Potential of ion chromatography coupled to isotope ratio mass spectrometry via a liquid interface for beverages authentication.

New tools for the determination of characteristic parameters for food authentication are requested to prevent food adulteration from which health concerns, unfair competition could follow. A new coupling in the area of compound-specific carbon 13 isotope ratio (δ(13)C) analysis was developed to simultaneously quantify δ(13)C values of sugars and organic acids. The coupling of ion chromatography (IC) together with isotope ratio mass spectrometry (IRMS) can be achieved using a liquid interface allowing a chemical oxidation (co) of organic matter. Synthetic solutions containing 1 polyol (glycerol), 3 carbohydrates (sucrose, glucose and fructose) and 12 organic acids (gluconic, lactic, malic, tartaric, oxalic, fumaric, citric and isocitric) were used to optimize chromatographic conditions (concentration gradient and 3 types of column) and the studied isotopic range (-32.28 to -10.65‰) corresponds to the values found in food products. Optimum chromatographic conditions are found using an IonPac AS15, an elution flow rate of 0.3mLmin(-1) and a linear concentration gradient from 2 to 76mM (rate 21mMmin(-1)). Comparison between δ(13)C value individually obtained for each compound with the coupling IRMS and elemental analyzer, EA-IRMS, and the ones measured on the mixture of compounds by IC-co-IRMS does not reveal any isotope fractionation. Thus, under these experimental conditions, IC-co-IRMS results are accurate and reproducible. This new coupling was tested on two food matrices, an orange juice and a sweet wine. Some optimization is necessary as the concentration range between sugars and organic acids is too large: an increase in the filament intensity of the IRMS is necessary to simultaneously detect the two compound families. These first attempts confirm the good results obtained on synthetic solutions and the strong potential of the coupling IC-co-IRMS in food authentication area.

The full evaporation technique: a promising alternative for residual solvents analysis in solid samples.

The static headspace technique is the most common approach to residual solvent analysis in pharmaceutical and environmental matrices. This paper presents an alternative tool where the volatile impurities are released from the matrix by working directly on a small amount of sample at a high equilibration temperature: the so-called Full Evaporation Technique (FET). The capability of this method was evaluated on a mixture of nine solvents, which belong to Class 3 in the classification of the European Pharmacopoeia Agency for residual solvents, at various levels of concentration: ethanol, acetone, 2-propanol, methyl acetate, 2-butanone, ethyl acetate, tetrahydrofuran, 2-methyl-1-propanol, 1-butanol. Data on linearity, accuracy, precision and sensitivity are reported. Use of an internal standard proved to be necessary when using such a method. The method is then successfully applied to the analysis of solvent traces in permethylated beta-cyclodextrin.