| The rhizome of Atractylodes macrocephala Koidz is a kind of traditional Chinese medicine with many functions, such as diuresis; diminish inflammatory and fight against senium. Moreover, recent pharmacological studies also found that it had anticancer function. The major purpose of this experiment research is to analyze and separate the volatile oil of Atractylodes macrocephala Koidz, the mechanism and dynamics property of oxidizing reaction of atractylon are also discussed, for the content of atractylon is higher than any other component in volatile oil of Atractylodes macrocephala Koidz, as well as wish to establish foundation for the quality standards system of this Chinese herb. Specifically, the following conclusions can be drawn:1. Volatile oil of Atractylodes macrocephala Koidz is extracted in this work, using supercritical fluid extraction (SFE), steam distillation, refluxing extraction, Soxhlet extraction, ultrasonic extraction and infusion extraction. The content of volatile oil extracted by these methods is analyzed by gas chromatography (GC), the percentage of these oil is calculated with area normalization method. 32 composition were identified by comparing with Nist02 and reference involved, which have 9 extra components than the reference reported.2. Concerns about the extracting technique of atractylone and atractylenolide HI, which is medically used to decrease blood pressure and anticancer. L9 (33) orthogonal test and GC are adopted to determine the content of Atractylone of herb and optimize the extracting process of Atractylone, that is: The ratio of n-hexane to herb is 6: 1 and the vibrating time is 2 h, then extracting in solvent for 22 h at 40℃. L9 (34) orthogonal test and HPLC are used to mensurate the content of atractylenolide HI and the best condition is screened out. That is: The ratio of ethanol (95%) to herb is 10: 1, extracting for 4 h for 2 times.3. Studies the efficiency of extracting and separating of volatile oil of Atractylodes macrocephala Koidz by supercritical fluid extraction technology (SFET) with two methods. They are: (1)adding moderator in extracting process; (2)changingthe critical state of carbon dioxide by adjusting temperature and pressure. Then introduced intensive factor y/, the separating efficiency of extraction is evaluated after the test. The results show: by first method, the y of sesquiterpenes, atractylone and sesquiterpenesolide of each is 3.518, 1.359 and 2.730; by second method, each of that is 3.292, 1.286 and 2.168.4. By using GC/MS, the process of oxidizing reaction of atractylone is traced, and five decomposition products are obtained, which is greatly different from the references-only two decomposition products, and the mechanism of oxidizing reaction of atractylone is investigated. The hypothesized mechanism of reaction is: atractylone is readily to additive react with water and to regenerate the semiacetalhydroxyl at 1, 4-site. The loop of it is opened and lead to the bond of C-0 broken because of the existence of water, thus carbonyl forms. Further, carbonyl is oxidized to regenerate carboxyl. As the carbon atom is sp2 hybridization, carboxyl can be attacked by hydroxyl from both sides of hybrid orbital, in this reaction, water is removed, the remaining atoms are joined to form atractylenolide I and zso-atractylenolide I. While the -H of 7-carbon of atractylenolide I is rather active and liable to be replaced by hydroxyl to form which is unstable and dehydrate within molecule to form atractylenolide II. Moreover, atractylenolideEQ dehydrated with atractylone between two molecules to regenerate a kind of new compound which need to be confirmed further.5. By quantitatively analyzing the percentage of pure atractylone and atractylone in herb, the kinetic parameter was attained, and the equations are: Ratei =￡j [x\M , Rate2 -k2 [xf89; the activation energy of each is SS-OSkJ-mol'1 and 63.17kJ-mor'.6. Based on the results of the mechanism of oxidizing reaction of atractylone, the method of the frying herbs of Atractylodes macrocephala Koidz was advanced: ?It should avoid to heating during extracting atractylone. Considering this, the techniques of atractylone was investigated, combining with homogeneous and orthogonal design, it is showed that infusion extraction can be the best choice; ?For extraction of atractylenolide HI, refluxing method is recommended and heating time should not be too long, thus to avoid atractylenolide HI transform to atractylenolide II bydehydrating reaction.This paper aims to establish the quality standard and to provide the foundation ofquality control of Chinese herb-Atractylodes macrocephala Koidz. Moreover, intents to make foundation theory investigate work for further realizing the innovation of theory and practice of herb's frying, as well as for researching and exploiting the new medicine with our own intellectual property rights. |
PDF Full Text Request