A new method for analysing the ingredients of rhynchophylline and isrhynchophylline in Uncaria Rhynchophylla Jacks using hyphenaed high efficiency thin layer chromatographic(TLC) and the surface-enhanced raman spectroscopic(SERS) technics is reported. The results show that the characteristic spectral bands of rhynchophylline can be obtained from the TLC spot with minimum amount of rhynchophylline sample of about 2 5 mm diameter. The difference between the SERS and solid spectra are found. Spectral band at 1 397 cm-1 was obtained wits great enhanced want. Molecule was absorbed in surface silver sol by pair of electrons in —OCH3. Isrhynchophylline sample spectrum band at 1 615 cm-1 obtained the greatest enhance. Isrhynchophylline molecule was absorbed in surface silver sol by pair of electron at N atom in ring indole. An absorption model of rhynchophylline and isrhynchophylline and silver sol is proposed. That effective combination of TLC and SERS can be used to analyse the chemical ingredients with high sensitivity.