Study On Volatile Oil Components Of Angelica Sinensis Diels And Atractylodes Macrocephala Koidz In Xiaoyao Tablets And Quality Evaluation Of Medicinal Materials

Objevtive:To establish the fingerprint of volatile oil in Xiaoyao Tablets and study the attribution of volatile components in Angelica sinensis and Atractylodes macrocephala.To optimize the extraction process of volatile oil and characterize the extraction status by quantitative indicator and explore process parameters and the regular effect on volatile components.To analyze the volatile components in extracts and Xiaoyao tablets,establish a method for the content of ligustilide.The fingerprints and content methods of Atractylodes macrocephala were established to improve the quality evaluation system of it.Method:1.The essential oil of Angelica sinensis and Atractylodes macrocephala and single-flavor medicine was extracted by steam distillation,the constituents were identified by GC-MS to determine the attribution.The fingerprints of volatile oil were established by GC-MS and the components were identified.2.Based on the index of volatile oil extraction,the extraction process of volatile oil was optimized by factorial experiment design.The extraction temperature was used as a quantitative index to characterize the extraction state.The extraction state,extraction rate,temperature of the solution and the middle of the condenser tube were examined in the temperature range of 120℃-170℃in the oil bath and the volatile components were identified by GC-MS.3.The volatile components in the extracts and Xiaoyao tablets were extracted by reflux extraction and the volatile components were identified by GC-MS.A content method of ligustilide was established to determine the extracts and preparations.4.GC-MS and UPLC fingerprints of Atractylodes macrocephala were established respectively to evaluate the quality of 33 batches of Atractylodes macrocephala in 6 places of origin and to determine Atractylolide III content by UPLC.Results:1.The components were mainly lactones and sesquiterpenoids,which derived from Angelica sinensis were more.37 common peaks were confirmed in fingerprints.The similarity of samples were greater than 0.980.（Z）-ligustilide and3-Butenylphthalide were derived from Angelica sinensis,atractylone from Atractylodes macrocephala,β-Basilene andα-Pinene were both.2.The extraction time and state had significant influence on the extraction of volatile oil.The optimal process was 6 times water,distillation time 6 h,and bump extraction.The extraction state was bumping and the rate reached peak at 160℃.As the temperature increased in the oil bath,the temperature of liquid was around 105°C,the middle of the condenser increased.The components were mainly monoterpenes collected at 120°C and were trans-α-ocalene and（1R）-α-pinene;the lactones and monoterpenes collected at 130°C and above,Z-ligustilide and 3-n-butenylphthalide were the main.The total content reached peak at 160℃,which was the best.3.The volatile components in the extract were Z-ligustilide,4-vinyl-2-methoxy-phenol,3-n-butenylphthalide,atractylone and trans caryophyllene,and were palmitic acid,menthol,Z-ligustilide,4-vinyl-2-methoxy-phenol in Xiaoyao tablets.The content range of ligustilide in the three batches of extracts and preparations was 58.62-68.02μg·g^-1 and 18.12-25.80μg·g^-1,respectively.4.Atractylodes from Zhejiang,Anhui and Hebei Province had higher content,but large differences.The content of Atractylodesin III ranged from 0.133-0.879 mg·g^-1,the highest was from Hunan Provance.It can be the preferred origin in Xiaoyao tablets.Conclusion:1.It provided technical method for quality control of volatile oil to establish GC-MS analysis methods and fingerprints of volatile oil of Angelica and Atractylodes.2.The extraction process conditions optimized was stable and feasible.The extraction temperature had certain influence on the process parameters,volatile oil extraction rate and volatile components.It provided reference and research ideas for guiding the development and utilization of volatile active ingredients of Xiaoyao tablets and other large compound Chinese medicines.3.A method for volatile components and determining ligustilide in extracts and Xiaoyao tablets were established to provide a technical method for comprehensive quality control of volatile oil in Xiaoyao tablets.4.The fingerprints of volatile and full-component and content determination methods of Atractylodes was established.It laid the foundation for the selection of Atractylodes macrocephalae in Xiaoyao tablets and for the improvement of quality evaluation system and subsequent in-depth research of it.