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采用液相色谱-四极杆飞行时间串联质谱法测定咪草烟及其代谢物。

Determination of Imazaquin and its metabolite by liquid chromatography-quadrupole-time of flight tandem mass.

机构信息

Department of Chemistry and Chemical Engineering, Binzhou University, Binzhou, Shandong, China.

出版信息

Bull Environ Contam Toxicol. 2010 Aug;85(2):142-6. doi: 10.1007/s00128-010-0076-z. Epub 2010 Jul 21.

Abstract

A method consisting of solvent extraction followed by liquid chromatography-quadrupole-time of flight- tandem mass spectrometry analysis was developed for the identification of Imazaquin and its metabolite. The relationships between detector response and sample concentrations showed a high degree of linearity (r > 0.998) over the range 0.03-10 microg/g. The recoveries obtained were in the acceptable range of 86%-104% between spiked. The relative standard deviation of this method was 6.4%-17.1%. A 35-day study of Imazaquin degradation was taken in agricultural soil from Binzhou, China. The degradation followed first order kinetics (C = 0.7672e(-0.0774t)), with half-life of less than 8.5 days. Investigation of the by-products from liquid chromatography-quadrupole-time of flight- tandem mass spectrometry has shown that there were four important metabolites 4-methylene-2-(quinolin-2-yl)-1H-imidazol-5(4H)-one, quinoline-3-carbaldehyde, 1-amino-2,3-dimethyl-1-oxobutan-2-ylium and 1H-[1,2]oxazino[4,5-b]quinolin-1-one in the degradation process. The accurate mass measurements error was 5 ppm in this study. The method was successfully applied to the analysis of imazaquin and its metabolite residues in soil.

摘要

建立了一种溶剂萃取-液相色谱-四极杆飞行时间串联质谱分析方法,用于鉴定咪唑喹啉及其代谢物。在 0.03-10 μg/g 的范围内,检测响应与样品浓度之间呈现高度线性关系(r>0.998)。在添加水平范围内,回收率在 86%-104%之间,可接受。该方法的相对标准偏差为 6.4%-17.1%。在中国滨州农业土壤中进行了为期 35 天的咪唑喹啉降解研究。降解遵循一级动力学(C=0.7672e(-0.0774t)),半衰期小于 8.5 天。通过液相色谱-四极杆飞行时间串联质谱对副产物的研究表明,在降解过程中有四个重要的代谢物:4-亚甲基-2-(喹啉-2-基)-1H-咪唑-5(4H)-酮、喹啉-3-甲醛、1-氨基-2,3-二甲基-1-氧代丁-2-基和 1H-[1,2]恶嗪并[4,5-b]喹啉-1-酮。在本研究中,精确质量测量误差为 5 ppm。该方法成功应用于土壤中咪唑喹啉及其代谢物残留的分析。

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