期刊
EUROPEAN JOURNAL OF MASS SPECTROMETRY
卷 21, 期 2, 页码 79-90出版社
IM PUBLICATIONS
DOI: 10.1255/ejms.1336
关键词
cortisol; hydrazide; hydrazine; MALDI-MS; reactive matrix; saliva
资金
- AIST research grant
- research grant program of LIXIL JS foundation
- Japan Society for the Promotion of Science (JSPS) KAKENHI [24619012]
- Ministry of Education, Culture, Sports, Science and Technology, Japan
- Grants-in-Aid for Scientific Research [26505011, 24619012] Funding Source: KAKEN
Fifty-one reagents (37 hydrazides and 14 hydrazines) were examined to determine if they could function as reactive matrices for the detection of steroids with carbonyl groups in matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Among these reagents, 3-hydroxy-2-naphthoic acid hydrazide reacted most efficiently with steroids with carbonyl groups, allowing detection of them at the 1 pmol level. Results from accurate mass measurement with a JMS-S3000 Spiral-TOF suggested that the ion peaks corresponding to the protonated fragment of a hydrazone were observed, in addition to the protonated molecular peaks of the resulting hydrazones ([M-D + H](+)) and their sodium adduct ([M-D + Na](+)). 3-Hydroxy-2-naphthoic acid hydrazide also could detect cortisol (1.93 ng) spiked in a human serum certified reference material, as well as cortisone and cortisol in a human saliva sample collected in the morning. Using a combination of 3-hydroxy-2-naphthoic acid hydrazide and alpha-cyano-4-hydroxycinammic acid (CHCA) (3-hydroxy-2-naphthoic acid hydrazide:CHCA = 4:1, v/v), even cortisone and cortisol in a human saliva sample collected in the afternoon, when levels are typically low, could be detected effectively.
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