Abstract: The ether extract of musk, artificially bred musk and original musk reacted with 2,4-dinitrophenylhydrazine to form corresponding phenylhydrazones. The products were determined by HPLC. The conditions of quantitative analysis of muscone hydrazone and qualitative analysis of △⁵-androstene-3β-hydroxy-17-one hydrazone and 3α-hydroxy-5α-androstan-17-one hydrazone, such as the choice of chromatographic columns and mobile phase were studied. The results of standard curve and recovery experiment are satisfactory. Dual detection and MS were used to identify and analyse the purity of the chromatographic peak of muscone hydrazone. Experiments of addition of standards were used to confirm the peaks of △⁵-androstene-3β-hydroxy-17-one hydrazone and 3α-hydroxy-5α-androstan-17-one hydrazone.