Document Detail

Simultaneous determination of DL: -lactic acid and DL: -3-hydroxybutyric acid enantiomers in saliva of diabetes mellitus patients by high-throughput LC-ESI-MS/MS.
MedLine Citation:
PMID:  22895741     Owner:  NLM     Status:  Publisher    
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.
Haruhito Tsutsui; Toshiki Mochizuki; Toshio Maeda; Ichiro Noge; Yutaka Kitagawa; Jun Zhe Min; Kenichiro Todoroki; Koichi Inoue; Toshimasa Toyo'oka
Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2012-8-16
Journal Detail:
Title:  Analytical and bioanalytical chemistry     Volume:  -     ISSN:  1618-2650     ISO Abbreviation:  Anal Bioanal Chem     Publication Date:  2012 Aug 
Date Detail:
Created Date:  2012-8-16     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  101134327     Medline TA:  Anal Bioanal Chem     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
Laboratory of Analytical and Bio-Analytical Chemistry, School of Pharmaceutical Sciences, University of Shizuoka, 52-1 Yada, Suruga-ku, Shizuoka, 422-8526, Japan.
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