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使用氘代内标物通过气相色谱/质谱法测定人血浆中的硫酸脱氢表雄酮:一种适用于常规临床应用的方法。

Determination of dehydroepiandrosterone sulfate in human plasma by gas chromatography/mass spectrometry using a deuterated internal standard: a method suitable for routine clinical use.

作者信息

Wudy S A, Wachter U A, Homoki J, Teller W M

机构信息

First Department of Pediatrics, University of Ulm/Donau, FRG.

出版信息

Horm Res. 1993;39(5-6):235-40. doi: 10.1159/000182742.

Abstract

A capillary gas chromatographic-mass spectrometric method for the determination of dehydroepiandrosterone sulfate (DHEA-S) in human plasma is described. [7,7-2H2]DHEA-S is used as internal standard. After desulfation by methanolysis, heptafluorobutyryl derivatives are prepared, and selected ion monitoring of characteristic fragment ions--m/z 270 for DHEA and m/z 272 for [7,7-2H2]DHEA--carried out. Requiring small amounts of plasma, the rapid, convenient work-up and the application of bench-top GC/MS instrumentation proved our method to be suited for routine clinical use in adults and children. The method needs no complex corrections for isotope contributions and provides good accuracy and precision. Comparative values of samples assayed by our GC/MS procedure and by a direct RIA indicated that the RIA overestimates the true concentration.

摘要

描述了一种用于测定人血浆中硫酸脱氢表雄酮(DHEA-S)的毛细管气相色谱-质谱法。以[7,7-2H2]DHEA-S作为内标。通过甲醇解脱硫后,制备七氟丁酰衍生物,并对特征碎片离子进行选择离子监测——DHEA的m/z 270和[7,7-2H2]DHEA的m/z 272。该方法所需血浆量少,操作快速、简便,且使用台式GC/MS仪器,证明适用于成人和儿童的常规临床应用。该方法无需对同位素贡献进行复杂校正,具有良好的准确度和精密度。通过我们的GC/MS程序和直接放射免疫分析法(RIA)测定的样品比较值表明,RIA高估了真实浓度。

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