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二茂铁羧酸酯的快速液相色谱 - 电化学 - 质谱联用分析

Fast liquid chromatography-electrochemistry-mass spectrometry of ferrocenecarboxylic acid esters.

作者信息

Diehl Georg, Karst Uwe

出版信息

J Chromatogr A. 2002 Oct 18;974(1-2):103-9. doi: 10.1016/s0021-9673(02)01310-9.

DOI:10.1016/s0021-9673(02)01310-9
PMID:12458930
Abstract

Rapid liquid chromatographic separations of ferrocenecarboxylic esters of various alcohols and phenols have been achieved on reversed-phase columns of 20 mm length. After separation, the ferrocene derivatives are oxidized electrochemically under formation of the charged ferrocinium species, which are easily detected by mass spectrometry using an atmospheric pressure chemical ionization source operated in the heated nebulizer mode. While a series of nine phenol derivatives was separated within less than 1.5 min, six alcohol derivatives eluted within 1 min. Limits of detection using a single quadrupole mass analyzer ranged from 60 to 190 nmol/l. Additional work was directed on the use of a graphite in-line filter instead of a silica-based reversed-phase column to achieve the separation.

摘要

在20毫米长的反相柱上实现了各种醇和酚的二茂铁羧酸酯的快速液相色谱分离。分离后,二茂铁衍生物在形成带电的二茂铁鎓物种的情况下进行电化学氧化,使用在加热雾化器模式下运行的大气压化学电离源,通过质谱法很容易检测到这些物种。一系列九种酚衍生物在不到1.5分钟内分离出来,六种醇衍生物在1分钟内洗脱出来。使用单四极杆质量分析仪的检测限为60至190纳摩尔/升。额外的工作致力于使用石墨在线过滤器代替基于硅胶的反相柱来实现分离。

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