TY - JOUR
T1 - Mass spectrometric profiling of saturated fatty acid esters of steroids separated by high-temperature gas chromatography
AU - Jung, Hyun Jin
AU - Lee, Won Yong
AU - Chung, Bong Chul
AU - Choi, Man Ho
PY - 2009/2/27
Y1 - 2009/2/27
N2 - 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.
AB - 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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U2 - 10.1016/j.chroma.2008.12.059
DO - 10.1016/j.chroma.2008.12.059
M3 - Article
C2 - 19144339
AN - SCOPUS:59049106573
SN - 0021-9673
VL - 1216
SP - 1463
EP - 1468
JO - Journal of Chromatography A
JF - Journal of Chromatography A
IS - 9
ER -