PMID- 20376914 OWN - NLM STAT- MEDLINE DCOM- 20100810 LR - 20190815 IS - 1873-264X (Electronic) IS - 0731-7085 (Linking) VI - 52 IP - 5 DP - 2010 Sep 5 TI - Simple and practical derivatization procedure for enhanced detection of carboxylic acids in liquid chromatography-electrospray ionization-tandem mass spectrometry. PG - 809-18 AB - 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 E2, 2-(-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. FAU - Higashi, Tatsuya AU - Higashi T AD - School of Pharmaceutical Sciences and Global COE Program, University of Shizuoka, 52-1 Yada, Suruga-ku, Shizuoka 422-8526, Japan. higashi@u-shizuoka-ken.ac.jp FAU - Ichikawa, Takuya AU - Ichikawa T FAU - Inagaki, Shinsuke AU - Inagaki S FAU - Min, Jun Zhe AU - Min JZ FAU - Fukushima, Takeshi AU - Fukushima T FAU - Toyo'oka, Toshimasa AU - Toyo'oka T LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - England TA - J Pharm Biomed Anal JT - Journal of pharmaceutical and biomedical analysis JID - 8309336 RN - 0 (Carboxylic Acids) SB - IM MH - Carboxylic Acids/*analysis MH - Chromatography, Liquid/*methods MH - Humans MH - Limit of Detection MH - Saliva/chemistry MH - Spectrometry, Mass, Electrospray Ionization/*methods MH - Tandem Mass Spectrometry/*methods EDAT- 2010/04/09 06:00 MHDA- 2010/08/11 06:00 CRDT- 2010/04/09 06:00 PHST- 2010/04/09 06:00 [entrez] PHST- 2010/04/09 06:00 [pubmed] PHST- 2010/08/11 06:00 [medline] AID - S0731-7085(10)00143-3 [pii] AID - 10.1016/j.jpba.2010.03.001 [doi] PST - ppublish SO - J Pharm Biomed Anal. 2010 Sep 5;52(5):809-18. doi: 10.1016/j.jpba.2010.03.001.