A New Era in Dietary Supplement Regulation: Sustainable Chemometric Approach for Quality Control of Four Dietary Ingredients in Slimming Preparations

Abstract

By the end of 2024, the largest reorganization in the modern history of the U.S. FDA took effect. This overhaul included the establishment of the Office of Food Chemical Safety, Dietary Supplements, and Innovation (OFCSDSI), underscoring the growing need for stringent oversight of the dietary supplement (DS) industry. Phenethylamines stimulants are on regulatory monitoring lists, yet they remain available in the DS market. With this reshaping of the regulatory framework of DS, there is an increasing demand for specific and sensitive analytical methods to monitor and control such dietary ingredients. This study introduces chemometrics as a pivotal tool in the enhanced regulatory oversight of DS. Advanced spectrophotometric techniques, coupled with chemometric models, were employed for the simultaneous quantitation of 2-Phenethylamine, caffeine, p-Hordenine, and p Synephrine in complex slimming supplement formulations. Three multivariate models—Partial Least Squares-1 (PLS-1), Genetic Algorithm-Partial Least Squares (GA-PLS), and Genetic Algorithm-Artificial Neural Networks (GA-ANN)—were evaluated. Notably, the GA-based models (GA-ANN) outperformed PLS-1 in resolving spectral overlap without preliminary separation steps, even in the presence of formulation additives. These findings demonstrate the potential of chemometrics as viable eco-friendly alternative for chromatography in routine quality control of DS under the FDA’s new regulatory paradigm.