The Reuse Of Waste Liquid From Gardenia Yellow Production

There are lots of effluent from the production of Gardenia Yellow.This effluent containsmany iridoids which are high economic value. Gardenoside is at most among them. It is notonly high value of application,but also the raw material of Genipin and Geniposidic acid.Inorder to fully exploit resources and reduce environmental pollution,this paper studied theextraction technology of Gardenoside from the effluent of Gardenia Yellow production andpreparation technology of Genipin and Geniposidic acid.(The size of all chromatographiccolumns in this study are500mm×30mm)①The extraction technology of Gardenoside from the effluent of Gardenia Yellowproduction: Using HPD700Resin.The pH level of this effluent was5-8.Flow velocity ofloading sample was6mL·min-1.Stop loading sample after the absorbance(238nm) of effluentliquid was about1%of the absorbance(238nm) of sample solution.Using distilled water toelute until the absorbance(238nm) of effluent liquid become zero,then eluted by5%(v/v)ethanol,finally eluted by45%(v/v) ethanol and collected coarse extracting liquid ofGardenoside.This extraction technology is stable,easy to operate and high recovery rate.Tooksamples from coarse extracting liquid to vacuum drying,after that detected by HPLC(highperformance liquid chromatography).The average purity was more than80%.②The preparation technology of Geniposidic acid: Adjusted the content of Gardenosidein the coarse extracting liquid into0.14g·mL-1.The hydrolysis temperature was70℃.Added1mol·L-1sodium hydroxide solution in batches.Measured pH level by acidimeter,controlled itslightly higher than10.The proportion between sodium hydroxide solution and Gardenosidesolution was1:2.The total heating time was140min,then the Gardenoside could behydrolyzed completely. After the solution cooled to room temperature,adjusted the pH levelinto3by1mol·L-1HCl solution.Keep settling stilly overnight,then removed insoluble matterby vacuum filtration and adjusted the pH level of filter liquor into5-7.After decolored byHPD100A resin,eluted it by5%(v/v) ethanol,then combined eluent with decoloredliquid.Absobed them by H103resin, eluted it by30%(v/v) ethanol.Dried the eluent byvacuum drying and finally obtained white crystals of Geniposidic acid by recrystallized inethanol.It’s purity was more than98%.③The preparation technology of Genipin: The size of chromatographic column is500 mm×30mm.The enzyme activity of immobilized enzyme was86U·g-1. Adjusted theconcentration of Gardenoside in the coarse extracting liquid into5%.The pH level of thissolution was5.0.Controlled the temperature of column oven into50℃. Flow velocity ofloading sample was3mL·min-1.Started collecting conversion solution when the effluentliquid was proved to contain Genipin by Arginine color reaction. Adjusted the pH level of thisconversion solution into4-6. Absobed them by HPD750resin and eluted it by10%(v/v)ethanol,then eluted Genipin by anhydrous ethanol. Dried the eluent by vacuum drying,thendissolved Genipin by distilled water and added the same amount of diethyl ether toextract,repeated two times.Dried aqueous phase into paste by rotary evaporator. Recrystallizedby acetone at4℃.Generally,white needle-like Genipin crystal was Formed after3days,it’spurity was more than98%.