1P-01 PDF
ステロイドホルモン検出用MALDI-MS反応マトリックス
Fifty-one reagents (37 hydrazides and 14 hydrazines) were examined to determine if they could function as reactive matrices to detect 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 and detected them at the 1 pmol level. Results from accurate mass measurement by 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 ([MD+H]+) and their sodium adduct ([MD+Na]+). The 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 CHCA (alpha-cyano-4-hydroxycinammic acid), (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.
References
Shigeri, Y., Yasuda, A., Sakai, M., Ikeda, S., Sato, H., and Kinumi, T. (2015) Hydrazide and hydrazine reagents as reactive matrices for MALDI-MS to detect steroids. Eur. J. Mass Spectrom., 21, 79-90