Comparison Of The Volatile Oil From Fructus Piperis Longi By SD And SFE-CO₂ And The Study On The Water Solution After Volatile Oil Extraction Refined By Membrane

The modernization process of TCM enable the traditional separation methods to face the challenges and opportunities.The separation system which use the refining of pharmacodynamics material in TCM as the target,is low concentration of raw materials solution,complex components,higher recovery rate.The existing traditional separation technologies use concentration margin as mass transfer impetus to separate the components from the high concentration to low concentration,such as distillation, extraction,crystallization,adsorption and ion exchange,etc.However,these technologies are often difficult to meet the requirements of the separation system. From the modern separation technology research and development trend,we can solve the above issues from the two sides:one is to study the new technology which is suitable for the separation of pharmacodynamics material in TCM,the other is to make use of the existing and newly developed separation technologies for effective combinations,or to joint two or more separation technologies into a more effective separation technology with a view of increasing product selectivity and yield,and achieving the purpose of process optimization.This topic using supercritical CO₂ extraction technology,membrane separation technology,as well as gas chromatography-mass spectrometry technique,and so on, which are more attention in recent years,systematically screened and investigated the optimal extraction and refining process of the volatile oil which is one of major pharmacodynamics ingredients from Fructus Piperis Longi by different extraction methods,analyzed the chemical composition of the volatile oil from Fructus Piperis Longi,etc.The objective was to explore the effectiveness and relevance of extraction and separation for the pharmacodynamics ingredients in TCM with different technologies and their joint application.The main study of this thesis:1.The method of HPLC was used to study the quality control of the single-flavor herbs for Fructus Piperis Longi.The herbs of different sources were collected for the study on the origin and content,so we could ensure the qualified and controlled original ingredients to be used in the experimental study;and we also studied the influencing factors(light,hearting temperature and time,PH,etc.) of Piperine stability in the extract(water extract,alcohol extract) of Fructus Piperis Longi. 2.The comparative studies on the orthogonal test results of two extraction process for the volatile oil from Fructus Piperis Longi by SD and SFE-CO₂ were carried out with orthogonal design L₉(3⁴).SD used the volatile oil extraction rate for indicator,the optimal extraction of which was one hour immersion,adding 6 times amount of water and extracting 7 hours;SFE-CO₂ used the composite score of the volatile oil extraction rate and the transfer rate of Piperine for indicator,the optimal extraction of which was extraction pressure 20MPa,extraction temperature 45℃and extraction time for 20min.3.The technology of GC-MS was used to study the chemical composition and relative content of the volatile oil from Fructus Piperis Longi by SD and SFE-CO₂. The result was that the volatile oil in appearance,yield,chemical composition and relative content were some differences by the two methods.The volatile oil from Fructus Piperis Longi extracted by SD was dark green,clear,transparent liquid,the extract rate was 0.6%,and the volatile oil from Fructus Piperis Longi extracted by SFE-CO₂ was orange,thick,semi-solid oil bar,the extract rate was 4.36%.The methods of TLC and HPLC were used to analysis and determine the Pipeline in the residue from Fructus Piperis Longi after volatile oil extraction,the surplus residue from Fructus Piperis Longi after extracting by SFE-CO₂ enriched the Piperine,the average content of which was 10.37mg/g,it was much higher than which in the surplus residue from Fructus Piperis Longi after extracting by SD.4.The microfiltration technology of ceramic membrane was used to comprehensively study the applicability of membrane structure parameters(membrane material,membrane pore size) to the system which was water solution after volatile oil extraction by SD and the impact of process parameters(operating pressure,liquid flow rate,operating temperature) on the membrane process with the membrane flux and transfer rate of pharmacodynamics ingredients for indicator.The ZrO₂ membrane with the pore size of 0.2μm had the greatest permeation flux and the highest reservation rate of effective components.The appropriate operating conditions were: operating pressure 0.15MPa,liquid flow rate 3m/s,operating temperature 50℃.And we also studied the change trend of material foundation(common nature macromolecule) and physical and chemical parameters(PH,conductivity,viscosity, etc.),which further tested and verified the relevance and effectiveness for this system by the technology.In this dissertation,the significance is as following: (1)The modern technologies which include extraction,separation and detection were used to comprehensively study the pharmacodynamics material from Fructus Piperis Longi.(2)We jointed two or more extraction and separation technologies for the study of effective components in TCM,which provided a basis for the feasibility of the use of new technology in the refining process of Chinese medicine complex system.