Correlation between the synthetic origin of methamphetamine samples and their 15N and 13C stable isotope ratios.

The active ingredient of ecstasy, N-methyl-3,4-methyldioxyphenylisopropylamine (MDMA) can be manufactured by a number of easy routes from simple precursors. We have synthesised 45 samples of MDMA following the five most common routes using N-precursors from 12 different origins and three different precursors for the aromatic moiety. The 13C and 15N contents of both the precursors and the MDMA samples derived therefrom were measured by isotope ratio mass spectrometry coupled to an elemental analyser (EA-IRMS). We show that within-pathway correlation between the 15N content of the precursor and that of the derived MDMA can be strong but that no general pattern of correlation can be defined. Rather, it is evident that the delta15N values of MDMA are strongly influenced by a combination of the delta15N values of the source of nitrogen used, the route by which the MDMA is synthesised, and the experimental conditions employed. Multivariate analysis (PCA) based on the delta15N values of the synthetic MDMA and of the delta15N and delta13C values of the N-precursors leads to good discrimination between the majority of the reaction conditions tested.

Analysis of the 13C natural abundance of CO2 gas from sparkling drinks by gas chromatography/combustion/isotope ratio mass spectrometry.

A simple and rapid method to measure naturally occurring delta(13)C values of headspace CO(2) of sparkling drinks has been set up, using direct injections on a gas chromatograph coupled to an isotope ratio mass spectrometer, through a combustion interface (GC/C/IRMS). We tested the method on CO(2) gas from several origins. No significant isotopic fractionation was observed nor influences by secondary compounds eventually present in the gas phase. Standard deviation for these measurements was found to be <0.1 per thousand.

Characterization of European wine glycerol: stable carbon isotope approach.

Glycerol of about 170 European wines was analyzed using gas chromatography-combustion-isotope ratio mass spectrometry technique. (13)C/(12)C isotopic ratio measurements were performed to characterize glycerol's delta(13)C values of genuine wine samples from European Union wine-producing countries. Glycerol was also successfully dosed using an internal reference, 1,5-pentanediol.

15N isotopic analyses: a powerful tool to establish links between seized 3,4-methylenedioxymethamphetamine (MDMA) tablets.

In this study the (15)N/(14)N isotopic ratios of 43 samples of 3,4-methylenedioxymethamphetamine (MDMA) samples were measured using Gas Chromatography-Combustion-Isotope-Ratio Mass Spectrometry (GC-C-IRMS). The results show a large discrimination between samples with a range of delta(15)N values between -16 and +19 per thousand. Comparison between delta(15)N values and other physical and chemical parameters shows a strong relationship between delta(15)N and brand logo or composition. Thus, it could be assumed that tablets from different seizures probably originated from the same clandestine manufacturing source. Hence, (15)N isotopic parameters provide an important additional tool to establish common origins between seizures of clandestine synthetic drugs.

Impurity profiling of seized MDMA tablets by capillary gas chromatography.

Impurity profiles of 3,4-methylenedioxymethylamphetamine (MDMA) tablets seized in France have been examined. The samples were extracted with methylene chloride under basic conditions and then analyzed by capillary gas chromatography. Almost 30 compounds were identified as precursors, intermediates and by-products. Palmitic and stearic acid were also found as tableting materials. The comparison of the different profiles obtained by the reported procedure provided very useful information about the synthetic processes used by clandestine laboratories and enabled a classification into several groups of profiles. According to these results, the reductive amination route appears to be the most common synthetic pathway in Western Europe. Furthermore, 3,4-methylenedioxyphenyl-2-propanone seems to be the most used precursor in clandestine laboratories.

Rate of carbon dioxide production and energy expenditure in fed and food-deprived adult dogs determined by indirect calorimetry and isotopic methods.

OBJECTIVE: To evaluate energy expenditure (EE) in dogs by estimating rate of CO2 production (rCO2). ANIMALS: 15 Beagles. PROCEDURE: Food was withheld for 24 hours, and all dogs received an IV infusion of 13C sodium bicarbonate for 8 hours. Breath samples were collected before infusion and at 30-minute intervals from 4 to 8 hours, and 13C enrichment in breath CO2 was measured, using gas chromatography-isotopic ratio mass spectrometry. Food was withheld from 6 dogs, and rCO2 and O2 consumption were measured, using a conventional indirect calorimeter. The CO2 production and O2 consumption were measured by use of indirect calorimetry in 6 other fed dogs that were injected with 2H2O and H2(18)O. Blood samples were collected before tracer injection, 4 hours later, and on days 4, 7, and 11. Deuterium and 18O enrichments in plasma water were determined. RESULTS: Mean rCO2 measured by indirect calorimetry was 516 +/- 34 and 410 +/- 16 micromol/kg(0.75)/min in 6 fed and 6 food-deprived dogs, respectively. The rCO2 calculated from 13C-bicarbonate dilution was 482 +/- 30 micromol/kg(0.75)/min. Mean rCO2 determined by use of the double-labeled water method was 1,036 +/- 46 mmol/kg(0.75)/d. Mean energy expenditure calculated from rCO2 determined by infusion of 13C bicarbonate, indirect calorimetry in fed and food-deprived dogs, and infusion of double-labeled water was 386 +/- 39, 379 +/- 25, 338 +/- 14, and 552 +/- 25 kJ/kg(0.75)/d, respectively. CONCLUSIONS AND CLINICAL RELEVANCE: Energy expenditure calculated by indirect calorimetry in unfed dogs can be considered representative of basal metabolic rate.