The use of negative ion thermospray liquid chromatography/tandem mass spectrometry for the determination of bile acids and their glycine conjugates

1991 ◽  
Vol 20 (11) ◽  
pp. 731-739 ◽  
Author(s):  
Christine Eckers ◽  
Philip B. East ◽  
Neville J. Haskins
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Bile Acids ◽  
Negative Ion ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

scholarly journals Simultaneous Determination of Flavonoids from Bamboo Leaf Extracts Using Liquid Chromatography-Tandem Mass Spectrometry

2021 ◽  
Author(s):  
Xiabing Li ◽  
Wuqun Tao ◽  
Hang Xun ◽  
Xi Yao ◽  
Jin Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Negative Ion ◽  
Tandem Mass ◽  
Bamboo Species ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractAn analytical method for the simultaneous determination of ten major functional flavonoids (isoorientin, orientin, vitexin, isovitexin, apigenin, luteolin, tricin, quercetin, rutin, and kaempferol) in different bamboo species was developed by liquid chromatography-tandem mass spectrometry. Chromatographic separation was carried out on a reversed-phase C-18 column with acetonitrile and water as the mobile phases. Detection was performed in negative ion electrospray ionization mode using multiple reaction monitoring mode. The correlation coefficients for the calibration curves ranged from 0.9955 to 0.9997. The limit of detection ranged from 1 to 45 ng/ml. The applicability of this analytical approach was confirmed by the successful analysis of real leaf samples of four bamboo species, family Poaceae: Pleioblastus amarus (Keng) Keng f., Phyllostachys glauca McClure, Phyllostachys edullis (Carrière) J.Houz, and Indocalamus latifolius (Keng) McClure. The total flavonoid contents were 3321.09, 3095.96, 4037.33, and 2808.42 mg/kg for P. amarus, P. glauca, P. edullis, and I. latifolius, respectively. Graphical abstract

scholarly journals Simultaneous determination of perfluoroalkyl substances and bile acids in human serum using ultra-high-performance liquid chromatography–tandem mass spectrometry

2019 ◽  
Vol 412 (10) ◽  
pp. 2251-2259 ◽  
Author(s):  
Samira Salihović ◽  
Alex M. Dickens ◽  
Ida Schoultz ◽  
Frida Fart ◽  
Lisanna Sinisalu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Bile Acids ◽  
Ion Source ◽  
Mass Spectrometry Analysis ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractThere is evidence of a positive association between per- and polyfluoroalkyl substances (PFASs) and cholesterol levels in human plasma, which may be due to common reabsorption of PFASs and bile acids (BAs) in the gut. Here we report development and validation of a method that allows simultaneous, quantitative determination of PFASs and BAs in plasma, using 150 μL or 20 μL of sample. The method involves protein precipitation using 96-well plates. The instrumental analysis was performed with ultra-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS), using reverse-phase chromatography, with the ion source operated in negative electrospray mode. The mass spectrometry analysis was carried out using multiple reaction monitoring mode. The method proved to be sensitive, robust, and with sufficient linear range to allow reliable determination of both PFASs and BAs. The method detection limits were between 0.01 and 0.06 ng mL−1 for PFASs and between 0.002 and 0.152 ng mL−1 for BAs, with the exception of glycochenodeoxycholic acid (0.56 ng mL−1). The PFAS measured showed excellent agreement with certified plasma PFAS concentrations in NIST SRM 1957 reference serum. The method was tested on serum samples from 20 healthy individuals. In this proof-of-concept study, we identified significant associations between plasma PFAS and BA levels, which suggests that PFAS may alter the synthesis and/or uptake of BAs.

scholarly journals Simultaneous Determination of Per- and Polyfluoroalkyl Substances and Bile Acids in Human Serum Using Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

2019 ◽  
Author(s):  
Samira Salihovic ◽  
Alex Dickens ◽  
Ida Schoultz ◽  
Frida Fart ◽  
Lisanna Sinisalu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Bile Acids ◽  
Ion Source ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Polyfluoroalkyl Substances

There is evidence of a positive association between per- and polyfluoroalkyl substances (PFAS) and cholesterol levels in human plasma, which may be due to common reabsorption of PFAS and bile acids (BAs) in the gut. Here we report development and validation of a method that allows simultaneous, quantitative determination of PFAS and BAs in plasma, using 150 uL or 20 uL of sample. The method involves protein precipitation using 96-well plates. The instrumental analysis was performed with ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS), using reverse-phase chromatography, with the ion source operated in negative electrospray mode. The mass spectrometry analysis was carried out using multiple reaction monitoring mode. The method proved to be sensitive, robust and with sufficient linear range to allow reliable determination of both PFAS and BAs. The method detection limits were between 0.01 and 0.06 ng⋅mL-1 for PFAS and between 0.002 and 0.152 ng⋅mL-1 for BAs, with the exception of glycochenodeoxycholic acid (0.56 ng⋅mL-1). The PFAS measured showed excellent agreement with certified plasma PFAS concentrations in NIST SRM 1957 reference plasma. The method was tested on serum samples from 20 healthy individuals. In this proof-of-concept study, we identified significant associations between plasma PFAS and BA levels, which suggests that PFAS may alter the synthesis and/or uptake of BAs.

scholarly journals Simultaneous Determination of Per- and Polyfluoroalkyl Substances and Bile Acids in Human Serum Using Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

2019 ◽  
Author(s):  
Samira Salihovic ◽  
Alex Dickens ◽  
Ida Schoultz ◽  
Frida Fart ◽  
Lisanna Sinisalu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Bile Acids ◽  
Ion Source ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Polyfluoroalkyl Substances

There is evidence of a positive association between per- and polyfluoroalkyl substances (PFAS) and cholesterol levels in human plasma, which may be due to common reabsorption of PFAS and bile acids (BAs) in the gut. Here we report development and validation of a method that allows simultaneous, quantitative determination of PFAS and BAs in plasma, using 150 uL or 20 uL of sample. The method involves protein precipitation using 96-well plates. The instrumental analysis was performed with ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS), using reverse-phase chromatography, with the ion source operated in negative electrospray mode. The mass spectrometry analysis was carried out using multiple reaction monitoring mode. The method proved to be sensitive, robust and with sufficient linear range to allow reliable determination of both PFAS and BAs. The method detection limits were between 0.01 and 0.06 ng⋅mL-1 for PFAS and between 0.002 and 0.152 ng⋅mL-1 for BAs, with the exception of glycochenodeoxycholic acid (0.56 ng⋅mL-1). The PFAS measured showed excellent agreement with certified plasma PFAS concentrations in NIST SRM 1957 reference plasma. The method was tested on serum samples from 20 healthy individuals. In this proof-of-concept study, we identified significant associations between plasma PFAS and BA levels, which suggests that PFAS may alter the synthesis and/or uptake of BAs.

Serum bile acids profiling by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and its application on pediatric liver and intestinal diseases

2020 ◽  
Vol 58 (5) ◽  
pp. 787-797 ◽  
Author(s):  
Xiaowei Fu ◽  
Yi Xiao ◽  
Jamie Golden ◽  
Sizhe Niu ◽  
Christopher P. Gayer
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Bile Acids ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
Tandem Mass ◽  
Reaction Monitoring ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractBackgroundA method for bile acid profiling measuring 21 primary and secondary bile acids in serum samples was developed and validated with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Sample preparation included spiking with internal standards followed by protein precipitation, centrifugation, drying under nitrogen gas and reconstitution. Extracted samples were injected onto a Phenomenex Kinetex C18 column (150 × 4.60 mm, 2.6 μm).MethodsData was collected with LC-MS/MS operated in negative ion mode with multiple reaction monitoring (MRM) and single reaction monitoring (SRM). The analytical run time was 12 min.ResultsThe method showed excellent linearity with high regression coefficients (>0.99) over a range of 0.05 and 25 μM for all analytes tested. The method also showed acceptable intra-day and inter-day accuracy and precision. As a proof of concept, the analytical method was applied to patients with neonatal intrahepatic cholestasis caused by citrin deficiency (NICCD), biliary atresia (BA), and necrotizing enterocolitis (NEC), and distinct bile acids profiles were demonstrated.ConclusionsThe method could be poised to identify possible biomarkers for non-invasive early diagnosis of these disorders.

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