Abstract: In this study, in order to determine chemical constituents of a traditional Chinese medicinal formula (TCMF) and identify their changes during the production process, both volatile and water-soluble components were detected for Yupingfeng (YPF) powder and its composed herbs of Radix Astragali (RA), Rhizoma Atractylodis Macrocephalae (RAM), and Radix Saposhnikoviae (RS). In the first part of the research, gas chromatography-mass spectrometry (GC-MS) was employed to analyze volatile components. Some chemometric resolution techniques were then investigated to treat the two-dimensional data produced. The results showed that 116, 12, 80, and 68 constituents were separated; 61, 11, 32, and 44 of them tentatively identified, which accounted for about 77.31%, 97.71%, 79.28%, and 86.01% of the total relative contents of essential oils from Received 22 October 2008; accepted 3 August 2009. This research work was financially supported by the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry of China. Address correspondence to Fan Gong, Department of Plant Science, Rothamsted Research, Harpenden, Hertfordshire, United Kingdom, AL5 2JQ. E-mail: fan.gong@bbsrc.ac.uk