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用于超临界流体色谱的流通柱电解池。

A flow-through column electrolytic cell for supercritical fluid chromatography.

作者信息

Yamamoto Kazuhiro, Ueki Tatsuya, Higuchi Naoyuki, Takahashi Kouji, Kotani Akira, Hakamata Hideki

机构信息

Department of Analytical Chemistry, School of Pharmacy, Tokyo University of Pharmacy and Life Sciences, Tokyo, Japan.

Center for Fundamental Laboratory Education, School of Pharmacy, Tokyo University of Pharmacy and Life Sciences, Tokyo, Japan.

出版信息

J Sep Sci. 2017 Oct;40(20):4085-4090. doi: 10.1002/jssc.201700317. Epub 2017 Sep 12.

Abstract

A novel flow-through column electrolytic cell was proposed as a detector to obtain current signals for supercritical fluid chromatography. The electrochemical cell consisted of two electrodes and its holder, and a working and a counter electrode were fabricated from 192 carbon strings, which were composed of 400 carbon fibers of 10 μm in diameter filled into a heat-shrinkable tube. These electrodes were placed in the center of a holder made from polyether ether ketone blocks and they were separated by polytetrafluoroethylene membrane filters. To evaluate the sensitivity of this cell, a standard solution of ferrocene was injected into the supercritical fluid chromatography system connected to the electrolytic cell. The ferrocene was eluted through a silica gel column using a mixture of a mobile phase of supercritical CO and a modifier of methanol containing ammonium acetate. The current peak area of ferrocene correlated to the ferrocene concentration in the range of 10-400 μmol/L (r = 0.999). Moreover, the limit of detection on the column estimated from a signal-to-noise ratio of 3 was 9.8  × 10  mol.

摘要

提出了一种新型流通柱电解池作为检测器,用于获取超临界流体色谱的电流信号。该电化学池由两个电极及其支架组成,工作电极和对电极由192根碳丝制成,这些碳丝由400根直径为10μm的碳纤维填充到热缩管中构成。这些电极置于由聚醚醚酮块制成的支架中心,并用聚四氟乙烯膜过滤器隔开。为评估该电解池的灵敏度,将二茂铁标准溶液注入连接到电解池的超临界流体色谱系统中。使用超临界CO流动相和含醋酸铵的甲醇改性剂的混合物,使二茂铁通过硅胶柱洗脱。二茂铁的电流峰面积在10 - 400μmol/L范围内与二茂铁浓度相关(r = 0.999)。此外,根据信噪比为3估算的柱上检测限为9.8×10⁻⁵mol。

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