Study On Separation Of Sapindus Saponin And Development Of Sapindus Saponin Shampoo

The dried fruits of sapindus were selected as materials.First of all,the dried fruits of sapindus were extracted with EtOH.The ethanol extracts were purified and concentrated,and the sapindus saponin concentrated were acquired.Next,the sapindus saponin concentrated were separated and purified by macroporous adsorption resin,silica column and preparative HPLC to obtain the relative purity of sapindus saponin reference substance.The purity of sapindus saponin reference substance was determined by HPLC,and the saponin composition structure in sapindus saponin reference substance were inferred by LC-MS.At the same time,sapindus saponin separation and purification technology by foam separation method were studied,and the method of Central-Composite design was used to optimize the technics of the sapindus saponin foam separation.Last,the shampoo formulas of the sapindus saponin with others anioic and auxiliary surfactants were studied,and the method of formula uniform design was used to optimize the formula of the mixture-natural and all-natural of sapindus saponin shampoo.The determine standards of sapindus shampoo were established.1.Sapindus saponin reference substance preparation and the molecular structure analysis by LC-MS1)The purity of sapindus saponin reference substance which prepared by macroporous adsorption resin,silica column and preparative HPLC was 86.96%determined by HPLC.2)The saponin composition of sapindus saponin was detected by LC-MS,6 saponins of Mukurozioside ?b;Pyishiauoside?b;Mukurozioside?b;Mukurozioside I a;Mukurozioside?a and Pyishiauoside?a were indentified.3)The optimal technology conditions for determining the total sapindus saponin by ultraviolet spectophotometry was following:0.4mL 5%vanillin-acetic acid,1.2mL perehloric acid and the sample was mixed and heated 20 min at 70 ? in hot water bath,and then was cooled 5min in ice water bath.last,added in 5mL acetic acid and determined by ultraviolet spectophotometry at the wavelength of UV is 481nm.2.Study on Separation and Purification of Sapindus saponin by foam separation1)The effect of the initial concentration,volume and pH of the sapindus saponin,the gas flow rate and separation temperature on the enrichment ratio,recovery rate and purity of foam separation process was investigated.The results showed that,when the initial concentration of the sapindus saponin was 2.0 g/L,the volume was 150 mL,the gas flow rate was 32 L/h,the temperature was 30 ?and pH value of the solution was 4.3 could the optimal foam separation technology be obtained.2)Through the response surface Central-Composite experimental design,sapindus saponin separation and purification technology use foam separation method and the dynamic relationship between separation parameters(the initial concentration of the sapindus saponin X1,the gas flow rate X2 and the separation temperature X3)and enrichment ratio,recovery rate,purity of process were studied.Relevant regression model was set up:The dynamic equation of enrichment ratio and separation parameter is:Y=2.15-0.52X1-0.084X2+0.041X12-0.13X22-0.23X32+0.27X1X2-0.21X12X2-0.12X12X3+0.11X1X22The dynamic equation of recovery rate and separation parameter is:Y=0.78-8.949E-003X1+0.074X2+0.027X3-0.026X12-4.738E-003X22-0.029X32+9.563E-003X1X2+0.022X1X22The dynamic equation of purity and separation parameter is:Y=0.75-0.04X1-0.011X3-0.014X12-0.024X22-0.023X32-7.112E-003X1X3+0.018X2X3-0.020X1 X2X3Regressed through Design-Expert7.0,the optimal technology conditions for enrichment ratio,recovery rate,purity in process of sapindus saponin foam separation.For enrichment ratio,the best condition were following:the initial concentration of the sapindus saponin was 1.50g/L,the gas flow rate was 28.0 L/h,the temperature was 28?,the volume was 150 mL,and pH value of the solution was 4.3.For recovery rate,the best condition were following:the initial concentration of the sapindus saponin was 2.40g/L,the gas flow rate was 36.0 L/h,the temperature was 25?,the volume was 150 mL,and pH value of the solution was 4.3.And for purity,the best condition were following:the initial concentration of the sapindus saponin was 1.50g/L,the gas flow rate was 32.0 L/h,the temperature was 28?,the volume was 150 mL,and pH value of the solution was 4.3.the relative deviation between actual value and predicted value in 5%under each optimal conditions.3.Study on formulas of Sapindus saponin shampoo1)The shampoo formulas of the sapindus saponin with others anioic surfactants were studied.And the method of formula uniform design was used to optimize the mixture-natural formulas of sapindus saponin shampoo were:12.5%AES,1%6501,2%K12A,2,3%CMEA,3.8%sapindus saponin(s),3.4%CAB,0.156%16-18 alcohol,0.828%CDL-39,1.398%TAB-2,0.756%camellia seed oil,2.502%M550,0.36%HD-203,1.5%pearling agent,a little caisson and essence,some water.The sensory and physiochemical standards of mixture-natural sapindus saponin shampoo from the optimize formulas could up to national institute shampoo standards.2)The sapindus saponin was selected as main materials to develop all-natural sapindus saponin shampoo with others auxiliary surfactants.The method of formula uniform design was used to optimize the all-natural formulas of sapindus saponin shampoo were:10%sapindus saponin(s),5%K12A,1.2%CMC,1.2%CAB,0.24%6501,0.25%TAB-2,0.48%M550,0.25%HD-203,1%pearling agent,a little caisson and essence,some water.The sensory and physiochemical standards of all-natural sapindus saponin shampoo from the optimize formulas could up to national institute shampoo standards.The content of effective materials in all-natural sapindus saponin shampoo wasless compared with mixture-natural sapindus saponin shampoo.It was illustrated that the all-naturalsapindus saponin shampoo could decrease the amount of chemical surfactants which might reduce the environmental issues.3)The content of total sapindus saponin of sapindus saponin shampoo was determined by ultraviolet spectophotometry.Through the precision test,the stabilization and recovery test,we might conclude that this method is reliable,accurate and steady with a good repeatability,and provided a reference for determination of total saponins in sapindus saponin shampoo.the content of total sapindus saponin of mixture-natural and all-natural sapindus saponin shampoo were 21.55mg/g,RSD=1.366%,and 53.67mg/g,RSD=1.256%.The determine standards of sapindus shampoo were established(in the Appendix).