Five new compounds from the stems of Ephedra equisetina.

Five new compounds were identified from the stems of Ephedra equisetina Bunge. Their structures were elucidated by spectroscopic methods, involving UV, IR, NMR spectrum and HRESIMS analyses. The absolute configuration of compound 2 was proved by comparing their experimental and calculated ECD spectrum. The vitro bioactive assay of all compounds suggested that compound 1, 3, 4, 5 and 6 may have potential anti-asthmatic activities.

Porous phenolic resin regulated by alcohol-based deep eutectic solvent for selective extraction and separation of tanshinones from Salvia miltiorrhiza.

Deep eutectic solvents (DES), regarded as promising green solvents, have gained attention due to their distinctive properties, particularly in analytical chemistry. While the use of DES in solvent extraction and separation has been extensively studied, its application in the synthesis of adsorbents has just begun. Phenolic resin, with its polyhydroxy structure and stable spherical morphology, could serve as an effective as adsorbents for enrichment of active ingredients in herbal medicine. Designing adsorbents with high selectivity and adsorption capacity presents a critical challenge in the enrichment of active ingredients in herbal medicine. In this study, alcohol-based DESs were employed as regulators of morphology and structure instead of organic solvents, facilitating the creation of polyhydroxy structure, adjustable pores and high specific surface areas. The resulting DES-regulated porous phenolic resin demonstrated enhanced extraction and separation capacity for active ingredients compared to conventional spherical phenolic resin owing to the alcohol-based DES offering more interaction modes with the analytes.

Computational simulation-assisted design and experimental verification of molecularly imprinted polymers for selective extraction of chlorogenic acid.

Chlorogenic acid (CGA) is an active ingredient in honeysuckle with a broad-spectrum of antibacterial activity, suppressing tumor growth and other pharmacological effects. However, it is susceptible to damage during traditional extraction and separation processes. Therefore, developing selective and efficient extraction methods of CGA is essential. Based on computational molecular simulations, a reliable and efficient molecularly imprinted polymers (MIPs) were successfully developed for selective extraction of CGA. MIPs and non-molecularly imprinted polymers (NIPs) were synthesized using a precipitation polymerization method, employing three different functional monomers: [methacrylic acid (MAA), 4-vinylpyridine (4-VP), and methyl methacrylate (MMA)], with CGA serving as the template molecule. To simulate the polymers and predict the optimal ratio between the template and functional monomer, the computational studies and adsorption performance experiments were carried out. The adsorption characteristics and thermal stability of polymers were evaluated by isothermal adsorption, adsorption kinetics, selective adsorption and thermogravimetric analysis, aiming to obtain the MIPs with specific recognition and selectivity for CGA. When the molar ratio of template CGA to functional monomer 4-VP was 1:8, the prepared MIPs was found to have the maximum adsorption capacity (14.85 mg g-1) and the highest imprinting factor (1.74) at the CGA concentration of 100 mg L-1. These results were consistent with those obtained by computational molecular simulation. This study not only provides good guidance for developing separation materials for extracting CGA from natural plants but also inspires the application of computer simulation and molecular docking techniques in the preparation of specific MIPs materials.

[Application of high-speed counter current chromatography in extraction and separation of alkaloids in natural products].

Alkaloids, widespread in plants, have a series of pharmacological activities and have been widely used to treat various diseases. Because alkaloids are usually presented in multicomponent mixtures and are deeply low in content, they are very difficult to extract and separate by traditional methods. High-speed counter current chromatography(HSCCC) is a kind of liquid-liquid chromatography without solid support phase, which has the advantages of large injection volume, low cost, and no irreversible adsorption. Compared with the traditional methods of extraction and separation of alkaloids, HSCCC can ensure the separation of many different alkaloids at one time, with a high recovery and large amount. In this paper, the advantages and disadvantages of HSCCC compared with traditional separation methods were discussed and the solvent system and elution mode of HSCCC used to separate alkaloids in recent years were summarized by referring to the relevant literature to provide some references for the separation of alkaloids by HSCCC.

Extraction and purification of grape seed polysaccharides using pH-switchable deep eutectic solvents-based three-phase partitioning.

T-butanol is widely used in three-phase partitioning (TPP), which is harmful to the environment. pH-switchable deep eutectic solvents (DESs) can be used as recyclable alternatives to t-butanol. This study aimed to construct DES-based TPP for extracting and purifying grape seed polysaccharides (GSP). The main influence factors were investigated in single-factor experiments. DES-1 (dodecanoic acid: octanoic acid = 1:1)-based extraction was screened, and the extraction yield reached the maximum of 98.04 mg/g under the optimal conditions. Furthermore, DES can be recycled, only suffering a small loss capacity in extraction yield after 25 cycles. Most importantly, the extractability of DES could be completely recovered after switching and regeneration. The molecular weight of obtained GSP was 60 kDa, and the main monosaccharides of GSP included mannose, glucose, galactose, and arabinose. This study provides an efficient and sustainable method for the extraction of bioactive substances.

Simultaneous recycling of Si and Ti from diamond wire saw silicon powder and Ti-bearing blast furnace slag via reduction smelting: An investigation of the effects of refractories on recycling.

The industrial wastes diamond wire saw silicon powder (DWSSP) and Ti-bearing blast furnace slag (TBFS) are important Si and Ti secondary resources, respectively. During the industrial application of recycling DWSSP and TBFS via reduction smelting, the refractories can dissolve into the molten slag, which can change the composition of the slag and influence the extraction of Si and Ti. Unfortunately, few studies on the reduction smelting of DWSSP and TBFS related to refractories have been reported, making such studies urgently needed. Therefore, the main purpose of this work was to reveal the dissolution mechanism of refractories (alumina and magnesia bricks) and the effect of refractory dissolution on Si-Ti alloy preparation. The results show that during the reduction smelting, the dissolution of alumina and magnesia bricks changed from direct dissolution into the molten slag to indirect dissolution, and the amount of magnesia bricks dissolved was less than that of aluminum bricks. Al3+ (aluminum brick) entering the slag could replace Si4+ in [SinO2n] to form [AlxSin-xO2n]x-, increasing the viscosity of the slag. The O2- (magnesia brick) entering the slag could dissociate [AlxSin-xO2n]x-, decreasing the viscosity of the slag. Therefore, compared with alumina bricks, magnesia bricks can promote slag-alloy separation and improve the extraction ratios of Ti and Si. In the case of magnesia bricks, the maximum reduction ratio of TiO2 was 98.4 %, and the maximum extraction ratio of Si was 95.8 %. This work provides essential experimental data for the Si-Ti alloys prepared via recycling DWSSP and TBFS.

Application of high-speed counter current chromatography in extraction and separation of alkaloids in natural products / 中国中药杂志

Alkaloids, widespread in plants, have a series of pharmacological activities and have been widely used to treat various diseases. Because alkaloids are usually presented in multicomponent mixtures and are deeply low in content, they are very difficult to extract and separate by traditional methods. High-speed counter current chromatography(HSCCC) is a kind of liquid-liquid chromatography without solid support phase, which has the advantages of large injection volume, low cost, and no irreversible adsorption. Compared with the traditional methods of extraction and separation of alkaloids, HSCCC can ensure the separation of many different alkaloids at one time, with a high recovery and large amount. In this paper, the advantages and disadvantages of HSCCC compared with traditional separation methods were discussed and the solvent system and elution mode of HSCCC used to separate alkaloids in recent years were summarized by referring to the relevant literature to provide some references for the separation of alkaloids by HSCCC.

Modern Research Progress of Polyphyllin Ⅰ： A Review / 中国实验方剂学杂志

Paridis Rhizoma， a traditional valuable Chinese herbal medicine， has the functions of clearing heat and removing toxin， relieving edema and pain， cooling liver and calming convulsion， which can be used to treat various diseases such as mumps， abscess， burn， bleeding， and tumor. It has been used in folk medicine for a long time and is the main raw material of various Chinese patent medicines such as Gongxuening Capsules and Yunnan Baiyao. Polyphyllin Ⅰ， an isospirostanol saponin and one of the main active components in Paridis Rhizoma， is distributed in the rhizome， pericarp， and leaves of Paris polyphylla. With high polarity， polyphyllin Ⅰ is mainly extracted by n-butanol extraction and macroporous adsorption resin chromatography， separated by silica gel column chromatography and preparative high performance liquid chromatography， and purified with the combination of methods. With anti-tumor， anti-inflammatory， antibacterial， and anti-virus effects， it is generally employed to treat liver cancer， lung cancer， gastric cancer and other cancers as well as arthritis， influenza， sore toxin， and bacterial infection. However， polyphyllin Ⅰ may cause stomach irritation， hemolysis， liver damage， kidney damage， heart damage， and other adverse reactions. Pharmacokinetic studies show that it has problems such as low bioavailability and poor intestinal absorption and permeability， which affect the clinical application of polyphyllin Ⅰ. This paper summarizes the research on the plant sources， extraction and separation methods， pharmacological effects， adverse reactions， and pharmacokinetics of polyphyllin Ⅰ in recent years， which is expected to provide a reference for the rational clinical application and other in-depth research work of polyphyllin Ⅰ.

Study on chemical constituents of Hippocampus trimaculatus Leach / 药学实践杂志

Objective To study the chemical constituents of Hippocampus trimaculatus Leach. Methods After extracted with ethanol, Hippocampus trimaculatus Leach was isolated and purified by silica gel column chromatography, Sephadex LH-20 gel column chromatography, and reversed-phase C18 column chromatography. The structures of compounds were identified by physical and chemical properties, spectral data and literature comparison. Results Eight compounds were isolated from Hippocampus trimaculatus Leach and identified as L-phenylalanine (1), alanine (2), inosine (3), cholesterol (4), N-acetyltyramine (5), uracil (6), D-mannitol (7), tetrodoine (8), respectively. Conclusion Compounds 5, 7, 8 are isolated from Hippocampus trimaculatus Leach for the first time.

A new flavonoid glycoside from Epimedium sagittatum / 药学学报

Fourteen flavonoids were isolated and purified from Epimedium sagittatum by various chromatography techniques such as macroporous adsorbent resin, silica gel, ODS, Sephadex LH-20, HW-40C and semi-preparative HPLC. Their structures were identified by analysis of physicochemical properties and spectral data, and determined as 3′-hydroxy-baohuoside-Ⅱ (1), huazhongilexone-7-O-β-D-glucopyranoside (2), kaempferol-3-O-α-L-rhamnoside (3), baohuoside-Ⅱ (4), icariside-Ⅱ (5), kaempferol 3,7-di-O-α-L-rhamnopyranoside (6), (+)-aromadendrin (7), kaempferol 3-O-(2-O-β-D-apiofuranosyl)-α-L-rhamnopyranoside (8), sagittatoside A (9), 2″-O-rhamnosyl icariside-II (10), apigenin-7-O-β-D-glucoside (11), quercetin 3-O-β-D-apiofuranoyl-(1→2)-α-L-rhamnopyranoside (12), kaempferol (13), icariin (14). Among them, compound 1 is a new compound, while compounds 2, 6-8, 11, and 12 were isolated from E.sagittatum for the first time.

A Critical Review of Emerging Hydrophobic Deep Eutectic Solvents' Applications in Food Chemistry: Trends and Opportunities.

Due to their low cost, biodegradability, and ease of preparation, deep eutectic solvents (DESs) are considered promising green alternatives to conventional solvents, as exploiting green solvents has been a research focus for achieving sustainable development goals. Most DESs in published studies are hydrophilic. On the other hand, the DES's hydrophilicity restricts its practical applicability to just polar molecules, which is a vital disadvantage to this extractant. Hydrophobic DES (HDES) has been developed as a new extractant adept at extracting nonpolar inorganic and organic compounds from aqueous systems. Although there has been little research on HDESs (HDES publications account for <10% of DES), specific intriguing applications have been discovered, requiring investigation and comparisons. As a result, this review covers the applications of emerging HDES in detecting pesticide residues, food additives, contaminants in food packaging, heavy metals, separation and extraction processes in food. According to the available literature, HDESs have the potential to overcome the limitations of hydrophilic DESs and be used in a broader range of applications in food with greater efficiency, which has received little attention. HDES is expected to substitute a lot of harmful organic extractants used for analytical reasons (food chemistry) in the future. Besides, the limitations of HDES were reviewed, and future studies were provided. This will serve as a reference for green chemistry advocates and practitioners in food science who want to minimize pollution and improve efficiency and benefit from the further development of HDESs.

Identification of Polysaccharides From Dipsacus asperoides and Their Effects on Osteoblast Proliferation and Differentiation in a High-Glucose Environment.

Polysaccharides (DAI-1 and DAI-2) from Dipsacus asperoides (D. asperoides) were obtained using mixed-bed ion exchange resin and Sephadex G-50 column chromatography following which their properties, structures, and activities were investigated. The results showed that DAI-1 and DAI-2 were homogeneous in nature, with glucose the only constituent, and had molecular masses of 17 and 4 kDa, respectively. Methylation analysis indicated that the backbones of DAI-1 and DAI-2 were mainly composed of (1→6)-linked glucose residues. DAI-1 possessed a small number of side chains and a branch point of (1→3, 6)-glucose, while DAI-2 lacked branching. Activity assays demonstrated that exposing osteoblasts to different DAI-1 concentrations (25, 50, or 100 µg/mL) in a high-glucose environment induced cell proliferation and led to a significant increase in bone morphogenetic protein 2 (BMP-2) and runt-related transcription factor 2 (Runx2) expressions at both the mRNA and protein levels. Moreover, DAI-1 treatment significantly increased alkaline phosphatase (ALP) and osteocalcin (OCN) activities in osteoblasts. Combined, our results suggested that DAI-1 may promote osteoblast proliferation and differentiation in a high-glucose environment.

A new diterpenoid acid from the rosin of Pinus kesiya var. langbianensis (A.Chev.) Gaussen ex Bui / 药学学报

One undescribed diterpenoid acid and six compounds were isolated from the 95% ethanol fraction of Pinus kesiya var. langbianensis (A.Chev.) Gaussen ex Bui resin by using various chromatographic methods, including MCI Gel, Sephadex LH-20, ODS, silica gel and semi-preparative HPLC. The planar structures were identified by spectroscopy methods (1D, 2D NMR, UV, IR, MS, etc.), and the absolute configuration of the new compound was determined by ECD calculation. Compound 1 is a new compound, and compounds 2, 5-7 were isolated from Pinus kesiya var. langbianensis (A.Chev.) Gaussen ex Bui for the first time.

Tannic acid-directed synthesis of magnetic and boronic acid-functionalized metal-organic frameworks for selective extraction and quantification of catecholamines in human urine.

A novel magnetic borate-functionalized metal-organic framework nanocomposite was designed and fabricated for selective enrichment of catecholamines from human urine. Firstly, the polytannic acid (PTA) layer with natural low-cost and ecofriendly polyphenol tannic acid as the organic ligand and Fe3+ as the cross-linker was coated onto the surface of Fe3O4. Then, the borate-functionalized metal-organic framework (MIL-100(Fe)-B) with 5-boronobenzene-1,3-dicarboxylic acid as a ligand fragment was modified onto the PTA-coated Fe3O4 through a metal-ligand-fragment coassembly strategy. The obtained smart porous adsorbent Fe3O4@PTA@MIL-100(Fe)-B was confirmed by means of several characterization methods and then applied as an effective magnetic solid phase extraction (MSPE) sorbent for specific extraction of trace catecholamines in human urine. The Plackett-Burman design was used for screening the variables significantly affecting the extraction efficiency. Then, the significant factors were further investigated by the Box-Behnken design to determine the optimal extraction conditions. Under the optimal conditions, a method for selective MSPE combined with high-performance liquid chromatography with a fluorescence detector for the quantitation of catecholamines in human urine was developed and validated. With the proposed method, the linearity range was from 0.500 to 500 ng mL-1 for norepinephrine and epinephrine and from 1.00 to 500 ng mL-1 for dopamine. The detection limits were 0.050, 0.11, and 0.20 ng mL-1 for norepinephrine, epinephrine, and dopamine, respectively. The recoveries from spiking experiments varied from 91.5 to 108% with relative standard deviations (RSDs) of 0.80-4.8%. The established method is rapid, sensitive, accurate, inexpensive, and ecofriendly and was successfully applied to the determination of the target catecholamines in human urine samples.

Mesoporous silica adsorbents modified with amino polycarboxylate ligands - functional characteristics, health and environmental effects.

A series of hybrid adsorbents were produced by surface modification with amino polycarboxylate ligands of industrially available microparticles (MP) of Kromasil® mesoporous nanostructured silica beads, bearing grafted amino propyl ligands. Produced materials, bearing covalently bonded functions as EDTA and TTHA, original Kromasil®, bearing amino propyl ligands, and bare particles, obtained by thermal treatment of Kromasil® in air, were characterized by SEM-EDS, AFM, FTIR, TGA and gas sorption techniques. Adsorption kinetics and capacity of surface-modified particles to adsorb Rare Earth Elements (REE), crucial for extraction in recycling processes, were evaluated under dynamic conditions, revealing specificity matching the ligand nature and the size of REE cations. A detailed comparison with earlier reported adsorbents for REE extraction was presented. The cytotoxicity was assessed using four different types of healthy cells, human skeletal muscles derived cells (SKMDC), fibroblast cells, macrophage cells (RAW264.7), and human umbilical vein endothelial cells (HUVECs), indicating lower toxicity of ligand-free MP than MP bearing amino poly-carboxylate functions. Internalization of the MP inside the cells and release of nitric oxide were observed. In addition, zebrafish embryos were exposed to high concentrations of MP and did not show any pronounced toxicity.

Application of choline chloride deep eutectic solvents and high-speed counter-current chromatography to the extraction and purification of flavonoids from the thorns of Gleditsia sinensis Lam.

INTRODUCTION: Flavonoids are the most important and effective constituents in the thorns of Gleditsia sinensis Lam., which have been known to show antimicrobial, antiviral, anticancer, and anticoagulant activities. However, efficient extraction and separation methods for these flavonoids are not currently established. OBJECTIVE: To develop an efficient method for efficient extraction and rapid separation of flavonoids from the thorns of G. sinensis using choline chloride deep eutectic solvents (DESs) and high-speed counter-current chromatography (HSCCC). METHODOLOGY: As for extraction, DES composed of choline chloride and 1,4-butanediol at 1:4 mole ratio, at an extraction temperature of 55°C, 20% of water content, 1:30 mg/mL for solid-liquid ratio, and 45 min for extraction time were selected as the optimised extraction method for flavonoids from the thorns of G. sinensis. As for separation, dichloromethane-methanol-n-butanol-water (4:3:0.5:2, v/v) was applied to develop a successful strategy for purification of the flavonoids by HSCCC. RESULTS: Totally, five flavonoids, including padmatin (1, 3.7 mg), isovitexin (2, 2.5 mg), 3',5,5',7-tetrahydroxyflavanonol (3, 11.2 mg), 7,4'-dihydroxy-5,3'-dimethoxyflavanonol (4, 4.1 mg), and quercetin (5, 3.8 mg), were successfully obtained from 250 mg of the extracted flavonoids by HSCCC. CONCLUSION: Results demonstrated that the combination of DES and HSCCC is a powerful technique for the extraction, and isolation of flavonoids from the thorns of G. sinensis compared with conventional organic solvent extraction and column chromatography, which have been proven to provide higher extraction efficiency for flavonoids and rapidly obtain the quality control markers of flavonoids from the investigated plant.

Multi-template molecularly imprinted solid phase extraction and its application in the extraction and separation of multi-components from traditional Chinese medicine / 药学学报

Multi-template molecularly imprinted solid phase extraction not only has the advantages of high selectivity, large adsorption capacity, easy preparation, reuse and low environmental pollution, but also can realize the enrichment and separation of many kinds of compounds. It has attracted wide attention in the extraction and separation of traditional Chinese medicine components. This study summarizes the latest development of multi-template molecularly imprinted solid phase extraction. At the same time, based on the classification of active components of traditional Chinese medicine (flavonoids, alkaloids, phenylpropanol, terpenes, etc.), the latest application of multi-template molecular imprinting solid phase extraction in multi-component separation of traditional Chinese medicine was reviewed, with a view to better application of multi-template molecularly imprinted polymer in active multi-component extraction and separation of traditional Chinese medicine and provide reference for the material basic research of the efficacy of traditional Chinese medicine.

[Extraction and Separation of Sinapine from Rapeseed Cake and the Mode of Action of Melanin Production Inhibition].

Brassica campestris L. is the important oil-bearing crop in China. Rapeseed cake is the main byproduct of rapeseed oil extraction. As the main active ingredient in rapeseed cake, sinapine has several important biological activities. Therefore, the inhibitory activity of sinapine on tyrosinase in vitro and its free radical-scavenging rate were determined. Tyrosinase activity in A-375 human melanocytes was also investigated and the effects of sinapine on the melanin content and its antioxidant effects on melanin biosynthesis were studied. The results showed that sinapine had significant antioxidant activity. Sinapine significantly inhibited A-375 human melanocytes in a dose-dependent manner. Sinapine inhibited melanin synthesis in A-375 cells by downregulating the mRNA and protein expression of TRP-1, TRP-2, and MITF factors. The results showed that rapeseed cake sinapine inhibited melanin production and could be used as a potential active ingredient in the development of whitening agents.

[Research progress of dummy template molecularly imprinted polymers in separation of natural products].

The dummy template molecularly imprinted polymers not only has such characteristics of normal imprinted polymers as rapid identification, easy preparation, stable structure and multiple reuse, but also can imprint the compounds in natural products that are not suitable as direct template. Therefore, it has drawn more and more attention in the field of the study of natural products. This paper summarizes the methods for the selection of dummy template molecules by investigating the relevant literatures in the past ten years, analyzes the advantages and disadvantages of dummy template molecules in the practical application, and based on the types of natural products active ingredients, this paper is the first to review of the latest progress in extraction and separation of dummy template molecularly imprinted polymers. We believed that this paper could provide references for better applications of the dummy template molecularly imprinted polymers to extract and separate natural products.

Evaluation of CO2-induced azole-based switchable ionic liquid with hydrophobic/hydrophilic reversible transition as single solvent system for coupling lipid extraction and separation from wet microalgae.

The utilization of microalgae as bioenergy source was limited by the excessive cost and energy consumption during the process of lipid extraction and separation. CO2-induced switchable ionic liquids (S-ILs) with reversible hydrophobic-hydrophilic conversion were synthesized and applied for lipid extraction and separation. The reversible transition mechanism of switchable IL is due to the formation of carbamate. The novel approach based on S-ILs was developed for lipid extraction from wet microalgae, which coupled microalgae cell disruption, lipid extraction, separation, and solvent recovery process without additional solvents. The highest lipid extraction efficiencies from wet microalgae were obtained by C6DIPA-Im, and the lipids were recovered from the extraction phase by simply bubbling CO2. Furthermore, C6DIPA-Im maintained more than 83.6 ±â€¯3.6% of its initial lipid extraction efficiency after recycling five times. The S-IL based extraction and separation method provides a new strategy for sustainable bioenergy production.