<p>Hydroxycitric acid has long been investigated as a phytochemical with an array of beneficial effects on human health. Thus, hydroxycitric acid forms an important component of commercially available herbal formulations and nutraceuticals with tremendous market potential. The development of herbal dietary supplement requires reliable, accurate, and sensitive analytical procedures for detecting and quantitating hydroxycitric acid across diverse biological matrices. Most studies evaluating hydroxycitric acid supplements focus on pharmacokinetic and toxicological analysis. In this article, we discuss a wide range of sample processing and analytical techniques for qualitative and quantitative hydroxycitric acid measurement. The matrices considered include plant extracts, herbal formulations, food samples, target cells and tissues, clinical samples, body fluids, and microbial cultures. Unlike existing reviews that primarily focus on biological and pharmacological aspects of hydroxycitric acid, this review provides a matrix-oriented analytical framework facilitating method selection across diverse sample types. Some emerging analytical considerations in terms of stereospecific detection and stability-constraints are further highlighted, to add a critical perspective. Based on a detailed assessment of the existing methods, this article serves as a guiding compilation for selecting suitable separation and extraction methods for future studies on bioactive hydroxycitric acid and its applications.</p> Graphical Abstract <p></p>