Different geographical regions of traditional Chinese medicine (TCM), its chemical composition is different, the accumulation of drug and medicinal properties is different. The accurate identification and analysis of different production area of medicinal herbs is critical for the quality control and pharmacological research of TCM. In this paper, a tri-step infrared spectroscopy (Fourier transform infrared spectroscopy (FTIR) combined with second derivative spectra and two-dimensional correlation infrared spectroscopy (2D-COS) were employed to identify and analyze the main components of Hubei(HB), Anhui(AH), Yunnan(YN) genuine Poria Cocos peels. The emergence of several characteristic absorption peaks of carbohydrates including 1　149, 1　079 1　036 cm-1, peaks around 1　619, 1　315, 780 cm-1 belonged to calcium oxalate suggested that HB and AH Poria Cocos peels contained calcium oxalate, but peaks around 797, 779, 537, 470 cm-1 belonged to kaoline suggested that YN Poria Cocos peels contained kaoline. Their carbohydrates were different by comparing the second derivative infrared spectra in the range of 1　640～450 cm-1 and Yongping come from YN contains both calcium oxalate and kaoline. Furthermore, the above differences were visually validated by two-dimensional correlation spectroscopy (2D-COS). It was demonstrated that the Tri-step infrared spectroscopy were successfully applied to fast analyze and identify Poria Cocos peels from different geographical regions and subsequently would be applicable to explain the relevance of geographical regions and medicinal properties for the TCM.