Analysis of aged sulfadiazine residues in soils using microwave extraction and liquid chromatography tandem mass spectrometry

Analysis of aged sulfadiazine residues in soils using microwave extraction and liquid chromatography tandem mass spectrometry
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DOI:
10.1007/s00216-008-2081-1
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发表时间:
2008-06-01
影响因子:
4.3
通讯作者:
Amelung, W.
Amelung, W.
中科院分区:
化学2区
文献类型:
--
作者:
Foerster, M.;Laabs, V.;Amelung, W.

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从土壤中有效提取磺胺嘧啶残留物是困难的,因为已知磺胺嘧啶会迅速形成螯合残留物。本研究的目的是优化极限萃取老化残留的磺胺嘧啶及其两个主要代谢产物,N-乙酰磺胺嘧啶和4-羟基磺胺嘧啶,从土壤中。为此,将两种代表性的农业土壤(Luvisol,Cambisol)与来自[C-14]磺胺嘧啶处理猪的粪便混合,并在实验室中于10 ℃下孵育。经过不同的提取试验与各种溶剂混合物(二至四组分混合物与水,甲醇,乙腈,丙酮,和/或乙酸乙酯),不同的pH值(pH 4和9),和提取温度(高达200摄氏度),土壤提取物进行了测量液体闪烁计数和液相色谱串联质谱。关于磺胺嘧啶产量,土壤提取物的稳定性,和共提取基质的量,微波提取土壤(15分钟,150摄氏度),使用乙腈/水1:4(v/v)是选择的方法从土壤中彻底提取老化磺胺嘧啶残留物。
An efficient extraction of sulfadiazine residues from soils is difficult, as sulfadiazine is known to form quickly sequestering residues. The objective of this study was to optimize an exhaustive extraction for aged residues of sulfadiazine and its two major metabolites, N-acetylsulfadiazine and 4-hydroxysulfadiazine, from soil. For this purpose two representative used agricultural soils (Luvisol, Cambisol) were blended with manure derived from [C-14]sulfadiazine-treated pigs and incubated at 10 degrees C in the laboratory. After different extraction tests with various solvent mixtures (two- to four-component mixtures with water, methanol, acetonitrile, acetone, and/or ethyl acetate), different pH values (pH 4 and 9), and extraction temperatures (up to 200 degrees C), soil extracts were measured by liquid scintillation counting and liquid chromatography coupled to tandem mass spectrometry. With respect to sulfadiazine yields, stability of soil extracts, and the amount of coextracted matrix, a microwave extraction of soil (15 min, 150 degrees C) using acetonitrile/water 1:4 (v/v) is the method of choice for the exhaustive extraction of aged sulfadiazine residues from soils.