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Article
Analysis of Fifteen Estrogen Metabolites Using Packed Column Supercritical Fluid Chromatography-Mass Spectrometry
Analytical Chemistry
  • Xia Xu
  • John M. Roman
  • Timothy D. Veenstra, Cedarville University
  • Jennifer Van Anda
  • Regina G. Ziegler
  • Haleem J. Issaq
Document Type
Article
Publication Date
3-1-2006
DOI
10.1021/ac051425c
PubMed ID
16503607
Abstract

Packed column supercritical fluid chromatography with tandem mass spectrometry was used for the separation of estrone, estradiol, estriol, 16-epiestriol, 17-epiestriol, 16-ketoestradiol, 16alpha-hydroxyestrone, 2-methoxyestrone, 4-methoxyestrone, 2-hydroxyestrone-3-methyl ether, 2-methoxyestradiol, 4-methoxyestradiol, 2-hydroxyestrone, 4-hydroxyestrone, and 2-hydroxyestradiol. A gradient of methanol in carbon dioxide (0-30% methanol in 15 min, 2% change/min) at a flow rate of 2 mL/min and cyanopropyl silica column connected in series with a diol column, both 2.1 mm i.d. x 150 mm long, packed with 5-mum spherical silica-based particles, resulted in the separation and quantification of all 15 estrogens in less than 10 min. The limit of detection (LOD) and limit of quantitation (LOQ) of this pSFC MS/MS method was determined to be 0.5 (S/N = 3), and 5 pg, respectively. Compared with RP-HPLC MS analysis of the same mixture in terms of speed of analysis and sensitivity, pSFC MS is much faster, 10 versus 70 min, with comparable LOD and LOQ.

Keywords
  • Carbon dioxide,
  • chromatography,
  • supercritical fluid,
  • estrogens,
  • metabolism,
  • methanol,
  • sensitivity,
  • specificity,
  • tandem mass spectrometry
Citation Information
Xia Xu, John M. Roman, Timothy D. Veenstra, Jennifer Van Anda, et al.. "Analysis of Fifteen Estrogen Metabolites Using Packed Column Supercritical Fluid Chromatography-Mass Spectrometry" Analytical Chemistry Vol. 78 Iss. 5 (2006) p. 1553 - 1558 ISSN: 0003-2700
Available at: http://works.bepress.com/timothy-veenstra/237/