Extractive ethoxycarbonylation in high-temperature gas chromatography-mass spectrometry based analysis of serum estrogens

Ju Yeon Moon, Se Mi Kang, Myeong Hee Moon, Jongki Hong, Ki Tae Kim, Dae Hoon Jeong, Young Nam Kim, Bong Chul Chung, Man Ho Choi

Research output: Contribution to journalArticle

5 Citations (Scopus)

Abstract

A comprehensive gas chromatography-mass spectrometry (GC-MS)-based profiling was developed as a practical assay for quantification of 18 endogenous estrogens in serum samples. The present GC-MS method was conducted with the two-phase extractive ethoxycarbonlyation (EOC) of the phenolic hydroxy groups of estrogen with ethyl chlorformate combined with the non-polar n-hexane extraction. The subsequent perfluoroacylation of aliphatic hydroxy groups with pentafluoropropionyl anhydride (PFPA) was conducted. The serum samples were separated through a high temperature GC column (MXT-1) within an 8-min run and analyzed in selected-ion monitoring mode with good chromatographic properties for 18 estrogens as their EOC-PFP derivatives. The limit of quantification (LOQ) was 0.025-0.10ng/mL for most estrogens analyzed except for E3 and 2-OH-E3 (0.5ng/mL each). The devised method was found to be linear over a 10 3-fold concentration range with a correlation coefficient (r 2>0.992), whereas the precision (% CV) and accuracy (% bias) ranged from 3.1 to 16.3% and from 93.5 to 111.1%, respectively. Decreased 2-methoxy-17β-estradiol levels were confirmed in patients with preeclampsia than healthy pregnant women. This technique can be used for a clinical diagnosis as well as understanding the pathogenesis in estrogen-related disorders.

Original languageEnglish
Pages (from-to)3742-3748
Number of pages7
JournalJournal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Volume879
Issue number31
DOIs
Publication statusPublished - 2011 Dec 1

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry
  • Biochemistry
  • Clinical Biochemistry
  • Cell Biology

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