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马铃薯中利谷隆及其三种代谢物的简化净化与液相色谱紫外测定法

Simplified cleanup and liquid chromatographic ultraviolet determination of linuron and three metabolites in potatoes.

作者信息

Miliadis G E, Siskos P A, Vasilikiotis G S

机构信息

Benaki Phytopathological Institute, Pesticide Residues Laboratory, Athens, Greece.

出版信息

J Assoc Off Anal Chem. 1990 May-Jun;73(3):435-7.

PMID:2376548
Abstract

A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of linuron and 3 of its metabolites, 3-(3,4-dichlorophenyl)-1-methyl urea (DCPMU), 3-(3,4-dichlorophenyl) urea (DCPU), and 3,4-dichloroaniline (DCA), in potatoes. Samples are extracted with acetone, partitioned into dichloromethane-hexane (1 + 1), and cleaned up using disposable silica cartridges. LC determination is performed using a LiChrosorb NH2 5 microns column, with an isopropanol-isooctane gradient mobile phase and UV detection at 248 nm. Recoveries of linuron and 2 of the metabolites from untreated samples fortified at 0.02-2 micrograms/g ranged from 80 to 102%, while recoveries for the metabolite DCA ranged from 60 to 78%. The detection limit was 0.015 micrograms/g for linuron and each metabolite; the minimum quantitation level was 0.5 micrograms/g. The developed method was applied to potato samples from a field experiment.

摘要

本文介绍了一种简单高效的方法,用于提取、净化和液相色谱(LC)测定马铃薯中的利谷隆及其3种代谢物,即3-(3,4-二氯苯基)-1-甲基脲(DCPMU)、3-(3,4-二氯苯基)脲(DCPU)和3,4-二氯苯胺(DCA)。样品用丙酮提取,分配至二氯甲烷-己烷(1 + 1)中,并用一次性硅胶柱净化。使用LiChrosorb NH2 5微米柱进行LC测定,采用异丙醇-异辛烷梯度流动相,并在248 nm处进行紫外检测。从未经处理的样品中添加0.02 - 2微克/克的利谷隆和2种代谢物的回收率在80%至102%之间,而代谢物DCA的回收率在60%至78%之间。利谷隆和每种代谢物的检测限为0.015微克/克;最低定量限为0.5微克/克。所开发的方法应用于田间试验的马铃薯样品。

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