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OBJECTIVE:To optimize the purification technology of total saponins from Asparagus cochinchinensis with macro-reticular resin. METHODS:Using content of total saponins from A. cochinchinensis as index,single factor test was used to investi-gate the macroreticular resin model,sampling adsorption time,mass concentration of the column,adsorption capacity,volume frac-tion and the amount of elution solvent,elution rate,and optimize the purification technology. And verification test was conducted. RESULTS:HPD-300 macroreticular resin showed strong absorption and desorption property. The optimal purification technology was that sampling adsorption time was 60 min,mass concentration of sample liquid was 0.1 g/mL,adsorption capacity was 120 mL(15 BV),it was eluded with 60% ethanol solution with 3 BV and elution rate was 4 BV/h. In the verification test,the average desorption rate of total saponins was 68.30%(RSD=0.95%,n=3). CONCLUSIONS:Optimized purification technology is sta-ble,feasible,and can easily separate and purify the total saponins from A. cochinchinensis.
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OBJECTIVE:To establish the method for determining 10 residual organic solvents in norvancomycin hydrochloride raw material. METHODS:Headspace gas chromatography was performed on the column of nitro modified polyethylene terephthal-ate glycol as stationary phase capillary column;the oven temperature program started at 40 ℃ for 3 min and increased at a rate of 8 ℃/min up to 150 ℃ for 10 min;the temperature was 200 ℃ with carrier gas of high-purity nitrogen gas,the constant flow rate was 5 ml/min with split ratio of 15∶1;the headspace vial equilibrium temperature was 85 ℃ with equilibrium time of 40 min,and the volume was 1 ml. RESULTS:The concentration of n-pentane,acetone,ethanol,benzene,acrylonitrile,toluene,xylene,chlo-robenzene,styrene,divinylbenzene had good linear relationship with its peak area values(r=0.995 7-0.999 9);the RSDs of preci-sion,repeatability tests was ≤6.6%;average recovery was in the range of 94.3%-106.6%(RSD=0.5%-4.5%,n=9). CONCLU-SIONS:The method is fast,sensitive and accurate,and can be used for the determination of residual organic solvents in norvanco-mycin hydrochloride raw material.
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Objective: Enriching secoiridoid glycoside in Gentiana manshurica kitag. Methods: Gentiana manshurica kitag. was extracted with 70% EtOH by cold macerating and purified with AB 8 macroreticular resin. Results: The content of gentiopicrin in the extract is 28.69%. Conclusion: AB 8 macroreticular resin fits in purification of water soluble secoiridoid glycoside in Gentiana manshurica kitag.
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Objective: To study the technological parameters of the purification process of total saponins of Rubus parvifolius L. with macroreticular resin. Methods: The adsorptive characteristics and elutive parameters of the process were studied by taking the elutive and purified ratio of total saponins of Rubus parvifolius L. as marker. Results: 19.3mL of the extractive of total saponins of Rubus parvifolius L. was purified with a column of macroreticular resin (R1cm?H20cm,dried weight 2.68g) and was washed with 100mL of distilled water, then was eluted with 100mL of 50% ethanol. Conclusion: With macroreticular resin to adsorb and purify, the elutive ratio of total saponins of Rubus parvifolius L. was over 79.2% and the purity reached 55.3%. So this process of applying macroreticular resin to adsorb and purify total saponins of Rubus parvifolius L. is feasible.
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AIM: To study the optimal condition and parameters for the enrichment process of paeoniflorin in Kunyining Granules (Radix Paeoniae Rubra, etc.) with macroreticular resin. METHODS: With the enrichment degree of paeoniflorin in Kunyining Granules as an index, the optimal conditions of the enrichment process were investigated. RESULTS: The optimal condition showed that the aqueous extract was taken into the macroporous resin column, and kept for 30 min, then the resin was washed by water to get rid of impurity and then we used six times as much 50% ethanol as aqueous extract to elute paeoniflorin. CONCLUSION: The process is feasible to enrich paeoniflorin from Kunyining Granules.
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AIM: To screen macroreticular resins for isolation and purification of flavonoids from the leaves of Diospyros kaki Linn (FLDK). METHODS: 8 kinds of macroreticular resins were assayed for their adsorbability and deadsorbability as well as the adsorption kinetics to FLDK. RESULTS: Polyamide and AB-8 resin were found with good adsorbability and deadsorbability as well as adsorption kinetics to FLDK. CONCLUSION: AB-8 resin and polyamide could be used for preparing high contents of FLDK. FLDK-P70, a flavonoid extract contained more than 77% of flavonoids was prepared from the extract of leaves of Diospyros kaki by polyamide adsorption column isolation.
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Objective: To study the technological parameters of the purification process of ginsenosides with macroreticular resin. Methods: The adsorptive characteristics and elutive parameters of the process were studied by taking the elutive and purified ratio of ginsenosides as marker. Results: 45ml of the extractive of ginseng (5.88mg/ml) was purified with a column of macroreticular resin (R15mm?H90mm, dried weight 2.52g) and washed with 100ml of distilled water, then eluted with 100ml of 50% ethanol. Conclusion: With macroreticular resin to adsorb and purify, the elutive ratio of ginsenosides was above 90% and the purity reached 60.1%. So this process of applying macroreticular resin to adsorb and purify ginsenosides is feasible.
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AIM: To study the technological parameters of the purification process of total salvianolic acid(TSA) of Radix Salvia Miltiorrhizae(RSM) with D101 macroreticular resin. METHODS: Based on orthogonal experiment,the reservation rate of TSA in macroreticular resin columniation was took as index to investigate the chief influential factors in the purification of TSA. RESULTS: The volume of distilled water and the content of TSA in RSU solution had significant effect on the reservation rate of TSA in macroreticular resin columniation. With the help of macroreticular resin,the reservation rate of TSA could reach 87.52%.Its purity was 77.74%,comparing with crude extract,increased by 3.6 times. CONCLUSION: The method of purifing TSA of RSM with D101 macroreticular resin is feasible,it could be applied to industrialized production of TSA of RSM.
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AIM: To study the technological parameters of the purification process of total flavonoids of Crataegus leaves with HPD-600 macroreticular resin. METHODS: Using orthogonal experiments,the adsorptive characteristics and elutive parameters of the process were studied by taking the elutive effects and purification ratio of total flavonoids of Crataegus leaves. RESULTS: Two significant factors which were the concentration of crude flavonoids solvent and elutant component were observed. CONCLUSION: The microwave-assisted extraction and purification process with macroreticular resin is employed,the content of total flavonoids is 80.75%, the rutin content is (1.38)%, The macroreticular resin can be used in the purification of flavonoids of Crataegus leaves.