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Active volatile components in drug pair (DP) Herba Ephedrae-Ramulus Cinnamomi (HE-RC), single drug HE and RC were analyzed by gas chromatography/mass spectrometry (GC/MS), chemometric resolution method (CRM) and overall volume integration. By means of CRM, the two-dimensional data obtained from GC-MS instruments were resolved into a pure chromatogram and a mass spectrum of each chemical compound. In total, 97, 62, and 78 volatile chemical components in volatile oil of HE, RC, and DP HE-RC, were respectively determined qualitatively and quantitatively, accounting for 90.08%, 91.62%, and 89.76% total contents of volatile oil of HE, RC, and DP HE-RC respectively. It is further demonstrated that the numbers of volatile components of DP HE-RC are almost the sum of those of two single drugs, but some relative contents of them are changed. Some new components, such as 1,6-dimethylhepta-1,3,5-triene, tetracyclo[4.2.1.1(2,5).0(9,10)]deca-3,7-diene, globulol and (E,E)-6,10,14-trimethyl-5,9,13-pentadecatrien-2-one are found in DP HE-RC because of chemical reactions and physical changes during decoction.