为了对玉米中的嗪草酮残留进行高效的分离、富集和测定，以嗪草酮为模板分子，采用原位聚合法制备了分子印迹聚合物，并将印迹聚合物作为固相萃取柱用于玉米样品的前处理过程，建立了在线富集液相色谱法测定玉米中嗪草酮残留的分析方法。研究结果表明，嗪草酮印迹聚合物具有良好的亲和性和特异选择性，在0.01~0.50 μg/mL质量浓度范围内有良好的线性关系(r=9991)，最低检出浓度(S/N=3)为1.8×10-3 μg/mL，在0.01，0.05，0.10 mg/kg 3个浓度的添加水平下，方法的平均回收率在80.9%~94.5%之间，相对标准偏差低于5.98%。方法简化了样品前处理步骤，提高了检测灵敏度度，分析时间短，无基质干扰，精密度和准确度高，可应用于玉米中嗪草酮残留的分析检测。
Abstract
For better resolution, enrichment and determinaiton of metribuzin residues in corn, a molecularly imprinted polymer with metribuzin as a template molecule synthesized by in situ polymerization was used as a solid-phase extraction sorbent for the on-line preconcentration and analysis of metribuzin residues in corn by liquid chromatography. The results showed that the molecularly imprinted polymer had significant molecularly imprinting effect and had high affinity and selectivity for metribuzin in water-containing system. Good linearity was obtained for metribuzin at the concentration of 0.01-0.50μg/mL with correlation coefficient of 0.9991. The detection limit (S/N=3) of the method for metribuzin was 1.8×10- 3μg/mL, the recoveries of metribuzin in corn at 0.01, 0.05 and 0.10 mg/kg were 80.9%- 94.5% and the relative standard deviations were less than 5.98%. The pretreatment procedure was simplified and the sensitivity was enhanced by using the method. The method was sensitive, reproducible, reliable, timesaving and no matrix interference. It could be used on the determination of metribuzin residues in corn.
关键词
分子印迹;在线富集;嗪草酮;残留;玉米
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Key words
molecularly imprinted polymer; on-line preconcentration; metribuzin; residue; corn
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参考文献
[1] Wauchope R D, Buttler T M, Hornsby a G, et al. The scs ars ces pesticide properties database for environmental decision- making[J]. Rev. Environ. Contam. Toxicol.,1992,123(1):1-155.
[2] GB 2763-2014.食品中农药最大残留限量[S].北京:中国标准出版社,2014.
[3] 邹伟,周昱.粮谷中嗪草酮残留量的气相色谱和气相色谱-质谱分析[J].福建分析测试,1999,6(2):12-16.
[4] 刘伟,吴文君.气-质联机对嗪草酮原药及其主要杂质的分析[J].农药,2006,45(9):42-43,45.
[5] GB/T 19649—2006.粮谷中 475种农药及相关化学品残留量的测定气相色谱质谱法[S].北京:中国标准出版社,2006.
[6] 廖耀祖,黄美荣,李新贵.纳米结构聚吡咯构建的生物传感器[J].分析化学,2009,37(2):291-298.
[7] 李成学,张娟琨,蒋树海,等.心肌肌钙蛋白 I的分子印迹电化学生物传感器[J].生物加工过程,2012,10(3):61-66.
[8] Li H, Nie L H, Li Y N, et al. Application of molecularly imprinted column for separation and purification of bioactive compound from cirsium segetum bunge[J]. Separ. Sci. Technol.,2009,44(2):370-385.
[9] Spegel P, Schweitz L, Andersson L I, et al. Novel vinylpyridine based cationic mip monoliths for enantiomer separation in cec[J]. Chromatographia,2009,69(3-4):277-285.
[10] 杜碧柏,许杨,黄云红,等.分子印迹固相萃取—高效液相色谱法测定饲料中磺胺类药物[J].分析化学,2012,40(12):1871-1876.
[11] 早热古丽·努尔,吐尔洪·买买提,佐拉木·买买提.齐多夫定替代模板分子印迹聚合物的制备及其在血清样品固相萃取中的应用[J].分析试验室,2013,32(5):6-10.
[12] 张飞,祝方,万鹏,等.重金属离子印迹技术及其在废水处理中的应用[J].水处理技术,2014,40(6):9-13.
[13] 张进,熊和琴,姚桃花,等.分子印迹电化学传感器检测环境中特丁津研究[J].环境科学与技术,2014,37(5):31-35.
[14] 夏环,王妍,荆涛,等.分子印迹固相萃取-高效液相色谱法测定蜂蜜中三种氟喹诺酮类抗生素残留[J].分析科学学报,2012,28(3):297- 302.
[15] 贺利民,刘开永,武力,等.分子印迹固相萃取气相色谱-质谱法测定鸡蛋中三聚氰胺[J].中国兽药杂志,2011,45(1):2-5,13
[16] 王超丽,雷孝,肖湘,等.传统法制备嗪草酮印迹聚合物[J].现代农药, 2007,6(6):40-44.
[17] 王锦,董欣荣,王超丽.嗪草酮印迹聚合物在环境污染监测中的应用[J].化学与生物工程,2011,28(11):70-72.
[18] Shaojun Zhang, Gengliang Yang, Zhenshan Zheng, et al. On- line pre-concentration and analysis of metribuzin residue in corn fields by molecularly imprinted polymer[J].Chromatographia,2009,69(7- 8):615-619.
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