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目的:优选蜣螂有效部位的制备工艺,探索通过提取液理化表征来进行过程控制的可行性。方法:采用单因素试验法,主要以有效组分多肽与氨基酸的含量为指标,结合流变学、表面化学、电学等方面的表征,系统考察影响蜣螂有效部位制备相关的提取、浓缩、分离、纯化、干燥各环节的各因素。结果:确定了蜣螂有效部位的制备工艺条件,即:取蜣螂药材粉碎为粗粉,用3倍量的85%乙醇浸泡48h,加85%乙醇10倍量,以4mL·min-1·kg-1的速度渗漉,收集漉液,滤过,滤液在50～55℃浓缩至1∶1,冷藏除脂后,通过DA201-C大孔树脂柱,先后用1BV水与4BV70%乙醇为洗脱剂进行洗脱,分别收集洗脱液。水洗脱液浓缩,干燥,加85%乙醇洗涤2次,取洗液,与70%乙醇洗脱液合并,浓缩,干燥,即得。同时,本实验对有效部位制备各环节的液相体系进行表征,发现与有效物质多肽相关的表面张力基本未变,而与无效物质盐密切相关的电导率降低了约90%,最大限度地保留了药物治病的有效信息,去除了无效信息。结论:筛选的蜣螂有效部位制备工艺条件稳定可靠,通过提取液理化表征来进行过程控制切实可行。
OBJECTIVE: To optimize the preparation process of the effective parts of Dung beetle and to explore the feasibility of process control through the physical and chemical characterization of the extract. Methods: The single factor test was used to study the effects of extracting, concentrating and separating the effective parts of Dung beetle in order to evaluate the contents of polypeptides and amino acids in the effective components and rheology, surface chemistry and electrical properties. , Purification, drying all aspects of the various factors. Results: The preparation conditions of the effective parts of Dung beetle were determined, that is, the dung beetle was crushed into coarse powder, soaked with 3 times the amount of 85% ethanol for 48h, added 10 times of 85% ethanol to 4mL · min -1 kg-1 speed percolation, collecting glistening fluid, filtration, the filtrate was concentrated at 50 ~ 55 ℃ to 1: 1, after degreasing refrigeration, through the DA201-C macroporous resin column, followed by 1BV water and 4BV70% ethanol as Eluent elution, were collected eluent. The aqueous eluate is concentrated, dried, washed twice with 85% ethanol, the washings are taken, combined with 70% ethanol eluent, concentrated and dried. At the same time, the experimental liquid phase of the preparation of the effective parts of the system were characterized and found that the active substance polypeptide-related surface tension remained unchanged, and closely related to the ineffective substance salt conductivity decreased by about 90%, to maximize the retention The effective treatment of medical information, remove the invalid information. Conclusion: The preparation conditions of effective part of Dung beetle are stable and reliable. It is practicable to carry out process control through physical and chemical characterization of extract.