Determination of the diol content of chromatographic supports by capillary electrophoresis

Anuja Chattopadhyay, David S. Hage

Research output: Contribution to journalArticlepeer-review

30 Scopus citations

Abstract

A capillary electrophoresis (CE) method was developed for determining the diol content of supports used in high-performance affinity or size exclusion chromatography. This method involved oxidizing the diol-bonded support with periodate, followed by the use of CE to separate and quantitate the iodate produced by this reaction. Both the oxidation and separation conditions were considered in optimizing this assay. The final method was performed by reacting a known amount of support with a 20-fold excess of periodate in pH 4.0, 0.5 M acetate buffer, with pyromellitic acid being used as an internal standard. After allowing 5-10 min for oxidation, the mixture was filtered and the filtrate was injected onto a 57 cm x 50 μm I.D. fused-silica capillary operated at 25 kV and containing pH 4.0, 0.5 M acetate as the running buffer. The total separation time was 5 min per run and gave a detection limit of 0.1 mM iodate (or 0.1 μmol diol groups) for a 6-nl injection of a 1-ml reaction mixture. By varying the amount the support that was assayed, this method could be used with either porous or non-porous supports. This technique showed good correlation with an iodometric titration but required much less sample and time to perform.

Original languageEnglish (US)
Pages (from-to)255-261
Number of pages7
JournalJournal of Chromatography A
Volume758
Issue number2
DOIs
StatePublished - Jan 17 1997

Keywords

  • Diols
  • Stationary phases, LC

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Organic Chemistry

Fingerprint Dive into the research topics of 'Determination of the diol content of chromatographic supports by capillary electrophoresis'. Together they form a unique fingerprint.

Cite this