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Analysis of fifteen estrogen metabolites using packed column supercritical fluid chromatography-mass spectrometry

  1. Author:
    Xu, X.
    Roman, J. M.
    Veenstra, T. D.
    Van Anda, J.
    Ziegler, R. G.
    Issaq, H. J.
  2. Author Address

    NCI, Lab Proteom & Analyt Technol, SAIC Frederick Inc, Frederick, MD 21702 USA. Mettler Toledo, Newark, DE 19702 USA. NCI, Div Canc Epidemiol & Genet, Epidemiol & Biostat Program, Bethesda, MD 20892 USA Issaq, HJ, NCI, Lab Proteom & Analyt Technol, SAIC Frederick Inc, Frederick, MD 21702 USA
    1. Year: 2006
    2. Date: MAR 1
  1. Journal: Analytical Chemistry
    1. 78
    2. 5
    3. Pages: 1553-1558
  2. Type of Article: Article
  1. 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, 16 alpha-hydroxyestrone, 2-methoxyestrone, 4-methoxyestrorre, 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-mu m 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

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