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, UUltimo
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 acidsFile | Dimensione | Formato | |
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