Development of a Rapid GC-MS Workflow for Simultaneous Quantification of Volatile Terpenes and Cannabinoids in Industrial Hemp Extracts

This study presents the development of a rapid and unified GC-MS workflow capable of simultaneously quantifying volatile terpenes and derivatized cannabinoids in industrial hemp extracts. Traditional analytical approaches typically rely on separate GC-MS and LC-MS methods, increasing operational time, cost, and complexity. The proposed workflow overcomes these limitations by integrating optimized temperature programming, tailored derivatization conditions, and a dual-class calibration strategy that accommodates the distinct physicochemical properties of terpenes and cannabinoids. Method validation demonstrated strong linearity, high accuracy, low detection limits, and robust repeatability across diverse analyte classes. Application to real hemp extracts confirmed the method’s ability to capture compositional variability and provide comprehensive phytochemical profiles relevant for product development, potency verification, and strain differentiation. The workflow also delivers significant throughput gains, reducing total runtime by approximately 40% compared with conventional dual-instrument approaches. Industrial laboratories benefit from simplified sample handling, reduced instrument maintenance, and improved scalability, while regulatory stakeholders gain access to a reliable tool for compliance testing and product labeling. Overall, this GC-MS workflow advances phytochemical analytics by offering an efficient, accurate, and practical solution for high-volume hemp testing and sets the foundation for future innovations involving expanded analyte coverage, automated sample preparation, and cross-validation with LC-MS platforms.