| Phenolic acid of Ligusticum chuanxiong(PALC)has strong inhibition of tyrosinase activity and antioxidant function,mainly composed of ferulic acid.Ferulic acid has been added to many cosmetics as a whitening agent with definite activity.However,it was unstable and easy degradation affected by light,temperature,pH value and so on,the paste was deteriorated.Therefore,PALC was encapsulated in internal water phase and prepared into water-in-oil-in-water(W/O/W)multiple emulsions through the preparation method,so as to isolate air and light and enhance the stability.This study mainly includes the following contents:Extraction quantity of three kinds of phenolic acids and total phenolic acids were taken as indexes,single factor test-orthogonal design was adopted to determine the optimal extraction process: the coarsest powder of chuanxiong was taken,8 times the amount of 70% ethanol was added,reflux extraction 2 times and 2 h for each time.filtration was conducted,filtrate was incorporated and concentrated to 0.5 g/mL(in terms of crude drugs).Elution rate of three kinds of phenolic acids was taken as index,single factor test was used,the optimum purification conditions were as follows: resin type of HPD100,sample solution concentration was 0.5 g /ml(in terms of crude drugs),adsorption rate of 2 BV/h,sample volume of 2 BV,diameter height ratio of 1:7,3 BV pure water elution was used for impurity removal,and then 5 BV 50% ethanol at a rate of 2 BV/h was used for purification.The eluate was collected and concentrated to 0.25 g/mL(in terms of crude drugs).Elution rate of three kinds of phenolic acids was taken as index was taken as indexes.single factor test was used,The optimum decolorization conditions were as follows: resin type D941,sample solution concentration was 0.25 g /ml(in terms of crude drugs),adsorption rate of 2 BV/h,sample volume of 8 BV,diameter height ratio of 1:7,10 BV 60% ethanol(containing 1.5 moL/L NaCL)at a rate of 2 BV/h was used for purification,The eluate was collected,concentrated and dried as solid.The content of three kinds of phenolic acid was taken as indexes.single factor test was used to determine the optimal extraction process: 8 times the amount of ethanol was added,reflux extraction 4 times and 1 h for each time.The content of three kinds of phenolic acid and the state of extract after dried were taken as indexes,different concentration temperatures and drying methods were investigated,finally the concentration temperature was 60℃,drying method was decompression drying(50℃).Water,heavy metal and resin residues were detected according to the relevant provisions of the Chinese pharmacopoeia(2015 edition),the water content was initially determined to be less than 4.2 %,heavy metals less than 10 ppm,there should be no resin residue.The TLC identification method and the content determination method were established,the chromatographic maps of the tested and control samples showed the same color spots.Content determination(HPLC method)was calculated accordingto the dry product,chlorogenic acid,caffeic acid,ferulic acid,three kinds of phenolic acid was contained 1.25%,0.12%,13.75%,15.12% respectively,total phenolic acid(UV method)was calculated accordingto the dry product was contained 53.63%.The inhibition rates of tyrosinase monophenolase and diphenolase were taken as indexes,the inhibition of tyrosinase activity by PALC extract was investigated preliminarily,PALC was used to prepare ferulic acid reference solution with the similar concentration,the inhibition of tyrosinase activity was stronger than ferulic acid,which laid a foundation for the application of PALC extract in whitening cosmetics.Colostrum centrifugal retention rate was taken as index,the single factor experiment was used to determine the colostrum preparation technology :sunflower seed oil and Ligusticum chuanxiong volatile oil distribution as early oil phase(volatile oil accounted for 0.1 % of sunflower seed oil,M/M),PGPR as the lipophilic emulsifier,dosage was 10 % of the oil phase,0.5% phenolic acid extract aqueous solution as the internal phase,the ratio of early oil phase and internal phase was 7:3,the high-speed dispersing emulsification machine with 10000 r/min emulsion 5 min,obtained.Multiple emulsions centrifugal retention rate was taken as index,the single factor experiment and pseudo ternary phase diagram were used to preliminarily screen the dosage range of the supplementary materials used for the preparation of multiple emulsions,D-optimum mixture design was used to optimum the multiple emulsions formula:colostrum as oil phase,tweens-80: span-80(1:1)as the hydrophilic emulsifier,1,3-butanediol as the emulsifier(Km value 3:1),pure water as the external water phase,oil phase-mixed emulsifier-water phase(15 %:22 %:63 %),magnetic stirrer with 2000 r/min emulsion 10 min,obtained.The multiple emulsions appearance was a white uniform emulsion,the average particle size was 268.8 cm,the average polydispersion coefficient was 0.243,the Zeta potential was-16.0 mV.The multiple emulsions stained by eosin indicator solution and observed under the microscope.The internal and external water phase were stained red,indicated that the multiple emulsions was W/O/W type.The preparation of W/O/W multiple emulsions of PALC was preliminarily evaluated,appearance character and skin irritation test were examined,content determination method of index components was established.The appearance of multiple emulsions was white emulsion,the content determination method was accurate and reliable,with strong specificity,it has no irritation to the skin.The factors affecting stability of the preparation were investigated,centrifugal test,light test,temperature test were examied.It was preliminarily confirmed that W/O/W multiple emulsions can improve the stability of aqueous solution of PALC extract,it had good stability under strong light,low temperature,room temperature,slightly stratified at high temperature and content no change in content 10 days. |
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