Study On UV Irradiation Oxidation, Component Analysis And Preparation Process Of Volatile Oil From Atractylodes Macrocephala Koidz

The volatile oil from Atractylodes macrocephala Koidz (VOA) has exact anti-tumor effect and small adverse reaction, but it is unstable, easily decomposes, thus is difficult to be developed anti-tumor new drug. Therefore, our research group in recent years has been committed to solve the instability of VOA, on the basis of previous work, this paper carried out the following research:1. The optimal oxidative decomposition conditions through UV-lamp irradiation were selected through monitoring content change of atractylon by HPLC, results showed that, the decomposition rate of atractylon in descending order was 254nm,30w; 254nm,8w and 365nm,8w respectively;2. The components in VOA before and after UV-lamp as well as sunlight irradiation were compared by GC-MS technique, to select the optimal irradiation conditions, and clarify the correlation between chemical components in decomposed VOA(DVOA) and anti-tumor effect. Results showed that, after two kind of irradiation oxidation, the overall change trend of components in VOA was consistent, while the disappeared, newly increased and content changed components had differences.With the decreasing percentage of atractylon and y-elemene, the percentages of anti-tumor active components including β-eudesmol, costunolide, isovelleral, atractylenolide Ⅰ and atractylenolide Ⅲ all significantly increased. Moreover, atractylon and y-elemene completely decomposed, and the increased percentages of lactone components were higher after UV-lamp irradation.3. The DVOA/β-CD inclusion complex was prepared by saturated water solution method. The fluorescence method was established for process evaluation, and the optimal inclusion conditions were selected by orthogonal test. Simultaneously, the characterization of inclusion complex was performed through ultraviolet spectra (UV), fluorescence spectra (FL) and microscopic imaging. Results showed that, DVOA and β-CD has formed stable inclusion complex, the optimal inclusion conditions were as follows: the mass ratio of β-CD to DVOA was 6:1, the inclusion temperature was 60 ℃ and the inclusion time was 1.5 h, the average inclusion ratio and oil ratio were 87.87% and 21.13% respectively; GC-MS analysis of components in DVOA before and after inclusion showed that,2 components was not included, the percentages of 5 components increased, the percentages of the rest decreased.4. The DVOA/HP-β-CD inclusion complex was prepared by the freeze drying method. The preparation process was evaluated using fluorescence method, and the optimal inclusion conditions were selected by orthogonal test. Simultaneously, the characterization of inclusion complex was performed through UV-vis, FL and microscopic imaging Results showed that, the optimal conditions of DVOA and HP-β-CD forming stable inclusion complex were as follows:the mass ratio of HP-β-CD to DVOA was 10:1, the inclusion temperature was 30 ℃ and the inclusion time was 2.0 h, the average inclusion ratio and oil ratio were 73.32% and 10.43% respectively; GC-MS analysis of components in DVOA before and after inclusion showed that, the components of DVOA were consistent before and after inclusion, and just the percentage of each component existed differences.5. The thermodynamical properties of DVOA with β-CD and HP-β-CD inclusion complex were studied by fluorescence spectrometry. Results showed that, the molar inclusion ratios of DVOA with β-CD and HP-β-CD were all 1:1, the inclusion stability was HP-β-CD>β-CD; At temperatures of 25 ℃,35 ℃ and 45 ℃, the inclusion constants of DVOA with HP-β-CD were 172,130 and 83 L/mol, the values of △G, AH and AS were all negative, and the AH value was less than the general reaction heat, indicated the inclusion stability of DVOA with HP-β-CD decreased with the rising of temperature; the inclusion could proceed spontaneously along with the releasing of heat, the inclusion process was the results of intermolecular hydrogen bond and Van der Waals force of DVOA molecules with HP-β-CD.6. The dissolution experiment of DVOA/HP-β-CD inclusion complex and their physical mixture were performed with the water as the dissolution media. HPLC technique was used for determination of their dissolution and dissolution rate. Results showed that, compared with physical mixture, the inclusion complex had lowest value of Td (P<0.01), and the dissolution rate was above 96% within 10 min.