Coupling continuous subcritical water extraction, filtration, preconcentration, chromatographic separation and UV detection for the determination of chlorophenoxy acid herbicides in soils.

Coupling continuous subcritical water extraction, filtration, preconcentration, chromatographic separation and UV detection for the determination of chlorophenoxy acid herbicides in soils.
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DOI:
10.1016/s0021-9673(02)00452-1
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发表时间:
2002-06
期刊:
Journal of chromatography. A
影响因子:
--
通讯作者:
J. Luque‐Garcia;M. D. Luque de Castro
J. Luque‐Garcia;M. D. Luque de Castro
中科院分区:
其他
文献类型:
--
作者:
J. Luque‐Garcia;M. D. Luque de Castro

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采用亚临界水萃取、过滤、富集、色谱分析相结合的方法测定了不同类型土壤中的酸性除草剂。两个实验设计用于浸出步骤的优化。在连续模式下以lml/min的流速和85°C使用水作为提取剂足以定量提取分析物。静态提取时间是不必要的,以减少提取时间为1小时。含有C18-Hydra作为吸附剂的微型柱被证明是用于在单独色谱分离之前定量预浓缩除草剂的优良材料。流动注射歧管被用作耦合四个步骤的接口,从而允许整个分析过程的自动化。目标分析物的回收率在94.2%和113.1%之间,重复性,表示为相对标准偏差,在0.61%和6.83%之间。
Subcritical water extraction has been coupled with filtration, preconcentration and chromatographic analysis for the determination of acid herbicides in different types of soil. Two experimental designs were used for the optimization of the leaching step. The use of water as extractant in the continuous mode at a flow-rate of 1 ml/min and 85°C was sufficient for quantitative extraction of the analytes. A static extraction time was unnecessary for reducing the extraction time to 1 h. A minicolumn containing C18-Hydra as sorbent proved an excellent material for the quantitative preconcentration of the herbicides prior to individual chromatographic separation. A flow-injection manifold was used as interface for coupling the four steps, thus allowing automation of the whole analytical process. Recoveries of the target analytes ranged between 94.2 and 113.1%, and repeatabilities, expressed as relative standard deviations, were between 0.61 and 6.83%.