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Objective To determine the technological conditions for the purification of the total alkaloid from the Corydalis Rhizoma (CR) by macroporous adsorption resin. Methods Total alkaloids of CR were determined by acid dye colorimetry, palmatine hydrochloride, dehydrocorydaline, tetrahydropalmatine, and corydaline were determined by HPLC. Six macroporous adsorption resins were investigated with the absorption rates, elution rates, and the content of the total alkaloid and four alkaloids of CR by static and dynamic adsorbing experiments. The purification process conditions of the total alkaloid of CR were optimized by the loading amount and volume flow of sample, the type and volume of the impurity removal of solvent and elution solvent and so on. The stability of the purification process was investigated by 5, 10 times enlargement. Results D141 type macroporous adsorption resin was the best choice for the purification of the total alkaloid from CR, the optimized parameters were as follows: Drug concentration was 0.6 g/mL of medicinal material and was added to the D141 macroporous resin column that the ratio of diameter to height range from 1:5 to 1:9 at a flow rate of 2 BV/h to 2 BV, 1.3 BV of purified water was used to remove impurities, and then 6 BV 95% ethanol was used as eluent at a flow rate of 2 BV/h. The purity of the total alkaloid of CR was up to 68.19% after purification, and the content of palmatine hydrochloride, dehydrocorydaline, tetrahydropalmatine, and corydaline was 1.95%, 11.74%, 4.93%, and 6.36%, respectively. The purity of the total alkaloid of the CR can reach more than 65% by 5 times and 10 times enlargement. Conclusion The purity of the total alkaloids can reach more than 65% after verification test, and the transfer rate of total alkaloids and four alkaloid monomers of CR can reach more than 85%, indicating that D141 macroporous adsorption resin can effectively purify total alkaloids from CR, and can be applied to industrial production.
ABSTRACT
OBJECTIVE:To study the purification technology of 4 active components from Tripterygium wilfordii by macropo-rous resin. METHODS:The purification abilities of nine macroporous resins(ADS-5,ADS-8,HPD100,HPD300,HPD400, HPD450,HPD700,HPD722 and HPD750) were studied with the adsorption and desorption rates of triptolide,wilforlide,trip-tonide and tripterine as the index by static adsorption and desorption experiments for 4 active components from T. wilfordii,so as to screen optimal macroporous resins. Using transfer rate of active component as index,single factor test was used to investigate the effects of different sampling method,ratio of mixing sample to total resin quantity,ratio of resin to medicinal material,cleaning so-lution(type,amount and cleaning flow rate),diameter- height ratio of resins,eluant(volume,flow rate)on adsorption,so as to determine the optimal elution technology;validation test was also conducted. RESULTS:HPD722 macroporous resin was chosen as adsorption resin;ratio of diameter to height was 1∶10,resin-medicinal material ratio was 1∶2,and ratio of mixing sample to to-tal resin quantity was 1∶10;wet column installing and mixing resin for sample loading were adopted. The macroporous resin was washed with 12 BV 20%ethanol at the rate of 12 BV/h,and then eluted with 12 BV 95%ethanol at the rate of 6 BV/h. The verifi-cation test results showed that the total transfer rate of 4 active components from T. wilfordii was more than 90%(RSD=0.99%, n=3). CONCLUSIONS:The optimized technology is stable and feasible,and suitable for the purification of 4 active components from T. wilfordii.
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Objective:To find the reasons for the low dissolution of clarithromycin tablets and study the interference from filter film adsorption at various time points to explore the appropriate processing approach for dissolution solution of clarithromycin tablets. Meth-ods:Clarithromycin tablets from two different manufacturers were used. The dissolution solution was prepared according to Japanese Orange Book. The dissolution was determined after different processing and the adsorption rate of the filter film was calculated. Re-sults:Totally 14 kinds of filter films were tested with different adsorption for clarithromycin, and the adsorption rate of some kinds of filter films exceeded the prescribed limit. Conclusion:The absorption rate of filter films for clarithromycin can be decreased by boiling the films and using American membranes. The interference from filter film adsorption can be reduced and inhibited by rejecting the first filtrate above 5ml or centrifuging dissolution solution.
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@#BACKGROUND: This study aimed to observe the effect of hemoperfusion (HP) cartridge on different internal environment indicators at different time points in patients with acute blood poisoning and to find alternative indicators for the detection of blood poisoning. METHODS: The levels of internal environment indicators (blood pH, PvCO2, PvO2, blood lactate, potassium, free calcium, bicarbonate, and blood glucose) before and after HP treatment were recorded for patients with acute poisoning at time points of 30 minutes and 120 minutes. After calculating the difference value δ, the statistical software was used to analyze the statistical difference of the influencea-v caused by HP cartridge at two time points. According to the formula, adsorption rate %= —— ×100, thea adsorption rate of each indicator was calculated respectively. RESULTS: The difference of indicators at different time points in inlet and outlet such as blood glucose, free-calcium, and lactate was statistically significant (P<0.05), but the difference in indicators such as pH, PvCO2, PvO2, potassium, sodium, and bicarbonate was not statistical y significant (P>0.05). CONCLUSION: During HP treatment, the indicators of blood glucose, free-calcium and lactate were significantly affected by HP cartridge, and the effect varies with time.
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Objective: To explore the optimal separation of the araloside A from Aralia chinensis by selecting appropriate macroporous resins and to systematically study the factors which affect the separation. Methods: Static and dynamic adsoption-desorption methods were adopted and evaluated for separating efficiency by measuring the concentration of araloside A in A. chinensis with HPLC. Results: Macroporous resin AB-8 had the best separating efficiency when the content in A. chinensis liquid was 0.1 g/mL equivalent to raw material. The volume of drug is 6 BV (resin bed volume) with the adsorption-power 2.5 BV/h and the volume of 50% ethanol as eluant 4 BV with desorption-power 2 BV/h. After the treatment of AB-8 resin, the purity of araloside A could reach 30% and total araloside to 80%. Conclusion: This method is simple and feasible with good effect of separation, which can meet the industrial requirements.
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Bovine pulmonary surfactant was obtained by endotracheal lavage of lungs from newly slaughtered calves followed by differential centrifugation.Lipid extracts of bovine surfactant contained 86.1?2.1% "of phospholipids (X?SD) , 1.8?1.1%of protein and smaller amounts of cholesterol, fatty acids, glycerides and carbohydrate. Phosphatidylcholine(83.4?5.6%)accounted for most of the phospholipids, of which disaturated phosphatidylcholine was 76.0? 4.7% .The physicochemical properties of bovine surfactant were measured with a modified Wilhelmy film balance made by the authors.The minimum surface tension was 2.4?1.5mN/m, stability index was 1.78?0.15, surface compresibility at 10mN/m was 0.022?0.004 m/mN, and surface concentration of phospholipids at 10mN/m was 1.112?0.283 nmol/cm2. The surfactant spread rapidly and could be quickly absorbed to the surface of the water.The results show that the bovine pulmonary surfactant we isolated is able to meet the criteria for investigations of surfactant replacement therapy.