Mass spectrometric profiling of saturated fatty acid esters of steroids separated by high-temperature gas chromatography

Hyun Jin Jung, Won Yong Lee, Bong Chul Chung, Man Ho Choi

Research output: Contribution to journalArticle

14 Citations (Scopus)

Abstract

An efficient analytical method for simultaneous determination of 12 SFEs in serum is described. The method involves solid-phase extraction to isolate of SFEs from interfering species, especially cholesteryl esters, conversion to trimethylsilyl (TMS) ether derivatives for the direct analysis by gas chromatography-mass spectrometry (GC-MS) using a high temperature MXT-1 (Silcosteel-treated stainless steel) capillary column. All SFEs as their TMS derivatives were well separated with excellent peak shapes within 12 min. Overall recoveries ranged from 88% to 119%, with a detection limits for SFEs ranged from 2 to 30 μg L-1. The linearity as correlation coefficient was higher than 0.99 except for pregnenolone-3-arachidate (r2 = 0.98) in the concentration range of 5-3000 μg L-1. Ten serum samples obtained from volunteers were also analyzed and quantitatively determined of DHEA-3-palmitate and pregnenolone-3-stearate in 1.8-1195.8 μg L-1 concentration. The devised high temperature GC-MS method could be useful for identification of SFEs in biological specimens including serum.

Original languageEnglish
Pages (from-to)1463-1468
Number of pages6
JournalJournal of Chromatography A
Volume1216
Issue number9
DOIs
Publication statusPublished - 2009 Feb 27

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Gas chromatography
Gas Chromatography
Mass spectrometry
Esters
Fatty Acids
Steroids
Derivatives
Pregnenolone
Gas Chromatography-Mass Spectrometry
Temperature
Dehydroepiandrosterone
Cholesterol Esters
Palmitates
Stainless Steel
Serum
Ether
Solid Phase Extraction
Recovery
Limit of Detection
Volunteers

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry
  • Organic Chemistry
  • Biochemistry

Cite this

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abstract = "An efficient analytical method for simultaneous determination of 12 SFEs in serum is described. The method involves solid-phase extraction to isolate of SFEs from interfering species, especially cholesteryl esters, conversion to trimethylsilyl (TMS) ether derivatives for the direct analysis by gas chromatography-mass spectrometry (GC-MS) using a high temperature MXT-1 (Silcosteel-treated stainless steel) capillary column. All SFEs as their TMS derivatives were well separated with excellent peak shapes within 12 min. Overall recoveries ranged from 88{\%} to 119{\%}, with a detection limits for SFEs ranged from 2 to 30 μg L-1. The linearity as correlation coefficient was higher than 0.99 except for pregnenolone-3-arachidate (r2 = 0.98) in the concentration range of 5-3000 μg L-1. Ten serum samples obtained from volunteers were also analyzed and quantitatively determined of DHEA-3-palmitate and pregnenolone-3-stearate in 1.8-1195.8 μg L-1 concentration. The devised high temperature GC-MS method could be useful for identification of SFEs in biological specimens including serum.",
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Mass spectrometric profiling of saturated fatty acid esters of steroids separated by high-temperature gas chromatography. / Jung, Hyun Jin; Lee, Won Yong; Chung, Bong Chul; Choi, Man Ho.

In: Journal of Chromatography A, Vol. 1216, No. 9, 27.02.2009, p. 1463-1468.

Research output: Contribution to journalArticle

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