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凝胶渗透色谱和弗罗里硅土柱净化后用液相色谱法测定蔬菜中苯脲类除草剂残留量

Determination of phenylurea herbicide residues in vegetables by liquid chromatography after gel permeation chromatography and Florisil cartridge cleanup.

作者信息

Sannino A

机构信息

Stazione Sperimentale per l'Industria delle Conserve Alimentari, Parma, Italy.

出版信息

J AOAC Int. 1998 Sep-Oct;81(5):1048-53.

PMID:9772748
Abstract

A liquid chromatographic method for quantitative determination of 9 phenylurea herbicide residues (metoxuron, metobromuron, monolinuron, chlortoluron, isoproturon, diuron, linuron, chloroxuron, and neburon) in potatoes, carrots, and mixed vegetables is described. Samples are extracted with acetone, partitioned with ethyl acetate-cyclohexane (50 + 50, v/v) and cleaned up by gel permeation chromatography with ethyl acetate-cyclohexane (50 + 50, v/v) as eluant. A small column (1 cm id) packed with Biobeads SX3 resin is used to reduce solvent consumption and analytical time. After solid-phase extraction on a Florisil cartridge, herbicide residues are successfully separated on a C18 column by gradient elution and determined by UV detection at 242 nm. Average recoveries of 9 compounds from different samples range from 70 to 98% at 0.010 and 0.100 mg/kg fortification levels. Quantitation limits are 0.010 mg/kg.

摘要

描述了一种用于定量测定土豆、胡萝卜和混合蔬菜中9种苯基脲类除草剂残留(灭草隆、甲氧隆、绿麦隆、氯甲苯隆、异丙隆、敌草隆、利谷隆、枯草隆和环草隆)的液相色谱方法。样品用丙酮提取,用乙酸乙酯 - 环己烷(50 + 50,v/v)进行分配,并用乙酸乙酯 - 环己烷(50 + 50,v/v)作为洗脱剂通过凝胶渗透色谱法进行净化。使用填充有Biobeads SX3树脂的小柱(内径1 cm)以减少溶剂消耗和分析时间。在弗罗里硅土柱上进行固相萃取后,除草剂残留通过梯度洗脱在C18柱上成功分离,并通过在242 nm处的紫外检测进行测定。在0.010和0.100 mg/kg的强化水平下,不同样品中9种化合物的平均回收率在70%至98%之间。定量限为0.010 mg/kg。

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