Determination of catechol and guaiacol estrogens in urine by capillary gas chromatography/mass spectrometry.
A gas chromatographic (GC)/mass spectrometric method for the simultaneous determination in urine of 2- and 4-hydroxyestrones and hydroxyestradiols, and their monomethyl ethers, is described. Separation of these catechol and guaiacol estrogens was achieved by derivatization into their trimethylsilyl and tert-butyldimethylsilyl ethers, followed by capillary GC on a DB-1 column. The calibration graphs were satisfactorily constructed for these estrogen metabolites by selected ion monitoring at the respective molecular ions using 2-bromoestrone and 4-hydroxyestradiol-d3 3-methyl ether as internal standards. The extraction and purification of the desired estrogens in biological fluids were effected by the combined use of Extrelut-3 and ion exchange columns. The sensitivity and reliability obtained by the newly developed method has proved to be satisfactory for the quantitation of catechol and guaiacol estrogens in human urine.
Hatano Research Institute, Food and Drug Safety Center, Kanagawa, Japan.
K
K
Saegusa
E
E
Suzuki
T
T
Anjo
Y
Y
Matsuki
T
T
Nambara
D004958:Estradiol / Q000031:analogs & derivatives / Q000652:urine; D004967:Estrogens / Q000652:urine*; D002393:Estrogens, Catechol / Q000652:urine*; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006139:Guaiacol / Q000652:urine*; D006801:Humans; D006894:Hydroxyestrones / Q000652:urine; D008745:Methylation; D011247:Pregnancy; D014297:Trimethylsilyl Compounds
D004967:Estrogens; D002393:Estrogens, Catechol; D006894:Hydroxyestrones; D014297:Trimethylsilyl Compounds; C026418:4-hydroxyestrone; D004958:Estradiol; D006139:Guaiacol; C001390:2-hydroxyestradiol; C014036:4-hydroxyestradiol; C024980:2-hydroxyestrone