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A rapid continuous‐flow technique for the quantitative determination of hydrogen isotope ratios in organic materials and water, at natural abundance levels, is described. Samples are pyrolysed in a helium stream at 1080°C over an inert form of carbon. Hydrogen is separated from the other pyrolysis gases by gas chromatography and enters the ion source of the isotope ratio mass spectrometer (IRMS) via a crimp. The 2H/1H ratio of the gas was determined by the simultaneous integration of the m/z 2 (1H1H) and m/z 3 (2H‰1H) ion beams over time. δ2H‰ values of organic and water samples were determined by comparison with organic and water standards, respectively. The precision of the on‐line δ2H‰ measurement is <3.3‰. The accuracy of the method was demonstrated by the analysis of a laboratory standard water (NTW), a European Community Bureau Reference material, N,N‐tetramethylurea (TMU) and an International Atomic Energy Association polyethylene reference material (IAEA‐CH‐7). The measured values were NTW ‐39.4‰, TMU ‐144.1‰ and IAEA‐CH‐7 ‐100.7‰ (reference values are NTW ‐38.5‰, TMU ‐147.4‰ and IAEA‐CH‐7 ‐100.3‰). No apparent memory effect was observed when measuring samples at the natural abundance level. Calibration of organic measurements with water reference materials did not give satisfactory results, probably owing to differences in their respective pyrolysis pathways. The potential of the technique for food analysis was demonstrated by measuring the δ2H‰ values of vanillin samples derived from natural and synthetic sources and by the analyses of hexamethylenetetramine synthesized from beet, cane and apple juice sugars. © Crown copyright 1998. Reproduced with the permission of the Controller of Her Majesty’s Stationery Office.

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Isotopic analysis was used to characterize authentic samples of orange juice (Citrus sinensis) from Brazil. Site specific natural isotopic fractionation nuclear magnetic resonance (SNIF-NMR) was used to determine deuterium/hydrogen ratios at the methyl [(D/H)I] and methylene [(D/H)II] sites of ethanol produced by fermentation of orange juice. Stable isotope ratio mass spectrometry (SIRMS) was used to determine the ratio of carbon isotopes (13C/12C) in the same ethanol and the ratio of oxygen isotopes (18O/16O) in the citrus juice water. The mean ratios found for these parameters in authentic hand-squeezed orange juice were as follows:  (D/H)I, 102.3 ppm (SD = 1.7); (D/H)II, 126.5 ppm (SD = 1.8); 13C/12C, δ13C = −26.6‰ PDB (SD = 0.9); and 18O/16O, δ18O = +2.27‰ SMOW (SD = 2.48). Retail samples taken from the Brazilian market place were evaluated by comparison against these data. No evidence was found for the addition of sugar to orange juice or for the dilution with tap water of samples labeled as freshly squeezed. Keywords: Authenticity; orange juice; SNIF-NMR; SIRMS; isotopic analysis; D/H; 13C/12C; 18O/16O