tadeo J L,Martin-Esteban A.Molecularly imprinted polymeric fibers for solid-phase microextraction[J].Anal Chem,2007,79(8):3099-3104.
[11]胡玉玲,朱飞,李家威,等.特丁津分子印迹整体萃取棒的研制及其萃取性能[J].分析化学,2009,37(3):466-470.
[12]Xu Z G,Wang L G,Chen Y L,et al.Polymer monolithic rods microextraction coupled with high performance liquid chromatography for the analysis of trimethoprim,sulfadiazine and sulfamethoxazole in honey samples[J].J Chem Pharm Res,2014,6(5):54-58.
[13]Jiang T H,Zhao L X,Chu B L,et al.Molecularly imprinted solid-phase extraction for the selective determination of 17β-estradiol in fishery samples with high performance liquid chromatography[J].Talanta,2009,78(2):442-447.
[2]黄健祥,胡玉斐,潘加亮,等.分子印迹样品前处理技术的研究进展[J].中国科学,2009,39(8):733-746.
[3]Hu Y L,Pan J L,Zhang K G,et al.Novel applications of molecularly imprinted polymers in sample preparation[J].Tr Anal Chem,2013,43:37-52.
[4]Tan J,Jiang Z T,Li R,et al.Molecularly-imprinted monoliths for sample treatment and separation[J].Tr Anal Chem,2012,39:207-217.
[5]Martin-Esteban A.Molecularly-imprinted polymers as a versatile,highly selective tool in sample preparation[J].Tr Anal Chem,2013,45:169-181.
[6]刘蓉,钟桐生,刘石泉,等.电聚合分子印迹传感器测定黑茶中芦丁的含量[J].化学研究与应用,2015,27(8):1118-1122.
[7]姜忠义,吴洪.分子印迹技术[M].北京:化学工业出版社,2003:1-6.
[8]Chen Y,Guo Z P,Wang X Y,et al.Sample preparation[J].J Chromatogr A,2008,1184(1-2):191-219.
[9]Xu Z G,Feng F,Liu Z M,et al.Molecularly imprinted polymer microextraction techniques for sample preparation[J].昆明理工大学学报:自然科学版,2014,39(4):112-121.
[10]Turiel E,Tadeo J L,Martin-Esteban A.Molecularly imprinted polymeric fibers for solid-phase microextraction[J].Anal Chem,2007,79(8):3099-3104.
[11]胡玉玲,朱飞,李家威,等.特丁津分子印迹整体萃取棒的研制及其萃取性能[J].分析化学,2009,37(3):466-470.
[12]Xu Z G,Wang L G,Chen Y L,et al.Polymer monolithic rods microextraction coupled with high performance liquid chromatography for the analysis of trimethoprim,sulfadiazine and sulfamethoxazole in honey samples[J].J Chem Pharm Res,2014,6(5):54-58.
[13]Jiang T H,Zhao L X,Chu B L,et al.Molecularly imprinted solid-phase extraction for the selective determination of 17β-estradiol in fishery samples with high performance liquid chromatography[J].Talanta,2009,78(2):442-447.