| ObjectiveIn this paper, a process conditions of extraction and purification of epigoitrin (EP) from Radix Isatidis had been studied systematically. Based on this, The process conditions were investigated by magnified test and design of industrial production. The purpose of the present study is to develop a accurate, fast, delicacy methods for analysis and detection of EP, tracking the experimental process, guiding the process parameters optimization and screening, to select the process and parameter conditions for extraction and purification of EP from Radix Isatidis, to illustrate the purification mechanism of EP from extracts Radix Isatidis by epigoitrin-imprinting Chitosan/Attapulgite (EP-ICA), to optimize the process and parameter conditions of magnified test, to obtain process workshop of5tons EP per year.MethodsThe studies were started with choosing the HPLC conditions of EP in extracts and Purification products of Radix Isatidis, The HPLC which suitable for analysis and detection of EP was established. Afterwards, the indexs was determined to screening the EP optimal process conditions of the extraction and purification through combined with the actual things of extracts and purifications quality control in industry. Using the index, various parameters influencing the extraction and purification of EP were studied in batch laboratory-scale experiments. Firstly, the optimal process conditions for the extraction of EP from Radix Isatidis were selected and obtained by orthogonal experimental design. Under this condition, the extracts of EP were gained. Secondly, EP-ICA was used to separate and purify EP from extracts of Radix Isatidis, the optimal process conditions for separation and purification of EP were selected and obtained by single factor experiment design in static/dynamic adsorption/desorption tests. Under this condition, the products of EP was got. Moreover, the separation and purification mechanism of EP from extracts Radix Isatidis were illustrated by adsorption kinetics and thermodynamics experiments. Based on above, the process workshop of5tons EP per year was designed and obtained by pilot-scale magnified test and design of industrial production.Results The C18analytical column was used. The mobile phase of methanol and water(10:90, v/v) was used to analysis EP at the wavelength of245nm, and the velocity of flow was1.0mL/min, the temperature was30℃. the injection volume was10μL. the response rate was0.05AuFs, the theoretical tower plate number are not less than6000. The method had a good linearity from the concentration of3.4-54.4μg/mL with the recovery of101.1%and the RSD of1.63%.The Process route of the extraction and purification of EP from Radix Isatidis in laboratory-scale were as follows:Radix Isatidis—Smash—Extraction—Filter Concentration—Dry—Dissolve—Adjust pH value—EP-ICA adsorption and separation—Concentration—Spray drying.The optimal conditions of extraction of EP from Radix Isatidis in laboratory-scale were as follows:solid to liquid (10%CaO solution) rate was1:20, extraction times was Three times, the extraction solvent was10%CaO solution and extraction time was4.5hours. Under this condition, the average yield of extracts EP was8.84%, the average concentration of EP in extracts EP was3.89%.The optimal conditions of separation and purification of EP from extracts EP by EP-ICA in laboratory-scale were as follows:the initial concentrations of EP in the sample solution was1.05mg/mL, the pH value in the sample solution was5, the adsorption temperature was35℃. For adsorption, the volume and flow rate of feeding samples were3BV and2.0BV/h, respectively. For desorption, EP-loaded resin column was washed by8BV ammonia-ethanol-aqueous solution(5:30:70), the flow rates were4.0BV/h. Under the optimal conditions, the saturated adsorption capacity on EP-ICA was38.72mg/g, the desorption rate was89.97%, the content of resveratrol in the product was90.74,with a recovery yield of83.45%.The adsorption mechanism of EP on EP-ICA were as follows:monolayer adsorption, a spontaneous process, endothermic, the adsorption process was controlled by physical rather than chemical mechanism. The experimental data of adsorption process fitted best to the pseudo-second-order kinetics model and Langmuir isotherm model coupled better correlation coefficients.The Process route of the extraction and purification of EP from Radix Isatidis in pilot-scale magnified test were as follows:Radix Isatidis—Smash—Tank group type dynamic reflux extraction—Filter—Adjust concentration and pH value—EP-ICA adsorption and separation—Concentration—Spray drying. The optimal conditions of extraction of EP from Radix Isatidis in pilot-scale magnified test were as follows:the powder of Radix Isatidis to CaO rate was1:1.5, solid to liquid rate was1:15, extraction time was3.0hours, the extraction of tank unit number was4.Under the optimal conditions and parameters in pilot-scale magnified test, the quantity of Medicinal materials and the diameter of adsorption bed were increased by100 times and10times, respectively.The extraction rate of extracts EP and the EP concentration herein were8.56%and3.77%, respectively. More than80%of laboratory-scale process, It indicated that the extraction process conditions can meet the requirements of the scale-up. The recovery rate of EP and the EP concentration of EP products were83.34%and90.06%, the value were99.25%and98.88%of laboratory-scale process, respectively. It showned that the effect increasing the diameter of adsorption bed is not obvious to products purity and recovery rates of EP. The saturated adsorption capacity on EP-ICA and desorption rate were33.87mg/g and85.86%. More than80%of laboratory-scale process, It prompted that the extraction process conditions can meet the requirements of the scale-up.To obtain process workshop of5tons EP per year. Several contents, such as Process design, material calculation, energy calculation, the main equipment type selection, workshop layout design, Labor organization and post to decide the number,Labor safeguardand safety production,"three wastes" treatment and comprehensive utilization were systematically investigated and designed.ConclusionThe optimal conditions were feasible and reliable, it can meet the requirements of industrialized production. The results suggested that this method could be utilised in large-scale production of EP extraction and purification from Radix Isatidis in industry. |
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