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Objective:To investigate the purification of antibacterial effective fraction of Syringae folium by macroporous resins. Methods:Static adsorption and desorption tests were carried out to screen the macroporous resins. The desorption experiment was per-formed on the selected D101 resin to optimize the separation process. The effects of resin amount, diameter length ratio, elution flow rate, elution solution concentration and volume were studied. Results:The optimal conditions were as follows:the elution solution was 55% ethanol, the adsorption flow rate was 1 BV·h-1 , the elution flow rate was 5 BV·h-1 , 6 BV 25% ethanol was used to eliminate impurity and 8 BV 55% ethanol was used to elute to obtain the effective fraction. Conclusion: The content of antibacterial effective component is above 65% after purified by D101 resin, indicating that the present method is suitable for large-scale preparation of anti-bacterial effective fraction of Syringae folium.
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Objective: To explore the optimal separation of polypeptides from Periplaneta americana by selecting appropriate macroporous resins and optimizing purification technology. Methods: Taking the index component test and inhibition experiment of tumor cells in vitro method as indexes, macroporous resins type was chosen and single factor test was adopted to evaluate some factors affecting separating technology. The elution position was analyzed by Automatic amino acid analyzer. Results: Macroporous resin HP20 had the best separating efficiency and the best purification conditions were as follows: the content in P. americana liquid 0.3 g/mL equivalent to raw material, the volume of drug 2 BV, the adsorption rate 2 BV/h, the volume of 70% ethanol as eluant 2 BV with elution rate of 2 BV/h. The recovery rate of polypeptides of elution position could reach 88.53% and the bound amino acids (polypeptides) was 55.64%. Conclusion: This technology is reasonable and feasible and has good separation effect, which could be used for enrichment and purification of antineoplastic compounds from P. americana.
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Objective: To explore the optimal separation and purification of extract in Sanao Sustained-release Tablets. Methods: Taking the adsorption ratio and desorption ratio of ephedrine hydrochloride, pseudoephedrine hydrochloride, amygdalin, and glycyrrhizinate as evaluation indexes to optimize the purification process of Sanao Sustained-release Tablets by multi index comprehensive score. Results: Macroporous resin HPD 300 had the best adsorption and desorption properties. In the course of adsorption, the optimum concentration of the sample liquid was 1.67 g crude drugs of per milliliter, the resin column size ratio was 1: 7, the concentration of sample solution was 0.6 g/mL crude drug, the sample flow rate was 4.0 BV/h. In the course of elution, 2 BV deionized water was used and the resin column chromatography was eluted with 5 BV of 70% EtOH by flow rate of 3 BV/h. Conclusion: Macroporous resin HPD 300 is suitable to separate and purify the extract from Sanao Sustained-release Tablets.
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Objective: To optimize the extraction and purification technology of phenylethanoid glycoside from Cistanche tubulosa. Methods: Orthogonal design L9(34) was employed to optimize the extraction conditions by taking the extraction yield of echinacoside and acteoside as indexes. The absorption-desorption characteristics of seven macroporous resins were evaluated, then the best purification conditions were optimized. Results: The optimal extraction conditions were as follows: The air-dried stems of C. tubulosa were powdered and extracted twice with 12-fold 50% ethanol for 1 h each time, temperature was 70℃; The supernatant was concentrated to 5-fold weight of the stems of C. tubulosa. The concentrated liquid was subjected to macroporous resin (HPD750) column and then eluted with deionezed water (3 BV) and 30% ethanol (4 BV), respectively. The 30% ethanol fraction was evaporated under vacuum to give the phenylethanoid glycoside-rich C. tubulosa stem extract. The purity of phenylethanoid glycoside was above 75%. Conclusion: The optimized extraction and purification process is stable, efficient, and suitable for industrial production.
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Objective In order to study the application of macroporous resins and so on to the purified active components of Euphorbia humifusa、Leaves of Flos Lonicerae、Chrysanthemum morifolium,adsorption and separation properties for 3 types of macroporous resins and polyamide were investigated.Methods The total flavone was used as the evaluating criteria,we selected suitable macroporous resins and studied optimum technological parameters of the adsorption and elution.Spectrophotometry was used for the determination of total flavone.Results The suitable macroporous resins which were used to the purified active components of traditional Chinese medicine were D101 and DA201 and DM301 for Euphorbia humifusa、DA201 for Leaves of Flos Lonicerae、D101 and DA201 and DM301 for Chrysanthemum morifolium,The concentration of the sample of Euphorbia humifusa for DA201 and D101 were 0.49～1.47 and 0.42～1.31 mg/ml.The concentration of the sample of Leaves of Flos Lonicerae for DA201 was 1.03～2.07 mg/ml.The concentration of the sample of Chrysanthemum morifolium for DA201 and D101 was 0.50～1.00 and 0.71～1.99 mg.ml.In the adsorption course,appeared leaking were 8 and 10、2、2 and 1 BV respectively.In the elution course,when the alcohol concentrations were 20%、30%、40% and 20%、30%、40%;10%、20%、30%;30%、40%、50% and 20%、30%、40%;respectively,the total flavone content in the elution solutions was higher.The influence of temperature to DA201 and D101 adsorpting total flavone for Euphorbia humifusa was not great.But the influence of temperature to DA201 and D101 adsorpting total flavone for Leaves of Flos Lonicerae and Chrysanthemum morifolium were certain degree.Conclusions It is obviously different to refine the total flavone active components of traditional Chinese medicine,while using 3 types of macroporous resins and polyamide.