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Hydrazide and Hydrazine Reagents as Reactive Matrices for Matrix-Assisted Laser desorption/ionization Mass Spectrometry to Detect Steroids With Carbonyl Groups

Yasushi Shigeri, Akikazu Yasuda, Masamichi Sakai, Shinya Ikeda, Ryuichi Arakawa, Hiroaki Sato, Tomoya Kinumi

Eur J Mass Spectrom (Chichester). 2015;21(2):79-90.

PMID: 26181281

Abstract:

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 1pmol 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 (1.93ng) 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 α- 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.

Chemicals Related in the Paper:

Catalog Number Product Name Structure CAS Number Price
AS2121445 Human serum (cortisol spiked) Human serum (cortisol spiked) Price
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