Isotope-dilution mass spectrometry for quantification of urinary active androgens separated by gas chromatography

Su Hyeon Lee, Man Ho Choi, Wonyong Lee, Bong Chul Chung

Research output: Contribution to journalLetter

3 Citations (Scopus)

Abstract

Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methods are needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry (GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which are clinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with β-glucuronidase, solid-phase extraction, liquid-liquid extraction using methyl tert-butyl ether and subsequent conversion to pen-tafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive and selective analysis in selected-ion monitoring mode. Flophemesyl-TMS derivatization not only eliminates matrix interference but also has a good peak resolution within a 6 min-run. A selective and sensitive GC technique with flophemesyl-TMS derivatives also allows accurate quantitative analysis of three active androgens when combined with IDMS. The limit of quantification of the three analytes was <50 pg/mL, and extraction recoveries ranged from 91.9 to 102.1%. The precision and accuracy were 1.2~6.5% and 89.0~106.7%, respectively. This GC-IDMS method can be useful for evaluating the drug efficacy and monitoring the biological processes responsible for male-pattern baldness and prostate diseases.

Original languageEnglish
Pages (from-to)29-32
Number of pages4
JournalMass Spectrometry Letters
Volume1
Issue number1
DOIs
Publication statusPublished - 2010 Dec 1

Fingerprint

Isotopes
Gas chromatography
Gas Chromatography
Androgens
Dilution
Mass spectrometry
Mass Spectrometry
Alopecia
Prostate
Epitestosterone
Derivatives
Biological Phenomena
Liquid-Liquid Extraction
Enzymatic hydrolysis
Monitoring
Drug Monitoring
Dihydrotestosterone
Glucuronidase
Solid Phase Extraction
Liquids

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry
  • Spectroscopy
  • Biochemistry, Genetics and Molecular Biology(all)

Cite this

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title = "Isotope-dilution mass spectrometry for quantification of urinary active androgens separated by gas chromatography",
abstract = "Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methods are needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry (GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which are clinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with β-glucuronidase, solid-phase extraction, liquid-liquid extraction using methyl tert-butyl ether and subsequent conversion to pen-tafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive and selective analysis in selected-ion monitoring mode. Flophemesyl-TMS derivatization not only eliminates matrix interference but also has a good peak resolution within a 6 min-run. A selective and sensitive GC technique with flophemesyl-TMS derivatives also allows accurate quantitative analysis of three active androgens when combined with IDMS. The limit of quantification of the three analytes was <50 pg/mL, and extraction recoveries ranged from 91.9 to 102.1{\%}. The precision and accuracy were 1.2~6.5{\%} and 89.0~106.7{\%}, respectively. This GC-IDMS method can be useful for evaluating the drug efficacy and monitoring the biological processes responsible for male-pattern baldness and prostate diseases.",
author = "{Hyeon Lee}, Su and {Ho Choi}, Man and Wonyong Lee and {Chul Chung}, Bong",
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Isotope-dilution mass spectrometry for quantification of urinary active androgens separated by gas chromatography. / Hyeon Lee, Su; Ho Choi, Man; Lee, Wonyong; Chul Chung, Bong.

In: Mass Spectrometry Letters, Vol. 1, No. 1, 01.12.2010, p. 29-32.

Research output: Contribution to journalLetter

TY - JOUR

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AU - Hyeon Lee, Su

AU - Ho Choi, Man

AU - Lee, Wonyong

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AB - Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methods are needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry (GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which are clinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with β-glucuronidase, solid-phase extraction, liquid-liquid extraction using methyl tert-butyl ether and subsequent conversion to pen-tafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive and selective analysis in selected-ion monitoring mode. Flophemesyl-TMS derivatization not only eliminates matrix interference but also has a good peak resolution within a 6 min-run. A selective and sensitive GC technique with flophemesyl-TMS derivatives also allows accurate quantitative analysis of three active androgens when combined with IDMS. The limit of quantification of the three analytes was <50 pg/mL, and extraction recoveries ranged from 91.9 to 102.1%. The precision and accuracy were 1.2~6.5% and 89.0~106.7%, respectively. This GC-IDMS method can be useful for evaluating the drug efficacy and monitoring the biological processes responsible for male-pattern baldness and prostate diseases.

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