Standing stocks and carbon isotopes of live benthic foraminifera from the South Atlantic

Live (Rose Bengal stained) and dead benthic foraminifera of surface and subsurface sediments from 25 stations in the eastern South Atlantic Ocean and the Atlantic sector of the Southern Ocean were analyzed to decipher a potential influence of seasonally and spatially varying high primary productivity on the stable carbon isotopic composition of foraminiferal tests. Therefore, stations were chosen so that productivity strongly varied, whereas conservative water mass properties changed only little. To define the stable carbon isotopic composition of dissolved inorganic carbon (d13CDIC) in ambient water masses, we compiled new and previously published d13CDIC data in a section running from Antarctica through Agulhas, Cape and Angola Basins, via the Guinea Abyssal Plain to the Equator. We found that intraspecific d13C variability of all species at a single site is constantly low throughout their distribution within the sediments, i.e. species specific and site dependent mean values calculated from all subbottom depths on average only varied by +/-0.09 per mil. This is important because it makes the stable carbon isotopic signal of species independent of the particular microhabitat of each single specimen measured and thus more constant and reliable than has been previously assumed. So-called vital and/or microhabitat effects were further quantified: (1) d13C values of endobenthic Globobulimina affinis, Fursenkoina mexicana, and Bulimina mexicana consistently are by between -1.5 and -1.0 per mil VPDB more depleted than d13C values of preferentially epibenthic Fontbotia wuellerstorfi, Cibicidoides pachyderma, and Lobatula lobatula. (2) In contrast to the Antarctic Polar Front region, at all stations except one on the African continental slope Fontbotia wuellerstorfi records bottom water d13CDIC values without significant offset, whereas L. lobatula and C. pachyderma values deviate from bottom water values by about -0.4 per mil and -0.6 per mil, respectively. This adds to the growing amount of data on contrasting cibicid d13C values which on the one hand support the original 1:1-calibration of F. wuellerstorfi and bottom water d13CDIC, and on the other hand document severe depletions of taxonomically close relatives such as L. lobatula and C. pachyderma. At one station close to Bouvet Island at the western rim of Agulhas Basin, we interpret the offset of -1.5 per mil between bottom water d13CDIC and d13C values of infaunal living Bulimina aculeata in contrast to about -0.6 +/- 0.1 per mil measured at eight stations close-by, as a direct reflection of locally increased organic matter fluxes and sedimentation rates. Alternatively, we speculate that methane locally released from gas vents and related to hydrothermal venting at the mid-ocean ridge might have caused this strong depletion of 13C in the benthic foraminiferal carbon isotopic composition. Along the African continental margin, offsets between deep infaunal Globobulimina affinis and epibenthic Fontbotia wuellerstorfi as well as between shallow infaunal Uvigerina peregrina and F. wuellerstorfi, d13C values tend to increase with generally increasing organic matter decomposition rates. Although clearly more data are needed, these offsets between species might be used for quantification of biogeochemical paleogradients within the sediment and thus paleocarbon flux estimates. Furthermore, our data suggest that in high-productivity areas where sedimentary carbonate contents are lower than 15 weight %, epibenthic and endobenthic foraminiferal d13C values are strongly influenced by 13C enrichment probably due to carbonate-ion undersaturation, whereas above this sedimentary carbonate threshold endobenthic d13C values reflect depleted pore water d13CDIC values.

Stable oxygen and carbon isotopes ratios of sediment core GeoB9528-3

The carbon isotopic composition of individual plant leaf waxes (a proxy for C3 vs. C4 vegetation) in a marine sediment core collected from beneath the plume of Sahara-derived dust in northwest Africa reveals three periods during the past 192,000 years when the central Sahara/Sahel contained C3 plants (likely trees), indicating substantially wetter conditions than at present. Our data suggest that variability in the strength of Atlantic meridional overturning circulation (AMOC) is a main control on vegetation distribution in central North Africa, and we note expansions of C3 vegetation during the African Humid Period (early Holocene) and within Marine Isotope Stage (MIS) 3 (approx. 50-45 ka) and MIS 5 (approx. 120-110 ka). The wet periods within MIS 3 and 5 coincide with major human migration events out of sub-Saharan Africa. Our results thus suggest that changes in AMOC influenced North African climate and, at times, contributed to amenable conditions in the central Sahara/Sahel, allowing humans to cross this otherwise inhospitable region.

(Table 1) Oxygen and carbon isotopes for foraminiferal taxa at DSDP Hole 76-540

We analyzed the oxygen and carbon isotopic composition of planktonic and benthic foraminifers picked from 13 late Eocene to late Oligocene samples from DSDP Site 540 (23°49.73'N, 84°22.25'W, 2926 m water depth) from the Gulf of Mexico. An enrichment occurs in 18O of about 0.5 to 0.8 per mil in both benthic foraminifers and surface-dwelling planktonic foraminifers between the latest Eocene and early Oligocene. This early Oligocene maximum is followed by lower 18O values. A 1.2 per mil d13C decrease in both benthic and planktonic foraminiferal data occurs from the late Eocene to the late Oligocene. There is a correspondence of the 13C signal to deep-sea records; however, the amplitude of this change is greater than previously seen in deep-sea cores, possibly as a result of proximity to terrestrial sources of carbon. The covarying isotopic changes in both benthic and planktonic foraminifers suggest global causes, such as ice volume increases and increased terrestrial carbon input to the ocean. However, during the latter part of the record (early-late Oligocene), the increases in the benthic 18O without accompanying increases observed with planktonic foraminifers suggest that changes in only one part of the system occurred; one potential explanation being a decrease in bottom-water temperatures without concomitant changes in the surface waters. The 18O differences between species of planktonic foraminifers and the difference between planktonic and benthic 18O data indicate that diagenesis problems are minimal. These preliminary results are encouraging given that these cores are partially lithified.

Alkenone stable carbon isotopes, carbonate stable carbon and oxygen isotopes, planktic foraminifera boron isotopes and atmospheric CO2 calculations and box model results from Ras il-Pellegrin section, Malta

The development of a permanent, stable ice sheet in East Antarctica happened during the middle Miocene, about 14 million years (Myr) ago. The middle Miocene therefore represents one of the distinct phases of rapid change in the transition from the "greenhouse" of the early Eocene to the "icehouse" of the present day. Carbonate carbon isotope records of the period immediately following the main stage of ice sheet development reveal a major perturbation in the carbon system, represented by the positive d13C excursion known as carbon maximum 6 ("M6"), which has traditionally been interpreted as reflecting increased burial of organic matter and atmospheric pCO2 drawdown. More recently, it has been suggested that the d13C excursion records a negative feedback resulting from the reduction of silicate weathering and an increase in atmospheric pCO2. Here we present high-resolution multi-proxy (alkenone carbon and foraminiferal boron isotope) records of atmospheric carbon dioxide and sea surface temperature across CM6. Similar to previously published records spanning this interval, our records document a world of generally low (~300 ppm) atmospheric pCO2 at a time generally accepted to be much warmer than today. Crucially, they also reveal a pCO2 decrease with associated cooling, which demonstrates that the carbon burial hypothesis for CM6 is feasible and could have acted as a positive feedback on global cooling.

Constraints on the upper Permian to upper Triassic marine carbon isotope curve : case studies from the Tethys

Secular variations of the seawater carbon isotopic composition provide evidence for paleoceanographic and paleoclimatic changes and may serve for chemiostratigraphic correlations. The present study aimed to improve the current knowledge on the Upper Permian and Triassic segment of the Phanerozoic marine carbon isotope curve, whose Triassic part was poorly constrained by previous studies. Profiles of inorganic carbon isotopes are provided for sections from Himalaya (Salt Range, Kashmir, Spiti and Nepal), Oman and North Dobrogea (Romania) on the basis of whole-rock carbonate analysis. The data acquired, together with a literature compilation confirmed that most of the Upper Permian is characterized by high δ13C values (averaging +40/00) but failed to detect a positive excursion as suggested by recent compilations. In the light of these observations, the large drop in δ13C values associated with the end-Permian mass extinction appears to be driven by a sudden transfer of previously stocked 13C depleted carbon, rather than by the overturn of a Late Permian stratified ocean. The Triassic data-set outlines significant secular variations. The best documented is a carbon isotope positive excursion just across the Lower-Middle Triassic boundary, globally developed since it was detected in various paleogeographic settings. It is interpreted to reflect variations in surface ocean chemistry, possibly related to increased primary productivity, at times when the biotic recovery after the end-Permian mass-extinction began to accelerate significantly and when a sharp rise in seawater δ34S values occurred globally. Strontium isotope data obtained from well preserved biogenic phosphates allow a refinement of the Middle Triassic segment of the seawater strontium isotope curve and show a major inflexion point of the seawater strontium isotope curve also near the Lower Triassic - Middle Triassic boundary. These facts suggest that the transition from the Early to the Middle Triassic was a time of revolutionary global change which represented an important step in the evolution of Mesozoic marine environments. A tentative carbon isotope curve for the Upper Permian to Upper Triassic time interval is proposed. Its major features are: ? high but constant δ13C values during the Late Permian ? a sharp drop in δ13C values in the latest Permian ? subsequent recovery of δ13C values ? a short-lived positive excursion across the Early-Middle Triassic boundary ? a gradual rise in δ13C values starting in the Late Ladinian or in the Early Carnian It is foreseen that these fluctuations of the carbon isotope curve may serve as chronostratigraphic markers and further assist in the correlation of Permian and Triassic carbonate deposits.

Strontium isotopes and sedimentology of a marine Triassic succession (upper Ladinian) of the westernmost Tethys, Spain

Chemical Stratigraphy, or the study of the variation of chemical elements within sedimentary sequences, has gradually become an experienced tool in the research and correlation of global geologic events. In this paper 87Sr/ 86Sr ratios of the Triassic marine carbonates (Muschelkalk facies) of southeast Iberian Ranges, Iberian Peninsula, are presented and the representative Sr-isotopic curve constructed for the upper Ladinian interval. The studied stratigraphic succession is 102 meters thick, continuous, and well preserved. Previous paleontological data from macro and micro, ammonites, bivalves, foraminifera, conodonts and palynological assemblages, suggest a Fassanian-Longobardian age (Late Ladinian). Although diagenetic minerals are present in small amounts, the elemental data content of bulk carbonate samples, especially Sr contents, show a major variation that probably reflects palaeoenvironmental changes. The 87Sr/86Sr ratios curve shows a rise from 0.707649 near the base of the section to 0.707741 and then declines rapidly to 0.707624, with a final values rise up to 0.70787 in the upper part. The data up to meter 80 in the studied succession is broadly concurrent with 87Sr/86Sr ratios of sequences of similar age and complements these data. Moreover, the sequence stratigraphic framework and its key surfaces, which are difficult to be recognised just based in the facies analysis, are characterised by combining variations of the Ca, Mg, Mn, Sr and CaCO3 contents

Source inference of exogenous gamma-hydroxybutyric acid (GHB) administered to humans by means of carbon isotopic ratio analysis: novel perspectives regarding forensic investigation and intelligence issues.

γ-Hydroxybutyric acid (GHB) is an endogenous short-chain fatty acid popular as a recreational drug due to sedative and euphoric effects, but also often implicated in drug-facilitated sexual assaults owing to disinhibition and amnesic properties. Whilst discrimination between endogenous and exogenous GHB as required in intoxication cases may be achieved by the determination of the carbon isotope content, such information has not yet been exploited to answer source inference questions of forensic investigation and intelligence interests. However, potential isotopic fractionation effects occurring through the whole metabolism of GHB may be a major concern in this regard. Thus, urine specimens from six healthy male volunteers who ingested prescription GHB sodium salt, marketed as Xyrem(®), were analysed by means of gas chromatography/combustion/isotope ratio mass spectrometry to assess this particular topic. A very narrow range of δ(13)C values, spreading from -24.810/00 to -25.060/00, was observed, whilst mean δ(13)C value of Xyrem(®) corresponded to -24.990/00. Since urine samples and prescription drug could not be distinguished by means of statistical analysis, carbon isotopic effects and subsequent influence on δ(13)C values through GHB metabolism as a whole could be ruled out. Thus, a link between GHB as a raw matrix and found in a biological fluid may be established, bringing relevant information regarding source inference evaluation. Therefore, this study supports a diversified scope of exploitation for stable isotopes characterized in biological matrices from investigations on intoxication cases to drug intelligence programmes.

Permian-Triassic of the Tethys: Carbon isotope sudies

Profiles of carbon isotopes were studied in marine limestones of Late Permian and Early Triassic age of the Tethyan region from 20 sections in Yugoslavia, Greece, Turkey, Armenian SSR, Iran, Pakistan, India, Nepal, and China. The Upper Permian sections continue the high positive values of 13C previously found in Upper Permian basins in NW Europe and western USA. In the more complete sections of Tethys it can now be demonstrated that the values of 13C drop from the Murgabian to the Dzhulfian Stages of the Upper Permian, then sharply to values near zero during the last two biozones of the Dorashamian. These levels of 13C sample the Tethys Sea and the world ocean, and equal values from deep-water sediments at Salamis Greece indicate that they apply to the whole water column. We hypothesize that the high values of 13C are a consequence of Late Paleozoic storage of organic carbon, and that the declines represent an episodic cessation of this organic deposition, and partial oxidation of the organic reservoir, extending over a period of several million years. The carbon isotope profile may reflect parallel complexity in the pattern of mass extinction in Late Permian time. Des profils isotopiques du carbone ont été établis dans des calcaires marins d'âge tardi-permien à  éo-triasique répartis dans 20 endroits du domaine téthysien: Yougoslavie, Grèce, Turquie, République d'Arménie, Iran, Pakistan, Inde, Népal et Chine. Les profils établis dans le Permien supérieur montrent les mêmes valeurs positives de 13C observées antérieurement dans des bassins de même âge en Europe occidentale et dans l'ouest des USA. Dans les profils les plus complets de la Téthys, il est maintenant établi que les valeurs de 13C décroissent depuis le Murgabien jusqu'au Dzhulfien (Permien supérieur) pour devenir proches de zéro dans les deux dernières biozones du Dorasharmen. Ces valeurs de 13C sont caractéristiques de la Téthys et de l'Océan mondial; elles s'appliquent à toutes les profondeurs d'eau, comme en témoignent les valeurs fournies par des sédiments de mer profonde à Salamis (Grèce). Nous formulons l'hypothèse que les hautes valeurs de 13C sont la conséquence du stockage du carbone organique au Paléozoïque supérieur et que leur décroissance traduit un arrêt épisodique de cette sédimentation organique, accompagné d'une oxydation partielle de la matière organique s'étendant sur une période de plusieurs Ma. L'influence parallèle des phénomènes d'extinction massive à le fin du Permien se refléterait également dans les profils isotopiques du carbone.

Foraminiferal assemblages and stable isotopes across the early Paleogene carbonate facies of Perth Abyssal Plain off Western Australia

Bulk carbonate content, planktic and benthic foraminiferal assemblages, stable isotope compositions of bulk carbonate and Nuttallides truempyi (benthic foraminifera), and non-carbonate mineralogy were examined across ~30 m of carbonate-rich Paleogene sediment at Deep Sea Drilling Project (DSDP) Site 259, on Perth Abyssal Plain off Western Australia. Carbonate content, mostly reflecting nannofossil abundance, ranges from 3 to 80% and generally exceeds 50% between 35 and 57 mbsf. A clay-rich horizon with a carbonate content of about 37% occurs between 55.17 and 55.37 mbsf. The carbonate-rich interval spans planktic foraminiferal zones P4c to P6b (~57-52 Ma), with the clay-rich horizon near the base of our Zone P5 (upper)-P6b. Throughout the studied interval, benthic species dominate foraminiferal assemblages, with scarce planktic foraminifera usually of poor preservation and limited species diversity. A prominent Benthic Foraminiferal Extinction Event (BFEE) occurs across the clay-rich horizon, with an influx of large Acarinina immediately above. The delta13C records of bulk carbonate and N. truempyi exhibit trends similar to those observed in upper Paleocene-lower Eocene (~57-52 Ma) sediment from other locations. Two successive decreases in bulk carbonate and N. truempyi delta13C of 0.5 and 1.0? characterize the interval at and immediately above the BFEE. Despite major changes in carbonate content, foraminiferal assemblages and carbon isotopes, the mineralogy of the non-carbonate fraction consistently comprises expanding clay, heulandite (zeolite), quartz, feldspar (sodic or calcic), minor mica, and pyrolusite (MnO2). The uniformity of this mineral assemblage suggests that Site 259 received similar non-carbonate sediment before, during and after pelagic carbonate deposition. The carbonate plug at Site 259 probably represents a drop in the CCD from ~57 to 52-51 Ma, as also recognized at other locations.

(Table 1) Stable carbon and oxygen isotopes of planktonic and benthic foraminifera in ODP Hole 1006A

During ODP Leg 166, the recovery of cores from a transect of drill sites across the Bahamas margin from marginal to deep basin environments was an essential requirement for the study of the response of the sedimentary systems to sea-level changes. A detailed biostratigraphy based on planktonic foraminifera was performed on ODP Hole 1006A for an accurate stratigraphic control. The investigated late middle Miocene-early Pliocene sequence spans the interval from about 12.5 Ma (Biozone N12) to approximately 4.5 Ma (Biozone N19). Several bioevents calibrated with the time scale of Berggren et al. (1995a,b) were identified. The ODP Site 1006 benthic oxygen isotope stratigraphy can be correlated to the corresponding deep-water benthic oxygen isotope curve from ODP Site 846 in the Eastern Equatorial Pacific (Shackleton et al., 1995. Proc. ODP Sci. Res. 138, 337-356), which was orbitally tuned for the entire Pliocene into the latest Miocene at 6.0 Ma. The approximate stratigraphic match of the isotopic signals from both records between 4.5 and 6.0 Ma implies that the paleoceanographic signal from the Bahamas is not simply a record of regional variations but, indeed, represents glacio-eustatic fluctuations. The ODP Site 1006 oxygen and carbon isotope record, based on benthic and planktonic foraminifera, was used to define paleoceanographic changes on the margin, which could be tied to lithostratigraphic events on the Bahamas carbonate platform using seismic sequence stratigraphy. The oxygen isotope values show a general cooling trend from the middle to late Miocene, which was interrupted by a significant trend towards warmer sea-surface temperatures (SST) and associated sea-level rise with decreased ice volume during the latest Miocene. This trend reached a maximum coincident with the Miocene/Pliocene boundary. An abrupt cooling in the early Pliocene then followed the warming which continued into the earliest Pliocene. The late Miocene paleoceanographic evolution along the Bahamas margin can be observed in the ODP Site 1006 delta13C values, which support other evidence for the beginning of the closure of the Panama gateway at 8 Ma followed by a reduced intermediate water supply of water from the Pacific into the Caribbean at about 5 Ma. A general correlation of lower sedimentation rates with the major seismic sequence boundaries (SSBs) was observed. Additionally, the SSBs are associated with transitions towards more positive oxygen isotope excursions. This observed correspondence implies that the presence of a SSB, representing a density impedance contrast in the sedimentary sequence, may reflect changes in the character of the deposited sediment during highstands versus those during lowstands. However, not all of the recorded oxygen isotope excursions correspond to SSBs. The absence of a SSB in association with an oxygen isotope excursion indicates that not all oxygen isotope sea-level events impact the carbonate margin to the same extent, or maybe even represent equivalent sea-level fluctuations. Thus, it can be tentatively concluded that SSBs produced on carbonate margins do record sea-level fluctuations but not every sea-level fluctuation is represented by a SSB in the sequence stratigraphic record.

(Table T2) Stable carbon and oxygen isotopes of DSDP Leg 30, Leg 33, ODP Leg 130 and Leg 192 sites, Ontong Java Plateau

Stable isotopic analyses of bulk carbonates recovered from Ontong Java Plateau during Ocean Drilling Program (ODP) Leg 192 (Holes 1183A and 1186A) show an ~0.5 per mil increase in d18O values from the upper Campanian/lower Maastrichtian to the upper Maastrichtian. This shift is consistent with widespread evidence for cooling at this time. Similar shifts were found at other localities on Ontong Java Plateau (Deep Sea Drilling Project [DSDP] Sites 288 and 289 and ODP Site 807) and at DSDP Site 317 on Manihiki Plateau. These data extend evidence for Maastrichtian cooling into the southwestern tropical and subtropical Pacific. The record of apparent cooling survives despite a significant diagenetic overprint at all sites. Comparing average Maastrichtian d18O values among sites suggests that diagenesis caused d18O to first be shifted toward higher values and then back toward lower values as burial depth increased. Carbon isotopes at the six sites show no apparent primary shifts, but at four sites, the Cretaceous/Tertiary boundary interval coincides with a negative excursion attributed to alteration of sediments near the boundary.

Age determination, uranium, carbon and oxygen isotopes ratios of a stalagmite of the Villars cave

The signature of Dansgaard-Oeschger events - millennial-scale abrupt climate oscillations during the last glacial period - is well established in ice cores and marine records (Labeyrie, 2000, doi:10.1126/science.290.5498.1905; Blunier and Brook, 2001, doi:10.1126/science.291.5501.109: Bond et al., 2001, doi:10.1126/science.1065680). But the effects of such events in continental settings are not as clear, and their absolute chronology is uncertain beyond the limit of 14C dating and annual layer counting for marine records and ice cores, respectively. Here we present carbon and oxygen isotope records from a stalagmite collected in southwest France which have been precisely dated using 234U/230Th ratios. We find rapid climate oscillations coincident with the established Dansgaard-Oeschger events between 83,000 and 32,000 years ago in both isotope records. The oxygen isotope signature is similar to a record from Soreq cave, Israel (Bar-Mathews et al., 2000, doi:10.1016/S0009-2541(99)00232-6), and deep-sea records (Bond et al., 1993, doi:10.1038/365143a0; Shackleton and Hall, 2001, doi:10.1029/2000PA000513), indicating the large spatial scale of the climate oscillations. The signal in the carbon isotopes gives evidence of drastic and rapid vegetation changes in western Europe, an important site in human cultural evolution. We also find evidence for a long phase of extremely cold climate in southwest France between 61.2 +/-0.6 and 67.4 0.9 kyr ago.

Isotopes, wool, and rangeland monitoring: Let the sheep do the sampling

Stable carbon isotope analyses of wool staples provided insight into the vegetation consumed by sheep at a temporal resolution not previously studied. Contemporary Australian and historic South African samples dating back to 1916 were analyzed for their stable carbon isotope ratio, a proxy for the proportion of C-3 and C-4 plant species consumed by animals. Sheep sample vegetation continuously throughout a year, and as their wool grows it integrates and stores information about their diet. In subtropical and tropical rangelands the majority of grass species are C-4. Since sheep prefer to graze, and their wool is an isotopic record of their diet, we now have the potential to develop a high resolution index to the availability of grass from a sheep's perspective. Isotopic analyses of wool suggest a new direction for monitoring grazing and for the reconstruction of past vegetation changes, which will make a significant contribution to traditional rangeland ecology and management. It is recommended that isotopic and other analyses of wool be further developed for use in rangeland monitoring programs to provide valuable feedback for land managers.

Dynamics of a paleoecosystem reef associated with oceanic change in carbonate sedimentary regime and carbon cycling (Oxfordian, Swiss Jura)

Herein we report an analysis of an Oxfordian (Upper Jurassic) paleoreef located in the Swiss Jura Mountains. The paleoreef is located in a Middle Oxfordian transitional interval in which sedimentation switched from marl-dominated to carbonate-dominated deposits. The paleoecosystem is composed of four successive fossil communities characterized by microsolenid corals and organisms that specialized in suspension feeding. Carbon isotopes measured from echinoid spine carbonates exhibit a positive trend from similar to 1.0 parts per thousand to 2.5 parts per thousand in delta(13)C values from the base to the top of the paleoreef. Comparison of delta(13)C curves with organic matter and belemnites shows different patterns not compatible with a global variation of the carbon cycle. Similar fossil assemblages and stratigraphic sequences identical in age are found along the continental margin of the Tethys-Atlantic Ocean. This biolithostratigraphic succession corresponds to increasing delta(13)C values of marine and biogenic carbonates, to the transition from marl-dominated to carbonate-dominated deposits, and to the development of carbonate platforms, which together suggest a change in the carbon cycling regime within the Tethys-Atlantic Ocean system.

Carbon isotopic ratio analysis by gas chromatography/combustion/isotope ratio mass spectrometry for the detection of gamma-hydroxybutyric acid (GHB) administration to humans.

Since GHB (gamma-hydroxybutyric acid) is naturally produced in the human body, clinical and forensic toxicologists must be able to discriminate between endogenous levels and a concentration resulting from exposure. To suggest an alternative to the use of interpretative concentration cut-offs, the detection of exogenous GHB in urine specimens was investigated by means of gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). GHB was isolated from urinary matrix by successive purification on Oasis MCX and Bond Elute SAX solid-phase extraction (SPE) cartridges prior to high-performance liquid chromatography (HPLC) fractioning using an Atlantis dC18 column eluted with a mixture of formic acid and methanol. Subsequent intramolecular esterification of GHB leading to the formation of gamma-butyrolactone (GBL) was carried out to avoid introduction of additional carbon atoms for carbon isotopic ratio analysis. A precision of 0.3 per thousand was determined using this IRMS method for samples at GHB concentrations of 10 mg/L. The (13)C/(12)C ratios of GHB in samples of subjects exposed to the drug ranged from -32.1 to -42.1 per thousand, whereas the results obtained for samples containing GHB of endogenous origin at concentration levels less than 10 mg/L were in the range -23.5 to -27.0 per thousand. Therefore, these preliminary results show that a possible discrimination between endogenous and exogenous GHB can be made using carbon isotopic ratio analyses.