Analysis of thiopurines using aqueous normal phase chromatography

Joseph J Pesek; Maria T Matyska; Joshua E Young

doi:10.1016/j.jpba.2014.02.019

Analysis of thiopurines using aqueous normal phase chromatography

J Pharm Biomed Anal. 2014 Jul:95:102-6. doi: 10.1016/j.jpba.2014.02.019. Epub 2014 Mar 3.

Authors

Joseph J Pesek¹, Maria T Matyska², Joshua E Young³

Affiliations

¹ Department of Chemistry, San Jose State University, San Jose, CA 95112, USA. Electronic address: pesek@sjsu.edu.
² Department of Chemistry, San Jose State University, San Jose, CA 95112, USA.
³ MicroSolv Technology Corporation, One Industrial Way West, Eatontown, NJ 01776, USA.

PMID: 24657678
DOI: 10.1016/j.jpba.2014.02.019

Abstract

The chromatography of several thiopurines is investigated using aqueous normal phase (ANP) conditions in conjunction with a silica hydride-based column. Both isocratic and gradient elution modes are tested. Detection of higher concentration samples is done by UV to demonstrate feasibility in this format while lower concentration samples utilize mass spectrometry (MS). Repeatability of successive runs is also tested with particular attention to gradient methods where the equilibration time of the stationary phase can be evaluated.

Keywords: Hydrophilic analytes; Metabolites; Pharmaceutical analysis; Silica hydride stationary phase.

MeSH terms

Chromatography, High Pressure Liquid / methods*
Guanine Nucleotides / analysis
Guanosine / analogs & derivatives
Guanosine / analysis
Thioguanine / analysis*
Thionucleosides / analysis*
Thionucleotides / analysis*

Substances

Guanine Nucleotides
Thionucleosides
Thionucleotides
Guanosine
6-thioguanylic acid
6-thioguanosine
Thioguanine