期刊
CHIRALITY
卷 29, 期 10, 页码 603-609出版社
WILEY
DOI: 10.1002/chir.22726
关键词
chiral derivatization; d; l-kynurenine; d; l-tryptophan; solid-phase extraction; tandem MS; triazole-bonded column
资金
- KAKENHI [25460224]
- Japan Society for the Promotion of Science (JSPS)
- Ministry of Education, Culture, Sports, Science, and Technology (MEXT)
- Grants-in-Aid for Scientific Research [25460224] Funding Source: KAKEN
d- and l-Tryptophan (Trp) and d- and l-kynurenine (KYN) were derivatized with a chiral reagent, (S)-4-(3-isothiocyanatopyrrolidin-1-yl)-7-(N,N-dimethylaminosulfonyl)-2,1,3-benzoxadiazole (DBD-PyNCS), and were separated enantiomerically by high-performance liquid chromatography (HPLC) equipped with a triazole-bonded column (Cosmosil HILIC) using tandem mass spectrometric (MS/MS) detection. Effects of column temperature, salt (HCO2NH4) concentration, and pH of the mobile phase in the enantiomeric separation, followed by MS detection of (S)-DBD-PyNCS-d,l-Trp and -d,l-KYN, were investigated. The mobile phase consisting of CH3CN/10mM ammonium formate in H2O (pH5.0) (90/10) with a column temperature of 50-60 degrees C gave satisfactory resolution (Rs) and mass-spectrometric detection. The enantiomeric separation of d,l-Trp and d,l-KYN produced Rs values of 2.22 and 2.13, and separation factors () of 1.08 and 1.08, for the Trp and KYN enantiomers, respectively. The proposed LC-MS/MS method provided excellent detection sensitivity of both enantiomers of Trp and KYN (5.1-19nM).
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