Highly sensitive determination of estrone and estradiol in human serum by liquid chromatography–electrospray ionization tandem mass spectrometry
| Autor: | Sayuri Kobayashi, Mitsuteru Numazawa, Yoko Watanabe, Seijiro Honma, Kouwa Yamashita, Mitsunobu Okuyama |
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| Rok vydání: | 2007 |
| Předmět: |
Spectrometry
Mass Electrospray Ionization Estrone Hydrochloride Electrospray ionization Clinical Biochemistry Mass spectrometry Biochemistry chemistry.chemical_compound Endocrinology Tandem Mass Spectrometry Liquid chromatography–mass spectrometry Humans Picolinic Acids Derivatization Molecular Biology Pharmacology Detection limit Chromatography Estradiol Organic Chemistry Selected reaction monitoring chemistry Solvents Female Chromatography Liquid |
| Zdroj: | Steroids. 72:819-827 |
| ISSN: | 0039-128X |
| DOI: | 10.1016/j.steroids.2007.07.003 |
| Popis: | A highly sensitive and specific quantification method of estrone and estradiol in human serum was described based upon the use of picolinoyl derivatization and liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) in a positive mode. Estrogens were treated with picolinoyl chloride hydrochloride or picolinic acid and 2-methyl-6-nitrobenzoic anhydride followed by a solid-phase extraction with ODS cartridge. Picolinoyl derivatization proceeded quantitatively even in a microscale, and the picolinoyl esters provided simple positive ESI-mass spectra showing [M+H](+) as base peaks for these estrogens. The picolinoyl derivatives of these estrogens showed 100-fold higher detection response compared to underivatized intact molecules by LC-ESI-MS (selected reaction monitoring). Using this derivatization, estrogens spiked in the charcoal treated human serum samples were analyzed with limit of quantification (LOQ), intra-day accuracy and precision of 1.0pg/ml, 96.0% and 9.9% for estrone, and 0.5pg/ml, 84.4% and 12.8% for estradiol, respectively. Estrone and estradiol added to the crude serum samples were recovered with comparable LOQ and accuracy obtained for the charcoal treated serum samples as well. |
| Databáze: | OpenAIRE |
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