Development of a dispersive liquid-liquid microextraction method for organophosphorus flame retardants and plastizicers determination in water samples
Development of a dispersive liquid-liquid microextraction method for organophosphorus flame retardants and plastizicers determination in water samples
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DOI：
10.1016/j.chroma.2007.08.006
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发表时间：
2007-09-28
影响因子：
4.1
通讯作者：
Cela, R.
中科院分区：
文献类型：
--
作者：
Garcia-Lopez, M.;Rodriguez, I.;Cela, R.
提出了一种快速、廉价、高效的样品前处理方法，用于水样中10种有机磷化合物的测定。采用分散液-液微萃取（DLLME）技术提取分析物，并通过气相色谱-氮磷检测（GC-NPD）进行测定。研究了几个变量（例如分散剂和萃取溶剂的类型和体积、离子强度、振荡时间和模式等）对萃取的影响。对样品制备步骤性能的影响进行了仔细评估。在最终工作条件下，将1 mL含2% 1，1，1-三氯乙烷的丙酮（20 μ L）加入10 mL含20%氯化钠的水中。将三元混合物以3500 rpm离心以允许相分离。除去水性上清液后，将沉淀提取物的等分试样进样至GC-NPD系统中。在上述条件下，该方法提供的富集因子为190 - 830倍（取决于所考虑的化合物），相对标准偏差低于10%（三（2-乙基己基）磷酸盐（TEHP）除外），定量限为0.01 - 0.08 ng/mL。基质效应进行了评估，使用不同的水样，并通过与固相微萃取比较的准确性进行了评价。(c)2007 Elsevier B. V.保留所有权利。
A fast, inexpensive and efficient sample preparation method for the determination of 10 organophosphorus compounds in water samples is presented. Analytes were extracted using the dispersive liquid-liquid microextraction (DLLME) technique and determined by gas chromatography with nitrogen-phosphorus detection (GC-NPD). The influence of several variables (e.g. type and volume of dispersant and extraction solvents, ionic strength, shaking time and mode, etc.) on the performance of the sample preparation step was carefully evaluated. Under final working conditions, 1 mL of acetone containing a 2% of 1,1,1-trichloroethane (20 mu L) was added to 10 mL of water with 20% of sodium chloride. The ternary mixture was centrifuged at 3500 rpm to allow phase separation. After removing the aqueous supernatant, an aliquot of the settled extract was injected in the GC-NPD system. Under the above conditions, the method provided enrichment factors between 190 and 830 times (depending on the considered compound), relative standard deviations below 10%, except for tris(2-ethylhexyl) phosphate (TEHP), and quantification limits between 0.01 and 0.08 ng/mL. Matrix effects were assessed using different water samples, and accuracy was evaluated by comparison with solid-phase microextraction. (c) 2007 Elsevier B.V. All rights reserved.