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从不同物理化学性质的土壤中水解研究和提取螺环菌胺。

Hydrolysis study and extraction of spiroxamine from soils of different physico-chemical properties.

机构信息

Dpto. Química Analítica, Facultad de Ciencias Químicas, Universidad Complutense de Madrid, 28040 Madrid, Spain.

出版信息

Chemosphere. 2009 Oct;77(6):821-8. doi: 10.1016/j.chemosphere.2009.07.078. Epub 2009 Sep 5.

Abstract

Spiroxamine, 8-(1,1-dimethylethyl)-N-ethyl-N-propyl-1,4-dioxa-spiro [4.5] decane-2-methanamine, is a novel broad-spectrum fungicide from the new class of spiroketalamines widely used in cereals and grapes. In this paper, the hydrolysis of the spiroxamine active substance has been investigated and the extraction procedure from soil samples has been optimized. The progress of degradation in water at a wide pH range (4-14), was continuously monitored by means of reversed phase LC-ESI-MS/MS in the positive ionization mode during 90 d incubation experiment. To establish the degradation kinetics, water solutions were incubated by triplicate in the dark under controlled temperature (20+/-2 degrees C) and the spiroxamine remaining concentration was determined. Pesticide metabolites such as desethyl, despropyl and N-oxide spiroxamine were not detected at significant amounts in all tested conditions and the degradations followed first-order kinetics (r(2)>or=0.979). The faster degradation was observed at both pH 4 and 14 with half-life times of 37 and 10 d, respectively. On the other hand, the spiroxamine fungicide has been determined in two types of soil (silt loam and sandy loam) at different spiked levels. At the level of the highest spiroxamine application rate for agricultural crops (750 g a.i. ha(-1)), recoveries higher than 96.0% were obtained, showing the effectiveness of the proposed methodology.

摘要

螺环菌胺,8-(1,1-二甲基乙基)-N-乙基-N-丙基-1,4-二氧杂螺[4.5]癸烷-2-甲胺,是一种新型的广谱杀菌剂,属于广泛用于谷物和葡萄的螺环酮胺类新类别。在本文中,研究了螺环菌胺活性物质的水解,并优化了从土壤样品中提取的程序。在 90 d 孵育实验中,通过反相 LC-ESI-MS/MS 在正离子模式下连续监测宽 pH 范围(4-14)下水的降解进展。为了建立降解动力学,在黑暗中、控制温度(20+/-2 摄氏度)下将水合溶液一式三份进行孵育,并确定螺环菌胺的剩余浓度。在所有测试条件下,均未以显著量检测到农药代谢物,如去乙基、去丙基和 N-氧化物螺环菌胺,降解遵循一级动力学(r(2)>or=0.979)。在 pH 4 和 14 下观察到更快的降解,半衰期分别为 37 和 10 d。另一方面,已在两种类型的土壤(粉壤土和沙壤土)中不同的螺环菌胺添加水平下进行了测定。在农业作物的最高螺环菌胺施用量(750 g a.i. ha(-1))水平下,回收率高于 96.0%,表明所提出的方法有效。

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