Abstract: From a Chinese herb Fu Mao Tie Bang Ghui, the root of Aconitum flavum Hand-Mazz, collected from Ning Xia Autonomous Region, two alkaloids Ⅰ and Ⅱ have been isolated. On the basis of spectroscopic analyses and chemical methods, Ⅰ and Ⅱ were identified as 3-acetylaconitine and aconitine respectively.3-acetylaconitine, C₃₆ H₄₉ O₁₂ N, mp. 196-197℃, α_D²⁴+18.6° (C. 1.0, CHCl₃) was discovered in nature for the first time.