LC/MS/MS of Steroids Having Vicinal Diol as Electrospray-Active Boronates
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- Higashi Tatsuya
- Faculty of Pharmaceutical Sciences, Tokyo University of Science
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- Kawasaki Katsumi
- Faculty of Pharmaceutical Sciences, Tokyo University of Science
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- Matsumoto Nagisa
- Faculty of Pharmaceutical Sciences, Tokyo University of Science
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- Ogawa Shoujiro
- Faculty of Pharmaceutical Sciences, Tokyo University of Science
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- Mitamura Kuniko
- Faculty of Pharmaceutical Sciences, Kinki University
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- Ikegawa Shigeo
- Faculty of Pharmaceutical Sciences, Kinki University
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Abstract
A derivatization procedure with (3-dimethylaminophenyl)dihydroxyborane (DAPB) was introduced to enhance the detectability of steroids having a vicinal diol in LC/electrospray ionization (ESI)-MS/MS. DAPB reacted with the vicinal diol on the steroids [4β-hydroxycholesterol (4-HCh), pregnanetriol (PT) and 20R,22R-dihydroxycholesterol] in pyridine at 50°C within 1 h. The resulting DAPB-derivatives were highly responsive in ESI-MS operating in the positive-ion mode and gave characteristic product ions during MS/MS, which enabled sensitive detection using a selected reaction monitoring mode; the detection responses of the DAPB-derivatives were increased by 20–160-fold over those of the intact steroids and the limits of detection were in the low femtomole or attomole range. The derivatization procedure was successfully applied to biological sample analysis; the derivatization followed by LC/ESI-MS/MS enabled the specific detection of trace amounts of 4-HCh in human plasma and PT in human urine with a small sample volume, simple pretreatment and short chromatographic run time.
Journal
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- Chemical and Pharmaceutical Bulletin
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Chemical and Pharmaceutical Bulletin 61 (3), 326-332, 2013
The Pharmaceutical Society of Japan
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Details 詳細情報について
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- CRID
- 1390282679154190976
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- NII Article ID
- 130003360741
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- NII Book ID
- AA00602100
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- COI
- 1:STN:280:DC%2BC3svit1OltA%3D%3D
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- ISSN
- 13475223
- 00092363
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- NDL BIB ID
- 024284104
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- PubMed
- 23449202
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- Text Lang
- en
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- Data Source
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- JaLC
- NDL
- Crossref
- PubMed
- CiNii Articles
- KAKEN
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- Abstract License Flag
- Disallowed