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土壤和肝脏中氯化二苯并 - 对 - 二噁英及二苯并呋喃提取与纯化程序的特点

Characteristics of an extraction and purification procedure for chlorinated dibenzo-p-dioxins and dibenzofurans in soil and liver.

作者信息

Albro P W, Schroeder J S, Harvan D J, Corbett B J

出版信息

J Chromatogr. 1984 Nov 16;312:165-82. doi: 10.1016/s0021-9673(01)92773-6.

Abstract

Liver is extracted with chloroform-methanol to give essentially quantitative transfer of endogenous chlorinated dibenzo-p-dioxins (CDDs) and dibenzofurans (CDFs) into the organic phase. A new procedure involving LH-20 Sephadex is used to remove most of the lipids from the extract. Soil is extracted by a simple, rapid and economical procedure giving very high recoveries of CDDs and CDFs from sandy soil, various types of clay, and humus-rich loam. Subsequent cleanup on basic and acidic alumina complete the preparation for gas chromatography-mass spectrometric analysis. The use of propylene glycol as a "keeper" and of 2,3,7-trichlorodibenzo-p-dioxin as a carrier minimizes losses during evaporation of solvents and on glass surfaces. Interactions of 2,3,7,8-CDD with organic material in loam slightly reduce recovery but there is no indication of high affinity binding sites, the losses being apparently associated with simple distribution coefficients. Special precautions needed to avoid losses of CDFs on alumina chromatography are described, and the effect of "aging" spiked soil is discussed.

摘要

用氯仿 - 甲醇提取肝脏,可使内源性氯化二苯并 - 对 - 二恶英(CDDs)和二苯并呋喃(CDFs)基本上定量转移至有机相中。采用一种涉及LH - 20葡聚糖凝胶的新方法从提取物中去除大部分脂质。通过一种简单、快速且经济的方法提取土壤,从砂土、各类黏土和富含有机质的壤土中对CDDs和CDFs具有非常高的回收率。随后在碱性和酸性氧化铝上进行净化处理,完成气相色谱 - 质谱分析的样品制备。使用丙二醇作为“保护剂”以及2,3,7 - 三氯二苯并 - 对 - 二恶英作为载体,可最大程度减少溶剂蒸发过程中以及在玻璃表面上的损失。2,3,7,8 - CDD与壤土中有机物质的相互作用会略微降低回收率,但没有迹象表明存在高亲和力结合位点,损失显然与简单的分配系数有关。描述了避免在氧化铝色谱上损失CDFs所需的特殊预防措施,并讨论了“老化”加标土壤的影响。

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