Exploratory Studies on the Effective Fractions of Tianshu Capsule

Tianshu capsule comes from Kim LiuWanSu《XuanMingLunFang》VolumeⅡof DCXW consisted with Rhizoma Chuanxiong and Rhizoma Gastrodiae. It has been been proved to be the original formula in treating migrine clinically.According to preliminary research results,in this study, reasonable technical means to better enrichment of volatile oil extraction、organic acids fraction of Rhizoma Chuanxiong、the total glycosides fraction ofGastrodia;Nitroglycerin-type experiments using rat model of migraine,with the scientific efficacy indicators,selected the best prescription of effective fractions of Tianshu Capsule.It is made into soft capsule on the basis of physico-chemical property.The reaserch carries out a systematic study and improvement on the extraction process,refining process, molding process, quality standards, pharmacodynamics,etc.Specific research contents and results are as follows:1. Preparation of effect fraction from Tianshu capsules1.) Preparation of volatile oil from Rhizoma ChuanxiongBy analyzing the transfer rate of Ligustilide and oil rate as the index, the best volatile oil extraction process by supercritical CO2 was decided through single factor experiments and orthogonal experiments:the extract pressure is 35Mpa, the temperature is 50℃, for 1 hour.2.) Preparation of organic acids extracts from Rhizoma ChuanxiongBy analyzing the transfer rate of ferulic acid and dry extract rate as the index, the best organic acids preparation process of Rhizoma Chuanxiong dregs after oil extraction was decided through single factor experiments and orthogonal experiments:70% ethanol refluxing extraction of 2 times, the extraction time is l.5 hour, and solid-liquid ratio is 1:10、1:8, combined filtrate。HPD-100 macroporous resin was assumed as the quality proportion of 8:1 (crude drug:macroporous resin),0.5g·ml-1of the extractive was added on a column of macroporous resin and was washed with distilled water of PH3.0、5% alcohol and 70% alcohol, successively, discard distilled water,5% ethanol site, collecting 70% ethanol wash off site.3.) Preparation of total glucoside extracts from Rhizoma GastrodiaBy analyzing the transfer rate of gastrodine and dry extract rate as the index, the best total glucoside preparation process of Rhizoma Gastrodia elata was decided through single factor experiments and orthogonal experiments:60% ethanol refluxing extraction of 3 times, the extraction time is2,1.5、1.5 hour, and solid-liquid ratio is 1:8、1:6、1:6, combined filtrate。AB-8 macroporous resin was assumed as the quality proportion of 1:2(crude drug:macroporous resin),0.5g·ml-1 of the extractive was added on a column of macroporous resin and was washed with distilled water、5% alcohol, successively, discard distilled water, collecting 5% ethanol wash off site.Decompressing and concertrating to the relative density 1.15(the temperature is 50℃),then adding 95% ethanol to 80% alcohol content, standing for 24h, filter through, then adding 40% NaOH solution to adjust PH to 8.0, standing for 24h, filter through, collecting filtrate, decompression and concertration.2.The research on quality criteria of effective fractions from Tianshu capsuleThe quality standard of effective fractions was established which contained the characteristics, indetification and so on. The Ligustilide contains no less than 8.0%, the total lactone no less than 26%, the ferulic acid contains no less than 4.0%, the organic acids no less than 45%, the gastrodine contains no less than 20% and the total glucoside no less than 25% according to assay study.It is formulated a stabilize and controllable quality criteria of the effective fractions by fingerprint study.3. The research on pharmacodynamics of effect fraction from Tianshu capsulePharmacological experiment were done to compare the drug efficacy between different dosages by adopting nitroglycerin type experimental rats,selecting scientific index.4. The research on formation technologyIt is made into soft capsule on the basis of physico-chemical property.According to the charaterstic of the soft capsule,the research choose the supplementary material of the contents.5. The research on quality standardThe quality standard of the soft capsule was established which contained the the characteristics,TLC, gross deviation, disintegration and determination of the Tianshu effect fraction soft capsule systematically, set the perfect quality standard. Each capsule contains Ligustilide no less thanl6mg, ferulic acid no less than 2.2mg, Gastrodin no less than 3mg, the total lactones no less than 52mg,the total organic acids no less than 24mg, the total glycosides no less than4.2mg. It gives the stable and reliable basis to the internal quality control of the preparation by fingerprint study.