Isotopic dilution method for bile acid profiling reveals new sulfate glycine-conjugated dihydroxy bile acids and glucuronide bile acids in serum.
J Pharm Biomed Anal
; 173: 1-17, 2019 Sep 05.
Article
em En
| MEDLINE
| ID: mdl-31100508
ABSTRACT
An ultrahigh performance liquid chromatography tandem mass spectrometry method (UHPLC-MS/MS) was developed for the determination of 41 target and 8 additional bile acids isomers (BAs) in biological fluids. BAs were analysed by solid-phase extraction on 50 µL biofluid-aliquots, followed by a properly optimised 27 min-chromatographic run. The method provided high sensitivity (limits of detection 0.0002-0.03 µM, limits of quantitation 0.0007-0.11 µM), linearity (R2>0.99) and precision (relative standard deviations ≤16%). A strategy of scheduled/ unscheduled injections of real samples together with neutral loss (80 Da and 176 Da) scans allowed us to find additional bile acid isomers not a priori included in the method, while high resolution full scan and MS/MS fragmentation analysis confirmed their structural adherence to the bile acid family. Moreover this is the first study quantifying four sulfate glycine conjugated-dihydroxy bile acid isomers, independently of the diet and postprandial time. Application to a dietary intervention kinetic study confirmed the existence of possible metabotypes amongst the study population (n = 20). A trend differentiating males from females was observed suggesting that serum samples from women contained smaller amounts of certain bile acids.
Palavras-chave
Texto completo:
1
Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Ácidos e Sais Biliares
/
Técnica de Diluição de Radioisótopos
/
Glucuronídeos
/
Glicina
Limite:
Female
/
Humans
/
Male
Idioma:
En
Revista:
J Pharm Biomed Anal
Ano de publicação:
2019
Tipo de documento:
Article