期刊
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
卷 196, 期 -, 页码 -出版社
ELSEVIER
DOI: 10.1016/j.jpba.2021.113939
关键词
Chiral resolution; Thiol; DL-cysteine; DL-homocysteine; Oxidative stress; NCS-OTPP; UHPLC-Q-Orbitrap HRMS
资金
- National Natural Science Foundation of China [81660594]
- Science and Technology Development Project, Education Department of Jilin Province of China [JJKH20191151KJ]
A high-sensitivity and -selectivity mass spectrometry derivatization reagent, NCS-OTPP, was developed for enantiomeric separation of chiral thiol compounds. Complete separation of GSH, DL-Cys, and DL-Hcy was achieved, with good linear relationships, precision, and recoveries. The thiol compounds were quantitatively related to oxidative stress state changes in saliva and urine.
A high-sensitivity and -selectivity mass spectrometry derivatization reagent, (R)-(5-(3-isothiocyanatopyrrolidin-1-yl)-5-oxopentyl) triphenylphosphonium (NCS-OTPP), was developed for the enantiomeric separation of chiral thiol compounds as prospectively important diagnostic markers for oxidative stress-related diseases. Complete separation of GSH, DL-Cys, and DL-Hcy was achieved. The parent ions of all derivatives had a fragment of m/z 473.18 and a structure of m/z 75.95 (R-S = C-S-R'), conducive to qualitative and quantitative analysis. Good linear relationships were obtained for all analytes (R-2 >= 0.9995). The intra-day and inter-day precision were 0.82-5.16 % and 1.02-4.18 % in saliva, and 0.81-3.45 % and 0.99-6.47 % in urine, with mean recoveries of 83.31-105.66 % and 84.09-101.11 %, respectively. The limit of detection (S/N = 3) was 19.20-57.60 nM. Free and total GSH, DL-Cys, and DL-Hcy were detected simultaneously in saliva and urine from 10 volunteers in the normal, stressed, and stable states by UHPLC-Q-Orbitrap HRMS. The thiol compounds were quantitatively related to oxidative stress state changes. (C) 2021 Elsevier B.V. All rights reserved.
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