Application of pressurized fluid extraction technique in the gas chromatography-mass spectrometry determination of sterols from marine sediment samples

Abstract

In order to determine steroid compounds in GC/MS an analytical method using pressurized fluid extraction (PIE) was developed. While extracting in-house reference material (coastal sediment) typical recovery in PFE ranged from 80 to 120% (+/- 2.5-14.5) and the average extraction yield in PFE in comparison to conventional soxhlet extraction was 115%. In particular, the PFE showed higher extraction efficiency for C-29 and then sterols. Optimizing parameters such as temperature and pressure is critical in achieving this efficiency. Sterols in the sediment were derivatized with silyl reagent BSTFA in acetone for the final determination. A short column florisil cleanup offered the best separation of the GC/MS sensitive derivatives from co-contaminants. Thirty-three coastal sediment samples were analyzed using PFE and Soxhlet extraction methods. The results on extraction efficiency, silyl derivatization kinetics and purification efficiency demonstrated that PIE is far superior in extracting sterols from sediment samples. It is simple, fast, efficient and amenable for automation. (c) 2007 Elsevier B.V. All rights reserved.