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

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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.
1993-04-30

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

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