Quantitative profiling of prostaglandins as oxidative stress biomarkers in vitro and in vivo by negative ion online solid phase extraction – Liquid chromatography–tandem mass spectrometry

2016 ◽  
Vol 498 ◽  
pp. 68-77 ◽  
Author(s):  
Marieke Teppner ◽  
Manfred Zell ◽  
Christophe Husser ◽  
Beat Ernst ◽  
Axel Pähler
Keyword(s):  
Solid Phase ◽  
Negative Ion ◽  
Oxidative Stress Biomarkers ◽  
Stress Biomarkers ◽  
Chromatography Tandem Mass Spectrometry ◽  
Online Solid Phase Extraction ◽  
Liquid Chromatography Tandem Mass ◽  
Quantitative Profiling

scholarly journals An online solid-phase extraction–liquid chromatography–tandem mass spectrometry method to study the presence of thyronamines in plasma and tissue and their putative conversion from 13C6-thyroxine

2010 ◽  
Vol 206 (3) ◽  
pp. 327-334 ◽  
Author(s):  
M T Ackermans ◽  
L P Klieverik ◽  
P Ringeling ◽  
E Endert ◽  
A Kalsbeek ◽  
...  
Keyword(s):  
Solid Phase ◽  
Thyroid Tissue ◽  
Spectrometry Method ◽  
Tissue Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Online Solid Phase Extraction ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Findings ◽  
Insufficient Sensitivity

Thyronamines are exciting new players at the crossroads of thyroidology and metabolism. Here, we report the development of a method to measure 3-iodothyronamine (T1AM) and thyronamine (T0AM) in plasma and tissue samples. The detection limit of the method was 0.25 nmol/l in plasma and 0.30 pmol/g in tissue both for T1AM and for T0AM. Using this method, we were able to demonstrate T1AM and T0AM in plasma and liver from rats treated with synthetic thyronamines. Although we demonstrated the in vivo conversion of 13C6-thyroxine (13C6-T4) to 13C6-3,5,3′-triiodothyronine, we did not detect 13C6-T1AM in plasma or brain samples of rats treated with 13C6-T4. Surprisingly, our method did not detect any endogenous T1AM or T0AM in plasma from vehicle-treated rats, nor in human plasma or thyroid tissue. Although we are cautious to draw general conclusions from these negative findings and in spite of the fact that insufficient sensitivity of the method related to extractability and stability of T0AM cannot be completely excluded at this point, our findings raise questions on the biosynthetic pathways and concentrations of endogenous T1AM and T0AM.

scholarly journals Bile Acids Quantification by Liquid Chromatography–Tandem Mass Spectrometry: Method Validation, Reference Range, and Interference Study

Diagnostics ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 462 ◽  
Author(s):  
Elisa Danese ◽  
Davide Negrini ◽  
Mairi Pucci ◽  
Simone De Nitto ◽  
Davide Ambrogi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Healthy Subjects ◽  
Reference Range ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Interference Study

Bile acids (BA) play a pivotal role in cholesterol metabolism. Their blood concentration has also been proposed as new prognostic and diagnostic indicator of hepatobiliary, intestinal, and cardiovascular disease. Liquid chromatography tandem mass spectrometry (LC–MS/MS) currently represents the gold standard for analysis of BA profile in biological samples. We report here development and validation of a LC–MS/MS technique for simultaneously quantifying 15 BA species in serum samples. We also established a reference range for adult healthy subjects (n = 130) and performed a preliminary evaluation of in vitro and in vivo interference. The method displayed good linearity, with high regression coefficients (>0.99) over a range of 5 ng/mL (lower limit of quantification, LLOQ) and 5000 ng/mL for all analytes tested. The accuracies were between 85–115%. Both intra- and inter-assay imprecision was <10%. The recoveries ranged between 92–110%. Each of the tested BA species (assessed on three concentrations) were stable for 15 days at room temperature, 4 °C, and −20 °C. The in vitro study did not reveal any interference from triglycerides, bilirubin, or cell-free hemoglobin. The in vivo interference study showed that pools obtained from hyper-cholesterolemic patients and hyper-bilirubinemic patients due to post-hepatic jaundice for benign cholestasis, cholangiocarcinoma and pancreatic head tumors had clearly distinct patterns of BA concentrations compared with a pool obtained from samples of healthy subjects. In conclusion, this study proposes a new suitable candidate method for identification and quantitation of BA in biological samples and provides new insight into a number of variables that should be taken into account when investigating pathophysiological changes of BA in human diseases.

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