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超声辅助碳纳米管分散固相萃取环境水样中三嗪类除草剂。

Effervescence-assisted carbon nanotubes dispersion for the micro-solid-phase extraction of triazine herbicides from environmental waters.

机构信息

Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, University of Córdoba, Córdoba, Spain.

出版信息

Anal Bioanal Chem. 2013 Apr;405(10):3269-77. doi: 10.1007/s00216-013-6718-3. Epub 2013 Jan 27.

Abstract

Extraction techniques are surface-dependent processes since their kinetic directly depends on the contact area between the sample and the extractant phase. The dispersion of the extractant (liquid or solid) increases this area improving the extraction efficiency. In this article, the dispersion of a nanostructured sorbent at the very low milligram level is achieved by effervescence thanks to the in situ generation of carbon dioxide. For this purpose, a special tablet containing the effervescence precursors (sodium carbonate as carbon dioxide source and sodium dihydrogen phosphate as proton donor) and the sorbent [multiwalled carbon nanotubes (MWCNTs)] is prepared. All the microextraction steps take place in a glass beaker containing 100 mL of the sample. After the extraction, the MWCNTs, enriched with the extracted analytes, are recovered by vacuum filtration. Methanol was selected to elute the retained analytes. The extraction mode is optimized and characterized using the determination of nine herbicides in water samples as model analytical problem. The absolute recoveries of the analytes were in the range 48-76 %, while relative recoveries were close to 100 % in all cases. These values permit the determination of these analytes at the low microgram per liter range with good precision (relative standard deviations lower than 9.3 %) using ultra performance liquid chromatography (UPLC) combined with ultraviolet detection (UV).

摘要

提取技术是一种依赖于表面的过程,因为其动力学直接取决于样品和萃取相之间的接触面积。萃取剂(液体或固体)的分散度增加了这一面积,从而提高了萃取效率。在本文中,通过利用二氧化碳的原位生成,通过冒泡作用实现了纳米结构吸附剂在非常低的毫克级别的分散。为此,制备了一种特殊的片剂,其中包含冒泡的前体(作为二氧化碳源的碳酸钠和作为质子供体的磷酸二氢钠)和吸附剂[多壁碳纳米管(MWCNTs)]。所有的微萃取步骤都在一个玻璃烧杯中进行,烧杯中含有 100 毫升的样品。萃取后,通过真空过滤回收吸附有被萃取分析物的 MWCNTs。选择甲醇来洗脱保留的分析物。使用水中九种除草剂的测定作为模型分析问题,对萃取模式进行了优化和表征。分析物的绝对回收率在 48-76%范围内,而在所有情况下相对回收率都接近 100%。这些值允许使用超高效液相色谱(UPLC)结合紫外检测(UV)在低微克/升范围内对这些分析物进行测定,具有良好的精密度(相对标准偏差低于 9.3%)。

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