Adsorption and desorption characteristics of flavonoids from white tea using macroporous adsorption resin.

White tea contains the highest flavonoids compared to other teas. While there have been numerous studies on the components of different tea varieties, research explicitly focusing on the flavonoid content of white tea remains scarce, making the need for a good flavonoid purification process for white tea even more important. This study compared the adsorption and desorption performance of five types of macroporous resins: D101, HP20, HPD500, DM301, and AB-8. Among the tested resins, AB-8 was selected based on its best adsorption and desorption performance to investigate the static adsorption kinetics and dynamic adsorption-desorption purification of white tea flavonoids. The optimal purification process was determined: adsorption temperature 25 °C, crude tea flavonoid extract pH 3, ethanol concentration 80 %, sample loading flow rate and eluent flow rate 1.5 BV/min, and eluent dosage 40 BV. The results indicated that the adsorption process followed pseudo-second-order kinetics. Under the above purification conditions, the purity of the total flavonoids in the purified white tea flavonoid increased from approximately 17.69 to 46.23 %, achieving a 2.61-fold improvement, indicating good purification results. The purified white tea flavonoid can be further used for nutraceutical and pharmaceutical applications.

Separation of Flavonoids and Purification of Chlorogenic Acid from Bamboo Leaves Extraction Residues by Combination of Macroporous Resin and High-Speed Counter-Current Chromatography.

Flavonoids are major active small-molecule compounds in bamboo leaves, which can be easily obtained from the bamboo leaves extraction residues (BLER) after the polysaccharides extraction. Six macroporous resins with different properties were screened to prepare and enrich isoorientin (IOR), orientin (OR), vitexin (VI), and isovitexin (IVI) from BLER, and the XAD-7HP resin with the best adsorption and desorption performance was selected for further evaluation. Based on the static adsorption experiments, the experimental results showed that the adsorption isotherm fitted well with the Langmuir isotherm model, and the adsorption process was better explained by the pseudo-second-order kinetic model. After the dynamic trial of resin column chromatography, 20 bed volume (BV) of upload sample and 60% ethanol as eluting solvent was used in a lab scale-up separation, and the results demonstrated that the content of four flavonoids could be increased by 4.5-fold, with recoveries between 72.86 and 88.21%. In addition, chlorogenic acid (CA) with purity of 95.1% was obtained in water-eluted parts during dynamic resin separation and further purified by high-speed countercurrent chromatography (HSCCC). In conclusion, this rapid and efficient method can provide a reference to utilize BLER to produce high-value-added food and pharmaceutical products.

An Effective Chromatography Process for Simultaneous Purification and Separation of Total Lignans and Flavonoids from Valeriana amurensis.

An effective chromatography process was developed and validated for simultaneous purification and separation of total lignans and flavonoids from Valeriana amurensis. The total lignans and flavonoids in Valeriana amurensis extract were prepurified with macroporous resin column chromatography, and the conditions were optimized as follows: 40 mg/mL Valeriana amurensis extract (2.0 g) solution was loaded onto an AB-8 resin column with a diameter-to-height ratio of 1:7, followed by adsorption for 6 h; then, the column was eluted successively with 5 BV water and 10% and 50% ethanol at a flow rate 2 BV/h. The obtained 50% ethanol fraction was further repurified and separated by polyamide resin column chromatography to obtain the total lignans and flavonoids, respectively. The chromatography conditions were optimized as follows: a 50% ethanol fraction (1.0 g) was mixed with 1.0 g polyamide resin and loaded onto a polyamide resin (60-100 mesh) column with a diameter-to-height ratio of 1:3; then, the column was eluted successively with 6 BV water and 40% and 80% ethanol at a flow rate of 4 BV/h. The total lignans and flavonoids were obtained from water and 80% ethanol fraction, respectively. The content and recovery of standard compounds in total lignans and flavonoids were analyzed with HPLC-PDA, and the feasibility of the process was confirmed.

Rubber Seed Oil-Based UV-Curable Polyurethane Acrylate Resins for Digital Light Processing (DLP) 3D Printing.

Novel UV-curable polyurethane acrylate (PUA) resins were developed from rubber seed oil (RSO). Firstly, hydroxylated rubber seed oil (HRSO) was prepared via an alcoholysis reaction of RSO with glycerol, and then HRSO was reacted with isophorone diisocyanate (IPDI) and hydroxyethyl acrylate (HEA) to produce the RSO-based PUA (RSO-PUA) oligomer. FT-IR and 1H NMR spectra collectively revealed that the obtained RSO-PUA was successfully synthesized, and the calculated C=C functionality of oligomer was 2.27 per fatty acid. Subsequently, a series of UV-curable resins were prepared and their ultimate properties, as well as UV-curing kinetics, were investigated. Notably, the UV-cured materials with 40% trimethylolpropane triacrylate (TMPTA) displayed a tensile strength of 11.7 MPa, an adhesion of 2 grade, a pencil hardness of 3H, a flexibility of 2 mm, and a glass transition temperature up to 109.4 °C. Finally, the optimal resin was used for digital light processing (DLP) 3D printing. The critical exposure energy of RSO-PUA (15.20 mJ/cm2) was lower than a commercial resin. In general, this work offered a simple method to prepare woody plant oil-based high-performance PUA resins that could be applied in the 3D printing industry.

Response surface optimization of the water immersion extraction and macroporous resin purification processes of anhydrosafflor yellow B from Carthamus tinctorius L.

In this study,based on a developed high performance liquid chromatographic quantitative method, the suitable extraction and purification conditions of anhydrosafflor yellow B (AHSYB) from safflower were determined by response surface methodology. The optimal water immersion extraction parameters were as follows: liquid to solid ratio of 22:1; extraction temperature of 75 °C; extraction time of 35 min. Under these conditions, the maximum extraction yield of AHSYB reached 0.465%. The aqueous extract was further purified by HPD-300 macroporous resin. The optimum adsorption conditions were: pH 2.8; adsorption flow rate of 1.9 mL/min; solution concentration of 0.06 g/mL. The optimum desorption conditions were: ethanol concentrations of 74%; desorption flow rate of 1.6 mL/min; elution volume of 4.4 BV. Under these conditions, the maximum adsorption ratio and desorption ratio reached 1.095 and 0.906 mg/g, respectively. The content of AHSYB reached 6.83%, which was 2.91 times higher than that before purification. PRACTICAL APPLICATION: The suitable conditions for water immersion extraction and macroporous resin purification of AHSYB are first determined, which facilitates the further utilization of AHSYB as a food and drug.

Preparative Separation of Flavonoids from Goji Berries by Mixed-Mode Macroporous Adsorption Resins and Effect on Aß-Expressing and Anti-Aging Genes.

Flavonoids are the main constituents of Goji berries and have good biological and pharmacological activities. The mixed-mode macroporous adsorption resins (MARs) for purification of flavonoids from Goji berries through computer-assisted calculation of the molecular size of flavonoids and the precise matching of MAR physical and chemical properties was firstly developed in the present study. Ten varieties of MARs with suitable molecular dimensions and polarities were used for investigating the adsorption/desorption behaviors of the flavonoids. Both AUKJ-1 and BWKX-1 showed higher separation efficiency than other MARs and then were mixed in different ratios to constitute a mixed-mode macroporous adsorption resin to obtain the optimal adsorption phase. Under optimal conditions, total flavonoid content of purified flavonoid (p-FLA) extract increased from 0.97% to 36.88% after one purification. The p-FLA extract from Goji berries significantly improved the expression of six genes with anti-aging effects and played an important role in aging-related Alzheimer's disease by down-regulating Aß expression.

Isolation of individual isoflavone species from soybean by solvent extraction followed by the combination of macroporous resin and aluminium oxide separation.

Growing interest in the health benefits of soy isoflavones has led to research in the isolation of individual isoflavone species for further application. Herein, we develop a new strategy to isolate daidzein, genistein, daidzin and genistin in soybean. We investigated the impact of solvents used and the extraction time on the extracted isoflavone contents from soybean. A 30-min extraction with 65% aqueous methanol gave a total isoflavone yield of 345 mg/100 g soybean, the highest value among tested conditions. Further, we proposed a two-stage adsorption/desorption chromatography comprising macroporous resin and aluminium oxide to isolate isoflavone. First, HP-20 resin was used to separate the glucosidic and aglyconic forms of isoflavone, then individual species of isoflavone could be isolated using aluminium oxide by specific retention of 5-hydroxy isoflavone. This process achieved overall high recovery (82-97%) and purity (92-95%) of the four isoflavones, which confirms a high separating efficiency for isoflavones from soybean.

Discoloration of Resin Composites Induced by Coffee and Tomato Sauce and Subjected to Surface Polishing: An In Vitro Study.

BACKGROUND The purpose of this study is to evaluate and compare color stability of 3 resin based restorative materials when immersed into staining media at 0, 3, 30, 45, 60, and 75 days, and to assess the efficacy of surface polishing in reducing possible discoloration. MATERIAL AND METHODS Ninety composite discs were prepared in a custom-made mold (5 mm diameter and 2 mm thick) from 3 different light cured composites (Filtek™ Z250, Harmonize™, and G-aenial). Color differences of all specimens were measured by a spectrophotometer according to the CIE L*a*b* system. After baseline color measurements, 30 discs from each composite group were randomly divided into 3 subgroups of 10 specimens each. Subgroups (n=10) were immersed for 75 days into different staining solutions: coffee, tomato sauce, and distilled water (control). Solutions were changed every week and color measurements were repeated every 15 days. At day 75, color measurements of the specimens were performed before and after surface polishing with aluminum oxide discs. The experimental data were statistically evaluated using repeated measures one-way ANOVA test followed by Tukey's multiple pairwise comparison with a significance level of 5%. RESULTS Of the 3 composites, G-aenial reported the highest color change deviation when immersed into coffee (ΔE=8.674), and tomato sauce (ΔE=7.737) at day 75, followed by Harmonize that also exhibited a significant difference for coffee (ΔE=4.7) and tomato sauce (ΔE=3.8) when compared to distilled water. While Filtek™ Z250 did not show any significant difference between the 3 storage solutions (P>0.05). Only G-aenial had significant color change (P<0.05) after polishing with aluminum oxide discs for all tested samples, whereas Filtek™ Z250 and Harmonize presented no significant difference after surface polishing (P>0.05). CONCLUSIONS Under the tested experimental conditions, Filtek™ Z250, among the 3 resin-based composites, exhibited the highest color stability when subjected to coffee and tomato sauce as well. Whereas, G-aenial presented the highest color deviation when immersed in both staining media. Surface polishing effectively reduced coffee and tomato sauce discolorations for G-aenial's specimens and had no significant effect regarding Filtek™ Z250 and Harmonize.

Enhancing effect of macroporous adsorption resin on gamma-aminobutyric acid production by Enterococcus faecium in whole-cell biotransformation system.

Gamma-aminobutyric acid (GABA) biosynthesis depended to a great extent on the biotransformation characterization of glutamate decarboxylase (GAD) and process conditions. In this paper, the enhancing effect of D101 macroporous adsorption resin (MAR) on the GABA production was investigated based on the whole-cell biotransformation characterization of Enterococcus faecium and adsorption characteristics of D101 MAR. The results indicated that the optimal pH for reaction activity of whole-cell GAD and pure GAD was 4.4 and 5.0, respectively, and the pH range retained at least 50% of GAD activity was from 4.8 to 5.6 and 4.0-4.8, respectively. No substrate inhibition effect was observed on both pure GAD and whole-cell GAD, and the maximum activity could be obtained when the initial L-glutamic acid (L-Glu) concentration exceeded 57.6 mmol/L and 96.0 mmol/L, respectively. Besides, GABA could significantly inhibit the activity of whole-cell GAD rather than pure GAD. When the initial GABA concentration of the reaction solution remained 100 mmol/L, 33.51 ± 9.11% of the whole-cell GAD activity was inhibited. D101 MAR exhibited excellent properties in stabilizing the pH of the conversion reaction system, supplementing free L-Glu and removing excess GABA. Comparison of the biotransformation only in acetate buffer, the GABA production, with 50 g/100 mL of D101 MAR, was significantly increased by 138.71 ± 5.73%. D101 MAR with pre-adsorbed L-Glu could significantly enhance the production of GABA by gradual replenishment of free L-Glu, removing GABA and maintaining the pH of the reaction system, which would eventually make the GABA production more economical and eco-friendly.

Ultrasound-assisted adsorption/desorption for the enrichment and purification of flavonoids from baobab (Adansonia digitata) fruit pulp.

This work described the purification and enrichment of flavonoids from baobab (Adansonia digitata) fruit pulp (BFP) by ultrasound-assisted adsorption/desorption procedure using macroporous resins. Four resins were tested and HPD-500 polar resin exhibited the best adsorption/desorption properties. Based on preliminary experiments and literature reports, the effects of various ultrasonic conditions including high power short time (HPST, 540 W for 5 min), medium power medium time (MPMT, 270 W for 15 min) and low power long time (LPLT, 45 W for 30 min) as well as different temperatures (T = 25-45 °C) on the adsorption of Total Flavonoids Content (TFC) were investigated in comparison with orbital shaking/no sonication (NS). Also, the effect of ultrasound on the desorption capacity and recovery of TFC was determined at different concentrations of ethanol (30-100%). Remarkably, ultrasonic treatment significantly increased the adsorption/desorption capacity and recovery and shortened the equilibrium time. The pseudo-second-order kinetic and Freundlich isotherm models better delineated the adsorption process under ultrasound. Moreover, the adsorption process was both spontaneous and thermodynamically favourable with physical adsorption and multilinear intraparticle diffusion being the predominant mechanisms of the whole process. HPST treatment at 25 °C with 80% ethanol as the desorption solvent most noticeably enhanced the adsorption/desorption of flavonoids and contributed to the highest recovery of TFC, Total Phenolic Content (TPC), and antioxidant capacity in addition to a 5-8-fold reduction in total sugar and acid contents when compared with NS treatment. Moreover, HPLC analysis revealed that the content of nine out of thirteen phenolic compounds from the HPST treatment was the highest, and the individual flavonoids content increased by 2-3-fold compared with the other treatments. Our analyses suggested that ultrasound can be employed as a practical approach to intensify the adsorption and desorption of functional compounds in BFP.

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.

Combined Use of Deep Eutectic Solvents, Macroporous Resins, and Preparative Liquid Chromatography for the Isolation and Purification of Flavonoids and 20-Hydroxyecdysone from Chenopodium quinoa Willd.

: Deep eutectic solvents (DESs) were used in combination with macroporous resins to isolate and purify flavonoids and 20-hydroxyecdysone from Chenopodium quinoa Willd by preparative high-performance liquid chromatography (HPLC). The extraction performances of six DESs and the adsorption/desorption performances of five resins (AB-8, D101, HPD 400, HPD 600, and NKA-9) were investigated using the total flavonoid and 20-hydroxyecdysone extraction yields as the evaluation criteria, and the best-performing DES (choline chloride/urea, DES-6) and macroporous resin (D101) were further employed for phytochemical extraction and DES removal, respectively. The purified extract was subjected to preparative HPLC, and the five collected fractions were purified in a successive round of preparative HPLC to isolate three flavonoids and 20-hydroxyecdysone, which were identified by spectroscopic techniques. The use of a DES in this study significantly facilitated the preparative-scale isolation and purification of polar phytochemicals from complex plant systems.

Fabrication and characterization of polyimide-based 'smooth' titanium nitride microelectrode arrays for neural stimulation and recording.

OBJECTIVE: As electrodes are required to interact with sub-millimeter neural structures, innovative microfabrication processes are required to enable fabrication of microdevices involved in such stimulation and/or recording. This requires the development of highly integrated and miniaturized systems, comprising die-integration-compatible technology and flexible microelectrodes. To elicit selective stimulation and recordings of sub-neural structures, such microfabrication process flow can beneficiate from the integration of titanium nitride (TiN) microelectrodes onto a polyimide substrate. Finally, assembling onto cuffs is required, as well as electrode characterization. APPROACH: Flexible TiN microelectrode array integration and miniaturization was achieved through microfabrication technology based on microelectromechanical systems (MEMS) and complementary metal-oxide semiconductor processing techniques and materials. They are highly reproducible processes, granting extreme control over the feature size and shape, as well as enabling the integration of on-chip electronics. This design is intended to enhance the integration of future electronic modules, with high gains on device miniaturization. MAIN RESULTS: (a) Fabrication of two electrode designs, (1) 2 mm long array with 14 TiN square-shaped microelectrodes (80 × 80 µm2), and (2) an electrode array with 2 mm × 80 µm contacts. The average impedances at 1 kHz were 59 and 5.5 kΩ, respectively, for the smaller and larger contacts. Both designs were patterned on a flexible substrate and directly interconnected with a silicon chip. (b) Integration of flexible microelectrode array onto a cuff electrode designed for acute stimulation of the sub-millimeter nerves. (c) The TiN electrodes exhibited capacitive charge transfer, a water window of -0.6 V to 0.8 V, and a maximum charge injection capacity of 154 ± 16 µC cm-2. SIGNIFICANCE: We present the concept, fabrication and characterization of composite and flexible cuff electrodes, compatible with post-processing and MEMS packaging technologies, which allow for compact integration with control, readout and RF electronics. The fabricated TiN microelectrodes were electrochemically characterized and exhibited a comparable performance to other state-of-the-art electrodes for neural stimulation and recording. Therefore, the presented TiN-on-polyimide microelectrodes, released from silicon wafers, are a promising solution for neural interfaces targeted at sub-millimeter nerves, which may benefit from future upgrades with die-electronic modules.

Separation and Enrichment of Three Coumarins from Angelicae Pubescentis Radix by Macroporous Resin with Preparative HPLC and Evaluation of Their Anti-Inflammatory Activity.

In order to enrich and separate three coumarins (columbianetin acetate, osthole and columbianadin) from Angelicae Pubescentis Radix (APR), an efficient method was established by combining macroporous resins (MARs) with preparative high-performance liquid chromatography (PHPLC). Five different macroporous resins (D101, AB-8, DA-201, HP-20 and GDX-201) were used to assess the adsorption and desorption characteristics of three coumarins. The result demonstrated that HP-20 resin possessed the best adsorption and desorption capacities for these three coumarins. Moreover, the adsorption dynamics profiles of three coumarins were well fitted to the pseudo second order equation (R2 > 0.99) for the HP-20 resin. The adsorption process was described by the three isotherms models including Langmuir (R2 > 0.98, 0.046 ≤ RL ≤ 0.103), Freundlich (R2 > 0.99, 0.2748 ≤ 1/n ≤ 0.3103) and Dubinin Radushkevich (R2 > 0.97). The contents of columbianetin acetate, osthole and columbianadin in the product were increased 10.69-fold, 19.98-fold and 19.68-fold after enrichment, respectively. Three coumarins were further purified by PHPLC and the purities of them reached above 98%. Additionally, the anti-inflammatory effects of these three coumarins were assessed by Lipopolysaccharide (LPS)-induced RAW 264.7 cells. It was found that the production of NO and MCP-1 was obviously inhibited by three coumarins. Columbianetin acetate, osthole and columbianadin could be used as potentially natural anti-inflammatory ingredients in pharmaceutical products. It was concluded that the new method combining MARs with PHPLC was efficient and economical for enlarging scale separation and enrichment of columbianetin acetate, osthole and columbianadin with anti-inflammatory effect from the APR extract.

CdSSe nanowire-chip based wearable sweat sensor.

BACKGROUND: Sweat, as an easily accessible bodily fluid, is enriched with a lot of physiological and health information. A portable and wearable sweat sensor is an important device for an on-body health monitoring. However, there are only few such devices to monitor sweat. Based on the fact that sweat is mainly composed of moisture and salt which is much more abundant than other trace ions in sweat, a new route is proposed to realize wearable sweat sensors using CdSSe nanowire-chips coated with a polyimide (PI) membrane. RESULTS: Firstly, the composition-graded CdS1-xSex (x = 0-1) nanowire-chip based sensor shows good photo-sensitivity and stress sensitivity which induces linear humidity dependent conductivity. This indicates good moisture response with a maximum responsivity (dI/I) 244% at 80% relative humidity (RH) even in the dark. Furthermore, the linear current decrease with salt increase illustrates the chip sensor has a good salt-sensing ability with the best salt dependent responsivity of 80%, which guarantees the high prediction accuracy in sweat sensing. The sensor current is further proven to nonlinearly correlate to the amount of sweat with excellent stability, reproducibility and recoverability. The wearable sweat sensor is finally applied on-body real-time sweat analysis, showing good consistence with the body status during indoor exercise. CONCLUSIONS: These results suggest that this CdSSe nanowire-chip based PI-coated integrated sensor, combined with inorganic and organic functional layers, provides a simple and reliable method to build up diverse portable and wearable devices for the applications on healthcare and athletic status.

A practicable strategy for enrichment and separation of four minor flavonoids including two isomers from barley seedlings by macroporous resin column chromatography, medium-pressure LC, and high-speed countercurrent chromatography.

Separation of minor compounds especially with similar polarities and structures from complex samples is a challenging work. In the present study, an efficient method was successfully established by macroporous resin column chromatography, medium-pressure liquid chromatography, and high-speed countercurrent chromatography for separation of four minor flavonoids from barley seedlings. Macroporous resin column chromatography and medium-pressure liquid chromatography were used for enrichment of these four flavonoids. High-pressure liquid chromatography analysis showed the total content of these four flavonoids increased from 2.2% in the crude extract to 95.3% in the medium-pressure liquid chromatography fraction. It was indicated that the combination of macroporous resin column chromatography and medium-pressure liquid chromatography could be a practicable strategy for enrichment of minor compounds from complex sample. Then, high-speed countercurrent chromatography was employed for separation of these four flavonoids using ethyl acetate/n-butanol/water (0.1% glacial acetic acid) (4:1:5, v/v/v) as solvent system. As a result, four flavonoids including two isomers with purities higher than 98% were obtained. Interestingly, two flavonoids existing in one high-pressure liquid chromatography peak were also successfully separated. All these indicated high-speed countercurrent chromatography had great potential for separation of compounds with similar structures and polarities. This study provides a reference for efficient enrichment and separation of minor compounds from complex sample.

A systematic study and effect of PLA/Al2O3 nanoscaffolds as dental resins: mechanochemical properties.

One of the major and important challenges in dental composite resin and restoration is the mechanical performance and property of materials. Nanotechnology can produce nanoscale materials that are used in dentistry to help stabilize and strengthen the dentistry. In this work, we study the synthesis and characterization of PLA/Al2O3 nanoscaffold in different conditions such as concentration, temperature, pH, microwave power and irradiation time. PLA/Al2O3 nanoscaffolds were prepared by a micelle-assisted hydrothermal method. Durability, stability and biodegradable nature of nanopolymers have created the much-applied potential for using this structures in many fields such as dental resin composites. Products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transition electron microscopy (TEM), Fourier transformed infrared spectrum (FT-IR), Dynamic light scattering (DLS) and atomic force microscopy (AFM). The synthesis factors were designed by Taguchi technique to control the process systematically. It was found that the intermolecular crosslinks between PLA and Al2O3 nanoparticles cause significant improves in the mechanical properties of PLA/Al2O3 nanoscaffold as dental nanocomposites. The flexural strength (88.0 MPa), modulus (7.5 GPa) and compressive strength (157.2 MPa) were calculated for PLA/Al2O3 nanoscaffolds loaded in Heliomolar Flow composite resins at 80 ppm (wt) concentration.

Enrichment and Purification of the Bioactive Flavonoids from Flower of Abelmoschus manihot (L.) Medic Using Macroporous Resins.

Flower of Abelmoschus manihot (FAM) is clinically effective to treat chronic kidney disease (CKD) with a relatively high dosage. To improve the efficacy and the compliance of patients, macroporous resins were adopted to enrich and purify flavonoids from FAM, which are thought to be the major renal protective constituents in FAM. After screening six different kinds of macroporous resins, HPD-100 was selected for its great adsorption and desorption capacity. Then, orthogonal design tests were used to optimize parameters in the processes of impurity removal and flavonoids of FAM desorption on column chromatogram. Moreover, process scale-up was performed, and purification effects maintained after amplification. After purification, the content of seven main flavonoids in the product increased from 8.29% to 51.43%. Protective and anti-inflammatory effects of crude extract and the flavonoid component of FAM after purification were investigated on the adriamycin-damaged HK-2 cells and lipopolysaccharide-stimulated Raw 264.7 cells models. Both bioactivities were improved greatly after purification for these two cell models. Therefore, the purification process had enriched the main bioactive constituents with potential alleviating kidney injury activities. The flavonoid component of FAM is worthy of being developed as an improved remedy for CKD with better patients' compliance.

Simultaneous Separation and Purification of Five Polymethoxylated Flavones from "Dahongpao" Tangerine (Citrus tangerina Tanaka) Using Macroporous Adsorptive Resins Combined with Prep-HPLC.

In this study, a preparative separation method was established to simultaneously isolate the polymethoxylated flavones (PMFs) from the peel of "Dahongpao" tangerine using macroporous adsorptive resins (MARs) combined with prep-HPLC. The total PMFs were enriched using MARs to remove most sugars, water-soluble pigments, and flavanones, and the eluents obtained were analyzed by ultra-performance liquid chromatography (UPLC) to determine the PMF composition. The separation and purification of PMFs were carried out by using a mass spectrometry-guided prep-HPLC with a gradient elution of acetonitrile-water (v/v), simultaneously. The purity of these PMFs was determined by UPLC, and their chemical structures were confirmed by electrospray ionization mass spectrometry (ESI-MS-MS), ultraviolet (UV), and nuclear magnetic resonance (NMR). Using the present method, five PMFs, including 5,6,7,4'-tetramethoxyflavone (1), nobiletin (2), tangeretin (3), sinensetin (4), and 5-hydroxy-6,7,8,3',4'-pentamethoxyflavone (5), can be purified simultaneously, and the purity of the compounds obtained were 95.3%, 99.7%, 99.5%, 98.9%, and 98.1%, respectively. The method reported here is simple, rapid, and efficient, and it can be used to separate PMFs from citrus fruit peels and, potentially, other plant materials.

Separation of Protactinium Employing Sulfur-Based Extraction Chromatographic Resins.

Protactinium-230 ( t1/2 = 17.4 d) is the parent isotope of 230U ( t1/2 = 20.8 d), a radionuclide of interest for targeted alpha therapy (TAT). Column chromatographic methods have been developed to separate no-carrier-added 230Pa from proton irradiated thorium targets and accompanying fission products. Results reported within demonstrate the use of novel sulfur bearing chromatographic extraction resins for the selective separation of protactinium. The recovery yield of 230Pa was 93 ± 4% employing a R3P═S type commercially available resin and 88 ± 4% employing a DGTA (diglycothioamide) containing custom synthesized extraction chromatographic resin. The radiochemical purity of the recovered 230Pa was measured via high purity germanium γ-ray spectroscopy to be >99.5% with the remaining radioactive contaminant being 95Nb due to its similar chemistry to protactinium. Measured equilibrium distribution coefficients for protactinium, thorium, uranium, niobium, radium, and actinium on both the R3P═S type and the DGTA resin in hydrochloric acid media are reported, to the best of our knowledge, for the first time.