Journal
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
Volume 52, Issue 5, Pages 809-818Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jpba.2010.03.001
Keywords
Carboxylic acid; Derivatization; LC-ESI-MS/MS; Sensitivity; Saliva
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Funding
- Japan Society for the Promotion of Science [2008-2010, 20590034]
- Ministry of Education, Culture, Sports, Science and Technology [2007-2011]
- Grants-in-Aid for Scientific Research [20590034] Funding Source: KAKEN
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A simple and practical derivatization procedure for increasing the detection responses of carboxylic acids in liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) has been developed. 2-Hydrazinopyridine (HP) and 2-picolylamine (PA) rapidly reacted with biologically and clinically important carboxylic acids [chenodeoxycholic acid, glycochenodeoxycholic acid, prostaglandin E(2), 2-(beta-carboxyethyl)-6-hydroxy-2,7,8-trimethylchroman (gamma-CEHC), alpha-lipoic acid, homovanillic acid (HVA) and 5-hydroxyindole-3-acetic acid] in the presence of 2,2'-dipyridyl disulfide and triphenylphosphine The resulting HP- and PA-derivatives were highly responsive in ESI-MS operating in the positive-ion mode and gave characteristic product ions during MS/MS, which enabled the sensitive detection using selected reaction monitoring. Among the two reagents. PA was of more practical use, the detection responses of the PA-derivatives were increased by 9-158-fold over the intact carboxylic acids and the limits of detection were in the low femtomole range (1.5-5 6 fmol on column). The PA-derivatization was successfully applied to a biological sample analysis, the derivatization followed by LC-ESI-MS/MS enabled the detection of trace amounts of bile acids, gamma-CEHC and HVA in human saliva with a simple pretreatment, small sample volume and short analysis time.
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