基于有效组分检测与理化表征相结合的蜣螂有效部位制备工艺研究

Preparation technology of effective fraction of Catharsius molossus based on determination of effective composition and characterization of physico-chemical property

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 technology of effective fraction of Catharsius molossus, and investigate the feasibility of process control by the physical and chemical characterization of extracts. Method： Used single-factor test method, choosed the main effective components of peptides and amino acids as indexes, combined with rheology, chemistry, electricity, and other characterization, the study researched the prepared technology of effective fraction of C. molossus including extraction, concentration, separation, purification, drying and so on. Result： The optimal preparation technology of effective fraction of C. molossus was that soaked an amount of crude drugs with three times of 85% ethanol for 48 h, added 10 times of 85% ethanol, percolated in 4 mL · min^-1 · kg^-1, collected percolation liquid, concentrated to 1：1 at 50-55 ℃, removed fat by frozen, adopted DA201-C macroporous resin, used 1 BV of water and 4 BV of 70% ethanol as eluting agent, collected eluant respectively. The water part was concentrated and dried, then washed twice with 85% ethanol, collected washing liquid and mixed with 70% ethanol eluant. The product was obtained by concentrating and dring. At the same time, the liquid-phase system of each link was characterized in preparation of effective fraction of C. molossus, which showed that the surface tension related to polypeptide was essentially unchanged, and the conductivity related to salt decreased by about 90% with ineffective substances closely related to salt. The results showed that the preparation technology maximumly retained the effective information, and removed the invalid information. Conclusion： The preparation technology of effective fraction of C. molossus is stable and reliable, and the process control in physico-chemical characterization of extracts is feasible.