Food fraud and adulteration is a major concern in terms of economic and public health. Multivariate methods combined with spectroscopic techniques have shown promise as a novel analytical strategy for addressing issues related to food fraud that cannot be solved by the analysis of one variable, particularly in complex matrices such distilled beverages. This review describes and discusses different aspects of whisky production, and recent developments of laboratory, in field and high throughput analysis. In particular, recent applications detailing the use of vibrational spectroscopy techniques combined with data analytical methods used to not only distinguish between brand and origin of whisky but to also detect adulteration are presented.