極性誘導体化による血中ステロイドの高感度ＬＣ／ＥＳＩ‐ＭＳ分析
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概要
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Polar derivatization method for electrospray ionization (ESI) was developed and applied to the sensitive analysis of nonpolar ketosteroid in plasma. 4-Androstene-3,17-dione (androstenedione) in human plasma was purified by solid-phase extraction with Bond Elut C18 and derivatized to the carboxymethyloxime form (androstenedioxime) as a polar derivative. Androstenedione-<I>d</I>6 as an internal standard was synthesized and its deuterium contents were satisfactory for the sensitive analysis of androstenedione. The LC/ESI-MS condition for androstenedioxime was performed and single peak was obtained without separation of four steric isomers. Sensitivity of androstenedioxime in this mehtod was enhanced 5 times higher than androstenedione. Calibration graphs were linear (<I>r</I>=0.999) from 2.5 to 100 ng/m<I>l</I> for androstenedione extracted from human plasma and inter-assay precision (RSD) was within 6%.
- 日本質量分析学会の論文
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