| 1. Research on quality control method of radix sophorae flavescentis.Objective:To set up quality control method of radix sophorae flavescentis;Methods:Using TLC for identification of radix sophorae flavescentis; determinating the content of total alkaloid in radix sophorae flavescentis by using visual spectrophotometry; HPLC method was adopted for the determination of indicative components. The analysis was performed with Agilent ZORBAX NH2 column (5?m, 4.6 mm×150 mm); The mobile phase was Acetonitrile-Ethanol-3%Phosphate (84:10:6),at a flow rate of 1 mL·min-1; The wavelength of the detector was 210 nm;Results:The identification method for radix sophorae flavescentis was of good specificity; The linearconcentration range of matrine were 42.56?425.6?g (r=0.9997) in the determinating the content of total alkaloid in radix sophorae flavescentis by using visual spectrophotometry and the average recovery were 100.2% with RSD of 1.70% (n=6); The linear concentration range of Sophocarpine, matrine, Oxysophocarpine, sophoridineand, oxymatrine were 0.1144?0.5720?g (r=0.9997), 0.2080?1.0400?g ( r=0.9997), 0.1836?0.9180?g (r=0.9998), 0.2088?1.044?g (r=0.9992), 0.2456?1.228?g(r=0.9999),average recovery and RSD%(n=6)were 101.6%?1.93,98.29%?1.87,103.85?1.79,99.87%?2.01,102.7%?2.19, respectively. Conclusions:The determination results showed that the method was easy and accurate which could be used to estimate quality of radix sophorae flavescentis. 2. Research on quality control method of Radix Astragali.Objective:To set up quality control method of Radix Astragali;Methods:Using TLC for identification of Radix Astragali; determinating the content of total saponins in Radix Astragali by using visual spectrophotometry; HPLC method was adopted for the determination of astragaloside IV. The analysis was performed with ODS column (5?m, 4.6 mm×200 mm); The mobile phase was Acetonitrile-water(30:70),at a flow rate of 1 mL·min-1; The wavelength of the detector was 203 nm;Results:The identification method for Radix Astragali was of good specificity; The linear concentration range of astragaloside IV were 0.0275?0.275mg in the determinating the content of total saponins in Radix Astragali by using visual spectrophotometry and the average recovery were 99.9% with RSD of 1.49% (n=6); HPLC was used to determine content of astragaloside IV in Radix Astragali and the linear concentration range of astragaloside IV were 1.1?11.0?g (r=0.9998),average recovery and RSD%(n=6)were 101.6%, 1.93 respectively; Conclusions:The determination results showed that the method was easy and accurate which could be used to estimate quality of Radix Astragali.3. Research on extraction and purification of matrineObjective:To optimize the process of extraction and purification of matrine;methods:Radix sophorae flavescentis were extracted with 60% alcohol. The optimum extraction process was optimized by applying orthogonal test. The extracting times, alcohol content, extracting period, amount of solvent were optimized with matrine and oxymatrine amount as indicator; selecting the type of resin with absorbing amount and release amount of matrine and oxymatrine as indicator; total alkaloid of radix sophorae flavescentis was absorbed and separated with cathode ion exchange resin and the process was monitored by HPLC to optimize the processing parameter; the total alkaloid was refined by leach and recrystallisation; Results:The optimized process of extraction and purification of matrine: The results are that herbs are to be extracted with 60% alcohol for 3 times, two hours for each time,12?10?10 times amount of alcohol as much as the herbs was added as solvent. Filtrating the extract liquid and reclaiming alcohol, then concentrating the liquid to the concentration 1 g·mL-1. then concentrated solution was adjust to pH2,centrifuging for 15 min (4000 r·min-1) to get sample solution. The sample solution pass through 732 type exchanging resin column, eluted with 80% alcohol(containing 20% of ammonia). Reclaiming alcohol and concentrating and drying to get total alkaloid. The process of refining of matrine: dissolving the total alkaloid with acid water and then extracted with ether to remove off impurities. The water layer was then adjusted to pH12-13 and extracted with ether and then reclaiming ether. The residue was dissolved with petroleum ether and refining matrine by recrystallisation with petroleum ether as solvent. Conclusions:The process could be used for extraction and purification of matrine?4. Research on extraction and purification of total saponins of AstragalusObjective:To optimize the process of extraction and purification of total saponins of Astragalus; Methods:The optimum extraction process was optimized by applying orthogonal test. The extracting times, alcohol content, extracting period, amount of solvent were optimized with total saponin amount as indicator; total saponins of Astragalus was absorbed and separated with m acroporous resin and the process was monitored by HPLC to optimize the processing parameter; Results:The optimized process of extraction and purification of total saponins of Astragalus: The results are that herbs are to be extracted with 60% alcohol for 3 times, 1.5 hours for each time,12?10?10 times amount of alcohol as much as the herbs was added as solvent. Filtrating the extract liquid and reclaiming alcohol, then concentrating the liquid to the concentration 1 g·mL-1. then concentrated solution was centrifuged for 15 min (4000 r·min-1) to get sample solution. The sample solution pass through resin column, eluted with 70% alcohol. Reclaiming alcohol and concentrating and drying to get total saponin. Conclusion:The process could be used for extraction and purification of total saponins of Astragalus.5. Study on Absorption of matrine in Rat IntestinesObjective:To study the absorption characters of matrine in various intestine segments; Methods:Phenol red was used as the indicator. The intestine absorption characters of matrine were detected by the in situ single pass intestine perfusion method. The concentrations of phenol red and matrine in the perfusate were determined by HPLC; Results:1.2×10-3 cm·min-1?The effective permeability ( Peff, 10-3 cm·min-1) of matrine in duodenum, jejunum, ileum and colon were more then 1.2×10-3 cm·min-1, respectively; Conclusion:Matrine could be well absorbed in general intestinal tract without specific absorption site. matrine is suitable for the sustained release dosage form to be administered twice a day.6. The pharmacokinetic reseatch of matrineObjective:Determine the pharmacokinetic parameter of matrine; Methods: A simple high-performance liquid chromatography (HPLC) method is described for the determination of matrine in in various samples. calculated pharmacokinetic parameters with pharmacokinetic software; The bind rates of matrine with protein were determined by balanceable dialysis. determining excretion rate from urine or feces after ig. Matrine at dose 40mg·kg-1?20 mg·kg-1?10 mg·kg-1; Results:The mean Cmax at doses of 10, 20 and 40mg were 0.903±0.086, 1.549±0.304 and 2.797±0.474?g·mL-1 occurring at 105±41.352, 105±16.432 and 95±12.247 min, respectively. The mean AUC0?t were 260.603±23.802, 356.135±40.698 and 619.73±109.395 mg?L-1?min, respectively and the mean AUC0??were 319.708±31.64, 531.737±78.999 and 671.229±119.348 mg?L-1?min, respectively. The t1/2 were 178.828±19.095, 293.543±57.266 and 109.189±2.978min, respectively, for the doses. The mean absolute bioavailability was 64.7% after i.g. matrine to rats at dose 10?20?40 mg·kg-1 . matrine distributed in rats wildly and the concentration in tissues range taked turns from kidney,liver,lung,heart,brain,muscle. The bind rates of matrine with protein were (47.8±11.45)%,(31.3±10.83)%,(29.0±8.36)% in plasma at concentration of 4.18?2.09?1.045?g?mL-1. The excretion rates of matrine were 37.652%?22.853%?22.383% after ig at the dose of 40mg·kg-1?20 mg·kg-1?10 mg·kg-1 in 0?48h from urine. so most of matrine was excreted from urine and almost no matrine excreted from feces. Conclusions:The pharmacokinetic profile of matrine could provide science evidence for the designing of dosage form and clinical application.7. the research on preparation process of kuqi sustained release tabletsObjective: Designing the manufacture process of sustained release tablets; To prepare matrine sustained - release tablet for prolong effective time and study on characteristics of the release trial in vitro.Methods:Based on sigle-factor tests and orthogonal test, the optimum preparation process was optimized;Matrine was used as a water soluble drug model to prepare sustained - release matrix tablets and the release rate of sustained - release tablet was determined by HPLC method in vitro. Results:The tablets prepared possessed the profile of sustained release preparation. The dissolution profiles of matrine sustained - release tablet conformed to Higuchi formula basically.The released amounts of ingredient in tablets were 20-40%,40-60% and more than 90%. Conclusions:The process could be used for preparation of sustained release tablets. 8. Research on quality control method of matrine and saponin of astragali.Objective:To set up quality control method of matrine and total saponins of Radix Astragali; Methods:Using TLC for identification of matrine and total saponins of Radix Astragali; determinating the content of total saponins of Radix Astragali by using visual spectrophotometry; HPLC method was adopted for the determination of matrine and astragaloside IV; Results:The quality standard of matrine and total saponins of Radix Astragali was studied and establish; Conclusions:The identification method was of good specificity;the method was easy and accurate which could be used to control the quality of matrine and total saponins of Radix Astragali.9. Research on quality control standards of kuqi sustained release tabletsObjective:To set up quality control standards of kuqi sustained release tablets; Methods:Using TLC for identification of matrine and total saponins of Radix Astragali; determinating the content of total saponins of Radix Astragali by using visual spectrophotometry; HPLC method was adopted for the determination of matrine and astragaloside IV; on the base of the test of release rate, release rate was prescribed. The release rate should be 20%?40%, 40%?60%, more than 90% of the indicated amount of matrine in 2 h,4h, 10 h, respectively; Results:The quality standard of kuqi sustained release tablets was established; Conclusions:The quality control standard established could be used for the quality control of kuqi sustained release tablets. |
PDF Full Text Request