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在注射器中搅拌:一种新型的磁搅拌辅助分散液液微萃取方法。

In-syringe-stirring: a novel approach for magnetic stirring-assisted dispersive liquid-liquid microextraction.

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Hradec Králové, Czech Republic.

出版信息

Anal Chim Acta. 2013 Jul 25;788:52-60. doi: 10.1016/j.aca.2013.05.049. Epub 2013 Jun 3.

DOI:10.1016/j.aca.2013.05.049
PMID:23845481
Abstract

For the first time, the use of a magnetic stirrer within the syringe of an automated syringe pump and the resulting possible analytical applications are described. A simple instrumentation following roughly the one from sequential injection analyzer systems is used in combination with an adaptor, which is placed onto the barrel of a glass syringe. Swirling around the longitudinal axis of the syringe and holding two strong neodymium magnets, it causes a rotating magnetic field and serves as driver for a magnetic stirring bar placed inside of the syringe. In a first study it was shown that this approach leads to a sealed but also automatically adaptable reaction vessel, the syringe, in which rapid and homogeneous mixing of sample with the required reagents within short time can be carried out. In a second study in-a-syringe magnetic stirring-assisted dispersive liquid-liquid microextraction (MSA-DLLME) was demonstrated by the application of the analyzer system to fluorimetric determination of aluminum in seawater samples using lumogallion. A linear working range up to 1.1 μmol L(-1) and a limit of detection of 6.1 nmol L(-1) were found. An average recovery of 106.0% was achieved for coastal seawaters with a reproducibility of 4.4%. The procedure lasted 210 s including syringe cleaning and only 150 μL of hexanol and 4.1 mL of sample were required.

摘要

首次描述了在自动化注射器泵的注射器内使用磁力搅拌器以及由此产生的可能的分析应用。一种简单的仪器,大致遵循顺序注射分析系统的仪器,与一个适配器结合使用,该适配器放置在玻璃注射器的桶上。它围绕注射器的纵轴旋转,并固定两个强钕磁铁,产生一个旋转磁场,并作为放置在注射器内的磁性搅拌棒的驱动器。在第一项研究中表明,这种方法导致了一个密封但也可自动适应的反应容器,即注射器,在其中可以在短时间内快速且均匀地混合样品与所需的试剂。在第二项研究中,通过将分析器系统应用于使用鲁米诺镓荧光测定海水样品中的铝,证明了在注射器中进行的磁搅拌辅助分散液-液微萃取(MSA-DLLME)。发现工作范围线性至 1.1 μmol L(-1),检测限为 6.1 nmol L(-1)。对于沿海海水,平均回收率为 106.0%,重现性为 4.4%。该过程持续 210 秒,包括注射器清洗,仅需 150 μL 正己醇和 4.1 mL 样品。

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