Highly selective separation and purification of chicoric acid from Echinacea purpurea by quality control methods in macroporous adsorption resin column chromatography.

Chicoric acid is the main phenolic active ingredient in Echinacea purpurea (Asteraceae), best known for its immune-enhancing ability, as well as used as a herbal medicine. To achieve further utilization of medicinal ingredients from E. purpurea, an efficient preparative separation of chicoric acid was developed based on macroporous adsorption resin chromatography. The separation characteristics of several different typical macroporous adsorption resins were evaluated by adsorption/desorption column experiments, and HPD100 was revealed as the optimal one, which exhibited that the adsorbents fitted well to the pseudo-second-order kinetics model and Langmuir isotherm model, and the optimal process parameters were obtained. The breakthrough curves could be predicted and end-point could be determined early. Besides, the optimal elution conditions of chicoric acid can be achieved using the quality control methods. As a result, the purity of chicoric acid was increased 15.8-fold (from 4 to 63%) after the treatment with HPD100. The process of the enrichment and separation of chicoric acid is considerate, because of its high efficiency and simple operation. The established separation and purification method of chicoric acid is expected to be valuable for further utilization of E. purpurea according to product application in pharmaceutical fields in the future.

Efficient direct preparation of antifungal Alteramide B from Lysobacter enzymogenes fermentation broth by macroporous resin adsorption.

Alteramide B (ATB) is an antifungal metabolite produced by Lysobacter enzymogenes. However, its separation method has not been explored. This study attempted to directly adsorb ATB from fermentation broth using macroporous adsorption resins (MARs) NKA resin exhibited better adsorption as well as desorption capacities. The static and dynamic adsorption characteristics were assessed to determine the following optimal separation conditions: initial fermentation broth with a pH of 12.0, 2 BV/h flow rate, 8 BV loading volume, and 6 BV 80% aqueous ethanol for elution. After a single treatment, ATB content in the final product was higher by 4.51-fold (i.e, from 12.72 ± 1.21% to 57.35 ± 3.46%), resulting in a recovery yield of 86.20 ± 4.47%. In addition, NKA resin showed superior reusability within eight cycles of adsorption/desorption. The developed method is thus a simple, efficient, and economical process for ATB separation.

Efficient enrichment of total flavonoids from Pteris ensiformis Burm. extracts by macroporous adsorption resins and in vitro evaluation of antioxidant and antiproliferative activities.

The aim of this work is to develop an efficient and economical method for the enrichment of total flavonoids from Pteris ensiformis Burm. extracts. Resin screening, adsorption kinetics, adsorption isotherms and thermodynamics were successively researched prior to the dynamic adsorption and desorption tests. NKA-II resin was chosen as the best adsorbent, and the adsorption data were best described by the pseudo-second-order kinetics model and Langmuir isotherm model. The optimum enrichment conditions were as follows: for adsorption the total flavonoids concentration, flow rate and volume of sample were 1.84 mg/mL, 2 BV/h and 5 BV, respectively, and for desorption the flavonoids-loaded NKA-II resin column was desorbed by 7 BV of 50% ethanol at a rate of 2 BV/h. The product had a 6.63-fold higher total flavonoids content than crude extracts, and the recovery yield of total flavonoids was 80.65%. Furthermore, flavonoids-enriched extracts exhibited higher in vitro scavenging activity against superoxide anion radical and hydroxyl radical than crude extracts. In addition, higher antiproliferative activity of flavonoids-enriched extracts against MCF-7 and HepG-2 cell lines was also found as compared to the crude extracts. The developed method is appropriate for large-scale enrichment of total flavonoids from Pteris ensiformis Burm. extracts in the food and pharmaceutical industries.

Design of an enhanced SAT using the graphene-MAR mixture for the removal of 17ß-E2 at a demonstration site of Qianjin farm in China.

An adsorption-enhanced soil aquifer treatment (SAT) system was designed to reduce the level of estrogens below the threshold stipulated by the standards. The 17ß-E2 adsorption by graphene and MARs (H103) was investigated and an optimum amount of graphene and MARs in the mixture was determined using the linear programming. The kinetics and isotherm characteristics of both adsorbents were well described by the Lagergren pseudo-second order and the Freundlich model, respectively. The 17ß-E2 adsorption on graphene and H103 was 88% and 70.37%, and the high temperature was beneficial to the 17ß-E2 adsorption on graphene while the thermodynamic behaviors of H103 were in direct contrast to that of graphene. The study found that the maximum economic benefits could be achieved when the mass of graphene and H103 in the mixture is 2.79 g and 13.20 kg, respectively.

Simultaneous Enrichment and Separation of Four Flavonoids from Zanthoxylum bungeanum Leaves by Ultrasound-Assisted Extraction and Macroporous Resins with Evaluation of Antioxidant Activities.

Quercitrin, hyperoside, rutin, and afzelin are the dominant flavonoids compounds from Zanthoxylum bungeanum leaves, and they play major roles in the antioxidant activity. Macroporous adsorption resin (MAR) treatment, a simple, low-cost and efficient method, was combined with ultrasound-assisted extraction (UAE) to enrich and purify these four flavonoids from Z. bungeanum leaves efficiently. The optimal conditions for UAE based on Response Surface Methodology (RSM) were determined to be an ethanol concentration of 60%, leaves size of 40 mesh, temperature of 50 °C and ultrasonic power of 400 W with four flavonoids contents of 120.84 mg/g. After the extraction process, five kinds of MARs (D4020, D-101, NKA-9, AB-8, and X-5) were tested through static adsorption/desorption to enrich and purify the ultrasonic-assisted extracts, and D-101 was selected as the most suitable resin. The optimal adsorption conditions were 5 bed volumes (BV) of sample solution with an initial concentration of 7.5 mg/mL and pH 5.0. Meanwhile, the optimal desorption parameters were 5 BV each of deionized water and 30% ethanol, then 10 BV 70% ethanol, and a flow rate of 2 BV/hr. Under the optimized conditions, the contents of quercitrin, hyperoside, rutin, and afzelin increased by 276.39%, 187.46%, 221.81%, and 288.45%, respectively, and the recovery yields were 85.47%, 73.53%, 81.35%, and 65.06%. In addition, laboratory preparative-scale separation indicated that the preparative separation of four flavonoids was feasible and easy. Moreover, the antioxidant activities of the purified products were significantly increased after enrichment. In conclusion, all of the results indicated that these methods are highly efficient, low cost, environmentally friendly and easy to scale up. PRACTICAL APPLICATION: This study provided an environmentally friendly, rapid, and highly productive method for the extraction and purification of four active compounds from Zanthoxylum bungeanum leaves. The results can be used for the utilization of Z. bungeanum leaves as a kind of food supplement in an industrial setting.

Absorption and desorption behaviour of the flavonoids from Glycyrrhiza glabra L. leaf on macroporous adsorption resins.

The kinetics of adsorption and desorption behaviours of five macroporous resins for enriching flavonoids from Glycyrrhizaglabra L. leaf were investigated. All five resins showed similar and effective adsorption and desorption properties. A pseudo-second-order kinetics model was suitable for evaluating the whole adsorption process. Additionally, two representative resins (XAD-16 and SP825) were chosen for adsorption thermodynamics study. The adsorption of the representative resins was an exothermic and physical adsorption process. Further column chromatography of XAD-16 and SP825 showed that the total flavonoids (from 16.8% to 55.6% by XAD-16 and to 53.9% by SP825) and pinocembrin (from 5.49% to 15.2% by XAD-16 and to 19.8% by SP825) were enriched in 90% ethanol fractions. Meanwhile, the antioxidant capacities and nitrite-scavenging capacities were 2-3times higher than those of the crude extract. The fractions with high flavonoid and pinocembrin contents could be used as biologically active ingredients in functional food.

Separation and purification of amygdalin from thinned bayberry kernels by macroporous adsorption resins.

To utilize the low-value thinned bayberry (Myrica rubra Sieb. et Zucc) kernels (TBKs) waste, an efficient method using macroporous adsorption resins (MARs) for separation and purification of amygdalin from TBKs crude extracts was developed. An aqueous crude sample was prepared from a methanol TBK extract, followed by resin separation. A series of MARs were initially screened for adsorption/desorption of amygdalin in the extract, and D101 was selected for characterization and method development. The static adsorption data of amygdalin on D101 was best fitted to the pseudo-second-order kinetics model. The solute affinity toward D101 at 30 °C was described and the equilibrium experimental data were well-fitted to Langmuir and Freundlich isotherms. Through one cycle of dynamic adsorption/desorption, the purity of amygdalin in the extract, determined by HPLC, increased about 17-fold from 4.8% to 82.0%, with 77.9% recovery. The results suggested that D101 resin effectively separate amygdalin from TBKs.

Stability of nitrofuran residues during honey processing and nitrofuran removal by macroporous adsorption resins.

There is increasing concern that the presence of antibiotics such as nitrofurans in animal-derived food products is harmful to human. This study originally assessed the effects of different honey processing steps on the stabilities of four nitrofuran metabolites (3-amino-2-oxazolidone, 1-aminohydantonin, semicarbazide and 3-amino-5-morpholinomethyl-2-oxazolidone). Macroporous adsorption resins (MARs) were evaluated for the removal of these residues. Nitrofuran metabolites were analysed by LC-MS/MS after each processing step. The results revealed that honey processing reduced nitrofuran metabolites in honey and the total loss was from 56.6% to 90.4%. Furthermore, LS-901 was the optimum MAR with adsorption rates of 69.9-91.8% for four metabolites. After removing nitrofuran metabolites, the honey could be safely used as winter feed for honeybees.

Research on separation and purification of extract from Dracocephalum moldevica with macroporous resins / 中草药

Objective: To investigate the technology for the separation and purification of extract in Dracocephalum moldevica (EDM) by macroporous resin. Methods: Static and dynamic adsorption-desorption were used to select the best one from seven different type macroporous resins; With the content of total flavonoids, tilianin, luteolin-7-O-β-D-glucuronide, and rosmarinic acid as indexes, the purification technology parameters of EDM were optimized. Results: HPD600 resin showed the best purifying profile, its optimum technology conditions were as follows: The optimum concentration of the sample liquid was 0.08 g/mL equivalent to raw material, the resin column diameter-height ratio was 1:9, the amount of used adsorption was 0.32 g dried medicinal herb/mL resin, sample flow rate was 1.5 BV/h, and adsorption time was 12 h. In the course of elution, the resin column chromatography was eluted with 6 BV of 70% ethanol after removing impurities with 4 BV of water by flow rate of 1.5 BV/h. The contents of total flavonoids, tilianin, luteolin-7-O-β-D-glucuronide, and rosmarinic acid were more than 53%, 5.5%, 4.7%, and 2.5%. Conclusion: Macroporous resin HPD600 is suitable to separate and purify EDM.

Study on Adsorptive Property of Total Flavones from Psidium guajava Leaf with FL-1 Macroporous Adsorption Resins / 中国中医药信息杂志

Objective To evaluate the performance of FL-1 macroporous absorption resin for absorption of total flavonoids from Psidium guajava leaf.Methods The concentration of total flavones in Psidium guajava leaf was determined by ultraviolet spectrophotometry and the absorption behavior of FL-1 macroporous adsorption resins to total flavones in Psidium guajava leaf was examined for the adsorption capacity and the volume of solution loaded.Results Optimal absorption of total flavonoids was achieved with the sample:total flavonoids concentration in the solution of 13.22 mg/mL,the ratio of total flavonoids concentration and macroporous adsorption resin was 1∶4,washing with 70% ethanol at the flow velocity of 2 BV/h.Conclusion FL-1 Macroporous absorption resin can be well applicable for enrichment of total flavonoids in Psidium guaijava leaf.

Adsorption and desorption of lycopene and ?-carotene using three macoroporous adsorption resins / 中草药

Object To study the separation effect of three macoroporous resins for lycopene and ? carotene, in order to optimize the suitable one. Methods The performances of adsorption and desorption for lycopene and ? carotene with three macroporous resins D4020, X 5 and AB 8 were compared, and adsorption dynamics process of resins was studied. Results The adsorptive capacities of X 5 resin for lycopene and ? carotene are the most, they are 7 44 and 11 2 mg/g, respectively. Desorption ratio of X 5 resin is the highest. Conclusion X 5 resin is an ideal adsorbent for lycopene and ? carotene extraction.