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Isolation and Purification of Isoaloeresin D and Aloin from Aloe vera by high-speed counter-current chromatography

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Chinese Herbal Medicines 2010年第2期2卷 148-152页

作者： WAN Jin-zhi1,CHEN Xin-xia1,QIU Chun-mei1,LIN Xiang-cheng2 1.Laboratory for Pharmaceutical Analysis and Quality Evaluation,School of Pharmaceutical Sciences,Sun Yat-sen University,Guangzhou 510006,China 2.Institute of Fine Chemicals and Synthetic Drugs,Sun Yat-sen University,Guangzhou 510006,China WAN Jin-zhi CHEN Xin-xiaQIU Chun-mei(Laboratory for Pharmaceutical Analysis and Quality EvaluationSchool of Pharmaceutical SciencesSun Yat-sen UniversityGuangzhou 510006China) LIN Xiang-cheng(Institute of Fine Chemicals and Synthetic Drugs Sun Yat-sen UniversityGuangzhou 510006China)

Objective To develop an efficient method to isolate and purify the main components isoaloeresin D and aloin from Aloe vera for its industrial *** high-speed counter-current chromatography was used to isolate isoaloeresin D and aloin in a one-step separation from dried crude extract of *** biphasic solvent system composed of hexane-ethyl acetate-acetone-water(0.2:5:1.5:5) was used at a flow rate of 1.0 mL/min,while the lipophilic phase was selected as the mobile phase and the apparatus was rotated at 840 r/*** effluent was detected at 254 *** Isoaloeresin D(53.1 mg) and aloin(106.9 mg) were separated from the crude extract(384.7 mg) with the purities of 98.6% and 99.5%,*** HSCCC is a powerful technique for isolation and separation of chemical composition from aloe.

关键词： Aloe vera aloin high-speed counter-current chromatography isoaloeresin D extraction and purification

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Rapid enrichment and separation minor ingredients based on Liquid-liquid extraction and Classical solvent system from Hydrocotyle sibthorpioides *** high-speed counter-current chromatography

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Rapid enrichment and separation minor ingredients based on L...

中国化学会第十二届全国天然有机化学学术会议

作者： Daoguang Song Xue Yang Tao Chen Xinyu Fan Zhiwei Sun Junjie Wang Zhi Chen Key Laboratory of Medicinal Animal and Plant Resources of the Qinghai-Tibetan Plateau Qinghai Normal University School of Life Science Qinghai Normal University Qinghai Key Laboratory of Tibetan Medicine Pharmacology and Safety Evaluation Northwest Institute of Plateau BiologyChinese Academy of Science School of Chemistry and Chemical engineering Qufu Normal University

Nowadays,high-speed counter-current chromatography(HSCCC) has been widely used for the separation of chemical compounds in natural *** of an efficient strategy method rapid enrichment and separation five minor ingredients based on liquid-liquid extraction and classical solvent system by HSCCC were reported in this *** a word,minor ingredients may have unknown activity and affect the quality of the *** this study,we tried using several solvent systems to enrich target compounds,and finally,we found a classical two phase solvent system consisting of dichloromethane/methanol/water(1.5:1:1,v/v/v) can fast and effective enrichment minor compound from complex and vast *** last,five minor ingredients were isolated from EtOAc-soluble fractions and named as:(1)p-hydroxybenzoic acid(5.8 mg),(2)Vanillic acid(3.7 mg),(3)Luteolin(12.7 mg),(4)Quercetin(10.1 mg) and(5)kaempferol(4.8 mg) from 3 g of EtOAc-soluble *** structures were identified by H NMR and 13 C NMR *** what’s important is that modern medicine believes that flavonoids such as kaempferol and quercetin are effective components for cough,asthma and blood pressure.

关键词： Hydrocotyle sibthorpioides Lam. minor ingredients high-speed counter-current chromatography

Preparative Separation and Purification of Bufadienolides from ChanSu by high-speed counter-current chromatography Combined with Preparative HPLC

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Preparative Separation and Purification of Bufadienolides fr...

中国化学会第9届天然有机化学学术会议

作者： Jialian Li,Xiao Wang,Hongbin Liu,Lei Fang~* Shandong Analysis and Test Center,Shandong Academy of Sciences,19 Keyuan Street,Jinan,Shandong 250014,China

＜正＞ChanSu,is prepared from the dried toad secretions derived from either Bufo bufo gargarizans Cantor or Bufo melsanostictus Schneider and has been widely used as a cardiotonic,diuretic,and antineoplastic *** researches have revealed that bufadienolides are the vast majority of *** has been proved to exhibit significant inhibitory activities against different kinds of human cancer cells,such as myeloid

关键词： high-speed counter-current chromatography Bufadienolides preparative HPLC

Rapid preparative separation of six bioactive compounds from Gentiana crassicaulis Duthie ex *** microwave-assisted extraction coupled with high-speed counter-current chromatography

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Rapid preparative separation of six bioactive compounds from...

第十一届全国博士生学术年会

作者：梁晋如 Yoichiro Ito 孙文基 Biomedicine Key Laboratory of shaanxi province Northwest University Bioseparation Technology Laboratory Biochemistry and Biophysics CenterNational HeartLungand Blood InstituteNational Institutes of HealthBethesdaMDUSA

A rapid method combining microwave-assisted extraction(MAE) and high-speed counter-current chromatography(HSCCC) was applied for preparative separation of six bioactive compounds including loganic acid(Ⅰ), isoorientin-4'-O-glucoside(Ⅱ),6'-O-fI-D-glucopyranosyl gentiopicroside(Ⅲ), swertiamarin(Ⅳ),gentiopicroside(Ⅴ),sweroside(Ⅵ) from traditional Tibetan medicine Gentiana crassicaulis Duthie ex *** parameters were predicted by central composite design-response surface methodology(CCD-RSM).That is,5.0 g dried roots of *** was extracted with 50 mL 57.5%aqueous ethanol under 630 W for 3.39 *** extract(gentian total glycosides) was separated by HSCCC with n-butanol-ethyl acetate-methanol-l%acetic acid water(7.5:0.5:0.5:3.5,v/v/v/v) using upper phase mobile in tail-to-head elution mode.16.3 mg,8.8 mg,12.8 mg, 25.1 mg,40.7 mg and 21.8 mg of compoundⅠ-Ⅵwere obtained in one run from 500 mg original sample with purities of 98.6%,96.7%,98.1%,99.1%,99.4%and 98.7%, respectively and the structures were identified by ESI-MS and *** study reveals that CCD-RSM is convenient and highly predictive for optimizing the extraction process,MAE coupled with HSCCC could be an efficient and expeditious method for extraction and separation of phytochemicals from ethnomedicine.

关键词： Central composite design-response surface methodology Gentiana crassicaulis Duthie ex Burk high-speed counter-current chromatography Microwave-assisted extraction

Extraction and purification of ustiloxin A from rice false smut balls by a combination of macroporous resin and high-speed countercurrent chromatography

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Food Production, Processing and Nutrition 2020年第1期2卷 287-299页

作者： Gang Wang Dan He Fengchun Zhao Junqiang Hu Yin-Won Lee Jianrong Shi Jianhong Xu Jiangsu Key Laboratory for Food Quality and Safety-State Key Laboratory Cultivation Base Ministry of Science and Technology/Key Laboratory for Control Technology and Standard for Agro-product Safety and QualityMinistry of Agriculture and Rural Affairs/Key Laboratory for Agro-product Safety Risk Evaluation(Nanjing)Ministry of Agriculture and Rural Affairs/Collaborative Innovation Center for Modern Grain Circulation and Safety/Institute of Food Safety and NutritionJiangsu Academy of Agricultural SciencesNanjingPeople’s Republic of China School of Food and Biological Engineering Jiangsu UniversityZhenjiangPeople’s Republic of China Department of Microbiology College of Life ScienceKey Laboratory for Agriculture MicrobiologyShandong Agricultural UniversityTai’anPeople’s Republic of China School of Agricultural Biotechnology Seoul National UniversitySeoul 08826Republic of Korea

Rice false smut is an emerging plant disease *** A(UstA)is the major mycotoxin found in rice false smut balls,which are fungal colonies in rice *** this study,a new method consisting of macroporous resin column chromatography and high-speed countercurrent chromatography(HSCCC)was developed for UstA *** was extracted by a 3.81%HCOOH solution and adsorbed by XAD-4 *** was then eluted by a 40%methanol solution supplemented with 0.1%trifluoroacetic acid(TFA).Further purification was achieved by HSCCC using a two-phase solvent system consisting of n-butanol/TFA/H_(2)O(1/0.05/1,v/v/v).Under the optimized conditions,225 mg of UstA was obtained with a purity of 97.39%in a single run,with a final recovery of 65.2%.An inhibitory effect on seed germination of wheat and maize caused by UstA was observed in a preliminary phytotoxicity assay.

关键词： Ustiloxin A Rice false smut Preparative purification Macroporous resin high-speed counter-current chromatography Phytotoxicity assay

Isolation and Purification of Triptolide from the Leaves of Tripterygium wilfordii Hook F

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Chinese Journal of Chemical Engineering 2010年第5期18卷 750-754页

作者：沈剑何潮洪 State Key Laboratory of Chemical Engineering( Department of Chemical and Biological Engineering Zhejiang University Hangzhou 310027 China

Triptolide is an important active component of Tripterygium wilfordii Hook F (TWHF) and possesses anti-inflammatory, immunosuppressive, male anti-fertility, and anticancer properties. A new method combining different techniques, including solid-liquid extraction, liquid-liquid partition, column chromatography and high-speed counter-current chromatography (HSCCC) but avoiding the use of chloroform, was developed for the isolation and purification of triptolide from the leaves of TWHF. 48 mg of triptolide at 96.5% purity was obtained from 1 kg of air-dried leaves of TWHF.

关键词： Tripterygium wilfordii Hook F triptolide high-speed counter-current chromatography

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Complementary Application of HSCCC and Semi-preparative HPLC for Rapid Separation of Phenylethanoid Glycosides from Penstemon digitalis

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Chinese Herbal Medicines 2013年第4期5卷 280-285页

作者： WANG Qi-yan XIE Jun FANG Sheng SHEN Xiu-lian LI Qi WU Xiu-hua TANG Shao-hu Department of Chemical Biology School of Chemistry and Chemical Engineering Anhui University of Technology School of Life Sciences Southwest University Department of Applied Chemistry School of Chemistry and Chemical Engineering Anhui University of Technology

Objective Echinacoside and verbascoside are known for their excellent neuroprotective,anti-inflammatory,and anti-oxidative activities,therefore large amount of pure compounds are urgently needed as authentic standards for various in vivo and in vitro ***,they are abundenty extracted from endangered Cistanche *** studies revealed that Penstemon spp.,comprising about 280 species,were rich natural sources for the exploitation and large scale preparation of phenylethanoid ***,rapid isolation and purification of various phenylethanoid glycosides from Penstemon *** *** The crude extract of *** was first enriched by AB-8,and then the high-speed counter-current chromatography(HSCCC)combined with semipreparative high performance liquid chromatography(HPLC)method was adopted to isolate and purify echinacoside and *** Eventually,verbascoside(67.2 mg)with the purity of 92.6%and echinacoside(3.96 mg)with the purity of 98.9%were obtained from 5 g powdered leaves of *** The present mode of HSCCC coupled with semi-preparative HPLC could be a powerful method for the rapid isolation and purification of other phenylethanoid glycosides.

关键词： echinacoside high-speed counter-current chromatography Penstemon digitalis semi-preparative high performance liquid chromatography verbascoside

Separation of a minor lignin from Sinopodophyllum emodi by MPLC and HSCCC guided by HPLC-MS

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Separation of a minor lignin from Sinopodophyllum emodi by M...

中国化学会第十九届全国有机分析及生物分析学术研讨会

作者： Tao Chen Hongmei Li Liang Tan Yulin Li Northwest Institute of Plateau Biology Chinese Academy of Sciences University of the Chinese Academy of Sciences

A minor lignin,4′-demethyldeoxypodophyllotoxin,was isolated from Sinopodophyllum ***,a crude extract of Sinopodophyllum emodi was analyzed by HPLC-MS to confirm the presence of the target ***,the target lignin was successfully enriched in the crude extract precipitate by medium-pressure LC with high recovery（85%）.Finally,an efficient separation was achieved by high-speed counter-current chromatographyusing a two-phase solvent system ofn-hexane-ethyl acetate-methanol-water（1:1:1:1,v/v/v/v）.These results clearly demonstrate that the combination of HPLC-MS,medium pressure LCand high-speed counter-current chromatography could be a powerful technique for the rapid screening,enrichment and separation of minor compounds from complex natural products.

关键词： Sinopodophyllum emodi high-speed counter-current chromatography HPLC-MS 4’-demethyldeoxypodophyllotoxin minor lignin