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对常山碱的稳定性及其降解动力学进行研究。结果表明,24 h内流动相作溶剂时,常山碱含量仅降低1%,但在水、甲醇、50%甲醇及10%乙腈溶液中其含量降低为起始含量的90%。当溶液pH介于3~7时,24 h内常山碱的保留率在98%以上,但在碱性溶液中(pH 9.0)含量降低约12%。温度越高,常山碱稳定性越差,40~80℃放置10 h后,常山碱降为起始含量的60%左右,但在20℃下放置10 h,其含量仅降低约5%;40,60℃放置10 h,常山碱主要转化为异常山碱,二者的总含量较起始总含量基本不变,但是80℃下放置10 h,常山碱和异常山碱的总含量降低为起始总含量的83.33%,说明高温下常山碱结构发生了彻底改变,而不仅仅是异构化为异常山碱。光照对常山碱稳定性影响显著,强光照射108 h,常山碱质量分数较起始含量降低23%左右,但在避光和自然光条件下,其含量仅降低10%左右。无论在人工胃液(pH 1.4)还是人工肠液(pH6.8)中,放置10 h后,常山碱质量分数降低均小于5%。常山碱固体在高温(60℃)、高湿[(75±1)%]和强光(3 000 lx)照射下放置10 d后,其含量分别减少0.27%,7.6%,5.39%。常山碱在水、甲醇、50%甲醇和10%乙腈溶剂中、碱性溶液、不同光照和不同温度(20,40℃)下的降解基本符合化学动力学一级反应。因此,无论是常山碱的制备纯化还是相关制剂的生产,都应在偏酸性溶液,低温、避光条件下快速操作完成,而常山碱固体则应在干燥、避光条件下保存。
The stability of Changshan base and its degradation kinetics were studied. The results showed that when the mobile phase was used as a solvent for 24 hours, the content of permafrost decreased by only 1%, but its content decreased to 90% of its initial content in water, methanol, 50% methanol and 10% acetonitrile solution. When the solution pH ranged from 3 to 7, the retention of Changshan base was above 98% within 24 h, but decreased about 12% in alkaline solution (pH 9.0). The higher the temperature, the poorer the stability of Changshan alkali. After being placed at 40 ~ 80 ℃ for 10 h, Changshan alkali reduced to about 60% of the initial content, but the content decreased only about 5% after being placed at 20 ℃ for 10 h. , When the temperature was 60 ℃ for 10 h, the content of Changshan alkali was mainly changed to abnormal Shan base. The total content of the two components was almost unchanged from the initial total content. However, the total content of Changshan base and the abnormal Shan base decreased after 10 h at 80 ℃ The initial total content of 83.33%, indicating that Changshan alkali structure underwent a radical change, not just isomerization into abnormal Shan base. The light had a significant effect on the stability of Changshan alkali. Under the light irradiation for 108 h, the content of theophylline was about 23% lower than the initial concentration, but the content decreased only about 10% under the conditions of dark and natural light. In the artificial gastric juice (pH 1.4) or artificial intestinal juice (pH6.8), the content of theophylline decreased by less than 5% after being placed for 10 h. The content of Changshan base solid decreased by 0.27%, 7.6% and 5.39% respectively after being exposed to high temperature (60 ℃), high humidity (75 ± 1)% and high light (3000 lx) for 10 days. Changshan alkali in water, methanol, 50% methanol and 10% acetonitrile solvent, alkaline solution, under different light and different temperature (20,40 ℃) degradation basically in line with the first order kinetics of chemical reaction. Therefore, both the preparation of pericardine preparation and purification or related preparations should be carried out in acidic solution, low temperature, dark conditions, fast operation, and permanganine solid should be stored in dry, dark conditions.