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  • 标题:キャピラリーガスクロマトグラフィーによるローヤルゼリー中のトランス-10-ハイドロキシ-2-デセン酸の定量
  • 本地全文:下载
  • 作者:太田 彦人 ; 瀬戸 康雄 ; 角田 紀子
  • 期刊名称:Journal of Health Science
  • 印刷版ISSN:1344-9702
  • 电子版ISSN:1347-5207
  • 出版年度:1993
  • 卷号:39
  • 期号:2
  • 页码:155-160
  • DOI:10.1248/jhs1956.39.2_155
  • 出版社:The Pharmaceutical Society of Japan
  • 摘要:The determination and confirmation of trans-10-hydroxydecenoic acid (10-HDA) in royal jelly (RJ) were developed by capillary gas chromatography (GC) and GC-chemical ionization mass spectrometry (CI-MS) equipped with an ion trap detector (ITD) as a mass spectrometer. It was found that 10-HDA extracted with dichloromethane at pH 2.5 was converted into trimethylsilyl (TMS) derivative in a constant yield by the reaction with N, O-bis (trimethylsilyl) acetamide at room temperature for 15 min. The recovery of 10-HDA (50 μg) was 99.5%. The TMS derivatives of raw RJ tested showed a satisfactory result of separation and sensitivity by GC using a DB-1 capillary column with a flame ionization detector. The linear dynamic detection range was approximately from 50 ng to 500 μg (16.7-167000 ppm) determined using n-eicosane as an internal standard. The minimum detectable amount of 10-HDA was found to be 50 ng (16.7 ppm) at the split ratio of 40 : 1 of the split injection. The amount of 10-HDA in the raw RJ sample was 2.28±0.04% determined by the GC method and 2.25±0.01% by the HPLC method as described previously, respectively. The TMS derivatives of 10-HDA and its related compounds in the raw RJ were confirmed by ITD-GC. The diagnostic ions of TMS-HDA were presented at m/z 331 (M+1), 315 (M-Me), and 241 (M-OTMS) in isobutane CI mode. The present GC method is an easier and more convenient method for the analysis of 10-HDA in RJ and is applicable for the determination and confirmation of 10-HDA in forensic and food samples.
  • 关键词:trans-10-hydroxydecenoic acid;royal jelly;trimethylsilyl derivative;GC;GC-MS;CI-MS
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