Study On The Preparation And Quality Standard Of Ultramicro Guipi Pills

Objective:Apply the technology of superfine comminution SFE-CO2 to the preparation of Guipi pills. Establish a reasonable and reliable route for the process and a feasible detective method for the quality standards.Method:(1)Use the volatile oil extraction rate as the primary screening indexes, optimize the extraction procedure for the volatile oil in Radix Aucklandiae and Rhizomo Atractylodis Macrocephalae by orthogonal design.(2)Use the package rate of volatile oil as the primary screening indexes, optimize the preparation ofβ-Cyclodextrin inclusion compound of volatile components.(3)Use TLC. GC/MS、DSC、XRD and so on to verify the formation of inclusion compound.(4)Use the extract rate of ferulic acid and the extract yield as the primary screening indexes, optimize the extraction procedure in ultramicro guipi pill by orthogonal design.(5)Use the sulfuric acid-phenol method and UV to determine the diameter of Poris cocos powder.(6)Identify Poria cocos wolf, Radix Aucklandiae, Radixet Rhizoma Glycyrrhizae and Radix Polygalae by TLC.(7)Establish the method to determine Astragaloside IV in the ultramicro Guipi Pills by HPLC-ELSD. Establish the method to determine Ferulic Acid in the ultramicro Guipi Pills by HPLC.(8)Eastablish the fingerprints of ultramicro Guipi pills by HPLC.Result:(1)The best extraction process for volatile components of Radix Aucklandiae and Rhizomo Atractylodis Macrocephalae as follows:use the supercritical CO2 extraction, the diameter of the crushing herbs fixed at 20 degrees, the pressure of extraction fixed at 30MPa, the temperature of extraction fixed at 50℃, the flow rate of CO2 fixed at 25 kg.h-1, extract for 2h.The effect of temperature on the volatile oil extraction rate by the supercritical CO2 extraction was significant.(2)The best technology for the preparation ofβ-Cyclodextrin inclusion compound as follows:grinding, the ratio of the volatile components andβ-Cyclodextrin was 1:10, add 3 times amount of water, grind for 3h. The inclusion time is a significant effect on the package rate of volatile oil.(3)Analyze volatile oil,the mixture of volatile oil andβ-Cyclodextrin inclusion compound by TCL、GC/MS、DSC、XRD to verify that there is no change between volatile oil and the mixture of volatile oil but the physical characterization among all three are obvious different.(4)The best extraction process by water as follows:10 times the volume of water,55℃dynamically extract for 1.5h, centrifuge,filter,filter residue add 8 times the amount of water,55℃dynamically extract for 1.0h.The time of extraction is significant for the extract rate of ferulic acid and the extract yield.(5)Directly use Poris cocos powder which diameter is 300degree.(6)Use TLC to identify the four kinds of herbs in ultramicro Guipi Pills.The fleck is limpid, blank space has no a disturbance.(7)Use HPLC-ELSD to determine the content of astragaloside in ultramicro Guipi Pills and carrying out a study on methodology, the recovery rate for astragaloside was 102.71%, RSD was 2.74%.Use HPLC to determine the content of ferulic Acid in ultramicro Guipi Pills and carrying out a study on methodology, the recovery rate for astragaloside was 98.05%, RSD was 1.06%.(8)Eastablish the fingerprints of ultramicro Guipi pills by HPLCConclusion:This is the first time to apply the technology of superfine comminution. SFE-CO2 andβ-Cyclodextrin inclusion to the preparation of Guipi pills. Establish a reasonable and reliable route for the process and a feasible detective method for the quality standards.The content of the active ingredient is high so the dose can be reduced and the resources of Chinese herbal medicine can be saved and the cost of the production can be lowered. Based on the above conclusions, the preparation of ultramicro Guipi pills are successful.It is a beneficial attempt for the development of a preparation of traditional Chinese medicine which is smaller dose, easily transport and administration.