Study On Manufacturing Technology Of Ellagic Acid From The Wastes Of Processing Tannin Acid In Chinese Gall

Galla Chinensis is the cecidium on the leaves of anacardiaceae plants such as Rhus chinensis Mill,Rhus punjabensis var.sinica Rehd.et Wils,or Rhua potaninii Maxim,which is rich in tannic acid,gallic acid,ellagic acid and so on.The content of tannic acid is up to about60%among them.lt is the main raw material of industrial production through hydrolysis. However,there are10-20%tannic acid remained and a planty of gallic acid and ellagic acid in the rejected material of tannic acid in the production of galla chinensis,the wasting of resources and the environmental pollution is serious. Ellagic acid is a ingredient with anticancer effect and a variety of physiological activities,which has an enormous potential for market growth.lt can be directly extracted and prepared from strawberry, pomegranate and galla chinensis or transformed and synthesized by tannic acid and gallic acid. Based on establishing HPLC method to high-speed and accurate analyse the content of ellagic acid. On one hand,the study works on the preliminary separation and enrichment of the ellagic acid in the rejected material of tannic acid in the production of galla chinensis,and then purified through HSCCC to prepare the high-purity of ellagic acid. On the other hand,discusses the feasibility of transformation from the remained tannic acid and gallic acid in rejected material of tannic acid in the production of galla chinensis to ellagic acid,and optimizes and establishes the transformed technology parameters by qualitative and quantitative analysis of the conversion products, providing a scientific basis for the comprehensive utilization of Galla Chinensis resource and the high performance preparation of ellagic acid.1.Establish a HPLC method to analyze the gallic acid and the ellagic acid in the extracts of galla chinensis quickly and accurately.The research shows that the separation was performed on an Agilent C18column(4.6mm×250mm,5μm).The temperature of the column was35℃.The gallic acid and the ellagic acid were eluted an a flow rate of1.0mL/min,using a mobile phase of acetonitrile and1%glacial acetic acid at248nm with the gradient(Omin-10min:18%acetonitrile,10min-15min:18%-20%acetonitrile).The linear range for the determination of gallic acid was from0.44μm to lmg with a regression coefficient of0.9995and the linear range for the determination of ellagic acid was from0.08to8μm with the same regression coefficient.The average recovery were96.74%and97.10%,the relative standard deviation were0.89%and1.53%. This method can quickly and accurately analyze the content of gallic acid and ellagic acid in the extracts of galla chinensis in15min simultaneously.2. Establish and optimize the method of extracting and preparing the ellagic acid from rejected material of tannic acid in the production of galla chinensis directly.By doing the research of The adsorption and desorption properties of eight macaroporous resins includingD101,NKA-1,AB-8.HPD500,HPD700,S-8,D001and732to the ellagic acid,the results indicated that the macroporous resins732was the best one for the preliminary separating and enrichment of ellagic acid of rejected material.The best operating conditions were found to be:sample loading,0.07mg/mL; sample volume,8BV; sample rate at3.5BV/h;the eluted ethanol,70%;eluted rate at2BV/h;eluted volume,6BV.Under such condition, the yield of ellagic acid was90.27%,and the purity was2.69%.Do further purification by HSCCC,the results indicated that l-butanol-2-propanol-water(3:2:5),use as a two-phase solvent system.The upper phase was used as the stationary phase,while the lower phase as the mobile phase.The separation process were performed at a flow-rate of2mL/min and a revolution speed of800r/min with injection volumn of200mg.Its yield was57.60%and purity was above90%.3.Based on the feasibility of transformation from the remained tannic acid and gallic acid of rejected material of tannic acid in the production of galla chinensis to ellagic acid,the research optimized and established the transformed technology parameters.By doing the transformation of the remained tannic acid and gallic acid in rejected material of tannic acid in the production of galla chinensis and qualitative analysis for the transformed products by HPLC, IR spectrum,MS,NMR and so on.The results indicated the best transformed technology parameter was:regulate the pH of rejected material to10by NaOH,and then inlet the O2for5hours,get the sediment after filtration,than wash the sediment by NaOH of pH10,hang the sediment in the HCL of Ph2.5,and filtrate after stirring for1.5hours,and wash the sediment with10%,20%ethanol and distilled water in order,after freeze-drying, gain the puritied of94.4%gellagic acid0.662g from the1000mL production waste (tannins sour concentration of0.8mg/mL, gallicacid concentration of0.2mg/mL).