Here, for the first time, we developed Raman spectroscopy in combination with chemometrics for the quantification of adulteration of fresh coconut water by dilution, and its masking with sugars. Coconut water was extracted from young Costa Rican coconuts and heat treated to emulate pasteurization. Samples were then adulterated by dilution with water and single sugars, mixtures of sugars, and high-fructose corn syrup (HFCS). A total of 155 samples were analysed with Raman spectroscopy at 785 nm excitation and 620 spectra analysed with chemometrics. Results showed successful quantification of dilution and adulteration with single sugars between 1.9 – 2.6%, masking of dilution with mixtures of sugars at 9.8%, and masking of dilution with HFCS at 7.1%. It can be concluded that Raman spectroscopy has significant potential as rapid accurate analytical method for the detection of adulteration in this product, with the ability to discern small abnormalities in sugar ratios within coconut water.