分子印迹固相萃取-高效液相色谱法检测果蔬中的乙酰甲胺磷
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摘要
本文建立了分子印迹固相萃取-高效液相色谱法检测蔬菜中的乙酰甲胺磷。选取乙酰甲胺磷为模板分子,采用溶胶-凝胶法制备分子印迹聚合物(MIPs),吸附实验表明MIPs对乙酰甲胺磷具较高的吸附容量和特异吸附性。以所制备的印迹材料为固相萃取吸附剂,在优化固相萃取条件下,结合高效液相色谱法分析4种实际样品中的乙酰甲胺磷残留。结果表明,乙酰甲胺磷的检出限为1.8×10-3μg/mL,加标回收率为82.7%～102.3%。与C18柱比较,分子印迹固相萃取(MISPE)柱可有效去除基质干扰,对目标物有良好的分离富集效果。
In this paper,a molecularly imprinted solid phase extraction(MISPE)-high performance liquid chromatography(HPLC)was developed for the determination of acephate in vegetables.Molecularly imprinted polymers(MIPs)were prepared by a sol-gel method using acephate as a template molecule.Adsorption experiments showed that MIPs had higher adsorption capacity and specific adsorption for acephate.The prepared imprinted material was used as a solid phase extractant.The residual acephate was analyzed in four actual samples by HPLC under optimized solid phase extraction conditions.The results showed that the detection limit of acephate was 1.8×10-3μg/mL,and the recovery of standard addition was 82.7%-102.3%.Compared with the C18 column,MISPE column can effectively remove matrix interference and have good separation and enrichment effects on the target.
In this paper,a molecularly imprinted solid phase extraction(MISPE)-high performance liquid chromatography(HPLC)was developed for the determination of acephate in vegetables.Molecularly imprinted polymers(MIPs)were prepared by a sol-gel method using acephate as a template molecule.Adsorption experiments showed that MIPs had higher adsorption capacity and specific adsorption for acephate.The prepared imprinted material was used as a solid phase extractant.The residual acephate was analyzed in four actual samples by HPLC under optimized solid phase extraction conditions.The results showed that the detection limit of acephate was 1.8×10-3μg/mL,and the recovery of standard addition was 82.7%-102.3%.Compared with the C18 column,MISPE column can effectively remove matrix interference and have good separation and enrichment effects on the target.
引文
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[4]REGULATION(EC).On Maximum Residue Levels of Pesticides In or On Food and Feed of Plant and Animal Origin.
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[8]LI J W,WEI S L,CHEN N N.Chinese Journal of Analytical Chemistry(利健文,韦寿莲,陈娜娜.分析化学),2017,45(7):1031.
[9]Malik A A,Nantasenamat C,Piacham T.Materials Science&Engineering C,2017:1341.
[10]LUO X P,LI C Z,DUAN Y Q,et al.Journal of Applied Polymer Science,2016,133(15):1.
[11]GAO L,PIAO C Y,CHEN L G.Analytical Letters,2015,48(5):752.
[12]SU L Q,GAO B X,ZHOU X Y.Chemical Research and Application(苏立强,高宝勋,邹雪莹.化学研究与应用),2017,29(7):920.
[13]GB/T 5009.103.2003.Determination of Methamidophos and Acephate Pesticide Residues in Vegetable Foods(植物性食品中甲胺磷和乙酰甲胺磷农药残留量的测定).
[14]ZHANG Z H,LIU L,NIE L H.Chinese Journal of Polymer Science(张朝晖,刘丽,聂丽华.高分子学报),2010,(6):677.
[15]WANG L B,SU L Q,HAN C N,et al.Journal of Analytical Science(王丽博,苏立强,韩超男,等.分析科学学报),2018,34(2):229.
[16]DU B B,XU Y,HUANG Y H,et al.Chinese Journal of Analytical Chemistry(杜碧柏,许杨,黄运红,等.分析化学),2012,40(12):1871.