复方川芎美白淡斑乳膏的制备工艺研究及质量评价

Preparation Process and Quality Evaluation of Compound Ligusticum Chuanxiong Whitening Cream

目的制备复方川芎美白淡斑乳膏并进行质量评价。方法按川芎-益母草-白芷-当归质量比4∶3∶2∶1制备中药提取液,以酪氨酸酶的抑制率及1,1-二苯基-2-三硝基苯肼(DPPH)自由基的清除率为评价指标确定中药提取液的最佳质量浓度。采用机械法制备复方川芎美白淡斑乳膏;采用目测法观察外观;采用生物显微镜观察粒度;采用pH计测定pH;采用高效液相色谱法测定阿魏酸的含量,色谱柱为Elite-ODS柱(200 mm×4.6 mm,5µm),流动相为甲醇-1%冰醋酸(30∶70,V/V),流速为1.0 mL/min,柱温为30℃,检测波长为321 nm,进样量为10µL;对制备样品的微生物限度及初步稳定性进行考察。结果中药提取液的质量浓度在1~50 mg/mL和1~10 mg/mL范围内分别与酪氨酸酶的抑制率及DPPH自由基的清除率呈显著正相关(P<0.01)。制备的复方川芎美白淡斑乳膏质地均匀、细腻、有光泽、硬度适中,易于挑起、涂抹;粒径小于2µm,且分布均匀;pH为6.8。阿魏酸的质量浓度在1.53~30.69µg/mL范围内与峰面积线性关系良好(r=0.9994,n=5);精密度、稳定性、重复性试验结果的RSD均小于2.0%;阿魏酸低、中、高质量浓度(88,132,176µg/mL)平均回收率分别为(99.51±0.97)%,(100.08±0.51)%,(100.97±0.73)%,RSD分别为0.97%,0.51%,0.73%(n=3);3批样品中阿魏酸的含量分别为179.63,185.38,179.30µg/g。微生物限度检测结果显示,样品中需氧菌总数为20 cfu/g,未检出霉菌和酵母菌。耐寒试验及耐热试验后,复方川芎美白淡斑乳膏的外观仍均匀、细腻,无油水分层现象,涂抹在皮肤上无粗颗粒;离心试验后,外观、性状无明显改变,且无油水分层现象。结论所建立的制备工艺操作简便,制备样品的质量稳定,可用于复方川芎美白淡斑乳膏的制备和质量控制。

Objective To prepare the Compound Ligusticum Chuanxiong Whitening Cream(LW-C),and to evaluate its quality.Methods A traditional Chinese medicine extract was prepared with a mass ratio of Chuanxiong Rhizoma∶Leonuri Herba∶Angelicae Dahuricae Radix∶Angelicae Sinensis Radix of 4∶3∶2∶1.The optimal concentration of the extract was determined with the inhibition rate of tyrosinase and the clearance rate of 1,1-diphenyl-2-trinitrophenylhydrazine(DPPH)free radicals as evaluation indexes.LW-C was prepared by the mechanical approach.The appearance was observed by the visual inspection method,the particle size was measured by the biological microscope,and the pH of LW-C was measured by the pH meter.The content of ferulic acid was determined by the high-performance liquid chromatography(HPLC)method,the chromatographic column was Elite ODS column(200 mm×4.6 mm,5µm),the mobile phase was methanol-1%glacial acetic acid(30∶70,V/V),the flow rate was 1.0 mL/min,the column temperature was 30℃,the detection wavelength was 321 nm,and the injection volume was 10µL.The microbial limits and preliminary stability of the prepared samples were investigated.Results The mass concentrations of traditional Chinese medicine extract in the ranges of 1-50 mg/mL and 1-10 mg/mL were significantly positively correlated with the inhibition rate of tyrosinase and the clearance rate of DPPH free radicals(P<0.01),respectively.The prepared LW-C was uniform,delicate,glossy texture,moderate hardness,and it was easy to pick up and apply.The particle size was less than 2µm and evenly distributed.The pH was 6.8.The linear range of ferulic acid was 1.53-30.69µg/mL(r=0.9994,n=5).The RSDs of precision,stability,and repeatability test results were all lower than 2.0%.The average recoveries of low-,medium-,and high-concentrations of ferulic acid(88,132,176µg/mL)were(99.51±0.97)%,(100.08±0.51)%,and(100.97±0.73)%,respectively,with RSDs of 0.97%,0.51%,and 0.73%(n=3).The content of ferulic acid in three batches of samples was 179.63µg/g,185.38µg/g,and 179.30µg/g,respectively.The microbial limit test results showed that the total number of aerobic bacteria in the sample was 20 cfu/g,and no mold or yeast was detected.After the cold and heat resistance tests,the appearance of the LW-C remained uniform and delicate,without oil-water stratification,and there were no coarse particles on the skin when applied.After centrifugation test,there was no significant change in appearance and properties,and there was no oil-water stratification phenomenon.Conclusion The established preparation process is simple to operate,and the quality of the prepared samples is stable.It can be used for the preparation and quality control of LW-C.