Analysis of anabolic steroids by partial filling micellar electrokinetic capillary chromatography and electrospray mass spectrometry

Lotta Kaarina Amundsen, Juha T. Kokkonen, Stella Rovio, Heli Sirén (Corresponding Author)

Research output: Contribution to journalArticleScientificpeer-review

41 Citations (Scopus)

Abstract

A partial filling micellar electrokinetic capillary chromatography (PF-MEKC) separation of six anabolic androgenic steroids (androstenedione, metandienone, fluoxymesterone, methyltestosterone, 17-epimetandienone and testosterone) is introduced. The method utilises a mixed micellar solution consisting of sodium dodecyl sulphate (SDS) and sodium taurocholate. The analytes are detected with a photodiode array detector at 247 nm wavelength. Methyltestosterone is used as internal standard. The detection limits were 39 μg/L for androstenedione, 40 μg/L for testosterone, 45 μg/L for fluoxymesterone, 45–90 μg/L for 17-epimetandienone, 59 μg/L for methyltestosterone and 90 μg/L for metandienone. Linear correlation between concentration (0.1–5.0 mg/L) and detector response was obtained with r2 of 0.994 for fluoxymesterone, 0.998 for 17-epimetandienone and 0.999 for androstenedione, metandienone and testosterone. In addition, ionisation of the investigated compounds in electrospray mass spectrometry (ESI-MS) was studied in positive ion mode. The most intense signal (100%) was the protonated molecular ion [M+H]+, except for 17-epimetandienone, which gave its strongest signal at m/z corresponding to [M−H2O+H]+. Finally, separation and identification of fluoxymesterone, androstenedione and testosterone by PF-MEKC–ESI-MS is described. This is the first use of PF-MEKC and PF-MEKC–ESI-MS assays for anabolic androgenic steroids.
Original languageEnglish
Pages (from-to)123 - 131
Number of pages9
JournalJournal of Chromatography A
Volume1040
Issue number1
DOIs
Publication statusPublished - 2004
MoE publication typeA1 Journal article-refereed

Fingerprint

Fluoxymesterone
Testosterone Congeners
Micellar Electrokinetic Capillary Chromatography
Methandrostenolone
Androstenedione
Methyltestosterone
Chromatography
Mass spectrometry
Testosterone
Mass Spectrometry
Steroids
Ions
Detectors
Taurocholic Acid
Electrospray Ionization Mass Spectrometry
Photodiodes
Sodium Dodecyl Sulfate
Ionization
Limit of Detection
Assays

Keywords

  • Doping analysis
  • Partial filling micellar electrokinetic chromatography
  • Steroids
  • Hormones

Cite this

Amundsen, Lotta Kaarina ; Kokkonen, Juha T. ; Rovio, Stella ; Sirén, Heli. / Analysis of anabolic steroids by partial filling micellar electrokinetic capillary chromatography and electrospray mass spectrometry. In: Journal of Chromatography A. 2004 ; Vol. 1040, No. 1. pp. 123 - 131.
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abstract = "A partial filling micellar electrokinetic capillary chromatography (PF-MEKC) separation of six anabolic androgenic steroids (androstenedione, metandienone, fluoxymesterone, methyltestosterone, 17-epimetandienone and testosterone) is introduced. The method utilises a mixed micellar solution consisting of sodium dodecyl sulphate (SDS) and sodium taurocholate. The analytes are detected with a photodiode array detector at 247 nm wavelength. Methyltestosterone is used as internal standard. The detection limits were 39 μg/L for androstenedione, 40 μg/L for testosterone, 45 μg/L for fluoxymesterone, 45–90 μg/L for 17-epimetandienone, 59 μg/L for methyltestosterone and 90 μg/L for metandienone. Linear correlation between concentration (0.1–5.0 mg/L) and detector response was obtained with r2 of 0.994 for fluoxymesterone, 0.998 for 17-epimetandienone and 0.999 for androstenedione, metandienone and testosterone. In addition, ionisation of the investigated compounds in electrospray mass spectrometry (ESI-MS) was studied in positive ion mode. The most intense signal (100{\%}) was the protonated molecular ion [M+H]+, except for 17-epimetandienone, which gave its strongest signal at m/z corresponding to [M−H2O+H]+. Finally, separation and identification of fluoxymesterone, androstenedione and testosterone by PF-MEKC–ESI-MS is described. This is the first use of PF-MEKC and PF-MEKC–ESI-MS assays for anabolic androgenic steroids.",
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Analysis of anabolic steroids by partial filling micellar electrokinetic capillary chromatography and electrospray mass spectrometry. / Amundsen, Lotta Kaarina; Kokkonen, Juha T.; Rovio, Stella; Sirén, Heli (Corresponding Author).

In: Journal of Chromatography A, Vol. 1040, No. 1, 2004, p. 123 - 131.

Research output: Contribution to journalArticleScientificpeer-review

TY - JOUR

T1 - Analysis of anabolic steroids by partial filling micellar electrokinetic capillary chromatography and electrospray mass spectrometry

AU - Amundsen, Lotta Kaarina

AU - Kokkonen, Juha T.

AU - Rovio, Stella

AU - Sirén, Heli

PY - 2004

Y1 - 2004

N2 - A partial filling micellar electrokinetic capillary chromatography (PF-MEKC) separation of six anabolic androgenic steroids (androstenedione, metandienone, fluoxymesterone, methyltestosterone, 17-epimetandienone and testosterone) is introduced. The method utilises a mixed micellar solution consisting of sodium dodecyl sulphate (SDS) and sodium taurocholate. The analytes are detected with a photodiode array detector at 247 nm wavelength. Methyltestosterone is used as internal standard. The detection limits were 39 μg/L for androstenedione, 40 μg/L for testosterone, 45 μg/L for fluoxymesterone, 45–90 μg/L for 17-epimetandienone, 59 μg/L for methyltestosterone and 90 μg/L for metandienone. Linear correlation between concentration (0.1–5.0 mg/L) and detector response was obtained with r2 of 0.994 for fluoxymesterone, 0.998 for 17-epimetandienone and 0.999 for androstenedione, metandienone and testosterone. In addition, ionisation of the investigated compounds in electrospray mass spectrometry (ESI-MS) was studied in positive ion mode. The most intense signal (100%) was the protonated molecular ion [M+H]+, except for 17-epimetandienone, which gave its strongest signal at m/z corresponding to [M−H2O+H]+. Finally, separation and identification of fluoxymesterone, androstenedione and testosterone by PF-MEKC–ESI-MS is described. This is the first use of PF-MEKC and PF-MEKC–ESI-MS assays for anabolic androgenic steroids.

AB - A partial filling micellar electrokinetic capillary chromatography (PF-MEKC) separation of six anabolic androgenic steroids (androstenedione, metandienone, fluoxymesterone, methyltestosterone, 17-epimetandienone and testosterone) is introduced. The method utilises a mixed micellar solution consisting of sodium dodecyl sulphate (SDS) and sodium taurocholate. The analytes are detected with a photodiode array detector at 247 nm wavelength. Methyltestosterone is used as internal standard. The detection limits were 39 μg/L for androstenedione, 40 μg/L for testosterone, 45 μg/L for fluoxymesterone, 45–90 μg/L for 17-epimetandienone, 59 μg/L for methyltestosterone and 90 μg/L for metandienone. Linear correlation between concentration (0.1–5.0 mg/L) and detector response was obtained with r2 of 0.994 for fluoxymesterone, 0.998 for 17-epimetandienone and 0.999 for androstenedione, metandienone and testosterone. In addition, ionisation of the investigated compounds in electrospray mass spectrometry (ESI-MS) was studied in positive ion mode. The most intense signal (100%) was the protonated molecular ion [M+H]+, except for 17-epimetandienone, which gave its strongest signal at m/z corresponding to [M−H2O+H]+. Finally, separation and identification of fluoxymesterone, androstenedione and testosterone by PF-MEKC–ESI-MS is described. This is the first use of PF-MEKC and PF-MEKC–ESI-MS assays for anabolic androgenic steroids.

KW - Doping analysis

KW - Partial filling micellar electrokinetic chromatography

KW - Steroids

KW - Hormones

U2 - 10.1016/j.chroma.2004.03.061

DO - 10.1016/j.chroma.2004.03.061

M3 - Article

VL - 1040

SP - 123

EP - 131

JO - Journal of Chromatography A

JF - Journal of Chromatography A

SN - 0021-9673

IS - 1

ER -