scholarly journals Validation of the doubly labeled water method using off-axis integrated cavity output spectroscopy and isotope ratio mass spectrometry

2018 ◽  
Vol 314 (2) ◽  
pp. E124-E130 ◽  
Author(s):  
Edward L. Melanson ◽  
Tracy Swibas ◽  
Wendy M. Kohrt ◽  
Vicki A. Catenacci ◽  
Seth A. Creasy ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Isotope Ratio ◽  
New Technologies ◽  
Mean Squared Error ◽  
Intraclass Correlation ◽  
Isotope Ratio Mass Spectrometry ◽  
Carbon Dioxide Production ◽  
Urine Samples ◽  
Doubly Labeled Water ◽  
Cavity Output

When the doubly labeled water (DLW) method is used to measure total daily energy expenditure (TDEE), isotope measurements are typically performed using isotope ratio mass spectrometry (IRMS). New technologies, such as off-axis integrated cavity output spectroscopy (OA-ICOS) provide comparable isotopic measurements of standard waters and human urine samples, but the accuracy of carbon dioxide production (V̇co2) determined with OA-ICOS has not been demonstrated. We compared simultaneous measurement V̇co2 obtained using whole-room indirect calorimetry (IC) with DLW-based measurements from IRMS and OA-ICOS. Seventeen subjects (10 female; 22 to 63 yr) were studied for 7 consecutive days in the IC. Subjects consumed a dose of 0.25 g H218O (98% APE) and 0.14 g 2H2O (99.8% APE) per kilogram of total body water, and urine samples were obtained on days 1 and 8 to measure average daily V̇co2 using OA-ICOS and IRMS. V̇co2 was calculated using both the plateau and intercept methods. There were no differences in V̇co2 measured by OA-ICOS or IRMS compared with IC when the plateau method was used. When the intercept method was used, V̇co2 using OA-ICOS did not differ from IC, but V̇co2 measured using IRMS was significantly lower than IC. Accuracy (~1–5%), precision (~8%), intraclass correlation coefficients ( R = 0.87–90), and root mean squared error (30–40 liters/day) of V̇co2 measured by OA-ICOS and IRMS were similar. Both OA-ICOS and IRMS produced measurements of V̇co2 with comparable accuracy and precision compared with IC.

scholarly journals Measurement of δ18O and δ2H of water and ethanol in wine by Off-Axis Integrated Cavity Output Spectroscopy and Isotope Ratio Mass Spectrometry

2021 ◽  
Author(s):  
Xing Wang ◽  
Henk G. Jansen ◽  
Haico Duin ◽  
Harro A. J. Meijer
Keyword(s):  
Mass Spectrometry ◽  
Isotope Ratio ◽  
Isotope Analysis ◽  
Isotope Ratio Mass Spectrometry ◽  
Growth Conditions ◽  
The Other ◽  
H Nmr ◽  
Cavity Output ◽  
Pre Treatment ◽  
Output Laser

AbstractThere are two officially approved methods for stable isotope analysis for wine authentication. One describes δ18O measurements of the wine water using Isotope Ratio Mass Spectrometry (IRMS), and the other one uses Deuterium-Nuclear Magnetic Resonance (2H-NMR) to measure the deuterium of the wine ethanol. Recently, off-axis integrated cavity output (laser) spectroscopy (OA-ICOS) has become an easier alternative to quantify wine water isotopes, thanks to the spectral contaminant identifier (SCI). We utilized an OA-ICOS analyser with SCI to measure the δ18O and δ2H of water in 27 wine samples without any pre-treatment. The OA-ICOS results reveal a wealth of information about the growth conditions of the wines, which shows the advantages to extend the official δ18O wine water method by δ2H that is obtained easily from OA-ICOS. We also performed high-temperature pyrolysis and chromium reduction combined with IRMS measurements to illustrate the “whole wine” isotope ratios. The δ18O results of OA-ICOS and IRMS show non-significant differences, but the δ2H results of both methods differ much more. As the δ2H difference between these two methods is mainly caused by ethanol, we investigated the possibility to deduce deuterium of wine ethanol from this difference. The results present large uncertainties and deviate from the obtained 2H-NMR results. The deviation is caused by the other constituents in the wine, and the uncertainty is due to the limited precision of the SCI-based correction, which need to improve to obtain the 2H values of ethanol as alternative for the 2H-NMR method.

scholarly journals Measurement of δ18O, δ17O, and 17O-excess in Water by Off-Axis Integrated Cavity Output Spectroscopy and Isotope Ratio Mass Spectrometry

2013 ◽  
Vol 85 (21) ◽  
pp. 10392-10398 ◽  
Author(s):  
Elena S. F. Berman ◽  
Naomi E. Levin ◽  
Amaelle Landais ◽  
Shuning Li ◽  
Thomas Owano
Keyword(s):  
Mass Spectrometry ◽  
Isotope Ratio ◽  
Isotope Ratio Mass Spectrometry ◽  
Cavity Output

scholarly journals Detection of Epitestosterone Doping by Isotope Ratio Mass Spectrometry

2002 ◽  
Vol 48 (4) ◽  
pp. 629-636 ◽  
Author(s):  
Rodrigo Aguilera ◽  
Caroline K Hatton ◽  
Don H Catlin
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Isotope Ratio ◽  
Isotope Ratio Mass Spectrometry ◽  
Urine Samples ◽  
Control Group ◽  
Δ13c Values ◽  
Testosterone Administration ◽  
The Mean ◽  
Healthy Males

Abstract Background: Epitestosterone is prohibited by sport authorities because its administration will lower the urinary testosterone/epitestosterone ratio, a marker of testosterone administration. A definitive method for detecting epitestosterone administration is needed. Methods: We developed a gas chromatography-combustion-isotope ratio mass spectrometry method for measuring the δ13C values for urinary epitestosterone. Sample preparation included deconjugation with β-glucuronidase, solid-phase extraction, and semipreparative HPLC. Epitestosterone concentrations were determined by gas chromatography-mass spectrometry for urines obtained from a control group of 456 healthy males. Epitestosterone δ13C values were determined for 43 control urines with epitestosterone concentrations ≥40 μg/L (139 nmol/L) and 10 athletes’ urines with epitestosterone concentrations ≥180 μg/L (624 nmol/L), respectively. Results: The log epitestosterone concentration distribution was gaussian [mean, 3.30; SD, 0.706; geometric mean, 27.0 μg/L (93.6 nmol/L)]. The δ13C values for four synthetic epitestosterones were low (less than or equal to −30.3‰) and differed significantly (P <0.0001). The SDs of between-assay precision studies were low (≤0.73‰). The mean δ13C values for urine samples obtained from 43 healthy males was −23.8‰ (SD, 0.93‰). Nine of 10 athletes’ urine samples with epitestosterone concentrations >180 μg/L (624 nmol/L) had δ13C values within ± 3 SD of the control group. The δ13C value of epitestosterone in one sample was −32.6‰ (z-score, 9.4), suggesting that epitestosterone was administered. In addition, the likelihood of simultaneous testosterone administration was supported by low δ13C values for androsterone and etiocholanolone. Conclusions: Determining δ13C values for urinary epitestosterone is useful for detecting cases of epitestosterone administration because the mean δ13C values for a control group is high (−23.8‰) compared with the δ13C values for synthetic epitestosterones.

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