Study On Clean Production Process Of Zinc Glycyrrhizinate

Glycyrrhizoma glycyrrhizae,as a traditional Chinese medicine,contains many active ingredients in its roots and rhizome,of which glycyrrhizic acid（GA）is one.GA has been applied in medicine,food,cosmetics and other fields due to its various pharmacological effects such as anti-inflammatory,antibacterial,antiviral,anti-tumor and anti-aids.Its derivatives glycyrrhizic acid zinc,can play a role of GA in the pharmacological,also can be used as agents,zinc supplementation of trace element supplement the human body,enhancing the using rate of GA and added value.Traditional method to extract GA or may cause pollution to the environment,the energy consumption is larger,some resources based on licorice root as a raw material,adopts the weak acid solvent to extraction of GA both to avoid the environmental pollution and resource waste,and won the high purity of GA crude products,reduce the burden of the subsequent GA purification.GA extract after membrane in removing impurity concentration,decolorization,further purification with ethanol extraction of GA.Due to the complex traditional preparation process of zinc glycyrrhizate and the low purity of zinc glycyrrhizate,the preparation process of zinc glycyrrhizate was improved and the preparation conditions were explored.The main conclusions are as follows:（1）Establish HPLC detection of glycyrrhizic acid conditions:the Acclaim^TM 120C₁₈ chromatographic column（4.6 mm×250 mm）,in the mobile phase of acetonitrile-glacial acetic acid and water（38:1:61）,the flow rate of 1.0 mL/min,detection wavelength of 254 nm,column temperature 30℃,sample quantity20μL under the conditions of determination of glycyrrhizic acid in glycyrrhiza content is 2.67%.（2）Screening and exploring the extraction method of GA;Compared to water,dilute ammonia water,ammonia and ethanol and weakly acidic solvent fagan extraction yield of oxalic acid and GA crude product purity,screening of GA extraction method.The single factor test was used to analyze the effects of material-liquid ratio,time,pH,temperature and times on the extraction rate of GA.The extraction parameters were optimized according to the response surface analysis.The optimal extraction parameters were:The ratio of liquid to 1:9 mL/g,time 1.5h,pH5.5,3 times,extraction rate:82.50%,crude GA purity is 29.32%,this method reduces the pressure of subsequent purification of GA and energy consumption small,no pollution to the environment.（3）Explore glycyrrhizic acid zinc synthesis condition,to determine 95%ethanol extraction of GA crude product is:the condition of 1:20,material liquid ratio,extraction time 2 h,extracting 3 times,GA extraction yield of 96.85%.According to the single factor analysis and orthogonal test to determine glycyrrhizic acid zinc precipitation conditions for the optimal:pH 5.5,zinc acetate was 2.3 mL,stirring time is 2.5 h,the reaction temperature is 70℃.Various factors influence size order:>reaction temperature>pH>stir time zinc acetate content.The precipitation rate of zinc glycyrrhizinate was 97.62%and the purity of glycyrrhizic acid was 90.37%.