Vinegar plays a multifaceted role in human diet, encompassing nutritive, functional, and taste-enhancing aspects. Quality of vinegar is influenced by quality of raw materials and production methods employed. Spectroscopic techniques offer distinct advantages in terms of speed and environmental friendliness, making them valuable tools for monitoring and controlling food production processes. This study has two major parts. In the first part, traditional and commercial grape vinegar production were monitored using both chemical parameters (total acidity, pH, brix, ethanol etc.) and mid-infrared (mid-IR) and UV-visible (UV-vis) profiles. These measured chemical parameters were predicted from spectral profiles in combination with multivariate statistical analysis techniques. In the second part, mid-IR, UV-vis and fluorescence spectroscopic techniques were used in determination of adulteration of both grape and apple vinegar with acetic acid and spirit vinegar at various ratios. Capability of spectroscopic methods combined with chemometrics were tested for prediction of various chemical parameters of vinegar as well as detection of adulteration of vinegar with different adulterants. Those techniques have proven to be effective in estimating the overall quantities of sugars, phenolics, flavonoids, and organic acids. Utilizing chemometric models with UV–vis and mid-IR data yielded high rates of correct classification, sensitivity, and specificity, particularly for adulteration levels exceeding 5% in vinegar. The performance of mid-IR spectroscopy demonstrated success in detecting the presence of spirit vinegar and acetic acid in apple vinegar. Overall, with this thesis, the usefulness of spectroscopic methods was highlighted by emphasizing the importance of chemometric tools for the parameter prediction and detection of vinegar adulteration