Liquid‐Liquid Extraction‐assisted Reversed‐Phase Preparation Solution Recovery Enhances the Recovery Rate and Stability of Volatile Components

ABSTRACT

Natural volatile components (VCs) are extensively applied in medicine, food, and daily chemicals. Characterizing their chemical compositions is essential for fundamental research. Reversed‐phase preparative chromatography is among the most widely used and efficient separation approaches. Nevertheless, the poor thermal stability and steam‐volatile nature of VCs pose substantial challenges for laboratory‐scale preparation and recovery. To address this problem, we report a laboratory‐grade liquid–liquid extraction‐assisted reversed‐phase preparative solution recovery (LERPSR) method designed to enhance the recovery efficiency and stability of VCs during reversed‐phase chromatography. Cost‐effective solvents were screened based on phase separation and miscibility. Ten VCs representing four categories were selected to evaluate the universality of LERPSR, while zedoary turmeric oil was used to validate its feasibility in complex matrices. The mechanism was investigated using computational chemistry. Results demonstrated that n ‐hexane outperformed isooctane. Compared with the direct vacuum recovery method, the LERPSR method with n ‐hexane improved the recovery of all 10 VCs, with seven showing statistical significance ( p  < 0.05). The recovery weight of characteristic components significantly increased in zedoary turmeric oil, exhibiting enhanced stability. Computational results aligned with experimental findings. Thus, LERPSR effectively improves the recovery and stability of VCs, offering a promising laboratory‐grade approach for preparation, quality control, and identification of VCs.