期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 404, 期 6-7, 页码 1925-1934出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-012-6320-0
关键词
Lactic acid; 3-Hydroxybutyric acid; Enantiomeric separation; Diabetes mellitus; Saliva; UPLC-ESI-MS/MS
资金
- Japan Society for the Promotion of Science
- Grants-in-Aid for Scientific Research [12J05726, 23790061, 24590055] Funding Source: KAKEN
A simultaneous determination method for the enantiomers of chiral carboxylic acids by the combination of ultraperformance liquid chromatography and mass spectrometry (UPLC-MS/MS) has been developed. (S)(+)-1-(2-Pyrrolidinylmethyl)-pyrrolidine (S-PMP) was used as the derivatization reagent for the high-throughput determination of biological chiral carboxylic acids, i.e., lactic acid (LA) and 3-hydroxybutyric acid (HA). The S-PMP efficiently reacted with the carboxylic acids under mild conditions at room temperature in the presence of 2,2'-dipyridyl disulfide and triphenylphosphine. The resulting S-PMP derivatives were highly responsive in the electrospray ionization (ESI)-MS operating in the positive-ion mode and gave characteristic product ions during the MS/MS, which enabled the sensitive detection using selected reaction monitoring. The derivatization was effective for the enantiomeric separation of the chiral carboxylic acids, and the resolution values of dl-LA and dl-HA were 4.91 and 9.37, respectively. Furthermore, a rapid separation of the derivatives of dl-LA and dl-HA within 7 min was performed using the UPLC system. The limits of detection on the column were in the low femtogram range (5-12 fg). The proposed procedure was successfully applied for the determination of the d- and l-isomers of LA and HA in the saliva of diabetes mellitus (DM) patients and healthy volunteers. The d-LA in DM patients was clearly higher than that in normal subjects. The derivatization followed by UPLC-ESI-MS/MS enabled the enantiomeric separation and detection of trace amounts of LA and HA in human saliva with a simple pretreatment and small sample volume.
作者
我是这篇论文的作者
点击您的名字以认领此论文并将其添加到您的个人资料中。
推荐
暂无数据