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

Ulaszewska, M.; Mancini, A.; Garcia-Aloy, M.; Del Bubba, M.; Tuohy, K.; Vrhovsek, U. (2019). Isotopic dilution method for bile acid profiling reveals new sulfateglycine-conjugated dihydroxy bile acids and glucuronide bileacids in serum. JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 173: 1-17. doi: 10.1016/j.jpba.2019.05.002 handle: http://hdl.handle.net/10449/54467

Isotopic dilution method for bile acid profiling reveals new sulfateglycine-conjugated dihydroxy bile acids and glucuronide bileacids in serum

Ulaszewska, M.
Primo
;
Mancini, A.;Garcia-Aloy, M.;Tuohy, K.;Vrhovsek, U
Ultimo
2019-01-01

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
Bile acids
Profiling
Postprandial kinetics
Metabotypes
Triple Quad
Orbitrap
Settore CHIM/10 - CHIMICA DEGLI ALIMENTI
2019
Ulaszewska, M.; Mancini, A.; Garcia-Aloy, M.; Del Bubba, M.; Tuohy, K.; Vrhovsek, U. (2019). Isotopic dilution method for bile acid profiling reveals new sulfateglycine-conjugated dihydroxy bile acids and glucuronide bileacids in serum. JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 173: 1-17. doi: 10.1016/j.jpba.2019.05.002 handle: http://hdl.handle.net/10449/54467
File in questo prodotto:
File Dimensione Formato  
2019 Marynka.pdf

accesso aperto

Tipologia: Versione editoriale (Publisher’s layout)
Licenza: Creative commons
Dimensione 4.52 MB
Formato Adobe PDF
4.52 MB Adobe PDF Visualizza/Apri

I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/10449/54467
Citazioni
  • ???jsp.display-item.citation.pmc??? 4
  • Scopus 17
  • ???jsp.display-item.citation.isi??? 14
social impact