柴银口服液醇沉工艺对黄芩苷收率的影响

Effect of Chaiyin Oral Liquid Alcohol Precipitation Process on Yield of Flavoside

目的:优化柴银口服液醇沉工艺条件,提高柴银口服液指标成分黄芩苷转移率。方法:采用单因素试验考察柴银口服液清膏醇沉时间,测定醇沉上清液中干物质得率,高效液相色谱法(HPLC)测定黄芩苷含量,并计算黄芩苷转移率,确定最佳醇沉时间;采用正交试验设计研究不同醇沉条件下柴银口服液清膏醇沉后黄芩苷含量及转移率,并进行主效应分析、主观分析。结果:不同醇沉时间(12、16、20、24、30、36 h)考察中,黄芩苷转移率分别为85.25%、87.98%、90.44%、92.03%、91.41%、89.17%,干物质得率分别为13.54%、14.18%、13.95%、14.27%、14.31%、13.58%,醇沉时间对干物质得率影响无统计学意义,当醇沉时间为24 h时,黄芩苷转移率最高,为92.03%。正交试验考察中,9个试验组的干物质得率、黄芩苷含量、黄芩苷转移率经主效应分析、直观分析等分析方法,得出当醇沉工艺为预醇沉碱化乙醇pH为8、碱化乙醇含醇量为60%、二次醇沉乙醇含醇量为85%时,黄芩苷转化率明显高于其余2个水平。结论:柴银口服液清膏最佳醇沉时间为24 h,最佳醇沉工艺条件为先加入2倍量pH为8、60%的碱化乙醇,再加85%乙醇至含醇量60%,此时扩大生产的平均黄芩苷转移率为90.08%。

Objective:To optimize the alcohol precipitation process of Chaiyin oral liquid.Methods:The single factor experiment was used to investigate the alcohol precipitation time of Chaiyin oral liquid ointment,determine the dry matter yield in the alcohol precipitation supernatant,determine the baicalin content by HPLC,and calculate the baicalin transfer rate to determine the optimal alcohol precipitation time.The cross-experiment design was used to study the content and transfer rate of baicalin in the Chaiyin oral liquid ointment under different alcohol precipitation conditions,and subjective analysis,and subjective analysis were performed.Results:In the investigation of different alcohol precipitation times(12,16,20,24,30,36 h),baicalin transfer rates were 85.25%,87.98%,90.44%,92.03%,91.41%,and 89.17%,and the dry matter yields were 13.54%,14.18%,13.95%,14.27%,14.31%and 13.58%,the alcohol precipitation time had no significant effect on the dry matter yield.When the alcohol precipitation time was 24 h,baicalin transfer rate was the highest,being 92.03%.In the orthogonal test,the dry matter yield,baicalin content,and baicalin transfer rate of the 9 test groups were analyzed by main effect analysis,and visual analysis.It was concluded that the alcohol precipitation process was pre-alcohol precipitation.When the pH of alkalinized ethanol was 8,the alcohol content of alkalinized ethanol was 60%,and the alcohol content of secondary alcohol precipitation ethanol was 85%,the flavone conversion was significantly higher than the other two levels.Conclusion:The best alcohol precipitation time of Chaiyin oral liquid clear cream is 24 hours.The optimal alcohol precipitation process conditions are to first add 2 times the amount of alkalinized ethanol with pH=8 and 60%,and then add 85%ethanol to 60%alcohol content.At this time,the average baicalin transfer rate of expanded production was 90.08%.