Estradiol-17 beta determined in plasma by gas chromatography-mass spectrometry with selected ion monitoring of mixed silyl ether-perfluoroacyl ester derivatives and use of various stable-isotope-labeled internal standards

Journal Article · Sat Apr 01 04:00:00 EST 1989 · Clin. Chem. (Winston-Salem, N.C.); (United States)

OSTI ID:6155946

Dehennin, L

A highly specific method is described for measuring estradiol-17 beta (E2) in plasma by gas chromatography-mass spectrometry (GC-MS) associated with stable isotope dilution. A mixed derivative, E2-3-trimethylsilyl ether-17-heptafluorobutyrate (E2-3-TMS-17-HFB), was found to have excellent analytical properties. The specificity of the derivatization procedure exploits a unique feature of estrogens: the selective exchange of a phenolic perfluoroacyl ester for a trialkylsilyl ether. No significant differences in E2 concentration could be ascribed to the use of /sup 2/H- or /sup 13/C-labeled analogs, thus ruling out interferences from possible isotope exchange commonly attributed to deuterated compounds. Precision is closely similar to that for methods in which the more common E2-3, 17-bis(trimethylsilyl) ether and E2-3, 17-bis(heptafluorobutyrate) derivatives are used. Sensitivity and specificity of the mixed 3-TMS-17-HFB derivative allow adequate determinations of E2, even in plasma from males, in 2-mL samples. Interlaboratory mean concentrations of E2 obtained by routine immunoassays were consistently higher than the target values estimated by GC-MS, particularly at concentrations less than 100 pmol/L.

• Research Organization: Fondation de Recherche en Hormonologie, Fresnes (France)
• OSTI ID: 6155946
• Journal Information: Clin. Chem. (Winston-Salem, N.C.); (United States), Journal Name: Clin. Chem. (Winston-Salem, N.C.); (United States) Vol. 35:4; ISSN CLCHA
• Country of Publication: United States
• Language: English

Related Subjects

550201* -- Biochemistry-- Tracer Techniques
59 BASIC BIOLOGICAL SCIENCES
ACCURACY
BIOLOGICAL MATERIALS
BLOOD
BLOOD PLASMA
BODY FLUIDS
CARBON 13
CARBON ISOTOPES
CHROMATOGRAPHY
COMPARATIVE EVALUATIONS
CONTROL
DEUTERIUM
ESTRADIOL
ESTRANES
ESTROGENS
EVEN-ODD NUCLEI
GAS CHROMATOGRAPHY
HORMONES
HYDROGEN ISOTOPES
HYDROXY COMPOUNDS
ISOTOPE APPLICATIONS
ISOTOPE DILUTION
ISOTOPES
LIGHT NUCLEI
MASS SPECTROSCOPY
MATERIALS
MATHEMATICS
MEASURING METHODS
NUCLEI
ODD-ODD NUCLEI
ORGANIC COMPOUNDS
QUALITY CONTROL
REGRESSION ANALYSIS
SEPARATION PROCESSES
SPECIFICITY
SPECTROSCOPY
STABLE ISOTOPES
STATISTICS
STEROID HORMONES
STEROIDS
TRACER TECHNIQUES