Quantification of serum dehydroepiandrosterone sulfate by liquid chromatography/atmospheric pressure chemical ionization mass spectrometry.

NAKAJIMA Masaharu, WAKABAYASHI Hiroyuki, YAMATO Susumu, SHIMADA Kenji

doi:10.2116/bunsekikagaku.45.517

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液体クロマトグラフィー／大気圧化学イオン化質量分析法による血清デヒドロエピアンドロステロンサルフェートの定量
エキタイクロマトグラフィータイキアツカガクイオンカシツリョウブンセキ
液体クロマトグラフィー : 大気圧化学イオン化質量分析法による血清デヒドロエピアンドロステロンサルフェートの定量(<特集>質量分析法の応用技術)

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Abstract

Liquid chromatography/atmospheric pressure chemical ionization mass spectrometry (LC/APCI-MS) combined with a column switching technique was applied to the quantification of serum dehydroepiandrosterone sulfate (DHEA-S). Human serum samples were directly injected into the sample preparation column (TSK precolumn BSA-ODS), and then DHEA-S was separated by an analytical column of Inertsil ODS-2. DHEA-S was detected on-line by a Hitachi M 1000 mass spectrometer equipped with an APCI interface. For the detection of DHEA-S, the drift, focus, and multiplier voltages were set at -70 V, -120 V and 2.4 kV, and the vaporizer and the desolvation temperatures were set at 280 and 399°C, respectively. The applied potential for the needle electrode was -10 μA. The detection limit of DHEA-S was 10 ng on-column with a signal-to-noise ratio of 3. The calibration curve was linear over the range of 50300 ng on-column. The proposed method was successfully developed for the determination of DHEA-S in human serum.

Journal

BUNSEKI KAGAKU

BUNSEKI KAGAKU 45 (6), 517-522, 1996

The Japan Society for Analytical Chemistry

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