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ANALYTICA CHIMICA ACTA · 2013 · IF 4.387

On-line coupling of macroporous resin column chromatography with direct analysis in real time mass spectrometry utilizing a surface flowing mode sample holder

Shanshan Zeng,Lu Wang,Teng Chen,Haibin Qu

A surface flowing mode sample holder was designed as an alternative sampling strategy for direct analysis in real time mass spectrometry (DART-MS). With the sample holder, the on-line coupling of macroporous resin column chromatography with DART-MS was explored and the new system was employed to monitor the column chromatography elution process of Panax notoginseng . The effluent from macroporous resin column was first diluted and mixed with a derivatization reagent on-line, and the mixture was then directly transferred into the ionization region of DART-MS by the sample holder. Notoginsenosides were methylated and ionized in a metastable helium gas stream , and was introduced into MS for detection. The on-line system showed reasonable repeatability with a relative standard deviation of 12.3% for the peak area. Three notoginsenosides, i.e. notoginsenoside R 1 , ginsenoside Rb 1 and ginsenoside Rg 1 , were simultaneously determined during the eluting process. The alteration of the chemical composition in the effluent was accurately identified in 9   min, agreeing well with the off-line analysis. The presented technique is more convenient compared to the traditional UPLC method. These results suggest that the surface flowing mode DART-MS has a good potential for the on-line process monitoring in the pharmaceutical industry .

CAS / MDL: 75-59-2
研究领域: 分析化学 · 中药学
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FOOD CHEMISTRY · 2014 · IF 3.259

Preliminary enrichment and separation of chlorogenic acid from Helianthus tuberosus L. leaves extract by macroporous resins

Peng-Cheng Sun,Ying Liu,Yue-Tao Yi,Hong-Juan Li,Ping Fan,Chuan-Hai Xia

In the present study, a simple and efficient method for the preparative separation of 3-CQA from the extract of Helianthus tuberosus leaves with macroporous resins was studied. ADS-21 showed much higher adsorption capacity and better adsorption/desorption properties for 3-CQA among the tested resins. The adsorption of 3-CQA on ADS-21 resin at 25   °C was fitted best to the Langmuir isotherm model and pseudo-second-order kinetic model. Dynamic adsorption/desorption experiments were carried out in a glass column packed with ADS-21 to optimise the separation process of 3-CQA from H. tuberosus leaves extract. After one treatment with ADS-21, the content of 3-CQA in the product was increased 5.42-fold, from 12.0% to 65.2%, with a recovery yield of 89.4%. The results demonstrated that the method was suitable for large-scale separation and manufacture of 3-CQA from H. tuberosus leaves.

研究领域: 植物化学 · 天然产物开发
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JOURNAL OF MOLECULAR CATALYSIS A-CHEMICAL · 2012 · IF 2.947

Catalyzed synthesis of poly(l-lactic acid) by macroporous resin Amberlyst-15 composite lactate utilizing melting polycondensation

Hui-xue Ren,Han-jie Ying,Ping-kai Ouyang,Ping Xu,Jing Liu

Efficient and pollution-free catalysts play an essential role in the ultimate biodegradation of products in the synthesis of biodegradable and recyclable poly( l -lactic acid) (PLLA). Therefore, macroporous resin was utilized as the solid acid for the first time, on which lactate that could be absorbed in vivo was composited to catalyze the synthesis of PLLA. It was discovered that macroporous resin Amberlyst-15 showed good catalytic activity in oligomerization and polymerization, and lactate showed different catalytic efficiencies due to the differences in ionic radius and ionic charge. Compared to the traditional catalysts of SnCl 2 ·2H 2 O/TSA, the composite catalyst can improve the quality, yield and optical purity of its product, which can also be recycled without any residual in products. PLLA with molar mass of about 110,000   g   mol −1 was synthesized at the yield of 93%. The product exhibits pure color (white), and its optical purity and crystallinity are 98% and 55%, respectively. A possible catalytic mechanism was proposed. The resulting PLLA products were characterized by GPC, 1 H NMR, DSC, and polarimeter.

CAS / MDL: 39389-20-3
研究领域: 材料科学 · 生物工程 · 化学工程
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CHINESE JOURNAL OF CHEMICAL ENGINEERING · 2020 · IF 2.627

Static and dynamic studies of adsorption by four macroporous resins to enrich oridonin from Rabdosia rubescens

Ling Meng,Xia Gui,Zhi Yun

Oridonin, one of the active ingredients in Rabdosia rubescens ( R. rubescens ), has been reported to induce cell apoptosis and cell cycle arrest in many cancers. Conventional extraction methods tend to result in unsatisfied enrichment and poor quality of oridonin present in a given biomass. This paper aims to evaluate the performance and separation characteristics of four different macroporous resins to arrive at the most suitable methodology for the isolation and purification of high-quality oridonin. Static absorption kinetics, thermodynamic and dynamic adsorption were evaluated. HP-20 was selected for further study due to its high adsorption capacity of 32 mg·g −1 and desorption ratio with 98.5%. The pseudo-second-order model was considered to be the most suitable for kinetic results, and Langmuir model was chosen to better describe the absorption thermodynamics. Under optimum conditions (flow rate of 4 ml·min −1 , bed depth with 6 cm and initial concentration of 2.15 mg·ml −1 ), the effective content of oridonin increased from 33.9% to 79.1% in the dry extract with a recovery of 81% and the purity of oridonin improved from 76% to 93%. The results confirm that HP-20 provides an efficient method to purify most oridonin from R. rubescens .

CAS / MDL: 64-17-5 67-56-1
研究领域: 药用植物学 · 药物化学 · 生物工程
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SEPARATION AND PURIFICATION TECHNOLOGY · 2023 · IF 8.6

Separation and purification of glabridin from a deep eutectic solvent extract of Glycyrrhiza glabra residue by macroporous resin and its mechanism

Xiaoyun Liu,Su Yan,Hua Zhou,Hao Wu,Shuya Wang,Xiaoyu Yong,Jun Zhou

Glabridin has beneficial antioxidant, anti-inflammatory, and tyrosinase inhibitory activities, with many applications in the pharmaceutical and cosmetics industries. After industrial extraction of glycyrrhizic acid, Glycyrrhiza glabra residue contains abundant glabridin. Glabridin was extracted from Glycyrrhiza glabra residue with a deep eutectic solvent (DES), followed by the recovery of the glabridin by organic solvent extraction, and then partial purification with hydrophobic macroporous resin. Ethyl acetate was the best extraction solvent, with an extraction yield of 91.63 %. Twelve macroporous resins were evaluated and LSA-21 yielded the best recovery of glabridin. Adsorption of glabridin by LSA-21 resin conformed to pseudo-second-order kinetic and Langmuir models. The thermodynamic parameters ΔH (enthalpy change) and ΔG (Gibbs free energy) were both negative, ΔS (entropy change) was positive. These results indicated that LSA-21 resin spontaneously and exothermically adsorbs glabridin to form a monolayer. The optimum conditions for separating and purifying glabridin by LSA-21 resin were 50 % ethanol aqueous solution(v/v) with a concentration of 56.90 µg/mL glabridin at a flow rate of 2 bed-volumes (BV)/h, and elution with 4 BV of ethanol at 2 BV/h, producing a glabridin yield of 97.80 %. The resin could be reused four times and the glabridin yield slightly decreased to 94 %. The overall recovery of glabridin from the DES Glycyrrhiza glabra extract solution after the ethyl acetate and LSA-21 steps was 89.61 %, with a purity of 17.38 %. This approach is an effective method for the recovery and purification of glabridin from a DES extract of Glycyrrhiza glabra residue, which has potential industrial application for producing glabridin and other natural plant products.

研究领域: 植物化学 · 药学 · 生物工程
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BIOTECHNOLOGY LETTERS · 2019 ·Vol. 42 ·期 2 ·269-276 · IF 2.154

The Immobilization of Candida antarctica lipase B by ZIF-8 encapsulation and macroporous resin adsorption: preparation and characterizations

Cai Xinyong,Zhang Mengjie,Wei Wei,Zhang Yinjun,Wang Zhao,Zheng Jianyong

A novel enzyme immobilization method employing metal–organic framework (MOF) encapsulation and macroporous resin adsorption was developed in this study. Candida antarctica lipase B (CALB) was firstly encapsulated onto metal–organic frame structures (Zeolitic imidazole framework-8, ZIF-8) and further bonded to macroporous resin by physical adsorption. Under optimized immobilization conditions, the activity of the prepared immobilized lipase (CALB-ZIF-8@D101) determined via the methyl esterification of oleic acid was 38.4 U/mg. Compared with free lipase, the immobilized lipase exhibited improved thermal and operational stability and organic solvent tolerance. These results demonstrate that the immobilization method of ZIF-8 encapsulation and macroporous resin adsorption enhanced enzyme properties at a superior level.

CAS / MDL: 9002-98-6
研究领域: 生物化学 · 酶工程 · 材料科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2016 · IF 3.299

Optimization of integrated extraction-adsorption process for the extraction and purification of total flavonoids from Scutellariae barbatae herba

Peng Huang,Qing Zhang,Hongye Pan,Lianjun Luan,Xuesong Liu,Yongjiang Wu

In the present study, integrated extraction-adsorption process was developed and applied to extract and purify total flavonoids from Scutellariae barbatae herba. Screening of macroporous resins, single factor experiments, an experimental design based on Box-Behnken design (BBD) and purification conditions study were carried out to optimize the integrated process. DM130 resin was chosen as adsorbent and the optimal extraction-adsorption conditions were determined as pH of extraction solvent 2, time 9   h, liquid/solid ratio 20:1   mL/g and flow rate 7   BV/h. 70% (5   BV) ethanol aqueous solution was selected as elution solvent. Through this procedure, the total flavonoids of Scutellariae barbatae herba can be totally extracted using water as extraction solvent rather than high concentration ethanol was used in traditional extraction method. Moreover, the integrated process can simplify operation, reduce energy consumption, and prevent the degradation of bioactive substances, thus improve the quality of products. Compared to the conventional method, the recovery yield and purity of total flavonoids obtained from this procedure increased by 1.50 and 1.16 times respectively. The results showed that the integrated procedure can be efficient and eco-friendly, as well as appropriate for large-scale extraction and purification of total flavonoids from Scutellariae barbatae herba .

研究领域: 中药学 · 天然产物化学
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Biomass Conversion and Biorefinery · 2023 · IF 4

Study on extraction, purification, and biological activities of forsythiaside A from Forsythia suspensa (Thunb.) Vahl leaf

Weng Di,Tian RongRong,Jin HaiXin,Zha ShengHua,Zhao QingSheng,Zhao Bing

In this study, a method to enrich forsythiaside A (FA) from the ball-milled powder of Forsythia suspensa leaves was established. Forsythiaside A was extracted by heating and stirring, and the extraction process was optimized by response surface methodology using the independent variables of extraction temperature, extraction time, liquid-to-material ratio, ethanol concentration, and pH value of the solution, respectively. Then five types of macroporous resins with different polarities were studied to explain the adsorption mechanism by static adsorption and desorption experiments. Different models were used to study the static adsorption thermodynamics and kinetic process of AB-8 resin on FA extracts, and optimal conditions of the process were optimized. Finally, the antioxidant abilities of purified FA were evaluated. The results showed that the optimum extraction conditions were 2.2 h, 53.4 °C, 45.7 mL/g, 60% ethanol, and pH 6, and the extraction efficiency of forsythiaside A could achieve 120.96 mg/g. The AB-8 macroporous resin was the most suitable resin with high adsorption and desorption rates. It was found that the Temkin model was able to calculate the adsorption parameters accurately. The adsorption kinetic process of the resin was in accordance with the pseudo-second-order kinetic model. The optimal process conditions were as follows: the optimum loading concentration of 5.83 mg/mL, the loading rate of 1 BV/h, and the loading volume of 7.51 BV; in the desorption process, deionized water was used to remove impurities first, and then, 30% ethanol was used with an elution rate of 1 BV/h. The purity of FA increased from 20.52 to 81.58%. The purified FA exhibited superior scavenging ability for DPPH radicals and ABTS radicals. Cytotoxicity experiments proved that it was safe and nontoxic and was capable of promoting cell growth. In conclusion, the present study provides a theoretical basis for industrially extracting and purifying FA on a reliable basis.

CAS / MDL: 30931-67-0
研究领域: 植物化学 · 药理学 · 天然产物研究
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PROCESS BIOCHEMISTRY · 2022 · IF 4.885

Static decolorization of polysaccharides from the leaves of Rhododendron dauricum: Process optimization, characterization and antioxidant activities

Zhengyu Hu,Ruiying Yu,Jinfeng Sun,Yuanqi Duan,Hongli Zhou,Wei Zhou,Gao Li

In this study, polysaccharides from the leaves of Rhododendron dauricum L. (RDPs) were decolorized using the static macroporous resin adsorption method. The RDPs were characterized and their antioxidant activities were investigated. An analytical hierarchy process (AHP) and a response surface method (RSM) were used to determine the optimum decolorization conditions as: a polysaccharide concentration of 8 mg/mL, decolorization time of 70 min, liquid–solid ratio of 6 mL/g, and decolorization temperature of 52 °C, with D101 as the best resin. Furthermore, two novel polysaccharides (RDP-1 and RDP-2) were isolated from R. dauricum leaves and characterized, which demonstrated that RDP-1 and RDP-2 were both composed of mannose , glucose, galactose , and arabinose in different molar ratios. These RDPs also exhibited a triple helix conformation, and primarily contained →6)-Glc p -(1→, →5)-Ara f -(1→, →2,4)-Man p -(1→, →6)-Gal p -(1→ and Glc p -(1→ residues with different connection sequences. Biological activity tests showed that the two polysaccharides possessed scavenging capacity against 1,1-Diphenyl-2-picrylhydrazyl (DPPH), hydroxyl, and 2,2-Azino-bis-(3-ethyl-benzothiazoline-6-sulfonic acid) (ABTS) radicals. The results indicated that the antioxidant activities of the RDPs obtained by the static decolorization method improved, which lays a theoretical foundation for developing techniques for utilising R. dauricum .

研究领域: 植物学 · 药学 · 分析化学 · 生物技术
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PREPARATIVE BIOCHEMISTRY & BIOTECHNOLOGY · 2025 · IF 1.9

Development of an efficient extraction and enrichment method for total flavonoids compounds from Erigeron breviscapus using ultrasound-assisted extraction and macroporous resin adsorption

Yang Li,Wei Zhao,Qifeng Li,Jiayu Zhang,Anquan Yang,Min Xie,Ranhua Xiong,Chaobo Huang

Erigeron breviscapus, a medicinal plant rich in flavonoids with diverse pharmacological properties is an important resource. To maximize the utilization of these valuable bioactive compounds, ultrasound-assisted extraction combined with response surface methodology was used to optimize the extraction conditions for total flavonoids. After comparing six macroporous resins’ adsorption and desorption characteristics, AB-8 was selected for enriching total flavonoids, and its adsorption kinetics and thermodynamics were investigated. The following parameters were chosen as optimal for the dynamic adsorption/desorption experiments using an AB-8 filled column: sample loading concentration of 1.14 mg/mL, sample loading flow rate of 2 BV/h, elution solvent of 70% ethanol, desorption flow rate of 1 BV/h, elution solvent volume of 5.5 BV, pH of 2, temperature of 25 °C. After enrichment, the concentration of flavonoids was 5.16 times higher than that of crude extract. LC-MS identified 54 flavonoid molecules with excellent antioxidant properties.

研究领域: 植物化学 · 药学 · 分析化学
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ACS Omega · 2023 · IF 4.1

Extraction and Purification of Aucubin from Eucommia ulmoides Seed Draff in Natural Deep Eutectic Solvents Using Macroporous Resins

Yunhui Liao,Feng Chen,Haishan Tang,Wubliker Dessie,Zuodong Qin

Aucubin (AU) is an active ingredient that exerts strong antioxidant and anti-inflammatory effects in the treatment of several diseases. In order to improve the efficiency of resource utilization of traditional biomass waste, Eucommia ulmoides seed-draff (EUSD) waste biomass was used as the raw material, and a series of deep eutectic solvents were selected to evaluate the extraction efficiency of aucubin from EUSD. A response surface experiment was designed based on a single-factor experiment to optimize the extract conditions. The results showed that the best conditions for aucubin extraction were an HBD–HBA ratio of 2.18, a liquid–solid ratio of 46.92 mL/g, a water percentage of 37.95%, a temperature of 321.03 K, and an extraction time of 59.55 min. The maximum amount of aucubin was 156.4 mg/g, which was consistent with the theoretical value (156.8 mg/g). Then, the performance of 12 resins for adsorption and desorption was contrasted. The results revealed that HPD950 resin exhibited the best performance, with an adsorption capacity of 95.2% and a desorption capacity of 94.3%. Additionally, the pseudo-second-order model provided the best match to the kinetics data, the Langmuir model provided the best fit to the isotherm data, and adsorption was a beneficial, spontaneous, exothermic, and physical process. In the recyclability test, the HPD950 resin had great potential and excellent sustainability in aucubin recovery. In the antioxidant activity study, the aucubin extract exerted a strong antioxidant ability with scavenging capabilities for four free radicals. Furthermore, the antifungal activity study found that the aucubin extract exhibited a good antifungal effect against 5 tested pathogens. The research results can provide a theoretical basis for the extraction of high-value components from waste biomass by deep eutectic solvent and a certain application value for the development and utilization of natural aucubin products.

研究领域: 植物化学 · 天然产物开发 · 环境科学
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JOURNAL OF CHEMICAL AND ENGINEERING DATA · 2019 · IF 2.298

Grafting of Poly(4-vinylpyridine) onto a Macroporous Resin for Sorption of 2-Naphthalenesulfonic Acid in Batch Experiments

Yue Sun,Weisheng Zheng,Rajendra Prasad Singh,Li Chen

In the current work, poly(4-vinylpyridine) (P4VP) was grafted on a macroporous polystyrene resin via free-radical polymerization by using the pendent vinyl group. The grafting conditions such as swelling agent, initiator concentration, reaction temperature, and amount of 4-vinylpyridine (4VP) monomer were optimized, and three resins with different 4VP monomer amounts (SC-1, SC-2, and SC-3) were chosen as adsorbents. P4VP-grafted resins were characterized by scanning electron microscopy, N2 sorption/desorption isotherms, Fourier transform infrared, and X-ray photoelectron spectroscopy. The sorption properties of 2-naphthalenesulfonic acid (NSA) on three resins were comparatively investigated. The experimental data revealed that the sorption process on three resins fitted well with the pseudo-second-order kinetics equation, and the equilibrium isotherms were in good agreement with the Langmuir model. The NSA sorption onto resins was an endothermic and spontaneous process, and SC-3 loaded with NSA can be efficiently regenerated by NaOH and ethanol mixed solution after sorption. The maximum sorption capacities of three resins indicated that P4VP-grafted resins possess good sorption ability toward NSA.

CAS / MDL: 94-36-0
研究领域: 化学工程 · 环境科学
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