A new direct extraction by gas-chromatography with flame ionization detector coupled to head space method for the determination of alcohol content of high matrix wine products

Abstract

Detection, identification, and quantitation of alcohol in any matrix rich medium is a common practice although sample preparation is inevitable and time consuming. A sensitive, precise and ultimately wide range method for detection, identification and quantification of main content/residual/impurity alcohols without any matrix interference that can be used for production phase quality control, pharmaceutical and/or bio-technological refinement or toxicological evaluation and for forensics is always needed. Even for quality control also for toxicological considerations, ethanol (EtOH) and very similar compound methanol has to be detected and identified definitely becomes vital. However, with the fermented products, the matrix becomes a challenging process, makes the methods inefficient or more extraction methods have to be implanted. Here we propose a new simple and reliable direct extraction method has been developed for the determination of alcohol content of high matrix wine products using the gas-chromatography with flame ionization detector coupled to head space. The method was developed with a rich and complex component mixture of fermented alcoholic beverages (wine) with very high matrix effects. Isopropanol (IPA) was preferred as an internal standard, and Triton X-100 (TX-100) was used as diluting solution in this method. The amount of TX-100, extraction temperature, and the total volume of solution in head space vial (20 mL) were optimized. 2.5% TX-100, 80 °C extraction temperature, and 2.0 ml of total volume were used as optimum condition. Stationary phase was the fused silica, Agilent J&W DB-624 column (30 m x 320 m x 1.8 m) and Helium was used as a mobile phase. GC oven temperature programme was 40C (5 min), 5C/min ramp to 60C (0 min) and 30C/min to 150C (1 min). Performance of the method was assessed by evaluating the recovery, accuracy, precision, linearity, limits of detection (LOD) and limit of quantification (LOQ). Calibration curve was drawn between the concentration of 2.5% to 15.0% EtOH (y = 1.572x – 0.702, R² = 0.9960, y; the ratio of peak area of EtOH to IPA, x: EtOH%). The slopes of standard addition and external calibration curve were statistically same. Recovery of the method was 97.5 ± 3.5 for tree different concentrations and the precision was %5.8 (n= 11). LOD and LOQ were calculated as 0.80% and 2.5%, respectively. The proposed method has a potential for application into the industry and academia with determination of the alcohol content/residual/impurity and also check the quality and content of the fermented medium without the effect of matrix.