Determination of total alkaloids in Alangium sinensis,optimization of extraction process and purification process of macroporous resin
Objective To establish a method for the determination of total alkaloids in Alangium chinese(Lour.)Harms,and to optimize its extraction process and the purification process of macroporous resin.Methods Acid dye colorimetry was used to determine the content of total alkaloids in Alangium sinensis.On the basis of single factor experiment,Box-Behnken design-response surface method was used to optimize the extraction process of total alkaloids from Alangia L.with concentration,volume and time of extraction solvent as factors and total alkaloid content as evaluation indexes.Static adsorption and desorption tests were used to screen 5 kinds of macroporous resins,and the types of macroporous resins were determined based on their adsorption and desorption properties.The static adsorption time,mass concentration of sample liquid and volume of sample liquid were investigated by single factor experiments to optimize the purification process of macroporous resins.Results The content of the acid dye was determined as bromocresol green,the dosage was 5 mL,the pH of disodium hydrogen phosphate and citrate buffer solution was 5.0,and the detection wavelength was 415 nm.The optimized extraction parameters were as follows:the extraction solvent concentration was 80%,the extraction solvent volume was 10 times,and the extraction time was 2.0 h.The optimal macroporous resin purification process was as follows:D101 macroporous adsorption resin was used,the mass concentration of sample liquid was 3.02 mg/mL,the pH of sample liquid was 6,the volume of sample liquid was 45 mL,the flow rate of sample liquid was 1.0 mL/min,the ratio of resin column diameter to height was 1:3,and the purification process was left for 60 minutes.The integral number of ethanol elution liquid was 90%,the elution flow rate was 2 mL/min,and the volume of ethanol elution liquid was 120 mL.Conclusion The method is sensitive and stable.The optimized extraction and purification process is stable and feasible,which provides a basis for clinical application development and industrial production.
Alangium chinesetotal alkaloidscontent determinationextraction processmacroporous resinpurification process