A new FT-IR method combined with multivariate analysis for the classification of vinegars from different raw materials and production processes.

BACKGROUND: Due to the diversity of vinegars on the market and the increase in demand, it is considered necessary to investigate and establish criteria for classifying them in order to obtain more information concerning their real origin. New spectroscopic techniques such us mid-infrared spectroscopy with Fourier transform (FT-IR) are capable of providing information in relation to these aspects. FT-IR combined with multivariate analysis has been used to classify vinegars according to the raw materials and production processes (with or without ageing in wood). Principal component analysis (PCA), partial least-squares discriminant analysis regression (PLS-DA) and stepwise linear discriminant analysis (SLDA) were used. RESULTS: The results obtained have been compared to those achieved using different analytical parameters (polyphenolic content, organic acids and volatile compounds). SLDA and PLS-DA results show the ability of mid-FT-IR spectra to discriminate among vinegars from different raw materials and with or without ageing in wood, with correct classification percentages similar to those obtained using different analytical parameters. CONCLUSION: The discriminative ability combined with other advantages (e.g. rapid and non-destructive analysis, low cost) makes this new FT-IR method a promising tool for the classification and/or differentiation of vinegars.

Traceability of phytosanitary products in the production of a Sherry wine vinegar.

In the present work, the monitoring of the evolution of the different phytosanitary products employed in the production of a Sherry wine vinegar has been carried out. The study covers the complete process, from the grape ripening to the vinegar fermentation. For the liquid sample analysis, a method based on SBSE (stir bar sorptive extraction) coupled to GC-MS and previously developed was used. For the grape samples, the use of two different extraction methods (ultrasound assisted extraction and microwave assisted extraction) was considered. Both methods were correctly optimized by means of factorial designs and were finally compared to each other. Considering the obtained results, the ultrasound extraction method was chosen to make the extraction of the solid samples. After the extraction process, the different extracts were analyzed by means of SBSE-GC-MS. The achieved results show the decrease of the phytosanitary product residues during the grape ripening, most of them being removed completely before the final product.

Solid-phase extraction method for determination of volatile compounds in traditional balsamic vinegar.

A solid-phase extraction method for the determination of volatile compounds in traditional balsamic vinegar (TBV) has been developed. The optimisation has been carried out using a two-level factorial design expanded further to a central composite design. LiChrolut-EN SPE cartridges were used and the optimised analytical conditions were: 7 g of TBV diluted 1:4, 5 mL of washing water, and elution with 10 mL of dichloromethane. The linear ranges and detection and quantitation limits were adequate for the analysis of the studied compounds in TBV. The accuracy of the method was also studied: recoveries up to 80% and repeatability values lower than 15% were obtained for the majority of the studied compounds. Two TBVs of different age were analysed by the optimised method.

Stir bar sorptive extraction of volatile compounds in vinegar: validation study and comparison with solid phase microextraction.

Stir bar sorptive extraction was evaluated for analysing volatiles in vinegar. The procedure developed shows detection and quantitation limits, and linear ranges adequate for analysing this type of compounds. The accuracy obtained was close to 100%, with repeatability values lower than 13%. The extraction efficiency is inversely affected by the acetic acid content. Although the absolute areas decrease, the compound area/internal standard area ratio remains constant, so for quantitative analysis, the acetic acid concentration does not affect the analytical data. The method was compared with a previous SPME method. Similar performance characteristics were obtained for both methodologies, with lower detection and quantitation limits and better repeatability reproducibility values for SBSE. Both analytical methods were used to analyse a variety of vinegars. The results obtained from both methods were in agreement.

Optimization of stir bar sorptive extraction applied to the determination of pesticides in vinegars.

Stir bar sorptive extraction (SBSE) has been evaluated for analysing pesticides in vinegar. The extraction analytical conditions have been optimised using a two-level factorial design expanded further to a central composite design. After optimization, the proposed analytical conditions are: sample volume 40 mL, sampling time 150 min, and stirring speed 1000 rpm. On the basis of the results, it was decided not to add NaCl. The SBSE procedure developed shows detection limits and linear ranges adequate for analysing this type of compound, giving recoveries close to 100%. The repeatability and reproducibility values obtained were lower than 18 and 23%, respectively. The method was applied to a variety of commercial vinegars. SBSE is a very simple, solvent-free, and fast technique with high sensitivities.