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首页> 外文期刊>Environmental toxicology and chemistry >DETERMINATION OF INSOLUBLE SOAP IN AGRICULTURAL SOIL AND SEWAGE SLUDGE SAMPLES BY LIQUID CHROMATOGRAPHY WITH ULTRAVIOLET DETECTION
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DETERMINATION OF INSOLUBLE SOAP IN AGRICULTURAL SOIL AND SEWAGE SLUDGE SAMPLES BY LIQUID CHROMATOGRAPHY WITH ULTRAVIOLET DETECTION

机译：紫外检测-液相色谱法测定农业土壤和污水污泥中的不溶性肥皂

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摘要

We have developed a new analytical procedure for determining insoluble Ca and Mg fatty acid salts (soaps) in agricultural soil and sewage sludge samples. The number of analytical methodologies that focus in the determination of insoluble soap salts in different environmental compartments is very limited. In this work, we propose a methodology that involves a sample clean-up step with petroleum ether to remove soluble salts and a conversion of Ca and Mg insoluble salts into soluble potassium salts using tripotassium ethylenediaminetetraacetate salt and potassium carbonate, followed by the extraction of analytes from the samples using microwave-assisted extraction with methanol. An improved esterification procedure using 2,4-dibromoacetophenone before the liquid chromatography with ultraviolet detection analysis also has been developed. The absence of matrix effect was demonstrated with two fatty acid Ca salts that are not commercial and are never detected in natural samples (C_(13:0) and C_(17:0)). Therefore, it was possible to evaluate the matrix effect because both standards have similar environmental behavior (adsorption and precipitation) to commercial soaps (C_(10:0) to C_(18:0)). We also studied the effect of the different variables on the clean-up, the conversion of Ca soap, and the extraction and derivatization procedures. The quantification limits found ranged from 0.4 to 0.8 mg/kg. The proposed method was satisfactorily applied for the development of a study on soap behavior in agricultural soil and sewage sludge samples.
机译：我们开发了一种新的分析程序，用于测定农业土壤和污水污泥样品中的不溶性Ca和Mg脂肪酸盐（肥皂）。专注于确定不同环境室中不溶性肥皂盐的分析方法的数量非常有限。在这项工作中，我们提出一种方法，该方法包括使用石油醚进行样品净化以除去可溶性盐，并使用三乙二胺四乙酸钾和碳酸钾将Ca和Mg不溶性盐转化为可溶性钾盐，然后萃取分析物样品通过微波辅助甲醇萃取从样品中分离出来。还开发了一种改进的酯化方法，该方法在使用紫外检测分析进行液相色谱分析之前，先使用2,4-二溴苯乙酮。两种脂肪酸Ca盐证明没有基质效应，这两种脂肪酸Ca盐都不市售，在天然样品中也从未检出（C_（13：0）和C_（17：0））。因此，可以评估基体效应，因为两种标准品都具有与商用肥皂（C_（10：0）至C_（18：0））相似的环境行为（吸附和沉淀）。我们还研究了不同变量对净化，Ca皂的转化以及萃取和衍生化过程的影响。发现的定量限为0.4至0.8 mg / kg。该方法令人满意地用于农业土壤和污水污泥样品中肥皂行为的研究。

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  • 来源
    《Environmental toxicology and chemistry》 |2010年第11期|p.2470-2476|共7页
  • 作者

    Samuel Cantarero; Alberto Zafra-G6mez; Oscar Ballesteros; Alberto Navalon; Jose L. Vilchez; Guillermo Crovetto; Coral Verge; Juan A. de Ferrer;

  • 作者单位

    Faculty of Sciences, Department of Analytical Chemistry, University of Granada, E-18071 Granada, Spain;

    rnFaculty of Sciences, Department of Analytical Chemistry, University of Granada, E-18071 Granada, Spain;

    rnFaculty of Sciences, Department of Analytical Chemistry, University of Granada, E-18071 Granada, Spain;

    rnFaculty of Sciences, Department of Analytical Chemistry, University of Granada, E-18071 Granada, Spain;

    rnFaculty of Sciences, Department of Analytical Chemistry, University of Granada, E-18071 Granada, Spain;

    rnFaculty of Sciences, Department of Analytical Chemistry, University of Granada, E-18071 Granada, Spain;

    rnCepsa Quimica. Avenida del Partenon 12, E-28042 Madrid, Spain;

    rnCepsa Quimica. Avenida del Partenon 12, E-28042 Madrid, Spain;

  • 收录信息 美国《科学引文索引》(SCI);美国《工程索引》(EI);美国《生物学医学文摘》(MEDLINE);美国《化学文摘》(CA);
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

    agricultural soil; sewage sludge; soap; microwave-assisted extraction; liquid chromatography;

    机译：农业土壤污水污泥;肥皂;微波辅助萃取液相色谱;

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