Development of sensitive derivatization method for aldosterone in liquid chromatography-electrospray ionization tandem mass spectrometry of corticosteroids

Kouwa Yamashita, Mitsunobu Okuyama, Risa Nakagawa, Seijiro Honma, Fumitoshi Satoh, Ryo Morimoto, Sadayoshi Ito, Madoka Takahashi, Mitsuteru Numazawa

Research output: Contribution to journalArticlepeer-review

45 Citations (Scopus)

Abstract

A highly sensitive quantification method of aldosterone by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) was investigated in a positive mode using recently developed picolinyl derivatization. Aldosterone was smoothly and quantitatively converted to the ethyl ether-picolinyl derivative by treatment with HCl-ethanol followed by the esterification with picolinic acid in the presence of 2-methyl-6-nitrobenzoic anhydride and 4-dimethylaminopyridine. The positive ion-ESI mass spectrum of the ethyl ether-picolinyl derivative was characterized by an appearance of protonated molecule ([M+H]+) as a base peak. The ethyl ether-picolinyl derivatization gave a successful result in a separation of aldosterone from corticosterone, dehydrocorticosterone and cortexolone, and also provided an approximately 10-fold higher ESI response in the positive-LC-ESI-MS/MS (selected reaction monitoring; SRM) when compared to that of underivatized molecule (negative mode). The limit of quantification of aldosterone by SRM using ethyl ether-picolinyl derivatization (m/z 494 → m/z 448) was 1 pg/0.2 ml serum with accuracy and precision of 92.6% and 5.6%, respectively.

Original languageEnglish
Pages (from-to)114-121
Number of pages8
JournalJournal of Chromatography A
Volume1200
Issue number2
DOIs
Publication statusPublished - 2008 Jul 25

Keywords

  • Aldosterone
  • Derivatization
  • Electrospray ionization tandem mass spectrometry
  • High-performance liquid chromatography
  • Picolinyl ester

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Organic Chemistry

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