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Determination of dehydroepiandrosterone sulphate in biological samples by liquid chromatography/atmospheric pressure chemical ionization‐mass spectrometry using [7,7,16,16‐ 2 H 4 ]‐dehydroepiandrosterone sulphate as an internal standard
Author(s) -
Nakajima Masaharu,
Yamato Susumu,
Shimada Kenji
Publication year - 1998
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/(sici)1099-0801(199807/08)12:4<211::aid-bmc737>3.0.co;2-n
Subject(s) - chemistry , atmospheric pressure chemical ionization , chromatography , chemical ionization , mass spectrometry , dehydroepiandrosterone , detection limit , analytical chemistry (journal) , ionization , androgen , ion , biochemistry , organic chemistry , hormone
A method for the determination of dehydroepiandrosterone sulphate (DHEA‐S) in biological samples is described. [7,7,16,16‐ 2 H 4 ]‐Dehydroepiandrosterone sulphate ( 2 H 4 ‐DHEA‐S) was synthesized and its applicability was examined as an internal standard with liquid chromatography/atmospheric pressure chemical ionization‐mass spectrometry (LC/APCI‐MS). Deuterium atoms in 2 H 4 ‐DHEA‐S molecules were not exchnaged to hydrogen atoms during the extraction procedure from biological specimens in the determination of DHEA‐S with LC/MS. The calibration curve of DHEA‐S was linear over the range of 2–500 ng on‐column. The detection lmit of DHEA‐S was 0.5 ng on‐column with a signal‐to‐noise ratio of 3. The relative standard deviations of intra‐ and inter‐assay with 200 ng of standard sample were 3.3 and 5.0%, respectively. These results were better than a similar method reported on previously (Nakajima et al. , 1996). The proposed method was successfully developed for the determination of DHEA‐S in bilogical samples. © 1998 John Wiley & Sons, Ltd.