Determination of 24S-Hydroxycholesterol in Human Cerebrospinal Fluid by Gas Chromatography/Mass Spectrometry

• Yamazaki Reiko

  Department of Bio-Analytical Chemistry, Faculty of Pharmaceutical Sciences, Niigata University of Pharmacy and Applied Life Sciences

• Nakagawa Saori

  Department of Bio-Analytical Chemistry, Faculty of Pharmaceutical Sciences, Niigata University of Pharmacy and Applied Life Sciences

• Tanabe Akiko

  Department of Bio-Analytical Chemistry, Faculty of Pharmaceutical Sciences, Niigata University of Pharmacy and Applied Life Sciences

• Ikeuchi Takeshi

  Department of Molecular Neuroscience, Brain Research Institute, Niigata University

• Miida Takashi

  Division of Clinical Preventive Medicine, Department of Community Preventive Medicine, Niigata University Graduate School of Medical and Dental Sciences Present address, Department of Clinical Laboratory Medicine, Juntendo University School of Medicine

• Yamato Susumu

  Department of Bio-Analytical Chemistry, Faculty of Pharmaceutical Sciences, Niigata University of Pharmacy and Applied Life Sciences

Bibliographic Information

Other Title

• ガスクロマトグラフィー／質量分析法によるヒト脳脊髄液中の２４Ｓ－ヒドロキシコレステロールの定量
• ガス クロマトグラフィー シツリョウ ブンセキホウ ニ ヨル ヒト ノウ セキズイエキチュウ ノ 24S ヒドロキシコレステロール ノ テイリョウ

Abstract

A simple pretreatment method for the determination of 24S-hydroxycholesterol in human cerebrospinal fluid by gas chromatography/mass spectrometry (GC/MS) has been developed. Esterified cholesterol was saponified by a high concentration of potassium hydroxide (25 M, 1 mL) in a small volume (10 mL) of a conical test tube with a stopper made of glass. Next, free cholesterol was extracted with a small volume of n-hexane. The combined extracts obtained by the twice extraction were then applied on a silica cartridge for solid-phase extraction. A slight amount of 24S-hydroxycholestertol was separated from a large amount of cholesterol using n-hexane and ethylacetate as an elution solvent. 24S-hydroxycholestertol and 27-hydroxycholesterol-26,26,26,27,27-D₅ as an internal standard were converted to trimethylsilyl ethers by the trimethylsilyl (TMS) reagent, and then the TMS derivatives were determined by GC/MS. The method was successfully applied to the determination of 24S-hydroxycholestertol in human cerebrospinal fluid from patients of non-neurodegenerative disorders. The pretreatment method reported here was simple and useful for one multi-specimen material pretreatment.

Journal

• BUNSEKI KAGAKU

  BUNSEKI KAGAKU 57 (9), 707-713, 2008

  The Japan Society for Analytical Chemistry

Keywords

• sample pretreatment
• small scale
• 24S-hydroxycholesterol
• cerebrospinal fluid
• GC/MS

Details

• CRID: 1390001204354911232
• NII Article ID: 110006885128
• NII Book ID: AN00222633
• DOI: 10.2116/bunsekikagaku.57.707
• COI: 1:CAS:528:DC%2BD1cXhtFCnsb3E
• NDL BIB ID: 9656887
• ISSN: 05251931
• Web Site: https://ndlsearch.ndl.go.jp/books/R000000004-I9656887
• Web Site: http://www.jstage.jst.go.jp/article/bunsekikagaku/57/9/57_9_707/_pdf
• Web Site: http://dl.ndl.go.jp/info:ndljp/pid/10897067
• Web Site: https://search.jamas.or.jp/link/ui/2008370335
• Text Lang: ja
• Data Source:
  • JaLC
  • NDL
  • Crossref
  • NDL-Digital
  • CiNii Articles
  • KAKEN
• Abstract License Flag: Disallowed