Branched-chain amino acids (BCAAs) are among the most widely used ingredients in sports nutrition and dietary supplements, valued for their role in muscle recovery, protein synthesis, and healthy aging. However, the rapid growth of this market has intensified concerns around product quality, authenticity, and accurate labeling. The structural similarity of valine, leucine, and isoleucine leads to strongly overlapping NMR signals, making their individual quantification challenging using conventional analytical approaches. This application note demonstrates how benchtop NMR spectroscopy combined with Advanced Chemical Profiling 2.0 enables automated, reliable quantification of BCAAs in complex supplement formulations. The presented workflow delivers operator-independent results, supports robust quality control, and allows fast verification of both individual BCAA content and their critical ratios from a single measurement.