Study On The Separation, Extraction And Structural Identification Of The Chemical Composition From Ligusticum Chuanxiong Hort

Chuanxiong is the dry root of Ligusticum chuanxiong Hort. contains a variety ofnatural active ingredients. Phenolic and lactones are the main ingredients in chuanxiongwhich has many pharmacologically activity of sedative, analgesic, protecting thecardiovascular, anti-bacterial, anti-oxidation, anti-radiation, et al. In recent years, studieshave shown that the compounds preparations containing chuanxiong has anti-Parkinsonactivity, therefore, study on the extraction, separation and structural identification of theactive components in chuanxiong has an important significance for the development ofnew drugs and improve the commercial value of chuanxiong.First, application HPLC-ESI-MS/MS technology for rapid separation andcharacterization of chemical constituents in chuanxiong,13structures of the compoundswere determined to β-sitosterol(1), Chuanxingol(2), Palmitic acid(3), SenkyunolideA(4), Z-ligustilide(5), Ferulic acid(6),3-n-Butylphthalide(7), Z′-3,8-dihydro-6,6′7,3′a-diligustilide(8), Wallichilide(9), Levistolide A(10), E-ligustilide(11), SenkyunolideP(12),3′,6,8′,3a-diligustilide(13), respectively. The result provided the basic data forthe study of chuanxiong chemical composition.In the present study, the solvent systems consisted of n-hexane-ethylacetate-methanol-water (4:3:4:2, V/V) for HSCCC was choose, the upper phase wasused as the stationary phase, the lower phase was used as the mobile phase, the flow ratewas1.6mL/min, the separation temperature was30℃, the revolution speed was1400rpm, and the detection wavelength was280nm. Four single compounds were obtainedfrom600mg of n-hexane extract of chuanxiong in one-step separation by HSCCC, thefour single compounds were senkyunolide A (75.8mg), levistolide A (3.5mg),Z-ligustilide (76.3mg) and wallichilide (0.8mg) according to the information of the ionfragmentation by HPLC-MS、ESI-MS/MS. Medium-pressure liquid chromatography was applied to the isolation andpurification of three single compounds from800mg of60%ethanol extract ofchuanxiong within40min in one-step, and acetonitrile-0.5%acetic acid was used as thetwo-phase solvent system, the three single compounds were chuanxingol (2.9mg),senkyunolide A (11.3mg) and Z-ligustilide (20.1mg) according to the information ofthe ion fragmentation by MS and ESI-MS/MS, and the purity of the single compoundswere higher than98%determined by HPLC.