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Sample records for countercurrent extraction test

  1. Counter-current extraction of sweet sorghum sugar for fermentation

    SciTech Connect

    Toledo, R.T.

    1985-01-01

    A small counter-current extractor in the form of a heated inclined screw was tested to remove residual sugar from the bagasse after sweet sorghum was passed through one roller mill. Roller milling alone recovered only 45% of total sugar. Combined efficiency of milling and extraction was 95%. Combined pressed juice (17% sugar) and extract (10% sugar) produces a 12.5% solids juice for fermentation.

  2. Counter-current carbon dioxide extraction of soy skim

    USDA-ARS?s Scientific Manuscript database

    The use of carbon dioxide in a counter-current fractionation column was investigated as a means to remove residual fat from soy skim after enzyme-assisted aqueous extraction of soybeans. The stainless steel column was 1.2 meters long with an internal diameter of 1.75 cm and filled protruded stainles...

  3. Evaluation of dual flow counter-current chromatography and intermittent counter-current extraction.

    PubMed

    Ignatova, Svetlana; Hewitson, Peter; Mathews, Ben; Sutherland, Ian

    2011-09-09

    The aim of this research is to compare two continuous extraction technologies, intermittent counter-current extraction (ICcE) and dual flow counter-current chromatography (DFCCC), in terms of loading and throughput using the GUESSmix, and show the advantages and disadvantages of the two methods. A model sample containing caffeine, vanillin, naringenin and carvone, with a total load of 11.2 g, was employed with a hexane-ethyl acetate-methanol-water (2:3:2:3) phase system to evaluate an ICcE method on a preparative (912 ml coil volume) DE-Midi instrument. While DFCCC was carried out on a specially designed preparative (561 ml coil volume) bobbin installed in a similar Midi instrument case. While similar throughputs of 7.8 g/h and 6.9 g/h were achieved for the ICcE and DFCCC methods respectively, ICcE was demonstrated to have a number of advantages over DFCCC.

  4. Phase distribution visualisation in continuous counter-current extraction.

    PubMed

    van den Heuvel, Remco; Sutherland, Ian

    2009-05-08

    Flow visualisation is essential when trying to understand hydrodynamic equilibrium in continuous counter-current extraction (CCCE) (also known as dual-flow counter-current chromatography). The technique allows two immiscible liquid phases to be pumped through the spinning coil simultaneously in opposite directions. When this process was described previously it was assumed that the phases were evenly distributed throughout the coil. Visualisation studies by van den Heuvel and Sutherland in 2007 showed that this was not the case. A special centrifuge, where the coil is cantilevered so that the coil and the fluids inside the coil can be visualised, was used to study the distribution of the phases. Factorial experimental design was used to systematically study the effect of the starting conditions inside the coil on the phase distribution at equilibrium. For each experiment the eluted volumes and the volume of upper phase in the coil at the end of the experiment (at equilibrium) were recorded. In addition, two photographs were taken when the phases in the coil had reached equilibrium. One of these photographs was taken during the experiment when the phases were still being pumped through and one when the flow was stopped. The systematic experiments showed that the initial phase inside the coil has no effect on the phase distribution achieved at equilibrium. Statistical analysis also showed that the lower phase flow rate has double the effect on the phase distribution compared to the upper phase flow rate. From these visualisation studies, it can be concluded that the balance of the phases flowing through the coil at equilibrium is complex. The volumes of upper and lower phase and how they are distributed does influence the separation. It is important therefore to understand the relationship between respective flow rates and the phase distribution if peak elution is to be accurately predicted.

  5. Intermittent counter-current extraction-Equilibrium cell model, scaling and an improved bobbin design.

    PubMed

    Hewitson, Peter; Sutherland, Ian; Kostanyan, Artak E; Voshkin, Andrei A; Ignatova, Svetlana

    2013-08-16

    This paper describes an equilibrium cell model for intermittent counter-current extraction that is analytically solved for the first time for continuous sample injection between a pair of columns. The model is compared with practice for injections of a model mixture of compounds on a standard high-performance counter-current chromatography instrument giving good agreement for compound elution order and the times to maximum concentration for the eluted components. An improved design of end fittings for the counter-current chromatography bobbins is described which permits on-column switching of the mobile and stationary phases. This on-column switching successfully eliminates the displaced stationary phase seen in fractions when operating ICcE with standard flying leads and gives a 6% reduction in the retention time of compounds and improved resolution due to the elimination of the time delay required to pump the previous mobile phase from standard flying leads.

  6. The Countercurrent Extraction of Ink: A Demonstration of the Chromatographic Mechanism.

    ERIC Educational Resources Information Center

    Bricker, Clark E.; Sloop, Gregory T.

    1985-01-01

    Describes an experiment (carried out in less than two hours) in which the merits of countercurrent extraction are immediately evident by visible colors. The experiment requires eight 125-ml separatory funnels, 250ml of 1-butanol, 250ml of 0.1-0.5 molar hydrochloric acid, and a small amount of Sheaffer's Skrip blue-black soluble ink. (JN)

  7. The Countercurrent Extraction of Ink: A Demonstration of the Chromatographic Mechanism.

    ERIC Educational Resources Information Center

    Bricker, Clark E.; Sloop, Gregory T.

    1985-01-01

    Describes an experiment (carried out in less than two hours) in which the merits of countercurrent extraction are immediately evident by visible colors. The experiment requires eight 125-ml separatory funnels, 250ml of 1-butanol, 250ml of 0.1-0.5 molar hydrochloric acid, and a small amount of Sheaffer's Skrip blue-black soluble ink. (JN)

  8. Counter-current carbon dioxide extraction of fat from soy skim

    USDA-ARS?s Scientific Manuscript database

    This research aims to investigate the use of counter-current carbon dioxide extraction method as a means to reduce residual fat in soy skim after the enzyme-assisted aqueous extraction of soybeans. Extractions with liquid CO2 at 25°C and 10.34 MPa and supercritical CO2 at 50°C and 25.16 MPa are comp...

  9. Mass transfer in countercurrent packed columns: Application to supercritical CO[sub 2] extraction of terpenes

    SciTech Connect

    Simoes, P.C.; Matos, H.A.; Carmelo, P.J.; Gomes de Azevedo, E.; Nunes da Ponte, M. . Faculdade de Ciencias e Tecnologia)

    1995-02-01

    Supercritical fluid extraction (SFE) is an alternative separation method to more conventional processes such as liquid extraction and distillation. However, up to now, few works have been devoted to the investigation of the efficiency of countercurrent packed columns under supercritical conditions from a mass transfer point of view. Mass transfer in a countercurrent column, filled with structured gauze packing, was measured for the separation of a mixture of terpenes (d-limonene/1,8-cineole) by supercritical carbon dioxide, at 313 and 318 K and pressures up to 9 MPa. The extraction efficiency was determined in terms of the overall mass transfer coefficient. Operating lines for this process had an appreciable curvature due to a high miscibility of the two contacting phases. The real slope of these lines had to be estimated. Available mass transfer models for packed columns predicted efficiencies diverging to a great extent from the experimental results.

  10. Hydrodynamics of a packed countercurrent column for the gas extraction

    SciTech Connect

    Stockfleth, R.; Brunner, G.

    1999-10-01

    The hydraulic capacity of a countercurrent column with gauze packing was examined at pressures between 8 and 30 MPa and temperatures between 313 and 373 K. The systems used were water + carbon dioxide, aqueous surfactant solution + carbon dioxide, and Toco, a substance whose physical properties are roughly similar to those of {alpha}-Tocopherol + carbon dioxide. A distinctive change in the flooding mechanisms from liquid layer flooding to bubble column flooding was observed. The different liquids, water and Toco, showed the same flooding behavior, indicating that the influence of the density on the flooding behavior prevails over the influence of any other physical property of the liquid. The foamability of the surfactant solution decreased significantly with increasing pressure--its influence on the flooding behavior could not be proved. The liquid holdup ranged between 2% and 6%. The dry pressure drop adhered to the Ergun equation.

  11. Scale-up of counter-current chromatography: demonstration of predictable isocratic and quasi-continuous operating modes from the test tube to pilot/process scale.

    PubMed

    Sutherland, Ian; Hewitson, Peter; Ignatova, Svetlana

    2009-12-11

    Predictable scale-up from test tube derived distribution ratios and analytical-scale sample loading optimisation is demonstrated using a model sample system of benzyl alcohol and p-cresol in a heptane:ethyl acetate:methanol:water phase system with the new 18 L Maxi counter-current chromatography centrifuge. The versatility of having a liquid stationary phase with its high loading capacity and flexible operating modes is demonstrated at two different scales by separating and concentrating target compounds using a mixture of caffeine, vanillin, naringenin and carvone using a quasi-continuous technique called intermittent counter-current extraction.

  12. Mathematical model of quasiequilibrium counter-current solvent extraction of rare-earth metals with variable feed compositions

    SciTech Connect

    Pyartman, A.K.; Puzikov, E.A.; Kopyrin, A.A.

    1995-07-01

    A mathematical model is proposed for the distribution of trivalent rare-earth metals as a function of the number of contacts in quasiequilibrium counter-current solvent extraction with variable feed compositions. An algorithm for computer calculations is given. The model is used to select the optimal conditions for separating a didymium mixture.

  13. Pulsed counter-current ultrasound-assisted extraction and characterization of polysaccharides from Boletus edulis.

    PubMed

    You, Qinghong; Yin, Xiulian; Ji, Chaowen

    2014-01-30

    Four methods for extracting polysaccharides from Boletus edulis, namely, hot-water extraction, ultrasonic clearer extraction, static probe ultrasonic extraction, and pulsed counter-current probe ultrasonic extraction (CCPUE), were studied. Results showed that CCPUE has the highest extraction efficiency among the methods studied. Under optimal CCPUE conditions, a B. edulis polysaccharide (BEP) yield of 8.21% was obtained. Three purified fractions, BEP-I, BEP-II, and BEP-III, were obtained through sequential purification by DEAE-52 and Sephadex G-75 chromatography. The average molecular weights of BEP-I, BEP-II, and BEP-III were 10,278, 23,761, and 42,736 Da, respectively. The polysaccharides were mainly composed of xylose, mannose, galactose, and glucose; of these, mannose contents were the highest. The antioxidant activities of the BEPs were further investigated by measurement of their ability to scavenge DPPH and hydroxyl radicals as well as their reducing power. The results indicated that the BEPs have good antioxidant activity.

  14. Countercurrent extraction of soluble sugars from almond hulls and assessment of the bioenergy potential.

    PubMed

    Holtman, Kevin M; Offeman, Richard D; Franqui-Villanueva, Diana; Bayati, Andre K; Orts, William J

    2015-03-11

    Almond hulls contain considerable proportions (37% by dry weight) of water-soluble, fermentable sugars (sucrose, glucose, and fructose), which can be extracted for industrial purposes. The maximum optimal solids loading was determined to be 20% for sugar extraction, and the addition of 0.5% (w/v) pectinase aided in maintaining a sufficient free water volume for sugar recovery. A laboratory countercurrent extraction experiment utilizing a 1 h steep followed by three extraction (wash) stages produced a high-concentration (131 g/L fermentable sugar) syrup. Overall, sugar recovery efficiency was 88%. The inner stage washing efficiencies were compatible with solution equilibrium calculations, indicating that efficiency was high. The concentrated sugar syrup was fermented to ethanol at high efficiency (86% conversion), and ethanol concentrations in the broth were 7.4% (v/v). Thin stillage contained 233 g SCOD/L, which was converted to biomethane at an efficiency of 90% with a biomethane potential of 297 mL/g SCODdestroyed. Overall, results suggested that a minima of 49 gal (185 L) ethanol and 75 m(3) methane/t hulls (dry whole hull basis) are achievable.

  15. Countercurrent supercritical fluid extraction and fractionation of high-added-value compounds from a hexane extract of olive leaves.

    PubMed

    Tabera, Javier; Guinda, Angeles; Ruiz-Rodríguez, Alejandro; Señoráns, Francisco J; Ibáñez, Elena; Albi, Tomás; Reglero, Guillermo

    2004-07-28

    Countercurrent supercritical fluid extraction (CC-SFE) at a pilot scale plant was used for fractionation of high-added-value products from a raw extract of olive leaves in hexane. Compounds found in the raw extract were waxes, hydrocarbons, squalene, beta-carotene, triglycerides, alpha-tocopherol, beta-sitosterol, and alcohols. The CC-SFE extraction process was investigated according to a 2(3) full factorial experimental design using the following variables and ranges: extraction pressure, 75-200 bar; extraction temperature, 35-50 degrees C; and ethanol as modifier, 0-10%. Data were analyzed in terms of extraction yield, enrichment, recovery, and selectivity. Higher extraction yields were attained at 200 bar. For most of the compounds analyzed enrichment was attained at the same conditions, that is, 75 bar, 35 degrees C, and 10% ethanol. Hydrocarbons were usually recovered in the separators, whereas waxes and alpha-tocopherol remain in the raffinate. Selectivity data reveal that alpha-tocopherol is the most easily separable compound. The influence of the experimental factors on the recovery of all the compounds was studied by means of regression models. The best fitted model was attained for beta-sitosterol, with R2 = 99.25%. Copyright 2004 American Chemical Society

  16. Preparative separation of flavonoid glycosides in leaves extract of Ampelopsis grossedentata using high-speed counter-current chromatography.

    PubMed

    Du, Qizhen; Chen, Ping; Jerz, Gerold; Winterhalter, Peter

    2004-06-18

    Preparative separation of flavonoid glycosides in leaves extract of Ampelopsis grossedentata was conducted using high-speed counter-current chromatograph (HSCCC) with a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:6:1.5:7.5, v/v). In a single operation, 28 mg of 5,7-dihydroxy-3',4'-trihydroxyflavone-3-O-6''-rhamnose and 18 mg of 5,7-dihydroxy-3',4'-dihydroxyflavone-3-O-6''-rhamnose was obtained from 150 mg of the extract. The chemical structure of the two compounds was elucidated by electrospray ionization (EIS) MS and NMR.

  17. High-performance countercurrent chromatography separation of Peucedanum cervaria fruit extract for the isolation of rare coumarin derivatives.

    PubMed

    Skalicka-Woźniak, Krystyna; Mroczek, Tomasz; Kozioł, Ewelina

    2015-01-01

    For the first time, rare major and minor compounds from fruits of Peucedanum cervaria were isolated. High-performance countercurrent chromatography with two different solvent systems, heptane/ethyl acetate/methanol/water (3:2:3:2 and 2:1:2:1, v/v), was successfully used in the reversed-phase mode. A scale-up process from analytical to semipreparative in a very short time was developed. The structures of isolated compounds were evaluated by high-performance liquid chromatography with diode array detection and electrospray ionization mass spectrometry, gas chromatography with mass spectrometry, and one- and two-dimensional NMR spectroscopy. (8S,9R)-9-(3-Methylbutenoyloxy)-O-acetyl-8,9-dihydrooroselol (compound B), (8S,9R)-9-(2-methyl-Z-butenoyloxy)-O-acetyl-8,9-dihydrooroselol (edultin, compound C), and (8S,9R)-9-acetoxy-O-(2α-methylbutyryl)-8,9-dihydrooroselol (compound D) were obtained using heptane/ethyl acetate/methanol/water (2:1:2:1, v/v) in <40 min. The method yielded 4.6 mg of a mixture of compounds B and C (11:89) and 3.7 mg of compound D. These amounts were obtained from the crude extract (0.5 g) in a single run. Although the compounds are known, their isolation by countercurrent chromatography and the analysis of their relative stereochemistry by two-dimensional NMR spectroscopy have been performed for the first time. Additionally, heptane/ethyl acetate/methanol/water (3:2:3:2, v/v) led to the isolation of oxypeucedanin (1.2 mg; compound A). This is the first time that angular dihydrofuranocoumarin was isolated from plant extract by countercurrent chromatography.

  18. PREPARATIVE SEPARATION OF AXIFOLIN-3-GLUCOSIDE, HYPEROSIDE AND AMYGDALIN FROM PLANT EXTRACTS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY.

    PubMed

    Wei, Yun; Xie, Qianqian; Ito, Yoichiro

    2009-01-01

    High-speed countercurrent chromatography (HSCCC) was successfully used to isolate three bioactive compounds, i.e., amygdalin from bitter almond and taxifolin-3-glucoside and quercetin-3-galactoside (hyperoside) from water extract of Agrimonia pilosa Ledeb, respectively. From 1 g of the crude extract 65 mg of amygdalin was isolated at 97% purity using a two-phase solvent system composed of ethyl acetate-n-butanol-water (5:2:5, v/v) by preparative HSCCC. From a 400 mg amount of crude extract of Agrimonia pilosa Ledeb, 11 mg of taxifolin-3-glucoside and 8 mg of hyperoside were isolated at 96% purity using a two-phase solvent system composed of ethyl acetate-methanol-water (25:1:25, v/v) similarly by preparative HSCCC. The final structural identification was performed by MS, (1)H-NMR and (13)C-NMR Spectra.

  19. Combined microwave-assisted extraction and high-speed counter-current chromatography for separation and purification of xanthones from Garcinia mangostana.

    PubMed

    Fang, Lei; Liu, Yuqin; Zhuang, Huiyong; Liu, Wei; Wang, Xiao; Huang, Luqi

    2011-10-15

    A microwave-assisted extraction (MAE) method is presented for the extraction of xanthones, α-mangostin and γ-mangostin from Garcinia mangostana. The MAE conditions including extraction temperature, liquid/solid ratio, extraction time and concentration of ethanol were optimized with an orthogonal test, and 5 g sample was extracted with the optimized conditions. The crude extraction of MAE was successfully isolated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (0.8:0.8:1:0.6, v/v) in one-step separation. The separation yielded 75 mg of α-mangostin at 98.5% purity, and 16 mg of γ-mangostin at 98.1% purity from 360 mg crude extract of G. mangostana in less than 7h. The purity of the two xanthones was determined by HPLC. Their structures were further identified by ESI-MS, (1)H NMR and (13)C NMR. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. An economical and efficient technology for the extraction of resveratrol from peanut (Arachis hypogaea) sprouts by multi-stage countercurrent extraction.

    PubMed

    Zhang, Qianghua; Bian, Yanhong; Shi, Yingying; Zheng, Shangyong; Gu, Xu; Zhang, Danyan; Zhu, Xiufang; Wang, Xiaoli; Jiang, Dingyun; Xiong, Qingping

    2015-07-15

    In this paper, an economical and efficient technology for the extraction of resveratrol from peanut sprouts by multi-stage countercurrent extraction (MSCE) was investigated based on the alkaline extraction and acid precipitation method (AEAP). Firstly, the MSCE equipment and operation procedures were designed. Then, the optimal parameters of MSCE were obtained by using single-factor experiments and Box-Behnken design (BBD) as follows: extraction temperature of 46.6 °C, CaO to raw material ratio of 6:100, water to raw material ratio of 8.8:1 and extraction time of 51.7 min. Finally, the performance of MSCE was compared against the single pot extraction (SPE) under optimal conditions. The results demonstrated that MSCE was a time-saving, energy-saving, and cost-saving extraction technology for manufacturing resveratrol from peanut sprouts. Copyright © 2015 Elsevier Ltd. All rights reserved.

  1. Two-stage fractionation of polar alkaloids from Rhizoma coptidis by countercurrent chromatography considering the strategy of reactive extraction.

    PubMed

    Li, Yang; Cai, Fanfan; Zhang, Min; Zhang, Hongyang; Wang, Yuerong; Hu, Ping

    2015-01-23

    Separation of polar alkaloids by countercurrent chromatography (CCC) is challengeable due to their close partition behaviors in solvent system. In this paper, a two-stage method for isolation of epiberberine, jatrorrhizine, palmatine, coptisine, and berberine from Rhizoma coptidis was presented. The first stage separation performed on CCC was based on the principle of reactive extraction. Trifluoroacetic acid was acted as a modulator to selectively react with alkaloids, which changed their partition coefficients in solvent system. Purified epiberberine and other partially separated targets were eluted by ammonium adjusted mobile phase. In the second stage, four alkaloids were purified in pH-zone-refining CCC mode. All the targets collected were over 97% pure determined by HPLC. The method developed demonstrates performing of reactive extraction on standard CCC as an option for separation of polar alkaloids from medicinal plants.

  2. Extraction and preparative purification of tanshinones from Salvia miltiorrhiza Bunge by high-speed counter-current chromatography.

    PubMed

    Sun, Ailing; Zhang, Yongqing; Li, Aifeng; Meng, Zhaoling; Liu, Renmin

    2011-07-01

    A method for extraction and preparative separation of tanshinones from Salvia miltiorrhiza Bunge was successfully established in this paper. Tanshinones from Salvia miltiorrhiza Bunge were extracted using ethyl acetate as the extractant under reflux. The extracts were then purified by high speed counter-current chromatography (HSCCC) with light petroleum-ethyl acetate-methanol-water (6:4:6.5:3.5, v/v) as the two phase solvent system. The upper phase was used as the stationary phase and the lower phase as the mobile phase. 8.2mg of dihydrotanshinone I, 5.8 mg of 1,2,15,16-tetrahydrotanshiquinone, 26.3mg of cryptotanshinone, 16.2mg of tanshinone I, 25.6 mg of neo-przewaquinone A, 68.8 mg of tanshinone IIA and 9.3mg of miltirone were obtained from 400mg of extracts from Salvia miltiorrhiza Bunge in one-step HSCCC separation, with the purity of 97. 6%, 95.1%, 99.0%, 99.1%, 93.2%, 99.3% and 98.7%, respectively, as determined by HPLC area normalization method. Their chemical structures were identified by ¹H NMR.

  3. Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

    PubMed

    Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

    2017-05-15

    A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Semi-industrial isolation of salicin and amygdalin from plant extracts using slow rotary counter-current chromatography.

    PubMed

    Du, Qizhen; Jerz, Gerold; Ha, Yangchun; Li, Lei; Xu, Yuanjin; Zhang, Qi; Zheng, Qunxiong; Winterhalter, Peterb; Ito, Yoichiro

    2005-05-13

    Salicin in the bark extract of Salix alba and amygdalin in the fruit extract of Semen armeniacae were each separated by slow rotary counter-current chromatography (SRCCC). The apparatus was equipped with a 40-L column made of 17 mm i.d. convoluted Teflon tubing. A 500g amount of crude extract containing salicin at 13.5% was separated yielding 63.5 g of salicin at 95.3% purity in 20h using methyl tert-butyl ether-l-butanol (1:3) saturated by methanol-water (1:5) as a stationary phase and methanol-water (1:5) saturated by methyl tert-butyl ether-1-butanol (1:3) as a mobile phase. A 400g amount of crude extract containing amygdalin at 55.3% was isolated to yield 221.2g of amygdalin at 94.1% purity in 19h using ethyl acetate-1-butanol (1:2) saturated by water as a stationary phase and water saturated by ethyl acetate-1-butanol (1:2) as a mobile phase. The flow rate of the mobile phase was 50 ml/min. The results show that industrial SRCCC separation of salicin and amygdalin is feasible using a larger column at a higher flow rate of the mobile phase.

  5. Microwave-Assisted Extraction and Purification of Arctiin and Arctigenin from Fructus Arctii by High-Speed Countercurrent Chromatography.

    PubMed

    Lü, Haitao; Sun, Zhaoyun; Shan, Hu; Song, Jiying

    2016-03-01

    An efficient method for the rapid extraction, separation and purification of bioactive lignans, arctiin and arctigenin, from Fructus arctii by microwave-assisted extraction coupled with high-speed countercurrent chromatography was developed. The optimal extraction conditions of arctiin and arctigenin were evaluated by orthogonal array. Arctigenin could be converted from arctiin by hydrochloric acid hydrolysis. The separations were performed at a preparative scale with two-phase solvents composed of ethyl acetate-ethanol-water (5 : 1 : 5, v/v/v) for arctiin, and n-hexane-ethyl acetate-ethanol-water (4 : 4 : 3 : 4, v/v/v/v) for arctigenin. From 500 mg of crude extract sample, 122.3 mg of arctiin and 45.7 mg of arctigenin were obtained with the purity of 98.46 and 96.57%, and the recovery of 94.3 and 81.6%, respectively. Their structures were determined by comparison with the high-performance liquid chromatography retention time of standard substance as well as UV, FT-IR, electrospray ion source (ESI)-MS, (1)H-NMR and (13)C-NMR spectrum. According to the antioxidant activity assay, arctigenin had stronger 1,1-diphenyl-2-picrylhydrazyl free radicals scavenging activity. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. Purification of coenzyme Q10 from fermentation extract: high-speed counter-current chromatography versus silica gel column chromatography.

    PubMed

    Cao, Xue-Li; Xu, Ya-Tao; Zhang, Guang-Ming; Xie, Sheng-Meng; Dong, Ying-Mao; Ito, Yoichiro

    2006-09-15

    High-speed counter-current chromatography (HSCCC) is applied to the purification of coenzyme Q(10) (CoQ(10)) for the first time. CoQ(10) was obtained from a fermentation broth extract. A non-aqueous two-phase solvent system composed of heptane-acetonitrile-dichloromethane (12:7:3.5, v/v/v) was selected by analytical HSCCC and used for purification of CoQ(10) from 500 mg of the crude extract. The separation yielded 130 mg of CoQ(10) at an HPLC purity of over 99%. The overall results of the present studies show the advantages of HSCCC over an alternative of silica gel chromatography followed by recrystallization. These advantages extend to higher purity (97.8% versus 93.3%), recovery (88% versus 74.3%) and yield (26.4% versus 23.4%). An effort to avoid the toxic, expensive solvent CH(2)Cl(2) was unsuccessful, but at least its percentage is low in the solvent system.

  7. Separation of three phenolic high-molecular-weight compounds from the crude extract of Terminalia Chebula Retz. by ultrasound-assisted extraction and high-speed counter-current chromatography.

    PubMed

    Zou, Deng-lang; Chen, Tao; Li, Hong-mei; Chen, Chen; Zhao, Jing-yang; Li, Yu-lin

    2016-04-01

    This study presents an efficient strategy for separation of three phenolic compounds with high molecular weight from the crude extract of Terminalia chebula Retz. by ultrasound-assisted extraction and high-speed counter-current chromatography. The ultrasound-assisted extraction conditions were optimized by response surface methodology and the results showed the target compounds could be well enriched under the optimized extraction conditions. Then the crude extract was directly separated by high-speed counter-current chromatography without any pretreatment using n-hexane/ethyl acetate/methanol/water (1:7:0.5:3, v/v/v/v) as the solvent system. In 180 min, 13 mg of A, 18 mg of B, and 9 mg of C were obtained from 200 mg of crude sample. Their structures were identified as Chebulagic acid (A, 954 Da), Chebulinic acid (B, 956 Da), and Ellagic acid (C) by (1) H NMR spectroscopy.

  8. Dynamic pH junction high-speed counter-current chromatography coupled with microwave-assisted extraction for online separation and purification of alkaloids from Stephania cepharantha.

    PubMed

    Yuan, Zhiquan; Xiao, Xiaohua; Li, Gongke

    2013-11-22

    A simple and efficient dynamic pH junction high-speed counter-current chromatography method was developed and further applied to the online extraction, separation and purification of alkaloids from Stephania cepharantha by coupling with microwave-assisted extraction. Mineral acid and organic base were added into the mobile phase and the sample solution, respectively, leading to the formation of a dynamic pH junction in the column and causing focus of alkaloids. Selective focus of analytes can be achieved on the basis of velocity changes of the pH junction through appropriate selection of solvent systems and optimization of additive concentrations. The extract can be directly introduced into the HSCCC for the online extraction, separation and purification of alkaloids from S. cepharantha. Continuous separation can be easily achieved with the same solvent system. Under the optimum conditions, 6.0 g original sample was extracted with 60 mL of the upper phase of hexane-ethyl acetate-methanol-water (1:1:1:1, v/v/v/v) containing 10% triethylamine under 50 °C and 400 W irradiation power for 10 min, the extracts were directly separated and purified by high-speed counter-current chromatography. A total of 5.7 mg sinomenine, 8.3mg 6,7-di-O-acetylsinococuline, 17.9 mg berbamine, 12.7 mg isotetrandrine and 14.6 mg cepharanthine were obtained with purities of 96.7%, 93.7%, 98.7%, 97.3% and 99.3%, respectively. The online method provides good selectivity to ionizable compounds and improves the separation and purification efficiency of the high-speed counter-current chromatography technique. It has good potential for separation and purification of effective compounds from natural products.

  9. Pressurized liquid extraction coupled with countercurrent chromatography for systematic isolation of chemical constituents by preprogrammed automatic control.

    PubMed

    Zhang, Yuchi; Guo, Liping; Liu, Chunming; Fu, Zi' ao; Cong, Lei; Qi, Yanjuan; Li, Dongping; Li, Sainan; Wang, Jing

    2013-09-15

    Pressurized liquid extraction (PLE) coupled with high-speed countercurrent chromatography (HSCCC) via an automated procedure was firstly developed to extract and isolate ginsenosides from Panax quinquefolium. The experiments were designed under the guidance of mathematical model. The partition coefficient (K) values of the target compounds and resolutions of peak profiles were employed as the research indicators, and exponential function and binomial formulas were used to optimizing the solvent systems and flow rates of the mobile phases in a three-stage separation. In the first stage, ethyl acetate, n-butanol, and water were simultaneously pumped into the solvent separator at the flow rates 11.0, 10.0, and 23.0mL/min, respectively. The upper phase of the solvent system in the solvent separator was used as both the PLE solvent and the HSCCC stationary phase, followed by elution with the lower phase of the corresponding solvent system to separate the common ginsenosides. In the second and third stages, rare ginsenosides were first separated by elution with ethyl acetate, n-butanol, methanol, and water (flow rates: 20.0, 3.0, 5.0, and 11.0mL/min, respectively), then with n-heptane, n-butanol, methanol, and water (flow rates: 17.5, 6.0, 5.0, and 22.5mL/min, respectively). Nine target compounds, with purities exceeding 95.0%, and three non-target compounds, with purities above 84.48%, were successfully separated at the semipreparative scale in 450min. The separation results prove that the PLE/HSCCC parameters calculated via mathematical model and formulas were accurately and scientifically. This research has opened up great prospects for industrial automation application.

  10. Countercurrent extraction of soluble sugars from almond hulls and assessment of the bioenergy potential

    USDA-ARS?s Scientific Manuscript database

    Almond hulls contain considerable proportions (37 % by dry weight) of water soluble, fermentable sugars (sucrose, glucose, fructose) which can be extracted for industrial purposes. Optimization found that 20 % solids content was the maximum practical solids/liquor ratio for sugar extraction and tha...

  11. Circulating ultrasound-assisted extraction, countercurrent chromatography, and liquid chromatography for the simultaneous extraction, isolation, and analysis of the constituents of Uncaria tomentosa.

    PubMed

    Zhang, Yuchi; Liu, Chunming; Qi, Yanjuan; Li, Sainan; Pan, Yan; Li, Yuchun

    2015-04-03

    A hyphenated automated technique for the online extraction, isolation, analysis, and identification of natural organic compounds was established. Circulating ultrasound-assisted extraction (CUAE) was coupled with countercurrent chromatography (CCC), high performance liquid chromatography (HPLC), and a diode array detector (DAD). This approach was applied to the fractionation and purification of alkaloids from Uncaria tomentosa. A biphasic solvent system of chloroform-methanol-water (6:4:5, v:v:v) was used for the CUAE and CCC separation of compounds from 500 g of U. tomentosa. Two CUAE/CCC/HPLC/DAD modes were established. Either the upper aqueous phase or the lower organic phase of the solvent system could be used as the extraction solvent. The target compounds were extracted by CUAE, and the extract was pumped into a sample loop before being directly injected into the CCC column, or pre-purified using a flash chromatography column before injection. The target compounds were eluted using either the organic or aqueous phase of the solvent system and the fractions were monitored using a UV detector. The target fractions were collected by a sample loop via a six-port valve, and analyzed by HPLC/DAD for purity and structural identification. This system isolated of 8.2mg, 7.4 mg, and 12.9 mg of rhynchophylline, corynoxine, and corynoxine B with HPLC purities of 96.15%, 95.34%, and 95.49%, respectively via the first mode; and isolated 26.6 mg, 24.6 mg, and 45.3mg of rhynchophylline, corynoxine, and corynoxine B with a HPLC purities of 98.22%, 97.18%, and 97.93% via the second mode. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

  12. Analysis of antioxidants from orange juice obtained by countercurrent supercritical fluid extraction, using micellar electrokinetic chromatography and reverse-phase liquid chromatography.

    PubMed

    Simó, Carolina; Ibañez, Elena; Señoráns, Francisco J; Barbas, Coral; Reglero, Guillermo; Cifuentes, Alejandro

    2002-11-06

    Antioxidants from orange juice were determined by the combined use of countercurrent supercritical fluid extraction (CC-SFE) prior to reverse-phase liquic chromatography (RP-LC) or micellar electrokinetic chromatography (MEKC). The separation of antioxidants found in the SFE fractions was achieved by using a new MEKC method and a published LC procedure, both using diode array detection. The characterization of the different antioxidants was further done by LC-mass spectrometry. Advantages and drawbacks of LC and MEKC for analyzing the antioxidants found in the different orange extracts are discussed. Although LC yields higher peak area and slightly better reproducibility than MEKC, the latter technique provides information about the CC-SFE extracts in analysis times 7 times faster than by LC. This analysis advantage can be used for the quick adjustment of CC-SFE conditions, thus providing a fast way to obtain orange fractions of specific composition.

  13. Countercurrent Process for Lignin Separation from Biomass Matrix

    SciTech Connect

    Kiran Kadam; Ed Lehrburger

    2006-03-31

    The overall goal of the project was to test the concept of using a twin-screw extruder to conduct autohydrolysis pretreatment of wheat straw in countercurrent fashion, demonstrate in situ solid/liquid separation, and produce a low-lignin cellulose product using ethanol as an extractant. The resultant solid product is suitable for sugar production through enzymatic hydrolysis and for pulp applications. Pilot-scale equipment was used to successfully demonstrate the process both for sugar and pulp applications.

  14. An effective high-speed countercurrent chromatographic method for preparative isolation and purification of mollugin directly from the ethanol extract of the Chinese medicinal plant Rubia cordifolia.

    PubMed

    Lu, Yanbin; Liu, Rui; Sun, Cuirong; Pan, Yuanjiang

    2007-06-01

    The medicinal plant Rubia cordifolia has been used widely in traditional Chinese medicine (TCM) for its antibacterial, antioxidant and anti-inflammatory activities. In this study, a preparative high-speed countercurrent chromatography (HSCCC) method for isolation and purification of the bioactive component mollugin directly from the ethanol extract of R. cordifolia was successfully established by using light petroleum (bp 60-90 degrees C)/ethanol/diethyl ether/water as the two-phase solvent system. The upper phase of light petroleum/ethanol/diethyl ether/water (5:4:3:1 v/v) was used as the stationary phase of HSCCC. Under the optimum conditions, 46 mg of mollugin at 98.5% purity, as determined by HPLC, could be yielded from 500 mg of the crude extract in a single HSCCC separation. The peak fraction of HSCCC was identified by 1H NMR and 13C NMR.

  15. Preparative separation of bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze using steam distillation extraction and one step high-speed counter-current chromatography.

    PubMed

    Wei, Yun; Du, Jilin; Lu, Yuanyuan

    2012-10-01

    In order to utilize and control the invasive weed, bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze were studied. Steam distillation extraction and one step high-speed counter-current chromatography were applied to separate and purify the caryophyllene oxide, 7,11-dimethyl-3-methylene-1,6,10-dodecatriene, and caryophyllene from essential oil of Flaveria bidentis (L.) Kuntze. The two-phase solvent system containing n-hexane/acetonitrile/ethanol (5:4:3, v/v/v) was selected for the one step separation mode according to the partition coefficient values (K) of the target compounds and the separation factor (α). The purity of each isolated fraction after a single high-speed counter-current chromatography run was determined by high performance liquid chromatography. A 3.2 mg of caryophyllene oxide at a purity of 92.6%, 10.4 mg of 7,11-dimethyl-3-methylene-1,6,10-dodecatriene at a purity of 99.1% and 5.7 mg of caryophyllene at a purity of 98.8% were obtained from 200 mg essential oil of Flaveria bidentis (L.) Kuntze. The chemical structures of these components were identified by GC-MS, (1) H-NMR, and (13) C-NMR.

  16. Comparison of slide coagglutination test and countercurrent immunoelectrophoresis for detection of group B streptococcal antigen in cerebrospinal fluid from infants with meningitis.

    PubMed Central

    Webb, B J; Edwards, M S; Baker, C J

    1980-01-01

    The usefulness of Phadebact streptococcus reagents for the detection of group B streptococcal antigen in cerebrospinal fluid was evaluated in 54 infants with meningitis and in 22 normal infants. Antigens was detected by slide coagglutination in 19 (82.6%) and by countercurrent immunoelectrophoresis in 20 (87.0%) of 23 cerebrospinal fluid specimens from infants with group B streptococcal meningitis at admission. After initiation of antimicrobial therapy, antigen could be detected in 11 of 19 (by slide coagglutination) and 7 of 18 (by countercurrent immunoelectrophoresis) cerebrospinal fluids. False-positive reactions were noted by slide coagglutination in one infant with S. bovis meningitis and one with group B streptococcal bacteremia without meningitis; none occurred with countercurrent immunoelectrophoresis. The commercial availiability, simplicity, sensitivity (82.6%), and specificity (96.4%) of the Phadebact slide coaggluatination test for detecting group B streptococcal antigen in cerebrospinal fluid suggest that it may be useful for the early and rapid diagnosis of group B streptococcal meningitis. PMID:6991524

  17. Separation and purification of steroidal saponins from Paris polyphylla by microwave-assisted extraction coupled with countercurrent chromatography using evaporative light scattering detection.

    PubMed

    Xiao, Xiao-Hua; Yuan, Zhi-Quan; Li, Gong-Ke

    2014-03-01

    A method of microwave-assisted extraction coupled with countercurrent chromatography using evaporative light scattering detection was successfully developed for the separation and purification of steroidal saponins from Paris polyphylla. The main extraction conditions including microwave power, liquid/solid ratio, irradiation time, and extraction temperature were optimized using an orthogonal array design method. A suitable two-phase solvent system consisting of n-heptane/n-butanol/acetonitrile/water (10:19:6:20, v/v/v/v) was employed in the separation and purification of the extracts of P. polyphylla. A total of 7.1 mg polyphyllin VII, 4.3 mg gracillin, 9.2 mg dioscin, and 10.2 mg polyphyllin I were obtained from 1.5 g P. polyphylla in less than 300 min, the purities of which determined by HPLC were 96.7, 97.3, 98.7, and 98.6%, respectively. The identification and characterization of these compounds were performed by LC-ESI-MS and 1H NMR spectroscopy. The results demonstrated that the proposed method is feasible, economical and efficient for the extraction, separation and purification of effective compounds from natural products.

  18. Application of an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum.

    PubMed

    Chen, Tao; Liu, Yongling; Zou, Denglang; Chen, Chen; You, Jinmao; Zhou, Guoying; Sun, Jing; Li, Yulin

    2014-01-01

    This study presents an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum. A new solvent system composed of petroleum ether/ethyl acetate/water (4:2:1, v/v/v) was developed for the liquid-liquid extraction of the crude extract from R. tanguticum. As a result, emodin, aloe-emodin, physcion, and chrysophanol were greatly enriched in the organic layer. In addition, an efficient method was successfully established to separate and purify the above anthraquinones by high-speed counter-current chromatography and preparative HPLC. This study supplies a new alternative method for the rapid enrichment, separation, and purification of emodin, aloe-emodin, physcione, and chrysophanol.

  19. Countercurrent Chromatographic Separation of Lipophilic Ascorbic Acid Derivatives and Extract from Kadsura Coccinea Using Hydrophobic Organic-Aqueous Two-Phase Solvent Systems.

    PubMed

    Shinomiya, Kazufusa; Li, Heran; Kitanaka, Susumu; Ito, Yoichiro

    2009-01-01

    Countercurrent chromatographic (CCC) separation of lipophilic ascorbic acid derivatives and the crude extract from Kadsura Coccinea was performed using the type-J multilayer coil planet centrifuge with a hydrophobic organic-aqueous two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/aqueous 0.1% trifluoroacetic acid at the volume ratio of (5 : 5 : 6 : 2). The lipophilic ascorbic acid derivatives were separated in the order of L-ascrobyl 2,6-dibutyrate, L-ascorbyl 6-palmitate and L-ascorbyl 6-stearate by eluting the lower phase as the mobile phase, and L-ascorbyl 2,6-dipalmitate was separated by eluting the upper phase at the opposite direction. The above solvent system was then applied to the CCC separation of the extract prepared from K. coccinea. With lower phase mobile, the extract was mainly separated into two peaks corresponding to lignans and triterpenoids accordingly. The HPLC analysis of the fractions showed that the former peak contained Kadsulignan N, Schizandrin H and Neokadsuranin as lignans, and the latter peak, Micranoic acid A, Neokadsuranic acid B and beta-Sitosterol as triterpenoids. The overall results indicate that the hydrophobic organic-aqueous two-phase solvent system used in the present studies was useful for the CCC separation of lignans and triterpenoids present in the natural products.

  20. Countercurrent Chromatographic Separation of Lipophilic Ascorbic Acid Derivatives and Extract from Kadsura Coccinea Using Hydrophobic Organic-Aqueous Two-Phase Solvent Systems

    PubMed Central

    Shinomiya, Kazufusa; Li, Heran; Kitanaka, Susumu; Ito, Yoichiro

    2009-01-01

    Countercurrent chromatographic (CCC) separation of lipophilic ascorbic acid derivatives and the crude extract from Kadsura Coccinea was performed using the type-J multilayer coil planet centrifuge with a hydrophobic organic-aqueous two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/aqueous 0.1% trifluoroacetic acid at the volume ratio of (5 : 5 : 6 : 2). The lipophilic ascorbic acid derivatives were separated in the order of L-ascrobyl 2,6-dibutyrate, L-ascorbyl 6-palmitate and L-ascorbyl 6-stearate by eluting the lower phase as the mobile phase, and L-ascorbyl 2,6-dipalmitate was separated by eluting the upper phase at the opposite direction. The above solvent system was then applied to the CCC separation of the extract prepared from K. coccinea. With lower phase mobile, the extract was mainly separated into two peaks corresponding to lignans and triterpenoids accordingly. The HPLC analysis of the fractions showed that the former peak contained Kadsulignan N, Schizandrin H and Neokadsuranin as lignans, and the latter peak, Micranoic acid A, Neokadsuranic acid B and beta-Sitosterol as triterpenoids. The overall results indicate that the hydrophobic organic-aqueous two-phase solvent system used in the present studies was useful for the CCC separation of lignans and triterpenoids present in the natural products. PMID:20046934

  1. Pilot-Scale Test of Counter-Current Ion Exchange (CCIX) Using UOP IONSIV IE-911

    SciTech Connect

    Wester, Dennis W. ); Fondeur, Fernando; Dennis, Richard; Pike, Jeff; Leugemors, Robert K. ); Taylor, Paul W.; Hang, Thong

    2001-09-24

    A pilot-scale test of a moving-bed configuration of a UOP IONSIV? IE-911 ion-exchange column was performed over 17 days at Severn Trent Services facilities. The objectives of the test, in order of priority, were to determine if aluminosilicate precipitation caused clumping of IE-911 particles in the column, to observe the effect on aluminum-hydroxide precipitation of water added to a simulant-filled column, to evaluate the extent of particle attrition, and to measure the expansion of the mass-transfer zone under the influence of column pulsing. The IE-911 moved through the column with no apparent clumping during the test, although analytical results indicate that little if any aluminosilicate precipitated onto the particles. A precipitate of aluminum hydroxide was not produced when water was added to the simulant-filled column, indicating that this upset scenario is probably of little concern. Particle-size distributions remained relatively constant with time and position in the column, indicating that particle attrition was not significant. The expansion of the mass-transfer zone could not be accurately measured because of the slow loading kinetics of the IE-911 and the short duration of the test; however, the information obtained indicates that back-mixing of sorbent is not extensive.

  2. Systematic and efficient separation of 11 compounds from Rhizoma Chuanxiong via counter-current chromatography-solid phase extraction-counter-current chromatography hyphenation.

    PubMed

    Liu, Qi; Zhou, Jianda; Yu, Jingang; Xie, Yixi; Jiang, Xinyu; Yang, Hua; Chen, Xiaoqing

    2014-10-17

    A counter-current chromatography (CCC)-solid phase extraction (SPE)-CCC system with high preparative capacity was used to realize rapid one-run systematic separation of natural products, in which two six-port valves and the SPE cartridge served as the interface. In the orthogonal separation system, equal column volumes of TEB-300A and TEB-300B were employed for the first dimension (1st-D) and second dimension (2nd-D), respectively. An optimized solid-phase column (25 mm × 10 mm i.d.) packed with Oasis HLB materials acted as the trapping SPE column. The analyte-focusing effect of the trapping column associated with the considerable preparative capacities of 1st-D and 2nd-D using totally different solvent systems significantly facilitated this one-run systematic separation of natural product. Therefore, this proposed approach was successfully applied to isolate chemical compounds from the crude extract of Rhizoma Chuanxiong. As a result, 11 compounds with widely different polarities were separated by running CCC for only one time. More importantly, this hyphenated strategy could serve as a rapid and efficient systematic pathway for the separation of natural products.

  3. Combination of integrated expanded bed adsorption chromatography and countercurrent chromatography for the direct extraction and purification of pseudohypericin and hypericin from St. John's wort (Hypericum perforatum L.).

    PubMed

    Cai, Fanfan; Li, Yang; Zhang, Min; Zhang, Hongyang; Wang, Yuerong; Hu, Ping

    2015-08-01

    St. John's wort has attracted particular attention because of its beneficial effects as an antidepressant, antiviral, and anticancer agent. A method for the combination of integrated expanded bed adsorption chromatography and countercurrent chromatography for the simultaneous extraction and purification of pseudohypericin and hypericin from the herb is presented in this paper. Firstly, the constituents were extracted and directly adsorbed by expanded bed adsorption chromatography under optimal conditions. The stepwise elution was then performed by expanded bed adsorption chromatography that enriched the targets with higher purities and recoveries compared to other methods. Secondly, the eluent fractions from expanded bed adsorption chromatography were further separated by two-step high-speed countercurrent chromatography. A two-step high-speed countercurrent chromatography method with a biphasic solvent system composed of n-hexane/ethyl acetate/methanol/water with a volume ratio of 1:2:1:2 was performed by stepwise changing the flow rate of the mobile phase. Consequently, 5.6 mg of pseudohypericin and 2.2 mg of hypericin with purities of 95.5 and 95.0%, respectively, were successfully obtained from 40 mg of crude sample. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Separation of polyphenols and caffeine from the acetone extract of fermented tea leaves (Camellia sinensis) using high-performance countercurrent chromatography.

    PubMed

    Choi, Soo Jung; Hong, Yong Deog; Lee, Bumjin; Park, Jun Seong; Jeong, Hyun Woo; Kim, Wan Gi; Shin, Song Seok; Yoon, Kee Dong

    2015-07-21

    Leaves from Camellia sienensis are a popular natural source of various beverage worldwide, and contain caffeine and polyphenols derived from catechin analogues. In the current study, caffeine (CAF, 1) and three tea polyphenols including (-)-epigallocatechin 3-O-gallate (EGCg, 2), (-)-gallocatechin 3-O-gallate (GCg, 3), and (-)-epicatechin 3-O-gallate (ECg, 4) were isolated and purified by flow-rate gradient high-performance countercurrent chromatography (HPCCC) using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:9:1:9, v/v). Two hundred milligrams of acetone-soluble extract from fermented C. sinensis leaves was separated by HPCCC to give 1 (25.4 mg), 2 (16.3 mg), 3 (11.1 mg) and 4 (4.4 mg) with purities over 98%. The structures of 1-4 were elucidated by QTOF-MS, as well as 1H- and 13C-NMR, and the obtained data were compared to the previously reported values.

  5. Online polar two phase countercurrent chromatography×high performance liquid chromatography for preparative isolation of polar polyphenols from tea extract in a single step.

    PubMed

    Chen, Wei-Bin; Li, Shu-Qi; Chen, Long-Jiang; Fang, Mei-Juan; Chen, Quan-Cheng; Wu, Zhen; Wu, Yun-Long; Qiu, Ying-Kun

    2015-08-01

    Herein, we report an on-line two-dimensional system constructed by counter-current chromatography (CCC) coupling with preparative high-performance liquid chromatography (prep-HPLC) for the separation and purification of polar natural products. The CCC was used as the first dimensional isolation column, where an environmental friendly polar two-phase solvent system of isopropanol and 16% sodium chloride aqueous solution (1:1.2, v/v) was introduced for low toxicity and favorable resolution. In addition, by applying the stop-and-go flow technique, effluents pre-fractionated by CCC was further purified by a preparative column packed with octadecyl silane (ODS) as the second dimension. The interface between the two dimensions was comprised of a 6-port switching valve and an electronically controlled 2-position 10-port switching valve connected with two equivalent holding columns. To be highlighted here, this rationally designed interface for the purpose of smooth desalination, absorption and desorption, successfully solved the solvent compatibility problem between the two dimensional separation systems. The present integrated system was successfully applied in a one-step preparative separation and identification of 10 pure compounds from the water extracts of Tieguanyin tea (Chinese oolong tea). In short, all the results demonstrated that the on-line 2D CCC×LC method is an efficient and green approach for harvesting polar targets in a single step, which showed great promise in drug discovery.

  6. Counter-current motion in counter-current chromatography.

    PubMed

    Ito, Yoichiro

    2014-12-12

    After the CCC2012 meeting, I have received an e-mail regarding the terminology of "Countercurrent Chromatography". It stated that the term "Countercurrent" is a misnomer, because its stationary phase is motionless in the column and that the method should be renamed as liquid-liquid separations or centrifugal separations. However, it was found that these names are already used for various other techniques as found via Google search. The term "Countercurrent Chromatography" was originally made after two preparative methods of Countercurrent distribution and liquid Chromatography, both having no countercurrent motion in the column. However, it is surprising to find that this F1 hybrid method "Countercurrent Chromatography" can clearly exhibit countercurrent motion within the separation column in both hydrodynamic and hydrostatic equilibrium systems. This justifies that "Countercurrent Chromatography" is a proper term for this chromatographic method. Published by Elsevier B.V.

  7. Extraction and Separation of Vitisin D, Ampelopsin B and cis-Vitisin A from Iris lactea Pall. var. chinensis (Fisch.) Koidz by Alkaline Extraction-Acid Precipitation and High-Speed Counter-Current Chromatography.

    PubMed

    Lv, Huanhuan; Zhou, Wenna; Wang, Xiaoyan; Wang, Zhenhua; Suo, Yourui; Wang, Honglun

    2016-01-01

    Naturally occurring oligostilbenes are receiving more attention because they exhibit several beneficial effects for health, including hepatoprotective, antitumor, anti-adipogenic, antioxidant, antiaging, anti-inflammatory, anti-microbial, antiviral, immunosuppressive and neuroprotective activities. Thus, they could be of some potentially therapeutic values for several diseases. In this study, we adopted the alkaline extraction-acid precipitation (AEAP) method for extraction of oligostilbenes from the seed kernel of Iris lactea Then, the high-speed counter-current chromatography (HSCCC) was used for preparative isolation and purification of oligostilbenes from the AEAP extracts. Finally, three oligostilbenes, namely vitisin D (73 mg), ampelopsin B (25 mg) and cis-vitisin A (16 mg), were successfully fractionated by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (2:5:3:6, v/v/v/v) from 300 mg of the AEAP extracts in ∼ 190 min. The purities of the three isolated oligostilbenes were all over 95.0% as analyzed by high performance liquid chromatography. They all were isolated from I. lacteal for the first time.The method of AEAP for the preparation of the oligostilbene-enriched crude sample was simple, and the HSCCC technique for the isolation and purification of oligostilbenes was efficient.

  8. Orthogonal test design for optimization of suitable conditions to separate C-phycocyanin from Spirulina platensis by high-speed counter-current chromatography using reverse micelle solvent system.

    PubMed

    Yin, Lianhong; Xu, Lina; Yu, Kun; Zhen, Yuhong; Han, Xu; Xu, Youwei; Qi, Yan; Peng, Jinyong; Tan, Aiping

    2011-06-01

    High-speed counter-current chromatography (HSCCC) was applied to separate C-phycocyanin (C-PC) from Spirulina platensis in the article. The suitable conditions were optimized by an orthogonal test design (L(9)(3)(3)), including the stationary phase of reverse micelle solvent system (0.10 g/mL cetyltrimethylammonium bromide [CTAB]/isooctane-hexylalcohol), mobile phase A (0.05 mol/L sodium phosphate buffer, pH 4.0, containing 0.2 mol/L KCl) and mobile phase B (0.05 mol/L sodium phosphate buffer, pH 8.0, containing 0.4 mol/L KCl). Under the selected conditions, 78.7 mg protein was purified from 200 mg crude extract of S. platensis, and the purity of the product was 4.25 based on the absorbance ratio of A(620)/A(280) , which was increased 6.85 times compared with the crude extract. Then, the protein was identified to be C-PC by MALDI-TOF/TOF-MS and sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) analysis compared with the standard. The application of HSCCC used in the separation of C-PC from S. platensis was first reported in the article. Furthermore, three kinds of tumor cell lines including human hepatoma cell line SMMC-7721, human ovarian carcinoma cell line ES-2, and human lung adenocarcinoma cell line SPCA-1 were used to evaluate the anticancer activities of the separated product, and the results showed that the separated C-PC had excellent anti-tumor actions with the IC(50) values at 2.998, 4.854, and 8.423 μg/mL, respectively, for 48 h treatment. The outcome indicates that an effective method for C-PC purification by HSCCC has been established.

  9. Ionic Liquid-Based Ultrasonic-Assisted Extraction of Forsythosides from the Leaf of Forsythia suspensa (Thunb.) Vahl and Subsequent Separation and Purification by High-Speed Counter-Current Chromatography.

    PubMed

    Sun, Yinshi; Hou, Zhiguang; Liu, Zhengbo; Wang, Jianhua

    2016-09-01

    An ionic liquid-based ultrasonic-assisted extraction (ILUAE) method was developed for the extraction of the two forsythosides, namely forsythosides I and A from the leaf of Forsythia suspensa (Thunb.) Vahl. Three kinds of l-alkyl-3-methylimidazolium ionic liquids with different alkyl chain and anion were investigated. The results indicated that ionic liquids showed remarkable effects on the extraction yields of forsythosides. In addition, several ILUAE ultrasonic parameters, such as the solvent concentration, solvent to solid ratio and extraction time have been optimized. Under these optimal conditions (e.g., with 0.6 M [C6MIM]Br, solvent to solid ratio of 15 mL/g and extraction time of 10 min), this approach gained the highest extraction yields of forsythoside I (0.89%) and forsythoside A (10.74%). Meanwhile, forsythosides in the ILUAE extract were separated and purified successfully through the high-speed counter-current chromatography with a two-phase solvent system consisting of ethyl acetate-ethanol-acetic acid-water (4 : 1 : 0.25 : 6, v/v). 5.4 mg of forsythoside I and 59.7 mg of forsythoside A were obtained from 120 mg of the prepurified sample in one-step separation, with the purity of 96.1 and 97.9%, respectively, as determined by high-performance liquid chromatography. Their structures were identified by (1)H nuclear magnetic resonance (NMR) and (13)C NMR.

  10. Spiral Countercurrent Chromatography

    PubMed Central

    Ito, Yoichiro; Knight, Martha; Finn, Thomas M.

    2013-01-01

    For many years, high-speed countercurrent chromatography conducted in open tubing coils has been widely used for the separation of natural and synthetic compounds. In this method, the retention of the stationary phase is solely provided by the Archimedean screw effect by rotating the coiled column in the centrifugal force field. However, the system fails to retain enough of the stationary phase for polar solvent systems such as the aqueous–aqueous polymer phase systems. To address this problem, the geometry of the coiled channel was modified to a spiral configuration so that the system could utilize the radially acting centrifugal force. This successfully improved the retention of the stationary phase. Two different types of spiral columns were fabricated: the spiral disk assembly, made by stacking multiple plastic disks with single or four interwoven spiral channels connected in series, and the spiral tube assembly, made by inserting the tetrafluoroethylene tubing into a spiral frame (spiral tube support). The capabilities of these column assemblies were successfully demonstrated by separations of peptides and proteins with polar two-phase solvent systems whose stationary phases had not been well retained in the earlier multilayer coil separation column for high-speed countercurrent chromatography. PMID:23833207

  11. A combination strategy for extraction and isolation of multi-component natural products by systematic two-phase solvent extraction-(13)C nuclear magnetic resonance pattern recognition and following conical counter-current chromatography separation: Podophyllotoxins and flavonoids from Dysosma versipellis (Hance) as examples.

    PubMed

    Yang, Zhi; Wu, Youqian; Wu, Shihua

    2016-01-29

    Despite of substantial developments of extraction and separation techniques, isolation of natural products from natural resources is still a challenging task. In this work, an efficient strategy for extraction and isolation of multi-component natural products has been successfully developed by combination of systematic two-phase liquid-liquid extraction-(13)C NMR pattern recognition and following conical counter-current chromatography separation. A small-scale crude sample was first distributed into 9 systematic hexane-ethyl acetate-methanol-water (HEMWat) two-phase solvent systems for determination of the optimum extraction solvents and partition coefficients of the prominent components. Then, the optimized solvent systems were used in succession to enrich the hydrophilic and lipophilic components from the large-scale crude sample. At last, the enriched components samples were further purified by a new conical counter-current chromatography (CCC). Due to the use of (13)C NMR pattern recognition, the kinds and structures of major components in the solvent extracts could be predicted. Therefore, the method could collect simultaneously the partition coefficients and the structural information of components in the selected two-phase solvents. As an example, a cytotoxic extract of podophyllotoxins and flavonoids from Dysosma versipellis (Hance) was selected. After the systematic HEMWat system solvent extraction and (13)C NMR pattern recognition analyses, the crude extract of D. versipellis was first degreased by the upper phase of HEMWat system (9:1:9:1, v/v), and then distributed in the two phases of the system of HEMWat (2:8:2:8, v/v) to obtain the hydrophilic lower phase extract and lipophilic upper phase extract, respectively. These extracts were further separated by conical CCC with the HEMWat systems (1:9:1:9 and 4:6:4:6, v/v). As results, total 17 cytotoxic compounds were isolated and identified. In general, whole results suggested that the strategy was very

  12. Countercurrent flow absorber and desorber

    DOEpatents

    Wilkinson, W.H.

    1984-10-16

    Countercurrent flow absorber and desorber devices are provided for use in absorption cycle refrigeration systems and thermal boosting systems. The devices have increased residence time and surface area resulting in improved heat and mass transfer characteristics. The apparatuses may be incorporated into open cycle thermal boosting systems in which steam serves both as the refrigerant vapor which is supplied to the absorber section and as the supply of heat to drive the desorber section of the system. 9 figs.

  13. Countercurrent flow absorber and desorber

    DOEpatents

    Wilkinson, William H.

    1984-01-01

    Countercurrent flow absorber and desorber devices are provided for use in absorption cycle refrigeration systems and thermal boosting systems. The devices have increased residence time and surface area resulting in improved heat and mass transfer characteristics. The apparatuses may be incorporated into open cycle thermal boosting systems in which steam serves both as the refrigerant vapor which is supplied to the absorber section and as the supply of heat to drive the desorber section of the system.

  14. Rapid separation of cyanidin-3-glucoside and cyanidin-3-rutinoside from crude mulberry extract using high-performance countercurrent chromatography and establishment of a volumetric scale-up process.

    PubMed

    Choi, Soo-Jung; Choi, Janggyoo; Lee, Chang Uk; Yoon, Shin Hee; Bae, Soo Kyung; Chin, Young-Won; Kim, Jinwoong; Yoon, Kee Dong

    2015-06-01

    This study describes the rapid separation of mulberry anthocyanins; namely, cyanidin-3-glucoside and cyanidin-3-rutinoside, using high-performance countercurrent chromatography, and the establishment of a volumetric scale-up process from semi-preparative to preparative-scale. To optimize the separation parameters, biphasic solvent systems composed of tert-butyl methyl ether/n-butanol/acetonitrile/0.01% trifluoroacetic acid, flow rate, sample amount and rotational speed were evaluated for the semi-preparative-scale high-performance countercurrent chromatography. The optimized semi-preparative-scale high-performance countercurrent chromatography parameters (tert-butyl methyl ether/n-butanol/acetonitrile/0.01% trifluoroacetic acid, 1:3:1:5, v/v; flow rate, 4.0 mL/min; sample amount, 200-1000 mg; rotational speed, 1600 rpm) were transferred directly to a preparative-scale (tert-butyl methyl ether/n-butanol/acetonitrile/0.01% trifluoroacetic acid, 1:3:1:5, v/v; flow rate, 28 mL/min; sample amount, 5.0-10.0 g; rotational speed, 1400 rpm) to achieve separation results identical to cyanidin-3-glucoside and cyanidin-3-rutinoside. The separation of mulberry anthocyanins using semi-preparative high-performance countercurrent chromatography and its volumetric scale-up to preparative-scale was addressed for the first time in this report.

  15. Fractionation of wheat gliadins by counter-current distribution using an organic two-phase system.

    PubMed

    Truust, H; Johansson, G

    1998-06-26

    A liquid liquid two-phase system based on N,N-dimethylformamide and the two polymers, poly(ethyleneglycol) and Ficoll, useful for partitioning of hydrophobic proteins, has been developed. The system has been applied to a counter-current distribution process in 56 steps for analysing the heterogeneity of proteins extracted with N,N-dimethylformamide from wheat flour. The counter-current distribution patterns of proteins, extracted from eight kinds of wheat, have been analysed. The minimum number of hypothetical proteins necessary to describe the patterns was found to be seven. The relative amount of these hypothetical components varied among the wheats.

  16. Steady-state and non-steady state operation of counter-current chromatography devices.

    PubMed

    Kostanyan, Artak E; Ignatova, Svetlana N; Sutherland, Ian A; Hewitson, Peter; Zakhodjaeva, Yulya A; Erastov, Andrey A

    2013-11-01

    Different variants of separation processes based on steady-state (continuous sample loading) and non-steady state (batch) operating modes of CCC columns have been analyzed and compared. The analysis is carried out on the basis of the modified equilibrium cell model, which takes into account both mechanisms of band broadening - interphase mass transfer and axial mixing. A full theoretical treatment of the intermittent counter-current chromatography with short sample loading time is performed. Analytical expressions are presented allowing the simulation of the intermittent counter-current chromatography separations for various experimental conditions. Chromatographic and extraction separations have been compared and advantages and disadvantages of the two methods have been evaluated. Further technical development of the CCC machines to implement counter-current extraction separations is considered.

  17. Separation of the potential G-quadruplex ligands from the butanol extract of Zanthoxylum ailanthoides Sieb. & Zucc. by countercurrent chromatography and preparative high performance liquid chromatography.

    PubMed

    Han, Tian; Cao, Xueli; Xu, Jing; Pei, Hairun; Zhang, Hong; Tang, Yalin

    2017-07-21

    G-quadruplex DNA structure is considered to be a very attractive target for antitumor drug design due to its unique role in maintaining telomerase activities. Therefore, discovering ligands with high stability of G-quadruplex structure is of great interest. In this paper, pH-zone refining counter current chromatography (CCC) and preparative high performance liquid chromatography (HPLC) were employed for the separation of potent G-quadruplex ligands from the n-butanol fraction of the crude extract of Zanthoxylum ailanthoides, which is a traditional Chinese medicine recently found to display high inhibitory activity against several human cancer cells. The 75% aqueous ethanol extract of the stem bark of Z. ailanthoides and its fractions with petroleum ether, ethyl acetate and n-butanol displayed almost the same G-quadruplex stabilization ability. Here, pH-zone refining CCC was used for the separation of the alkaloids from the n-butanol fraction by a seldom used solvent system composed of dichloromethane-methanol-water (4:1:2.5) with 10mM TEA in the organic stationary phase as retainer and 10mM HCl in the aqueous mobile phase as eluter. Compounds I, II and III were obtained, with purity greater than 95%, in the quantities of 31.2, 94.0, and 26.4mg respectively from 300mg of lipophilic fraction within 80min, which were identified as three tetrahydroprotoberberines isolated for the first time in this plant. In addition, a phenylpropanoid glycoside compound IV (Syringin), an isoquinoline (Magnoflorine, V), and two lignin isomers (+)-lyoniresiol-3α-O-β-d-glucopyranoside (VI) and (-)-lyoniresinol -3α-O-β-D -glucopyranoside (VII) were isolated by traditional CCC together with preparative HPLC. Compounds IV, V, VI and VII were obtained, with purity greater than 95%, in the quantities of 4.0, 13.2, 6.7, and 6.5mg respectively from 960mg of hydrophilic fraction. Among the seven isolated compounds, tetrahydroprotoberberine I, II and III were found to display remarkable

  18. An Activity Model to Demonstrate Countercurrent Exchange.

    ERIC Educational Resources Information Center

    Benner, D. B.

    1998-01-01

    Discusses the scant coverage in high school textbooks of countercurrent exchange for the efficient movement of molecules across biological membranes. Argues that this is one of the most intriguing of the physiological adaptive mechanisms. (DDR)

  19. An Activity Model to Demonstrate Countercurrent Exchange.

    ERIC Educational Resources Information Center

    Benner, D. B.

    1998-01-01

    Discusses the scant coverage in high school textbooks of countercurrent exchange for the efficient movement of molecules across biological membranes. Argues that this is one of the most intriguing of the physiological adaptive mechanisms. (DDR)

  20. Isolation of chlorophylls a and b from spinach by counter-current chromatography.

    PubMed

    Jubert, Carole; Bailey, George

    2007-01-26

    A method for the isolation of chlorophylls from spinach by counter-current chromatography was developed. An initial extraction protocol was devised to avoid the notorious sensitivity of chlorophylls to degradation by light, heat, oxygen, acids and bases. Further purification and separation of chlorophylls a and b were achieved using counter-current chromatography. Chlorophyll structures and purities were established by HPLC, fast atom bombardment mass spectrometry and nuclear magnetic resonance. Purity was estimated to be >95% (100% by HPLC). Typical yields from 30g of freeze-dried spinach were 300mg of chlorophyll a and 100mg of chlorophyll b.

  1. Wave-driven Countercurrent Plasma Centrifuge

    SciTech Connect

    A.J. Fetterman and N.J. Fisch

    2009-03-20

    A method for driving rotation and a countercurrent flow in a fully ionized plasma centrifuge is described. The rotation is produced by radiofrequency waves near the cyclotron resonance. The wave energy is transferred into potential energy in a manner similar to the α channeling effect. The countercurrent flow may also be driven by radiofrequency waves. By driving both the rotation and the flow pattern using waves instead of electrodes, physical and engineering issues may be avoided.

  2. Inverse hydrochemical models of aqueous extracts tests

    SciTech Connect

    Zheng, L.; Samper, J.; Montenegro, L.

    2008-10-10

    Aqueous extract test is a laboratory technique commonly used to measure the amount of soluble salts of a soil sample after adding a known mass of distilled water. Measured aqueous extract data have to be re-interpreted in order to infer porewater chemical composition of the sample because porewater chemistry changes significantly due to dilution and chemical reactions which take place during extraction. Here we present an inverse hydrochemical model to estimate porewater chemical composition from measured water content, aqueous extract, and mineralogical data. The model accounts for acid-base, redox, aqueous complexation, mineral dissolution/precipitation, gas dissolution/ex-solution, cation exchange and surface complexation reactions, of which are assumed to take place at local equilibrium. It has been solved with INVERSE-CORE{sup 2D} and been tested with bentonite samples taken from FEBEX (Full-scale Engineered Barrier EXperiment) in situ test. The inverse model reproduces most of the measured aqueous data except bicarbonate and provides an effective, flexible and comprehensive method to estimate porewater chemical composition of clays. Main uncertainties are related to kinetic calcite dissolution and variations in CO2(g) pressure.

  3. Counter-current acid leaching process for copper azole treated wood waste.

    PubMed

    Janin, Amélie; Riche, Pauline; Blais, Jean-François; Mercier, Guy; Cooper, Paul; Morris, Paul

    2012-09-01

    This study explores the performance of a counter-current leaching process (CCLP) for copper extraction from copper azole treated wood waste for recycling of wood and copper. The leaching process uses three acid leaching steps with 0.1 M H2SO4 at 75degrees C and 15% slurry density followed by three rinses with water. Copper is recovered from the leachate using electrodeposition at 5 amperes (A) for 75 min. Ten counter-current remediation cycles were completed achieving > or = 94% copper extraction from the wood during the 10 cycles; 80-90% of the copper was recovered from the extract solution by electrodeposition. The counter-current leaching process reduced acid consumption by 86% and effluent discharge volume was 12 times lower compared with the same process without use of counter-current leaching. However, the reuse of leachates from one leaching step to another released dissolved organic carbon and caused its build-up in the early cycles.

  4. Isolation of bitter acids from hops (Humulus lupulus L.) using countercurrent chromatography.

    PubMed

    Dahlberg, Clinton J; Harris, Guy; Urban, Jan; Tripp, Matthew L; Bland, Jeffrey S; Carroll, Brian J

    2012-05-01

    Commercially available hops (Humulus lupulus L.) bitter acid extracts contain a mixture of three major congeners (co-, n-, and ad-) in addition to cis/trans diastereomers for each congener. Individual isomerized α-acids were obtained by the consecutive application of two separate countercurrent chromatography methods. First, individual isomerized α-acid congeners as a mixture of cis/trans diastereomers were obtained using a solvent system consisting of hexane and aqueous buffer. The second purification, capable of separating cis/trans diastereomers, was accomplished using a quaternary solvent system; an alternative procedure using β-cyclodextrin followed by countercurrent chromatography was also investigated. The NaBH(4) reduction of the purified isomerized α-acid compounds followed by countercurrent chromatography purification resulted in individual ρ iso α-acids (>95%). Similarly, catalytic hydrogenation of the purified isomerized α-acid compounds followed by countercurrent chromatography purification produced individual tetrahydro isomerized α-acids (>95%). Reported herein is a widely applicable approach that focuses on three critical variables--solvent system composition, pH, and buffer-to-sample ratio--that enable the efficient purification of individual bitter acids (≥95%) from commercially available hops extracts. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Purification of SoyScreen using critical carbon dioxide in a counter-current fractionation column

    USDA-ARS?s Scientific Manuscript database

    This research evaluated the use of critical carbon dioxide (CO2) in a counter-current fractionation column for purifying SoyScreen, a mixture of feruloylated glycerides. The process concept was tested using a mixture consisting of triacylglycerides (TAGs), ethyl ferulate and fatty acid ethyl esters...

  6. Solvent System Selection Strategies in Countercurrent Separation

    PubMed Central

    Liu, Yang; Friesen, J. Brent; McAlpine, James B.; Pauli, Guido F.

    2015-01-01

    The majority of applications in countercurrent and centrifugal partition chromatography, collectively known as countercurrent separation, are dedicated to medicinal plant and natural product research. In countercurrent separation, the selection of the appropriate solvent system is of utmost importance as it is the equivalent to the simultaneous choice of column and eluent in liquid chromatography. However, solvent system selection is often laborious, involving extensive partition and/or analytical trials. Therefore, simplified solvent system selection strategies that predict the partition coefficients and, thus, analyte behavior are in high demand and may advance both the science of countercurrent separation and its applications. The last decade of solvent system selection theory and applications are critically reviewed, and strategies are classified according to their data input requirements. This offers the practitioner an up-to-date overview of rationales and methods for choosing an efficient solvent system, provides a perspective regarding their accuracy, reliability, and practicality, and discusses the possibility of combining multiple methods for enhanced prediction power. PMID:26393937

  7. DNAPL Extraction/Oleofilter Test Report

    SciTech Connect

    White, R.M.; Hazel, C.

    1997-11-03

    A short term, low flow DNAPL extraction test was performed from May 29 - 30, 1997, to gather additional information about the possibility of using monitoring well MSB-3D to recover source contamination from the M-Area Aquifer. Although no visible, free phase material was recovered, the groundwater did contain perchloroethylene (PCE) at and above aqueous solubility. Improvements in the pumping configuration were identified for future trials. Prior to final treatment in the M1 air stripper, the groundwater was passed through an Oleofiltration system to evaluate its capability as a treatment technology. The Oleofilter uses a combination of conventional gravity assisted separation with coalescing plates and a final polishing filter using proprietary coated granules to remove hydrocarbons. Although free phase DNAPL was not processed through the Oleofilter, the groundwater containing high levels of dissolved PCE was treated efficiently. Initially the Oleofilter removed 99 percent of the PCE. As the test progressed, this removal rate decreased to 83 percent as the granules became loaded with PCE. Longer term testing, perhaps with periodic backflushing, is required to determine the effective granule capacity.

  8. Application of perfluorocarbons in novel continuous counter-current protein chromatography.

    PubMed

    Owen, R O; McCreath, G E; Chase, H A

    1996-01-01

    In this work the development of a process capable of extracting proteins from particulate-containing solutions (such as fermentation broths) on a continuous basis, and in which absorbent and process streams are contacted counter-currently is described. The process consists of four stages, required for the loading, washing, elution and regeneration of the adsorbent. Because of its counter-current nature, it has improved performance over existing (though not yet commercialized) continuous processes, which have been based on CSTR-type contractors (e.g. PERCAS (McCreath et al., 1993). The improved efficiency has been shown by carrying out extraction of lysozyme from a single component feed stream. The adsorbent used in this work is a Procion Red HE-7B-derivatized perfluorocarbon support, which has shown particular suitability for continuous processes due to its inherently high mechanical strength and high density. Results illustrating yields obtained using this equipment are presented and discussed.

  9. Efficient methods for isolating five phytochemicals from Gentiana macrophylla using high-performance countercurrent chromatography.

    PubMed

    Rho, Taewoong; Jung, Mila; Lee, Min Won; Chin, Young-Won; Yoon, Kee Dong

    2016-12-01

    Efficient high-performance countercurrent chromatography methods were developed to isolate five typical compounds from the extracts of Gentiana macrophylla. n-Butanol-soluble extract of G. macrophylla contained three hydrophilic iridoids, loganic acid (1), swertiamarin (2) and gentiopicroside (3), and a chromene derivative, macrophylloside D (4) which were successfully isolated by flow rate gradient (1.5 mL/min in 0-60 min, 5.0 mL/min in 60-120 min), and consecutive flow rate gradient HPCCC using n-butanol/0.1% aqueous trifluoroacetic acid (1:1, v/v, normal phase mode) system. The yields of 1-4 were 22, 16, 122, and 6 mg, respectively, with purities over 97% in a flow rate gradient high-performance countercurrent chromatography, and consecutive flow rate gradient high-performance countercurrent chromatography gave 1, 2, 3 (54, 41, 348 mg, respectively, purities over 97%) and 4 (13 mg, purity at 95%) from 750 mg of sample. The main compound in methylene chloride soluble extract, 2-methoxyanofinic acid, was successfully separated by n-hexane/ethyl acetate/methanol/water (4:6:4:6, v/v/v/v, flow-rate: 4 mL/min, reversed phase mode) condition. The structures of five isolates were elucidated by (1) H, (13) C NMR and ESI-Q-TOF-MS spectroscopic data which were compared with previously reported values.

  10. Experimental Investigation of Micro Counter-Current Flow Using High-Speed Micro PIV

    NASA Astrophysics Data System (ADS)

    Shinohara, Kyosuke; Sugii, Yasuhiko; Aota, Arata; Hibara, Akihide; Kitamori, Takehiko; Okamoto, Koji

    2004-11-01

    Microfluidic devices have been developed for chemical analysis as micro total analysis systems (u-TAS). To utilize scale merits, continuous-flow chemical processing and micro unit operations had been proposed as microfluidic device including mixing, phase confluence, solvent extraction, and so on. Recently, as one of these integrated chemical processes, micro counter-current flow system had been developed for highly efficient solvent extraction. The system consisted of oil flow and water flow in inverse direction. Using the system, more efficient extraction of Co (II) complex than theoretical prediction was confirmed. In this paper, in order to investigate the fundamental characteristics of the micro counter-current flow, velocity fields of the micro counter-current flow were measured using high-speed micro PIV system. The system consisted of a high-speed CMOS camera with an image intensifier, an epi-fluorescent microscope with an objective lens and a color filter, and a CW laser. The velocity fields of water were visualized for a time resolution of 500 us and a spatial resolution of 2.2 x 2.2 um. Transient micro vortices at the water-butyl acetate interface were captured clearly.

  11. Countercurrent Separation of Natural Products: An Update.

    PubMed

    Friesen, J Brent; McAlpine, James B; Chen, Shao-Nong; Pauli, Guido F

    2015-07-24

    This work assesses the current instrumentation, method development, and applications in countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC), collectively referred to as countercurrent separation (CCS). The article provides a critical review of the CCS literature from 2007 since our last review (J. Nat. Prod. 2008, 71, 1489-1508), with a special emphasis on the applications of CCS in natural products research. The current state of CCS is reviewed in regard to three continuing topics (instrumentation, solvent system development, theory) and three new topics (optimization of parameters, workflow, bioactivity applications). The goals of this review are to deliver the necessary background with references for an up-to-date perspective of CCS, to point out its potential for the natural product scientist, and thereby to induce new applications in natural product chemistry, metabolome, and drug discovery research involving organisms from terrestrial and marine sources.

  12. Countercurrent Separation of Natural Products: An Update

    PubMed Central

    2015-01-01

    This work assesses the current instrumentation, method development, and applications in countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC), collectively referred to as countercurrent separation (CCS). The article provides a critical review of the CCS literature from 2007 since our last review (J. Nat. Prod.2008, 71, 1489–1508), with a special emphasis on the applications of CCS in natural products research. The current state of CCS is reviewed in regard to three continuing topics (instrumentation, solvent system development, theory) and three new topics (optimization of parameters, workflow, bioactivity applications). The goals of this review are to deliver the necessary background with references for an up-to-date perspective of CCS, to point out its potential for the natural product scientist, and thereby to induce new applications in natural product chemistry, metabolome, and drug discovery research involving organisms from terrestrial and marine sources. PMID:26177360

  13. Separation of Catalpol from Rehmannia glutinosa Libosch. by High-Speed Countercurrent Chromatography

    PubMed Central

    Tong, Shengqiang; Chen, Lin; Zhang, Qing; Liu, Jian; Yan, Jizhong; Ito, Yoichiro

    2015-01-01

    The bioactive iridoid component catalpol was successfully separated by high-speed countercurrent chromatography with high purity from the partially purified crude extract of Rehmannia glutinosa. A polar two-phase solvent system composed of ethyl acetate–n-butanol–water (2:1:3, v/v/v) was selected by thin-layer chromatography and run on a preparative scale where the lower aqueous phase was used as the mobile phase with a head-to-tail elution mode. A 105 mg quantity of the partially purified sample containing 39.2% catalpol was loaded on a 270-mL capacity high-speed countercurrent separation column, yielding 35 mg of catalpol at 95.6% purity. The chemical structure of catalpol was determined by comparison with the high-performance liquid chromatography retention time of standard substance as well as the 1H NMR spectrum. PMID:25214499

  14. Solvent extraction of methane from simulated geopressured-geothermal fluids: sub-pilot test results

    SciTech Connect

    Quong, R.; Otsuki, H.H.; Locke, F.E.

    1982-01-14

    The extraction of methane dissolved in 15 wt % sodium chloride solution at 150/sup 0/C and 1000 psi has been demonstrated using n-hexadecane as the solvent in a sub-pilot scale extraction column operated in a continuous, countercurrent flow mode. Greater than 90% recovery of methane was obtained with solvent/brine mass flow ratios in the range of .040 to .045. The height of an ideal stage in this experimental Elgin-type spray column is estimated to be 1.5 ft. Application of this process on actual geopressured fluids is technically feasible, and when combined with direct drive injection disposal is economically attractive. Design and operation of a methane saturated-brine supply system to provide simulated geopressured fluid continuously at 150/sup 0/C and 1000 psi are also described.

  15. Combined application of macroporous resin and high speed counter-current chromatography for preparative separation of three flavonoid triglycosides from the leaves of Actinidia valvata Dunn.

    PubMed

    Qu, Liping; Xin, Hailiang; Su, Yonghua; Zheng, Guoyin; Ling, Changquan

    2012-04-01

    In this paper, the combined techniques of macroporous resin column chromatography and high speed counter-current chromatography were applied for preparative separation of flavonoid triglycosides from the leaves of Actinidia valvata Dunn, a famous Chinese medicinal herb. Twelve kinds of macroporous resins were investigated by adsorption and desorption tests. HPD-300 resin showed the maximum effectiveness and thus was selected for the first cleaning-up, in which 20% ethanol was used to remove the undesired constituents and 60% ethanol to elute the targets. The crude extract was then purified by high speed counter-current chromatography with the solvent system composed of ethyl acetate-n-butanol-water (2:1:3 and 4:1:5, v/v). Three flavonoid triglycosides, namely, kaempferol 3-O-α-L-rhamnopyranosyl-(1→3)-α-L-rhamnopyranosyl-(1→6)-β-D-galactopyranoside, kaempferol 3-O-α-L-rhamnopyranosyl-(1→3)-(4-O-acetyl-α-L-rhamnopyranosyl)-(1→6)-β-D-galactopyranoside and kaempferol 3-O-α-L-rhamnopyranosyl-(1→3)-(2,4-di-O-acetyl-α-L-rhamnopyranosyl)-(1→6)-β-D-galactopyranoside, were obtained. The purities of the separated compounds were all over 95% as determined by HPLC area normalization method. Their chemical structures were confirmed by UV, MS, NMR, and the standards.

  16. Triangular Helical Column for Centrifugal Countercurrent Chromatography

    PubMed Central

    Ito, Yoichiro; Yu, Henry

    2009-01-01

    Effective column space and stationary phase retention have been improved by changing the configuration of the helical column originally used for toroidal coil countercurrent chromatography. The use of an equilateral triangular core for the helix column doubles effective column space and retains the stationary phase over 40% of the total column capacity without increasing the column pressure. The present results suggest that the stationary phase retention and the peak resolution will be further improved using new column designs fabricated by a new technology called “laser sintering for rapid prototyping.” PMID:20046940

  17. Multilevel soil-vapor extraction test for heterogeneous soil

    SciTech Connect

    Widdowson, M.A.; Haney, O.R.; Reeves, H.W.; Aelion, C.M.; Ray, R.P.

    1997-02-01

    The design, performance, and analysis of a field method for quantifying contaminant mass-extraction rates and air-phase permeability at discrete vertical locations of the vadose zones are presented. The test configuration consists of a multiscreen extraction well and multilevel observation probes located in soil layers adjacent to the extraction well. For each level tested an inflatable packer system is used to pneumatically isolate a single screen in the extraction well, and a vacuum is applied to induce air flow through the screen. Test data include contaminant concentration and flow characteristics at the extraction well, and transient or steady-state pressure drawdown data at observation probes located at variable radii from the extraction well. The test method is applicable to the design of soil-vapor extraction (SVE) and bioventing remediation systems in a variety of geologic settings, particularly stratified soils. Application of the test method at a gasoline-polluted site located in the Piedmont physiographic region is described. Contaminant mass-extraction rates, expressed in terms of volatile hydrocarbons, varied from 0.16 to 14 kg/d.

  18. Centrifugal contractors for laboratory-scale solvent extraction tests

    SciTech Connect

    Leonard, R.A.; Chamberlain, D.B.; Conner, C.

    1995-12-31

    A 2-cm contactor (minicontactor) was developed and used at Argonne National Laboratory for laboratory-scale testing of solvent extraction flowsheets. This new contactor requires only 1 L of simulated waste feed, which is significantly less than the 10 L required for the 4-cm unit that had previously been used. In addition, the volume requirements for the other aqueous and organic feeds are reduced correspondingly. This paper (1) discusses the design of the minicontactor, (2) describes results from having applied the minicontactor to testing various solvent extraction flowsheets, and (3) compares the minicontactor with the 4-cm contactor as a device for testing solvent extraction flowsheets on a laboratory scale.

  19. Elution-extrusion counter-current chromatography for the separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix.

    PubMed

    Chu, Chu; Zhang, Shidi; Tong, Shengqiang; Li, Xingnuo; Li, Qingyong; Yan, Jizhong

    2015-09-01

    In this work, a simple and efficient protocol for the rapid separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix was developed by combining macroporous resin and elution-extrusion counter-current chromatography. The crude extract was firstly subjected to a D101 macroporous resin column eluted with water and a series of different concentrations of ethanol. Then, effluents of 30 and 95% ethanol were collected as sample 1 and sample 2 for further counter-current chromatography purification. Finally, a pair of isomers, 96 mg of compound 1 and 48 mg of compound 2 with purities of 91.1 and 96.2%, respectively, was isolated from 200 mg of sample 1. The other pair of isomers, 14 mg of compound 3 and 8 mg of compound 4 with purities of 93.6 and 88.9%, respectively, was isolated from 48 mg of sample 2. Their purities were analyzed by high-performance liquid chromatography, and their chemical structures were identified by mass spectrometry and (1) H NMR spectroscopy. Compared to a normal counter-current chromatography separation, the separation time and solvent consumption of elution-extrusion counter-current chromatography were reduced while the resolutions were still good. The established protocol is promising for the separation of natural products with great disparity of content in herbal medicines. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Synthesis of medronic acid monoesters and their purification by high-performance countercurrent chromatography or by hydroxyapatite

    PubMed Central

    Vepsäläinen, Jouko; Turhanen, Petri A

    2016-01-01

    Summary We achieved the synthesis of important medronic acid monoalkyl esters via the dealkylation of mixed trimethyl monoalkyl esters of medronic acid. Two methods were developed for the purification of medronic acid monoesters: 1) small scale (10–20 mg) purification by using hydroxyapatite and 2) large scale (tested up to 140 mg) purification by high-performance countercurrent chromatography (HPCCC). PMID:27829921

  1. Pneumatic pumping test for soil vacuum extraction

    SciTech Connect

    Cho, J.S.; DiGiulio, D.C.

    1992-08-01

    In-situ pneumatic pumping tests were performed to estimate the pneumatic permeability at a site containing soils contaminated with aviation gasoline. Determination of pneumatic permeability was necessary to evaluate soil-air discharge or pore volume exchange rates. Pressure propagation was measured in clustered vapor probes during the application of vacuum and positive pressure. An analytical solution for soil-air pressure distribution with a non-linear data fitting algorithm was adopted to obtain the pneumatic permeability from soil-air pressure distribution. Pneumatic pumping tests indicated substantially higher air discharge rates in the immediate vicinity of wells. The air discharge rate dissipated rapidly as distance from the wells increased. Application of increased vacuum or injection pressure resulted in substantially increased air flow in the immediate vicinity with small changes at a distance. This fact indicates that effective design should be based on air flow fields near wells, and the site specific design criteria should be determined with carefully conducted tests.

  2. Preparation of Simulated Waste Solutions for Solvent Extraction Testing

    SciTech Connect

    Peterson, R.A.

    2000-06-27

    Personnel will need to routinely prepare 0.5 to 10 L batches of salt solutions simulating Savannah River Site (SRS) soluble waste for solvent extraction testing. This report describes the compositions and preparation methods.

  3. Interior. Distillation apparatus used for extracting small test amounts of ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    Interior. Distillation apparatus used for extracting small test amounts of latex from plant fiber. - Thomas A. Edison Laboratories, Building No. 2, Main Street & Lakeside Avenue, West Orange, Essex County, NJ

  4. Countercurrent distribution of biological cells

    NASA Technical Reports Server (NTRS)

    Brooks, D. E.

    1982-01-01

    Detailed physiochemical studies of dextran/poly(ethylene glycol) (PEG) two phase systems were carried out to characterize and provide understanding of the properties of the systems which determine cell partition and the electrophoretic behavior of phase drops responsible for electric field driven phase separation. A detailed study of the electrostatic and electrokinetic potentials developed in these systems was carried out. The salt partition was examined both in phase systems and with pure polymer solutions via equilibrium dialysis and mechanism of sulfate, chloride and phosphate partition shown to be exclusion by PEG rather than binding by dextran. Salt partition was shown to have a strong effect on the polymer compositions of the phases as well, an effect which produces large changes in the interfacial tension between them. These effects were characterized and the interfacial tension shown to obey a power law with respect to its dependence on the length of the tie line describing the system composition on a phase diagram. The electrostatic potential differences measured via salt bridges were shown to obey thermodynamic predictions. The electrophoretic mobilities measured were utilized to provide a partial test of Levine's incomplete theory of phase drop electrophoresis. The data were consistent with Levine's expression over a limited range of the variables tested.

  5. Solvent Extraction External Radiation Stability Testing

    SciTech Connect

    Peterson, R.A.

    2001-01-05

    Personnel irradiated a number of samples of calixarene-based solvent. Analysis of these samples indicated that measurable loss of the calixarene occurred at very high doses (-16 Mrad). No measurable loss of the Cs-7SB modifier occurred at equivalent doses. The primary degradation product, 4-sec-butylphenol, observed during analysis of the samples came from degradation of the modifier. Also, TOA proved more susceptible to damage than the other components of the solvent. The total degradation of the solvent proved relatively minor. The consistent solvent performance, as indicated by the measured D Cs values, after exposure at high total doses serves as evidence of the relatively low degree of degradation of the solvent components. Additional tests employing internal irradiation of solvents with both simulants and SRS tank waste will be completed by the end of March 2001 to provide confirmation of the results presented herein.

  6. Multidimensional counter-current chromatographic system and its application.

    PubMed

    Yang, F; Quan, J; Zhang, T Y; Ito, Y

    1998-04-17

    A multidimensional counter-current chromatographic system was set up for the first time with two sets of high-speed counter-current chromatography instruments. This system was successfully applied to the preparative separation of isorhamnetin, kaempferol and quercetin from crude flavone aglycones of Ginkgo biloba L. and Hippophae rhamnoides L. with a two-phase solvent system composed of chloroform-methanol-water (4:3:2, v/v/v).

  7. Modeling of multicomponent countercurrent gas permeators

    SciTech Connect

    Kovvali, A.S.; Admassu, W. . Dept. of Chemical Engineering); Vemury, S. . Dept. of Chemical Engineering)

    1994-04-01

    Modeling of gas permeation in hollow-fiber or spiral wound modules necessitates considering the effect of permeate pressure variation along the module length which could have a significant effect on the prediction of the exit compositions and membrane area requirements depending on the membrane characteristics and module geometry. The transport equations governing the permeator performance are a set of coupled nonlinear differential equations. The complexity of the solution procedure for these equations increases with the number of components in the mixture and consideration of pressure variation. Thus, there is a need for simplified solution methodologies which could reduce the computational efforts. This paper presents a solution methodology to solve the multicomponent gas permeator transport equations in a countercurrent flow pattern, taking the permeate pressure variation into consideration. The present method yields analytical expressions for flow rates, permeate pressure, membrane area, and compositions along the length of the permeator.

  8. Multifraction separation in countercurrent chromatography (MCSGP).

    PubMed

    Krättli, Martin; Müller-Späth, Thomas; Morbidelli, Massimo

    2013-09-01

    The multicolumn countercurrent solvent gradient purification (MCSGP) process is a continuous countercurrent multicolumn chromatography process capable of performing three fraction separations while applying a linear gradient of some modifier. This process can then be used either for the purification of a single species from a multicomponent mixture or to separate a three component mixture in one single operation. In this work, this process is extended to the separation of multifractions, in principle with no limitation. To achieve this goal the MCSGP standard process is extended by introducing one extra separation section per extra fraction to be isolated. Such an extra separation section is realized in this work through a single additional column, so that a n fraction MCSGP process can be realized using a minimum of n columns. Two separation processes were considered to experimentally demonstrate the possibility of realizing a four-fraction MCSGP unit able to purify two intermediate products in a given multicomponent mixture. The first one was a model mixture containing four different proteins. The two proteins eluting in the center of the chromatogram were purified with yields equal to 95% for the early eluting and 92% for the later eluting one. The corresponding purities were 94% and 97%, respectively. Such performance was well superior to that of the batch operation with the same modifier gradient which for the same purity values could not achieve yields larger than 67% and 81%, respectively. Similar performance improvements were found for the second separation where two out of seven charge variants which constitute the mAb Cetuximab currently available on the market have been purified in one single operation using a four-fraction MCSGP unit. In this case, yields of 81% and 65% were obtained with purities of 90% and 89%, respectively. These data compare well with the corresponding data from batch chromatography where with the same gradient and for the same

  9. Use of two-stage membrane countercurrent cascade for natural gas purification from carbon dioxide

    NASA Astrophysics Data System (ADS)

    Kurchatov, I. M.; Laguntsov, N. I.; Karaseva, M. D.

    2016-09-01

    Membrane technology scheme is offered and presented as a two-stage countercurrent recirculating cascade, in order to solve the problem of natural gas dehydration and purification from CO2. The first stage is a single divider, and the second stage is a recirculating two-module divider. This scheme allows natural gas to be cleaned from impurities, with any desired degree of methane extraction. In this paper, the optimal values of the basic parameters of the selected technological scheme are determined. An estimation of energy efficiency was carried out, taking into account the energy consumption of interstage compressor and methane losses in energy units.

  10. Separation of salidroside from Rhodiola crenulata by high-speed counter-current chromatography.

    PubMed

    Han, Xiao; Zhang, Tianyou; Wei, Yun; Cao, Xueli; Ito, Yoichiro

    2002-09-20

    High-speed counter-current chromatography (HSCCC) was used to purify salidroside from an extract of Rhodiola crenulata with two steps using a two-phase solvent system composed of ethyl acetate-n-butanol-water (1:4:5, v/v) in the first run and chloroform-methanol-isopropanol-water (5:6:1:4) in the second run. The method yielded 21.9 mg of salidroside from 1.216 g of the crude sample at 98% purity determined by HPLC analyses. Identification was performed by 1H NMR, 13C NMR, and MS.

  11. Electrochemical corrosion testing of fasteners in extracts of treated wood

    Treesearch

    Samuel L. Zelinka; Douglas R. Rammer; Donald S. Stone

    2008-01-01

    A recent change in wood preservatives has highlighted the need for a rapid, quantitative test to measure the corrosion rates of metals in contact with treated wood that could be used to evaluate new fasteners or new wood preservatives. A new method was developed where polarisation resistance tests were conducted on fasteners exposed to a water extract of wood treated...

  12. RESULTS OF THE EXTRACTION-SCRUB-STRIP TESTING USING AN IMPROVED SOLVENT FORMULATION AND SALT WASTE PROCESSING FACILITY SIMULATED WASTE

    SciTech Connect

    Peters, T.; Washington, A.; Fink, S.

    2012-01-09

    The Office of Waste Processing, within the Office of Technology Innovation and Development, is funding the development of an enhanced solvent - also known as the next generation solvent (NGS) - for deployment at the Savannah River Site to remove cesium from High Level Waste. The technical effort is a collaborative effort between Oak Ridge National Laboratory (ORNL) and Savannah River National Laboratory (SRNL). As part of the program, the Savannah River National Laboratory (SRNL) has performed a number of Extraction-Scrub-Strip (ESS) tests. These batch contact tests serve as first indicators of the cesium mass transfer solvent performance with actual or simulated waste. The test detailed in this report used simulated Tank 49H material, with the addition of extra potassium. The potassium was added at 1677 mg/L, the maximum projected (i.e., a worst case feed scenario) value for the Salt Waste Processing Facility (SWPF). The results of the test gave favorable results given that the potassium concentration was elevated (1677 mg/L compared to the current 513 mg/L). The cesium distribution value, DCs, for extraction was 57.1. As a comparison, a typical D{sub Cs} in an ESS test, using the baseline solvent formulation and the typical waste feed, is {approx}15. The Modular Caustic Side Solvent Extraction Unit (MCU) uses the Caustic-Side Solvent Extraction (CSSX) process to remove cesium (Cs) from alkaline waste. This process involves the use of an organic extractant, BoBCalixC6, in an organic matrix to selectively remove cesium from the caustic waste. The organic solvent mixture flows counter-current to the caustic aqueous waste stream within centrifugal contactors. After extracting the cesium, the loaded solvent is stripped of cesium by contact with dilute nitric acid and the cesium concentrate is transferred to the Defense Waste Processing Facility (DWPF), while the organic solvent is cleaned and recycled for further use. The Salt Waste Processing Facility (SWPF), under

  13. Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of caged polyprenylated xanthones from gamboge.

    PubMed

    Xu, Min; Fu, Wenwei; Zhang, Baojun; Tan, Hongsheng; Xiu, Yanfeng; Xu, Hongxi

    2016-02-01

    An efficient method for the preparative separation of four structurally similar caged xanthones from the crude extracts of gamboge was established, which involves the combination of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography for the first time. pH-zone-refining counter-current chromatography was performed with the solvent system composed of n-hexane/ethyl acetate/methanol/water (7:3:8:2, v/v/v/v), where 0.1% trifluoroacetic acid was added to the upper organic stationary phase as a retainer and 0.03% triethylamine was added to the aqueous mobile phase as an eluter. From 3.157 g of the crude extract, 1.134 g of gambogic acid, 180.5 mg of gambogenic acid and 572.9 mg of a mixture of two other caged polyprenylated xanthones were obtained. The mixture was further separated by conventional high-speed counter-current chromatography with a solvent system composed of n-hexane/ethyl acetate/methanol/water (5:5:10:5, v/v/v/v) and n-hexane/methyl tert-butyl ether/acetonitrile/water (8:2:6:4,v/v/v/v), yielding 11.6 mg of isogambogenic acid and 10.4 mg of β-morellic acid from 218.0 mg of the mixture, respectively. The purities of all four of the compounds were over 95%, as determined by high-performance liquid chromatography, and the chemical structures of the four compounds were confirmed by electrospray ionization mass spectrometry and NMR spectroscopy. The combinative application of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography shows great advantages in isolating and enriching the caged polyprenylated xanthones.

  14. COUNTERCURRENT FLOW LIMITATION EXPERIMENTS AND MODELING FOR IMPROVED REACTOR SAFETY

    SciTech Connect

    Vierow, Karen

    2008-09-26

    This project is investigating countercurrent flow and “flooding” phenomena in light water reactor systems to improve reactor safety of current and future reactors. To better understand the occurrence of flooding in the surge line geometry of a PWR, two experimental programs were performed. In the first, a test facility with an acrylic test section provided visual data on flooding for air-water systems in large diameter tubes. This test section also allowed for development of techniques to form an annular liquid film along the inner surface of the “surge line” and other techniques which would be difficult to verify in an opaque test section. Based on experiences in the air-water testing and the improved understanding of flooding phenomena, two series of tests were conducted in a large-diameter, stainless steel test section. Air-water test results and steam-water test results were directly compared to note the effect of condensation. Results indicate that, as for smaller diameter tubes, the flooding phenomena is predominantly driven by the hydrodynamics. Tests with the test sections inclined were attempted but the annular film was easily disrupted. A theoretical model for steam venting from inclined tubes is proposed herein and validated against air-water data. Empirical correlations were proposed for air-water and steam-water data. Methods for developing analytical models of the air-water and steam-water systems are discussed, as is the applicability of the current data to the surge line conditions. This report documents the project results from July 1, 2005 through June 30, 2008.

  15. Factors influencing extract of Hibiscus sabdariffa staining of rat testes.

    PubMed

    Bassey, R B; Bakare, A A; Peter, A I; Oremosu, A A; Osinubi, A A

    2012-08-01

    Some plant extracts can be used in biology and medicine to reveal or identify cellular components and tissues. We investigated the effects of time and concentration on staining of histological sections of rat testes by an acidified extract of Hibiscus sabdariffa. An ethanolic extract of H. sabdariffa was diluted using 1% acetic acid in 70% ethanol to stain histological sections of testes at concentrations of 0.2, 0.1 and 0.05 g/ml for 5, 10, 15, 30, 45 and 60 min. The sections of testes were stained deep red. The staining efficiency of H. sabdariffa was greater at a high concentration and required less time to achieve optimal staining. H. sabdariffa is a strongly basic dye that can be used for various diagnostic purposes. Staining time and concentration must be considered to achieve optimal results.

  16. A new application of an aqueous diphase solvent system in one-step preparation of polysaccharide from the crude water extract of Radix Astragali by high-speed counter-current chromatography.

    PubMed

    Yin, Jun-Yi; Jiang, Zhi-Hong; Yu, Hua; Xie, Ming-Yong; Hsiao, Wen-Luan; Lu, Ai-Ping; Han, Quan-Bin

    2012-11-02

    Polysaccharide's purification remains challenge to separation technology. Conventional methods involve time-consuming and complicated operations and always cause significant variation in the isolates' chemistry. This paper reports an aqueous diphase solvent system, namely PEG1000-MgSO(4)-H(2)O, which succeeded in one-step CCC separation of a polysaccharide (43 mg) from the water extract (1.67 g) of Radix Astragali. The solvent composition was set as 12:16:72 (w/w/w) of which the lower phase was used as the mobile phase at a flow rate of 0.8 mL/min in a 1000 mL column. The purified polysaccharide bears an average molecular weight of 1095 kDa and consists of galacturonic acid (76.5%), galactose (7.7%), arabinose (4.2%) and glucose (5.0%). Methylation analysis result showed it was composed of 58.4% of 1,4-linked Glcp, 11.8% of T-linked Araf, 10.5% of T-linked Glcp, 9.1% of 1,4,6-linked Galp and 5.1% of 1,3,6-linked Galp, etc. This success shows a short way between the crude water extract and purified polysaccharides, which minimizes the chemical variation caused by purification methods.

  17. Studies of extraction, storage, and testing of pine pollen

    Treesearch

    J. W. Duffield

    1953-01-01

    This report assembles the results of a number of small exploratory studies on the extraction, storage, and viability testing of pollen of several species of pines. These studies indicate clearly the need for more knowledge of the physiology of pollen — particularly of the relation between atmospheric humidity at the time of pollen shedding and the subsequent reactions...

  18. AGS new fast extraction system and the single bunch extraction test

    SciTech Connect

    Weng, W.T.

    1983-01-01

    For the neutrino physics program and for the CBA injection, a new fast extraction system has been implemented to improve the extraction efficiency and the quality of the extracted beam. Central to the new system is a new fast kicker, placed at the H5 straight section, capable of rising between bunches, t/sub r/ < 170 nsec, and staying constant for 2.6 ..mu..sec with flat top ripple less than +-1.5%. So far, the system has been operated for longer than 3000 hours and routinely extracts 10/sup 13/ ppp at 99% efficiency. Experiment 745 on QCD test requires a single AGS bunch of 40 nsec. For this purpose another fast kicker was placed at the E5 straight section and powered by a new pulser to produce a half sinusoidal pulse with both a rise and fall time of 200 nsec. A single AGS bunch was extracted through the slow beam channel at 22 GeV/c leaving the remaining 11 bunches undisturbed which continued to be accelerated to 29.4 GeV/c and extracted by the H5 kicker through the fast beam channel. Because the ring circumference ratio of CBA to the AGS is 4-3/4, some of the injected beam from the AGS has to contain 11 bunches instead of 12; consequently, this single bunch extraction mode will also be used for CBA injection.

  19. Separation and purification of five alkaloids from Aconitum duclouxii by counter-current chromatography.

    PubMed

    Wang, Yarong; Cai, Shining; Chen, Yang; Deng, Liang; Zhou, Xumei; Liu, Jia; Xu, Xin; Xia, Qiang; Lin, Mao; Zhang, Jili; Huang, Weili; Wang, Wenjun; Xiang, Canhui; Cui, Guozhen; Du, Lianfeng; He, Huan; Qi, Baohui

    2015-07-01

    C19 -diterpenoid alkaloids are the main components of Aconitum duclouxii Levl. The process of separation and purification of these compounds in previous studies was tedious and time consuming, requiring multiple chromatographic steps, thus resulted in low recovery and high cost. In the present work, five C19 -diterpenoid alkaloids, namely, benzoylaconine (1), N-deethylaconitine (2), aconitine (3), deoxyaconitine (4), and ducloudine A (5), were efficiently prepared from A. duclouxii Levl (Aconitum L.) by ethyl acetate extraction followed with counter-current chromatography. In the process of separation, the critical conditions of counter-current chromatography were optimized. The two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water/NH3 ·H2 O (25%) (1:1:1:1:0.1, v/v) was selected and 148.2 mg of 1, 24.1 mg of 2, 250.6 mg of 3, 73.9 mg of 4, and 31.4 mg of 5 were obtained from 1 g total Aconitum alkaloids extract, respectively, in a single run within 4 h. Their purities were found to be 98.4, 97.2, 98.2, 96.8, and 96.6%, respectively, by ultra-high performance liquid chromatography analysis. The presented separation and purification method was simple, fast, and efficient, and the obtained highly pure alkaloids are suitable for biochemical and toxicological investigation.

  20. High-speed counter-current chromatographic separation of phytosterols.

    PubMed

    Schröder, Markus; Vetter, Walter

    2011-07-01

    Phytosterols are bioactive compounds which occur in low concentrations in plant oils. Due to their beneficial effects on human health, phytosterols have already been supplemented to food. Commercial phytosterol standards show insufficient purity and/or are very expensive. In this study, we developed a high-speed counter-current chromatography (HSCCC) method for the fractionation and analysis of a commercial crude β-sitosterol standard (purity ∼60% according to supplier). Different solvent systems were tested in shake-flask experiments, and the system n-hexane/methanol/aqueous silver nitrate solution (34/24/1, v/v/v) was finally used for HSCCC fractionation. About 50 mg phytosterols was injected and distributed into 57 fractions. Selected fractions were condensed and re-injected into the HSCCC system. This measure provided pure sitostanol (>99%) and β-sitosterol (∼99%), as well as a mixture of campesterol and stigmasterol without further phytosterols. An enriched HSCCC fraction facilitated the mass spectrometric analysis of further 11 minor phytosterols (after trimethylsilylation). It was also shown that the commercial product contained about 0.3% carotinoids which eluted without delay into an early HSCCC fraction and which were separated from the phytosterols.

  1. Interannual variability of the South Indian Countercurrent

    NASA Astrophysics Data System (ADS)

    Menezes, Viviane V.; Phillips, Helen E.; Vianna, Marcio L.; Bindoff, Nathaniel L.

    2016-05-01

    In the present work, we investigate the interannual variability of the South Indian Countercurrent (SICC), a major and still understudied current of the Indian Ocean circulation. To characterize the interannual variability of the SICC, four different data sets (altimetry, GLORYS, OFAM3, and SODA) are analyzed using multiple tools, which include Singular Spectrum Analysis and wavelet methods. The quasi-biennial band dominates the SICC low-frequency variance, with the main peak in the 1.5-1.8 year interval. A secondary peak (2.1-2.5 year) is only found in the western basin. Interannual and decadal-type modulations of the quasi-biennial signal are also identified. In addition, limitations of SODA before the 1960s in the SICC region are revealed. Within the quasi-biennial band, the SICC system presents two main patterns with a multiple jet structure. One pattern is characterized by a robust northern jet, while in the other the central jet is well developed and northern jet is weaker. In both patterns, the southern jet has always a strong signature. When the northern SICC jet is stronger, the northern cell of the subtropical gyre has a triangular shape, with its southern limb having a strong equatorward slant. The quasi-biennial variability of the SICC is probably related to the Indian Ocean tropical climate modes that are known to have a strong biennial characteristic.

  2. Extraction of manganese by alkyl monocarboxylic acid in a mixed extractant from a leaching solution of spent lithium-ion battery ternary cathodic material

    NASA Astrophysics Data System (ADS)

    Joo, Sung-Ho; Shin, Dongju; Oh, ChangHyun; Wang, Jei-Pil; Shin, Shun Myung

    2016-02-01

    We investigate the separation of manganese by an antagonistic effect from a leaching solution of ternary cathodic material of spent lithium-ion batteries that contain 11,400 mg L-1 Co, 11,700 mg L-1 Mn, 12,200 mg L-1 Ni, and 5300 mg L-1 Li using a mixture of alkyl monocarboxylic acid and di-(2-ethylhexyl)phosphoric acid extractants. pH isotherm, distribution coefficient, separation factor, McCabe-Thiele diagram, selective scrubbing, and countercurrent extraction tests are carried out to prove an antagonistic effect and to recover manganese using alkyl monocarboxylic in the mixed extractant. Slope analysis is used to determine the extraction mechanism between a mixture of extractants and valuable metals. An increasing concentration of alkyl monocarboxylic acid in the mixture of extractants results in a decrease in distribution coefficient of cobalt and manganese, however, the separation factor value (β(Mn/Co)) increases at pH 4.5. This is caused by slope analysis where alkyl monocarboxylic acid disrupts the extraction mechanism between di-(2-ethylhexyl)phosphoric acid and cobalt. Finally, continuous countercurrent extraction in a mini-plant test demonstrate the feasibility of manganese recovery from cobalt, nickel, and lithium.

  3. Caustic-Side Solvent Extraction Full-Scale Test

    SciTech Connect

    Lentsch, R.D.; Stephens, A.B.; Bartling, K.E.; Singer, S.A.

    2008-07-01

    A Full-Scale Test (FST) program was performed by Parsons and its team members General Atomics and Energy Solutions to assess the performance of full-scale centrifugal contactors specified for the Department of Energy Salt Waste Processing Facility (SWPF). The SWPF, to be located at the Savannah River Site (SRS) in Aiken, South Carolina, will remove highly radioactive waste constituents, principally actinides, strontium (Sr), and cesium (Cs) radionuclides, from salt waste solutions currently stored in SRS high-level waste tanks. Caustic-side Solvent Extraction (CSSX) removes Cs from waste feed that has been treated upstream to remove actinides and Sr. CSSX uses a custom solvent to extract Cs from the salt solution in a series of single stage centrifugal contactors. The test system comprised (a) eleven 25.4 cm (10'') full-scale contactors (versus 36 in SWPF) for the extraction, scrub, strip, and wash stages; (b) two solvent recovery coalescers; and (c) the associated hardware and control system, packaged in four skid mounted modules. This paper describes the results of tests performed to define both hydraulic performance parameters (maximum hydraulic capacity and phase carryover) and solvent extraction performance parameters (Cs mass transfer efficiencies) using simulated SWPF waste and actual CSSX solvent. The test results confirmed key design features of the CSSX process and, as a consequence, the use of CSSX in the SWPF. In conclusion: Total throughput was initially limited to 85% of maximum flow during FST. Minor system modifications performed prior to mass transfer testing series resulted in the realization of 100% throughput. The 100% flow equates to slightly more than 35.6 x 10{sup 6} L/yr (9.4 Mgal/yr) of waste processed in SWPF which is anticipated to be the peak plant throughput. To achieve the best hydraulic performance in extraction, it is recommended that the extraction contactors be operated at the highest reasonable speed possible (>2100 rpm

  4. Preparative isolation and purification of harpagoside from Scrophularia ningpoensis hemsley by high-speed counter-current chromatography.

    PubMed

    Tong, Shengqiang; Yan, Jizhong; Lou, Jianzhong

    2006-01-01

    The bioactive component harpagoside was successfully separated from the crude extract of Scrophularia ningpoensis Hemsley by one-step purification using high-speed counter-current chromatography (HSCCC). A two-phase solvent system containing n-butanol:ethyl acetate:water (1:9:10) was selected following consideration of the partition coefficient of the target compound. A 276 mg quantity of the crude extract was loaded onto a 250 mL HSCCC column and yielded 11 mg harpagoside at over 97% purity. The chemical structure of harpagoside was determined by HPLC-ESI/MS and 1H-NMR.

  5. Preparative isolation of three anthraquinones from Rumex japonicus by high-speed counter-current chromatography.

    PubMed

    Guo, Shuying; Feng, Bo; Zhu, Ruonan; Ma, Jiankang; Wang, Wei

    2011-01-27

    Three anthraquinones--emodin, chrysophanol, and physcion--were successfully purified from the dichloromethane extract of the Chinese medicinal herb Rumex japonicus by high-speed counter-current chromatography (HSCCC). The extract was separated with n-hexane-ethanol-water (18:22:3, v/v/v) as the two-phase solvent system and yielded 3.4 mg of emodin, 24.1 mg of chrysophanol, and 2.0 mg of physcion from 500 mg of sample with purities of 99.2 %, 98.8% and 98.2%, respectively. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the chemical structures of the three anthraquinones were confirmed by ¹H-NMR and ¹³C-NMR analysis. This is the first time these anthraquinones have been obtained from R. japonicus by HSCCC.

  6. Countercurrent soil washing system for remediation of viscous hydrocarbons, heavy metals, radionuclides

    SciTech Connect

    Kuhlman, M.I.; Karlsson, M.K.; Downie, C.A.

    1995-12-31

    Drying augers and multicell DAF tanks are excellent machines in which to countercurrently wash soil and remove hazardous hydrocarbons, metals or radionuclides. An auger works well because it preferentially moves soil along one side of its trough. Thus, when enough high pressure and temperature water jets are placed along that path, contaminants can be melted, or dissolved and scoured from the soil. Contaminants and fines flow down the opposite side of the auger and out for extraction in a series of flotation tanks. Countercurrent washing of the silt results when soil settles in tanks through rising water and air bubbles then is pumped through cyclones placed above the next DAF tank of the series. LNAPLs, DNAPLs, or metallic contaminants made hydrophobic by chemicals in the system are removed at the overflow of the cyclones or by flotation in the tanks. The overflow from the cyclones and DAF tanks flows into the previous tank of the series. Examples of contaminants remediated include; arsenic, cadmium, lead and mercury, Naturally Occurring Radioactive Materials (NORM), uranium, solid oils, polyaromatic hydrocarbons in creosote and coal tars, and polychlorinated hydrocarbons.

  7. Planetary Airplane Extraction System Development and Subscale Testing

    NASA Technical Reports Server (NTRS)

    Teter, John E., Jr.

    2006-01-01

    The Aerial Regional-scale Environmental Survey (ARES) project will employ an airplane as the science platform from which to collect science data in the previously inaccessible, thin atmosphere of Mars. In order for the airplane to arrive safely in the Martian atmosphere, a number of sequences must occur. A critical element in the entry sequence at Mars is an extraction maneuver to separate the airplane quickly (in less than a second) from its protective backshell to reduce the possibility of re-contact, potentially leading to mission failure. This paper describes the development, testing, and lessons learned from building a 1/3 scale model of this airplane extraction system. This design, based on the successful Mars Exploration Rover (MER) extraction mechanism, employs a series of trucks rolling along tracks located on the surface of the central parachute can. Numerous tests using high speed video were conducted at the Langley Research Center to validate this concept. One area of concern was that that although the airplane released cleanly, a pitching moment could be introduced. While targeted for a Mars mission, this concept will enable environmental surveys by aircraft in other planetary bodies with a sensible atmosphere such as Venus or Saturn's moon, Titan.

  8. Planetary Airplane Extraction System Development and Subscale Testing

    NASA Technical Reports Server (NTRS)

    Teter, John E., Jr.

    2006-01-01

    The Aerial Regional-scale Environmental Survey (ARES) project employs an airplane as the science platform from which to collect science data in the previously inaccessible, thin atmosphere of Mars. In order for the airplane to arrive safely in the Martian atmosphere a number of sequences must occur. A critical element in the entry sequence at Mars is an extraction maneuver to separate the airplane quickly (in less than a second) from its protective backshell to reduce the possibility of re-contact, potentially leading to mission failure. This paper describes the development, testing, and lessons learned from building a 1/3 scale model of this airplane extraction system. This design, based on the successful Mars Exploration Rover (MER) extraction mechanism, employs a series of trucks rolling along tracks located on the surface of the central parachute can. Numerous tests using high speed video were conducted at the Langley Research Center (LaRC) to validate this concept. One area of concern was that that although the airplane released cleanly, a pitching moment could be introduced. While targeted for a Mars mission, this concept will enable environmental surveys by aircraft in other planetary bodies with a sensible atmosphere such as Venus or Saturn s moon, Titan.

  9. Do Sverdrup transports account for the Pacific North Equatorial Countercurrent

    SciTech Connect

    Meyers, G.

    1980-02-20

    Poleward and equatorward geostrophic transports calculated from density are nearly equal to Sverdrup transports calculated from the curl of the wind stress in the North and South Pacific subtropical gyres. But the Sverdrup transports do not account for the Pacific North Equatorial Countercurrent.

  10. Solvent extraction studies with high-burnup Fast Flux Test Facility fuel in the Solvent Extraction Test Facility

    SciTech Connect

    Benker, D.E.; Bigelow, J.E.; Bond, W.D.; Chattin, F.R.; King, L.J.; Kitts, F.G.; Ross, R.G.; Stacy, R.G.

    1986-10-01

    A batch of high-burnup fuel from the Fast Flux Test Facility (FFTF) was processed in the Solvent Extraction Test Facility (SETF) during Campaign 9. The fuel had a burnup of {similar_to}0 MWd/kg and a cooling time of {similar_to} year. Two runs were made with this fuel; in the first, the solvent contained 30% tri-n-butyl phosphate (TBP) and partitioning of the uranium and plutonium was effected by reducing the plutonium with hydroxylamine nitrate (HAN); in the second, the solvent contained 10% TBP and a low operating temperature was used in an attempt to partition without reducing the plutonium valence. The plutonium reoxidation problem, which was present in previous runs that used HAN, may have been solved by lowering the temperature and acidity in the partition contactor. An automatic control system was used to maintain high loadings of heavy metals in the coextraction-coscrub contactor in order to increase its efficiency while maintaining low losses of uranium and plutonium to the aqueous raffinate. An in-line photometer system was used to measure the plutonium concentration in an intermediate extraction stage; and based on this data, a computer algorithm determined the appropriate adjustments in the addition rate of the extractant. The control system was successfully demonstrated in a preliminary run with purified uranium. However, a variety of equipment and start up problems prevented an extended demonstration from being accomplished during the runs with the FFTF fuel.

  11. Solvent extraction studies with low-burnup Fast Flux Test Facility fuel in the Solvent Extraction Test Facility

    SciTech Connect

    Benker, D.E.; Bigelow, J.E.; Bond, W.D.; Chattin, F.R.; King, L.J.; Kitts, F.G.; Ross, R.G.; Stacy, R.G.

    1985-01-01

    A batch of irradiated Fast Flux Test Facility (FFTF) fuel was processed for the first time in the Solvent Extraction Test Facility (SETF) at the Oak Ridge National Laboratory (ORNL) during Campaign 7. The average burnup of the fuel was only 0.2 atom %, but the cooling time was short enough ({similar_to}2 years) so that {sup 95}Zr was detected in the feed. This short cooling permitted our first measurement of {sup 95}Zr decontamination factors (DFs) without having to use tracers. No operational problems were noted in the operation of the extraction-scrubbing contactor, and low uranium and plutonium losses (< 0.01%) were measured. Fission product DFs were improved noticeably by increasing the number of scrub stages from six to eight. Two flowsheet options for making pure uranium and plutonium products (total partitioning) were tested. Each flowsheet used hydroxylamine nitrate for reducing plutonium. Good products were obtained (uranium DFs of > 10{sup 3} and plutonium DFs of > 10{sup 4}), but each flowsheet was troubled with plutonium reoxidation. Adding hydrazine and lowering the plutonium concentration lessened the problem but did not eliminate it. About 370 g of plutonium was recovered from these tests, purified by anion exchange, converted to PuO{sub 2}, and transferred to the fuel refabrication program. 7 references.

  12. [Experimental studies on the extract technology of tea polysaccharide from green tea by orthogonal test].

    PubMed

    Xu, Xuan; Luo, Xiaofeng; Chen, Zhaoxing; Li, Qinyu; Chen, Jianjing; Luo, Yifan

    2005-04-01

    The effect factor of extraction of tea polysaccharide was investigated with orthogonal test. The effects of extraction conditions on yield, purity of tea polysaccharide and cost of extraction were discussed. The results show that the optimum conditions for extracting tea polysaccharide from green tea are as follows: extraction time is 30 minutes with water at 95 degrees C, extraction times with chloroform is 3, extraction times with CH3COOC2H5 is 1 and concentration of alcohol is 60%.

  13. Genotoxicity testing of Ambelania occidentalis (Apocynaceae) leaf extract in vivo.

    PubMed

    Castro, L S; Perazzo, F F; Maistro, E L

    2009-04-22

    Ambelania occidentalis is routinely used in folk medicine for treating gastrointestinal disorders, even though there have been no safety trials. We evaluated the genotoxic potential of hydro-alcoholic extracts of this plant in mice; induced DNA damage was assessed in peripheral blood leukocytes and micronucleus induction was assessed in polychromatic erythrocytes from bone marrow. The extract was administered by an oral route at single doses of 1000, 1500 and 2000 mg/kg body weight. N-nitroso-N-ethylurea was used as a positive control. The comet assay was performed on peripheral blood leukocytes at 4 and 24 h after treatment, and the micronucleus test was carried out on bone marrow cells collected at 24 and 48 h after treatment. The ratio of polychromatic/normochromatic erythrocytes was scored for cytotoxicity assessment. No increase in the number of micronucleated polychromatic erythrocytes from bone marrow or in leukocyte DNA damage was observed. The hydro-alcoholic extracts of A. occidentalis had no mutagenic or cytotoxic effects in the mouse cells.

  14. Separation of flavonoids from Millettia griffithii with high-performance counter-current chromatography guided by anti-inflammatory activity.

    PubMed

    Tang, Huan; Wu, Bo; Chen, Kai; Pei, Heying; Wu, Wenshuang; Ma, Liang; Peng, Aihua; Ye, Haoyu; Chen, Lijuan

    2015-02-01

    Millettia griffithii is a unique Chinese plant located in the southern part of Yunnan Province. Up to now, there is no report about its phytochemical or related bioactivity research. In our previous study, the n-hexane crude extract of Millettia griffithii revealed significant anti-inflammatory activity at 100 μg/mL, inspiring us to explore the anti-inflammatory constituents. Four fractions (I, II, III, and A) were fractionated from n-hexane crude extract by high-performance counter-current chromatography with solvent system composed of n-hexane/ethyl acetate/methanol/water (8:9:8:9, v/v) and then were investigated for the potent anti-inflammatory activity. Fraction A, with the most potent inhibitory activity was further separated to give another four fractions (IV, V, VI, and B) with solvent system composed of n-hexane/ethyl acetate/methanol/water (8:4:8:4, v/v). Compound V and fraction B exhibited remarkable anti-inflammatory activity with nitric oxide inhibitory rate of 80 and 65%, which was worth further fractionation. Then, three fractions (VII, VIII, and IX) were separated from fraction B with a solvent system composed of n-hexane/ethyl acetate/methanol/water (8:1:8:1, v/v), with compound VIII demonstrating the most potent inhibitory activity (80%). Finally, the IC50 values of compound V and VIII were tested as 38.2 and 14.9 μM. The structures were identified by electrospray ionization mass spectrometry and(1)H and (13)C NMR spectroscopy.

  15. Isolation and purification of series bioactive components from Hypericum perforatum L. by counter-current chromatography.

    PubMed

    Cao, Xueli; Wang, Qiaoe; Li, Yan; Bai, Ge; Ren, Hong; Xu, Chunming; Ito, Yoichiro

    2011-03-01

    Counter-current chromatography (CCC) combined with pre-separation by ultrasonic solvent extraction was successively used for the separation of series bioactive compounds from the crude extract of Hypericum perforatum L. The petroleum ether extract was separated by the solvent system of n-heptane-methanol-acetonitrile (1.5:0.5:0.5, v/v) and n-heptane-methanol (1.5:1, v/v) in gradient elution, yielding a phloroglucinol compound, hyperforin with HPLC purity over 98%. The ethyl acetate extract was separated by using the solvent system composed of hexane-ethyl acetate-methanol-water (1:1:1:1 and 1:3:1:3, v/v) in gradient through both reverse phase and normal phase elution mode, yielding a naphthodianthrone compound, hypericin with HPLC purity about 95%. The n-butanol extract was separated with the solvent system composed of n-butanol-ethyl acetate-water (1:4:5 and 1.5:3.5:5, v/v) in elution and back-extrusion mode, yielding two of flavones, rutin and hyperoside, with HPLC purity over 95%. HPLC-MS, reference sample and UV spectrum were selectively used in separation to search for target compounds from HPLC-DAD profiles of different sub-extracts. The structures of isolated compounds were further identified by ESI-MS, ¹HNMR and ¹³CNMR.

  16. Isolation of the new minor constituents dihydropyranochromone and furanocoumarin from fruits of Peucedanum alsaticum L. by high-speed counter-current chromatography.

    PubMed

    Skalicka-Woźniak, Krystyna; Mroczek, Tomasz; Garrard, Ian; Głowniak, Kazimierz

    2009-07-24

    A preparative high-speed counter-current chromatography (HSCCC) method was successfully used for isolation of two new minor compounds--alsaticol and alsaticocoumarin A. A two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:1:1:1) was developed. Compounds were obtained from the dichloromethane extract of Peucedanum alsaticum fruits and their identification was performed with NMR and MS methods. Optimized HSCCC offers a rapid method of obtaining new natural compounds.

  17. Preliminary applications of cross-axis synchronous flow-through coil planet centrifuge for large-scale preparative counter-current chromatography.

    PubMed

    Zhang, T Y; Lee, Y W; Fang, Q C; Xiao, R; Ito, Y

    1988-11-11

    The cross-axis synchronous flow-through coil planet centrifuge with a 20-cm revolutional radius and a total capacity of 1600 ml was successfully applied to preparative counter-current chromatography of various biological samples, which include sea buckthorn extract, steroid reaction mixture, indole plant hormones, and dinitrophenylamino acids. The present system offers advantages of stable balance of the centrifuge, a large column capacity, and high resolution.

  18. Performance characteristics of countercurrent separation in analysis of natural products of agricultural significance.

    PubMed

    Friesen, J Brent; Pauli, Guido F

    2008-01-09

    A standard test mix consisting of 21 commercially available natural products of agricultural significance, termed the GUESSmix, was employed to measure the countercurrent chromatography performance characteristics of a very popular quaternary solvent system family made up of hexane-ethyl acetate-methanol-water (HEMWat). The polarity range of the GUESSmix combined with the elution-extrusion countercurrent chromatography (EECCC) technique and the newly developed reciprocal symmetry (ReS) and reciprocal shifted symmetry (ReSS) plots allow liquid-liquid distribution ratios ( K D) to be plotted for every compound eluted on a scale of zero to infinity. It was demonstrated that 16 of the 21 GUESSmix compounds are found in the optimal range of resolution (0.25 < K(D) < 16) of at least one HEMWat solvent system. The HEMWat solvent systems represented by the ratios 4:6:5:5, 4:6:4:6, and 3:7:4:6 possess the most densely populated optimal ranges of resolution for this standard mix. ReS plots have been shown to reveal the symmetrical reversibility of the EECCC method in reference to K(D) = 1. This study lays the groundwork for evaluation and comparison of solvent system families proposed in the literature, as well as the creation of new solvent system families with desired performance characteristics.

  19. Studies on the performance of different coiled column configurations for compact type-I countercurrent chromatography.

    PubMed

    Yang, Yi; Gu, Dongyu; Aisa, Haji Akber; Ito, Yoichiro

    2011-05-01

    Three types of novel coiled column configurations, i.e. a triangular coiled column and elliptical coiled columns I and II, were designed for type-I countercurrent chromatography and their performances were evaluated with two solvent systems each with suitable test samples. Three dinitrophenyl (DNP) amino acids (DNP-DL-glu, DNP-β-ala and DNP-L-ala) were separated with a moderately hydrophobic two-phase solvent system composed of hexane-ethyl acetate-metanol-0.1 M hydrochloric acid (1:1:1:1, v/v), while two dipeptides (tryptophyl-tyrosine and valyl-tyrosine) were separated with a polar solvent system composed of 1-butanol-acetic acid-water (4.75:0.25:5, v/v). The overall results indicated that the performance of compact type-I countercurrent chromatography was improved by elliptical coiled column I which was mounted with its maximum coil diameter perpendicular to the surface of the column holder. Hydrodynamic effects involved in these separations were discussed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Separation of two major chalcones from Angelica keiskei by high-speed counter-current chromatography.

    PubMed

    Kil, Yun-Seo; Nam, Joo-Won; Lee, Jun; Seo, Eun Kyoung

    2015-08-01

    Angelica keiskei (Shin-sun cho) is an edible higher plant with the beneficial preventive effects on cancer, hypertension, and coronary heart disease. Two bioactive chalcones of Shin-sun cho, xanthoangelol (1) and 4-hydroxyderricin (2), were separated simultaneously by using high-speed counter-current chromatography with a two-phase solvent system composed of n-hexane-EtOAc-MeOH-H2O (9:5:9:4). Only nonconsuming processes, solvent fractionations and Sephadex LH-20 column chromatography, were conducted as presteps. Xanthoangelol (1, 35.9 mg, 99.9 % purity at 254 and 365 nm) and 4-hydroxyderricin (2, 4.4 mg, 98.7 % purity at 254 nm and 98.8 % purity at 365 nm) were successfully purified from 70 mg of the processed extract from A. keiskei. The structures of two compounds were confirmed by (1)H- and (13)C-NMR analysis.

  1. Solvent extraction studies with intermediate-burnup Fast Flux Test Facility fuel in the Solvent Extraction Test Facility

    SciTech Connect

    Benker, D. E.; Bigelow, J. E.; Bond, W. D.; Chattin, F. R.; King, L. J.; Kitts, F. G.; Ross, R. G.; Stacy, R. G.

    1986-04-01

    In Campaign 8, two batches of irradiated fuel from the Fast Flux Test Facility (FFTF) were processed, using 30% TBP-NPH, in the Solvent Extraction Test Facility (SETF). The burnups were about 36 and 55 MWd/kg with 1.3- and 1-year cooling times, respectively. The latter fuel had the highest burnup and shortest cooling time of any fuel ever handled in the SETF. No major problems were noted during the operation of the mixer-settlers, and low uranium and plutonium losses (<0.02%) were achieved. Zirconium and ruthenium decontamination factors (DFs) were improved by increasing the number of scrub stages and increasing the peak solvent loading in the coextraction-coscrub bank. The use of an in-line photometer to measure the uranium and plutonium concentrations in a process stream permitted high solvent loadings of heavy metals to be achieved in the extraction bank while maintaining low losses to the aqueous raffinate. The investigation of two flowsheet options for making separate uranium and plutonium products (organic backscrub and selective uranium extraction) that was started in Campaign 7 was continued. High-quality products were again obtained (uranium and plutonium DFs of {similar_to}0{sup 4}). Plutonium reoxidation was still extensive even though hydrazine was added to the aqueous strip for the organic backscrub flowsheet. Two different plutonium oxalate precipitation procedures [Pu(III) and Pu(IV)] were used in the preparation of the plutonium oxide products; this was done so that the fuel fabrication characteristics of the oxide from the two procedures could be compared. A total of {similar_to}50 g of plutonium was recovered and shipped to the fuel refabrication program.

  2. Flooding in counter-current two-phase flow

    SciTech Connect

    Ragland, W.A.; Ganic, E.N.

    1982-01-01

    Flooding is a phenomenon which is best described as the transition from counter-current to co-current flow. Early notice was taken of this phenomenon in the chemical engineering industry. Flooding also plays an important role in the field of two-phase heat transfer since it is a limit for many systems involving counter-current flow. Practical applications of flooding limited processes include wickless thermosyphons and the emergency core cooling system (ECCS) of pressurized water nuclear reactors. The phenomenon of flooding also is involved in the behavior of nuclear reactor core materials during severe accident conditions where flooding is one of the mechanisms governing the motion of the molten fuel pin cladding.

  3. Partitioning of trivalent actinides from a Purex raffinate using a TODGA-based solvent-extraction process

    SciTech Connect

    Modolo, G.; Vijgen, H.; Malmbeck, R.; Magnusson, D.; Sorel, C.

    2008-07-01

    A TODGA/TBP process has been developed to separate trivalent actinides from a PUREX raffinate using a mixture of tetraoctyl-diglycolamide (TODGA) and tributylphosphate (TBP). Batch extraction experiments allowed us to choose and optimize the composition of the organic extractant and the aqueous feed solutions. With the aid of computer-code calculations, a countercurrent process has been developed, and an optimized flowsheet has been tested with a spiked feed solution and finally with a genuine PUREX raffinate. The results of the two tests were very promising, demonstrating that more than 99.9% of the trivalent actinides are extracted, and very high decontamination factors are obtained to the non-lanthanide fission products. Co-extracted ruthenium (10% during spiked test, 18% during hot test) is less efficiently back-extracted and therefore requires further process development. (authors)

  4. Experimental study of heat and mass transfer in a buoyant countercurrent exchange flow

    NASA Astrophysics Data System (ADS)

    Conover, Timothy Allan

    Buoyant Countercurrent Exchange Flow occurs in a vertical vent through which two miscible fluids communicate, the higher-density fluid, residing above the lower-density fluid, separated by the vented partition. The buoyancy- driven zero net volumetric flow through the vent transports any passive scalars, such as heat and toxic fumes, between the two compartments as the fluids seek thermodynamic and gravitational equilibrium. The plume rising from the vent into the top compartment resembles a pool fire plume. In some circumstances both countercurrent flows and pool fires can ``puff'' periodically, with distinct frequencies. One experimental test section containing fresh water in the top compartment and brine (NaCl solution) in the bottom compartment provided a convenient, idealized flow for study. This brine flow decayed in time as the concentrations approached equilibrium. A second test section contained fresh water that was cooled by heat exchangers above and heated by electrical elements below and operated steadily, allowing more time for data acquisition. Brine transport was reduced to a buoyancy- scaled flow coefficient, Q*, and heat transfer was reduced to an analogous coefficient, H*. Results for vent diameter D = 5.08 cm were consistent between test sections and with the literature. Some results for D = 2.54 cm were inconsistent, suggesting viscosity and/or molecular diffusion of heat become important at smaller scales. Laser Doppler Velocimetry was used to measure velocity fields in both test sections, and in thermal flow a small thermocouple measured temperature simultaneously with velocity. Measurement fields were restricted to the plume base region, above the vent proper. In baseline periodic flow, instantaneous velocity and temperature were ensemble averaged, producing a movie of the average variation of each measure during a puffing flow cycle. The temperature movie revealed the previously unknown cold core of the puff during its early development. The

  5. Con-Current versus Counter-Current Dialysate Flow during CVVHD. A Comparative Study for Creatinine and Urea Removal.

    PubMed

    Baldwin, Ian; Baldwin, Marie; Fealy, Nigel; Neri, Mauro; Garzotto, Francesco; Kim, Jeong Chul; Giuliani, Anna; Basso, Flavio; Nalesso, Federico; Brendolan, Alessandra; Ronco, Claudio

    2016-01-01

    Dialysate fluid connection to the membrane in continuous dialysis may affect solute clearance. Although circuit connections are routinely made counter-current to blood flow in intermittent dialysis, no study has assessed the effect of this dialysate fluid flow direction on removal of small solutes creatinine and urea during treatment using continuous veno-venous haemodialysis (CVVHD). To assess if dialysate flow direction during CVVHD affects small solute removal. This ethics-approved study recruited a convenience sample of 26 adult ICU patients requiring continuous dialysis to assess urea and creatinine removal for con-current vs. counter-current dialysate flow direction. The circuit was adjusted from continuous veno-venous haemodiafiltration to CVVHD 20 min prior to sampling with no fluid removal. Blood (b) and spent dialysate fluid (f) were taken in both concurrent and counter-current fluid flow at 1 (T1) and 4 (T4) hours with a new treatment. Blood flow was 200 ml/min. Dialysate flow 33 ml/min. Removal of urea and creatinine was expressed as the diafiltrate/plasma concentration ratio: Uf/b and Cf/b respectively. Data lacking normal distribution are presented as median with 25th and 75th interquartile ranges (IQR), otherwise as mean with SD and assessed with the independent t test for paired data. p < 0.5 was considered significant. Fifteen male patients were included with a median (IQR) age of 67 years (52-75), and APACHE x0399;x0399; score 17 (14-19) with all patients meeting RIFLE criteria 'F'. At both times, the counter-current dialysate flow was associated with higher mean (SD) diafiltrate/plasma concentration ratios: T1 0.87 (0.16) vs. 0.77 (0.10), p = 0.006; T2 0.96 (0.16) vs. 0.76 (0.09), p < 0.001 for creatinine and T1 0.98 (0.09) vs. 0.81 (0.09), p < 0.001; T2 0.99 (0.07) vs. 0.82 (0.08), p < 0.001 for urea. Counter-current dialysate flow during CVVHD for ICU patients is associated with an approximately 20% increase in removal of small solutes

  6. DISCRISET: a battery of tests for fast waste classification--application of tests on waste extracts.

    PubMed

    Deprez, K; Robbens, J; Nobels, I; Vanparys, C; Vanermen, G; Tirez, K; Michiels, L; Weltens, R

    2012-12-01

    The Hazardous Waste Directive (HWD, Council Directive 91/689/EC, 1991) provides a framework for classification of hazardous waste, based on 15 Hazard (H)-criteria. For complex wastes the HWD foresees the application of toxicity tests on the waste material itself to assess its toxic properties. However, these proposed test methods often involve mammalian testing, which is not acceptable from an ethical point of view, nor is it feasible economically. The DISCRISET project was initiated to investigate the use of alternative chemical and biological fast screening tests for waste hazard classification. In the first part of the project, different methods were reviewed and a testing strategy was proposed to minimize time and cost of analysis by a tiered approach. This includes as a first tier chemical analysis followed by a general acute toxicity screen as a second tier and as a third tier mechanistic toxicity tests to assess chronic toxicity (genotoxicity, hormone disturbance, teratogenic effects, immunologic activity). In this phase of the project, selected methods were applied to 16 different waste samples from various sources and industries. The first tier chemical tests are recommended for the full characterization of the leachate fraction (inorganics) but not for the organic fraction of samples. Here the chemical characterization is only useful if toxic content is known or suspected. As second tier the fast bacterial test Microtox is validated as a general toxicity screen for the organic fraction (worst case organic extract). Samples that are not classified in tier 1 or 2 are then further investigated in the third tier by the mechanistic toxicity tests and tested for their potential chronic toxicity: immune activity (TNF-α upregulation) is indicative for corrosive, irritating or sensitising effects (H4/H8/H15), reproductive effects (H10) are indicated by hormone disturbance and early life stage abnormalities in fish larvae when exposed to the extracts and

  7. 40 CFR Appendix Ix to Part 268 - Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B)

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 26 2010-07-01 2010-07-01 false Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B) IX Appendix IX to Part 268 Protection of.... 268, App. IX Appendix IX to Part 268—Extraction Procedure (EP) Toxicity Test Method and...

  8. 40 CFR Appendix Ix to Part 268 - Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B)

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 27 2011-07-01 2011-07-01 false Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B) IX Appendix IX to Part 268 Protection of.... 268, App. IX Appendix IX to Part 268—Extraction Procedure (EP) Toxicity Test Method and...

  9. 40 CFR Appendix Ix to Part 268 - Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B)

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 27 2014-07-01 2014-07-01 false Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B) IX Appendix IX to Part 268 Protection of.... 268, App. IX Appendix IX to Part 268—Extraction Procedure (EP) Toxicity Test Method and Structural...

  10. Rapid metal extractability tests from polluted mining soils by ultrasound probe sonication and microwave-assisted extraction systems.

    PubMed

    García-Salgado, Sara; Quijano, M Ángeles

    2016-12-01

    Ultrasonic probe sonication (UPS) and microwave-assisted extraction (MAE) were used for rapid single extraction of Cd, Cr, Cu, Ni, Pb, and Zn from soils polluted by former mining activities (Mónica Mine, Bustarviejo, NW Madrid, Spain), using 0.01 mol L(-1) calcium chloride (CaCl2), 0.43 mol L(-1) acetic acid (CH3COOH), and 0.05 mol L(-1) ethylenediaminetetraacetic acid (EDTA) at pH 7 as extracting agents. The optimum extraction conditions by UPS consisted of an extraction time of 2 min for both CaCl2 and EDTA extractions and 15 min for CH3COOH extraction, at 30% ultrasound (US) amplitude, whereas in the case of MAE, they consisted of 5 min at 50 °C for both CaCl2 and EDTA extractions and 15 min at 120 °C for CH3COOH extraction. Extractable concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The proposed methods were compared with a reduced version of the corresponding single extraction procedures proposed by the Standards, Measurements and Testing Programme (SM&T). The results obtained showed a great variability on extraction percentages, depending on the metal, the total concentration level and the soil sample, reaching high values in some areas. However, the correlation analysis showed that total concentration is the most relevant factor for element extractability in these soil samples. From the results obtained, the application of the accelerated extraction procedures, such as MAE and UPS, could be considered a useful approach to evaluate rapidly the extractability of the metals studied.

  11. Preparative isolation and purification of antioxidative diarylheptanoid derivatives from Alnus japonica by high-speed counter-current chromatography.

    PubMed

    Lim, Soon Sung; Lee, Min Young; Ahn, Hong Ryul; Choi, Soon Jung; Lee, Jae-Yong; Jung, Sang Hoon

    2011-12-01

    This study employed the online HPLC-2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS)(+) bioassay to rapidly determine the antioxidant compounds occurring in the crude extract of Alnus japonica. The negative peaks of the ABTS(+) radical scavenging detection system, which indicated the presence of antioxidant activity, were monitored by measuring the decrease in absorbance at 734 nm. The ABTS(+)-based antioxidant activity profile showed that three negative peaks exhibited antioxidant activity. High-speed counter-current chromatography (HSCCC) was used for preparative scale separation of the three active peaks from the extract. The purity of the isolated compounds was analyzed by HPLC and their structures were identified by (1)H- and (13)C-nuclear magnetic resonance spectrometry (NMR), heteronuclear multiple bond correlation (HMBC), and heteronuclear single quantum correlation (HSQC). Two solvent systems composed of n-hexane/ethylacetate/methanol/water (4:6:4:6, v/v) and of ethyl acetate/methanol/water (1:0.1:1, v/v) were performed in high-speed counter-current chromatography. Consequently, a total of 527 mg of hirsutanonol 5-O-β-D-glucopyranoside, 80.04 mg of 3-deoxohirsutenonol 5-O-β-D-glucopyranoside, and 91.0 mg of hirsutenone were obtained with purity of 94.7, 90.5, and 98.6%, respectively.

  12. A Laboratory Exercise Using a Physical Model for Demonstrating Countercurrent Heat Exchange

    ERIC Educational Resources Information Center

    Loudon, Catherine; Davis-Berg, Elizabeth C.; Botz, Jason T.

    2012-01-01

    A physical model was used in a laboratory exercise to teach students about countercurrent exchange mechanisms. Countercurrent exchange is the transport of heat or chemicals between fluids moving in opposite directions separated by a permeable barrier (such as blood within adjacent blood vessels flowing in opposite directions). Greater exchange of…

  13. A Laboratory Exercise Using a Physical Model for Demonstrating Countercurrent Heat Exchange

    ERIC Educational Resources Information Center

    Loudon, Catherine; Davis-Berg, Elizabeth C.; Botz, Jason T.

    2012-01-01

    A physical model was used in a laboratory exercise to teach students about countercurrent exchange mechanisms. Countercurrent exchange is the transport of heat or chemicals between fluids moving in opposite directions separated by a permeable barrier (such as blood within adjacent blood vessels flowing in opposite directions). Greater exchange of…

  14. Preparative isolation and purification of xanthohumol from hops (Humulus lupulus L.) by high-speed counter-current chromatography.

    PubMed

    Chen, Qi-He; Fu, Ming-Liang; Chen, Miao-Miao; Liu, Jing; Liu, Xiao-Jie; He, Guo-Qing; Pu, Shou-Cheng

    2012-05-01

    Xanthohumol (XN) and related prenylflavonoids are the main bioactive components of hops (Humulus lupulus L.). The current work is to investigate the use of high-speed counter-current chromatography (HSCCC) in search for high isolation of xanthohumol from hops. A solvent system consisted of n-hexane-ethyl acetate-methanol-water at a volume ratio of 5:5:4:3 was employed. The results demonstrated that the constructed method could be well applied for the isolation of xanthohumol from hops extract. After HSCCC isolation procedure, the purity of xanthohumol was over 95% assayed by HPLC and the yield of extraction was 93.60%. The chemical structure identification of xanthohumol was carried out by UV, (1)H NMR and (13)C NMR. The present results demonstrated that xanthohumol could be efficiently obtained using a single HSCCC step from H. lupulus L. extract.

  15. Testing the reliability of information extracted from ancient zircon

    NASA Astrophysics Data System (ADS)

    Kielman, Ross; Whitehouse, Martin; Nemchin, Alexander

    2015-04-01

    Studies combining zircon U-Pb chronology, trace element distribution as well as O and Hf isotope systematics are a powerful way to gain understanding of the processes shaping Earth's evolution, especially in detrital populations where constraints from the original host are missing. Such studies of the Hadean detrital zircon population abundant in sedimentary rocks in Western Australia have involved analysis of an unusually large number of individual grains, but also highlighted potential problems with the approach, only apparent when multiple analyses are obtained from individual grains. A common feature of the Hadean as well as many early Archaean zircon populations is their apparent inhomogeneity, which reduces confidence in conclusions based on studies combining chemistry and isotopic characteristics of zircon. In order to test the reliability of information extracted from early Earth zircon, we report results from one of the first in-depth multi-method study of zircon from a relatively simple early Archean magmatic rock, used as an analogue to ancient detrital zircon. The approach involves making multiple SIMS analyses in individual grains in order to be comparable to the most advanced studies of detrital zircon populations. The investigated sample is a relatively undeformed, non-migmatitic ca. 3.8 Ga tonalite collected a few kms south of the Isua Greenstone Belt, southwest Greenland. Extracted zircon grains can be combined into three different groups based on the behavior of their U-Pb systems: (i) grains that show internally consistent and concordant ages and define an average age of 3805±15 Ma, taken to be the age of the rock, (ii) grains that are distributed close to the concordia line, but with significant variability between multiple analyses, suggesting an ancient Pb loss and (iii) grains that have multiple analyses distributed along a discordia pointing towards a zero intercept, indicating geologically recent Pb-loss. This overall behavior has

  16. Alkaline-side extraction of technetium from tank waste using crown ethers and other extractants

    SciTech Connect

    Bonnesen, P.V.; Moyer, B.A.; Presley, D.J.; Armstrong, V.S.; Haverlock, T.J.; Counce, R.M.; Sachleben, R.A.

    1996-06-01

    The chemical development of a new crown-ether-based solvent-extraction process for the separation of (Tc) from alkaline tank-waste supernate is ready for counter-current testing. The process addresses a priority need in the proposed cleanup of Hanford and other tank wastes. This need has arisen from concerns due to the volatility of Tc during vitrification, as well as {sup 99}Tc`s long half-life and environmental mobility. The new process offers several key advantages that direct treatability--no adjustment of the waste composition is needed; economical stripping with water; high efficiency--few stages needed; non-RCRA chemicals--no generation of hazardous or mixed wastes; co-extraction of {sup 90}Sr; and optional concentration on a resin. A key concept advanced in this work entails the use of tandem techniques: solvent extraction offers high selectivity, while a subsequent column sorption process on the aqueous stripping solution serves to greatly concentrate the Tc. Optionally, the stripping solution can be evaporated to a small volume. Batch tests of the solvent-extraction and stripping components of the process have been conducted on actual melton Valley Storage Tank (MVST) waste as well as simulants of MVST and Hanford waste. The tandem process was demonstrated on MVST waste simulants using the three solvents that were selected the final candidates for the process. The solvents are 0.04 M bis-4,4{prime}(5{prime})[(tert-butyl)cyclohexano]-18-crown-6 (abbreviated di-t-BuCH18C6) in a 1:1 vol/vol blend of tributyl phosphate and Isopar{reg_sign} M (an isoparaffinic kerosene); 0.02 M di-t-BuCH18C6 in 2:1 vol/vol TBP/Isopar M and pure TBP. The process is now ready for counter-current testing on actual Hanford tank supernates.

  17. Improved spiral tube assembly for high-speed counter-current chromatography

    PubMed Central

    Ito, Y.; Clary, R.; Powell, J.; Knight, M.; Finn, T. M.

    2009-01-01

    The original spiral tube support (STS) assembly is improved by changing the shape of the tubing, with 1-cm presses perpendicularly along the length. This modification interrupts the laminar flow of the mobile phase. The tubing in the 4 return grooves to the center of the rotor is flattened by a specially made pressing tool to decrease the dead volume and thus increase the column efficiency. The performance of this spiral tube assembly was tested in separations of dipeptides and proteins with suitable polar two-phase solvent systems. The results revealed that the present system yields high partition efficiency with a satisfactory level of stationary phase retention in a short elution time. The present high-speed counter-current chromatographic system will be efficiently applied to a broad spectrum of two-phase solvent systems including aqueous-aqueous polymer phase systems which are used for separation of biopolymers such as proteins and nucleic acids. . PMID:19062024

  18. New analytical spiral tube assembly for separation of proteins by counter-current chromatography

    PubMed Central

    Ma, Xiaofeng; Ito, Yoichiro

    2015-01-01

    A new spiral column assembly for analytical separation by counter-current chromatography is described. The column is made from a plastic spiral tube support which has 12 interwoven spiral grooves. The PTFE tubing of 1.6 mm ID was first flattened by extruding through a narrow slit and inserted into the grooves to make 5 spiral layers with about 60 ml capacity. The performance of the spiral column assembly was tested with separation of three stable protein samples including cytochrome C, myoglobin and lysozyme in a polymer phase system composed of polyethylene glycol 1000 and dibasic potassium phosphate each at 12.5 % (w/w) in water. At 2 ml/min, three protein samples were well resolved in one hour. The separation time may be further shortened by application of higher revolution speed and flow rate by improving the strength of the spiral tube support in the future. PMID:26074099

  19. Separation and purification of neohesperidin from the albedo of Citrus reticulata cv. Suavissima by combination of macroporous resin and high-speed counter-current chromatography.

    PubMed

    Zhang, Jiukai; Zhu, Xiaoyan; Luo, Fenglei; Sun, Chongde; Huang, Jianzhen; Li, Xian; Chen, Kunsong

    2012-01-01

    In this article, a simple and efficient protocol for rapid preparation and separation of neohesperidin from the albedo of Citrus reticulata cv. Suavissima was established by the combination of macroporous resin column chromatography and high-speed counter-current chromatography (HSCCC). Six types of resin were investigated by adsorption and desorption tests, and D101 macroporous resin was selected for the first cleaning-up procedure, in which 55% aqueous ethanol was used to elute neohesperidin. After treatment with D101 resin, the neohesperidin purity increased 11.83-fold from 4.92% in the crude extract to 58.22% in the resin-refined sample, with a recovery of 68.97%. The resin-refined sample was directly subjected to HSCCC purification with a two-phase solvent system composed of ethyl acetate-n-butanol-water (4:1:5, v/v), and 23.6 mg neohesperidin with 97.47% purity was obtained from 60 mg sample in only one run. The recovery of neohesperidin in HSCCC separation procedure was 65.85%. The chemical structure of the purified neohesperidin was identified by both HPLC and LC-MS. The established purification process will be helpful for further characterization and utilization of Citrus neohesperidin.

  20. Countercurrent assisted quantitative recovery of metabolites from plant-associated natural deep eutectic solvents.

    PubMed

    Liu, Yang; Garzon, Jahir; Friesen, J Brent; Zhang, Yu; McAlpine, James B; Lankin, David C; Chen, Shao-Nong; Pauli, Guido F

    2016-07-01

    NAtural Deep Eutectic Solvents (NADES) are chemically simple but physiologically important plant constituents that exhibit unique solubilizing properties of other metabolites, including bioactive constituents. The high polarity of NADES introduces a challenge in the ability of conventional solid-support based chromatography to recover potential bioactive metabolites. This complicates the systematic explanation of the NADES' functions in botanical extracts. The present study utilizes countercurrent separation (CCS) methodology to overcome the recovery challenge. To demonstrate its feasibility, Glucose-Choline chloride-Water (GCWat, 2:5:5, mole/mole) served as a model NADES, and four widely used marker flavonoids with different polarities (rutin, quercetin, kaempferol, and daidzein) were chosen as model target analytes. In order to prepare GCWat with high consistency, a water drying study was performed. The unique capabilities of the recently introduced CherryOne system, offering volumetric phase metering, were used to monitor the CCS operations. The collected fractions were analyzed using UHPLC and NMR/quantitative NMR. CCS was able to recover the analytes from the NADES matrix with quantitative recoveries of 95.7%, 94.6%, 97.0%, and 96.7% for rutin, quercetin, kaempferol, and daidzein respectively. The CCS strategy enables recovery of target metabolites from NADES-containing crude extracts as well as from other chemical mixtures, and moreover offers a means of using NADES as environmentally friendly extraction solvents.

  1. Purification of betulinic acid from Eugenia florida (Myrtaceae) by high-speed counter-current chromatography.

    PubMed

    Frighetto, Nelson; Welendorf, Rodolfo Max; Pereira da Silva, Ana Maria; Nakamura, Marcos Jun; Siani, Antonio Carlos

    2005-01-01

    A high yield of betulinic acid (up to 17% from the ethanolic extract) was found in the leaves of Eugenia florida collected in south-eastern Brazil, making this species a potential commercial source of the title compound. Extracts of E. florida were subjected to solvent partition, and rapid high-speed counter-current chromatography (HSCCC) was applied to the semi-crude extracts to afford betulinic acid in high purity. The mobile and stationary phases were derived from the two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (10:5:2.5:1). The developing solvent system (stationary and mobile phases) for optimum HSCCC separation was chosen by dissolving the fraction to be chromatographed in the proposed solvent mixture and determining the amount of betulinic acid in each phase by densitometric TLC. Purified betulinic acid was characterized by 13C-NMR, GC-MS and co-injection of its methyl ester with standards in GC-FID. The HSCCC technique is commonly employed to isolate triterpene glycosides, but is applied in this study to an aglycone.

  2. Countercurrent assisted quantitative recovery of metabolites from plant-associated natural deep eutectic solvents

    PubMed Central

    Friesen, J. Brent; Zhang, Yu; McAlpine, James B.; Lankin, David C.; Chen, Shao-Nong; Pauli, Guido F.

    2016-01-01

    NAtural Deep Eutectic Solvents (NADES) are chemically simple but physiologically important plant constituents that exhibit unique solubilizing properties of other metabolites, including bioactive constituents. The high polarity of NADES introduces a challenge in the ability of conventional solid-support based chromatography to recover potential bioactive metabolites. This complicates the systematic explanation of the NADES’ functions in botanical extracts. The present study utilizes countercurrent separation (CCS) methodology to overcome the recovery challenge. To demonstrate its feasibility, Glucose-Choline chloride-Water (GCWat, 2:5:5, mole/mole) served as a model NADES, and four widely used marker flavonoids with different polarities (rutin, quercetin, kaempferol, and daidzein) were chosen as model target analytes. In order to prepare GCWat with high consistency, a water drying study was performed. The unique capabilities of the recently introduced CherryOne system, offering volumetric phase metering, were used to monitor the CCS operations. The collected fractions were analyzed using UHPLC and NMR/quantitative NMR. CCS was able to recover the analytes from the NADES matrix with quantitative recoveries of 95.7%, 94.6%, 97.0%, and 96.7% for rutin, quercetin, kaempferol, and daidzein respectively. The CCS strategy enables recovery of target metabolites from NADES-containing crude extracts as well as from other chemical mixtures, and moreover offers a means of using NADES as environmentally friendly extraction solvents. PMID:27118320

  3. [Droplet countercurrent chromatography to isolate ecdysteroids from the herb Silene tatarica (L>)].

    PubMed

    Báthori, M; Máthe, I

    1996-05-01

    Our research project was to isolate ecdysteroids from Silene tatarica (L.) Pers., which plant belongs to Caryophyllaceae family. This plant as a species of the Silence genus has been considered as a good potential source of ecdysteroids, including new, hitherto never identified natural product(s). The raw material of isolation was the herba of Silene tatarica (L.) Pers. that was cultivated in the fields of the Ecological and Botanical Research Institute of the Hungarian Academy of Sciences (Vácrátót, Hungary) and the plants were collected in June of 1994. The isolation procedure started with methanol extraction of the ground and milled herba. To improve the recovery, the extraction was done with boiling methanol under reflux for 20 minutes. The crude extract was purified using simple techniques, such as fractioned precipitation (with acetone), solvent-solvent partition (benzene-aqueous methanol). Further purification includes droplet counter-current chromatography (chloroform-methanol-water, 65:20:20, v/v/v) and straight-phase HPLC (silica stationary phase, dichloromethane-150 propanol-water. 125:25:2 v/v/v, mobile phase). Structural identification was done by using mass spectrometry and NMR spectroscopy. Three of the isolated ecdysteroids were identified as 20-hydroxyecdysone, 2-deoxy-20-hydroxyecdysone and 20-hydroxyecdysone-22-benzoate these compounds have never been detected in Silene tatarica (L.) Pers. Structural elucidation of the fourt isolated ecdysteroid resulted in a new natural product with the chemical structure of 2-deoxy-20-hydroxyecdysone 22-benzoate.

  4. Testing sequential quantum measurements: how can maximal knowledge be extracted?

    PubMed Central

    Nagali, Eleonora; Felicetti, Simone; de Assis, Pierre-Louis; D'Ambrosio, Vincenzo; Filip, Radim; Sciarrino, Fabio

    2012-01-01

    The extraction of information from a quantum system unavoidably implies a modification of the measured system itself. In this framework partial measurements can be carried out in order to extract only a portion of the information encoded in a quantum system, at the cost of inducing a limited amount of disturbance. Here we analyze experimentally the dynamics of sequential partial measurements carried out on a quantum system, focusing on the trade-off between the maximal information extractable and the disturbance. In particular we implement two sequential measurements observing that, by exploiting an adaptive strategy, is possible to find an optimal trade-off between the two quantities. PMID:22720131

  5. Schinus terebinthifolius countercurrent chromatography (Part III): Method transfer from small countercurrent chromatography column to preparative centrifugal partition chromatography ones as a part of method development.

    PubMed

    das Neves Costa, Fernanda; Hubert, Jane; Borie, Nicolas; Kotland, Alexis; Hewitson, Peter; Ignatova, Svetlana; Renault, Jean-Hugues

    2017-03-03

    Countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC) are support free liquid-liquid chromatography techniques sharing the same basic principles and features. Method transfer has previously been demonstrated for both techniques but never from one to another. This study aimed to show such a feasibility using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. Heptane - ethyl acetate - methanol -water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds. The optimized separation methodology previously described in Part I and II, was scaled up from an analytical hydrodynamic CCC column (17.4mL) to preparative hydrostatic CPC instruments (250mL and 303mL) as a part of method development. Flow-rate and sample loading were further optimized on CPC. Mobile phase linear velocity is suggested as a transfer invariant parameter if the CPC column contains sufficient number of partition cells. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Qualitative and quantitative evaluation of solvent systems for countercurrent separation.

    PubMed

    Friesen, J Brent; Ahmed, Sana; Pauli, Guido F

    2015-01-16

    Rational solvent system selection for countercurrent chromatography and centrifugal partition chromatography technology (collectively known as countercurrent separation) studies continues to be a scientific challenge as the fundamental questions of comparing polarity range and selectivity within a solvent system family and between putative orthogonal solvent systems remain unanswered. The current emphasis on metabolomic investigations and analysis of complex mixtures necessitates the use of successive orthogonal countercurrent separation (CS) steps as part of complex fractionation protocols. Addressing the broad range of metabolite polarities demands development of new CS solvent systems with appropriate composition, polarity (π), selectivity (σ), and suitability. In this study, a mixture of twenty commercially available natural products, called the GUESSmix, was utilized to evaluate both solvent system polarity and selectively characteristics. Comparisons of GUESSmix analyte partition coefficient (K) values give rise to a measure of solvent system polarity range called the GUESSmix polarity index (GUPI). Solvatochromic dye and electrical permittivity measurements were also evaluated in quantitatively assessing solvent system polarity. The relative selectivity of solvent systems were evaluated with the GUESSmix by calculating the pairwise resolution (αip), the number of analytes found in the sweet spot (Nsw), and the pairwise resolution of those sweet spot analytes (αsw). The combination of these parameters allowed for both intra- and inter-family comparison of solvent system selectivity. Finally, 2-dimensional reciprocal shifted symmetry plots (ReSS(2)) were created to visually compare both the polarities and selectivities of solvent system pairs. This study helps to pave the way to the development of new solvent systems that are amenable to successive orthogonal CS protocols employed in metabolomic studies.

  7. Counter-current chromatography of black tea infusions.

    PubMed

    Wedzicha, B L; Lo, M F; Donovan, T J

    1990-05-04

    Counter-current chromatography using a multilayer coil planet centrifuge, with solvent system ethyl acetate-butanol-water, permits the separation of black tea infusions into fractions which include pure SII and a mixture of SI and SIa thearubigins. Good resolution of several components of the infusion may be achieved in elution times of 1 to 2 h. The appearance of chromatograms is altered on decaffeinating the infusion. The effect of stationary phase composition is considered. Resolution of the peaks improves with butanol content.

  8. Isolation of a furan fatty acid from Hevea brasiliensis latex employing the combined use of pH-zone-refining and conventional countercurrent chromatography.

    PubMed

    Englert, Michael; Ulms, Kerstin; Wendlinger, Christine; Vetter, Walter

    2016-02-01

    Furan fatty acids are valuable and bioactive minor fatty acids that usually contribute <0.1% to the fatty acid content of food samples. Their biological role still remains unclear as authentic furan fatty acid standards are not readily available and thorough experimental studies verifying the relevance of furan fatty acids are thus virtually impossible. An efficient protocol for the isolation of the furan fatty acid 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid from hydrolyzed and centrifuged latex of Hevea brasiliensis was developed using countercurrent chromatography. A first run using pH-zone-refining countercurrent chromatography provided 48.4 mg of 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid from 210 mg latex extract in a purity of 95%. The purity was increased to 99% by means of one second run in conventional countercurrent chromatography mode. The Structure and purity of 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid were determined by gas chromatography coupled to mass spectrometry and (1)H and (13)C NMR spectroscopy.

  9. Preparative isolation and analysis of alcohol dehydrogenase inhibitors from Glycyrrhiza uralensis root using ultrafiltration combined with high-performance liquid chromatography and high-speed countercurrent chromatography.

    PubMed

    Chen, Miao; Liu, Liangliang; Chen, Xiaoqing

    2014-07-01

    A simple, rapid, and effective assay based on ultrafiltration combined with high-performance liquid chromatography and high-speed countercurrent chromatography was developed for screening and purifying alcohol dehydrogenase inhibitors from Glycyrrhiza uralensis root extract. Experiments were carried out to optimize binding conditions including alcohol dehydrogenase concentration, incubation time, temperature, and pH. By comparing the chromatograms, three compounds were found possessing alcohol dehydrogenase binding activity in Glycyrrhiza uralensis root. Under the target-guidance of ultrafiltration combined with the high-performance liquid chromatography experiment, liquiritin (1), isoliquiritin (2), and liquiritigenin (3) were separated by high-speed countercurrent chromatography using ethyl acetate/methanol/water (5:1:4) as the solvent system. The alcohol dehydrogenase inhibitory activities of these three isolated compounds were assessed; compound 2 showed strongest inhibitory activity with an IC50 of 8.95 μM. The results of the present study indicated that the combinative method using ultrafiltration, high-performance liquid chromatography and high-speed countercurrent chromatography could be widely applied for the rapid screening and isolation of enzyme inhibitors from complex mixtures.

  10. Isolation of chlorogenic acid from Mutellina purpurea L. herb using high-performance counter-current chromatography.

    PubMed

    Sieniawska, Elwira; Skalicka-Woźniak, Krystyna

    2014-01-01

    The aim of the study was to explore proper isolation conditions of chlorogenic acid from the herb of Mutelina purpurea L. - a new source of this bioactive molecule. The accelerated solvent extraction (ASE) with 40% aqueous solution of methanol combined with high-performance counter-current chromatography (HPCCC) was utilised for the efficient extraction and the separation of chlorogenic acid from the M. purpurea herb in less than 30 min. The structure of the obtained compound was confirmed by mass spectrometry and NMR analysis. The preparative HPCCC was performed using the mixture of ethyl acetate, butanol and water (4:1:5, v/v/v) in the reverse-phase mode. The chlorogenic acid was isolated from this herb for the first time, yielding 96% purity. The ASE with 40% methanol combined with HPCCC separation was proven to be a useful tool for quick and efficient isolation of chlorogenic acid from M. purpurea.

  11. Separation and purification of harmine and harmaline from Peganum harmala using pH-zone-refining counter-current chromatography.

    PubMed

    Wang, Xiao; Geng, Yanling; Wang, Daijie; Shi, Xingang; Liu, Jianhua

    2008-10-01

    pH-zone-refining counter-current chromatography was successfully applied to the separation of alkaloids from a crude extract of Peganum harmala L. using a multilayer coil planet centrifuge. The experiment was performed with a two-phase solvent system composed of methyl tert-butyl ether/THF/water (2:2:3 by volume) where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 1.2 g of the crude extract, 554 mg harmine and 325 mg harmaline were obtained each with a purity of over 96% as determined by HPLC. The structures of the isolated compounds were identified by electron ionization MS (EI-MS), (1)H NMR, and (13)C NMR.

  12. Counter-current acid leaching process for the removal of Cu, Pb, Sb and Zn from shooting range soil.

    PubMed

    Lafond, Stéphanie; Blais, Jean-François; Mercier, Guy; Martel, Richard

    2013-01-01

    This research explores the performance of a counter-current leaching process (CCLP) for Cu, Pb, Sb and Zn extraction in a polluted shooting range soil. The initial metal concentrations in the soil were 1790 mg Cu/kg, 48,300 mg Pb/kg, 840 mg Sb/kg and 368 mg Zn/kg. The leaching process consisted of five one-hour acid leaching steps, which used 1 M H2SO4 + 4 M NaCl (20 degrees C, soil suspension = 100 g/L) followed by two water rinsing steps. Ten counter-current remediation cycles were completed and the average metal removal yields were 98.3 +/- 0.3% of Cu, 99.5 +/- 0.1% of Pb, 75.5 +/- 5.1% of Sb and 29.1 +/- 27.2% of Zn. The quality of metal leaching did not deteriorate throughout the 10 remediation cycles completed for this study. The CCLP reduced acid and salt use by approximately 68% and reduced water consumption by approximately 60%, exceeding reductions achieved by a standard acid leaching process.

  13. Isolation and purification of arctigenin from Fructus Arctii by enzymatic hydrolysis combined with high-speed counter-current chromatography.

    PubMed

    Liu, Feng; Xi, Xingjun; Wang, Mei; Fan, Li; Geng, Yanling; Wang, Xiao

    2014-02-01

    Enzymatic hydrolysis pretreatment combined with high-speed counter-current chromatography for the transformation and isolation of arctigenin from Fructus Arctii was successfully developed. In the first step, the extract solution of Fructus Arctii was enzymatic hydrolyzed by β-glucosidase. The optimal hydrolysis conditions were 40°C, pH 5.0, 24 h of hydrolysis time, and 1.25 mg/mL β-glucosidase concentration. Under these conditions, the content of arctigenin was transformed from 2.60 to 12.59 mg/g. In the second step, arctigenin in the hydrolysis products was separated and purified by high-speed counter-current chromatography with a two-phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (10:25:15:20, v/v), and the fraction was analyzed by HPLC, ESI-MS, and (1)H NMR spectroscopy. Finally, 102 mg of arctigenin with a purity of 98.9% was obtained in a one-step separation from 200 mg of hydrolyzed sample. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. [The investigation of nickel dissolution from nitinol under different extraction conditions in biological tests].

    PubMed

    Wen, Xiantao; He, Xueying; Li, Jian; Tang, Juli; Huang, Yongfu

    2013-03-01

    The dissolution of nickel from nitinol alloy under different extraction conditions was investigated when biological tests of nitinol medical devices were carried out. It discussed the equivalence of these extraction conditions and found the best extraction conditions. In the experiment, two brands of nitinol were chosen and extracted under different extraction conditions according to GB/T 16886-12. Plasma emission spectrometer was used to analyse the concentration of nickel in extract liquid. The results show that there is no equivalence among these extraction conditions for nitinol materials. And it is suggested that (37 +/- 1) degree C, (72 +/- 2) h could be used as normal extraction condition and (70 +/- 2) degrees C, (24 +/- 2) h as accelerated extraction condition.

  15. Separation of chlorogenic acid and concentration of trace caffeic acid from natural products by pH-zone-refining countercurrent chromatography.

    PubMed

    Lu, Yuanyuan; Dong, Genlai; Gu, Yanxiang; Ito, Yoichiro; Wei, Yun

    2013-07-01

    Chlorogenic acid and caffeic acid were selected as test samples for separation by the pH-zone-refining countercurrent chromatography (CCC). The separation of these test samples was performed with a two-phase solvent system composed of methyl-tert-butyl-ether/acetonitrile/water at a volume ratio of 4:1:5 v/v/v where trifluoroacetic acid (TFA; 8 mM) was added to the organic stationary phase as a retainer and NH4 OH (10 mM) to the aqueous mobile phase as an eluter. Chlorogenic acid was successfully separated from Flaveria bidentis (L.) Kuntze (F. bidentis) and Lonicerae Flos by pH-zone-refining CCC, a slightly polar two-phase solvent system composed of methyl-tert-butyl-ether/acetonitrile/n-butanol/water at a volume ratio of 4:1:1:5 v/v/v/v was selected where TFA (3 mM) was added to the organic stationary phase as a retainer and NH4 OH (3 mM) to the aqueous mobile phase as an eluter. A 16.2 mg amount of chlorogenic acid with the purity of 92% from 1.4 g of F. bidentis, and 134 mg of chlorogenic acid at the purity of 99% from 1.3 g of crude extract of Lonicerae Flos have been obtained. These results suggest that pH-zone-refining CCC is suitable for the isolation of the chlorogenic acid from the crude extracts of F. bidentis and Lonicerae Flos. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Rapid isolation and purification of phorbol esters from Jatropha curcas by high-speed countercurrent chromatography.

    PubMed

    Hua, Wan; Hu, Huiling; Chen, Fang; Tang, Lin; Peng, Tong; Wang, Zhanguo

    2015-03-18

    In this work, a high-speed countercurrent chromatography (HSCCC) method was established for the preparation of phorbol esters (PEs) from Jatropha curcas. n-Hexane-ethyl acetate-methanol-water (1.5:1.5:1.2:0.5, v/v) was selected as the optimum two-phase solvent system to separate and purify jatropha factor C1 (JC1) with a purity of 85.2%, as determined by HPLC, and to obtain a mixture containing four or five PEs. Subsequently, continuous semipreparative HPLC was applied to further purify JC1 (99.8% as determined by HPLC). In addition, UPLC-PDA and UPLC-MS were established and successfully used to evaluate the isolated JC1 and PE-rich crude extract. The purity of JC1 was only 87.8% by UPLC-UV. A peak (a compound highly similar to JC1) was indentified as the isomer of JC1 by comparing the characteristic UV absorption and MS spectra. Meanwhile, this strategy was also applied to analyze the PE-rich crude extract from J. curcas. It is interesting that there may be more than 15 PEs according to the same quasi-molecular ion peaks, highly similar sequence-specific fragment ions, and similar UV absorption spectrum.

  17. Sample injection strategy to increase throughput in counter-current chromatography: Case study of Honokiol purification.

    PubMed

    Peng, Aihua; Hewitson, Peter; Ye, Haoyu; Zu, Liansuo; Garrard, Ian; Sutherland, Ian; Chen, Lijuan; Ignatova, Svetlana

    2016-12-09

    Counter-current chromatography (CCC) has been widely used as a preparative separation method to purify natural products from plant extracts and fermentation broths. Traditionally, throughput optimization in CCC has focused on sample concentration and sample volume. In this paper sample injection was considered as consisting of three variables: injection flow rate, post-injection flow rate and sample solvent. The effects of these parameters were studied using a honokiol purification from a Magnolia officinalis bark extract as a case study aiming to achieve the highest throughput/yield ratio for greater than 99% purity of this potential anti-cancer drug obtained for submission to the Chinese FDA. An injection method was established that increased the throughput of honokiol by 46.5% (from 3.05g/h to 4.47g/h), and decreased the solvent consumption of mobile phase and stationary phase per gram of honokiol by 40.0% (from 0.68L/g to 0.41L/g) and 48.4% (from 0.40L/g to 0.21L/g) respectively. These results show the importance of understanding the whole injection process when optimizing a given CCC separation. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Solvent extraction studies of coprocessing flowsheets: Results from Campaign 6 of the Solvent Extraction Test Facility (SETF)

    SciTech Connect

    Benker, D.E.; Bigelow, J.E.; Chattin, F.R.; Collins, E.D.; King, L.J.; Ross, R.G.; Savage, H.C.; Stacy, R.G.

    1986-11-01

    A series of five solvent extraction tests were made in the Solvent Extraction Test Facility (SETF) during Campaign 6. Each test used a coprocessing flowsheet that included coextraction-coscrubbing of the heavy metals followed by partial partitioning of the uranium and plutonium into separate uranium and uranium-plutonium products. The separation of the uranium and plutonium was aided by the addition of HNO{sub 2} to the organic backscrub stream. Two of these tests compared the performance of the traditional Purex solvent, tri-n-butyl phosphate (TBP), with a potential replacement, tri-2-ethylhexyl phosphate (TEHP). The remaining three tests were made with a chemically-degraded TBP solvent to compare the effectiveness of two solvent cleanup methods - treatment with silica gel or scrubbing with sodium carbonate and water.

  19. Stability and potency of raw and boiled shrimp extracts for skin prick test.

    PubMed

    Pariyaprasert, Wipada; Piboonpocanun, Surapon; Jirapongsananuruk, Orathai; Visitsunthorn, Nualanong

    2015-06-01

    The difference of stability between raw and boiled shrimp extracts used in prick tests has never been investigated despite its potential consequences in tests development. The aim of this study was to compare the raw and boiled shrimp extracts of two species; Macrobrachium rosenbergii (freshwater shrimp) and Penaeus monodon (seawater shrimp) held at 4 ?C for different periods of time for their stability and potency in vivo by using the skin prick test (SPT) method. Raw and boiled M. rosenbergii and P. monodon extracts were prepared and stored at 4 ?C for 1, 7, 14 and 30 days. Thirty patients were pricked with raw and boiled shrimp extracts at all storage times, as well as prick to prick skin test (PTP) to fresh raw and boiled shrimps of both species. The mean wheal diameter (MWD) resulting from prick tests for all shrimp extracts was measured and compared. The shrimp extracts of all storage times yielded positive skin test results in the range of 90% - 100%. Raw P. monodon extracts induced larger wheals than boiled extracts at all storage times. There was no significant difference of MWD between raw and boiled M. rosenbergii extracts on day 1, 7, and 14. Significant correlations between MWD of PTP to fresh shrimps and SPT to all shrimp extracts were observed. All shrimp extracts were sterile at all storage times. Raw and boiled M. rosenbergii and P. monodon extracts were stable and sterile at 4 ?C for at most 30 days. SPT with these extracts induced more than 10 mm in shrimp allergy patients and the results were comparable with PTP to fresh shrimps.

  20. Rigging Test Bed Development for Validation of Multi-Stage Decelerator Extractions

    NASA Technical Reports Server (NTRS)

    Kenig, Sivan J.; Gallon, John C.; Adams, Douglas S.; Rivellini, Tommaso P.

    2013-01-01

    The Low Density Supersonic Decelerator project is developing new decelerator systems for Mars entry which would include testing with a Supersonic Flight Dynamics Test Vehicle. One of the decelerator systems being developed is a large supersonic ringsail parachute. Due to the configuration of the vehicle it is not possible to deploy the parachute with a mortar which would be the preferred method for a spacecraft in a supersonic flow. Alternatively, a multi-stage extraction process using a ballute as a pilot is being developed for the test vehicle. The Rigging Test Bed is a test venue being constructed to perform verification and validation of this extraction process. The test bed consists of a long pneumatic piston device capable of providing a constant force simulating the ballute drag force during the extraction events. The extraction tests will take place both inside a high-bay for frequent tests of individual extraction stages and outdoors using a mobile hydraulic crane for complete deployment tests from initial pack pull out to canopy extraction. These tests will measure line tensions and use photogrammetry to track motion of the elements involved. The resulting data will be used to verify packing and rigging as well, as validate models and identify potential failure modes in order to finalize the design of the extraction system.

  1. Rigging Test Bed Development for Validation of Multi-Stage Decelerator Extractions

    NASA Technical Reports Server (NTRS)

    Kenig, Sivan J.; Gallon, John C.; Adams, Douglas S.; Rivellini, Tommaso P.

    2013-01-01

    The Low Density Supersonic Decelerator project is developing new decelerator systems for Mars entry which would include testing with a Supersonic Flight Dynamics Test Vehicle. One of the decelerator systems being developed is a large supersonic ringsail parachute. Due to the configuration of the vehicle it is not possible to deploy the parachute with a mortar which would be the preferred method for a spacecraft in a supersonic flow. Alternatively, a multi-stage extraction process using a ballute as a pilot is being developed for the test vehicle. The Rigging Test Bed is a test venue being constructed to perform verification and validation of this extraction process. The test bed consists of a long pneumatic piston device capable of providing a constant force simulating the ballute drag force during the extraction events. The extraction tests will take place both inside a high-bay for frequent tests of individual extraction stages and outdoors using a mobile hydraulic crane for complete deployment tests from initial pack pull out to canopy extraction. These tests will measure line tensions and use photogrammetry to track motion of the elements involved. The resulting data will be used to verify packing and rigging as well, as validate models and identify potential failure modes in order to finalize the design of the extraction system.

  2. Syringe test (modified larval immersion test): a new bioassay for testing acaricidal activity of plant extracts against Rhipicephalus microplus.

    PubMed

    Sindhu, Zia-ud-Din; Jonsson, Nicholas N; Iqbal, Zafar

    2012-09-10

    We report a new bioassay "syringe test" (modified larval immersion test) for in vitro evaluation of acaricidal activity of crude plant extracts. Prepared syringes, containing eggs of tick, were incubated until 14 d after hatching of eggs, when the bioassay was performed on the larvae. Lethal concentrations for 50% of larvae (LC(50)), LC(90) and LC(99) values were calculated for each tested product. 95% confidence intervals for LC(50) were very narrow, indicating a high degree of repeatability for the new bioassay on larvae of R. microplus. Bioassays were applied to six crude aqueous-methanol extracts from five plants (Acacia nilotica, Buxus papillosa, Fumaria parviflora, Juniperus excelsa, and Operculina turpethum), of which three showed discernible effects. Twenty-four hours post exposure, LC(99) values were 11.9% (w/v) for F. parviflora, 20.8% (w/v) and 29.2% (w/v) for B. papillosa and A. nilotica, respectively. After six days of exposure these values were; 9.1% (w/v), 9.2% (w/v) and 15.5 (w/v) for F. parviflora, A. nilotica and B. papillosa, respectively.

  3. [Purification of ovalbumin from hen egg white by high-speed counter-current aqueous two-phase chromatography].

    PubMed

    Zhi, Wen-Bo; Deng, Qiu-Yun; Song, Jiang-Nan; Ouyang, Fan

    2005-01-01

    High-speed counte-recurrent chromatography (HSCCC) is a continuous liquid-liquid partition chromatography without solid matrix, which has the significant features of high resolution and high recovery. The separation of bio-macromolecule in aqueous two-phase systems (ATPs) with HSCCC is still under research, and the establishment of high-speed counter-current aqueous two-phase chromatography (HSCCC-ATP) relies on the improvement of equipment structure and optimization of operation parameters. By using a multi-column high-speed counter-current chromatograph, the separation of protein mixture and the purification of ovalbumin from hen egg white were studied. The effects of pH and PEG concentration on the partition coefficients of proteins were tested in PEG1000-phosphate ATPs, and distinct differences among partition coefficients of proteins were found at pH 9.2 and 15.0% (W/W) PEG concentration in said system. The separation of protein mixture, consisting of cytochrome C, lysozyme and myoglobin was successfully performed in 15.0% (W/W) PEG1000-17.0% (W/W) potassium phosphate ATPs at pH 9.2 with high-speed counter-current chromatograph at rotation speed of 850r/min and flow rate of 0.8mL/min, using upper phase as stationary phase. pH and PEG concentration also had distinct effects on the partition coefficients of the major protein components in hen egg white, including ovaltransferrin, ovalbumin and lysozyme. The optimal pH value and PEG concentration for the purification of ovalbumin by HSCCC-ATP were found to be 9.2 and 16.0% (W/W) respectively. Ovalbumin was successfully purified to homogeneity from the hen egg white sample in 16.0% (W/W) PEG1000-17.0% (W/W) potassium phosphate ATPs at pH 9.2 with high-speed counter-current chromatograph at rotation speed of 850r/min and flow rate of 1.8mL/min, using upper phase as stationary phase. The purification recovery of ovalbumin was around 95%.

  4. Kenikir leaves (C. caudatus) extract antibacterial test toward the growth of Staphylococcus aureus in-vitro

    NASA Astrophysics Data System (ADS)

    Astutiningrum, Theresia; Feroniasanti, Y. M. Lauda

    2017-08-01

    The skin wound could cause bacterial infection if not to be treated. One of the cause is Staphylococcusaureus bacteria. Kenikir leaves has been used to be consumed and for traditional medication. This research aims to know the antibacterial activity of Kenikir leaves extract, to test the difference of antibacterial activity through different extraction method of Kenikir leaves and also to know minimum inhibitory concentration. The method that was used to test antibacterial activity was Kirby-Bauer method. Antibacterial activity was characterized by the presence of clear zone around paper discs which were called an inhibitory zone. Method to test a minimum inhibitory concentration were solid dilution. The research used two methods of extraction, namely maceration with ethanol solvent and mashed with aquades solvent. Extract concentrations that were used were 30%, 45%, 60%.Result showed that Kenikir leaves extracts had antibacterial activity. The results of antibacterial activity of the extracts showed that there was no difference between the two extraction method. Mashed extract of Kenikir leaves had a smallest inhibiton zone at concentration of 30% which were 6,76 mm and the largest was 7,58 mm at concentration of 60%. Ethanol extract of Kenikir leaves at concentration of 30% had an inhibiton zone of 7,25 mm and concentration of 60% had 8,59 mm. Minimum Inhibitory Concentration of antibacterial activity was not obtained. Kenikir leaves extract belongs to bacteriostatic group because of the compound could only inhibit the growth of bacteria.

  5. Differences among heat-treated, raw, and commercial peanut extracts by skin testing and immunoblotting.

    PubMed

    Maleki, Soheila J; Casillas, Adrian M; Kaza, Ujwala; Wilson, Brian A; Nesbit, Jacqueline B; Reimoneqnue, Chantrel; Cheng, Hsiaopo; Bahna, Sami L

    2010-12-01

    Peanut allergenicity has been reported to be influenced by heat treatment, yet the commonly available extracts for skin prick testing (SPT) are derived from raw extracts. To assess the effect of heat treatment on the SPT reactivity and specific IgE binding to peanut. Three commercial extracts and 3 laboratory-prepared extracts, including raw, roasted, and boiled, were used for SPT in 19 patients with suspected peanut allergy and in 4 individuals who eat peanut without any symptoms. Serum samples were obtained to measure total IgE in addition to specific IgE binding to the study extracts by immunoblotting. Peanut allergy was confirmed with challenge test unless the individual had a convincing history of a severe reaction. Eleven study participants were considered peanut allergic based on a strong history or positive challenge test result. SPT with the prepared and commercial reagents showed that the boiled extract had the highest specificity (67% vs 42%-63% for the other extracts). The prepared extracts showed similar SPT sensitivity (81%). Three patients with a history of severe reaction and elevated specific IgE levels to peanut to the 3 study extracts had variable SPT reactivity to 1 or more of the commercial extracts. IgE binding to Ara h 2 was found in nearly all patients, regardless of their clinical reactivity. None of the extracts tested showed optimal diagnostic reliability regarding both sensitivity and specificity. Perhaps testing should be performed with multiple individual extracts prepared by different methods. Copyright © 2010 American College of Allergy, Asthma & Immunology. Published by Elsevier Inc. All rights reserved.

  6. A micro hot test of the Chalmers-GANEX extraction system on used nuclear fuel

    SciTech Connect

    Bauhn, L.; Hedberg, M.; Aneheim, E.; Ekberg, C.; Loefstroem-Engdahl, E.; Skarnemark, G.

    2013-07-01

    In the present study, a 'micro hot test' has been performed using the Chalmers-GANEX (Group Actinide Extraction) system for partitioning of used nuclear fuel. The test included a pre-extraction step using N,N-di-2- ethylhexyl-butyramide (DEHBA) in n-octanol to remove the bulk part of the uranium. This pre-extraction was followed by a group extraction of actinides using the mixture of TBP and CyMe{sub 4}-BTBP in cyclohexanone as suggested in the Chalmers-GANEX process, and a three stage stripping of the extracted actinides. Distribution ratios for the extractions and stripping were determined based on a combination of γ- and α-spectrometry, as well as ICP-MS measurements. Successful extraction of uranium, plutonium and the minor actinides neptunium, americium and curium was achieved. However, measurements also indicated that co-extraction of europium occurs to some extent during the separation. These results were expected based on previous experiments using trace concentrations of actinides and lanthanides. Since this test was only performed in one stage with respect to the group actinide extraction, it is expected that multi stage tests will give even better results. (authors)

  7. Removal of cesium from simulated liquid waste with countercurrent two-stage adsorption followed by microfiltration.

    PubMed

    Han, Fei; Zhang, Guang-Hui; Gu, Ping

    2012-07-30

    Copper ferrocyanide (CuFC) was used as an adsorbent to remove cesium. Jar test results showed that the adsorption capacity of CuFC was better than that of potassium zinc hexacyanoferrate. Lab-scale tests were performed by an adsorption-microfiltration process, and the mean decontamination factor (DF) was 463 when the initial cesium concentration was 101.3μg/L, the dosage of CuFC was 40mg/L and the adsorption time was 20min. The cesium concentration in the effluent continuously decreased with the operation time, which indicated that the used adsorbent retained its adsorption capacity. To use this capacity, experiments on a countercurrent two-stage adsorption (CTA)-microfiltration (MF) process were carried out with CuFC adsorption combined with membrane separation. A calculation method for determining the cesium concentration in the effluent was given, and batch tests in a pressure cup were performed to verify the calculated method. The results showed that the experimental values fitted well with the calculated values in the CTA-MF process. The mean DF was 1123 when the dilution factor was 0.4, the initial cesium concentration was 98.75μg/L and the dosage of CuFC and adsorption time were the same as those used in the lab-scale test. The DF obtained by CTA-MF process was more than three times higher than the single-stage adsorption in the jar test.

  8. Scaling of Counter-Current Imbibition Process in Low-Permeability Porous Media, TR-121

    SciTech Connect

    Kvoscek, A.R.; Zhou, D.; Jia, L.; Kamath, J.

    2001-01-17

    This project presents the recent work on imaging imbibition in low permeability porous media (diatomite) with X-ray completed tomography. The viscosity ratio between nonwetting and wetting fluids is varied over several orders of magnitude yielding different levels of imbibition performance. Also performed is mathematical analysis of counter-current imbibition processes and development of a modified scaling group incorporating the mobility ratio. This modified group is physically based and appears to improve scaling accuracy of countercurrent imbibition significantly.

  9. Microwave corneosurfametry and the short-duration dansyl chloride extraction test for rating concentrated irritant surfactants.

    PubMed

    Goffin, V; Piérard, G E

    2001-01-01

    There are ethical concerns to conduct in vivo tests in the animal and human to provide evidence that cosmetics and other topical products are safe. To compare two methods, namely the short-duration dansyl chloride extraction test and the microwave corneosurfametry bioassay, to test the irritation potential of concentrated surfactant systems. Five surfactants and water were tested using the in vivo test and the bioassay. A significant linear correlation was found between data yielded by the two procedures. The short-duration dansyl chloride extraction test and the microwave corneosurfametry bioassay provide similar information. The latter has the advantage of being safe.

  10. A mutagenicity and cytotoxicity study of limonium effusum aqueous extracts by Allium, Ames and MTT tests.

    PubMed

    Eren, Y; Ozata, A; Konuk, M; Akyil, D; Liman, R

    2015-01-01

    Nowadays plants or plant extracts have become very important for alternative medicine. Plants and their extracts have many therapeutical advantages but some of them are potentially toxic, mutagenic, carcinogenic and teratogenic. Root, stem and leafparts of Limonium effusum were used in this study and this species is an endemic species for Turkey. Mutagenic and cytotoxic effects of root, stem and leaf aqueous extracts were observed with Allium, Ames and MTT tests. Allium root growth inhibition test and mitotic index studies showed that aqueous extracts have dose-dependent toxic effects. Chromosome aberration studies indicated that especially sticky chromosome, anaphase-telophase disorder and laggard chromosome anomalies were highly observed. Ames test performed with Limonium effusum root aqueous extracts, showed weak mutagenic effects in Salmonella typhimurium TA98 strain with S9. MTT test based on mitochondrial activity indicated that most of the aqueous extracts have cytotoxic effects. This study aimed to determine the possible mutagenic and cytotoxic effects of L. effusum aqueous extracts by using bacterial, plant and mammalian cells. This research showed that some low concentrations of the L. effusum extracts have inhibited cytotoxic effects but high concentrations have induced cytotoxicity. On the other hand only a weak mutagenic activity was identified by Ames test with TA98 S9(+).

  11. Novel Design for Centrifugal Countercurrent Chromatography: I. Zigzag Toroidal Column

    PubMed Central

    Yang, Yi; Aisa, Haji Akber; Ito, Yoichiro

    2009-01-01

    The toroidal coil using an equilateral triangular core has improved both retention of the stationary phase and peak resolution of the conventional toroidal coil in centrifugal countercurrent chromatography. To further improve the retention of stationary phase and peak resolution, a novel zigzag toroidal coil was designed and the performance of the system was evaluated at various flow rates. The results indicated that both retention of stationary phase and peak resolution were improved as the flow rate was decreased. Modification of the tubing by pressing at given intervals with a pair of pliers improved the peak resolution without increasing the column pressure. All these separations were performed under low column pressure indicating the separation can be further improved by increasing the column length and/or revolution speed without damaging the separation column. PMID:20046954

  12. Countercurrent direct contact heat exchange process and system

    DOEpatents

    Wahl, III, Edward F.; Boucher, Frederic B.

    1979-01-01

    Recovery of energy from geothermal brines and other hot water sources by direct contact heat exchange with a working fluid, such as a hydrocarbon working fluid, e.g. isobutane. The process and system consists of a plurality of stages, each stage including mixing and settling units. In the first stage, hot brine and arm working fluid are intimately mixed and passed into a settler wherein the brine settles to the bottom of the settler and the hot working fluid rises to the top. The hot working fluid is passed to a heat engine or turbine to produce work and the working fluid is then recycled back into the system. The system is comprised of a series of stages each containing a settler and mixer, and wherein the working fluid and the brine flow in a countercurrent manner through the stages to recover the heat from the brine in increments and raise the temperature of the working fluid in increments.

  13. A laboratory exercise using a physical model for demonstrating countercurrent heat exchange.

    PubMed

    Loudon, Catherine; Davis-Berg, Elizabeth C; Botz, Jason T

    2012-03-01

    A physical model was used in a laboratory exercise to teach students about countercurrent exchange mechanisms. Countercurrent exchange is the transport of heat or chemicals between fluids moving in opposite directions separated by a permeable barrier (such as blood within adjacent blood vessels flowing in opposite directions). Greater exchange of heat or chemicals between the fluids occurs when the flows are in opposite directions (countercurrent) than in the same direction (concurrent). When a vessel loops back on itself, countercurrent exchange can occur between the two arms of the loop, minimizing loss or uptake at the bend of the loop. Comprehension of the physical principles underlying countercurrent exchange helps students to understand how kidneys work and how modifications of a circulatory system can influence the movement of heat or chemicals to promote or minimize exchange and reinforces the concept that heat and chemicals move down their temperature or concentration gradients, respectively. One example of a well-documented countercurrent exchanger is the close arrangement of veins and arteries inside bird legs; therefore, the setup was arranged to mimic blood vessels inside a bird leg, using water flowing inside tubing as a physical proxy for blood flow within blood vessels.

  14. Extracting Information from Wrong Answers in Computerized Adaptive Testing

    DTIC Science & Technology

    1993-10-01

    examples of the Operating Characteristic Functions obtained when Model 8 is applied to real test data are given. In general, inspection of "goodness-of-fit...34 plots indicates that Model 8 provides superior data fit and higher item information functions than the well-known 3-parameter logistic ( dichotomous ... dichotomous and polychotomous item-response models are applied to test data obtained from applicants for military enlistment. Results of this research

  15. Studies on the Performance of Different Coiled Column Configurations for Compact Type-I Counter-current Chromatography

    PubMed Central

    Yang, Yi; Gu, Dongyu; Aisa, Haji Akber; Ito, Yoichiro

    2011-01-01

    Three types of novel coiled column configurations, i.e., a triangular coiled column and elliptical coiled columns I and II, were designed for type-I countercurrent chromatography and their performances were evaluated with two solvent systems each with suitable test samples. Three DNP-amino acids (DNP-DL-glu, DNP-β-ala and DNP-L-ala) were separated with a moderately hydrophobic two-phase solvent system composed of hexane-ethyl acetate-metanol-0.1M hydrochloric acid (1:1:1:1, v/v), while two dipeptides (tryptophyl tyrosine and valyl-tyrosine) were separated with a polar solvent system composed of 1-butanol-acetic acid-water (4.75:0.25:5, v/v). The overall results indicated that the performance of compact type-I counter-current chromatography was improved by elliptical coiled column II which was mounted with its maximum coil diameter perpendicular to the surface of the column holder. Hydrodynamic effects involved in these separations were discussed. PMID:21491597

  16. Isolation and purification of orientin and vitexin from Trollius chinensis Bunge by high-speed counter-current chromatography.

    PubMed

    Yu, Xiao-Xue; Huang, Jie-Yun; Xu, Dan; Xie, Zhi-Yong; Xie, Zhi-Sheng; Xu, Xin-Jun

    2014-01-01

    Orientin and vitexin are the two main bioactive compounds in Trollius chinensis Bunge. In this study, a rapid method was established for the isolation and purification of orientin and vitexin from T. chinensis Bunge using high-speed counter-current chromatography in one step, with a solvent system of ethyl acetate-ethanol-water (4:1:5, v/v/v). A total of 9.8 mg orientin and 2.1 mg vitexin were obtained from 100 mg of the ethyl acetate extract, with purities of 99.2% and 96.0%, respectively. Their structures were identified by UV, MS and NMR. The method was efficient and convenient, which could be used for the preparative separation of orientin and vitexin from T. chinensis Bunge.

  17. Isolation and purification of oridonin from the whole plant of Isodon rubescens by high-speed counter-current chromatography.

    PubMed

    He, Fa; Bai, Yuhua; Wang, Jing; Wei, Jing; Yu, Chunyue; Li, Sen; Yang, Weili; Han, Chenghua

    2011-09-14

    Semi-preparative high-speed counter-current chromatography (HSCCC) was successfully used for isolation and purification of oridonin from Isodon rubescens by using a two-phase-solvent system composed of n-hexane-ethyl acetate-methanol-water (2.8:5:2.8:5, v/v/v/v). The targeted compound isolated, collected and purified by HSCCC was analyzed by high performance liquid chromatography (HPLC). A total of 40.6 mg of oridonin with the purity of 73.5% was obtained in less than 100 min from 100 mg of crude Isodon rubescens extract. The chemical structure of the compound was identified by IR, 1H-NMR and 13C-NMR.

  18. Preparative separation of high-purity cordycepin from Cordyceps militaris(L.) Link by high-speed countercurrent chromatography

    PubMed Central

    Zhu, Licai; Liang, Yong; Lao, Deqiang; Zhang, Tianyou; Ito, Yoichiro

    2009-01-01

    A high-speed counter-current chromatography (HSCCC) technique in a preparative scale has been applied to separate and purify cordycepin from the extract of Cordyceps militaris(L.) Link by a one-step separation. A high efficiency of HSCCC separation was achieved on a two-phase solvent system of n-hexane–n-butanol–methanol–water (23:80:30:155, v/v/v/v) by eluting the lower mobile phase at a flow rate of 2 ml/min under a revolution speed of 850 rpm. HSCCC separation of 216.2 mg crude sample (contained cordycepin at 44.7% purity after 732 cation-exchange resin clean-up) yielded 64.8 mg cordycepin with purity of 98.9% and 91.7% recovery. Identification of the target compound was performed by UV, IR, MS, 1H NMR and 13C NMR. PMID:21643461

  19. Separation and purification of astaxanthin from Phaffia rhodozyma by preparative high-speed counter-current chromatography.

    PubMed

    Du, Xiping; Dong, Congcong; Wang, Kai; Jiang, Zedong; Chen, Yanhong; Yang, Yuanfan; Chen, Feng; Ni, Hui

    2016-09-01

    An effective high-speed counter-current chromatography (HSCCC) method was established for the preparative isolation and purification of astaxanthin from Phaffia rhodozyma. With a two-phase solvent system composed of n-hexane-acetone-ethanol-water (1:1:1:1, v/v/v/v), 100mg crude extract of P. rhodozyma was separated to yield 20.6mg of astaxanthin at 92.0% purity. By further one step silica gel column chromatography, the purity reached 99.0%. The chemical structure of astaxanthin was confirmed by thin layer chromatography (TLC), UV spectroscopy scanning, high performance liquid chromatography with a ZORBAX SB-C18 column and a Waters Nova-pak C18 column, and ESI/MS/MS.

  20. Sequential determination of anionic-type detergents by complexation with methylene blue using dual high speed counter-current chromatography.

    PubMed

    Kitazume, Eiichi; Koikawa, Saki; Hui, Lu; Sannohe, Syou; Yang, Yanjun; Maki, Yonosuke; Ito, Yoichiro

    2012-05-04

    A new dual high-speed counter-current chromatographic system using organic extraction phase and aqueous mobile phase containing methylene blue was applied to the analysis of anionic-type detergents. After selecting appropriate conditions such as flow rate of each mobile phase and sample volume, the new system was successfully applied to the analysis of anionic detergent in river water. As all the analytical procedures can be made in a closed system, the method has no health hazard. The present method is safe, precise, and highly sensitive, and can be applied for sequential determination of multiple samples in a short analysis time. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Preparative isolation and purification of theaflavins and catechins by high-speed countercurrent chromatography.

    PubMed

    Wang, Kunbo; Liu, Zhonghua; Huang, Jian-an; Dong, Xinrong; Song, Lubing; Pan, Yu; liu, Fang

    2008-05-15

    High-speed countercurrent chromatography (HSCCC) has been applied for the separation of theaflavins and catechins. The HSCCC run was carried out with a two-phase solvent system composed of hexane-ethyl acetate-methanol-water-acetic acid (1:5:1:5:0.25, v/v) by eluting the lower aqueous phase at 2 ml/min at 700 rpm. The results indicated that pure theaflavin, theaflavins-3-gallate, theaflavins-3'-gallate and theaflavin-3,3'-digallate could be obtained from crude theaflavins sample and black tea. The structures of the isolated compounds were positively confirmed by (1)H NMR and (13)C NMR, MS analysis, HPLC data and TLC data. Meanwhile, catechins including epigallocatechin gallate, gallocatechin gallate, epicatechin gallate and epigallocatechin were isolated from the aqueous extract of green tea by using the same solvent system. This study developed a modified method combined with enrichment theaflavins method by using HSCCC for separation of four individual theaflavins, especially for better separation of theaflavins monogallates.

  2. Purification of Active Myrosinase from Plants by Aqueous Two-Phase Counter-Current Chromatography

    PubMed Central

    Wade, Kristina L.; Ito, Yoichiro; Ramarathnam, Aarthi; Holtzclaw, W. David; Fahey, Jed W.

    2014-01-01

    Introduction Myrosinase (thioglucoside glucohydrolase; E.C. 3.2.1.147), is a plant enzyme of increasing interest and importance to the biomedical community. Myrosinase catalyses the formation of isothiocyanates such as sulforaphane (frombroccoli) and 4-(α-l-rhamnopyranosyloxy)benzyl isothiocyanate (from moringa), which are potent inducers of the cytoprotective phase-2 response in humans, by hydrolysis of their abundant glucosinolate (β-thioglucoside N-hydroxysulphate) precursors. Objective To develop an aqueous two-phase counter-current chromatography (CCC) system for the rapid, three-step purification of catalytically active myrosinase. Methods A high-concentration potassium phosphate and polyethylene glycol biphasic aqueous two-phase system (ATPS) is used with a newly developed CCC configuration that utilises spiral-wound, flat-twisted tubing (with an ovoid cross-section). Results Making the initial crude plant extract directly in the ATPS and injecting only the lower phase permitted highly selective partitioning of the myrosinase complex before a short chromatography on a spiral disk CCC. Optimum phase retention and separation of myrosinase from other plant proteins afforded a 60-fold purification. Conclusion Catalytically active myrosinase is purified from 3-day broccoli sprouts, 7-day daikon sprouts, mustard seeds and the leaves of field-grown moringa trees, in a CCC system that is predictably scalable. PMID:25130502

  3. Preparative separation of cacao bean procyanidins by high-speed counter-current chromatography.

    PubMed

    Li, Lingxi; Zhang, Shuting; Cui, Yan; Li, Yuanyuan; Luo, Lanxin; Zhou, Peiyu; Sun, Baoshan

    2016-11-15

    In this work, an efficient method for preparative separation of procyanidins from raw cacao bean extract by high-speed counter-current chromatography (HSCCC) was developed. Under the optimized solvent system of n-hexane-ethyl acetate-water (1:50:50, v/v/v) with a combination of head-tail and tail-head elution modes, various procyanidins fractions with different polymerization degrees were successfully separated. UPLC, QTOF-MS and (1)H NMR analysis verified that these fractions contained monomer up to pentamer respectively. Dimeric procyanidin B2 (purity>86%) could be isolated by HSCCC in a single run. Other individual procyanidins in these fractions could be further isolated and purified by preparative HPLC. The developed HSCCC together with preparative HPLC techniques appeared to be a useful tool for large preparation of different procyanidins from cacao beans. Furthermore, by antioxidant activity assays, it was proved that both fractions and individual procyanidins possessed greater antioxidant activities compared to standard trolox. The antioxidant activities of procyanidins increase as the increase of their polymerization degree. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. [Preparative isolation and purification of scopoletin from Lycium barbarum L. by high-speed countercurrent chromatography].

    PubMed

    Li, Xiaoduo; Li, Xuegang; Song, Shanghua; Zhang, Bo; Liu, Xujing; Ye, Xiaoli

    2012-09-01

    An effective and rapid method for the separation of scopoletin from Lycium barbarum L. by high-speed counter-current chromatography (HSCCC) was established. The ethyl alcohol extract of the Lycium barbarum L. was initially separated using D-101 macroporous resins and further purified by HSCCC. The thin layer chromatography coupling with fluorometric spectrophotometry (TLC-F) method was used to determine the partitioning coefficient of scopoletin in different solvent systems. The results showed the solvent system of chloroformmethanol-water (10:7:3, v/v/v) was the best one for the HSCCC separation. A total of 10.2 mg of scopoletin with high purity (98. 3%, analyzed by high performance liquid chromatography (HPLC)) was obtained in one step by the following separation procedures: the upper phase as the stationary phase, the lower phase as the mobile phase, with a flow rate of 1.5 mL/min, with the apparatus rotated at 850 r/min, and detected at 365 nm. The structure of the obtained compound was identified by 'H-nuclear magnetic resonance and 13C-nuclear magnetic resonance. The sample could be injected into HSCCC twice successively and the whole separation was achieved with satisfactory peak resolution. These results suggested that the TLC-F method is useful in measuring the partitioning coefficients of the target compound in HSCCC solvent systems and HSCCC is a fast and convenient method for the separation of scopoletin.

  5. Concentrical coils counter-current chromatography for natural products isolation: Salvia miltiorrhiza Bunge as example.

    PubMed

    Zhang, Lihong; Wang, Yanyan; Guo, Xiuyun; Wu, Shihua

    2017-02-22

    Countercurrent chromatography (CCC) is an efficient separation technique without the solid support matrix, largely depending on the partition of two-immiscible liquid phases in the separation column. Since the helical coil planet centrifuge was invented in early 1970s by Yoichiro Ito, a series of coils columns, including spiral coils and conical coils columns have been developed for CCC separation. In this work, we introduced a new simple and efficient concentrical coils column for CCC separation, which was prepared by winding the whole polytetrafluoroethylene (PTFE) tube into the circular grooves from the rotation axis in the same direction. Once the PTFE tube filled in all space of one round of the circular groove, it was jumped into the nearby outer circular groove through the gap and until the whole groove was filled. The three same concentrical coils distributed on three disc-shaped holders were connected by the same PTFE tube to form concentrical coils separation column. The separation capacity was further investigated using ten tanshinones of the extracts of a Traditional Chinese Medicine Salvia miltiorrhiza Bunge as a model natural product. All results indicated that the concentrical coils column could hold satisfactory retention of the stationary phase, higher theoretical plate number and better resolution for CCC separation of more than ten tanshinones. It may be an alternative CCC column for non-targeted and targeted isolation of bioactive natural products.

  6. Preparative separation of grape skin polyphenols by high-speed counter-current chromatography.

    PubMed

    Luo, Lanxin; Cui, Yan; Zhang, Shuting; Li, Lingxi; Li, Yuanyuan; Zhou, Peiyu; Sun, Baoshan

    2016-12-01

    To develop an efficient method for large preparation of various individual polyphenols from white grape skins (Fernão Pires; Vitis vinifera) by preparative high-speed counter-current chromatography (HSCCC) and preparative-HPLC, an optimized preparative HSCCC condition with two-phase solvent system composed of Hex-EtOAc-H2O (1:50:50, v/v) was used to separate grape skin polyphenols into various fractions. Both the tail-head and head-tail elution modes were used with a flow rate of 3.0ml/min and a rotary speed of 950rpm. Afterwards, a preparative-HPLC separation was applied to isolate individual polyphenols in each of the fractions from HSCCC. Total of 7 fractions (Fraction A to G) were obtained from grape skin extract by HSCCC. After preparative-HPLC isolation, fifteen individual compounds were obtained, most of which presented high yields and purity (all over 90%). The HSCCC method followed with preparative-HPLC appeared to be convenient and economical, constituting an efficient strategy for the isolation of grape skin polyphenols.

  7. Two-dimensional counter-current chromatography for the preparative separation of prenylflavonoids from Artocarpus altilis.

    PubMed

    Lu, Yanbin; Sun, Cuirong; Wang, Yu; Pan, Yuanjiang

    2007-06-01

    A two-dimensional counter-current chromatographic system (2D-CCC) for preparative isolation and purification of three prenylflavonoids from Artocarpus altilis is presented. An upright CCC instrument (CCC1, total capacity: 1600 ml) was used as the first dimension. Effluent of interest from CCC1 was collected on-line into a 30 ml sample loop by a laboratory-prepared column-switching interface and introduced into a high-speed CCC instrument (CCC2, total capacity: 210 ml) for the second dimension separation. With this 2D-CCC system and a pair of two-phase solvent systems composed of n-hexane-ethyl acetate-methanol-water (5:5:7:3 and 5:5:6.5:3.5, v/v/v/v), which had been selected by high-speed CCC, about a 500 mg amount of the crude extract was separated, yielding 9 mg of compound 1, 28 mg of compound 2 and 78 mg of compound 3. The purities of the three prenylflavonoids were 98.7 (1), 98.3 (2) and 97.2% (3), respectively, as determined by HPLC analysis. Their chemical structures were identified by electrospray ionization MS, (1)H NMR and (13)C NMR.

  8. [Genetic effects of root extracts of Glycyrrhiza glabra L. on different test-systems].

    PubMed

    Agabeĭli, R A

    2012-01-01

    The antimutagenic and geroprotective activities of root extracts of Glycyrrhiza glabra have been demonstrated both on plant test systems--Allium fistulosum L., Allium cepa L., Vicia faba L. and on animals--Vistar rats. The possibilities of the mobilization of Glycyrrhiza glabra root extracts as antimutagenic agents are discussed.

  9. Selective Separation and Extraction of Vanadium (V) Over Manganese (II) from Co-Leaching Solution of Roasted Stone Coal and Pyrolusite Using Solvent Extraction

    NASA Astrophysics Data System (ADS)

    Cai, Z. L.; Feng, Y. L.; Zhou, Y. Z.; Li, H. R.; Wang, W. D.

    2013-11-01

    Based on the novel technology for selective separation and extraction of vanadium (V) over manganese (II) from co-leaching solution of roasted stone coal and pyrolusite using solvent extraction, the extraction effect of vanadium (V) and manganese (II) has been studied and many technical conditions have also been optimized. Meanwhile, countercurrent simulation experiments were conducted to verify the results of the experiments. The results indicated that with three countercurrent extraction stages, 99.21% vanadium (V) was extracted using 5% (v/v) N235 and 5% (v/v) secondary octyl alcohol at initial aqueous pH of 3.0 and O/A phase ratio of 1.0. Vanadium (V) could be completely stripped after three-stage countercurrent experiments with 20 wt.% NH4Cl at O/A phase ratio of 1.0. The process flow sheet for the recovery of vanadium (V), as well as manganese (II), was proposed.

  10. 40 CFR Appendix Ix to Part 268 - Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B)

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 28 2013-07-01 2013-07-01 false Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B) IX Appendix IX to Part 268 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) LAND DISPOSAL RESTRICTIONS...

  11. PNEUMATIC PUMP TEST FOR DESIGN OF SOIL VACUUM EXTRACTION

    EPA Science Inventory

    In-situ pneumatic pumping tests were performed to estimate the pneumatic permeability at a site containing soils contaminated with aviation gasoline. Determination of pneumatic permeability was necessary to evaluate soil-air discharge or pore volume exchange rates. Pressure propa...

  12. PNEUMATIC PUMP TEST FOR DESIGN OF SOIL VACUUM EXTRACTION

    EPA Science Inventory

    In-situ pneumatic pumping tests were performed to estimate the pneumatic permeability at a site containing soils contaminated with aviation gasoline. Determination of pneumatic permeability was necessary to evaluate soil-air discharge or pore volume exchange rates. Pressure propa...

  13. FIELD TEST OF AIR SPARGING COUPLED WITH SOIL VAPOR EXTRACTION

    EPA Science Inventory

    A controlled field study was designed and conducted to assess the performance of air sparging for remediation of petroleum fuel and solvent contamination in a shallow (3-m deep) groundwater aquifer. Sparging was performed in an insolation test cell (5 m by 3 m by 8-m deep). A soi...

  14. Separation of polar betalain pigments from cacti fruits of Hylocereus polyrhizus by ion-pair high-speed countercurrent chromatography.

    PubMed

    Wybraniec, Sławomir; Stalica, Paweł; Jerz, Gerold; Klose, Bettina; Gebers, Nadine; Winterhalter, Peter; Spórna, Aneta; Szaleniec, Maciej; Mizrahi, Yosef

    2009-10-09

    Polar betacyanin pigments together with betaxanthins from ripe cactus fruits of Hylocereus polyrhizus (Cactaceae) were fractionated by means of preparative ion-pair high-speed countercurrent chromatography (IP-HSCCC) also using the elution-extrusion (EE) approach for a complete pigment recovery. HSCCC separations were operated in the classical 'head-to-tail' mode with an aqueous mobile phase. Different CCC solvent systems were evaluated in respect of influence and effectiveness of fractionation capabilities to separate the occurring pigment profile of H. polyrhizus. For that reason, the additions of two different volatile ion-pair forming perfluorinated carboxylic acids (PFCA) were investigated. For a direct comparison, five samples of Hylocereus pigment extract were run on preparative scale (900 mg) in 1-butanol-acetonitrile-aqueous TFA 0.7% (5:1:6, v/v/v) and the modified systems tert.-butyl methyl ether-1-butanol-acetonitrile-aqueous PFCA (2:2:1:5, v/v/v/v) using 0.7% and 1.0% trifluoroacetic acid (TFA) or heptafluorobutyric acid (HFBA) in the aqueous phase, respectively. The chemical affinity to the organic stationary CCC solvent phases and in consequence the retention of these highly polar betalain pigments was significantly increased by the use of the more lipophilic fluorinated ion-pair reagent HFBA instead of TFA. The HFBA additions separated more effectively the typical cacti pigments phyllocactin and hylocerenin from betanin as well as their iso-forms. Unfortunately, similar K(D) ratios and selectivity factors alpha around 1.0-1.1 in all tested solvent systems proved that the corresponding diastereomers, 15S-type pigments cannot be resolved from the 15R-epimers (iso-forms). Surprisingly, additions of the stronger ion-pair reagent (HFBA) resulted in a partial separation of hylocerenin from phyllocactin which were not resolved in the other solvent systems. The pigments were detected by means of HPLC-DAD and HPLC-electrospray ionization-MS using also

  15. Organic-solvent extraction of model biomaterials for use in the in vitro chromosome aberration test.

    PubMed

    Matsuoka, Atsuko; Haishima, Yuji; Hasegawa, Chie; Matsuda, Yoshie; Tsuchiya, Toshie

    2008-07-01

    We prepared polyurethane (PU) containing 0.4% or 4% 4,4'-methylenedianiline (MDA) as model materials to investigate the effectiveness of sample preparation by organic-solvent extraction for the in vitro chromosome aberration (CA) test. MDA itself (0.4 mg/mL) was positive only in the presence of an exogenous metabolizing system (S9 mix). The culture medium extract of PU containing 4% MDA (PU/4% MDA) was negative with and without S9 mix. Methanol and acetone extracts, on the other hand, induced structural CAs without S9 mix, which we did not expect because MDA requires S9 mix for activity. On chemical analysis, however, we found that the ratio of MDA extracted by the organic solvents to that extracted by the culture medium of PU/4% MDA was about 15:1. Interestingly, oligomers consisting of poly(tetramethyleneglycol) derivatives (OTMG) were also extracted by the organic solvents. The data suggest that the induction of structural CAs in the absence of S9 mix may have been partly due to synergism of MDA and OTMG. CA tests of MDA and PTMG-1000 in combination confirmed that to be the case. Thus, organic-solvent extraction may be more effective than medium extraction in evaluating the biological safety of biomaterials. Detailed chemical analysis of extracts was performed. (c) 2007 Wiley Periodicals, Inc.

  16. Field Test Design Simulations of Pore-Water Extraction for the SX Tank Farm

    SciTech Connect

    Truex, Michael J.; Oostrom, Martinus

    2013-09-01

    A proof of principle test of pore water extraction is being performed by Washington River Protection Solutions for the U.S. Department of Energy, Office of River Protection. This test is being conducted to meet the requirements of Hanford Federal Facility Agreement and Consent Order (HFFACO) (Ecology et al. 1989) Milestone M 045-20, and is described in RPP-PLAN-53808, 200 West Area Tank Farms Interim Measures Investigation Work Plan. To support design of this test, numerical simulations were conducted to help define equipment and operational parameters. The modeling effort builds from information collected in laboratory studies and from field characterization information collected at the test site near the Hanford Site 241-SX Tank Farm. Numerical simulations were used to evaluate pore-water extraction performance as a function of the test site properties and for the type of extraction well configuration that can be constructed using the direct-push installation technique. Output of simulations included rates of water and soil-gas production as a function of operational conditions for use in supporting field equipment design. The simulations also investigated the impact of subsurface heterogeneities in sediment properties and moisture distribution on pore-water extraction performance. Phenomena near the extraction well were also investigated because of their importance for pore-water extraction performance.

  17. EXTRACTION OF URANIUM

    DOEpatents

    Schmieding, E.G.; Ruehle, A.E.

    1961-04-11

    A method is given for extracting metal values from an aqueous feed wherein the aqueous feed is passed countercurrent to an organic extractant through a plurality of decanting zones and a portion of the mixture contained in each decanting zone is recycled through a mixing zone associated therewith. The improvement consists of passing more solvent from the top of one decanting zone to the bottom of the preceding decanting zone than can rise to the top thereof and recycling that portion of the solvent that does not rise to the top back to the first named decanting zone through its associated mixing zone.

  18. Papaver Rhoeas L. Hydroalcoholic Extract Exacerbates Forced Swimming Test-Induced Depression in Mice

    PubMed Central

    Osanloo, Naser; Najafi-Abedi, Akram; Jafari, Fatemeh; Javid, Farshid; Pirpiran, Mohsen; Memar Jafari, Mohammad-Reza; Mousavi Khosravi, Seyed Ali; Rahimzadeh Behzadi, Mohammad; Ranjbaran, Mina; Sahraei, Hedayat

    2016-01-01

    Introduction: Depression is one of the most frequent psychiatric disorders in the world with occurs with higher incidence in women. In the present study, the effect of water-alcoholic extract of Papaver rhoeas L. on forced swimming test (FST) in Swiss-Webster mice were examined. Methods: We used Swiss-Webster mice (20–25 g) to execute FST on them. The plant extract (1, 10, 30, and 100 mg/kg) was injected to the animals 30 minutes before each session. Fluoxetine (20 mg/kg) was used as standard antidepressant drug. In another group of animals, 30 minutes after extract administration, blood samples were taken from retro-orbital sinus for corticosterone assay. Yet in third group, the drugs were injected to the animals and 30 minutes later, their activities were tested in an open field apparatus. Results: Our experiments showed that the extract efficiently reduced FST time both in male and female mice dose-dependently. This effect was comparable with fluoxetine. In addition, corticosterone assay indicated that plasma corticosterone in animals which received extract was higher than those amounts in fluoxetine and saline controls. Moreover, the animals did not show any motor activity deficit in all doses of the extract and fluoxetine compared to saline control. Conclusion: The extract of Papaver rhoeas can reduce immobility time which is comparable to the effect of fluoxetine. Also the effect of the extract is contrary to its effects on plasma corticosterone level and or animals’ activity. PMID:27563412

  19. Design of Countercurrent Separation of Ginkgo biloba Terpene Lactones by Nuclear Magnetic Resonance

    PubMed Central

    Qiu, Feng; Friesen, Brent J.; McAlpine, James B.; Pauli, Guido F.

    2012-01-01

    Terpene lactones such as bilobalide, ginkgolides A, B, C, and J are major bioactive compounds of Ginkgo biloba L. Purification of these compounds is tedious due to their similar chemical properties. For the purpose of developing an effective and efficient method for both analytical and preparative separation of terpene lactones in G. biloba, an innovative orthogonality-enhanced high-speed countercurrent chromatography (HSCCC) method was established. Taking advantage of quantitative 1H NMR (qHNMR) methodology, partition coefficients (K) of individual terpene lactones were calculated directly from crude G. biloba leaf extract, using their H-12 signals as distinguishing feature. The partitioning experiment assisted the design of a two dimensional (2D) HSCCC procedure using a pair of orthogonal HSCCC solvent systems (SSs), ChMWat +4 and HEMSoWat +3/0.05%. It was surprising that the resolution of ginkgolides A and B was improved by 25% in the HEMWat +3 SS modified with 0.5% DMSO. Consequently, all five terpene lactones could be well separated with qHNMR purity > 95% from G. biloba leaf extract. The separation was further evaluated by offline qHNMR analysis of HSCCC fractions associated with Gaussian curve fitting. The results showed less than 2% error in HSCCC retention predicted from the partitioning experiment. This compelling consistency demonstrates that qHNMR-derived K determination (“K-by-NMR”) can be used to predict CCC fractionation and target purification of analytes from complex mixtures. Furthermore, Gaussian curve fitting enabled an accurate prediction of less than 2% impurity in the CCC fraction, which demonstrates its potential as a powerful tool to study the presence of minor constituents, especially when they are beyond the detection limit of conventional spectroscopic detectors. PMID:22579361

  20. Optimization of Antifungal Extracts from Ficus hirta Fruits Using Response Surface Methodology and Antifungal Activity Tests.

    PubMed

    Chen, Chuying; Wan, Chunpeng; Peng, Xuan; Chen, Yuhuan; Chen, Ming; Chen, Jinyin

    2015-10-29

    The fruits of Ficus hirta (FH) display strong antifungal activity against Penicillium italicum and Penicillium digitatum. In order to optimize the extraction conditions of antifungal extracts from FH fruit, various extraction parameters, such as ethanol concentration, extraction time, solvent to solid ratio and temperature, were chosen to identify their effects on the diameters of inhibition zones (DIZs) against these two Penicillium molds. Response surface methodology (RSM) was applied to obtain the optimal combination of these parameters. Results showed that the optimal extraction parameters for maximum antifungal activity were: 90% (v/v) ethanol concentration, 65 min extraction time, 31 mL/g solvent to solid ratio and 51 °C temperature. Under the abovementioned extraction conditions, the experimental DIZs values obtained experimentally were 57.17 ± 0.75 and 39.33 ± 0.82 mm, which were very close to the values of 57.26 and 39.29 mm predicted by the model. Further, nine kinds of phytopathogens were tested in vitro to explore the antifungal activity of the FH extracts. It was found for the first time that the FH extracts showed significant inhibition on the growth of P. italicum, A. citri, P. vexans, P. cytosporella and P. digitatum.

  1. Solvent extraction studies of 10% TBP flowsheets in the solvent extraction test facility using irradiated fuel from the Fast Flux Test Facility

    SciTech Connect

    Benker, D.E.; Bigelow, J.E.; Bond, W.D.; Campbell, D.O.; Chattin, F.R.; King, L.J.; Kitts, F.G.; Ross, R.G.; Stacy, R.G.

    1988-03-01

    Two solvent extraction experiments were made in the Solvent Extraction Test Facility (SETF) during Campaign 10 to continue the evaluation of: (1) a computer control system for the coextraction-coscrub contractor; and (2) a partitioning technique that separates uranium and plutonium without the aid of chemical reductants. The Fast Flux Test Facility (FFTF) fuel used in this campaign had burnups of {approximately}55 and {approximately}60 (average) MWd/kg. During both experiments, the computer control system successfully maintained stable, efficient operation. The control system used an in-line photometer to monitor the plutonium concentration in the extraction section; and based on this data, it adjusted the addition rate of the extractant to maintain high loadings of heavy metal in the solvent and low raffinate losses. The uranium and plutonium partitioning relied entirely on the differences between the U(VI) and Pu(IV) distribution coefficients (since no reductant was used to adjust the plutonium valence). In order to enhance this difference, the TBP concentration and operating temperature were relatively low in comparison to traditional Purex flowsheets. Final product purities of 99{percent} were achieved for both the uranium and plutonium in one cycle of partitioning.

  2. CMOS-MEMS Test-Key for Extracting Wafer-Level Mechanical Properties

    PubMed Central

    Chuang, Wan-Chun; Hu, Yuh-Chung; Chang, Pei-Zen

    2012-01-01

    This paper develops the technologies of mechanical characterization of CMOS-MEMS devices, and presents a robust algorithm for extracting mechanical properties, such as Young’s modulus, and mean stress, through the external electrical circuit behavior of the micro test-key. An approximate analytical solution for the pull-in voltage of bridge-type test-key subjected to electrostatic load and initial stress is derived based on Euler’s beam model and the minimum energy method. Then one can use the aforesaid closed form solution of the pull-in voltage to extract the Young’s modulus and mean stress of the test structures. The test cases include the test-key fabricated by a TSMC 0.18 μm standard CMOS process, and the experimental results refer to Osterberg’s work on the pull-in voltage of single crystal silicone microbridges. The extracted material properties calculated by the present algorithm are valid. Besides, this paper also analyzes the robustness of this algorithm regarding the dimension effects of test-keys. This mechanical properties extracting method is expected to be applicable to the wafer-level testing in micro-device manufacture and compatible with the wafer-level testing in IC industry since the test process is non-destructive. PMID:23235449

  3. Separation of five compounds from leaves of Andrographis paniculata (Burm. f.) Nees by off-line two-dimensional high-speed counter-current chromatography combined with gradient and recycling elution.

    PubMed

    Zhang, Li; Liu, Qi; Yu, Jingang; Zeng, Hualiang; Jiang, Shujing; Chen, Xiaoqing

    2015-05-01

    An off-line two-dimensional high-speed counter-current chromatography method combined with gradient and recycling elution mode was established to isolate terpenoids and flavones from the leaves of Andrographis paniculata (Burm. f.) Nees. By using the solvent systems composed of n-hexane/ethyl acetate/methanol/water with different volume ratios, five compounds including roseooside, 5,4'-dihydroxyflavonoid-7-O-β-d-pyranglucuronatebutylester, 7,8-dimethoxy-2'-hydroxy-5-O-β-d-glucopyranosyloxyflavon, 14-deoxyandrographiside, and andrographolide were successfully isolated. Purities of these isolated compounds were all over 95% as determined by high-performance liquid chromatography. Their structures were identified by UV, mass spectrometry, and (1) H NMR spectroscopy. It has been demonstrated that the combination of off-line two-dimensional high-speed counter-current chromatography with different elution modes is an efficient technique to isolate compounds from complex natural product extracts.

  4. Recovery of Butanol by Counter-Current Carbon Dioxide Fractionation with its Potential Application to Butanol Fermentation

    PubMed Central

    Solana, Miriam; Qureshi, Nasib; Bertucco, Alberto; Eller, Fred

    2016-01-01

    A counter-current CO2 fractionation method was applied as a mean to recover n-butanol and other compounds that are typically obtained from biobutanol fermentation broth from aqueous solutions. The influence of operating variables, such as solvent-to-feed ratio, temperature, pressure and feed solution composition was experimentally studied in terms of separation efficiency, butanol removal rate, total removal and butanol concentration in the extract at the end of the continuous cycle. With respect to the temperature and pressure conditions investigated, results show that the highest separation efficiency was obtained at 35 °C and 10.34 MPa. At these operating conditions, 92.3% of the butanol present in the feed solution was extracted, and a concentration of 787.5 g·L−1 of butanol in the extract was obtained, starting from a feed solution of 20 g·L−1. Selectivity was calculated from experimental data, concluding that our column performs much better than a single equilibrium stage. When adding ethanol and acetone to the feed solution, ethanol was detected in the water-rich fraction (raffinate), whereas the highest concentration of acetone was found in the butanol rich fraction (extract). PMID:28773654

  5. Recovery of Butanol by Counter-Current Carbon Dioxide Fractionation with its Potential Application to Butanol Fermentation.

    PubMed

    Solana, Miriam; Qureshi, Nasib; Bertucco, Alberto; Eller, Fred

    2016-06-30

    A counter-current CO₂ fractionation method was applied as a mean to recover n-butanol and other compounds that are typically obtained from biobutanol fermentation broth from aqueous solutions. The influence of operating variables, such as solvent-to-feed ratio, temperature, pressure and feed solution composition was experimentally studied in terms of separation efficiency, butanol removal rate, total removal and butanol concentration in the extract at the end of the continuous cycle. With respect to the temperature and pressure conditions investigated, results show that the highest separation efficiency was obtained at 35 °C and 10.34 MPa. At these operating conditions, 92.3% of the butanol present in the feed solution was extracted, and a concentration of 787.5 g·L(-1) of butanol in the extract was obtained, starting from a feed solution of 20 g·L(-1). Selectivity was calculated from experimental data, concluding that our column performs much better than a single equilibrium stage. When adding ethanol and acetone to the feed solution, ethanol was detected in the water-rich fraction (raffinate), whereas the highest concentration of acetone was found in the butanol rich fraction (extract).

  6. EFFECTS OF TREATMENTS ON SOIL-LEAD BIOAVAILABILITY: IMPLICATIONS OF IN-VITRO EXTRACTION TESTING

    EPA Science Inventory

    A field-scale study on the use of phosphate amendments to reduce lead bioavailabity from soil is being conducted at the Joplin site. One of the tools used to evaluate whether lead bioavailability is being reduced is an in vitro extraction test. The in vitro test simulates the gas...

  7. EFFECTS OF TREATMENTS ON SOIL-LEAD BIOAVAILABILITY: IMPLICATIONS OF IN-VITRO EXTRACTION TESTING

    EPA Science Inventory

    A field-scale study on the use of phosphate amendments to reduce lead bioavailabity from soil is being conducted at the Joplin site. One of the tools used to evaluate whether lead bioavailability is being reduced is an in vitro extraction test. The in vitro test simulates the gas...

  8. Bioassay-guided isolation of an active compound with protein tyrosine phosphatase 1B inhibitory activity from Sargassum fusiforme by high-speed counter-current chromatography.

    PubMed

    Wang, Miao; Gu, Dongyu; Guo, Xinfeng; Li, Haoquan; Wang, Yi; Guo, Hong; Yang, Yi; Tian, Jing

    2016-11-01

    A rapid and efficient method using high-speed counter-current chromatography was established for the bioassay-guided separation of an active compound with protein tyrosine phosphatase 1B inhibitory activity from Sargassum fusiforme. Under the bioassay guidance, the ethyl acetate extract with the best IC50 value of 0.37 ± 0.07 μg/mL exhibited a potential protein tyrosine phosphatase 1B inhibitory activity, which was further separated by high-speed counter-current chromatography. The separation was performed with a two-phase solvent system composed of n-hexane/methanol/water (5:4:1, v/v). As a result, dibutyl phthalate (19.7 mg) with the purity of 95.3% was obtained from 200 mg of the ethyl acetate extract. Its IC50 was 14.05 ± 0.06 μM, which was further explained by molecular docking. The result of molecular docking showed that dibutyl phthalate enfolded in the catalytic site of protein tyrosine phosphatase 1B. The main force between dibutyl phthalate and protein tyrosine phosphatase 1B was the hydrogen bond interaction with Gln266. In addition, hydrogen bond, van der Waals force and hydrophobic interaction with the amino acids (Ala217, Ile219, and Gly220) were also responsible for the stable protein-ligand complex.

  9. Evaluation of Cytotoxicity and Genotoxicity of Inula viscosa Leaf Extracts with Allium Test

    PubMed Central

    Aşkin Çelik, Tülay; Aslantürk, Özlem Sultan

    2010-01-01

    I. viscosa has been used for years in folk medicine for its anti-inflammatory, antipyretic, antiseptic, and paper antiphlogistic activities. In this study, cytotoxic and genotoxic effects of I. viscosa leaf extracts on the root meristem cells of Allium cepa have been examined. Onion bulbs were exposed to 2.5 mg/ml, 5 mg/ml, and 10 mg/ml concentrations of the extracts for macroscopic and microscopic analysis. Tap water has been used as a negative control and Ethyl methanesulfonate (EMS) (2 · 10−2 M) has been used as a positive control. The test concentrations have been determined according to doses which are recommended for use in alternative medicine. There has been statistically significant (P < .05) inhibition of root growth depending on concentration by the extracts when compared with the control groups. All the tested extracts have been observed to have cytotoxic effects on cell division in A. cepa. I. viscosa leaf extract induces the total number of chromosomal aberrations and micronuclei (MNC) formations in A. cepa root tip cells significantly when compared with control groups. Also, this paper shows for the first time the induction of cell death, ghost cells, cells with membrane damage, and binucleated cells by extract treatment. These results suggest the cytotoxic and genotoxic effects of the I. viscosa leaf extracts on A. cepa. PMID:20617136

  10. Rational development of solvent system families in counter-current chromatography.

    PubMed

    Friesen, J Brent; Pauli, Guido F

    2007-06-01

    Application of a mixture of 21 commercially available natural products, termed the GUESSmix, established a standard test that allows for a systematic analysis and comparison of the properties of biphasic solvent systems in counter-current/partition chromatography. Because the GUESSmix is comprised of compounds with varying polarities, functional groups, and structural features, it proves to be a rational method for mapping the optimal resolution polarity range of a particular solvent system. The mapping of optimal resolution polarity ranges of solvent systems provided for the description of the overall optimal resolution polarity range of a solvent system family, comprised of the same solvents in different proportions. By comparing the GUESSmix performance in the individual members of a solvent system family, the solvent system that best functions as the representative of, or portal to, the solvent system families was determined. The GUESSmix also afforded a method to compare the overall optimal resolution polarity ranges of solvent system families. Based on performance of GUESSmix chromatograms, the counter-current chromatography (CCC) properties of a two ternary literature solvent systems, ethyl acetate/n-butanol/water (EBuWat) and t-butylmethylether/acetonitrile/water (terAcWat), were explored in order to contrast and compare their CCC potential. A quaternary solvent system, hexane/t-butylmethylether/acetonitrile/water (HterAcWat), was also formulated and studied. The results indicated that the GUESSmix is fit for the purpose of developing and evaluating CCC solvent system families with desired performance characteristics.

  11. Improved spiral tube assembly for high-speed counter-current chromatography.

    PubMed

    Ito, Y; Clary, R; Powell, J; Knight, M; Finn, T M

    2009-05-08

    The original spiral tube support (STS) assembly is improved by changing the shape of the tubing, with 1-cm presses perpendicularly along the length. This modification interrupts the laminar flow of the mobile phase. The tubing in the four return grooves to the center of the rotor is flattened by a specially made pressing tool to increase the number of spiral layers and decrease the dead space volume, thus increasing the column efficiency. The performance of this spiral tube assembly was tested in separations of dipeptides and proteins with suitable polar two-phase solvent systems. The results revealed that the present system yields high partition efficiency with a satisfactory level of stationary phase retention in a short elution time. The present high-speed counter-current chromatographic (HSCCC) system will be efficiently applied to a broad spectrum of two-phase solvent systems including aqueous-aqueous polymer phase systems (TPAS) which are used for separation of biopolymers such as proteins and nucleic acids.

  12. Accurate early-time and late-time modeling of countercurrent spontaneous imbibition

    NASA Astrophysics Data System (ADS)

    March, Rafael; Doster, Florian; Geiger, Sebastian

    2016-08-01

    Spontaneous countercurrent imbibition into a finite porous medium is an important physical mechanism for many applications, included but not limited to irrigation, CO2 storage, and oil recovery. Symmetry considerations that are often valid in fractured porous media allow us to study the process in a one-dimensional domain. In 1-D, for incompressible fluids and homogeneous rocks, the onset of imbibition can be captured by self-similar solutions and the imbibed volume scales with √t. At later times, the imbibition rate decreases and the finite size of the medium has to be taken into account. This requires numerical solutions. Here we present a new approach to approximate the whole imbibition process semianalytically. The onset is captured by a semianalytical solution. We also provide an a priori estimate of the time until which the imbibed volume scales with √t. This time is significantly longer than the time it takes until the imbibition front reaches the model boundary. The remainder of the imbibition process is obtained from a self-similarity solution. We test our approach against numerical solutions that employ parametrizations relevant for oil recovery and CO2 sequestration. We show that this concept improves common first-order approaches that heavily underestimate early-time behavior and note that it can be readily included into dual-porosity models.

  13. Wall pressure measurements of flooding in vertical countercurrent annular air–water flow

    SciTech Connect

    Choutapalli, I., Vierow, K.

    2010-01-01

    An experimental study of flooding in countercurrent air-water annular flow in a large diameter vertical tube using wall pressure measurements is described in this paper. Axial pressure profiles along the length of the test section were measured up to and after flooding using fast response pressure transducers for three representative liquid flow rates representing a wide range of liquid Reynolds numbers (ReL = 4Γ/μ; Γ is the liquid mass flow rate per unit perimeter; μ is the dynamic viscosity) from 3341 to 19,048. The results show that flooding in large diameter tubes cannot be initiated near the air outlet and is only initiated near the air inlet. Fourier analysis of the wall pressure measurements shows that up to the point of flooding, there is no dominant wave frequency but rather a band of frequencies encompassing both the low frequency and the broad band that are responsible for flooding. The data indicates that flooding in large diameter vertical tubes may be caused by the constructive superposition of a plurality of waves rather than the action of a single large-amplitude wave.

  14. Countercurrent reverse osmosis for ethanol-water separation. Final report, August 7, 1981-November 6, 1982

    SciTech Connect

    Lee, E.K.L.; Babcock, W.C.; Bresnahan, P.A.

    1983-03-01

    The objective of this program was to investigate the technical and economic feasibility of producing concentrated ethanol from dilute feedstocks using a membrane process called countercurrent reverse osmosis (CCRO). A number of commerical membranes prepared in our laboratory for their suitability for CCRO application were evaluated. Included were some of the best RO membranes currently available for desalination. In all cases the membranes exhibited decreasing ethanol-water selectivities with increasing ethanol concentration in the feed stream, becoming essentially non-selective toward a 50- to 60-vol % ethanol feed. Thus, it appears that even with state-of-the-art membranes, concentration of ethanol above 50 vol % is not possible. It was also observed various degrees of degradation among the membranes. To test the feasibility of using CCRO to reduce osmotic pressure across the membranes, experiments were performed in which ethanol solutions were introduced on the permeate side of the membrane. In only one membrane (developed at Bend Research and designated 3N8) was a large effect observed. the results obtained with 3N8 membranes were used as the basis for projecting the performance of the CCRO process. An economic analysis of CCRO was conducted, including a comparison of the economics of CCRO with distillation. The results of this analysis suggest that CCRO is more energy-efficient than distillation for a given product concentration and output rate, but that it involves higher capital equipment costs.

  15. Production, Extraction, and Qualitative Testing of Penicillin: A Biochemistry Experiment for Health Science Chemistry Courses

    NASA Astrophysics Data System (ADS)

    Stevens, Richard E.; Billingsley, Kara C.

    1998-10-01

    This laboratory procedure guides students through the growth of a submerged Penicillium chrysogenum culture. Subsequent steps include extraction of the penicillin by adsorption onto activated charcoal, extraction with acetone, and qualitative testing of the drug on a bacterial culture. The laboratory procedure is designed for freshman-level health science chemistry courses. This procedure produces minimal waste, which can be disposed of by the appropriate use of an autoclave.

  16. Reciprocal symmetry plots as a representation of countercurrent chromatograms.

    PubMed

    Friesen, J Brent; Pauli, Guido F

    2007-03-15

    Traditionally, chromatograms in countercurrent chromatography (CCC) have been plotted with retention volume or time on the x-axis. However, the distribution constant (K) is a more appropriate, reproducible value for the x-axis, because it is a physicochemical property of a particular analyte in a particular solvent system. Therefore, K is independent of both the total column volume and the stationary-phase volume ratio (SF) of the column. Going one step beyond simple K plots, the reciprocal symmetry (ReS) plot, with K and 1/K positioned on either side of a line of symmetry on the x-axis, represents all K values, zero to infinity. Based on experimental evidence, using a mixture of CCC reference standards, the ReS plot demonstrates both the invertible and "symmetric" nature of CCC, a consequence of the exchange of the mobile and stationary phases by reversing the direction of the flow and the symmetry of the liquid-liquid partitioning process between two immiscible phases, respectively. Moreover, the interval of optimal resolution can be centered on the ReS plot to focus on K values of interest, establishing the reciprocal shifted symmetry (ReSS) plots in CCC. Improved representation of peak shape across the whole CCC polarity range is an added advantage of ReSS plots over both K and classical retention volume plots.

  17. Binary concepts and standardization in counter-current separation technology.

    PubMed

    Friesen, J B; Pauli, G F

    2009-05-08

    Counter-current separation (CS) technology is currently faced with the challenge of being fit for the purpose of omics analysis, which involves highly complex samples and digitized research environments. Resembling a network of binary decisions, CS requires standardization of operation parameters in order to be efficient. While recent CS engineering solutions uniformly involve centrifugal force designs to overcome the limitation of the earth's 1xg force, factors of instrument design, operation, and graphical representation of the outcome are equally important targets for standardization. For example, chromatograms that emphasize the unique K-based nature of CS, such as reciprocal symmetry (ReS) plots, foster the fundamental understanding of CS operation. Because significant differences exist in underlying mechanism (e.g., stationary phase volume), outcome (e.g., construction of chromatograms), and scale (e.g., factors affecting overall method sensitivity) of solid-liquid vs. liquid-liquid chromatography technologies, standardization will enable the systematic exploration of the differential properties of the two LC technologies, and will be key to making CS fit for the digital omics age.

  18. Annual and longitudinal variations of the Pacific North Equatorial Countercurrent

    NASA Technical Reports Server (NTRS)

    Lolk, Nina K.

    1992-01-01

    The climatological annual cycle of the Pacific North Equatorial Countercurrent (NECC) simulated by an ocean general circulation model (OGCM) was studied. The longitudinal variation of transports, degree of geostrophy, and the relationship between Ekman pumping and vertical displacement of the thermocline were emphasized. The longitudinal variation was explored using six sections along 150 deg E, 180 deg, 160 deg W, 140 deg W, 125 deg W, and 110 deg W. A primitive equation OGCM of the Pacific Ocean was run for three years and the fields used were from the third year. The fields consisted of zonal, meridional, and vertical current components and temperature and salinity averaged every three days. The model was forced with the Hellerman and Rosenstein climatological wind stress. The mean annual eastward transport (19.9 Sv) was largest at 160 deg W. The maximum-current boundaries along 160 deg W were 9.2 deg N (1.0 deg), 5.1 deg N (1.1 deg), and 187 m (90.6 m). The annual-cycle amplitude of the NECC was greatest between 160 deg W and 140 deg W. Although the NECC is geostrophic to the first order, deviations from geostrophy were found in the boreal spring and summer near the southern boundary and near the surface. Meridional local acceleration played a role between 3 deg N-5 deg N.

  19. Robust design of binary countercurrent adsorption separation processes

    SciTech Connect

    Storti, G. ); Mazzotti, M.; Morbidelli, M.; Carra, S. )

    1993-03-01

    The separation of a binary mixture, using a third component having intermediate adsorptivity as desorbent, in a four section countercurrent adsorption separation unit is considered. A procedure for the optimal and robust design of the unit is developed in the frame of Equilibrium Theory, using a model where the adsorption equilibria are described through the constant selectivity stoichiometric model, while mass-transfer resistances and axial mixing are neglected. By requiring that the unit achieves complete separation, it is possible to identify a set of implicity constraints on the operating parameters, that is, the flow rate ratios in the four sections of the unit. From these constraints explicit bounds on the operating parameters are obtained, thus yielding a region in the operating parameters space, which can be drawn a priori in terms of the adsorption equilibrium constants and the feed composition. This result provides a very convenient tool to determine both optimal and robust operating conditions. The latter issue is addressed by first analyzing the various possible sources of disturbances, as well as their effect on the separation performance. Next, the criteria for the robust design of the unit are discussed. Finally, these theoretical findings are compared with a set of experimental results obtained in a six port simulated moving bed adsorption separation unit operated in the vapor phase.

  20. Eddy properties in the Subtropical Countercurrent, Western Philippine Sea

    NASA Astrophysics Data System (ADS)

    Ramp, S. R.; Colosi, J. A.; Worcester, P. F.; Bahr, F. L.; Heaney, K. D.; Mercer, J. A.; Van Uffelen, L. J.

    2017-07-01

    An array of six oceanographic moorings with acoustic and environmental sensors was deployed in the central Philippine Sea from April 2010 to April 2011. The location spanned 18-23°N, 124 - 130°E in the Subtropical Countercurrent (STCC). The most prominent feature of the data set was a densely-packed eddy field with about equal numbers of cyclones and anticyclones moving westward at 6-12 km d-1. Eddies of either sign displaced the thermocline about ±50 m and had surface velocities exceeding 110 cm s-1. While warm eddies were slightly larger than cold eddies, the distance to maximum radial velocity was similar for both at about 65 km, close to the local Rossby radius of deformation. The steepness parameter U/c in the eddies ranged from 3 to 10, accompanied by relative vorticity of order 0.1-0.3 f, suggesting nonlinear, quasigeostrophic features with trapped cores rather than linear waves. This was borne out by the water mass analysis which showed high salinity, high spice North Pacific Tropical Water (NPTW) being transported westward in the warm eddy cores. The total KE and APE in eddies of both signs was about 1×1015 J with 85% of the APE and 74% of the KE located above 250 m depth. This equipartitioning of energy suggests mature eddies near equilibrium, that had been evolving for some time as they propagated into the area from the east.

  1. Two-zone countercurrent smelter system and process

    DOEpatents

    Cox, James H.; Fruehan, Richard J.; Elliott, deceased, John F.

    1995-01-01

    A process for continuously smelting iron ore by use of coal to yield molten iron or semi-steel is disclosed. The process comprises the steps of establishing a melt covered by slag; inducing the slag and the molten iron to flow countercurrently to one another, toward opposite ends of the smelter; maintaining iron oxide-reducing conditions in that zone of the smelter towards which the slag flows; maintaining carbon-oxidizing conditions in that zone of the smelter towards which the molten iron flows; continuously or semicontinuously tapping the slag from the reducing zone end of the smelter; continuously or semicontinuously tapping the molten iron from the oxidizing zone end of the smelter; and adding to both zones iron ore, coal, oxygen, and flux at addition rates sufficient to keep the molten iron in the reducing zone substantially saturated with carbon, maintain in the slag being tapped an FeO content of about 5 weight percent or less, and maintain in the molten iron being tapped a carbon content of about 0.5 to 5 weight percent. A slag dam preferably is included in the smelter, to impede the backflow of the slag from the reducing zone to the oxidizing zone. A metal bath dam with one or more flow-through portals also is preferably used, submerged below the slag dam, to impede the backflow of the hot metal.

  2. Two-zone countercurrent smelter system and process

    DOEpatents

    Cox, J.H.; Fruehan, R.J.; Elliott, J.F.

    1995-01-03

    A process for continuously smelting iron ore by use of coal to yield molten iron or semi-steel is disclosed. The process comprises the steps of establishing a melt covered by slag; inducing the slag and the molten iron to flow countercurrently to one another, toward opposite ends of the smelter; maintaining iron oxide-reducing conditions in that zone of the smelter towards which the slag flows; maintaining carbon-oxidizing conditions in that zone of the smelter towards which the molten iron flows; continuously or semicontinuously tapping the slag from the reducing zone end of the smelter; continuously or semicontinuously tapping the molten iron from the oxidizing zone end of the smelter; and adding to both zones iron ore, coal, oxygen, and flux at addition rates sufficient to keep the molten iron in the reducing zone substantially saturated with carbon, maintain in the slag being tapped an FeO content of about 5 weight percent or less, and maintain in the molten iron being tapped a carbon content of about 0.5 to 5 weight percent. A slag dam preferably is included in the smelter, to impede the backflow of the slag from the reducing zone to the oxidizing zone. A metal bath dam with one or more flow-through portals also is preferably used, submerged below the slag dam, to impede the backflow of the hot metal. 8 figures.

  3. Countercurrent fixed-bed gasification of biomass at laboratory scale

    SciTech Connect

    Di Blasi, C.; Signorelli, G.; Portoricco, G.

    1999-07-01

    A laboratory-scale countercurrent fixed-bed gasification plant has been designed and constructed to produce data for process modeling and to compare the gasification characteristics of several biomasses (beechwood, nutshells, olive husks, and grape residues). The composition of producer gas and spatial temperature profiles have been measured for biomass gasification at different air flow rates. The gas-heating value always attains a maximum as a function of this operating variable, associated with a decrease of the air-to-fuel ratio. Optical gasification conditions of wood and agricultural residues give rise to comparable gas-heating values, comprised in the range 5--5.5 MJ/Nm{sup 3} with 28--30% CO, 5--7% CO{sub 2}, 6--8% H{sub 2}, 1--2% CH{sub 4}, and small amounts of C{sub 2}- hydrocarbons (apart from nitrogen). However, gasification of agricultural residues is more difficult because of bed transport, partial ash sintering, nonuniform flow distribution, and the presence of a muddy phase in the effluents, so that proper pretreatments are needed for largescale applications.

  4. Counter-current flow limitation in thin rectangular channels

    NASA Astrophysics Data System (ADS)

    Cheng, Lap Y.

    The phenomenon of counter-current flow limitation (CCFL) in thin rectangular channels is important in determining the heat removal capability of research reactors which use plate-type fuel elements similar to the MTR design. An analytical expression for predicting CCFL in narrow rectangular channels was derived from the momentum equations for the liquid and gas phase. The model assumes that the liquid downflow is in the form of a film along the narrower side walls of the channel, while the gas flow occupies the wide span of the rectangular channel. The average thickness of liquid film is related to the rate of gas flow through a stability criterion for the liquid film. The CCFL correlation agrees with air/water data taken at relatively high gas velocities. Depending on the magnitude of the dimensionless channel width, the new CCFL correlation approaches zero liquid penetration either in the form of a Wallis correlation or in terms of a Kutateladze number. The new correlation indicates that for a thin rectangular channel, the constant C in the Wallis flooding correlation depends on the aspect ratio of the channel. The approach to the appropriate asymptotic solutions also justifies the use of twice the wide span as the correct length scale for thin rectangular channels.

  5. Ultraefficient reduced model for countercurrent two-layer flows

    NASA Astrophysics Data System (ADS)

    Lavalle, Gianluca; Vila, Jean-Paul; Lucquiaud, Mathieu; Valluri, Prashant

    2017-01-01

    We investigate the dynamics of two superposed layers with density contrast flowing countercurrent inside a channel, when the lower layer is much thinner than the wavelength of interfacial waves. We apply a low-dimensional film model to the bottom (heavier) layer and introduce a fast and efficient method to predict the onset of flow reversal in this phase. We study three vertical scenarios with different applied pressure gradients and compare the temporal growth rates of linear and weakly nonlinear waves to the Orr-Sommerfeld problem and to the weakly nonlinear theory, respectively. At the loading point, i.e., when a large wave hump stands at the interface, our spatiotemporal analysis shows that the system is absolutely unstable. We then present profiles of nonlinear saturated waves, pressure field, and streamline distribution in agreement with direct numerical simulation. The reduced model presented here allows us to explore the effect of the upper-layer speed on the wave pattern, showing that the wave profile is very sensitive when the mean film thickness, rather than the liquid flow rate, is maintained constant in the simulation. In addition, we show the strong effect of surface tension on both the maximum wave hump and the crest steepness before the loading point. Finally, we reveal how the nonlinear wave speed affects the vortex distribution within the lower layer by analyzing the stream function under different scenarios.

  6. Enantioselective Recognition in Solution: The Case of Countercurrent Chromatography

    NASA Astrophysics Data System (ADS)

    Rubio, Núria; Minguillón, Cristina

    Countercurrent chromatography (CCC) is a preparative separation technique that works with a liquid stationary phase. Biphasic liquid systems are needed to perform a separation. Since a chiral selector is required to perform enantiomer separations, special requirements are imposed in CCC. The chiral selector (CS) must be located in the stationary phase since partitioning with the mobile phase would cause losses of the valuable chiral selector in the mobile phase. Sulfated cyclodextrins and proteins were used as polar CS located in the polar stationary phase (reversed phase mode). Apolar CSs such as N-dodecyl-L-proline 3,5-dimethylanilide or Whelk-O selectors, quinine and quinidine derivatives, cellulose or amylose apolar derivatives were used located in the apolar stationary phase (normal phase mode). The special CCC displacement method called pH-zone refining was found useful in the increase of the loading capacity for cellulose, quinine, quinidine, and proline-derived selectors. Dual and multidual mode uses of CCC could produce an increase in peak separation thereby broadening the applicability of moderately enantioselective CSs.

  7. Use of limonene in countercurrent chromatography: a green alkane substitute.

    PubMed

    Faure, Karine; Bouju, Elodie; Suchet, Pauline; Berthod, Alain

    2013-05-07

    Counter-current chromatography (CCC) is a preparative separation technique working with the two liquid phases of a biphasic liquid system. One phase is used as the mobile phase when the other, the stationary phase, is held in place by centrifugal fields. Limonene is a biorenewable cycloterpene solvent coming from orange peel waste. It was evaluated as a possible substitute for heptane in CCC separations. The limonene/methanol/water and heptane/methanol/water phase diagrams are very similar at room temperature. The double bonds of the limonene molecule allows for possible π-π interactions with solutes rendering limonene slightly more polar than heptane giving small differences in solute partition coefficients in the two systems. The 24% higher limonene density is a difference with heptane that has major consequences in CCC. The polar and apolar phases of the limonene/methanol/water 10/9/1 v/v have -0.025 g/cm(3) density difference (lower limonene phase) compared to +0.132 g/cm(3) with heptane (upper heptane phase). This precludes the use of this limonene system with hydrodynamic CCC columns that need significant density difference to retain a liquid stationary phase. It is an advantage with hydrostatic CCC columns because density difference is related to the working pressure drop: limonene allows one to work with high centrifugal fields and moderate pressure drop. Limonene has the capability to be a "green" alternative to petroleum-based solvents in CCC applications.

  8. Hydrogen isotope separation by bipolar electrolysis with countercurrent electrolyte flow

    SciTech Connect

    Ramey, D.W.; Petek, M.; Taylor, R.D.; Fisher, P.W.; Kobisk, E.H.; Ramey, J.; Sampson, C.A.

    1980-04-01

    Separation of hydrogen isotopes has been successfully demonstrated using bipolar electrolysis combined with electrolyte flow countercurrent to the transport of hydrogen isotope species. Use of multibipolar electrode cells in a squared-off cascade is shown theoretically to be capable of efficient tritium separation. Experimental operation of multibipolar cells and analysis of their operation by McCabe-Thiele techniques is described. Palladium-25% silver alloy was found to be suitable as a material for bipolar electrodes permitting high hydrogen throughput with chemical and mechanical stability. Bipolar separation factors, at high current density, using NaOH (NaOD) as the electrolyte, are large (..cap alpha../sub DT/ = 2.0, ..cap alpha../sub HT/ = 11 at 90/sup 0/C). Calculated mass transfer, as determined using a squared-off cascade model, together with observed electrical power consumption suggest that about 21 percent less power will be required for bipolar electrolytic separation as compared with normal electrolysis. This estimate only represents the present level of development. Separation of tritium from light and heavy water using the bipolar electrolysis process appears to offer significant advantages as compared with direct electrolysis. The simplicity and efficiency of the multibipolar cell offer great potential for designing a very compact separation facility which, in turn, will minimize containment cost when high tritium concentrations are encountered.

  9. Stability of steam-water countercurrent stratified flow

    SciTech Connect

    Lee, S C

    1985-10-01

    Two flow instabilities which limit the normal condensation processes in countercurrent stratified steam-water flow have been identified experimentally: flooding and condensation-induced waterhammer. In order to initiate condensation-induced waterhammer in nearly horizontal or moderately-inclined steam/subcooled-water flow, two conditions, the appearance of a wavy interface and complete condensation of the incoming steam, are necessary. Analyses of these conditions are performed on a basis of flow stability and heat transfer considerations. Flooding data for several inclinations and channel heights are collected. Effects of condensation, inclination angle and channel height on the flooding characteristics are discussed. An envelope theory for the onset of flooding in inclined stratified flow is developed, which agrees well with the experimental data. Some empirical information on basic flow parameters, such as mean film thickness and interfacial friction factor required for this theory are measured. The previous viewpoints on flooding appear not to conflict with the present experimental data in nearly horizontal flow but the flooding phenomena in nearly vertical flow appear to be more complicated than those described by these viewpoints because of liquid droplet entrainment.

  10. Local properties of countercurrent stratified steam-water flow

    SciTech Connect

    Kim, H J

    1985-10-01

    A study of steam condensation in countercurrent stratified flow of steam and subcooled water has been carried out in a rectangular channel/flat plate geometry over a wide range of inclination angles (4/sup 0/-87/sup 0/) at several aspect ratios. Variables were inlet water and steam flow rates, and inlet water temperature. Local condensation rates and pressure gradients were measured, and local condensation heat transfer coefficients and interfacial shear stress were calculated. Contact probe traverses of the surface waves were made, which allowed a statistical analysis of the wave properties. The local condensation Nusselt number was correlated in terms of local water and steam Reynolds or Froude numbers, as well as the liquid Prandtl number. A turbulence-centered model developed by Theofanous, et al. principally for gas absorption in several geometries, was modified. A correlation for the interfacial shear stress and the pressure gradient agreed with measured values. Mean water layer thicknesses were calculated. Interfacial wave parameters, such as the mean water layer thickness, liquid fraction probability distribution, wave amplitude and wave frequency, are analyzed.

  11. Herbal preparation extract for skin after radiotherapy treatment. Part One--Preclinical tests.

    PubMed

    Skalska-Kamińska, Agnieszka; Woźniak, Anna; Paduch, Roman; Kocjan, Ryszard; Rejdak, Robert

    2014-01-01

    Naran R is a herbal composition made of Plantago lanceolate folium, Malvae arboreae flos, Calendulae flos, Chamomillae inflorescentia, Lamii albi flos to prepare compresses or to wash skin with inflammations. The extract of this preparation is mixed to be applied as an ointment on patients' skin after radiotherapy. Experiments performed in vitro are part of pre-clinical tests with Naran R ointment. This study examined the impact of the plant composition for ethanol-water extract on human skin fibroblasts (HSF) culture. Samples of extract, prepared from patented amounts of herbs, were in the range of 25-225 μg/mL. Six methods were applied: standard spectrophotometric 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay, neutral red (NR) uptake assay, DPPH free radical scavenging test, labeling of cytoskeleton F-actin, staining of argyrophilic nucleolar organizer regions (AgNORs) and trypan blue coloration. The extract concentration 75 μg/mL was established as safe for application on human skin. In labeling of F-actin with rhodamine-phalloidin dye at this concentration the cytoskeleton was stable. The extract did not influence the membrane stability and had positive influence on the proliferation activity. It was confirmed in AgNOR test during incubation with extract, which led to formation of larger amount of smaller nucleolins. In DPPH scavenging activity test, the extract revealed over 8% higher free-radical scavenging activity in comparison to control. After trypan blue staining, the extract in concentration 125 μg/mL significantly lowered the cell viability. When the cytotoxic and anti-proliferative activity of the extracts were analyzed, MTT and Neutral Red (NR) methods were used. The cells' viability was maintained on a constant level (80-110%) after 24, 48 and 72 h of incubation. During all time of NR test (72 h) and even when 225 μg/mL of extract was applied, the viability of cells was in range 80-110% of control. Positive influence

  12. The Antinociceptive Effects of Hydroalcoholic Extract of Borago Officinalis Flower in Male Rats Using Formalin Test

    PubMed Central

    Shahraki, Mohammad Reza; Ahmadimoghadm, Mahdieh; Shahraki, Ahmad Reza

    2015-01-01

    Introduction: Borago officinalis flower (borage) is a known sedative in herbal medicine; the aim of the present study was to evaluate the antinociceptive effect of borage hydroalcoholic extract in formalin test male rats. Methods: Fifty-six adult male albino Wistar rats were randomly divided into seven groups: Control groups of A (intact), B (saline), and C (Positive control) plus test groups of D, E, F, and G (n=8). The groups D, E, and F received 6.25, 12.5, and 25 mg/kg, Borago officinalis flower hydroalcholic extract before the test, respectively but group G received 25 mg/kg borage extract and aspirin before the test. A biphasic pain was induced by injection of formalin 1%. The obtained data were analyzed by SPSS software ver. 17 employing statistical tests of Kruskal-Wallis and Mann-Whitney. The results were expressed as mean±SD. Statistical differences were considered significant at P<0.05. Results: The results revealed that the acute and chronic pain behavior score in test groups of D, E, F, and G significantly decreased compared to groups A and B, but this score did not show any difference compared to group C. Moreover, chronic pain behavior score in group G was significantly lower than all other groups. Discussion: The results indicated that Borago officinalis hydroalcoholic extract affects the acute and chronic pain behavior response in formaline test male rats. PMID:26649166

  13. The Antinociceptive Effects of Hydroalcoholic Extract of Borago Officinalis Flower in Male Rats Using Formalin Test.

    PubMed

    Shahraki, Mohammad Reza; Ahmadimoghadm, Mahdieh; Shahraki, Ahmad Reza

    2015-10-01

    Borago officinalis flower (borage) is a known sedative in herbal medicine; the aim of the present study was to evaluate the antinociceptive effect of borage hydroalcoholic extract in formalin test male rats. Fifty-six adult male albino Wistar rats were randomly divided into seven groups: Control groups of A (intact), B (saline), and C (Positive control) plus test groups of D, E, F, and G (n=8). The groups D, E, and F received 6.25, 12.5, and 25 mg/kg, Borago officinalis flower hydroalcholic extract before the test, respectively but group G received 25 mg/kg borage extract and aspirin before the test. A biphasic pain was induced by injection of formalin 1%. The obtained data were analyzed by SPSS software ver. 17 employing statistical tests of Kruskal-Wallis and Mann-Whitney. The results were expressed as mean±SD. Statistical differences were considered significant at P<0.05. The results revealed that the acute and chronic pain behavior score in test groups of D, E, F, and G significantly decreased compared to groups A and B, but this score did not show any difference compared to group C. Moreover, chronic pain behavior score in group G was significantly lower than all other groups. The results indicated that Borago officinalis hydroalcoholic extract affects the acute and chronic pain behavior response in formaline test male rats.

  14. Genotoxicity testing of Persicariae Rhizoma (Persicaria tinctoria H. Gross) aqueous extracts.

    PubMed

    Lee, Won Ho; Choi, Seong Hun; Kang, Su Jin; Song, Chang Hyun; Park, Soo Jin; Lee, Young Joon; Ku, Sae Kwang

    2016-07-01

    Persicariae Rhizoma (PR) has been used as an anti-inflammatory and detoxification agent in Korea, and contains the biologically active dyes purple indirubin and blue indigo. Despite synthetic indigo showing genotoxic potential, thorough studies have not been carried out on the genotoxicity of PR. The potential genotoxicity of an aqueous extract of PR containing indigo (0.043%) and indirubin (0.009%) was evaluated using a standard battery of tests for safety assessment. The PR extract did not induce any genotoxic effects under the conditions of this study. The results of a reverse mutation assay in four Salmonella typhimurium strains and one Escherichia coli strain indicated that PR extract did not increase the frequency of revertant colonies in any strain, regardless of whether S9 mix was present or not. The PR extract also did not increase chromosomal aberrations in the presence or absence of S9 mix. Although slight signs of diarrhea were restrictedly detected in the mice treated with 2,000 mg/kg PR extract, no noteworthy changes in the frequency of micronucleated polychromatic erythrocytes were observed at doses ≤2,000 mg/kg in a bone marrow micronucleus test. These results indicate the potential safety of the PR extract, particularly if it is consumed in small amounts compared with the quantities used in the genotoxicity tests.

  15. Genotoxicity testing of Persicariae Rhizoma (Persicaria tinctoria H. Gross) aqueous extracts

    PubMed Central

    LEE, WON HO; CHOI, SEONG HUN; KANG, SU JIN; SONG, CHANG HYUN; PARK, SOO JIN; LEE, YOUNG JOON; KU, SAE KWANG

    2016-01-01

    Persicariae Rhizoma (PR) has been used as an anti-inflammatory and detoxification agent in Korea, and contains the biologically active dyes purple indirubin and blue indigo. Despite synthetic indigo showing genotoxic potential, thorough studies have not been carried out on the genotoxicity of PR. The potential genotoxicity of an aqueous extract of PR containing indigo (0.043%) and indirubin (0.009%) was evaluated using a standard battery of tests for safety assessment. The PR extract did not induce any genotoxic effects under the conditions of this study. The results of a reverse mutation assay in four Salmonella typhimurium strains and one Escherichia coli strain indicated that PR extract did not increase the frequency of revertant colonies in any strain, regardless of whether S9 mix was present or not. The PR extract also did not increase chromosomal aberrations in the presence or absence of S9 mix. Although slight signs of diarrhea were restrictedly detected in the mice treated with 2,000 mg/kg PR extract, no noteworthy changes in the frequency of micronucleated polychromatic erythrocytes were observed at doses ≤2,000 mg/kg in a bone marrow micronucleus test. These results indicate the potential safety of the PR extract, particularly if it is consumed in small amounts compared with the quantities used in the genotoxicity tests. PMID:27347027

  16. Developments in beet and cane sugar extraction

    SciTech Connect

    Iverson, C.; Schwartzberg, H.G.

    1984-01-01

    This paper reviews the various types of extractors used in the extraction of sugar from beet and sugar cane. The types of extractors described are as follows:- Countercurrent Screw - Conveyor Extractors, (Tower Extractors, Slope Extractors), Countercurrent Drag Chain Extractors, Multistage Cross-Flow Extractors, Trommel Extractors, Multistage Scroll Extractors, Diffustion Batteries. Reduced capital costs and power expenditures and slightly higher cane sugar yields can be obtained by combined milking and diffusion extraction as opposed to multi-stage milling. The mechanical reliability of the machinery is emphasized and special attention is given to extraction procedures. Nowadays the trend in beet and cane sugar extraction is toward the use of larger and larger units which helps minimize labor and capital costs per unit of product.

  17. Extraction of model performance from wall data in a 2-dimensional transonic flexible walled test section

    NASA Technical Reports Server (NTRS)

    Goodyer, M. J.

    1982-01-01

    Data obtained from the boundary of a test section provides information on the model contained within it. A method for extracting some of this data in two dimensional testing is described. Examples of model data are included on lift, pitching moment and wake displacement thickness. A FORTRAN listing is also described, having a form suitable for incorporation into the software package used in the running of such a test section.

  18. Cytotoxicity of aqueous extracts of Rosmarinus officinalis L. (Labiatae) in plant test system.

    PubMed

    Cardoso, G H S; Dantas, E B S; Sousa, F R C; Peron, A P

    2014-11-01

    This study investigated the cytotoxic activity of Rosmarinus officinalis L. (rosemary) aqueous extract on the cell cycle of Allium cepa. To this end, crude aqueous leaf extracts at four concentrations, 0.02, 0.04, 0.06 and 0.08 mg/mL, were tested on A. cepa meristematic root cells, at exposure times of 24 and 48 h. Slides were prepared by the crushing technique, and cells analyzed throughout the cell cycle, totaling 5,000 for each control group and concentration. The four concentrations tested, including the lowest and considered ideal for use, at all exposure times, showed a significant antiproliferative effect on the cell cycle of this test system and presented a high number of cells in prophase. Our results evidenced the cytotoxicity of rosemary extracts, under the studied conditions.

  19. SAMPLE RESULTS FROM THE NEXT GENERATION SOLVENT PROGRAM REAL WASTE EXTRACTION-SCRUB-STRIP TESTING

    SciTech Connect

    Peters, T.; Washington, A.

    2013-06-03

    Savannah River National Laboratory (SRNL) performed multiple Extraction-Scrub-Strip (ESS) testing using real waste solutions, and three Next Generation Solvent (NGS) variations, which included radiologically clean pure NGS, a blend of radiologically clean NGS and radiologically clean BOBCalixC6 (NGS-MCU), and a blend of radiologically clean NGS and radiologically contaminated BOBCalixC6 from the MCU Solvent system. The results from the tests indicate that both the NGS and the NGS-MCU blend exhibit adequate extraction, scrub and strip behavior.

  20. Sample Results From The Next Generation Solvent Program Real Waste Extraction-Scrub-Strip Testing

    SciTech Connect

    Peters, T. B.; Washington, A. L. II

    2013-08-08

    Savannah River National Laboratory (SRNL) performed multiple Extraction-Scrub-Strip (ESS) testing using real waste solutions, and three Next Generation Solvent (NGS) variations, which included radiologically clean pure NGS, a blend of radiologically clean NGS and radiologically clean BOBCalixC6 (NGS-MCU), and a blend of radiologically clean NGS and radiologically contaminated BOBCalixC6 from the MCU Solvent system. The results from the tests indicate that both the NGS and the NGS-MCU blend exhibit adequate extraction, scrub and strip behavior.

  1. In vitro human skin irritation test for evaluation of medical device extracts.

    PubMed

    Casas, J W; Lewerenz, G M; Rankin, E A; Willoughby, J A; Blakeman, L C; McKim, J M; Coleman, K P

    2013-12-01

    The aim of this study was to determine if the EpiDerm™ reconstructed human skin model (MatTek Corp.) could be an acceptable alternative to the ISO 10993-required rabbit skin irritation test for assessing medical device biocompatibility. Eleven medical device polymers were tested. Four extracts were prepared per polymer, two each with saline and sesame oil; half were spiked with two R-38 irritants, lactic acid for saline extracts and heptanoic acid for the sesame oil extracts. Tissue viability was assessed by MTT reduction and the proinflammatory response was assessed by IL-1α release. LOAELs of 2% for lactic acid in saline and 0.7% for heptanoic acid in sesame oil were determined. A cell viability reduction of >50% was indicative of skin irritation. Cells exposed to saline extracts spiked with 3.25% lactic acid had significantly reduced mean cell viabilities (12.6-17.2%). Cells exposed to sesame oil extracts spiked with 1.25% heptanoic acid also exhibited reduced mean cell viabilities (25.5%-41.7%). All spiked cells released substantial amounts of IL-1α (253.5-387.4pg/ml) signifying a proinflammatory response. These results indicate that the EpiDerm™ model may be a suitable in vitro replacement for the assessment of the irritation potential of medical device extracts.

  2. Distribution ratio, distribution constant and partition coefficient. Countercurrent chromatography retention of benzoic acid.

    PubMed

    Berthod, Alain; Mekaoui, Nazim

    2011-09-09

    There is some confusion in chromatography between terms such as solute distribution ratio, distribution constant and partition coefficient. These terms are very precisely defined in the field of liquid-liquid systems and liquid-liquid extraction as well as in the field of chromatography with sometimes conflicting definitions. Countercurrent chromatography (CCC) is a chromatographic technique in which the stationary phase is a support-free liquid. Since the mobile phase is also liquid, biphasic liquid systems are used. This work focuses on the exact meaning of the terms since there are consequences on experimental results. The retention volumes of solutes in CCC are linearly related to their distribution ratios. The partition coefficient that should be termed (IUPAC recommendation) distribution constant is linked to a single definite species. Using benzoic acid that can dimerize in heptane and ionize in aqueous phase and an 18 mL hydrodynamic CCC column, the role and relationships between parameters and the consequences on experimental peak position and shape are discussed. If the heptane/water distribution constant (marginally accepted to be called partition coefficient) of benzoic acid is 0.2 at 20 °C and can be tabulated in books, its CCC measured distribution ratio or distribution coefficient can change between zero (basic aqueous mobile phase) and more than 25 (acidic aqueous mobile phase and elevated concentration). Benzoic acid distribution ratio and partition coefficient coincide only when both dimerization and ionization are quenched, i.e. at very low concentration and pH 2. It is possible to quench dimerization adding butanol in the heptane/water system. However, butanol additions also affect the partition coefficient of benzoic acid greatly by increasing it. Copyright © 2010 Elsevier B.V. All rights reserved.

  3. Comparison of QIAGEN automated nucleic acid extraction methods for CMV quantitative PCR testing.

    PubMed

    Miller, Steve; Seet, Henrietta; Khan, Yasmeen; Wright, Carolyn; Nadarajah, Rohan

    2010-04-01

    We examined the effect of nucleic acid extraction methods on the analytic characteristics of a quantitative polymerase chain reaction (PCR) assay for cytomegalovirus (CMV). Human serum samples were extracted with 2 automated instruments (BioRobot EZ1 and QIAsymphony SP, QIAGEN, Valencia, CA) and CMV PCR results compared with those of pp65 antigenemia testing. Both extraction methods yielded results that were comparably linear and precise, whereas the QIAsymphony SP had a slightly lower limit of detection (1.92 log(10) copies/mL vs 2.26 log(10) copies/mL). In both cases, PCR was more sensitive than CMV antigen detection, detecting CMV viremia in 12% (EZ1) and 21% (QIAsymphony) of antigen-negative specimens. This study demonstrates the feasibility of using 2 different extraction techniques to yield results within 0.5 log(10) copies/mL of the mean value, a level that would allow for clinical comparison between different laboratory assays.

  4. Genotoxicity testing of extracts from aflatoxin-contaminated peanut meal, following chemical decontamination.

    PubMed

    Hoogenboom, L A; Polman, T H; Neal, G E; Verma, A; Guyomard, C; Tulliez, J; Gautier, J P; Coker, R D; Nagler, M J; Heidenreich, E; Delort-Laval, J

    2001-04-01

    One of the most important concerns in the decontamination of aflatoxin-containing feed commodities is the safety of the products for food-producing animals and for human consumption of products derived from these animals. A new method, based on the use of florisil and C18 solid phase extraction columns, was developed for the preparation of extracts from decontaminated peanut meal, which allowed testing with in vitro genotoxicity assays without interference of the residual aflatoxin B1. Recovery of degradation products in the extracts was evaluated by the use of radiolabelled [14C]-aflatoxin B1 (AFB1) added to naturally-contaminated peanut meal (3.5 mg AFB1/kg). The meal was treated by a small-scale version of an industrial decontamination process based on ammoniation. Following decontamination, more than 90% of the label could not be extracted from the meal. AFB1 accounted for about 10% of the radiolabel present in the extractable fraction, indicating a total AFB1 reduction of more than 99%. Decontamination of the meal by a number of other small- and industrial-scale ammonia-based processes resulted in similar efficiencies. Application of the extraction procedure resulted in AFB1-rich and AFB1-poor fractions, the latter containing half of the extractable decontamination products but less than 1% of the residual AFB1. Testing in the Salmonella/microsome mutagenicity assay (TA 100, with S9-mix) of the original crude extracts and AFB1-rich fractions prepared from non-treated and decontaminated meal, showed the positive results expected from the AFB1 contents as determined by HPLC analysis. Analysis and testing of the AFB1-poor fractions showed that the various decontamination processes not only resulted in a successful degradation of AFB1 but also did not produce other potent mutagenic compounds. Slight positive results obtained with these extracts were similar for the untreated and treated meals and may be due to unknown compounds originally present in the meal

  5. Developing and testing an alkaline-side solvent extraction process for technetium separation from tank waste.

    SciTech Connect

    Leonard, R.A.; Conner, C.; Liberatore, M.W.; Bonnesen, P.V.; Moyer, B.A.; Presley, D.J.; Lumetta, G.J.

    1997-12-05

    Engineering development and testing of the SRTALK solvent extraction process are discussed in this paper. This process provides a way to carry out alkaline-side removal and recovery of technetium in the form of pertechnetate anion from nuclear waste tanks within the DOE complex. The SRTALK extractant consists of a crown ether, bis-4,4'(5')[(tert-butyl)cyclohexano] -18-crown-6, in a modifier, tributyl phosphate, and a diluent, Isopar{reg_sign}L. The SRTALK flowsheet given here separates technetium from the waste and concentrates it by a factor often to minimize the load on the downstream evaporator for the technetium effluent. In this work, we initially generated and correlated the technetium extraction data, measured the dispersion number for various processing conditions, and determined hydraulic performance in a single-stage 2-cm centrifugal contactor. Then we used extraction-factor analysis, single-stage contactor tests, and stage-to-stage process calculations to develop a SRTALK flowsheet. Key features of the flowsheet are (1) a low organic-to-aqueous (O/A) flow ratio in the extraction section and a high O/A flow ratio in the strip section concentrate the technetium and (2) the use of a scrub section to reduce the salt load in the concentrated technetium effluent. Finally, the SRTALK process was evaluated in a multistage test using a synthetic tank waste. This test was very successful. Initial tests with actual waste from the Hanford nuclear waste tanks show the same technetium extractability as determined with the synthetic waste feed. Therefore, technetium removal from actual tank wastes should also work well using the SRTALK process.

  6. Sensitization to fungi: epidemiology, comparative skin tests, and IgE reactivity of fungal extracts.

    PubMed

    Mari, A; Schneider, P; Wally, V; Breitenbach, M; Simon-Nobbe, B

    2003-10-01

    Several fungal species are known to cause severe respiratory and cutaneous allergic diseases. Extracts from several allergenic fungi are used for in vivo and in vitro tests, as standard preparations are still not available. The aims are to define the pattern of in vivo and in vitro IgE reactivity to fungal species in an allergic population with respiratory symptoms; to determine the influence of different extract preparations on diagnostic results; and to evaluate whether there exists a relationship between the diagnostic pattern of reactivity and the pattern of specific IgE reactivity in immunoblots. Skin prick tests were applied to a cohort of 4962 respiratory subjects, aged 3-80 years. Fungal extracts from Alternaria, Aspergillus, Candida, Cladosporium, Penicillium, Saccharomyces, and Trichophyton were used, along with extracts from pollens, mites, and animal dander. Demographical and diagnostic data were recorded. IgE detection was carried out with the same allergenic extracts plus Malassezia. Comparative skin tests and IgE detection were carried out using extracts from three commercial suppliers. IgE immunoblots were carried out with the same panel of commercial fungal extracts and were compared with in-house extracts. Data analysis was carried out by grouping the population on the basis of their reactivity to a single, to two or to more than two, mould species. Nineteen percent of the allergic population reacted to at least one fungal extract by means of the skin test. Alternaria and Candida accounted for the largest number of positive tests, and along with Trichophyton they were the main sensitizers in the subset of patients with an isolated sensitization. The prevalence of skin test reactivity increased for these three fungi in the subsets with two associated reactivities and, furthermore, in the subset showing reactivity to more than two mould species. In the latter group, a steady increase of the skin test reactivity was recorded for all the other fungal

  7. Countercurrent Gaseous Diffusion Model of Oxidation Through a Porous Coating

    SciTech Connect

    Holcomb, G.R.

    1996-07-01

    A countercurrent gaseous diffusion model was developed to describe oxidation through porous coatings and scales. The specific system modeled involved graphite oxidized through a porous alumina (Al{sub 2}O{sub 3}) overcoat between 570 C (1,058 F) and 975 C (1,787 F). The model separated the porous Al{sub 2}O{sub 3} coating into two gas diffusion regions separated by a flame front, where oxygen (O{sub 2}) and carbon monoxide (CO) react to form carbon dioxide (CO{sub 2}). In the outer region O{sub 2} and CO{sub 2} counterdiffused. In the inner region, CO{sub 2} and CO counterdiffused. Concentration gradients of each gaseous specie in the pores of the Al{sub 2}O{sub 3} were determined, and the oxidation rate was calculated. The model was verified by oxidation experiments using graphite through various porous Al{sub 2}O{sub 3} overcoats. The Al{sub 2}O{sub 3} overcoats ranged in fractional porosity and in average pore radius from 0.077 {micro}m (3.0 x 10{sup -6} in., Knudsen diffusion) to 10.0 {micro}m (3.9 x 10{sup -4} in., molecular diffusion). Predicted and measured oxidation rates were shown to have the same dependence upon porosity, pore radius, temperature, and oxygen partial pressure (P{sub O{sub 2}}). Use of the model was proposed for other oxidation systems and for chemical vapor infiltration (CVI). This work was part of the U.S. Bureau of Mines corrosion research program.

  8. Pleistocene dynamics of the Pacific South Equatorial Countercurrent

    NASA Astrophysics Data System (ADS)

    Nuernberg, D.; Raddatz, J.; Rippert, N.; Tiedemann, R.

    2014-12-01

    The Western Pacific Warm Pool (WPWP) with extremely high sea-surface-temperatures (SST) is a key area for global climate. It also acts as a crossroad for mode and intermediate water masses such as the South Equatorial Countercurrent (SECC) transporting water masses originating from higher latitudes. The SECC flows above the main thermocline and strongly interacts with the Intertropical Convergence Zone (ITCZ) and South Pacific Convergence Zone (SPCZ). To constrain changes in sea-surface and subsurface water mass dynamics affecting thermocline depth, we reconstruct SST, subSST and salinity conditions using combined δ18O and Mg/Ca signals of surface (Globigerinoides ruber, Globigerinoides sacculifer) and subsurface dwelling (Globorotalia tumida) planktonic foraminifera. Our study is based on RV SONNE SO-225 piston cores retrieved from Manihiki plateau, which is located at the southeastern margin of the WPWP (between ~ 5°S-15°S and 170-160°W). The proxy records cover the last ~ 3 Myr SSTMg/Ca remained nearly constant throughout the entire Pleistocene varying between ~30 to 32 (°C), while the subSSTMg/Ca reconstructions reveal pronounced variations from ~10 to 16 (°C). Our results imply that the WPWP thermocline depth has undergone significant vertical movements throughout the Pleistocene. Notably, thermocline depth is continuously decreasing from the early to the late Pleistocene, and coincides with the change from the 41 kyr to a dominant 100 kyr climate periodicity between 1 and 1.7 Ma. We hypothesize that the repeated change in thermocline depth is due to either 1) changes in mode or intermediate water masses advection from Southern Ocean sources via "ocean tunneling", 2) changes in the tropical Pacific wind regime, and/or 3) changes in the Western Pacific Monsoon sytem.

  9. A novel multiple batch extraction test to assess contaminant mobilization from porous waste materials

    NASA Astrophysics Data System (ADS)

    Iden, S. C.; Durner, W.; Delay, M.; Frimmel, F. H.

    2009-04-01

    Contaminated porous materials, like soils, dredged sediments or waste materials must be tested before they can be used as filling materials in order to minimize the risk of groundwater pollution. We applied a multiple batch extraction test at varying liquid-to-solid (L/S) ratios to a demolition waste material and a municipal waste incineration product and investigated the release of chloride, sulphate, sodium, copper, chromium and dissolved organic carbon from both waste materials. The liquid phase test concentrations were used to estimate parameters of a relatively simple mass balance model accounting for equilibrium partitioning. The model parameters were estimated within a Bayesian framework by applying an efficient MCMC sampler and the uncertainties of the model parameters and model predictions were quantified. We tested isotherms of the linear, Freundlich and Langmuir type and selected the optimal isotherm model by use of the Deviance Information Criterion (DIC). Both the excellent fit to the experimental data and a comparison between the model-predicted and independently measured concentrations at the L/S ratios of 0.25 and 0.5 L/kg demonstrate the applicability of the model for almost all studied substances and both waste materials. We conclude that batch extraction tests at varying L/S ratios provide, at moderate experimental cost, a powerful complement to established test designs like column leaching or single batch extraction tests. The method constitutes an important tool in risk assessments, because concentrations at soil water contents representative for the field situation can be predicted from easier-to-obtain test concentrations at larger L/S ratios. This helps to circumvent the experimental difficulties of the soil saturation extract and eliminates the need to apply statistical approaches to predict such representative concentrations which have been shown to suffer dramatically from poor correlations.

  10. Preparative isolation and purification of rupestonic acid from the Chinese medicinal plant Artemisia rupestris L. by high-speed counter-current chromatography.

    PubMed

    Ma, Yanming; Aisha, Haji Akber; Liao, Lixin; Aibai, Sirafil; Zhang, Tianyou; Ito, Yoichiro

    2005-05-27

    Rupestonic acid was purified for the first time by high-speed counter-current chromatography from a dichloromethane extract of the traditional Chinese medicinal plant Artemisia rupestris L. The separation was performed in two steps with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (6:4:3.5:6.5, v/v) with 0.5% acetic acid in stationary-phase. From 200 mg of the crude extract, 27.9 mg of rupestonic acid was obtained at over 98% purity as determined by HPLC analysis, and its chemical structure was confirmed by MS, 1H and 13C nuclear magnetic resonance.

  11. Single-step purification of dracorhodin from dragon's blood resin of Daemonorops draco using high-speed counter-current chromatography combined with pH modulation.

    PubMed

    Shi, Jianmei; Hu, Ruilin; Lu, Yanbin; Sun, Cuirong; Wu, Tianxing

    2009-12-01

    Dracorhodin is a major constituent found in "Dragon's blood" resin of Daemonorops draco Willd. Blume. This natural flavylium compound is a potent pharmaceutical substance due to its biological and pharmacological activities such as antimicrobial, antiviral, antitumor and cytotoxic activity. An effective high-speed counter-current chromatography method was successfully established for the isolation and purification of dracorhodin directly from extract of D. draco by using a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water (2:3:2:3 v/v). Under the optimal conditions, 6.6 mg dracorhodin was obtained from 100 mg crude resin. The isolated fraction of counter-current chromatography was determined by HPLC, NMR, UV/visible and ESI/MS combined with pH modulation, since dracorhodin is unstable in solution which exists in different forms depending on pH values. The data were compared with those of the reference substance, and the literatures as well. The purity of dracorhodin was over 98% based on the HPLC result.

  12. Separation and purification of four flavonol diglucosides from the flower of Meconopsis integrifolia by high-speed counter-current chromatography.

    PubMed

    Huang, Yanfei; Han, Yatao; Chen, Keli; Huang, Bisheng; Liu, Yuan

    2015-12-01

    Flavonoids are the main components of Meconopsis integrifolia (Maxim.) Franch, which is a traditional Tibetan medicine. However, traditional chromatography separation requires a large quantity of raw M. integrifolia and is very time consuming. Herein, we applied high-speed counter-current chromatography in the separation and purification of flavonoids from the ethanol extracts of M. integrifolia flower. Ethyl acetate/n-butanol/water (2:3:5, v/v/v) was selected as the optimum solvent system to purify the four components, namely quercetin-3-O-β-d-glucopyrannosy-(1→6)-β-d-glucopyranoside (compound 1, 60 mg), quercetin 3-O-[2'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 2, 40 mg), quercetin 3-O-[3'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 3, 11 mg), and quercetin 3-O-[6'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 4, 16 mg). Among the four compounds, 3 and 4 were new acetylated flavonol diglucosides. After the high-speed counter-current chromatography separation, the purities of the four flavonol diglucosides were 98, 95, 90, and 92%, respectively. The structures of these compounds were identified by mass spectrometry and NMR spectroscopy. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Simultaneous separation of triterpenoid saponins and flavonoid glycosides from the roots of Glycyrrhiza uralensis Fisch by pH-zone-refining counter-current chromatography.

    PubMed

    Xu, Jinfang; Luo, Jianguang; Kong, Lingyi

    2013-10-01

    Glycosides including triterpenoid saponins and flavonoid glycosides are the main constituents of Glycyrrhiza uralensis Fisch (licorice) and exhibit prominent pharmacological activities. However, conventional methods for the separation of glycosides always cause irreversible adsorption and unavoidable loss of sample due to their high hydrophilicities. The present paper describes a convenient method for the simultaneous separation of triterpenoid saponins and flavonoid glycosides from licorice by pH-zone-refining counter-current chromatography. Ethyl acetate/n-butanol/water (2:3:5, v/v) with 10 mM TFA in the upper organic stationary phase and 10 mM ammonia in the lower aqueous mobile phase was used as the biphasic solvent system. Three triterpenoid saponins and two flavonoid glycosides including licorice-saponin A3 (63.3 mg), glycyrrhizic acid (342.2 mg), 3-O-[β-D-glucuronopyranosyl-(1 → 2)-β-D-galactopyranosyl]glycyrrhetic acid (56.0 mg), liquiritin apioside (232.6 mg), and liquiritin (386.5 mg) were successfully obtained from licorice ethanol extract (2 g) in one step. This method subtly takes advantage of the common acidic properties of triterpenoid saponins and flavonoid glycosides, and obviously is much more efficient and convenient than the previous methods. It is also the first time that the separation of acidic triterpenoid saponins by using pH-zone-refining counter-current chromatography has been reported.

  14. Application of step-wise gradient high-performance counter-current chromatography for rapid preparative separation and purification of diterpene components from Pseudolarix kaempferi Gordon.

    PubMed

    He, Shichao; Li, Shucai; Yang, Jianhong; Ye, Haoyu; Zhong, Shijie; Song, Hang; Zhang, Yongkui; Peng, Cheng; Peng, Aihua; Chen, Lijuan

    2012-04-27

    In general, simultaneously separation and purification of components with a broad polarity range from traditional Chinese medicine (TCM) is a challenge by an ordinary high-speed counter-current chromatography (HSCCC) method. In this paper, we describes a rapid and efficient separation method of combining three-step gradient elution and two-step flow-rate gradient elution using high-performance counter-current chromatography (HPCCC) to separate 8 diterpene compounds simultaneously within 80 min in a single run from the alcohol extract of Pseudolarix kaempferi Gordon. This separation process produced 166 mg pseudolaric acid B O-β-d-glucopyranoside (PABGly), 152 mg pseudolaric acid C (PAC), 8 mg deacetylpseudolaric acid A (deacetylPAA), 5 mg pseudolaric acid A O-β-d-glucopyranoside (PAAGly), 484 mg pseudolaric acid B (PAB), 33 mg pseudolaric acid B methyl ester (PAB methyl ester), 10mg pseudolaric acid A (PAA) and 18 mg pseudolaric acid H (PAH) from 1.0 g crude sample with purities of 98.6%, 99.6%, 92.3%, 92.2%, 99.2%, 99.4%, 98.3%, 91.0%, respectively. Our study indicates that the suitable combination of step-wise gradient elution and flow-rate gradient elution using HPCCC is an effective strategy to separate complex components from natural products. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Extraction and Separation Modeling of Orion Test Vehicles with ADAMS Simulation

    NASA Technical Reports Server (NTRS)

    Fraire, Usbaldo, Jr.; Anderson, Keith; Cuthbert, Peter A.

    2013-01-01

    The Capsule Parachute Assembly System (CPAS) project has increased efforts to demonstrate the performance of fully integrated parachute systems at both higher dynamic pressures and in the presence of wake fields using a Parachute Compartment Drop Test Vehicle (PCDTV) and a Parachute Test Vehicle (PTV), respectively. Modeling the extraction and separation events has proven challenging and an understanding of the physics is required to reduce the risk of separation malfunctions. The need for extraction and separation modeling is critical to a successful CPAS test campaign. Current PTV-alone simulations, such as Decelerator System Simulation (DSS), require accurate initial conditions (ICs) drawn from a separation model. Automatic Dynamic Analysis of Mechanical Systems (ADAMS), a Commercial off the Shelf (COTS) tool, was employed to provide insight into the multi-body six degree of freedom (DOF) interaction between parachute test hardware and external and internal forces. Components of the model include a composite extraction parachute, primary vehicle (PTV or PCDTV), platform cradle, a release mechanism, aircraft ramp, and a programmer parachute with attach points. Independent aerodynamic forces were applied to the mated test vehicle/platform cradle and the separated test vehicle and platform cradle. The aero coefficients were determined from real time lookup tables which were functions of both angle of attack ( ) and sideslip ( ). The atmospheric properties were also determined from a real time lookup table characteristic of the Yuma Proving Grounds (YPG) atmosphere relative to the planned test month. Representative geometries were constructed in ADAMS with measured mass properties generated for each independent vehicle. Derived smart separation parameters were included in ADAMS as sensors with defined pitch and pitch rate criteria used to refine inputs to analogous avionics systems for optimal separation conditions. Key design variables were dispersed in a Monte

  16. Pore Water Extraction Test Near 241-SX Tank Farm at the Hanford Site, Washington, USA

    SciTech Connect

    Eberlein, Susan J.; Parker, Danny L.; Tabor, Cynthia L.; Holm, Melissa J.

    2013-11-11

    A proof-of-principle test is underway near the Hanford Site 241-SX Tank Farm. The test will evaluate a potential remediation technology that will use tank farm-deployable equipment to remove contaminated pore water from vadose zone soils. The test system was designed and built to address the constraints of working within a tank farm. Due to radioactive soil contamination and limitations in drilling near tanks, small-diameter direct push drilling techniques applicable to tank farms are being utilized for well placement. To address space and weight limitations in working around tanks and obstacles within tank farms, the above ground portions of the test system have been constructed to allow deployment flexibility. The test system utilizes low vacuum over a sealed well screen to establish flow into an extraction well. Extracted pore water is collected in a well sump,and then pumped to the surface using a small-diameter bladder pump.If pore water extraction using this system can be successfully demonstrated, it may be possible to target local contamination in the vadose zone around underground storage tanks. It is anticipated that the results of this proof-of-principle test will support future decision making regarding interim and final actions for soil contamination within the tank farms.

  17. [Optimization of extraction technology for salidroside, tyrosol, crenulatin and gallic acid in Rhodiolae Crenulatae Radix et Rhizoma with orthogonal test].

    PubMed

    Luo, Xin; Wang, Xue-jing; Zhao, Yi-wu; Huang, Wen-zhe; Wang, Zhen-zhong; Xiao, Wei

    2015-09-01

    The extracting technology of salidroside, tyrosol, crenulatin and gallic acid from Rhodiolae Crenulatae Radix et Rhizoma was optimized. With extraction rate of salidroside, tyrosol, crenulatin and gallic acid as indexes, orthogonal test was used to evaluate effect of 4 factors on extracting technology, including concentration of solvent, the dosage of solvent, duration of extraction, and frequency of extraction. The results showed that, the best extracting technology was to extract in 70% alcohol with 8 times the weight of herbal medicine for 2 times, with 3 hours once. High extraction rate of salidroside, tyrosol, crenulatin and gallic acid were obtained with the present technology. The extracting technology was stable and feasible with high extraction rate of four compounds from Rhodiolae Crenulatae Radix et Rhizoma, it was suitable for industrial production.

  18. Toxicity of Glandularia selloi (Spreng.) Tronc. leave extract by MTT and neutral red assays: influence of the test medium procedure

    PubMed Central

    Figueiró, Luciana Rizzieri; Comerlato, Luana Christine; Da Silva, Marcia Vignoli; Zuanazzi, José Ângelo Silveira; Von Poser, Gilsane Lino

    2016-01-01

    Cytotoxicity assays using cell cultures may be an alternative to assess biological toxicity of plant extracts with potential phytotherapeutic properties. This study compared three methods to prepare culture media for the exposure of Vero cells to plant extracts. Leaves of Glandularia selloi (Spreng.) Tronc. were used to prepare culture medium with aqueous extract, extract in culture medium and methanol extract. Toxicity was assessed using the MTT and neutral red (NR) assays. In general, alterations in the cellular functions were found in all extracts and assays. Cytotoxic effect occurred at lower doses in aqueous extract and the range of effect of the methanol extract was small. The procedure of preparing the test medium has an effect on the outcome of the assay. Cytotoxicity of plant extract can be assessed by MTT and NR assays. Aqueous extract added to the culture medium presented the best profile to assess cytotoxicity. PMID:28652844

  19. Toxicity of Glandularia selloi (Spreng.) Tronc. leave extract by MTT and neutral red assays: influence of the test medium procedure.

    PubMed

    Figueiró, Luciana Rizzieri; Comerlato, Luana Christine; Da Silva, Marcia Vignoli; Zuanazzi, José Ângelo Silveira; Von Poser, Gilsane Lino; Ziulkoski, Ana Luiza

    2016-03-01

    Cytotoxicity assays using cell cultures may be an alternative to assess biological toxicity of plant extracts with potential phytotherapeutic properties. This study compared three methods to prepare culture media for the exposure of Vero cells to plant extracts. Leaves of Glandularia selloi (Spreng.) Tronc. were used to prepare culture medium with aqueous extract, extract in culture medium and methanol extract. Toxicity was assessed using the MTT and neutral red (NR) assays. In general, alterations in the cellular functions were found in all extracts and assays. Cytotoxic effect occurred at lower doses in aqueous extract and the range of effect of the methanol extract was small. The procedure of preparing the test medium has an effect on the outcome of the assay. Cytotoxicity of plant extract can be assessed by MTT and NR assays. Aqueous extract added to the culture medium presented the best profile to assess cytotoxicity.

  20. Integrating Multiple On-line Knowledge Bases for Disease-Lab Test Relation Extraction.

    PubMed

    Zhang, Yaoyun; Soysal, Ergin; Moon, Sungrim; Wang, Jingqi; Tao, Cui; Xu, Hua

    2015-01-01

    A computable knowledge base containing relations between diseases and lab tests would be a great resource for many biomedical informatics applications. This paper describes our initial step towards establishing a comprehensive knowledge base of disease and lab tests relations utilizing three public on-line resources. LabTestsOnline, MedlinePlus and Wikipedia are integrated to create a freely available, computable disease-lab test knowledgebase. Disease and lab test concepts are identified using MetaMap and relations between diseases and lab tests are determined based on source-specific rules. Experimental results demonstrate a high precision for relation extraction, with Wikipedia achieving the highest precision of 87%. Combining the three sources reached a recall of 51.40%, when compared with a subset of disease-lab test relations extracted from a reference book. Moreover, we found additional disease-lab test relations from on-line resources, indicating they are complementary to existing reference books for building a comprehensive disease and lab test relation knowledge base.

  1. Integrating Multiple On-line Knowledge Bases for Disease-Lab Test Relation Extraction

    PubMed Central

    Zhang, Yaoyun; Soysal, Ergin; Moon, Sungrim; Wang, Jingqi; Tao, Cui; Xu, Hua

    2015-01-01

    A computable knowledge base containing relations between diseases and lab tests would be a great resource for many biomedical informatics applications. This paper describes our initial step towards establishing a comprehensive knowledge base of disease and lab tests relations utilizing three public on-line resources. LabTestsOnline, MedlinePlus and Wikipedia are integrated to create a freely available, computable disease-lab test knowledgebase. Disease and lab test concepts are identified using MetaMap and relations between diseases and lab tests are determined based on source-specific rules. Experimental results demonstrate a high precision for relation extraction, with Wikipedia achieving the highest precision of 87%. Combining the three sources reached a recall of 51.40%, when compared with a subset of disease-lab test relations extracted from a reference book. Moreover, we found additional disease-lab test relations from on-line resources, indicating they are complementary to existing reference books for building a comprehensive disease and lab test relation knowledge base. PMID:26306271

  2. An open-source framework for stress-testing non-invasive foetal ECG extraction algorithms.

    PubMed

    Andreotti, Fernando; Behar, Joachim; Zaunseder, Sebastian; Oster, Julien; Clifford, Gari D

    2016-05-01

    Over the past decades, many studies have been published on the extraction of non-invasive foetal electrocardiogram (NI-FECG) from abdominal recordings. Most of these contributions claim to obtain excellent results in detecting foetal QRS (FQRS) complexes in terms of location. A small subset of authors have investigated the extraction of morphological features from the NI-FECG. However, due to the shortage of available public databases, the large variety of performance measures employed and the lack of open-source reference algorithms, most contributions cannot be meaningfully assessed. This article attempts to address these issues by presenting a standardised methodology for stress testing NI-FECG algorithms, including absolute data, as well as extraction and evaluation routines. To that end, a large database of realistic artificial signals was created, totaling 145.8 h of multichannel data and over one million FQRS complexes. An important characteristic of this dataset is the inclusion of several non-stationary events (e.g. foetal movements, uterine contractions and heart rate fluctuations) that are critical for evaluating extraction routines. To demonstrate our testing methodology, three classes of NI-FECG extraction algorithms were evaluated: blind source separation (BSS), template subtraction (TS) and adaptive methods (AM). Experiments were conducted to benchmark the performance of eight NI-FECG extraction algorithms on the artificial database focusing on: FQRS detection and morphological analysis (foetal QT and T/QRS ratio). The overall median FQRS detection accuracies (i.e. considering all non-stationary events) for the best performing methods in each group were 99.9% for BSS, 97.9% for AM and 96.0% for TS. Both FQRS detections and morphological parameters were shown to heavily depend on the extraction techniques and signal-to-noise ratio. Particularly, it is shown that their evaluation in the source domain, obtained after using a BSS technique, should be

  3. A Novel Mobile-Immobile Model for Push-Pull Test with Delayered Extraction

    NASA Astrophysics Data System (ADS)

    Chen, K.; Zhan, H.; Yang, Q.

    2015-12-01

    Push-Pull test is a mature tracer test that could be used to estimate aquifer transport properties at the scale of meters by injection and then extraction at the same well. However, current mathematical model for Push-Pull test cannot capture the characteristics of a heterogeneous aquifer and does not consider the stage of tracer incubation in aquifer. A novel mobile-immobile model is proposed to explain the effect of tracer incubation in a confined heterogeneous aquifer. This model takes into account three stages, including tracer injection, incubation and extraction. Advection and dispersion both exist in the mobile zone. For the immobile zone, only dispersion is taken into consideration to interpret the effect of heterogeneity that impedes solute transport. The experimental data of three wells at a potential CO2 sequestration site with slightly fractured and heterogeneous aquifer were given to calibrate the model parameters. It is found that the decreasing rate of concentration is controlled by mass transfer rate between the mobile and immobile zones. The initial concentration of extraction decreases with longer incubation time and increases with higher injection concentration. The concentration decreasing rates of those three wells are almost the same before extraction volume/injection volume of 6, which implies that dilution dominates in this period. After that, the decreasing rate deviates with each other. A possible reason is that degradation plays more important role with longer reaction time.

  4. Isolation and purification of prenylated phenolics from Amorpha fruticosa by high-speed counter-current chromatography.

    PubMed

    Chen, Chu; Wu, Yan; Chen, Yang; Du, Leilei

    2015-08-01

    Prenylated phenolics such as amorfrutins are recently identified potent anti-inflammatory and antidiabetic natural products. In this work, high-speed counter-current chromatography was investigated for the isolation and purification of prenylated phenolics from the fruits of Amorpha fruticosa by using a two-phase solvent system composed of n-hexane/ethanol/water (5:4:1, v/v). As a result, 14.2 mg of 5,7-dihydroxy-8-geranylflavanone, 10.7 mg of amorfrutin A and 17.4 mg of amorfrutin B were obtained from 200 mg of n-hexane-soluble crude extract in one step within 250 min. The purities of 5,7-dihydroxy-8-geranylflavanone, amorfrutins A and B were 95.2, 96.7 and 97.1%, respectively, as determined by ultra high performance liquid chromatography. The structural identification was performed by mass spectrometry and (1) H and (13) C NMR spectroscopy. The results indicated that the established method is an efficient and convenient way to purified prenylated phenolics from A. fruticosa extract.

  5. Comprehensive multi-channel multi-dimensional counter-current chromatography for separation of tanshinones from Salvia miltiorrhiza Bunge.

    PubMed

    Meng, Jie; Yang, Zhi; Liang, Junling; Zhou, Hui; Wu, Shihua

    2014-01-03

    Multi-dimensional chromatography offers the increased resolution and peak capacity by coupling of multiple columns with the same or different separation mechanisms. In this work, a novel multi-channel multi-dimensional counter-current chromatography (CCC) has been successfully constructed and used for several two-dimensional (2D) and three-dimensional (3D) CCC separations including 2D A×B/A×C, A×B-C and A-B×C, and 3D A×B×C systems. These 2D and 3D CCC systems were further applied to separate the bioactive tanshinones from the extract of Tanshen (or Danshen, Salvia miltiorrhiza Bunge), a famous Traditional Chinese Medicine (TCM). As a result, the developed 2D and 3D CCC methods were successful and efficient for resolving the tanshinones from complex extracts. Compared to the 1D multiple columns CCC separation, the 2D and 3D CCC decrease analysis time, reduce solvent consumption and increase sample throughput significantly. It may be widely used for current drug development, metabolomic analysis and natural product isolation.

  6. Equations for Calculating Recovery of Soluble Values in a Countercurrent Decantation Washing System

    NASA Astrophysics Data System (ADS)

    Scandrett, H. F.

    Mud washing variables are equated in a manner which simplifies the calculation of multistage countercurrent systems. Imperfect mixing is accommodated. In a simplified case, the number of stages becomes the exponent in the term which sets the ratio of concentration differences at the terminals.

  7. How-to-Do-It: Countercurrent Heat Exchange in Vertebrate Limbs.

    ERIC Educational Resources Information Center

    Franklin, George B.; Plakke, Ronald K.

    1988-01-01

    Describes principals of physics that are manifested in simple biological systems of heat conservation structures. Outlines materials needed, data collection, analysis, and discussion questions for construction and operation of two models, one that is a countercurrent heat exchange model and one that is not. (RT)

  8. Sarcoplasmic reticulum K(+) (TRIC) channel does not carry essential countercurrent during Ca(2+) release.

    PubMed

    Guo, Tao; Nani, Alma; Shonts, Stephen; Perryman, Matthew; Chen, Haiyan; Shannon, Thomas; Gillespie, Dirk; Fill, Michael

    2013-09-03

    The charge translocation associated with sarcoplasmic reticulum (SR) Ca(2+) efflux is compensated for by a simultaneous SR K(+) influx. This influx is essential because, with no countercurrent, the SR membrane potential (Vm) would quickly (<1 ms) reach the Ca(2+) equilibrium potential and SR Ca(2+) release would cease. The SR K(+) trimeric intracellular cation (TRIC) channel has been proposed to carry the essential countercurrent. However, the ryanodine receptor (RyR) itself also carries a substantial K(+) countercurrent during release. To better define the physiological role of the SR K(+) channel, we compared SR Ca(2+) transport in saponin-permeabilized cardiomyocytes before and after limiting SR K(+) channel function. Specifically, we reduced SR K(+) channel conduction 35 and 88% by replacing cytosolic K(+) for Na(+) or Cs(+) (respectively), changes that have little effect on RyR function. Calcium sparks, SR Ca(2+) reloading, and caffeine-evoked Ca(2+) release amplitude (and rate) were unaffected by these ionic changes. Our results show that countercurrent carried by SR K(+) (TRIC) channels is not required to support SR Ca(2+) release (or uptake). Because K(+) enters the SR through RyRs during release, the SR K(+) (TRIC) channel most likely is needed to restore trans-SR K(+) balance after RyRs close, assuring SR Vm stays near 0 mV. Copyright © 2013 Biophysical Society. Published by Elsevier Inc. All rights reserved.

  9. Sarcoplasmic Reticulum K+ (TRIC) Channel Does Not Carry Essential Countercurrent during Ca2+ Release

    PubMed Central

    Guo, Tao; Nani, Alma; Shonts, Stephen; Perryman, Matthew; Chen, Haiyan; Shannon, Thomas; Gillespie, Dirk; Fill, Michael

    2013-01-01

    The charge translocation associated with sarcoplasmic reticulum (SR) Ca2+ efflux is compensated for by a simultaneous SR K+ influx. This influx is essential because, with no countercurrent, the SR membrane potential (Vm) would quickly (<1 ms) reach the Ca2+ equilibrium potential and SR Ca2+ release would cease. The SR K+ trimeric intracellular cation (TRIC) channel has been proposed to carry the essential countercurrent. However, the ryanodine receptor (RyR) itself also carries a substantial K+ countercurrent during release. To better define the physiological role of the SR K+ channel, we compared SR Ca2+ transport in saponin-permeabilized cardiomyocytes before and after limiting SR K+ channel function. Specifically, we reduced SR K+ channel conduction 35 and 88% by replacing cytosolic K+ for Na+ or Cs+ (respectively), changes that have little effect on RyR function. Calcium sparks, SR Ca2+ reloading, and caffeine-evoked Ca2+ release amplitude (and rate) were unaffected by these ionic changes. Our results show that countercurrent carried by SR K+ (TRIC) channels is not required to support SR Ca2+ release (or uptake). Because K+ enters the SR through RyRs during release, the SR K+ (TRIC) channel most likely is needed to restore trans-SR K+ balance after RyRs close, assuring SR Vm stays near 0 mV. PMID:24010658

  10. Counter-current carbon dioxide purification of partially deacylated sunflower oil

    USDA-ARS?s Scientific Manuscript database

    High oleic sunflower oil was partially deacylated by propanolysis to produce a mixture of diglycerides and triglycerides. To remove by-product fatty acid propyl esters (FAPEs) from this reaction mixture, a liquid carbon dioxide (L-CO2) counter-current fractionation method was developed. The fracti...

  11. Lack of toxicological effect through mutagenicity test of polyphenol extracts from peanut shells.

    PubMed

    Gao, Feng; Ye, Haiqing; Yu, Yali; Zhang, Tiehua; Deng, Xuming

    2011-12-01

    The toxicological effect of polyphenols extracted from peanut shells was investigated in animal models. The safety data were needed to proceed with further clinical trials. The oral LD50 of peanut shells polyphenols was determined to be higher than 15,000mg/kg body weight. We also carried out a sperm abnormality test, a chromosomal aberration test and a micronucleus test in rats. The peanut shell polyphenols did not cause any abnormalities in the system. Furthermore, the administration of peanut shell polyphenols did not significantly alter changes in body weight or clinical signs. These results strongly indicated that peanut shell polyphenols did not induce mutagenicity. The results of this study suggested a lack of toxicological effect and supported the further use of polyphenol-rich extracts from peanut shells as a potential natural antioxidant. Copyright © 2011 Elsevier Ltd. All rights reserved.

  12. CONSTRUCTION AND POWER TEST OF THE EXTRACTION KICKER MAGNET FOR SNS ACCUMULATOR RING.

    SciTech Connect

    PAI, C.; HAHN, H.; HSEUH, H.; LEE, Y.; MENG, W.; MI,J.; SANDBERG, J.; TODD, R.; ET AL.

    2005-05-16

    Two extraction kicker magnet assemblies that contain seven individual pulsed magnet modules each will kick the proton beam vertically out of the SNS accumulator ring into the aperture of the extraction Lambertson septum magnet. The proton beam then travels to the 1.4 MW SNS target assembly. The 14 kicker magnets and major components of the kicker assembly have been fabricated in BNL. The inner surfaces of the kicker magnets were coated with TiN to reduce the secondary electron yield. All 14 PFN power supplies have been built, tested and delivered to OWL. Before final installation, a partial assembly of the kicker system with three kicker magnets was assembled to test the functions of each critical component in the system. In this paper we report the progress of the construction of the kicker components, the TIN coating of the magnets, the installation procedure of the magnets and the full power test of the kicker with the PFN power supply.

  13. Lunasin and Bowman-Birk protease inhibitor concentrations of protein extracts from enzyme-assisted aqueous extraction of soybeans.

    PubMed

    Leite Nobrega de Moura, Juliana Maria; Hernandez-Ledesma, Blanca; de Almeida, Neiva Maria; Hsieh, Chia-Chien; de Lumen, Ben O; Johnson, Lawrence A

    2011-07-13

    Lunasin and Bowman-Birk protease inhibitor (BBI) are two soybean peptides to which health-promoting properties have been attributed. Concentrations of these peptides were determined in skim fractions produced by enzyme-assisted aqueous extraction processing (EAEP) of extruded full-fat soybean flakes (an alternative to extracting oil from soybeans with hexane) and compared with similar extracts from hexane-defatted soybean meal. Oil and protein were extracted by using countercurrent two-stage EAEP of soybeans at 1:6 solids-to-liquid ratio, 50 °C, pH 9.0, and 120 rpm for 1 h. Protein-rich skim fractions were produced from extruded full-fat soybean flakes using different enzyme strategies in EAEP: 0.5% protease (wt/g extruded flakes) used in both extraction stages; 0.5% protease used only in the second extraction stage; no enzyme used in either extraction stage. Countercurrent two-stage protein extraction of air-desolventized, hexane-defatted soybean flakes was used as a control. Protein extraction yields increased from 66% to 89-96% when using countercurrent two-stage EAEP with extruded full-fat flakes compared to 85% when using countercurrent two-stage protein extraction of air-desolventized, hexane-defatted soybean flakes. Extruding full-fat soybean flakes reduced BBI activity. Enzymatic hydrolysis reduced BBI contents of EAEP skims. Lunasin, however, was more resistant to both enzymatic hydrolysis and heat denaturation. Although using enzymes in both EAEP extraction stages yielded the highest protein and oil extractions, reducing enzyme use to only the second stage preserved much of the BBI and Lunasin.

  14. Co-current and counter-current imbibition in independent tubes of non-axisymmetric geometry.

    PubMed

    Unsal, E; Mason, G; Morrow, N R; Ruth, D W

    2007-02-01

    Experiments that illustrate and quantify the basics of co- and counter-current spontaneous imbibition have been conducted in a series of simple model pore systems. The fundamental pore geometry is a rod in an angled round-bottomed slot with the rod touching a capping glass plate. The capillaries thus formed by the surfaces of the slot, rod and plate do not have circular cross-sections but more complicated geometric structures with angular corners. The tubes formed at each side of the rod connect at both ends. A viscous, refined oil was applied from one end. For co-current experiments, the opposite end was left open to the atmosphere and oil imbibed into both tubes. For counter-current experiments the opposite end was sealed and connected to a sensitive pressure transducer. Oil imbibed into the smaller capillary and expelled air as a series of bubbles from the end of the larger capillary. Bubble snap-off was observed to be rate-dependent and occurred at a lower curvature than that of the cylindrical meniscus that just fits inside the tube. Only the corners of the larger capillary filled with oil during counter-current imbibition. Meniscus curvatures were calculated using the Mayer and Stowe-Princen method and were compared with actual values by measuring the capillary rise in the tubes; agreement was close. A simple model for co-current and counter-current imbibition has also been developed and the predictions compared with the experimental results. The model results were in agreement with the experiments. The experiments demonstrate that the capillary back pressure generated by the interfaces and bubbles in counter-current imbibition can slow the process significantly.

  15. Rigging Test Bed Enables Development of Multi-Stage Decelerator Extraction

    NASA Technical Reports Server (NTRS)

    Kenig, Sivan J.; Brandeau, Erich J.; Gallon, John C.

    2015-01-01

    The Low Density Supersonic Decelerator (LDSD) project developed a Parachute Deployment System (PDS) for use on its Supersonic Flight Dynamics Tests (SFDT). The PDS involves a multi-stage pilot driven extraction of a supersonic parachute. The uncertainties and complexities of developing the design for the lines and rigging of the PDS were addressed through testing in the Rigging Test Bed (RTB). The RTB provided a facility capable of simulating a variety of extraction scenarios with full scale hardware on the ground. Through more than 100 tests conducted in the facility, a wealth of data and experience were gained that fueled the PDS development. The utility of this testing and the lessons learned are presented in this paper. The goal is to inform the development of similar systems in the future and highlight the value and flexibility this type of testing offers rapid hardware development. The RTB provided a great compliment to the analytical models greatly compressing what would have otherwise been a very lengthy analytical effort or potentially much expanded flight test campaign.

  16. Analysis of energy extraction in the 1995 Hijiori 25-day circulation test

    SciTech Connect

    Kruger, P.; Sato, Yoshitero; Shinohara, Nobuo

    1996-12-31

    A 25-day circulation test was carried out in the summer of 1995 to characterize the two-production wells in the deeper reservoir of the Hijiori HDR resource. The test protocol included two stimulations of the injection well and two short step-rate injection tests during the circulation period. The test data showed that the flow in the two production wells originated from both the deeper reservoir at 2200 m and the original upper reservoir at 1800 m. For analysis of thermal extraction, the test data for the two production wells were treated as independent zonal sectors, as described by Kruger and Yamaguchi for the Hijiori 90-day circulation test of the upper reservoir and Kruger and Yamamoto for the Ogachi 151-day circulation test. Temperature cross-sections were calculated across each zonal sector. The two methods provide an estimation of the thermal energy extracted from the two reservoir zonal sectors during the circulation period and an estimate of the reservoir lifetime to the selected abandonment temperature.

  17. Intra-Die Spatial Correlation Extraction with Maximum Likelihood Estimation Method for Multiple Test Chips

    NASA Astrophysics Data System (ADS)

    Fu, Qiang; Luk, Wai-Shing; Tao, Jun; Zeng, Xuan; Cai, Wei

    In this paper, a novel intra-die spatial correlation extraction method referred to as MLEMTC (Maximum Likelihood Estimation for Multiple Test Chips) is presented. In the MLEMTC method, a joint likelihood function is formulated by multiplying the set of individual likelihood functions for all test chips. This joint likelihood function is then maximized to extract a unique group of parameter values of a single spatial correlation function, which can be used for statistical circuit analysis and design. Moreover, to deal with the purely random component and measurement error contained in measurement data, the spatial correlation function combined with the correlation of white noise is used in the extraction, which significantly improves the accuracy of the extraction results. Furthermore, an LU decomposition based technique is developed to calculate the log-determinant of the positive definite matrix within the likelihood function, which solves the numerical stability problem encountered in the direct calculation. Experimental results have shown that the proposed method is efficient and practical.

  18. Using the liquid nature of the stationary phase in countercurrent chromatography. IV. The cocurrent CCC method.

    PubMed

    Berthod, Alain; Hassoun, Mahmoud

    2006-05-26

    The retention volumes of solutes in countercurrent chromatography (CCC) are directly proportional to their distribution coefficients, K(D) in the biphasic liquid system used as mobile and stationary phase in the CCC column. The cocurrent CCC method consists in putting the liquid "stationary" phase in slow motion in the same direction as the mobile phase. A mixture of five steroid compounds of widely differing polarities was used as a test mixture to evaluate the capabilities of the method with the biphasic liquid system made of water/methanol/ethyl acetate/heptane 6/5/6/5 (v/v) and a 53 mL CCC column of the coil planet centrifuge type. It is shown that the chromatographic resolution obtained in cocurrent CCC is very good because the solute band broadening is minimized as long as the solute is located inside the "stationary" phase. Pushing the method at its limits, it is demonstrated that the five steroids can still be (partly) separated when the flow rate of the two liquid phases is the same (2 mL/min). This is due to the higher volume of upper phase (72% of the column volume) contained inside the CCC column producing a lower linear speed compared to the aqueous lower phase linear speed. The capabilities of the cocurrent CCC method compare well with those of the gradient elution method in HPLC. Continuous detection is a problem due to the fact that two immiscible liquid phases elute from the column. It was partly solved using an evaporative light scattering detector.

  19. Novel design for centrifugal counter-current chromatography: VI. Ellipsoid column.

    PubMed

    Gu, Dongyu; Yang, Yi; Xin, Xuelei; Aisa, Haji Akber; Ito, Yoichiro

    2015-01-01

    A novel ellipsoid column was designed for centrifugal counter-current chromatography. Performance of the ellipsoid column with a capacity of 3.4 mL was examined with three different solvent systems composed of 1-butanol-acetic acid-water (4:1:5, v/v) (BAW), hexane-ethyl acetate-methanol-0.1 M HCl (1:1:1:1, v/v) (HEMH), and 12.5% (w/w) PEG1000 and 12.5% (w/w) dibasic potassium phosphate in water (PEG-DPP) each with suitable test samples. In dipeptide separation with BAW system, both stationary phase retention (Sf) and peak resolution (Rs) of the ellipsoid column were much higher at 0° column angle (column axis parallel to the centrifugal force) than at 90° column angle (column axis perpendicular to the centrifugal force), where elution with the lower phase at a low flow rate produced the best separation yielding Rs at 2.02 with 27.8% Sf at a flow rate of 0.07 ml/min. In the DNP-amino acid separation with HEMW system, the best results were obtained at a flow rate of 0.05 ml/min with 31.6% Sf yielding high Rs values at 2.16 between DNP-DL-glu and DNP-β-ala peaks and 1.81 between DNP-β-ala and DNP-L-ala peaks. In protein separation with PEG-DPP system, lysozyme and myolobin were resolved at Rs of 1.08 at a flow rate of 0.03 ml/min with 38.9% Sf. Most of those Rs values exceed those obtained from the figure-8 column under similar experimental conditions previously reported.

  20. Modeling gradient elution in countercurrent chromatography: efficient separation of tanshinones from Salvia miltiorrhiza Bunge.

    PubMed

    Wu, Shihua; Wu, Dingfang; Liang, Junling; Berthod, Alain

    2012-04-01

    Countercurrent chromatography (CCC) is a support-free liquid-liquid chromatography using centrifugal fields to hold the liquid stationary phase. CCC has been widely applied in the separation of various natural and synthetic components using a variety of biphasic liquid systems. The related hexane or heptane/ethyl acetate/methanol or ethanol/water biphasic liquid systems demonstrated their significance in CCC. Gradient is difficult in CCC since any composition change in one phase induces a composition change of the other phase to maintain phase equilibrium. This work provides a new insight into linear gradient elution in CCC that is feasible with some biphasic liquid systems such as selected compositions of the hexane/ethyl acetate/ethanol/water systems. The equations modeling solute motion inside the CCC column are proposed. Particular compositions of the liquid system, namely the hexane/ethyl acetate/ethanol/water 8:2:E:W compositions with E + W = 10, were studied from W = 1 to 9. They showed moderate changes in the upper organic phase compositions. The model is tested with the separation of tanshinones from the rhizome of Salvia miltiorrhiza Bunge. Different linear solvent gradient profiles were experimentally performed between 8:2:5:5 and 8:2:3:7 compositions and the results were evaluated using the proposed model. Five tanshinones including dihydrotanshinone I, cryptotanshinone, tanshinone I, 1,2-dihydrotanshinquinone, and tanshinone IIA have been successfully separated (>95% purities) using a gradient profile optimized by the developed model. The gradient model can be used only with biphasic liquid systems in which one phase shows minimum composition changes when the other phase composition changes notably. This case is not the general case for biphasic liquid systems but can be applied with specific compositions of the quaternary hexane or heptane/ethyl acetate/methanol or ethanol/water most useful CCC liquid systems. © 2012 Wiley-VCH Verlag GmbH & Co. KGa

  1. Novel design for centrifugal counter-current chromatography: VI. Ellipsoid column

    PubMed Central

    Gu, Dongyu; Yang, Yi; Xin, Xuelei; Aisa, Haji Akber; Ito, Yoichiro

    2014-01-01

    A novel ellipsoid column was designed for centrifugal counter-current chromatography. Performance of the ellipsoid column with a capacity of 3.4 mL was examined with three different solvent systems composed of 1-butanol-acetic acid-water (4:1:5, v/v) (BAW), hexane-ethyl acetate-methanol-0.1 M HCl (1:1:1:1, v/v) (HEMH), and 12.5% (w/w) PEG1000 and 12.5% (w/w) dibasic potassium phosphate in water (PEG-DPP) each with suitable test samples. In dipeptide separation with BAW system, both stationary phase retention (Sf) and peak resolution (Rs) of the ellipsoid column were much higher at 0° column angle (column axis parallel to the centrifugal force) than at 90° column angle (column axis perpendicular to the centrifugal force), where elution with the lower phase at a low flow rate produced the best separation yielding Rs at 2.02 with 27.8% Sf at a flow rate of 0.07 ml/min. In the DNP-amino acid separation with HEMW system, the best results were obtained at a flow rate of 0.05 ml/min with 31.6% Sf yielding high Rs values at 2.16 between DNP-DL-glu and DNP-β-ala peaks and 1.81 between DNP-β-ala and DNP-L-ala peaks. In protein separation with PEG-DPP system, lysozyme and myolobin were resolved at Rs of 1.08 at a flow rate of 0.03 ml/min with 38.9% Sf. Most of those Rs values exceed those obtained from the figure-8 column under similar experimental conditions previously reported. PMID:25309116

  2. [Isolation and purification of solanesol from potato leaves by high-speed counter-current chromatography and identification by atmospheric pressure chemical ionization mass spectrometry].

    PubMed

    Hu, Jiangyong; Liang, Yong; Xie, Ya; Huang, Zhaofeng; Zhong, Hanzuo

    2007-07-01

    Preparative high-speed counter-current chromatography (HSCCC) was used for the isolation and purification of solanesol from potato leaves. Experimental conditions of the extraction of solanesol from potato leaves have been optimized. An ultrafine extraction method was applied in this study. The efficiency using an ultrafine extraction was found to be improved in the investigation, the yields of solanesol by different extraction methods were 0.083% by ultrafine extraction and 0.050% by ultrasonic extraction. Using n-hexane-methanol (10:7, v/v) as the two-phase solvent system, preparative HSCCC was successfully performed with the yield of 5 mg solanesol at 98.7% of purity from 60 mg of crude extract in the one-step separation. The mobile phase was the lower phase and operated at a flow rate of 1.5 mL/min, while the apparatus rotated at 800 r/min. The solanesol was identified by the atmospheric pressure chemical ionization mass spectrometry (APCI-MS). The ionization and cleavage mechanisms of solanesol in APCI-MS and APCI-MS/MS are discussed.

  3. Optimization of the fractional precipitation of paclitaxel from a Taxus chinensis cell culture using response surface methodology and its isolation by consecutive high-speed countercurrent chromatography.

    PubMed

    Liang, Zhikun; Xie, Zhisheng; Lam, Shingchung; Xu, Xinjun

    2014-09-01

    A consecutive preparation method for the isolation and purification of paclitaxel from the Taxus Chinensis cell culture was developed in this study. The process involved alkaline Al2O3 chromatography, fractional precipitation, and high-speed countercurrent chromatography. The original cell culture materials were first extracted with methanol using ultrasound-assisted extraction, and then the extract (the content of paclitaxel is 1.5%) was separated by alkaline Al2O3 column chromatography. Subsequently, fractional precipitation was used to obtain paclitaxel. In particular, response surface methodology was used to optimize the factors of fractional precipitation (methanol concentration, material-to-solvent ratio, and precipitating time were optimized as 48.14%, 8.85 mg/mL, and 48.71 h, respectively) and the yield of fractional precipitation product was 30.64 ± 0.60 mg (the content of paclitaxel is 89.3%, 27.37 ± 0.54 mg) from a 100 mg fraction by Al2O3 column separation (the content of paclitaxel is 32.4%). Then, the product was used for further isolation by high-speed countercurrent chromatography. About 1.00 g paclitaxel (200 ± 2 mg in each loading) with a purity up to 99.61% was isolated from 1.25 g of fractional precipitation product with a solvent system of n-hexane/ethyl acetate/methanol/water (1.2:1.8:1.5:1.5, v/v/v/v) in one run of five consecutive sample loadings without exchanging a new solvent system.

  4. Evaluation of cytogenotoxic effects of cold aqueous extract from Achyrocline satureioides by Allium cepa L test.

    PubMed

    Sabini, María C; Cariddi, Laura N; Escobara, Franco M; Bachetti, Romina A; Sutil, Sonia B; Contigiani, Marta S; Zanon, Silvia M; Sabini, Liliana I

    2011-07-01

    Achyrocline satureioides ("marcela del campo") is native to America. Numerous investigations have reported several bioactive properties such as anti-inflammatory, hepatoprotective, immunomodulatory, antimicrobial and antiviral. Nowadays, few medicinal plants have been scientifically evaluated to test its safety, efficacy and potential benefits, despite the great public interest in these herbs. The aim of this work was to evaluate the cytotoxic and genotoxic activities of cold aqueous extract obtained from A. satureioides using Allium cepa L test. The results demonstrated the absence of genotoxicity of the extract. Only higher concentrations induced cytotoxicity but interestingly this effect was reversible and was not associated with mutagenicity. The contribution of this research provides assurance of safety in the application of Achyrocline satureioides in treatment of microbial diseases and other pathologies helping to define selective toxicity.

  5. A technique for extracting blood samples from mice in fire toxicity tests

    NASA Technical Reports Server (NTRS)

    Bucci, T. J.; Hilado, C. J.; Lopez, M. T.

    1976-01-01

    The extraction of adequate blood samples from moribund and dead mice has been a problem because of the small quantity of blood in each animal and the short time available between the animals' death and coagulation of the blood. These difficulties are particularly critical in fire toxicity tests because removal of the test animals while observing proper safety precautions for personnel is time-consuming. Techniques for extracting blood samples from mice were evaluated, and a technique was developed to obtain up to 0.8 ml of blood from a single mouse after death. The technique involves rapid exposure and cutting of the posterior vena cava and accumulation of blood in the peritoneal space. Blood samples of 0.5 ml or more from individual mice have been consistently obtained as much as 16 minutes after apparent death. Results of carboxyhemoglobin analyses of blood appeared reproducible and consistent with carbon monoxide concentrations in the exposure chamber.

  6. Comparison of bioassays by testing whole soil and their water extract from contaminated sites.

    PubMed

    Leitgib, Laura; Kálmán, Judit; Gruiz, Katalin

    2007-01-01

    The harmful effects of contaminants on the ecosystems and humans are characterised by their environmental toxicity. The aim of this study was to assess applicability and reliability of several environmental toxicity tests, comparing the result of the whole soils and their water extracts. In the study real contaminated soils were applied from three different inherited contaminated sites of organic and inorganic pollutants. The measured endpoints were the bioluminescence inhibition of Vibrio fischeri (bacterium), the dehydrogenase activity inhibition of Azomonas agilis (bacterium), the reproduction inhibition of Tetrahymena pyriformis (protozoon), and Panagrellus redivivus (nematode), the mortality of Folsomia candida (springtail), the root and shoot elongation inhibition of Sinapis alba (plant: white mustard) and the nitrification activity inhibition of an uncontaminated garden soil used as "test organism". Besides the standardised or widely used methods some new, direct contact ecotoxicity tests have been developed and introduced, which are useful for characterisation of the risk of contaminated soils due to their interactive nature. Soil no. 1 derived from a site polluted with transformer oil (PCB-free); Soil no. 2 originated from a site contaminated with mazout; Soil no. 3 was contaminated with toxic metals (Zn, Cd, Cu, Pb, As). In most cases, the interactive ecotoxicity tests indicated more harmful effect of the contaminated soil than the tests using soil extracts. The direct contact environmental toxicity tests are able to meet the requirements of environmental toxicology: reliability, sensibility, reproducibility, rapidity and low cost.

  7. Valx: A system for extracting and structuring numeric lab test comparison statements from text

    PubMed Central

    Hao, Tianyong; Liu, Hongfang; Weng, Chunhua

    2017-01-01

    Objectives To develop an automated method for extracting and structuring numeric lab test comparison statements from text and evaluate the method using clinical trial eligibility criteria text. Methods Leveraging semantic knowledge from the Unified Medical Language System (UMLS) and domain knowledge acquired from the Internet, Valx takes 7 steps to extract and normalize numeric lab test expressions: 1) text preprocessing, 2) numeric, unit, and comparison operator extraction, 3) variable identification using hybrid knowledge, 4) variable - numeric association, 5) context-based association filtering, 6) measurement unit normalization, and 7) heuristic rule-based comparison statements verification. Our reference standard was the consensus-based annotation among three raters for all comparison statements for two variables, i.e., HbA1c and glucose, identified from all of Type 1 and Type 2 diabetes trials in ClinicalTrials.gov. Results The precision, recall, and F-measure for structuring HbA1c comparison statements were 99.6%, 98.1%, 98.8% for Type 1 diabetes trials, and 98.8%, 96.9%, 97.8% for Type 2 Diabetes trials, respectively. The precision, recall, and F-measure for structuring glucose comparison statements were 97.3%, 94.8%, 96.1% for Type 1 diabetes trials, and 92.3%, 92.3%, 92.3% for Type 2 diabetes trials, respectively. Conclusions Valx is effective at extracting and structuring free-text lab test comparison statements in clinical trial summaries. Future studies are warranted to test its generalizability beyond eligibility criteria text. The open-source Valx enables its further evaluation and continued improvement among the collaborative scientific community. PMID:26940748

  8. Separation of betalains from berries of Phytolacca americana by ion-pair high-speed counter-current chromatography.

    PubMed

    Jerz, Gerold; Skotzki, Tanja; Fiege, Kathrin; Winterhalter, Peter; Wybraniec, Sławomir

    2008-05-09

    The first preparative fractionation of betalain pigments by means of ion-pair high-speed counter-current chromatography (IP-HSCCC) from berry extracts of Phytolacca americana (Phytolaccaceae) is presented. A novel HSCCC solvent system consisting of 1-butanol-acetonitrile-water (5:1:6, v/v/v) was applied using ion-pair forming trifluoroacetic acid at low concentration (0.7%, v/v). Affinity of polar betacyanins and betaxanthins to the organic stationary phase of the biphasic HSCCC solvent mixture was considerably improved. Partitioning coefficient values and influence of increasing trifluoroacetic acid additions to the biphasic solvent mixture were measured for all identified betacyanins and betaxanthins. Gentle separation by IP-HSCCC of the injected pigment extract (900 mg) yielded sufficient amounts of the principal pigments 15S-betanin/15R-isobetanin. The pure epimers separated by C18-HPLC were immediately studied by one- and two-dimensional NMR. In the recovered fractions, minor concentrated betacyanins and betaxanthins were significantly enriched by IP-HSCCC and were detected for the first time in the extracts of P. americana. IP-HSCCC and C18-HPLC were shown to be complementary techniques in the isolation procedure of recovering minor concentrated, highly polar and chemically instable betacyanins and betaxanthin from complex plant matrices. Altogether, identification of 17 betalains was achieved by HPLC-diode array detection-electrospray ionization MS/MS in the HSCCC fractions with their respective isomers, also resulting in the tentative elucidation of betacyanins with novel salicylic acid substitution pattern in the berry extracts of P. americana.

  9. The Generally Useful Estimate of Solvent Systems (GUESS) method enables the rapid purification of methylpyridoxine regioisomers by countercurrent chromatography

    PubMed Central

    Liu, Yang; Friesen, J. Brent; Klein, Larry L.; McAlpine, James B.; Lankin, David C.; Pauli, Guido F.; Chen, Shao-Nong

    2016-01-01

    The TLC-based Generally Useful Estimate of Solvent Systems (GUESS) method was employed for countercurrent chromatography solvent system selection, in order to separate the three synthetic isomers: 3-O-methylpyridoxine, 4′-O-methylpyridoxine (ginkgotoxin) and 5′-O-methylpyridoxine. The Rf values of the three isomers indicated that ChMWat +2 (chloroformmethanol-water 10:5:5, v/v/v) was appropriate for the countercurrent chromatography. The isomer separation was highly selective and demonstrated that the TLC-based GUESS method can accelerate solvent system selection for countercurrent chromatography. Accordingly, the study re-emphasizes the practicality of TLC as a tool to facilitate the rapid development of new countercurrent and centrifugal partition chromatography methods for this solvent system. Purity and structure characterization of all samples was performed by quantitative 1H NMR. PMID:26680272

  10. The Generally Useful Estimate of Solvent Systems (GUESS) method enables the rapid purification of methylpyridoxine regioisomers by countercurrent chromatography.

    PubMed

    Liu, Yang; Friesen, J Brent; Klein, Larry L; McAlpine, James B; Lankin, David C; Pauli, Guido F; Chen, Shao-Nong

    2015-12-24

    The TLC-based Generally Useful Estimate of Solvent Systems (GUESS) method was employed for countercurrent chromatography solvent system selection, in order to separate the three synthetic isomers: 3-O-methylpyridoxine, 4'-O-methylpyridoxine (ginkgotoxin), and 5'-O-methylpyridoxine. The Rf values of the three isomers indicated that ChMWat+2 (chloroform-methanol-water 10:5:5, v/v/v) was appropriate for the countercurrent separation. The isomer separation was highly selective and demonstrated that the TLC-based GUESS method can accelerate solvent system selection for countercurrent separation. Accordingly, the study re-emphasizes the practicality of TLC as a tool to facilitate the rapid development of new countercurrent and centrifugal partition chromatography methods for this solvent system. Purity and structure characterization of all samples was performed by quantitative (1)H NMR.

  11. Identifying Natural syNergist from Pongamia pinnata Using High-Speed Counter-Current Chromatography Combined with Isobolographic Analysis.

    PubMed

    Yin, Hao; Wei, Yubai; Chen, Rouwen; Zhang, Si; Long, Lijuan; Yin, Hang; Tian, Xinpeng; He, Weihong

    2017-03-03

    For identifying the synergistic compounds from Pongamia pinnata, an approach based on high-speed counter-current chromatography (HSCCC) combined with isobolographic analysis was designed to detect the synergistic effects in the complex mixture [...].

  12. FIELD IMPLEMENTATION PLAN FOR A WILLISTON BASIN BRINE EXTRACTION AND STORAGE TEST

    SciTech Connect

    Hamling, John; Klapperich, Ryan; Stepan, Daniel; Sorensen, James; Pekot, Lawrence; Peck, Wesley; Jacobson, Lonny; Bosshart, Nicholas; Hurley, John; Wilson, William; Kurz, Marc; Burnison, Shaughn; Salako, Olarinre; Musich, Mark; Botnen, Barry; Kalenze, Nicholas; Ayash, Scott; Ge, Jun; Jiang, Tao; Dalkhaa, Chantsalmaa; Oster, Benjamin; Peterson, Kyle; Feole, Ian; Gorecki, Charles; Steadman, Edward

    2016-03-31

    The Energy & Environmental Research Center (EERC) successfully completed all technical work of Phase I, including development of a field implementation plan (FIP) for a brine extraction and storage test (BEST) in the North Dakota portion of the Williston Basin. This implementation plan was commissioned by the U.S. Department of Energy (DOE) National Energy Technology Laboratory (NETL) as a proxy for managing formation pressure plumes and measuring/monitoring the movement of differential pressure and CO2 plumes in the subsurface for future saline CO2 storage projects. BEST comprises the demonstration and validation of active reservoir management (ARM) strategies and extracted brine treatment technologies. Two prospective commercial brine injection sites were evaluated for BEST to satisfy DOE’s goals. Ultimately, an active saltwater disposal (SWD) site, Johnsons Corner, was selected because it possesses an ideal combination of key factors making it uniquely suited to host BEST. This site is located in western North Dakota and operated by Nuverra Environmental Solutions (Nuverra), a national leader in brine handling, treatment, and injection. An integrated management approach was used to incorporate local and regional geologic characterization activities with geologic and simulation models, inform a monitoring, verification, and accounting (MVA) plan, and to conduct a risk assessment. This approach was used to design a FIP for an ARM schema and an extracted brine treatment technology test bed facility. The FIP leverages an existing pressure plume generated by two commercial SWD wells. These wells, in conjunction with a new brine extraction well, will be used to conduct the ARM schema. Results of these tests will be quantified based on their impact on the performance of the existing SWD wells and the surrounding reservoir system. Extracted brine will be injected into an underlying deep saline formation through a new injection well. The locations of proposed

  13. A PCM/forced convection conjugate transient analysis of energy storage systems with annular and countercurrent flows

    NASA Technical Reports Server (NTRS)

    Cao, Y.; Faghri, A.; Juhasz, A.

    1991-01-01

    Latent heat energy storage systems with both annular and countercurrent flows are modeled numerically. The change of phase of the phase-change material (PCM) and the transient forced convective heat transfer for the transfer fluid are solved simultaneously as a conjugate problem. A parametric study and a system optimization are conducted. It is found that the energy storage system with the countercurrent flow is an efficient way to absorb heat energy in a short period for pulsed power load space applications.

  14. A PCM/forced convection conjugate transient analysis of energy storage systems with annular and countercurrent flows

    NASA Technical Reports Server (NTRS)

    Cao, Y.; Faghri, A.; Juhasz, A.

    1991-01-01

    Latent heat energy storage systems with both annular and countercurrent flows are modeled numerically. The change of phase of the phase-change material (PCM) and the transient forced convective heat transfer for the transfer fluid are solved simultaneously as a conjugate problem. A parametric study and a system optimization are conducted. It is found that the energy storage system with the countercurrent flow is an efficient way to absorb heat energy in a short period for pulsed power load space applications.

  15. The Dependability of General-Factor Loadings: The Effects of Factor-Extraction Methods, Test Battery Composition, Test Battery Size, and Their Interactions

    ERIC Educational Resources Information Center

    Floyd, Randy G.; Shands, Elizabeth I.; Rafael, Fawziya A.; Bergeron, Renee; McGrew, Kevin S.

    2009-01-01

    To understand the extent to which the general-factor loadings of tests are inherent in their characteristics or due to the sampling of tests, the number of tests in the correlation matrix, and the factor-extraction methods used to obtain them, test scores from a large sample of young adults were inserted into independent and overlapping batteries…

  16. The Dependability of General-Factor Loadings: The Effects of Factor-Extraction Methods, Test Battery Composition, Test Battery Size, and Their Interactions

    ERIC Educational Resources Information Center

    Floyd, Randy G.; Shands, Elizabeth I.; Rafael, Fawziya A.; Bergeron, Renee; McGrew, Kevin S.

    2009-01-01

    To understand the extent to which the general-factor loadings of tests are inherent in their characteristics or due to the sampling of tests, the number of tests in the correlation matrix, and the factor-extraction methods used to obtain them, test scores from a large sample of young adults were inserted into independent and overlapping batteries…

  17. Preparative isolation and purification of harpagoside and angroside C from the root of Scrophularia ningpoensis Hemsley by high-speed counter-current chromatography.

    PubMed

    Tian, Jinfeng; Ye, Xiaoli; Shang, Yuanhong; Deng, Yafei; He, Kai; Li, Xuegang

    2012-10-01

    In this study, the bioactive component harpagoside and angroside C in the root of Scrophularia ningpoensis Hemsley was simultaneously separated by high-speed counter-current chromatography (HSCCC). A two-phase solvent system containing chloroform/n-butanol/methanol/water (4:1:3:2, v/v/v/v) was selected following consideration of the partition coefficient of the target compound. The crude extract (200 mg) was loaded onto a 280-mL HSCCC column and yielded 22 mg harpagoside and 31 mg angroside C with the purity of higher than 98 and 98.5%, respectively. It is feasible to isolate active compounds harpagoside and angroside C from S. ningpoensis using HSCCC.

  18. Preparative isolation and purification of celastrol from Celastrus orbiculatus Thunb. by a new counter-current chromatography method with an upright coil planet centrifuge.

    PubMed

    Wu, Shihua; Sun, Cuirong; Wang, Kuiwu; Pan, Yuanjiang

    2004-02-27

    A new counter-current chromatography (CCC) method with an upright coil planet centrifuge, which holds four identical multilayer coil columns in the symmetrical positions around the centrifuge axis, was applied to the isolation and purification of celastrol from the roots of Celastrus orbiculatus Thunb. The crude celastrol was obtained by elution with light petroleum from ethanol extracts using 15 cm x 5 cm i.d. silica gel flash chromatography. Preparative CCC with a two-phase system composed of light petroleum (bp 60-90 degrees C)-ethyl acetate-tetrachloromethane-methanol-water (1:1:8:6:1, v/v) was successfully performed, yielding 798 mg celastrol at 99.5% purity from 1020 mg of the crude sample in one step separation.

  19. Isolation and purification of three flavonoid glycosides from the leaves of Nelumbo nucifera (Lotus) by high-speed counter-current chromatography.

    PubMed

    Deng, Shengguo; Deng, Zeyuan; Fan, Yawei; Peng, You; Li, Jing; Xiong, Dongmei; Liu, Rong

    2009-08-15

    Semi-preparative high-speed counter-current chromatography (HSCCC) was successfully used for isolation and purification of flavonoid glycosides from the leaves of Nelumbo nucifera (Lotus) by using a two-phase-solvent system composed of n-hexane-ethyl acetate-methanol-water (1:5:1:5, v/v/v/v). The targeted compounds isolated, collected and purified by HSCCC were analyzed by high performance liquid chromatography (HPLC). A total of 4.6 mg of isoquercitrin, 9.1 mg of hyperoside and 3.0 mg of astragalin with the purity of 95.8%, 97.5% and 98.3%, respectively, were obtained in one-step separation and less than 6 h from 80 mg of crude extract from the leaves of N. nucifera. The chemical structures of all the three compounds were identified by MS, (1)H NMR, (13)C NMR. Astragalin was obtained from N. nucifera for the first time.

  20. Purification of six lignans from the stems of Schisandra chinensis by using high-speed counter-current chromatography combined with preparative high-performance liquid chromatography.

    PubMed

    Zhu, Lijie; Li, Bin; Liu, Xiuying; Huang, Guohui; Meng, Xianjun

    2015-11-01

    A method for the preparative purification of lignans from Schisandra chinensis was established using a combination of high-speed counter-current chromatography (HSCCC) and preparative high-performance liquid chromatography (HPLC). The crude extracts obtained from S. chinensis by using 70% ethanol were separated on a macroporous resin column and then eluted with a graded ethanol series. A two-phase solvent system consisting of n-hexane-ethyl acetate-methanol-water (1:1:1:1, v/v) was used for HSCCC, and a mobile phase of acetonitrile-water (50:50, v/v) was used for preparative HPLC. The results obtained using HSCCC were compared with those obtained using preparative HPLC, and their advantages were further integrated to improve the separation efficiency. Six known lignans were identified by electrospray ionisation mass spectrometry and (1)H nuclear magnetic resonance (NMR) and (13)C NMR analyses; the purities of all the compounds were more than 91%.

  1. Schinus terebinthifolius countercurrent chromatography (Part II): Intra-apparatus scale-up and inter-apparatus method transfer.

    PubMed

    Costa, Fernanda das Neves; Vieira, Mariana Neves; Garrard, Ian; Hewitson, Peter; Jerz, Gerold; Leitão, Gilda Guimarães; Ignatova, Svetlana

    2016-09-30

    Countercurrent chromatography (CCC) is being widely used across the world for purification of various materials, especially in natural product research. The predictability of CCC scale-up has been successfully demonstrated using specially designed instruments of the same manufacturer. The reality is that the most of CCC users do not have access to such instruments and do not have enough experience to transfer methods from one CCC column to another. This unique study of three international teams is based on innovative approach to simplify the scale-up between different CCC machines using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. The optimized separation methodology, recently developed by the authors (Part I), was repeatedly performed on CCC columns of different design available at most research laboratories across the world. Hexane - ethyl acetate - methanol - water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds to monitor stationary phase retention and calculate peak resolution. It has been demonstrated that volumetric, linear and length scale-up transfer factors based on column characteristics can be directly applied to different i.d., volume and length columns independently on instrument make in an intra-apparatus scale-up and inter-apparatus method transfer. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Ethyl acetate-n-butanol gradient solvent system for high-speed countercurrent chromatography to screen bioactive substances in okra.

    PubMed

    Ying, Hao; Jiang, Heyuan; Liu, Huan; Chen, Fangjuan; Du, Qizhen

    2014-09-12

    High-speed countercurrent chromatographic separation (HSCCC) possesses the property of zero-loss of sample, which is very useful for the screening of bioactive components. In the present study, the ethyl acetate-n-butanol gradient HSCCC solvent system composed of n-hexane-ethyl acetate-n-butanol-water was investigated for the screening of bioactive substances. To screen the antiproliferative compounds in okra extract, we used the stationary phase ethyl acetate-n-butanol-water (1:1:10) as the stationary phase, and eluted the antiproliferative components by 6-steps of gradient using mobile phases n-hexane-ethyl acetate (1:2), n-hexane-ethyl acetate (1:4), n-hexane-ethyl acetate (0:4), n-butanol-ethyl acetate (1:4) n-butanol-ethyl acetate (1:2), n-butanol-ethyl acetate (2:2), and n-butanol-ethyl acetate (2:1). The fractions collected from HSCCC separation with the gradient solvent system were assayed for antiproliferative activity against cancer cells. Bioactive components were identified: a major anti-cancer compound, 4'-hydroxy phenethyl trans-ferulate, with middle activity, and a minor anti-cancer compound, carolignan, with strong activity. The result shows that the gradient solvent system is potential for the screening of bioactive compounds from natural products.

  3. [Isolation and purification of diarylheptanoids from Alpinia officinarum Hance by high-speed counter-current chromatography].

    PubMed

    Ye, Qiongxian; Tan, Xiong; Zhu, Longping; Zhao, Zhimin; Yang, Depo; Yin, Sheng; Wang, Dongmei

    2012-03-01

    Three diarylheptanoids were isolated and purified from Alpinia officinarum Hance by high-speed counter-current chromatography (HSCCC). A two-phase solvent system composed of hexane-ethyl acetate-methanol-water (2: 3: 1.75: 1, v/v/v/v) was used. The lower phase was used as the stationary phase. From 122.20 mg petroleum ether extract of A. officinarum, 5R-hydroxy-7-(4-hydroxy-3-methoxyphenyl )-1-phenyl-3-heptanone (7.37 mg), 7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-4E-en-3-heptanone (9.11 mg) and 1,7-diphenyl-4E-en-3-heptanone (15.44 mg) with purities over 93% were obtained within 140 min in one-step separation by HSCCC under the conditions of a flow rate of 1.5 mL/min and 858 r/min. The obtained compounds were analyzed by high performance liquid chromatography to provide their purities, and their structures were confirmed by using mass spectrometry, 1H-nuclear magnetic resonance (1H-NMR) and 13C-NMR. The established HSCCC method is relatively simple, fast and suitable for the isolation and purification of diarylheptanoids from A. officinarum.

  4. Isolation and purification of seven lignans from Magnolia sprengeri by high-speed counter-current chromatography.

    PubMed

    Sun, Yu; Yu, Zongyuan; Duan, Wenjuan; Fang, Lei; Xu, Shuangshuang; Wang, Xiao

    2011-12-01

    Seven lignans including (-)-maglifloenone, futoenone, magnoline, cylohexadienone, fargesone C, fargesone A and fargesone B were isolated and purified from Magnolia sprengeri Pamp. using high-speed counter-current chromatography (HSCCC) with two-step separation. In the first step, a stepwise elution mode with the two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (1:0.8:0.6:1.2, 1:0.8:0.8:1, v/v) was used and 15.6 mg of (-)-maglifloenone, 19.2 mg of futoenone, 10.8 mg of magnoline, 14.7 mg of cylohexadienone and 217 mg residues were obtained from 370 mg crude extract. In the second step, the residues were successfully separated by HSCCC with the solvent system composed of petroleum ether-ethyl acetate-methanol-water (1:0.8:1.2:0.6, v/v), yielding 33.2 mg of fargesone C, 47.5 mg of fargesone A and 17.7 mg of fargesone B. The purities of the separated compounds were all over 95% determined by HPLC. The chemical structures of these compounds were confirmed by (1)H NMR, (13)C NMR and ESI-MS. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Purification of two triterpenoids from Schisandra chinensis by macroporous resin combined with high-speed counter-current chromatography.

    PubMed

    Zhu, Lijie; Li, Bin; Liu, Xiuying; Meng, Xianjun

    2014-10-01

    A method for preparative purification of corosolic acid and nigranoic acid from Schisandra chinensis (SC) was established using a combination of macroporous absorption resin column separation and high-speed counter-current chromatography (HSCCC). The crude extracts obtained from SC using 70% ethanol were separated on a macroporous resin column and then eluted with a graded ethanol series. The 70% ethanol fraction was used as the sample for separation of the two triterpenoids by HSCCC. The two-phase solvent system used for HSCCC separation was chloroform-n-butanol-methanol-water (10:0.5:7:4, v/v/v/v). The upper phase was used as the stationary phase of HSCCC. Corosolic acid (16.4 mg) of 96.3% purity and nigranoic acid (9.5 mg) of 98.9% purity were obtained in a one-step HSCCC separation from 100 mg of the sample. The structures of corosolic acid and nigranoic acid were identified by (1)H-nuclear magnetic resonance (NMR) and (13)C-NMR.

  6. Separation and purification of glucosinolates from crude plant homogenates by high-speed counter-current chromatography.

    PubMed

    Fahey, Jed W; Wade, Kristina L; Stephenson, Katherine K; Chou, F Edward

    2003-05-09

    Glucosinolates are anionic, hydrophilic plant secondary metabolites which are of particular interest due to their role in the prevention of cancer and other chronic and degenerative diseases. The separation and purification of glucosinolates from a variety of plant sources (e.g. seeds of broccoli, arugula and the horseradish tree), was achieved using high-speed counter-current chromatography (HSCCC). A high-salt, highly polar system containing 1-propanol-acetonitrile-saturated aqueous ammonium sulfate-water (1:0.5:1.2:1), was run on a semi-preparative scale and then transferred directly to preparative scale. Up to 7 g of a concentrated methanolic syrup containing about 10% glucosinolates was loaded on an 850-ml HSCCC column, and good separation and recovery were demonstrated for 4-methylsulfinylbutyl, 3-methylsulfinylpropyl, 4-methylthiobutyl, 2-propenyl and 4-(rhamnopyranosyloxy)benzyl glucosinolates. Multiple injections (5 to 6 times) were performed with well-preserved liquid stationary phase under centrifugal force. Pooled sequential runs with broccoli seed extract yielded about 20 g of its predominant glucosinolate, glucoraphanin, which was produced at > 95% purity and reduced to powdered form.

  7. Preparative purification of five bioactive components from Agrimonia pilosa Ledeb by high-speed counter-current chromatography.

    PubMed

    Wang, Yan; Liu, Mozhen; Zheng, Lingli; Yin, Lianhong; Xu, Lina; Qi, Yan; Ma, Xiaochi; Liu, Kexin; Peng, Jinyong

    2012-08-01

    High-speed counter-current chromatography (HSCCC) coupled with ultraviolet (UV) detection or evaporative light-scattering detection was successfully applied for preparative separation of five bioactive compounds from Agrimonia pilosa Ledeb. In preliminary process, D101 macroporous resin was used to separate the crude extract of the plant and four fractions (20, 40, 50, and 60% aqueous ethanol elutions) were produced. Then, these fractions were directly subjected to HSCCC purification. Five chemicals including taxifolin-3-glucoside (6.4 mg), quercetin-3-rhamnoside (13.0 mg), tiliroside (14.7 mg), agrimonolide (21.4 mg), and tormentic acid (29.8 mg) with the purities of 94.24, 95.37, 97.42, 95.29, and 96.34% were separated from each 200 mg prepared fraction. The purities were analyzed by high-performance liquid chromatography, and the chemical structures of the products were identified by UV detection, mass spectrometry, nuclear magnetic resonance, and the standards. This paper used a simple method to separate five bioactive compounds from A. pilosa Ledeb, and it could provide a new idea for the purification of bioactive compounds from other medicinal plants.

  8. Delamination propensity of pharmaceutical glass containers by accelerated testing with different extraction media.

    PubMed

    Guadagnino, Emanuel; Zuccato, Daniele

    2012-01-01

    The delamination of pharmaceutical glass is a serious issue, as it can cause glass particles to appear in vials, a problem that has forced a number of drug product recalls in recent years. In Type I pharmaceutical glass vials, delamination occurs generally at the bottom and shoulder, where extensive flaming during the conversion process can favor a strong evaporation of alkali and borate species and the formation of heavily enriched silica layers. The contact with parenteral preparations dissolved in an alkaline medium increases the rate of glass corrosion, while the differential hydration of these layers can cause the detachment of flakes. The purpose of this study was to investigate the effect of the pH and the composition of the extraction solutions on the propensity of different glass types to delaminate. Repeated autoclave extractions at 121 °C were carried out on different glass types with different extraction media, including organic extractants like citric and glutaric acid. When vials were in contact with alkaline solutions and similarly aggressive media, an increase in silica extraction values indicated glass corrosion and an increasing risk for further delamination. Under such conditions expansion 33 glass is extensively corroded, showing high silica concentration and heavy flaking as compared to other glass types. Sulfur-treated glass also showed early flaking, even if SiO(2) concentration was very low. A similar ranking was observed with extractions carried out with glutaric and citric acids, but at far much higher SiO(2) concentration levels. Extractions with 0.9% KCl solution can be used as an accelerated test to highlight the propensity of a glass to delaminate, but in no case it can be taken as a guarantee that the glass will not delaminate when exposed to the pharmaceutical drug, whose extraction ability requires case-by-case study. How can injectable drug manufacturers prevent glass delamination? The issue of delamination is a serious one, as it

  9. Improvement on the extraction method of RNA in mites and its quality test.

    PubMed

    Zhao, YaE; Hu, Li; Yang, Yuan Jun; Niu, Dong Ling; Wang, Rui Ling; Li, Wen Hao; Ma, Si Jia; Cheng, Juan

    2016-02-01

    To solve the long-existing difficult problems in extracting RNA and constructing a complementary DNA (cDNA) library for trace mites, we conducted a further comparative experiment among three RNA extraction methods (TRIzol method, Omega method, and Azanno method) based on our previous attempts at the construction of cDNA library of mites, with Psoroptes cuniculi still used as the experimental subject. By subsequently decreasing the number of mites, the least number of mites needed for RNA extraction of each method were found by criteria of completeness, concentration, and purity of the extracted RNA. Specific primers were designed according to the allergen Pso c1, Pso c2, and Actin gene sequences of Psoroptes to test the reliability of cDNA library. The results showed that Azanno method needed only 10 mites with sensitivity 204 times higher than previously used TRIzol method and 20 times higher than Omega method; clear RNA band was detected by agarose gel electrophoresis; and ultraviolet spectrophotometer determination showed that RNA concentration, 260/280, and 260/230 were in the range of 102 to 166 ng/μl, 1.83 to 1.99, and 1.49 to 1.72, respectively. Finally, specific primers detection showed that the amplified sequences had 98.33, 98.19, and 99.52% identities with those of P. cuniculi or Psoroptes ovis in GenBank, respectively, indicating that the cDNA library constructed using 10 mites was successful and it could meet the requirements for molecular biology research. Therefore, we concluded that Azanno method was more effective than TRIzol method and Omega method in RNA extraction and cDNA library construction of trace mites.

  10. Sample Results From The Extraction, Scrub, And Strip Test For The Blended NGS Solvent

    SciTech Connect

    Washington, A. L. II; Peters, T. B.

    2014-03-03

    This report summarizes the results of the extraction, scrub, and strip testing for the September 2013 sampling of the Next Generation Solvent (NGS) Blended solvent from the Modular Caustic Side-Solvent Extraction Unit (MCU) Solvent Hold Tank. MCU is in the process of transitioning from the BOBCalixC6 solvent to the NGS Blend solvent. As part of that transition, MCU has intentionally created a blended solvent to be processed using the Salt Batch program. This sample represents the first sample received from that blended solvent. There were two ESS tests performed where NGS blended solvent performance was assessed using either the Tank 21 material utilized in the Salt Batch 7 analyses or a simulant waste material used in the V-5/V-10 contactor testing. This report tabulates the temperature corrected cesium distribution, or DCs values, step recovery percentage, and actual temperatures recorded during the experiment. This report also identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. The calculated extraction DCs values using the Tank 21H material and simulant are 59.4 and 53.8, respectively. The DCs values for two scrub and three strip processes for the Tank 21 material are 4.58, 2.91, 0.00184, 0.0252, and 0.00575, respectively. The D-values for two scrub and three strip processes for the simulant are 3.47, 2.18, 0.00468, 0.00057, and 0.00572, respectively. These values are similar to previous measurements of Salt Batch 7 feed with lab-prepared blended solvent. These numbers are considered compatible to allow simulant testing to be completed in place of actual waste due to the limited availability of feed material.

  11. Preparation of salvianolic acid A by the degradation reaction of salvianolic acid B in subcritical water integrated with pH-zone-refining counter-current chromatography.

    PubMed

    Li, Huaizhi; Cheng, Yan; Dong, Hongjing; Wang, Xiao; Li, Jia; Gao, Qianshan

    2016-10-14

    Salvianolic acid A is the major bioactive compound in Danshen, however, due to the chemical instability and low content in Danshen, it is difficult to extract amount of salvianolic acid A. Therefore, this study was to establish an effective strategy for obtaining adequate amount of salvianolic acid A, subcritical water extraction was used to degrade salvianolic acid B and prepare salvianolic acid A. Different reaction conditions including temperature, time, concentration and pH value in subcritical water were investigated. Under 40mg/mL of reactant concentration, 180°C of temperature, 4.0 of pH value and 60min of reaction time, the highest yield rate of salvianolic acid A reached 34.86%. Then, the degradation products were successfully separated by pH-zone-refining counter-current chromatography with the solvent system Pet-EtAc-n-BuOH-H2O (2:3:1:9, v/v), where 10mM TFA was added in stationary phase and 10mM NH3·H2O in mobile phase. As a result, a total of 227.3mg of salvianolic acid A at 98.2% purity, 38.9mg of danshensu at 99.3% purity, 9.5mg of salvianolic acid D at 92.7% purity, and 32.8mg of protocatechuic aldehyde at 93.1% purity were obtained from 1.2g degradation products of salvianolic acid B by one-step purification. The results demonstrated that the combinative application of subcritical water and pH-zone-refining counter-current chromatography is a potential technique for the preparative separation of salvianolic acid A from salvianolic acid B. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Antibiotic purification from fermentation broths by counter-current chromatography: analysis of product purity and yield trade-offs.

    PubMed

    Booth, A J; Ngiam, S H; Lye, G J

    2004-12-01

    Counter-current chromatography (CCC) is a low pressure, liquid-liquid chromatographic technique which has proven to be a powerful purification tool for the high-resolution fractionation of a variety of active pharmaceutical compounds. The successful integration of CCC into either existing or new manufacturing processes requires the predictable purification of target compounds from crude, fermentation-derived, feed streams. This work examines the feasibility of CCC for the purification of fermentation-derived erythromycin A (EA) from its structurally and chemically similar analogues. At the laboratory scale, the effect of feed pre-treatment using either clarified, forward extracted (butyl acetate) or back extracted broth on EA separation was investigated. This defined the degree of impurity removal required, i.e. back extracted broth, to ensure a reproducible elution profile of EA during CCC. Optimisation and scale-up of the separation studied the effects of mobile phase flow (2-40 ml.min(-1)) and solute loading (0.1-10 g) on the attainable EA purity and yield. The results in all cases demonstrated a high attainable EA purity (>97% w/w) with throughputs up to 0.33 kg.day(-1). Secondly, a predictive scale-up model was applied demonstrating, that from knowledge of the solute distribution ratio of EA (K(EA)) at the laboratory scale, the EA elution time at the pilot scale could be predicted to within 3-10%, depending upon the solute injection volume. In addition, this study has evaluated a "fractionation diagram" approach to visually determine the effects of key operational variables on separation performance. This resulted in accurate fraction cut-point determination for a required degree of product purity and yield. Overall, the results show CCC to be a predictable and scaleable separation technique capable of handling real feed streams.

  13. Flat-Twisted Tubing: Novel Column Design for Spiral High-Speed Counter-Current Chromatography

    PubMed Central

    Yang, Yi; Aisa, Haji Akber; Ito, Yoichiro

    2009-01-01

    The original spiral tube assembly for high-speed counter-current chromatography (HSCCC) is further improved by a new tube configuration called “flat-twisted tubing” which was made by extruding the tube (1.6 mm I.D.) through a narrow slot followed by twisting along its axis forming about 1 cm twisted screw pitch. This modification interrupts the laminar flow of the mobile phase through the tube and continuously mixes the two phases through the column. The performance of this spiral tube assembly was tested by three types of two-phase solvent systems with different polarity each with a set of suitable test samples such as DNP-amino acids, dipeptides and proteins at the optimal elution modes. In general all these test samples yielded higher resolution with the lower mobile phase than the upper mobile phase. In the most hydrophobic two-phase solvent system composed of hexane-ethyl acetate-metanol-0.1M hydrochloric acid (1:1:1:1, v/v), DNP-amino acids were separated with Rs-a (peak resolution based on the same column capacity adjusted for comparison) at 4.40 and 73 % of stationary phase retention at a flow rate of 0.5 ml/min with the lower mobile phase. In the polar solvent system composed of 1-butanol-acetic acid-water (4: 1: 5, v/v), dipeptide samples were resolved with Rs-a at 4.06, compared to 2.79 with the cross-pressed tube assembly at 45 % stationary phase retention, each at a flow rate of 1 ml/min. Finally in the aqueous-aqueous polymer phase systems composed of polyethylene glycol 1000 – dibasic potassium phosphate each 12.5% (w/w) in water, protein samples were resolved with Rs-a at 2.53 compared to 1.10 with the cross-pressed tube assembly at 52 % of stationary phase retention, each at a flow rate of 1 ml/min. These results indicate that the present system substantially improves the partition efficiency with a satisfactory level of stationary phase retention by the lower mobile phase. PMID:19486987

  14. Flat-twisted tubing: novel column design for spiral high-speed counter-current chromatography.

    PubMed

    Yang, Yi; Aisa, Haji Akber; Ito, Yoichiro

    2009-07-03

    The original spiral tube assembly for high-speed counter-current chromatography (HSCCC) is further improved by a new tube configuration called "flat-twisted tubing" which was made by extruding the tube (1.6 mm I.D.) through a narrow slot followed by twisting along its axis forming about 1cm twisted screw pitch. This modification interrupts the laminar flow of the mobile phase through the tube and continuously mixes the two phases through the column. The performance of this spiral tube assembly was tested by three types of two-phase solvent systems with different polarities each with a set of suitable test samples such as DNP-amino acids, dipeptides and proteins at the optimal elution modes. In general all these test samples yielded higher resolution with the lower mobile phase than the upper mobile phase. In the most hydrophobic two-phase solvent system composed of hexane-ethyl acetate-methanol-0.1 M hydrochloric acid (1:1:1:1, v/v/v/v), DNP-amino acids were separated with Rs-a (peak resolution based on the same column capacity adjusted for comparison) at 4.40 and 73% of stationary phase retention at a flow rate of 0.5 ml/min with the lower mobile phase. In the polar solvent system composed of 1-butanol-acetic acid-water (4:1:5, v/v/v), dipeptide samples were resolved with Rs-a at 4.06, compared to 2.79 with the cross-pressed tube assembly at 45% stationary phase retention, each at a flow rate of 1 ml/min. Finally in the aqueous-aqueous polymer phase systems composed of polyethylene glycol 1000 - dibasic potassium phosphate each 12.5% (w/w) in water, protein samples were resolved with Rs-a at 2.53 compared to 1.10 with the cross-pressed tube assembly at 52% of stationary phase retention, each at a flow rate of 1 ml/min. These results indicate that the present system substantially improves the partition efficiency with a satisfactory level of stationary phase retention by the lower mobile phase.

  15. Biodiesel production from soybean oil deodorizer distillate enhanced by counter-current pulsed ultrasound.

    PubMed

    Yin, Xiulian; You, Qinghong; Ma, Haile; Dai, Chunhua; Zhang, Henan; Li, Kexin; Li, Yunliang

    2015-03-01

    Biodiesel production from soybean oil deodorizer distillate enhanced by counter-current pulsed ultrasound was studied. Effect of static probe ultrasonic enhanced transesterification (SPUE) and counter-current probe ultrasonic enhanced transesterification (CCPUE) on the biodiesel conversion were compared. The results indicated that CCPUE was a better method for enhancing transesterification. The working conditions of CCPUE were studied by single-factor experiment design and the results showed that the optimal conditions were: initial temperature 25 °C, methanol to triglyceride molar ratio 10:1, flow rate 200 mL/min, catalyst content 1.8%, ultrasound working on-time 4 s, off-time 2 s, total working time 50 min. Under these conditions, the average biodiesel conversion of three experiments was 96.1%. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Chromatographic separation of three monoclonal antibody variants using multicolumn countercurrent solvent gradient purification (MCSGP).

    PubMed

    Müller-Späth, Thomas; Aumann, Lars; Melter, Lena; Ströhlein, Guido; Morbidelli, Massimo

    2008-08-15

    Multicolumn countercurrent solvent gradient purification (MCSGP) is a continuous chromatographic process developed in recent years (Aumann and Morbidelli, 2007a; Aumann et al., 2007) that is particularly suited for applications in the field of bioseparations. Like batch chromatography, MCSGP is suitable for three-fraction chromatographic separations and able to perform solvent gradients but it is superior in terms of solvent consumption, yield, purity, and productivity due to the countercurrent movement of the liquid and the solid phases. In this work, the MCSGP process is applied to the separation of three monoclonal antibody variants on a conventional preparative cation exchange resin. The experimental process performance was compared to simulations based on a lumped kinetic model. Yield and purity values of the target variant of 93%, respectively were obtained experimentally. The batch reference process was clearly outperformed by the MCSGP process.

  17. Reconfigurable Special Test Circuit of physics-based IGBT models parameter extraction

    NASA Astrophysics Data System (ADS)

    Rodríguez, Marco A.; Claudio, Abraham; Cotorogea, Maria; González, Leobardo H.; Aguayo, Jesús

    2010-11-01

    Physics-based models of power electronic devices are the most accurate for circuit simulation purposes. However, many parameters of such models are related to device physics and structure and are not directly available for the user. The IGBT is still the most used power semiconductor device for applications at medium power and frequency ranges, due to its good compromise between on-state loss, switching loss, and ease of control. This paper presents a procedure for extracting the most important parameters of the IGBT, with physical background and electrical measurements. The goal is to develop a deeply understanding of the device-structure and to simulate correctly both steady-state and transient period with any circuit simulation software without the IGBT model provided by the manufacturer. The method consists of seven test setups and seven algorithms for extracting 13 physical and structural parameters needed in most physics-based IGBT models; by using only one Reconfigurable Special Test Circuit in order to achieve the different test setups conditions.

  18. Skin prick testing with standardized extracts from 3 different manufacturers. A comparative randomized study.

    PubMed

    Nielsen, N H; Dirksen, A; Mosbech, H; Launbjerg, J; Biering, I; Søborg, M

    1992-01-01

    The aim of this study was to compare skin reactivity to routine allergen prick test with panels of allergens, supplied by three different manufacturers. The allergens comprised ten aero-allergens commonly used for skin prick test in Northern Europe, and included pollen, dander, house dust mites, and moulds. Two hundred consecutive patients were tested. The methods for standardization of allergen extracts, declaration of allergenic potency, and recommended lancets differed. The equipment were Soluprick SQ (Allergologisk Laboratorium A/S, Denmark) (ALK), Alphatest (Dome/Hollister-Stier, U.K.) (DHS), and Phazet (Pharmacia, Sweden) (PHA). The coefficient of variation for the allergen coated PHA (same lancet was applied twice) was 0.31, and for ALK and DHS allergen extracts 0.13 and 0.18, respectively. The frequencies of patients with positive reactions to the various allergens were generally similar, although DHS appeared to elicit less positive reactions to Timothy, dog, and Dermatophagoides pteronnyssinus. For the individual physician, it may be important to know the allergenic activity of the different allergens in his routine panel compared to the activity in other similar panels.

  19. Inert gas clearance from tissue by co-currently and counter-currently arranged microvessels

    PubMed Central

    Lu, Y.; Michel, C. C.

    2012-01-01

    To elucidate the clearance of dissolved inert gas from tissues, we have developed numerical models of gas transport in a cylindrical block of tissue supplied by one or two capillaries. With two capillaries, attention is given to the effects of co-current and counter-current flow on tissue gas clearance. Clearance by counter-current flow is compared with clearance by a single capillary or by two co-currently arranged capillaries. Effects of the blood velocity, solubility, and diffusivity of the gas in the tissue are investigated using parameters with physiological values. It is found that under the conditions investigated, almost identical clearances are achieved by a single capillary as by a co-current pair when the total flow per tissue volume in each unit is the same (i.e., flow velocity in the single capillary is twice that in each co-current vessel). For both co-current and counter-current arrangements, approximate linear relations exist between the tissue gas clearance rate and tissue blood perfusion rate. However, the counter-current arrangement of capillaries results in less-efficient clearance of the inert gas from tissues. Furthermore, this difference in efficiency increases at higher blood flow rates. At a given blood flow, the simple conduction-capacitance model, which has been used to estimate tissue blood perfusion rate from inert gas clearance, underestimates gas clearance rates predicted by the numerical models for single vessel or for two vessels with co-current flow. This difference is accounted for in discussion, which also considers the choice of parameters and possible effects of microvascular architecture on the interpretation of tissue inert gas clearance. PMID:22604885

  20. Inert gas clearance from tissue by co-currently and counter-currently arranged microvessels.

    PubMed

    Lu, Y; Michel, C C; Wang, W

    2012-08-01

    To elucidate the clearance of dissolved inert gas from tissues, we have developed numerical models of gas transport in a cylindrical block of tissue supplied by one or two capillaries. With two capillaries, attention is given to the effects of co-current and counter-current flow on tissue gas clearance. Clearance by counter-current flow is compared with clearance by a single capillary or by two co-currently arranged capillaries. Effects of the blood velocity, solubility, and diffusivity of the gas in the tissue are investigated using parameters with physiological values. It is found that under the conditions investigated, almost identical clearances are achieved by a single capillary as by a co-current pair when the total flow per tissue volume in each unit is the same (i.e., flow velocity in the single capillary is twice that in each co-current vessel). For both co-current and counter-current arrangements, approximate linear relations exist between the tissue gas clearance rate and tissue blood perfusion rate. However, the counter-current arrangement of capillaries results in less-efficient clearance of the inert gas from tissues. Furthermore, this difference in efficiency increases at higher blood flow rates. At a given blood flow, the simple conduction-capacitance model, which has been used to estimate tissue blood perfusion rate from inert gas clearance, underestimates gas clearance rates predicted by the numerical models for single vessel or for two vessels with co-current flow. This difference is accounted for in discussion, which also considers the choice of parameters and possible effects of microvascular architecture on the interpretation of tissue inert gas clearance.

  1. [Extraction technology of effervescent granules for arresting cold pain optimized by orthogonal tests].

    PubMed

    Sun, X; Zhang, Z; Ma, L; Zhang, W

    1996-03-01

    In the extraction technology of Effervescent Granules for Arresting Cold Pain (Hantongding Paoteng Chongji), the drug combinative modes, solvent pH and drug granularity were optimized by orthogonal tests, with the total alkaloid, paeoniflorin and glycyrrhetinic acid as indexes. The experimental results show that it is better to decoct together all the recipe ingredients, with water of pH2 for the first decoction, then water of pH8 for the second decoction, and to make its granularities ranging from the original herbal pieces to particles which can pass through a No. 2 sieve.

  2. Straw man 900-1000 GeV crystal extraction test beam for Fermilab collider operation

    SciTech Connect

    Carrigan, R.A. Jr.

    1996-10-01

    A design for a 900-1000 GeV, 100 khz parasitic test beam for use during collider operations has been developed. The beam makes use of two bent crystals, one for extraction and the other one for redirecting the beam in to the present Switchyard beam system. The beam requires only a few modifications in the A0 area and largely uses existing devices. It should be straight-forward to modify one or two beam lines in the fixed target experimental areas to work above 800 GeV. Possibilities for improvements to the design,to operate at higher fluxes are discussed.

  3. SOLVENT EXTRACTION PROCESS FOR THE SEPARATION OF URANIUM AND THORIUM FROM PROTACTINIUM AND FISSION PRODUCTS

    DOEpatents

    Rainey, R.H.; Moore, J.G.

    1962-08-14

    A liquid-liquid extraction process was developed for recovering thorium and uranium values from a neutron irradiated thorium composition. They are separated from a solvent extraction system comprising a first end extraction stage for introducing an aqueous feed containing thorium and uranium into the system consisting of a plurality of intermediate extractiorr stages and a second end extractron stage for introducing an aqueous immiscible selective organic solvent for thorium and uranium in countercurrent contact therein with the aqueous feed. A nitrate iondeficient aqueous feed solution containing thorium and uranium was introduced into the first end extraction stage in countercurrent contact with the organic solvent entering the system from the second end extraction stage while intro ducing an aqueous solution of salting nitric acid into any one of the intermediate extraction stages of the system. The resultant thorium and uranium-laden organic solvent was removed at a point preceding the first end extraction stage of the system. (AEC)

  4. Selective isolation of components from natural volatile oil by countercurrent chromatography with cyclodextrins as selective reagent.

    PubMed

    Tong, Shengqiang; Lu, Mengxia; Chu, Chu; Yan, Jizhong; Huang, Juan; Ying, Yongfei

    2016-04-29

    Selective separation of chemical components from seven kinds of volatile oil by countercurrent chromatography with three types of cyclodextrins as selective reagent was investigated in this work. Preparative separation of chemical components from volatile oil is generally quite challenging due to their extremely complexity of the composition. A biphasic solvent system n-hexane-0.10 mol L(-1) cyclodextrin (1:1, v/v) was selected for separation of components from volatile oil and three types of cyclodextrins were investigated, including β-cyclodexrin, methyl-β-cyclodexrin and hydroxypropyl-β-cyclodexrin. All kinds of volatile oils are from seven kinds of traditional Chinese herb. Results showed that some chemical components could be well separated with high purity from each kind of volatile oil using different type of cyclodextrin as selective reagent. For example, germacrone and curcumenone could be selectively separated from volatile oil of Curcumae Rhizoma with methyl-β-cyclodexrin and hydroxypropyl-β-cyclodexrin as selector respectively, and other five components were selectively separated from volatile oil of Chuanxiong Rhizoma, Myristicae Semen, Aucklandiae Radix and Angelicae Sinensis Radix by countercurrent chromatography with different cyclodexrin as selective reagent. Separation mechanism for separation of components from volatile oil by countercurrent chromatography with cyclodextrin as selective reagent was proposed. Peak resolution of the present separation method could be greatly influenced by the chemical compositions of volatile oil. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Long-Term Observations of a Coastal Countercurrent on the Southeast Florida Shelf

    NASA Astrophysics Data System (ADS)

    Soloviev, A.

    2010-12-01

    Coastal circulation along the southeast Florida shelf is strongly related to the dynamics of the Florida Current as a part of the western boundary current system. We have conducted long-term observations with a mooring array deployed on the Ft. Lauderdale FL shelf. The array consists of a bottom ADCP mooring at 11 m isobath on the Dania Beach Shelf providing almost continuous observations since 1999 and a bottom ADCP mooring deployed on the Miami Terrace near Pompano Beach at 240 m isobath since 2007. There is a strong variability of the coastal current at this location on time scales ranging from hours to months, which is explained by the proximity to the Florida Current. An interesting feature revealed during these observations is an intermittent coastal countercurrent. This coastal countercurrent is seasonally modulated, reversing its direction during the summer season. The appearance of the countercurrent on the southeast Florida shelf and its relation to the Florida Current and undercurrent have not yet been completely understood. The possible physical mechanism behind this feature of the coastal circulation on the Southeast Florida shelf and practical applications are being discussed.

  6. Standardized Rat Model Testing Effects of Inflammation and Grafting on Extraction Healing.

    PubMed

    Willett, Emily S; Liu, Jingpeng; Berke, Molly; Giannini, Peter J; Schmid, Marian; Jia, Zhenshan; Wang, Xiaobei; Wang, Xiaoyan; Samson, Kaeli; Yu, Fang; Wang, Dong; Nawshad, Ali; Reinhardt, Richard A

    2017-08-01

    Loss of alveolar ridge width and height after tooth extraction is well documented, but models to evaluate ridge preservation are neither standardized nor cost-effective. This rat model characterizes the pattern of bone turnover and inflammation after extraction and bone grafting with or without local simvastatin (SIM). Fifty retired-breeder rats underwent extraction of the maxillary right first molar and standard surgical defect creation under inhalation/local anesthesia. The left side of each animal served as unmanipulated control. Untreated groups (n = 8 to 9 per group) were compared (analysis of variance, t test) at days 0, 7, 14, and 28 for alveolar ridge height and width and for markers of inflammation and bone turnover by microcomputed tomography, histology, and enzyme-linked immunosorbent assay. Seventeen additional specimens had defects grafted with either bone mineralized matrix (BMM) or a BMM+SIM conjugate. Extraction-induced bone loss (BL) was noted on buccal, palatal, and interproximal height (P <0.05) and ridge width (P <0.01). Week 1 inflammation positively correlated with ridge height; thereafter, a more intense inflammatory reaction corresponded to reduction in alveolar bone height and density (r = 0.74; P <0.05; Spearman). BMM+SIM preserved the most interproximal bone height (P <0.01), increased ridge width and bone density (P <0.01), enhanced 7-day prostaglandin E2 (P <0.01), and reduced 28-day inflammation density (P <0.05). The standard defect used in the current study paralleled human postextraction alveolar BL. Defect grafting, especially BMM+SIM, reduced inflammation and preserved bone.

  7. Antidepressant activity of some Hypericum reflexum L. fil. extracts in the forced swimming test in mice.

    PubMed

    Sánchez-Mateo, C C; Bonkanka, C X; Prado, B; Rabanal, R M

    2007-05-30

    We previously reported that oral administration of the methanol extract obtained from the aerial part in blossom of Hypericum reflexum L. fil. was active in the tetrabenazine and forced swimming test. In the present study, the effect of the aqueous, butanol and chloroform fractions obtained from the methanol extract of this species on the central nervous system was investigated in mice, particularly in animal models of depression. Antidepressant activity was detected in the butanol and chloroform fractions of this species using the forced swimming test since both fractions induced a significant reduction of the immobility time, producing no effects or only a slight depression on spontaneous motor activity when assessed in a photocell activity meter. Moreover, these fractions did not alter significantly the pentobarbital-induced sleeping time. On the other hand, the chloroform fraction produced a slight but significant hypothermia and was also effective in antagonizing the ptosis induced by tetrabenazine. Furthermore, the butanol fraction produced a slight potentiation of the head twitches and syndrome induced by 5-HTP. Taken together, these data indicate that the butanol and chloroform fractions from Hypericum reflexum possess antidepressant-like effects in mice, providing further support for the traditional use of these plants in the Canary Islands folk medicine against central nervous disorders.

  8. In vitro lipolysis tests on lipid nanoparticles: comparison between lipase/co-lipase and pancreatic extract.

    PubMed

    Jannin, Vincent; Dellera, Eleonora; Chevrier, Stéphanie; Chavant, Yann; Voutsinas, Christophe; Bonferoni, Cristina; Demarne, Frédéric

    2015-01-01

    Solid lipid nanoparticles (SLNs) and nanostructured lipid carriers (NLC) are lipid nanocarriers aimed to the delivery of drugs characterized by a low bioavailability, such as poorly water-soluble drugs and peptides or proteins. The oral administration of these lipid nanocarriers implies the study of their lipolysis in presence of enzymes that are commonly involved in dietary lipid digestion in the gastrointestinal tract. In this study, a comparison between two methods was performed: on one hand, the lipase/co-lipase assay, commonly described in the literature to study the digestion of lipid nanocarriers, and on the other hand, the lipolysis test using porcine pancreatic extract and the pH-stat apparatus. This pancreatic extract contains both the pancreatic lipase and carboxyl ester hydrolase (CEH) that permit to mimic in a biorelevant manner the duodenal digestive lipolysis. The test was performed by means of a pH-stat apparatus to work at constant pH, 5.5 or 6.25, representing respectively the fasted or fed state pH conditions. The evolution of all acylglycerol entities was monitored during the digestion by sampling the reaction vessel at different time points, until 60 min, and the lipid composition of the digest was analyzed by gas chromatography. SLN and NLC systems obtained with long-chain saturated acylglycerols were rapidly and completely digested by pancreatic enzymes. The pH-stat titration method appears to be a powerful technique to follow the digestibility of these solid lipid-based nanoparticles.

  9. Extraction procedure testing of solid wastes generated at selected metal ore mines and mills

    NASA Astrophysics Data System (ADS)

    Harty, David M.; Terlecky, P. Michael

    1986-09-01

    Solid waste samples from a reconnaissance study conducted at ore mining and milling sites were subjected to the U.S. Environmental Protection Agency extraction procedure (EP) leaching test Sites visited included mines and mills extracting ores of antimony (Sb), mercury (Hg), vanadium (V), tungsten (W), and nickel (Ni). Samples analyzed included mine wastes, treatment pond solids, tailings, low grade ore, and other solid wastes generated at these facilities Analysis of the leachate from these tests indicates that none of the samples generated leachate in which the concentration of any toxic metal parameter exceeded EPA criteria levels for those metals. By volume, tailings generally constitute the largest amount of solid wastes generated, but these data indicate that with proper management and monitoring, current EPA criteria can be met for tailings and for most solid wastes associated with mining and milling of these metal ores. Long-term studies are needed to determine if leachate characteristics change with time and to assist in development of closure plans and post closure monitoring programs.

  10. Development of an efficient fractionation method for the preparative separation of sesquiterpenoids from Tussilago farfara by counter-current chromatography.

    PubMed

    Song, Kwangho; Lee, Kyoung Jin; Kim, Yeong Shik

    2017-03-17

    A novel application of counter-current chromatography (CCC) to enrich plant extracts using direct and continuous injection (CCC-DCI) was developed to fractionate sesquiterpenoids from the buds of Tussilago farfara L. In this study, an n-hexane-acetonitrile-water (HAcW) solvent system was separately pumped into the CCC column, and an extraction solution (45% acetonitrile) was directly and continuously injected into the CCC column. Since the extraction solution was used as a mobile phase in this method, solvent consumption could be greatly reduced. To enrich the extraction solution (315.9g/5.4L), only 4.2L water, 4.6L acetonitrile, and 1.2L n-hexane were used, including the extraction step. Finally, 6.8g of a sesquiterpenoid-enriched (STE) fraction was obtained from the crude extract (315.9g) of Tussilago farfara (1kg) in a single CCC run with a separation time of 8.5h. The sample injection capacity of CCC-DCI was greater than 300g; this amount of sample could not be handled in conventional CCC or other fractionation methods with the same column volume. Moreover, three major sesquiterpenoids (1: tussilagone, 2: 14-acetoxy-7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-notonipetranone, and 3: 7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-3, 14-dehydro-Z-notonipetranone) were purified from the STE fraction by CCC, and their chemical structures were elucidated by (1)H NMR and (13)C NMR. A quantification study was conducted, and the contents of compounds 1-3 in the CCC-DCI fraction were higher than those of conventional multi-step fractionations performed in series: solvent partitioning and open column chromatography. Furthermore, the average CCC-DCI recoveries were 96.1% (1), 96.9% (2), and 94.6% (3), whereas the open column chromatography recoveries were 77.7% (1), 66.5% (2), and 58.4% (3). The developed method demonstrates that CCC is a useful technique for enriching target components from natural products. Copyright © 2017 Elsevier B.V. All

  11. Mutagenicity evaluation of Schistosoma spp. extracts by the umu-test and V79/HGPRT gene mutation assay.

    PubMed

    Osada, Yoshio; Kumagai, Takashi; Masuda, Kyoko; Suzuki, Tomoyuki; Kanazawa, Tamotsu

    2005-03-01

    Schistosomiasis has been suspected of being a risk factor for various types of cancers for sometime, e.g., bladder cancer, colorectal cancer and hepatic cancer. Among them, the etiological relationship between urinary schistosomiasis and bladder cancer is now widely accepted. However, mechanisms of the carcinogenesis are still unclear. Here, we tested the mutagenicity of the parasite extracts by the umu-test and hypoxanthine guanine phosphoribosyltransferase (HGPRT) gene mutation assay, which both overcome disadvantages of the Ames plate assay. Adult worm extracts and egg extracts of Schistosoma haematobium and Schistosoma mansoni were tested. Under our experimental conditions, neither worm nor egg extracts were shown to have any mutagenicity in both tests even in the presence of S9 mix. Our results suggest that there is very little possibility of immediate gene mutation due to the parasite-derived substances in schistosomiasis-related carcinogenesis.

  12. Preparative Separation of Main Ustilaginoidins from Rice False Smut Balls by High-Speed Counter-Current Chromatography

    PubMed Central

    Sun, Weibo; Dong, Xuejiao; Xu, Dan; Meng, Jiajia; Fu, Xiaoxiang; Wang, Xiaohan; Lai, Daowan; Zhou, Ligang; Liu, Yang

    2016-01-01

    Ustilaginoidins are bis-naphtho-γ-pyrone mycotoxins isolated from the rice false smut balls (FSBs) infected by the pathogen Villosiclava virens in rice spikelets on panicles. In order to obtain large amounts of pure ustilaginoidins to further evaluate their biological activities and functions, phytotoxicity on rice, security to human and animals as well as to accelerate their applications as pharmaceuticals, preparative high-speed counter-current chromatography (HSCCC) was successfully applied to the isolation and purification of seven bis-naphtho-γ-pyrone mycotoxins, namely ustilaginoidins A (1), G (2), B (3), H (4), I (5), C (6), and J (7) from the ethyl acetate crude extract of rice FSBs. Both 1 and 2 were prepared by HSCCC from the low-polarity fraction of the crude extract using the two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water at the volume ratio of 6.5:3.5:5.0:5.0. Similarly, 3, 4 and 5 were prepared from the medium-polarity fraction using the system at the volume ratio of 4.0:5.0:5.0:6.0, and 6 and 7 were prepared from the higher-polarity fraction using the system at volume ratio of 3.0:5.0:4.0:6.7. A total of 6.2 mg of 1, 5.1 mg of 2, 3.9 mg of 3, 1.2 mg of 4, 5.7 mg of 5, 3.5 mg of 6, and 6.1 mg of 7 with purities of 88%, 82%, 91%, 80%, 92%, 81% and 83%, respectively, were yielded from total 62 mg fraction samples in three independent HSCCC runs. The structures of the purified ustilaginoidins were characterized by means of physicochemical and spectrometric analysis. PMID:26771638

  13. SW-846 Test Method 3200: Mercury Species Fractionation and Quantification by Microwave Assisted Extraction, Selective Solvent Extraction and/or Solid Phase Extraction

    EPA Pesticide Factsheets

    a sequential extraction and separation procedure that maybe used in conjunction with a determinative method to differentiate mercury species that arepresent in soils and sediments. provides information on both total mercury andvarious mercury species.

  14. Equine infectious anemia: preparation of a liquid antigen extract for the agar-gel immunodiffusion and complement-fixation tests.

    PubMed

    Boulanger, P; Bannister, G L; Carrier, S P

    1972-04-01

    An agar-gel immunodiffusion test recommended for the diagnosis of equine infectious anemia was evaluated. Our preliminary observations confirmed those of Coggins concerning the mechanism of the test and the results obtained. Furthermore, emphasis was put on the difficulties encountered in the production of spleen antigens with an optimum amount of reactivity. Acetone-ether extraction procedures for the preparation of a liquid antigen extract are described. This type of antigen was reactive in the complement-fixation test in 1:8 or greater dilution and it is proposed to use the complement-fixation test in assessing and standardizing the liquid antigen extract activity to be used in the immunodiffusion test. This antigen can also be concentrated or diluted, if required, to meet the reactivity of a standard antigen used in the test.

  15. Equine Infectious Anemia: Preparation of a Liquid Antigen Extract for the Agar-gel Immunodiffusion and Complement-fixation Tests

    PubMed Central

    Boulanger, P.; Bannister, G. L.; Carrier, S. P.

    1972-01-01

    An agar-gel immunodiffusion test recommended for the diagnosis of equine infectious anemia was evaluated. Our preliminary observations confirmed those of Coggins concerning the mechanism of the test and the results obtained. Furthermore, emphasis was put on the difficulties encountered in the production of spleen antigens with an optimum amount of reactivity. Acetone-ether extraction procedures for the preparation of a liquid antigen extract are described. This type of antigen was reactive in the complement-fixation test in 1:8 or greater dilution and it is proposed to use the complement-fixation test in assessing and standardizing the liquid antigen extract activity to be used in the immunodiffusion test. This antigen can also be concentrated or diluted, if required, to meet the reactivity of a standard antigen used in the test. ImagesFig. 1.Fig. 2.Fig. 3.Fig. 4.Fig. 5.Fig. 6. PMID:4259924

  16. Extraction-Separation Performance and Dynamic Modeling of Orion Test Vehicles with Adams Simulation: 3rd Edition

    NASA Technical Reports Server (NTRS)

    Varela, Jose G.; Reddy, Satish; Moeller, Enrique; Anderson, Keith

    2017-01-01

    NASA's Orion Capsule Parachute Assembly System (CPAS) Project is now in the qualification phase of testing, and the Adams simulation has continued to evolve to model the complex dynamics experienced during the test article extraction and separation phases of flight. The ability to initiate tests near the upper altitude limit of the Orion parachute deployment envelope requires extractions from the aircraft at 35,000 ft-MSL. Engineering development phase testing of the Parachute Test Vehicle (PTV) carried by the Carriage Platform Separation System (CPSS) at altitude resulted in test support equipment hardware failures due to increased energy caused by higher true airspeeds. As a result, hardware modifications became a necessity requiring ground static testing of the textile components to be conducted and a new ground dynamic test of the extraction system to be devised. Force-displacement curves from static tests were incorporated into the Adams simulations, allowing prediction of loads, velocities and margins encountered during both flight and ground dynamic tests. The Adams simulation was then further refined by fine tuning the damping terms to match the peak loads recorded in the ground dynamic tests. The failure observed in flight testing was successfully replicated in ground testing and true safety margins of the textile components were revealed. A multi-loop energy modulator was then incorporated into the system level Adams simulation model and the effect on improving test margins be properly evaluated leading to high confidence ground verification testing of the final design solution.

  17. Highly Effective DNA Extraction Method for Nuclear Short Tandem Repeat Testing of Skeletal Remains from Mass Graves

    PubMed Central

    Davoren, Jon; Vanek, Daniel; Konjhodzić, Rijad; Crews, John; Huffine, Edwin; Parsons, Thomas J.

    2007-01-01

    Aim To quantitatively compare a silica extraction method with a commonly used phenol/chloroform extraction method for DNA analysis of specimens exhumed from mass graves. Methods DNA was extracted from twenty randomly chosen femur samples, using the International Commission on Missing Persons (ICMP) silica method, based on Qiagen Blood Maxi Kit, and compared with the DNA extracted by the standard phenol/chloroform-based method. The efficacy of extraction methods was compared by real time polymerase chain reaction (PCR) to measure DNA quantity and the presence of inhibitors and by amplification with the PowerPlex 16 (PP16) multiplex nuclear short tandem repeat (STR) kit. Results DNA quantification results showed that the silica-based method extracted on average 1.94 ng of DNA per gram of bone (range 0.25-9.58 ng/g), compared with only 0.68 ng/g by the organic method extracted (range 0.0016-4.4880 ng/g). Inhibition tests showed that there were on average significantly lower levels of PCR inhibitors in DNA isolated by the organic method. When amplified with PP16, all samples extracted by silica-based method produced 16 full loci profiles, while only 75% of the DNA extracts obtained by organic technique amplified 16 loci profiles. Conclusions The silica-based extraction method showed better results in nuclear STR typing from degraded bone samples than a commonly used phenol/chloroform method. PMID:17696302

  18. Isolation of dimeric, trimeric, tetrameric and pentameric procyanidins from unroasted cocoa beans (Theobroma cacao L.) using countercurrent chromatography.

    PubMed

    Esatbeyoglu, Tuba; Wray, Victor; Winterhalter, Peter

    2015-07-15

    The main procyanidins, including dimeric B2 and B5, trimeric C1, tetrameric and pentameric procyanidins, were isolated from unroasted cocoa beans (Theobroma cacao L.) using various techniques of countercurrent chromatography, such as high-speed countercurrent chromatography (HSCCC), low-speed rotary countercurrent chromatography (LSRCCC) and spiral-coil LSRCCC. Furthermore, dimeric procyanidins B1 and B7, which are not present naturally in the analysed cocoa beans, were obtained after semisynthesis of cocoa bean polymers with (+)-catechin as nucleophile and separated by countercurrent chromatography. In this way, the isolation of dimeric procyanidin B1 in considerable amounts (500mg, purity>97%) was possible in a single run. This is the first report concerning the isolation and semisynthesis of dimeric to pentameric procyanidins from T. cacao by countercurrent chromatography. Additionally, the chemical structures of tetrameric (cinnamtannin A2) and pentameric procyanidins (cinnamtannin A3) were elucidated on the basis of (1)H NMR spectroscopy. Interflavanoid linkage was determined by NOE-correlations, for the first time. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. Characterization and testing of amidoxime-based adsorbent materials to extract uranium from natural seawater

    SciTech Connect

    Kuo, Li-Jung; Janke, Christopher James; Wood, Jordana; Strivens, Jonathan E.; Gill, Gary

    2015-11-19

    Extraction of uranium (U) from seawater for use as a nuclear fuel is a significant challenge due to the low concentration of U in seawater (~3.3 ppb) and difficulties to selectively extract U from the background of major and trace elements in seawater. The Pacific Northwest National Laboratory (PNNL) s Marine Sciences Laboratory (MSL) has been serving as a marine test site for determining performance characteristics (adsorption capacity, adsorption kinetics, and selectivity) of novel amidoxime-based polymeric adsorbents developed at Oak Ridge National Laboratory (ORNL) under natural seawater exposure conditions. This report describes the performance of three formulations (38H, AF1, AI8) of amidoxime-based polymeric adsorbent produced at ORNL in MSL s ambient seawater testing facility. The adsorbents were produced in two forms, fibrous material (40-100 mg samples) and braided material (5-10 g samples), exposed to natural seawater using flow-through columns and recirculating flumes. All three formulations demonstrated high 56 day uranium adsorption capacity (>3 gU/kg adsorbent). The AF1 formulation had the best uranium adsorption performance, with 56-day capacity of 3.9 g U/kg adsorbent, saturation capacity of 5.4 g U/kg adsorbent, and ~25 days half-saturation time. The two exposure methods, flow-through columns and flumes were demonstrated to produce similar performance results, providing confidence that the test methods were reliable, that scaling up from 10 s of mg quantities of exposure in flow-through columns to gram quantities in flumes produced similar results, and that the manufacturing process produces a homogenous adsorbent. Adsorption kinetics appear to be element specific, with half-saturation times ranging from minutes for the major cations in seawater to 8-10weeks for V and Fe. Reducing the exposure time provides a potential pathway to improve the adsorption capacity of U by reducing the V/U ratio on the adsorbent.

  20. Characterization and Testing of Amidoxime-Based Adsorbent Materials to Extract Uranium from Natural Seawater

    SciTech Connect

    Kuo, Li-Jung; Janke, Christopher J.; Wood, Jordana R.; Strivens, Jonathan E.; Das, Sadananda; Oyola, Yatsandra; Mayes, Richard T.; Gill, Gary A.

    2016-04-20

    Extraction of uranium (U) from seawater for use as a nuclear fuel is a significant challenge due to the low concentration of U in seawater (~3.3 ppb) and difficulties to selectively extract U from the background of major and trace elements in seawater. The Pacific Northwest National Laboratory (PNNL)’s Marine Sciences Laboratory (MSL) has been serving as a marine test site for determining performance characteristics (adsorption capacity, adsorption kinetics, and selectivity) of novel amidoxime-based polymeric adsorbents developed at Oak Ridge National Laboratory (ORNL) under natural seawater exposure conditions. This manuscript describes the performance of three formulations (38H, AF1, AI8) of amidoxime-based polymeric adsorbents produced at ORNL in MSL’s ambient seawater testing facility. The adsorbents were produced in two forms, fibrous material (40-100 mg samples) and braided material (5-10 g samples), and exposed to natural seawater using flow-through columns and recirculating flumes. All three formulations demonstrated high 56 day uranium adsorption capacity (>3 g U/kg adsorbent). The AF1 formulation had the best uranium adsorption performance, with a 56 day capacity of 3.9 g U/ kg adsorbent, a saturation capacity of 5.4 g U/kg adsorbent, and ~25 days half-saturation time. The two exposure methods, flowthrough columns and flumes, were demonstrated to produce similar performance results, providing confidence that the test methods were reliable, that scaling up from 10’s of mg quantities of exposure in flow-through columns to gram quantities in flumes produced similar results, and confirm that the manufacturing process produces a homogeneous adsorbent. Adsorption kinetics appear to be element specific, with half-saturation times ranging from minutes for the major cations in seawater, to 8-10 weeks for V and Fe. Reducing the exposure time provides a potential pathway to improve the adsorption capacity of U by reducing the V/U ratio on the adsorbent.

  1. Testing sequential extraction methods for the analysis of multiple stable isotope systems from a bone sample

    NASA Astrophysics Data System (ADS)

    Sahlstedt, Elina; Arppe, Laura

    2017-04-01

    Stable isotope composition of bones, analysed either from the mineral phase (hydroxyapatite) or from the organic phase (mainly collagen) carry important climatological and ecological information and are therefore widely used in paleontological and archaeological research. For the analysis of the stable isotope compositions, both of the phases, hydroxyapatite and collagen, have their more or less well established separation and analytical techniques. Recent development in IRMS and wet chemical extraction methods have facilitated the analysis of very small bone fractions (500 μg or less starting material) for PO43-O isotope composition. However, the uniqueness and (pre-) historical value of each archaeological and paleontological finding lead to preciously little material available for stable isotope analyses, encouraging further development of microanalytical methods for the use of stable isotope analyses. Here we present the first results in developing extraction methods for combining collagen C- and N-isotope analyses to PO43-O-isotope analyses from a single bone sample fraction. We tested sequential extraction starting with dilute acid demineralization and collection of both collagen and PO43-fractions, followed by further purification step by H2O2 (PO43-fraction). First results show that bone sample separates as small as 2 mg may be analysed for their δ15N, δ13C and δ18OPO4 values. The method may be incorporated in detailed investigation of sequentially developing skeletal material such as teeth, potentially allowing for the investigation of interannual variability in climatological/environmental signals or investigation of the early life history of an individual.

  2. Accelerated separation of GC-amenable lipid classes in plant oils by countercurrent chromatography in the co-current mode.

    PubMed

    Hammann, Simon; Englert, Michael; Müller, Marco; Vetter, Walter

    2015-12-01

    Triacylglycerols represent the major part (>90%) in most plant oils and have to be eliminated, when the minor compounds such as phytosterols or tocopherols should be analyzed. Here, we used an all liquid-liquid chromatographic technique, countercurrent chromatography (CCC), to fractionate the minor lipids before gas chromatography (GC) analysis. To cover the wide range of polarity of the minor compounds, we used the co-current mode, in which both mobile and stationary phase are pumped through the system. This allowed to elute substances which partitioned almost exclusively in the stationary phase within 90 min. After testing with standard compounds, the method was applied to the separation of sesame oil and sunflower oil samples. The abundant triacylglycerols could be effectively separated from tocopherols, phytosterols, diacylglycerols, and free fatty acids in the samples, and these compounds could be analyzed (after trimethylsilylation) by GC coupled with mass spectrometry. After the enrichment caused by the CCC fractionation, we were also able to identify the tocopherol derivative α-tocomonoenol, which had not been described in sunflower oil before. Also, separation of sesame oil yielded a mixture of the polar compounds sesamin and sesamolin without further impurities.

  3. Separation and purification of two taxanes and one xylosyl-containing taxane from Taxus wallichiana Zucc.: A comparison between high-speed countercurrent chromatography and reversed-phase flash chromatography.

    PubMed

    Tao, Junfei; Yan, Rongwei; Zhao, Leilei; Wang, Dongmei; Xu, Xinjun

    2017-03-01

    10-Deacetylbaccatin III, an important semisynthetic precursor of paclitaxel and docetaxel, can be extracted from Taxus wallichiana Zucc. A process for the isolation and purification of 10-deacetylbaccatin III (1), baccatin III (2), and 7β-xylosyl-10-deacetyltaxol (3) from the leaves and branches of Taxus wallichiana Zucc. via macroporous resin column chromatography combined with high-speed countercurrent chromatography or reversed-phase flash chromatography was developed in this study. After fractionation by macroporous resin column chromatography, 80% methanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis. A solvent system composed of n-hexane, ethyl acetate, methanol, and water (1.6:2.5:1.6:2.5, v/v/v/v) was used for the high-speed countercurrent chromatography separation at a flow rate of 2.5 mL/min. The reversed-phase flash chromatography separation was performed using methanol/water as the mobile phase at a flow rate of 3 mL/min. The high-speed countercurrent chromatography separation produced compounds 1 (10.2 mg, 94.4%), 2 (2.1 mg, 98.0%), and 3 (4.6 mg, 98.8%) from 100 mg of sample within 110 min, while the reversed-phase flash chromatography separation purified compounds 1 (9.8 mg, 95.6%) and 3 (4.9 mg, 97.9%) from 100 mg of sample within 120 min. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Genotoxic effect of Lythrum salicaria extract determined by the mussel micronucleus test.

    PubMed

    Eck-Varanka, Bettina; Kováts, Nóra; Hubai, Katalin; Paulovits, Gábor; Ferincz, Árpád; Horváth, Eszter

    2015-12-01

    A wide range of aquatic plants have been proven to release allelochemicals, of them phenolics and tannin are considered rather widely distributed. Tannins, however, have been demonstrated to have genotoxic capacity. In our study genotoxic potential of Lythrum salicaria L. (Purple Loosestrife, family Lythraceae) was assessed by the mussel micronucleus test, using Unio pictorum. In parallel, total and hydrolysable tannin contents were determined. Results clearly show that the extract had a high hydrolysable tannin content and significant mutagenic effect. As L. salicaria has been long used in traditional medicine for chronic diarrhoea, dysentery, leucorrhoea and blood-spitting, genotoxic potential of the plant should be evaluated not only with regard to potential effects in the aquatic ecosystem, but also assessing its safe use as a medicinal herb.

  5. Assessment of the embryotoxicity of four Chinese herbal extracts using the embryonic stem cell test.

    PubMed

    Li, Lin-Yan; Cao, Fen-Fang; Su, Zhi-Jian; Zhang, Qi-Hao; Dai, Xiao-Yong; Xiao, Xue; Huang, Ya-Dong; Zheng, Qing; Xu, Hua

    2015-08-01

    Rhizoma Atractylodes macrocephala, Radix Isatidis, Coptis chinensis and Flos Genkwa are common herbal remedies used by pregnant woman in China. In this study, their potential embryotoxicity was assessed using the embryonic stem cell test (EST) and a prediction model. The potential embryotoxicity of the herbs was based on three endpoints: the concentrations of the compounds that inhibited the proliferation of 50% of embryonic stem cells (ESCs) (IC50ES), the concentrations that inhibited 50% of 3T3 cells (IC503T3), and the concentrations that inhibited the differentiation of 50% of ESCs (ID50ES). The results revealed that Rhizoma Atractylodes macrocephala and Radix Isatidis are non-embryotoxic compounds. Coptis chinensis extracts appeared to demonstrated weak embryotoxicity, and Flos Genkwa exhibited strong embryotoxicity. These results may be useful in guiding the clinical use of these herbs and in expanding the application of the EST to the field of traditional Chinese medicine.

  6. Decreased oxygen extraction during cardiopulmonary exercise test in patients with chronic fatigue syndrome

    PubMed Central

    2014-01-01

    Background The insufficient metabolic adaptation to exercise in Chronic Fatigue Syndrome (CFS) is still being debated and poorly understood. Methods We analysed the cardiopulmonary exercise tests of CFS patients, idiopathic chronic fatigue (CFI) patients and healthy visitors. Continuous non-invasive measurement of the cardiac output by Nexfin® (BMEYE B.V. Amsterdam, the Netherlands) was added to the cardiopulmonary exercise tests. The peak oxygen extraction by muscle cells and the increase of cardiac output relative to the increase of oxygen uptake (ΔQ’/ΔV’O2) were measured, calculated from the cardiac output and the oxygen uptake during incremental exercise. Results The peak oxygen extraction by muscle cells was 10.83 ± 2.80 ml/100ml in 178 CFS women, 11.62 ± 2.90 ml/100 ml in 172 CFI, and 13.45 ± 2.72 ml/100 ml in 11 healthy women (ANOVA: P=0.001), 13.66 ± 3.31 ml/100 ml in 25 CFS men, 14.63 ± 4.38 ml/100 ml in 51 CFI, and 19.52 ± 6.53 ml/100 ml in 7 healthy men (ANOVA: P=0.008). The ΔQ’/ΔV’O2 was > 6 L/L (normal ΔQ’/ΔV’O2 ≈ 5 L/L) in 70% of the patients and in 22% of the healthy group. Conclusion Low oxygen uptake by muscle cells causes exercise intolerance in a majority of CFS patients, indicating insufficient metabolic adaptation to incremental exercise. The high increase of the cardiac output relative to the increase of oxygen uptake argues against deconditioning as a cause for physical impairment in these patients. PMID:24456560

  7. Extraction-Separation Performance and Dynamic Modeling of Orion Test Vehicles with Adams Simulation: 2nd Edition

    NASA Technical Reports Server (NTRS)

    Fraire, Usbaldo, Jr.; Anderson, Keith; Varela, Jose G.; Bernatovich, Michael A.

    2015-01-01

    NASA's Orion Capsule Parachute Assembly System (CPAS) project has advanced into the third generation of its parachute test campaign and requires technically comprehensive modeling capabilities to simulate multi-body dynamics (MBD) of test articles released from a C-17. Safely extracting a 30,000 lbm mated test article from a C-17 and performing stable mid-air separation maneuvers requires an understanding of the interaction between elements in the test configuration and how they are influenced by extraction parachute performance, aircraft dynamics, aerodynamics, separation dynamics, and kinetic energy experienced by the system. During the real-time extraction and deployment sequences, these influences can be highly unsteady and difficult to bound. An avionics logic window based on time, pitch, and pitch rate is used to account for these effects and target a favorable separation state in real time. The Adams simulation has been employed to fine-tune this window, as well as predict and reconstruct the coupled dynamics of the Parachute Test Vehicle (PTV) and Cradle Platform Separation System (CPSS) from aircraft extraction through the mid-air separation event. The test-technique for the extraction of CPAS test articles has evolved with increased complexity and requires new modeling concepts to ensure the test article is delivered to a stable test condition for the programmer phase. Prompted by unexpected dynamics and hardware malfunctions in drop tests, these modeling improvements provide a more accurate loads prediction by incorporating a spring-damper line-model derived from the material properties. The qualification phase of CPAS testing is on the horizon and modeling increasingly complex test-techniques with Adams is vital to successfully qualify the Orion parachute system for human spaceflight.

  8. Mutagenicity and clastogenicity of extracts of Helicobacter pylori detected by the Ames test and in the micronucleus test using human lymphoblastoid cells.

    PubMed

    Arimoto-Kobayashi, Sakae; Ohta, Kaori; Yuhara, Yuta; Ayabe, Yuka; Negishi, Tomoe; Okamoto, Keinosuke; Nakajima, Yoshihiro; Ishikawa, Takeshi; Oguma, Keiji; Otsuka, Takanao

    2015-07-01

    Epidemiological studies have demonstrated a close association between infection with Helicobacter pylori (H.pylori) and the development of gastric carcinoma. Chronic H.pylori infection increases the frequency of mutation in gastric epithelial cells. However, the mechanism by which infection of H.pylori leads to mutation in gastric epithelial cells is unclear. We suspected that components in H.pylori may be related to the mutagenic response associated with DNA alkylation, and could be detected with the Ames test using a more sensitive strain for alkylating agents. Our investigation revealed that an extract of H.pylori was mutagenic in the Ames test with Salmonella typhimurium YG7108, which is deficient in the DNA repair of O(6)-methylguanine. The extract of H.pylori may contain methylating or alkylating agents, which might induce O (6)-alkylguanine in DNA. Mutagenicity of the alkylating agents N-methyl-N-nitrosourea (MNU) and N-methyl-N'-nitro-N-nitrosoguanidine in the Ames test with S.typhimurium TA1535 was enhanced significantly in the presence of the extract of H.pylori. The tested extracts of H.pylori resulted in a significant induction of micronuclei in human-derived lymphoblastoid cells. Heat instability and dialysis resistance of the extracts of H.pylori suggest that the mutagenic component in the extracts of H.pylori is a heat-unstable large molecule or a heat-labile small molecule strongly attached or adsorbed to a large molecule. Proteins in the extracts of H.pylori were subsequently fractionated using ammonium sulphate precipitation. However, all fractions expressed enhancing effects toward MNU mutagenicity. These results suggest the mutagenic component is a small molecule that is absorbed into proteins in the extract of H.pylori, which resist dialysis. Continuous and chronic exposure of gastric epithelial cells to the alkylative mutagenic component from H.pylori chronically infected in the stomach might be a causal factor in the gastric carcinogenesis

  9. Sensitivity testing of trypanosome detection by PCR from whole blood samples using manual and automated DNA extraction methods.

    PubMed

    Dunlop, J; Thompson, C K; Godfrey, S S; Thompson, R C A

    2014-11-01

    Automated extraction of DNA for testing of laboratory samples is an attractive alternative to labour-intensive manual methods when higher throughput is required. However, it is important to maintain the maximum detection sensitivity possible to reduce the occurrence of type II errors (false negatives; failure to detect the target when it is present), especially in the biomedical field, where PCR is used for diagnosis. We used blood infected with known concentrations of Trypanosoma copemani to test the impact of analysis techniques on trypanosome detection sensitivity by PCR. We compared combinations of a manual and an automated DNA extraction method and two different PCR primer sets to investigate the impact of each on detection levels. Both extraction techniques and specificity of primer sets had a significant impact on detection sensitivity. Samples extracted using the same DNA extraction technique performed substantially differently for each of the separate primer sets. Type I errors (false positives; detection of the target when it is not present), produced by contaminants, were avoided with both extraction methods. This study highlights the importance of testing laboratory techniques with known samples to optimise accuracy of test results.

  10. Continuing assessment of the 5 day sodium carbonate-ammonium nitrate extraction assay as an indicator test for silicon fertilizers

    USDA-ARS?s Scientific Manuscript database

    The five day sodium carbonate-ammonium nitrate extraction assay has been proposed by the AAFPCO as a standard test to identify fertilizers that provide plant-available Si. A single-lab validation test was previously performed; however, the analysis lacked any correlation to a grow-out study. To do...

  11. Isolation of β-carotene, α-carotene and lutein from carrots by countercurrent chromatography with the solvent system modifier benzotrifluoride.

    PubMed

    Englert, Michael; Hammann, Simon; Vetter, Walter

    2015-04-03

    A carotenoid purification method with dual-mode countercurrent chromatography (CCC) for β-carotene, α-carotene and lutein from a fresh carrot extract was developed. The fluorinated liquid benzotrifluoride (IUPAC name: (trifluoromethyl)benzene) was used as a novel modifier in the non-aqueous ternary solvent system n-hexane/benzotrifluoride/acetonitrile. The ternary phase diagram of the type I solvent system was used to select two-phase solvent mixtures which enabled an efficient preparative separation of α-carotene, β-carotene and lutein from concomitant pigments in crude carrot extract. By means of the modifier, high separation factors (α ≥ 1.2) were obtained, allowing baseline resolution between α-carotene and β-carotene due to specific chemical interactions such as π-π molecular interactions. After optimizing the injection step with a pseudo-ternary phase diagram, 51 mg of β-carotene, 32 mg of α-carotene and 4 mg of lutein could be isolated from 100.2mg crude carrot extract in a short time and with high purities of 95% and 99% by using dual-mode CCC, respectively. Temperatures > 22°C had a negative impact on the separation of α-carotene and β-carotene. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Isolation of anti-tumor compounds from the stem bark of Zanthoxylum ailanthoides Sieb. & Zucc. by silica gel column and counter-current chromatography.

    PubMed

    Cao, Xue-Li; Xu, Jing; Bai, Ge; Zhang, Hong; Liu, Yan; Xiang, Jun-Feng; Tang, Ya-Lin

    2013-06-15

    Silica gel column chromatography combined with high performance counter-current chromatography (HPCCC) was employed for the separation of potential anti-tumor compounds from a petroleum ether fraction of a crude extract of Zanthoxylum ailanthoides Sieb. & Zucc. This traditional Chinese medicine was recently found to display high inhibitory activity against A-549 human cancer cells in vitro and Lewis lung cancer in vivo. A 75% aqueous ethanol extract of the stem bark of Z. ailanthoides was fractionated with petroleum ether, ethyl acetate and n-butanol. In this paper, the petroleum ether fraction was pre-separated by silica gel column chromatography with a petroleum ether-ethyl acetate gradient. Two fractions were further separated and purified by HPCCC using n-hexane-ethyl acetate-methanol-water (3:1:2:1, v/v) and petroleum-ethyl acetate-methanol-water (8:6:7:7, v/v). Finally, coumarins and lignans including luvangetin, xanthyletin, hinokinin and asarinin were isolated and identified by MS, (1)H and (13)C NMR. In total, 56mg of xanthyletin (1), 140mg of hinokinin (2), 850mg of luvangetin (3) and 74mg of asarinin (4) were obtained from approximately 50g of petroleum ether extract, in 96.0%, 94.0%, 99.0% and 94.0% purity, respectively, as determined by HPLC. The separation method proved to be efficient, especially for those minor components. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Preparative Isolation of 5 Antioxidant Constituents from the Medicinal Mushroom Phellinus baumii (Agaricomycetes) by High-Speed Countercurrent Chromatography and Preparative High-Performance Liquid Chromatography.

    PubMed

    Ye, Libin; Zheng, Hongjian; Zhang, Zhong; Yang, Yan

    2017-01-01

    Four extract fractions from the fruiting bodies of Phellinus baumii were acquired. Preliminary investigation of radical scavenging ability showed that the ethyl acetate extract exhibited the strongest antioxidant activity. To gain insight into the antioxidant mechanism, 5 antioxidant constituents were prepared from the ethyl acetate extract using high-speed countercurrent chromatography with a solvent system consisting of n-hexane, ethyl acetate, methanol, and water (0.8:3:1.5:2.5, v/v/v/v), and preparative high-performance liquid chromatography. Electrospray ionization mass spectrometry and nuclear magnetic resonance spectra were used to analyze the structures of these compounds and revealed that they were caffeic acid (compound 1), inoscavin A (compound 2), 3,4-dihydroxy benzaldehyde (compound 3), coumarin (compound 4), and naringenin (compound 5). Compound 2 showed strong antioxidant activity, and compounds 1, 3, and 5 showed moderate antioxidant activity. Thus, a more clearly and usefully scientific background is provided herein for the development of relative functional foods or biomedical products using Ph. baumii as the raw material.

  14. Neptunium - Uranium - Plutonium Co-Extraction in TBP-based Solvent Extraction Processes for Spent Nuclear Fuel Recycling

    SciTech Connect

    Arm, S.T.; Abrefah, J.; Lumetta, G.J.; Sinkov, S.I.

    2007-07-01

    The US, through the Global Nuclear Energy Partnership, is currently engaged in efforts aimed at closing the nuclear fuel cycle. Neptunium behavior is important to understand for transuranic recycling because of its complex oxidation chemistry. The Pacific Northwest National Laboratory is investigating neptunium oxidation chemistry in the context of the PUREX process. Neptunium extraction in the PUREX process relies on maintaining either IV or V oxidation states. Qualitative conversion of neptunium(V) to neptunium(VI) was achieved within 5 hours in 6 M nitric acid at 95 deg. C. However, the VI state was not maintained during a batch contact test simulating the PUREX process and neptunium reduced to the V state, rendering it inextractable. Vanadium(V) was found to be effective in maintaining neptunium(VI) by adding it to a simulated irradiated nuclear fuel feed in 6 M nitric acid and to the scrub acid in the batch contact simulation of the PUREX process. Computer simulations of the PUREX process with a typical irradiated nuclear fuel in 6 M nitric acid as feed indicated little impact of the higher acid concentration on the behavior of fission products of moderate extractability. We plan to perform countercurrent tests of this modified PUREX process in the near future. (authors)

  15. Online-storage recycling counter-current chromatography for preparative isolation of naphthaquinones from Arnebia euchroma (Royle) Johnst.

    PubMed

    He, Jian-Ming; Zhang, Shi-Yue; Mu, Qing

    2016-09-16

    Counter-current Chromatography (CCC) has gradually become a popular method for preparative separation, especially in natural product isolation. As an effective separation method, one-dimensional (1D) CCC often results in insufficiently resolved peaks, due to limitations in the separation efficiency and peak capacity in an equipment. Therefore, two dimensional (2D)/multi-dimensional (multi-D) CCC strategies with recycling elution mode were developed to achieve successful separation of target compounds. However, the reported 2D or multi-D CCC approaches lead to experimental costs, complicated procedures, higher requirements for equipment, and increased time consumption. In this study, an online-storage recycling (OSR) CCC strategy was designed to achieve sequential recycling elution for multi-fractions of effluent in non-stop separation with single instrument using three 6-port valves and two storage loops, which would be realized by introducing 2D or multi-D CCC method before. In this non-stop separation system, the fraction C of effluent was subjected to recycling separation while the other fractions (A and B) were storing online, following which these two fractions were subjected to subsequent recycling separations in order, after the completion of the previous recycling elution. Then, six natural occurring naphthaquinone analogues, namely, shikonin (1), propionylshikonin (2), deoxyshikonin (3), isobutyrylshikonin (4), β, β-dimethylacrylshikonin (5) and isovalerylshikonin (6), were isolated from the crude extract of Arnebia euchroma in single run. The purities of all compounds were > 95.0% as determined by HPLC, and their structures were determined by means of UV, MS, (1)H NMR, (13)C NMR, and optical rotatory dispersion (ORD).

  16. Efficient counter-current chromatographic isolation and structural identification of two new cinnamic acids from Echinacea purpurea.

    PubMed

    Lu, Ying; Li, JiaYin; Li, MiLu; Hu, Xia; Tan, Jun; Liu, Zhong Hua

    2012-10-01

    Two new cinnamic acids, 2-O-caffeoyl-3-O-isoferuloyltartaric (3), and 2, 3-di-O-isoferuloyltartaric acid (5), along with three known caffeic acids, cichoric acid (1), 2-O-caffeoyl-3-O-feruloyltartaric acid (2) and 2-O-caffeoyl-3-O-p-coumaroyltartaric acid (4), have been successfully isolated and purified from Echinacea purpurea. In this study, we investigated an efficient method for the preparative isolation and purification of cinnamic acids from E. purpurea by high-speed counter-current chromatography (HSCCC). The separation was performed using a two-phase solvent composed of n-hexane-ethyl-acetate-methanol-0.5% aqueous acetic acid (1:3:1:4, v/v). The upper phase was used as the stationary phase and the lower phase as the mobile phase, with a flow rate of 1.6 mL/min. From 250 mg of crude extracts, 65.1 mg of 1, 8.3 mg of 2, 4.0 mg of 3, 4.5 mg of 4, and 4.3 mg of 5 were isolated in one-step, with purities of 98.5%, 97.7%, 94.6%, 94.3%, and 98.6%, respectively, as evaluated by HPLC-DAD. The chemical structures were identified by electro spray ionization mass spectrometry (ESI-MS) and one- and two-dimensional NMR spectra. HSCCC was very efficient for the separation and purification of the cinnamic acids from

  17. Skin tests and histamine release with P1-depleted Dermatophagoides pteronyssinus body extracts and purified P1.

    PubMed

    van der Zee, J S; van Swieten, P; Jansen, H M; Aalberse, R C

    1988-05-01

    Monoclonal antibodies were raised against P1 and Dp X, two major allergens in Dermatophagoides pteronyssinus extracts. The concentrations of IgE antibodies to P1 and Dp X in sera of mite-sensitive patients were determined in RAST with immunosorbent-bound monoclonal antibodies used for insolubilization of the allergens. The major allergen-specific IgE titers were compared with the total IgE response against D. pteronyssinus. The results of these serologic assays confirmed studies in the literature that P1 and Dp X are major allergens. The contribution of IgE anti-P1 to the total antimite response frequently exceeded 50% and, in general, appeared to be higher than the contribution of IgE anti-Dp X. Twenty percent of the mite-sensitive patients had no detectable IgE to either P1 or Dp X. The contribution of P1 to the biologic activity of D. pteronyssinus body extracts was derived from the effect of P1 depletion on the reactivity in the histamine-release test and skin test. This technique was preferred to the study of purified allergen because biologic activity of the nonabsorbed components is not affected. Immunization of rabbits with affinity-purified P1 yielded monospecific polyclonal antisera. Mite extracts depleted with either monoclonal or polyclonal anti-P1 were applied in the histamine-release test. The skin test was performed with extracts depleted with polyclonal anti-P1. In addition, the activity of affinity-purified P1 was investigated in these tests. The results indicated that P1 depletion of D. pteronyssinus body extracts had no detectable effect on the activity in most patients, namely, at least 70% of the activity was retained in the depleted extract. There was a considerable variation between patients in the sensitivity for purified P1, as compared to the sensitivity for whole D. pteronyssinus extracts. In the histamine-release test, the activity of purified P1 was up to 35% of the activity of the D. pteronyssinus body extract but did not exceed 10% in

  18. 2,2-diphenyl-1-picrylhydrazyl (DPPH*) test demonstrates antiradical activity of Dorstenia psilurus and Dorstenia ciliata plant extracts.

    PubMed

    Kansci, Germain; Dongo, Etienne; Genot, Claude

    2003-12-01

    Plants of the Dorstenia genus, used in traditional medicine and as food ingredient in Africa, are rich in polyphenolic compounds which can be involved in prevention of disease and food spoilage through their antioxidant activity. The antiradical activities of extracts of Dorstenia psilurus. D. ciliata and a phenolic compound (6-prenylapigenin) from D. ciliata were evaluated with the 2,2-diphenyl-1-picrylhydrazyl (DPPH*) test. D. psilurus chloroform and D. ciliata ethyl acetate extracts were shown to exhibit antiradical activities, with slow kinetic action. The efficient concentrations at different kinetic times "EC50,t" for the D. ciliata extract: 699, 479, 311 and 251 g/kg after 30, 60, 120 and 180 min, respectively, were always much lower than for the D. psilurus extract: 2341, 2312, 1672 and 1281 g/kg at the same times. The antiradical activity of 6-prenylapigenin was weak compared to the extracts. These results suggest the antioxidant activities of Dorstenia extracts and might help to understand their traditional use. We propose "EC50, t", calculated on the curves obtained with DPPH test, as a parameter to screen and compare antiradical activities of plant extracts with slow kinetic behaviour.

  19. Characterization and testing of amidoxime-based adsorbent materials to extract uranium from natural seawater

    DOE PAGES

    Kuo, Li-Jung; Janke, Christopher James; Wood, Jordana; ...

    2015-11-19

    Extraction of uranium (U) from seawater for use as a nuclear fuel is a significant challenge due to the low concentration of U in seawater (~3.3 ppb) and difficulties to selectively extract U from the background of major and trace elements in seawater. The Pacific Northwest National Laboratory (PNNL) s Marine Sciences Laboratory (MSL) has been serving as a marine test site for determining performance characteristics (adsorption capacity, adsorption kinetics, and selectivity) of novel amidoxime-based polymeric adsorbents developed at Oak Ridge National Laboratory (ORNL) under natural seawater exposure conditions. This report describes the performance of three formulations (38H, AF1, AI8)more » of amidoxime-based polymeric adsorbent produced at ORNL in MSL s ambient seawater testing facility. The adsorbents were produced in two forms, fibrous material (40-100 mg samples) and braided material (5-10 g samples), exposed to natural seawater using flow-through columns and recirculating flumes. All three formulations demonstrated high 56 day uranium adsorption capacity (>3 gU/kg adsorbent). The AF1 formulation had the best uranium adsorption performance, with 56-day capacity of 3.9 g U/kg adsorbent, saturation capacity of 5.4 g U/kg adsorbent, and ~25 days half-saturation time. The two exposure methods, flow-through columns and flumes were demonstrated to produce similar performance results, providing confidence that the test methods were reliable, that scaling up from 10 s of mg quantities of exposure in flow-through columns to gram quantities in flumes produced similar results, and that the manufacturing process produces a homogenous adsorbent. Adsorption kinetics appear to be element specific, with half-saturation times ranging from minutes for the major cations in seawater to 8-10weeks for V and Fe. Reducing the exposure time provides a potential pathway to improve the adsorption capacity of U by reducing the V/U ratio on the adsorbent.« less

  20. Testing the ‘microbubble effect’ using the Cavitron technique to measure xylem water extraction curves

    PubMed Central

    Pivovaroff, Alexandria L.; Burlett, Régis; Lavigne, Bruno; Cochard, Hervé; Santiago, Louis S.; Delzon, Sylvain

    2016-01-01

    Plant resistance to xylem cavitation is a major drought adaptation trait and is essential to characterizing vulnerability to climate change. Cavitation resistance can be determined with vulnerability curves. In the past decade, new techniques have increased the ease and speed at which vulnerability curves are produced. However, these new techniques are also subject to new artefacts, especially as related to long-vesselled species. We tested the reliability of the ‘flow rotor’ centrifuge technique, the so-called Cavitron, and investigated one potential mechanism behind the open vessel artefact in centrifuge-based vulnerability curves: the microbubble effect. The microbubble effect hypothesizes that microbubbles introduced to open vessels, either through sample flushing or injection of solution, travel by buoyancy or mass flow towards the axis of rotation where they artefactually nucleate cavitation. To test the microbubble effect, we constructed vulnerability curves using three different rotor sizes for five species with varying maximum vessel length, as well as water extraction curves that are constructed without injection of solution into the rotor. We found that the Cavitron technique is robust to measure resistance to cavitation in tracheid-bearing and short-vesselled species, but not for long-vesselled ones. Moreover, our results support the microbubble effect hypothesis as the major cause for the open vessel artefact in long-vesselled species. PMID:26903487

  1. Field test of single well DNAPL characterization using alcohol injection/extraction

    SciTech Connect

    Jerome, K.M.; Looney, B.B.; Rhoden, M.L.; Riha, B.; Burdick, S.

    1996-10-29

    Soils and groundwater beneath an abandoned process sewer line in the A/M Area of the Savannah River Site (SRS) contain elevated levels of volatile organic compounds, specifically trichloroethylene (TCE) and tetrachloroethylene (PCE), two common chlorinated solvents. These compounds have low aqueous solubilities, thus when released to the subsurface in sufficient quantity, tend to exist as immiscible fluids or nonaqueous phase liquids (NAPLs). Because chlorinated solvents are also denser than water, they are referred to by the acronym DNAPLs, or dense non-aqueous phase liquids. Technologies targeted at efficient characterization or removal of DNAPL are not currently proven. The authors performed injection/extraction characterization tests in six existing wells in A/M Area. Water concentrations for TCE and/or PCE in these wells ranged from 0% to 100% of solubility. For each test, small amounts of solubilizing solution were used to try to confirm or deny the presence or absence of DNAPL in the immediate vicinity of the well screen.

  2. Basic Test Framework for the Evaluation of Text Line Segmentation and Text Parameter Extraction

    PubMed Central

    Brodić, Darko; Milivojević, Dragan R.; Milivojević, Zoran

    2010-01-01

    Text line segmentation is an essential stage in off-line optical character recognition (OCR) systems. It is a key because inaccurately segmented text lines will lead to OCR failure. Text line segmentation of handwritten documents is a complex and diverse problem, complicated by the nature of handwriting. Hence, text line segmentation is a leading challenge in handwritten document image processing. Due to inconsistencies in measurement and evaluation of text segmentation algorithm quality, some basic set of measurement methods is required. Currently, there is no commonly accepted one and all algorithm evaluation is custom oriented. In this paper, a basic test framework for the evaluation of text feature extraction algorithms is proposed. This test framework consists of a few experiments primarily linked to text line segmentation, skew rate and reference text line evaluation. Although they are mutually independent, the results obtained are strongly cross linked. In the end, its suitability for different types of letters and languages as well as its adaptability are its main advantages. Thus, the paper presents an efficient evaluation method for text analysis algorithms. PMID:22399932

  3. Testing the 'microbubble effect' using the Cavitron technique to measure xylem water extraction curves.

    PubMed

    Pivovaroff, Alexandria L; Burlett, Régis; Lavigne, Bruno; Cochard, Hervé; Santiago, Louis S; Delzon, Sylvain

    2016-01-01

    Plant resistance to xylem cavitation is a major drought adaptation trait and is essential to characterizing vulnerability to climate change. Cavitation resistance can be determined with vulnerability curves. In the past decade, new techniques have increased the ease and speed at which vulnerability curves are produced. However, these new techniques are also subject to new artefacts, especially as related to long-vesselled species. We tested the reliability of the 'flow rotor' centrifuge technique, the so-called Cavitron, and investigated one potential mechanism behind the open vessel artefact in centrifuge-based vulnerability curves: the microbubble effect. The microbubble effect hypothesizes that microbubbles introduced to open vessels, either through sample flushing or injection of solution, travel by buoyancy or mass flow towards the axis of rotation where they artefactually nucleate cavitation. To test the microbubble effect, we constructed vulnerability curves using three different rotor sizes for five species with varying maximum vessel length, as well as water extraction curves that are constructed without injection of solution into the rotor. We found that the Cavitron technique is robust to measure resistance to cavitation in tracheid-bearing and short-vesselled species, but not for long-vesselled ones. Moreover, our results support the microbubble effect hypothesis as the major cause for the open vessel artefact in long-vesselled species.

  4. Antidepressant-Like Effects of Lindera obtusiloba Extracts on the Immobility Behavior of Rats in the Forced Swim Test.

    PubMed

    Lim, Dong Wook; Lee, Mi-Sook; Her, Song; Cho, Suengmok; Lee, Chang-Ho; Kim, In-Ho; Han, Daeseok

    2016-02-27

    Lindera obtusiloba extracts are commonly used as an alternative medicine due to its numerous health benefits in Korea. However, the antidepressant-like effects of L. obtusiloba extracts have not been fully elucidated. In this study, we aimed to determine whether L. obtusiloba extracts exhibited antidepressant-like activity in rats subjected to forced swim test (FST)-induced depression. Acute treatment of rats with L. obtusiloba extracts (200 mg/kg, p.o.) significantly reduced immobility time and increased swimming time without any significant change in climbing. Rats treated with L. obtusiloba extracts also exhibited a decrease in the limbic hypothalamic-pituitary-adrenal (HPA) axis response to the FST, as indicated by attenuation of the corticosterone response and decreased c-Fos immunoreactivity in the hippocampus CA3 region. In addition, L. obtusiloba extracts, at concentrations that were not affected by cell viability, significantly decreased luciferase activity in response to cortisol in a concentration-dependent manner by the glucocorticoid binding assay in HeLa cells. Our findings suggested that the antidepressant-like effects of L. obtusiloba extracts were likely mediated via the glucocorticoid receptor (GR). Further studies are needed to evaluate the potential of L. obtusiloba extracts as an alternative therapeutic approach for the treatment of depression.

  5. Two-Step Purification of Cordycepin from Cordyceps Millitaris by High-Speed Countercurrent Chromatography

    PubMed Central

    Ju, Xiuyun; Sun, Yong; Cao, Xiaoying; Jiang, Jihong; Zhang, Tianyou; Ito, Yoichiro

    2009-01-01

    Cordycepin is successfully isolated and purified from Cordyceps millitaris in two-step purification by high-speed countercurrent chromatography. Two solvent systems, ethyl acetate–1-butanol–water (3:2:5, v/v/v) and trichloromethane–methanol–1-butanol–water (2:1:0.25:1, v/v/v/v), were used for the two-step purification. The purity of the prepared cordycepin was 98.1% according to the high-performance liquid chromatography analysis. PMID:20046921

  6. Modeling and separation of rare earth elements by countercurrent electromigration: A new separation column

    SciTech Connect

    Correa, S.M. |; Arbilla, G.; Carvalho, M.S.

    1998-07-01

    The separation of a samarium (90%) and europium (10%) mixture in {alpha}-hydroxy isobutyric acid was performed in a new countercurrent electromigration system. The mobilities of these elements were estimated, and samarium of better than 99.9% purity was obtained. The equilibrium of multicoordinate complexes of these elements with {alpha}-hydroxy isobutyric acid ({alpha}-HIBA) plays an important role in the separation process. The equilibrium concentrations of the involved species were calculated by a computational procedure, and a kinetic study of the complexation reaction was also performed.

  7. High-speed counter-current chromatographic isolation of ricinine, an insecticide from Ricinus communis.

    PubMed

    Cazal, Cristiane de Melo; Batalhão, Jaqueline Raquel; Domingues, Vanessa de Cássia; Bueno, Odair Corrêa; Filho, Edson Rodrigues; Forim, Moacir R; da Silva, Maria Fátima G Fernandes; Vieira, Paulo Cezar; Fernandes, João Batista

    2009-05-08

    The alkaloid ricinine, an insecticide for leaf-cutting ant (Atta sexdens rubropilosa), was obtained from Ricinus communis. A two-phase solvent system composed of CH(2)Cl(2)/EtOH/H(2)O (93:35:72, v/v/v) was used for high-speed counter-current chromatographic (HSCCC) isolation of ricinine in high yield and with over 96% purity, as determined by liquid and gas chromatography-mass spectrometry (LC-MS and GC-MS). Identification of ricinine was performed by comparison of (1)H NMR, (13)C NMR and LC-MS/MS data.

  8. Preparation and testing of E. coli S30 in vitro transcription translation extracts.

    PubMed

    Zawada, James F

    2012-01-01

    Crude cell-free extracts are useful tools for investigating biochemical phenomena and exploiting complex enzymatic processes such as protein synthesis. Extracts derived from E. coli have been used for over 50 years to study the mechanism of protein synthesis. In addition, these S30 extracts are commonly used as a laboratory tool for protein production. The preparation of S30 extract has been streamlined over the years and now it is a relatively simple process. The procedure described here includes some suggestions for extracts to be used for ribosome display.

  9. Allium cepa chromosome aberration and micronucleus tests applied to study genotoxicity of extracts from pesticide-treated vegetables and grapes.

    PubMed

    Feretti, D; Zerbini, I; Zani, C; Ceretti, E; Moretti, M; Monarca, S

    2007-06-01

    The Allium cepa assay is an efficient test for chemical screening and in situ monitoring for genotoxicity of environmental contaminants. The test has been used widely to study genotoxicity of many pesticides revealing that these compounds can induce chromosomal aberrations in root meristems of A. cepa. Pesticide residues can be present in fruit and vegetables and represent a risk for human health. The mutagenic and carcinogenic action of herbicides, insecticides and fungicides on experimental animals is well known. Several studies have shown that chronic exposure to low levels of pesticides can cause birth defects and that prenatal exposure is associated with carcinogenicity. This study evaluated the potential application of plant genotoxicity tests for monitoring mutagens in edible vegetables. The presence of pesticides and genotoxic compounds extracted from 21 treated vegetables and eight types of grapes sampled from several markets in Campania, a region in Southern Italy, was monitored concurrently. The extracts were analysed for pesticides by gas chromatography and high-performance liquid chromatography, and for genotoxicity using two plant tests: the micronucleus test and the chromosomal aberration test in A. cepa roots. Thirty-three pesticides were detected, some of which are not approved. Genotoxicity was found in some of the vegetables and grapes tested. Allium cepa tests proved to be sensitive in monitoring genotoxicity in food extracts. The micronucleus test in interphase cells gave a much higher mutagenicity than the chromosomal aberration test in anaphase-telophase cells.

  10. [Preliminary screening tests of molluscicidal effect of extracts from Eucalyptus leaves].

    PubMed

    Chen, Ting-Ting; Zhou, Xiao-Nong; Zhu, Dan; Li, Ming-Ya

    2012-12-01

    To investigate the molluscicidal effects of extracts from five Eucalyptus leaves collected from Guangdong Province, China. According to the WHO recommended indoor immersed method, the molluscicidal effects of extracts from five Eucalyptus leaves with 250, 100, 10 mg/L of water extraction, alcohol precipitation and organic solvent extraction were investigated. The dose-effect relationship showed that all the mortality rates of Oncomelania hupensis reached 80% with the volatile oil from five Eucalyptus leaves immersed at the concentrations of 100 mg/L for 48 h, and the mortality rates were both 93.3% with the volatile oil from Corymbia citriodora and Eucalyptus urophylla leaves. The mortality rate was up to 95% with the chloroform extract, and the mortality rate reached 60% at the concentrations of 10 mg/L for 48 h. The volatile oils from five Eucalyptus leaves and the chloroform extract in alcohol extraction from Eucalyptus urophylla leaves are better than other solvents.

  11. SOLVENT EXTRACTION PROCESS FOR SEPARATING ACTINIDE AND LANTHANIDE METAL VALUES

    DOEpatents

    Hildebrandt, R.A.; Hyman, H.H.; Vogler, S.

    1962-08-14

    A process of countercurrently extracting an aqueous mineral acid feed solution for the separation of actinides from lanthanides dissolved therern is described. The feed solution is made acid-defrcient with alkali metal hydroxide prior to.contact with acid extractant; during extraction, however, acid is transferred from organic to aqueous solution and the aqueous solution gradually becomes acid. The acid-deficient phase ' of the process promotes the extraction of the actinides, while the latter acid phase'' of the process improves retention of the lanthanides in the aqueous solution. This provides for an improved separation. (AEC)

  12. Mechanical Mercury Extraction Process® Test Results at Combie Reservoir

    NASA Astrophysics Data System (ADS)

    Monohan, C.; Alpers, C. N.; Marvin-DiPasquale, M. C.

    2016-12-01

    More than 4,500,000 kilograms (10,000,000 pounds) of mercury (Hg) were used during hydraulic and hard rock mining during the California Gold Rush era, and it is estimated that 10-30% of liquid Hg was lost to the environment. Mercury is entrained in river gravels containing hydraulic mining debris and is incorporated into the aquatic food chain, causing numerous environmental and public health problems for California communities today. One of the problems is that Hg-contaminated sediment accumulates in water-supply reservoirs such as the Combie Reservoir. Sand miners and irrigation districts have removed these accumulated materials for more than 30 years. The Combie Reservoir Sediment and Mercury Removal Project is to dredge Hg-contaminated sediment from Combie Reservoir while implementing an innovative recovery process to remove the free elemental Hg (Hg(0)) from the dredged material. The project is estimated to take 3 to 5 years to complete and would remove and treat an estimated 100,000 cubic meters (135,000 cubic yards) of sediment from the upstream end of Combie Reservoir. The dredged material will be processed with the Pegasus Mercury Extraction Process® which passes the material through a specialized centrifuge, thereby removing Hg(0) as well as other heavy minerals, including gold (Au) and Au-Hg amalgam. To measure the effectiveness of removal process, multiple equipment tests were conducted in September and October 2009. Total Hg (THg), methylmercury (MeHg) and reactive Hg(II) (operationally defined by reduction of divalent inorganic Hg(II) to Hg(0) with tin(II)) were measured in heads (input material) and tails (output material) from replicate closed system tests. Mass balances were calculated for water, sediment and the above forms of Hg to estimate Hg removal effectiveness in different grain-size fractions. The free Hg(0) in the sand size fraction (> 0.063 mm) that was removed by the Pegasus Mercury Extraction Process® represents approximately 93% of

  13. Testing single extraction methods and in vitro tests to assess the geochemical reactivity and human bioaccessibility of silver in urban soils amended with silver nanoparticles.

    PubMed

    Cruz, N; Rodrigues, S M; Tavares, D; Monteiro, R J R; Carvalho, L; Trindade, T; Duarte, A C; Pereira, E; Römkens, Paul F A M

    2015-09-01

    To assess if the geochemical reactivity and human bioaccessibility of silver nanoparticles (AgNPs) in soils can be determined by routine soil tests commonly applied to other metals in soil, colloidal Ag was introduced to five pots containing urban soils (equivalent to 6.8 mg Ag kg(-1) soil). Following a 45 days stabilization period, the geochemical reactivity was determined by extraction using 0.43 M and 2 M HNO3. The bioaccessibility of AgNPs was evaluated using the Simplified Bioaccessibility Extraction Test (SBET) the "Unified BARGE Method" (UBM), and two simulated lung fluids (modified Gamble's solution (MGS) and artificial lysosomal fluid (ALF)). The amount of Ag extracted by 0.43 M and 2 M HNO3 soil tests was <8% and <50%, respectively of the total amount of Ag added to soils suggesting that the reactivity of Ag present in the soil can be relatively low. The bioaccessibility of Ag as determined by the four in vitro tests ranged from 17% (ALF extraction) to 99% (SBET) indicating that almost all Ag can be released from soil due to specific interactions with the organic ligands present in the simulated body fluids. This study shows that to develop sound soil risk evaluations regarding soil contamination with AgNPs, aspects of Ag biochemistry need to be considered, particularly when linking commonly applied soil tests to human risk assessment.

  14. Preparative isolation of flavonoid compounds from Oroxylum indicum by high-speed counter-current chromatography by using ionic liquids as the modifier of two-phase solvent system.

    PubMed

    Liu, Renmin; Xu, Lili; Li, Aifeng; Sun, Ailing

    2010-04-01

    A preparative high-speed counter-current chromatography method for isolation and purification of flavonoid compounds from Oroxylum indicum was successfully established by using ionic liquids as the modifier of the two-phase solvent system. Two flavonoid compounds including baicalein-7-O-diglucoside and baicalein-7-O-glucoside were purified from the crude extract of O. indicum by using ethyl acetate-water-[C(4)mim][PF(6)] (5:5:0.2, v/v) as two-phase solvent system. 36.4 mg of baicalein-7-O-diglucoside and 60.5 mg of baicalein-7-O-glucoside were obtained from 120 mg of the crude extract. Their purities were 98.7 and 99.1%, respectively, as determined by HPLC area normalization method. The chemical structures of the isolated compounds were identified by (1)H-NMR and (13)C-NMR.

  15. Chemical analysis and biological testing of a polar fraction of ambient air, diesel engine, and gasoline engine particulate extracts.

    PubMed

    Strandell, M; Zakrisson, S; Alsberg, T; Westerholm, R; Winquist, L; Rannug, U

    1994-10-01

    Extracts of gasoline and diesel vehicle exhaust and ambient air particles were fractionated into five fractions according to polarity on a silica gel column. Two medium polar fractions showing high genotoxic activity in the Ames test were further subfractionated, using normal-phase high-performance liquid chromatography. Chemical analyses were performed by means of gas chromatography combined with mass spectrometry and flame ionization and detection. The crude extracts, fractions, and subfractions were assayed with the Ames test, with and without S9, and the most abundant compounds in the subfractions are reported.

  16. Chemical analysis and biological testing of a polar fraction of ambient air, diesel engine, and gasoline engine particulate extracts.

    PubMed Central

    Strandell, M; Zakrisson, S; Alsberg, T; Westerholm, R; Winquist, L; Rannug, U

    1994-01-01

    Extracts of gasoline and diesel vehicle exhaust and ambient air particles were fractionated into five fractions according to polarity on a silica gel column. Two medium polar fractions showing high genotoxic activity in the Ames test were further subfractionated, using normal-phase high-performance liquid chromatography. Chemical analyses were performed by means of gas chromatography combined with mass spectrometry and flame ionization and detection. The crude extracts, fractions, and subfractions were assayed with the Ames test, with and without S9, and the most abundant compounds in the subfractions are reported. PMID:7529708

  17. New lab-made coagulant based on Schinopsis balansae tannin extract: synthesis optimization and preliminary tests on refractory water pollutants

    NASA Astrophysics Data System (ADS)

    Sánchez-Martín, J.; Beltrán-Heredia, J.; Coco-Rivero, B.

    2014-09-01

    Quebracho colorado tannin extract was used as a coagulant raw material for water and wastewater treatment. The chemical synthesis follows a Mannich reaction mechanism and provides a fully working coagulant that can remove several pollutants from water. This paper addresses the optimization of such synthesis and confirms the feasibility of the coagulant by testing it in a preliminary screening for the elimination of dyes and detergents. The optimum combination of reagents was 6.81 g of diethanolamine (DEA) and 2.78 g of formaldehyde (F) per g of tannin extract. So obtained coagulant was succesfully tested on the removal of 9 dyes and 8 detergents.

  18. Orthogonal test design for optimizing the extraction of total flavonoids from Inula helenium

    PubMed Central

    Guo, Chun-Yan; Wang, Jin; Hou, Yong; Zhao, Yong-Ming; Shen, Li-Xia; Zhang, Dan-Shen

    2013-01-01

    Background: Inula helenium, which belongs to thecomposite family, is an important crude drug in traditional Chinese medicine. Materials and Methods: The effects of ethanol concentration, liquid to solid ratio, extraction temperature, and duration of microwave irradiation on the flavonoid extraction yield were studied through a single-factor experiment. An orthogonal array (L9(34)) was then constructed to achieve the best extraction conditions. Results: Variance analysis revealed that ethanol concentration significantly affected the extraction yield. The optimal conditions were as follows: ethanol concentration, 50% (v/v); liquid to solid ratio, 15:1; duration of microwave irradiation, 240 s; and extraction temperature, 60°C. Conclusion: Under these optimal conditions, the total flavonoid yield was 18.34 ± 0.64 mg/g. The use of a microwave-assisted process dramatically reduced the time needed for extraction of flavonoids from I. helenium. PMID:23930000

  19. Orthogonal test design for optimizing the extraction of total flavonoids from Inula helenium.

    PubMed

    Guo, Chun-Yan; Wang, Jin; Hou, Yong; Zhao, Yong-Ming; Shen, Li-Xia; Zhang, Dan-Shen

    2013-07-01

    Inula helenium, which belongs to thecomposite family, is an important crude drug in traditional Chinese medicine. The effects of ethanol concentration, liquid to solid ratio, extraction temperature, and duration of microwave irradiation on the flavonoid extraction yield were studied through a single-factor experiment. An orthogonal array (L9(3(4))) was then constructed to achieve the best extraction conditions. Variance analysis revealed that ethanol concentration significantly affected the extraction yield. The optimal conditions were as follows: ethanol concentration, 50% (v/v); liquid to solid ratio, 15:1; duration of microwave irradiation, 240 s; and extraction temperature, 60°C. Under these optimal conditions, the total flavonoid yield was 18.34 ± 0.64 mg/g. The use of a microwave-assisted process dramatically reduced the time needed for extraction of flavonoids from I. helenium.

  20. LiDAR DTMs and anthropogenic feature extraction: testing the feasibility of geomorphometric parameters in floodplains

    NASA Astrophysics Data System (ADS)

    Sofia, G.; Tarolli, P.; Dalla Fontana, G.

    2012-04-01

    resolution topography have been proven to be reliable for feasible applications. The use of statistical operators as thresholds for these geomorphic parameters, furthermore, showed a high reliability for feature extraction in mountainous environments. The goal of this research is to test if these morphological indicators and objective thresholds can be feasible also in floodplains, where features assume different characteristics and other artificial disturbances might be present. In the work, three different geomorphic parameters are tested and applied at different scales on a LiDAR DTM of typical alluvial plain's area in the North East of Italy. The box-plot is applied to identify the threshold for feature extraction, and a filtering procedure is proposed, to improve the quality of the final results. The effectiveness of the different geomorphic parameters is analyzed, comparing automatically derived features with the surveyed ones. The results highlight the capability of high resolution topography, geomorphic indicators and statistical thresholds for anthropogenic features extraction and characterization in a floodplains context.

  1. Evaluation of the extraction method for the cytotoxicity testing of latex gloves.

    PubMed

    Baek, Hyun Sook; Yoo, Ja Young; Rah, Dong Kyun; Han, Dong-Wook; Lee, Dong Hee; Kwon, Oh-Hun; Park, Jong-Chul

    2005-08-31

    In this study, the cytotoxicity of medical latex gloves to cultured L-929 cells was determined using various extraction conditions. According to the extraction time and temperature, three types of extraction conditions were used: 1) 24 h at 37 degrees C; 2) 72 h at 37 degrees C; 3) 72 h at 50 degrees C. Also, four different extraction vehicles were used, namely, distilled water (DW), 9 g/l sodium chloride (saline) in DW, and culture media with or without serum. Under the above-mentioned conditions, the samples were extracted and then 2-fold serially diluted in the concentration range 3.13 - 50%. When extracted with either DW or saline for 24 h or 72 h at 37 degrees C, only 50% diluted samples showed distinct cytotoxicity to L-929 cells. Moreover, no cytotoxic potentials were observed when gloves were extracted with DW or saline at 50 degrees C for 72 h. Cytotoxicity was markedly greater when gloves were extracted with culture medium, irrespective of the presence of serum in the medium. These results suggest that optimal extraction conditions should be established for the cytotoxicity evaluations of biomaterials and medical devices.

  2. Round and Extracted Nb3Sn Strand Tests for LARP Magnet R&D

    SciTech Connect

    Barzi, Emanuela; Bossert, Rodger; Caspi, Shlomo; Dietderich, Dan; Ferracin, Paolo; Ghosh, Arup; Turrioni, Daniele; Yamada, Ryuji; Zlobin, Alexander V.

    2006-06-01

    The first step in the magnet R&D of the U.S. LHC Accelerator Research Program (LARP) is fabrication of technology quadrupoles TQS01 and TQC01. These are two-layer magnets which use cables of same geometry made of 0.7 mm MJR Nb{sub 3}Sn. Through strand billet qualification and tests of strands extracted from the cables, predictions of magnet performance are made. Measurements included the critical current, I{sub c}, using the voltage-current (VI) method at constant field, the stability current, I{sub S}, as the minimal quench current obtained with the voltage-field (VH) method at constant current in the sample, and RRR. Magnetization was measured at low and high fields to determine the effective filament size and to detect flux jumps. Effects of heat treatment duration and temperature on I{sub c} and I{sub S} were also studied. The Nb{sub 3}Sn strand and cable samples, the equipment, measurement procedures, and results are described. Based on these results, strand specifications were formulated for next LARP quadrupole models.

  3. Herpes murine model as a biological assay to test dialyzable leukocyte extracts activity.

    PubMed

    Salinas-Jazmín, Nohemí; Estrada-Parra, Sergio; Becerril-García, Miguel Angel; Limón-Flores, Alberto Yairh; Vázquez-Leyva, Said; Medina-Rivero, Emilio; Pavón, Lenin; Velasco-Velázquez, Marco Antonio; Pérez-Tapia, Sonia Mayra

    2015-01-01

    Human dialyzable leukocyte extracts (DLEs) are heterogeneous mixtures of low-molecular-weight peptides that are released on disruption of peripheral blood leukocytes from healthy donors. DLEs improve clinical responses in infections, allergies, cancer, and immunodeficiencies. Transferon is a human DLE that has been registered as a hemoderivate by Mexican health authorities and commercialized nationally. To develop an animal model that could be used routinely as a quality control assay for Transferon, we standardized and validated a murine model of cutaneous HSV-1 infection. Using this model, we evaluated the activity of 27 Transferon batches. All batches improved the survival of HSV-1-infected mice, wherein average survival rose from 20.9% in control mice to 59.6% in Transferon-treated mice. The activity of Transferon correlated with increased serum levels of IFN-γ and reduced IL-6 and TNF-α concentrations. Our results demonstrate that (i) this mouse model of cutaneous herpes can be used to examine the activity of DLEs, such as Transferon; (ii) the assay can be used as a routine test for batch release; (iii) Transferon is produced with high homogeneity between batches; (iv) Transferon does not have direct virucidal, cytoprotective, or antireplicative effects; and (v) the protective effect of Transferon in vivo correlates with changes in serum cytokines.

  4. Herpes Murine Model as a Biological Assay to Test Dialyzable Leukocyte Extracts Activity

    PubMed Central

    Salinas-Jazmín, Nohemí; Estrada-Parra, Sergio; Becerril-García, Miguel Angel; Limón-Flores, Alberto Yairh; Vázquez-Leyva, Said; Pavón, Lenin; Velasco-Velázquez, Marco Antonio; Pérez-Tapia, Sonia Mayra

    2015-01-01

    Human dialyzable leukocyte extracts (DLEs) are heterogeneous mixtures of low-molecular-weight peptides that are released on disruption of peripheral blood leukocytes from healthy donors. DLEs improve clinical responses in infections, allergies, cancer, and immunodeficiencies. Transferon is a human DLE that has been registered as a hemoderivate by Mexican health authorities and commercialized nationally. To develop an animal model that could be used routinely as a quality control assay for Transferon, we standardized and validated a murine model of cutaneous HSV-1 infection. Using this model, we evaluated the activity of 27 Transferon batches. All batches improved the survival of HSV-1-infected mice, wherein average survival rose from 20.9% in control mice to 59.6% in Transferon-treated mice. The activity of Transferon correlated with increased serum levels of IFN-γ and reduced IL-6 and TNF-α concentrations. Our results demonstrate that (i) this mouse model of cutaneous herpes can be used to examine the activity of DLEs, such as Transferon; (ii) the assay can be used as a routine test for batch release; (iii) Transferon is produced with high homogeneity between batches; (iv) Transferon does not have direct virucidal, cytoprotective, or antireplicative effects; and (v) the protective effect of Transferon in vivo correlates with changes in serum cytokines. PMID:25984538

  5. Design of adaptive digital filters for phase extraction in complex fringe patterns obtained using the Ronchi test

    NASA Astrophysics Data System (ADS)

    Caum, Jesus; Arasa, Josep; Royo, Santiago; Ares, Miguel

    2012-05-01

    A powerful technique is presented for processing complex fringe patterns with high noise levels and arbitrary distributions of spatial frequencies, which can successfully extract the phase information. Artifacts that arise from phase extraction in local filtering approaches are avoided by using a simple design and implementation strategy for the adaptive filter, based on the theory of digital filter design used in electronics, and applied to pixel rows (or columns) in the fringe-pattern. The filter designed in this manner is then applied to phase extraction in an experimental fringe pattern measured in a digital Ronchi test setup using a Carré phase-shifting procedure. The filtering strategy has a very low computational cost and allows phase extraction in noisy ronchigrams regardless their spatial frequency distribution, provided the fringes are still visible.

  6. Reverse osmosis concentrate treatment via a PAC-MF accumulative countercurrent adsorption process.

    PubMed

    Zhao, Chunxia; Gu, Ping; Cui, Hangyu; Zhang, Guanghui

    2012-01-01

    Organic pollutants in reverse osmosis (RO) concentrates from wastewater reclamation are mainly comprised of low molecular weight biorefractory compounds. Generally, advanced oxidation methods for oxidizing these organics require a relatively high level of energy consumption. In addition, conventional adsorption removal methods require a large dose of activated carbon. However, the dose can be reduced if its full adsorption capacity can be used. Therefore, the combined technology of powdered activated carbon (PAC) adsorption and microfiltration (MF) membrane filtration was studied to develop a countercurrent two-stage adsorption process. A PAC accumulative adsorption prediction method was proposed based on the verification of a PAC multi-stage adsorption capacity equation. Moreover, the prediction method was amended for a more accurate prediction of the effluent quality because adsorption isotherm constants were affected by the initial adsorbate concentration. The required PAC dose for the accumulative countercurrent two-stage adsorption system was 0.6 g/L, whereas that of the conventional adsorption process was 1.05 g/L when the dilution factor(F) was 0.1 and the COD and DOC removal rates were set to 70% and 68.1%, respectively. Organic pollutants were satisfactorily removed with less consumption of PAC. Effluent from this combined technology can be further reclaimed by an RO process to improve the overall recovery rate to between 91.0% and 93.8% with both economic and environmental benefits.

  7. Purification of semiconducting single-walled carbon nanotubes by spiral counter-current chromatography.

    PubMed

    Knight, Martha; Lazo-Portugal, Rodrigo; Ahn, Saeyoung Nate; Stefansson, Steingrimur

    2017-02-03

    Over the last decade man-made carbon nanostructures have shown great promise in electronic applications, but they are produced as very heterogeneous mixtures with different properties so the achievement of a significant commercial application has been elusive. The dimensions of single-wall carbon nanotubes are generally a nanometer wide, up to hundreds of microns long and the carbon nanotubes have anisotropic structures. They are processed to have shorter lengths but they need to be sorted by diameter and chirality. Thus counter-current chromatography methods developed for large molecules are applied to separate these compounds. A modified mixer-settler spiral CCC rotor made with 3 D printed disks was used with a polyethylene glycol-dextran 2-phase solvent system and a surfactant gradient to purify the major species in a commercial preparation. We isolated the semi-conducting single walled carbon nanotube chiral species identified by UV spectral analysis. The further development of spiral counter-current chromatography instrumentation and methods will enable the scalable purification of carbon nanotubes useful for the next generation electronics. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Counter-current thermocapilllary migration of bubbles in microchannels using self-rewetting liquids

    NASA Astrophysics Data System (ADS)

    Nazareth, Robson; Saenz, Pedro; Valluri, Prashant; Sefiane, Khellil

    2015-11-01

    The study of bubble transport in microchannels is of great interest in evaporative cooling of microdevices technologies. This is because bubble transport under heat-transfer or phase-change causes several flow instabilities that are less understood and hinder informed design of microcooling devices. Bubble motion in microchannels under temperature gradients is highly influenced by thermocapillary forces due surface tension gradients. Most studies until now so far are mainly based on pure liquids which present a linear temperature (inverse) dependence of surface tension. In this work, we consider motion of a bubble (formed of inert gas) in the so-called self-rewetting fluid that presents a parabolic (quadratic) dependence of surface tension on temperature, in a temperature range that includes a surface tension minimum. We particularly investigate the counter-current thermocapillary migration of bubbles in these liquids, as experimentally depicted by Shanahan and Sefiane (2014), by means of direct numerical simulations. We present a model that solves the 3D governing equations of mass, momentum, interface and energy for the two-phase system composed by incompressible, Newtonian and immiscible fluids. We resolve the deformable interface by means of a Volume-of-Fluid method. Our results indicate that there exists a pressure drop limit beyond which there would be no counter-current migration of bubbles.

  9. Counter-current thermocapillary migration of bubbles in self-rewetting liquids

    NASA Astrophysics Data System (ADS)

    Nazareth, R.; Saenz, P.; Sefiane, K.; Kim, J.; Valluri, P.

    2016-11-01

    In this work, we study the counter-current thermocapillary propulsion of a suspended bubble in the fluid flowing inside a channel subject to an axial temperature gradient when the surface tension dependence on temperature is non-monotonic. We use direct numerical simulations to address the two-phase conservation of mass, momentum and energy with a volume-of-fluid method to resolve the deformable interface. Two distinct regimes of counter-current bubble migration are characterized: i) "exponential decay" where the bubble decelerates rapidly until it comes to a halt at the spatial position corresponding to the minimum surface tension and ii) "sustained oscillations" where the bubble oscillates about the point of minimum surface tension. We illustrate how these sustained oscillations arise at low capillary number O(10-5) and moderate Reynolds number O(10) and, they are dampened by viscosity at lower Reynolds number. These results are in agreement with the experiments by Shanahan and Sefiane (Sci. Rep. 4, 2014). The work was supported by the Science without Borders program from CAPES agency of Brazilian Ministry of Education and the European Commission's Thermapower Project (294905).

  10. The dynamic connection of the Indonesian Throughflow, South Indian Ocean Countercurrent and the Leeuwin Current

    NASA Astrophysics Data System (ADS)

    Lambert, E.; Le Bars, D.; de Ruijter, W. P. M.

    2015-09-01

    East of Madagascar, wind and surface buoyancy fluxes reinforce each other, leading to frontogenesis, outcrop and an eastward along-front flow: the South Indian Ocean Countercurrent (SICC). In the east the Leeuwin Current (LC) is a unique eastern boundary current which flows poleward along Australia. It is often described as a regional coastal current forced by an off-shore meridional density gradient or a sea surface slope, yet little is known of the forcing and dynamics that control these open ocean meridional gadients. To complete this understanding, we make use of both an ocean general circulation model and a conceptual two-layer model. The SICC impinges on west Australia and adds to a sea level slope and a southward geostrophic coastal jet: the Leeuwin Current. The SICC and the LC are thus dynamically connected. An observed transport maximum of the LC around 22° S is directly related to this impingement of the SICC. The circulation of the Indonesian Throughflow (ITF) through the Indian Ocean appears to be partly trapped in the upper layer north of the outcrop line and is redirected along this outcrop line to join the eastward flow of the SICC. Shutdown of the ITF in both models strongly decreases the Leeuwin Current transport and breaks the connection between the LC and SICC. In this case, most of the SICC was found to reconnect to the internal gyre circulation in the Indian Ocean. The Indonesian Throughflow, South Indian Ocean Countercurrent and the Leeuwin Current are thus dynamically coupled.

  11. Extraction and isolation of saponins.

    PubMed

    Majinda, Runner R T

    2012-01-01

    Due to their special structural features, extraction and isolation of saponins poses a serious challenge. Conventional methods have been explored as well as the recent, relatively greener, efficient, solvent-economic, time-saving, newer methods of extraction. Both traditional and recent methods of isolation are also discussed. Finally, examples are given involving both conventional and newer methods of extraction and isolation. Though in general it is difficult to use a single technique for isolation of saponins, recent literature work seems to point to the fact that high speed counter-current separation coupled to evaporative light scattering detector (ELSD) gives superior separation. The ELSD appears to have circumvented the long-standing problem of saponin detection as most of these do not have a chromophore, and hence making UV detection only nonspecific and at range 200-210 nm.

  12. Extraction of DBP and MBP from actinides: application to the recovery of actinides from TBP-sodium carbonate scrub solutions. [Aralex process

    SciTech Connect

    Horwitz, E.P.; Mason, G.W.; Bloomquist, C.A.A.; Leonard, R.A.; Bernstein, G.J.

    1980-01-01

    A flowsheet for the recovery of actinides from TBP-Na/sub 2/CO/sub 3/ scrub waste solutions has been developed, based on batch extraction data, and tested, using laboratory scale counter-current extraction techniques. The process, called the ARALEX process, utilizes 2-ethyl-1-hexanol (2-EHOH) to extract the TBP degradation products (HDBP and H/sub 2/MBP) from acidified Na/sub 2/CO/sub 3/ scrub waste leaving the actinides in the aqueous phase. Dibutyl and monobutyl phosphoric acids are attached to the 2-EHOH molecules through hydrogen bonds. These hydrogen bonds also diminish the ability of the HDBP and H/sub 2/MBP to complex actinides and thus all actinides remain in the aqueous raffinate. Dilute sodium hydroxide solutions can be used to back-extract the dibutyl and monobutyl phosphoric acid esters as their sodium salts. The 2-EHOH can then be recycled. After extraction of the acidified carbonate waste with 2-EHOH, the actinides may be readily extracted from the raffinate with DHDECMP or, in the case of tetra- and hexavalent actinides, with TBP. The ARALEX process is relatively simple and involves inexpensive and readily available chamicals. The ARALEX process can also be applied to other actinide waste streams which contain appreciable concentrations of polar organic compounds that interfere with conventional actinide ion exchange and liquid-liquid extraction procedures. One such application is the removal of detergents from laundry or clean-up solutions contaminated with actinides.

  13. Efficient Preparation of Streptochlorin from Marine Streptomyces sp. SYYLWHS-1-4 by Combination of Response Surface Methodology and High-Speed Counter-Current Chromatography.

    PubMed

    Li, Lin; He, Shan; Ding, Lijian; Yuan, Ye; Zhu, Peng; Epstein, Slava; Fan, Jianzhong; Wu, Xiaokai; Yan, Xiaojun

    2016-05-27

    Since first isolated from the lipophilic extract of Streptomyces sp. SF2583, streptochlorin, has attracted a lot of attention because of its various pharmacological properties, such as antibiotic, antiallergic, antitumor, and anti-inflammatory activities. For the efficient preparation of streptochlorin from a producing strain Streptomyces sp. SYYLWHS-1-4, we developed a combinative method by using response surface methodology (RSM) and high-speed counter-current chromatography (HSCCC). In the fermentation process, we used RSM to optimize the condition for the efficient accumulation of streptochlorin, and the optimal parameters were: yeast extract 1.889 g/L, soluble starch 8.636 g/L, K₂HPO₄ 0.359 g/L, CaCl₂ 2.5 g/L, MgSO₄ 0.625 g/L, marine salt 25 g/L, medium volume 50%, initial pH value 7.0, temperature 27.5 °C, which enhanced streptochlorin yield by 17.7-fold. During the purification process, the preparative HSCCC separation was performed using a petroleum ether-ethyl acetate-methanol-water (9:0.8:5:5, v/v/v/v) biphasic solvent system, where 300 mg of crude sample yielded 16.5 mg streptochlorin with over 95% purity as determined by UPLC. Consequently, the combination method provided a feasible strategy for highly effective preparation of streptochlorin, which ensured the supply of large amounts of streptochlorin for in vivo pharmacological assessments or other requirements.

  14. Preparative isolation and purification of senkyunolide-I, senkyunolide-H and ferulic acid from Rhizoma Chuanxiong using counter-current chromatography.

    PubMed

    Wei, Yun; Hu, Jia; Li, Hao; Liu, Jiangang

    2011-12-01

    Three active compounds, senkyunolide-I, senkyunolide-H and ferulic acid (FA), were successfully isolated and purified from the extracts of Rhizoma Chuanxiong by counter-current chromatography (CCC). Based on the principle of the partition coefficient values (k) for target compounds and the separation factor (α) between target compounds, the two-phase solvent system that contains n-hexane-ethyl acetate-methanol-water at an optimized volume ratio of 3:7:4:6 v/v was selected for the CCC separation, and the lower phase was employed as the mobile phase in the head-to-tail elution mode. In a single run, 400 mg of the crude extract yielded pure senkyunolide-I (6.4 mg), senkyunolide-H (1.7 mg) and FA (4.4 mg) with the purities of 98, 93 and 99%, respectively. The CCC fractions were analyzed by high-performance liquid chromatography, and the structures of the three active compounds were identified by MS and (1)H NMR.

  15. Isolation of the minor and rare constituents from fruits of Peucedanum alsaticum L. using high-performance counter-current chromatography.

    PubMed

    Skalicka-Woźniak, Krystyna; Mroczek, Tomasz; Garrard, Ian; Głowniak, Kazimierz

    2012-04-01

    A high-performance counter-current chromatography (HPCCC) method was applied for the first time for the preparative separation and purification of three rare compounds which occur as minor constituents in the fruits of Peucedanum alsaticum L.: 5-substituted coumarin notoptol and two dihydropyranochromones: divaricatol and ledebouriellol. A scale-up process from analytical to preparative in a very short time was developed. In order to purify a range of rare and minor compounds with different polarity two separate experiments were performed, one in reverse phase, the other in normal phase, using the same crude extract. A two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water (1:1:1:1) was developed. The components purified and collected were analyzed by high-performance liquid chromatography. The method yielded 0.7 mg of notoptol, 1.46 mg of ledebouriellol at purity of 99.5%, and 10 mg of mixtures of divaricatol, alsaticol and alsaticocoumarin, where divaricatol present 22% by peak area. These amounts were obtained from 1 g of the crude extract in a single run. This is the first time when minor notoptol, ledebouriellol, and divaricatol were isolated in a single run using HPCCC method and first time when these were identified in plant from Peucedanum genus.

  16. Recovery of butanol by counter-current carbon dioxide fractionation with its potential application to butanol fermentation

    USDA-ARS?s Scientific Manuscript database

    A counter-current CO2 fractionation method was studied as a means to recover butanol (also known as 1-butanol or n-butanol) and other compounds that are typically obtained from biobutanol fermentation broth from aqueous solutions. The influence of operating parameters, such as solvent-to-feed ratio,...

  17. Isolation of chavibetol from essential oil of Pimenta pseudocaryophyllus leaf by high-speed counter-current chromatography.

    PubMed

    dos Santos, Bruna C B; da Silva, Júlio César T; Guerrero, Palimécio G; Leitão, Gilda G; Barata, Lauro E S

    2009-05-08

    Counter-current chromatography (CCC) was used to isolate chavibetol from the essential oil of leaves of Pimenta pseudocaryophyllus (Gomes) Landrum. Chavibetol was obtained in high purity (98%) and mass recovery (94.4%). Methyleugenol was also isolated. The CCC biphasic solvent system used was composed of hexane:n-butanol:methanol:water (12:4:4:3, v/v/v/v).

  18. Intradermal testing of horses with and without insect bite hypersensitivity in The Netherlands using an extract of native Culicoides species.

    PubMed

    Sloet van Oldruitenborgh-Oosterbaan, Marianne M; van Poppel, Miriam; de Raat, Inge J; van den Boom, Robin; Savelkoul, Huub F J

    2009-10-01

    Intradermal tests using a Culicoides nubeculosus extract have proven unreliable for diagnosis of equine insect bite hypersensitivity (IBH) in the Netherlands. The aim of this study was to evaluate the diagnostic value of an extract derived from the Dutch species C. obsoletus and C. pulicaris. Thirteen pairs of horses were tested, each pair consisting of one horse with IBH and the other a healthy control. Each horse was injected intradermally with 0.1 mL of three concentrations of Culicoides whole body extract (1 : 1000 w/v, 1 : 10,000 w/v and 1 : 25,000 w/v), histamine solution (0.01 mg/mL, positive control) and phosphate-buffered saline (negative control). Skin responses were evaluated after 30 min and at 1, 4 and 24 h. At all time points the absolute wheal diameter elicited by Culicoides extract 1 : 1000 w/v was significantly larger (P < 0.01) in the IBH horses than in the control horses. Using the 1 : 10,000 w/v extract the difference was significant at 1, 4 and 24 h and using the 1 : 25,000 w/v extract only at 24 h. The relative wheal diameter was greater in IBH than in control horses at all concentrations and time points except at 0.5 h for the 1 : 10,000 w/v and 1 : 25,000 w/v concentrations. At the 1 : 1000 w/v concentration, the sensitivity and specificity was 92% using the relative wheal diameter. These results indicate that intradermal testing using 1 : 1000 w/v concentration Culicoides extracts relevant to the locality provides useful support for a clinical diagnosis of equine insect hypersensitivity.

  19. Extracting material response from simple mechanical tests on hardening-softening-hardening viscoplastic solids

    NASA Astrophysics Data System (ADS)

    Mohan, Nisha

    Compliant foams are usually characterized by a wide range of desirable mechanical properties. These properties include viscoelasticity at different temperatures, energy absorption, recoverability under cyclic loading, impact resistance, and thermal, electrical, acoustic and radiation-resistance. Some foams contain nano-sized features and are used in small-scale devices. This implies that the characteristic dimensions of foams span multiple length scales, rendering modeling their mechanical properties difficult. Continuum mechanics-based models capture some salient experimental features like the linear elastic regime, followed by non-linear plateau stress regime. However, they lack mesostructural physical details. This makes them incapable of accurately predicting local peaks in stress and strain distributions, which significantly affect the deformation paths. Atomistic methods are capable of capturing the physical origins of deformation at smaller scales, but suffer from impractical computational intensity. Capturing deformation at the so-called meso-scale, which is capable of describing the phenomenon at a continuum level, but with some physical insights, requires developing new theoretical approaches. A fundamental question that motivates the modeling of foams is `how to extract the intrinsic material response from simple mechanical test data, such as stress vs. strain response?' A 3D model was developed to simulate the mechanical response of foam-type materials. The novelty of this model includes unique features such as the hardening-softening-hardening material response, strain rate-dependence, and plastically compressible solids with plastic non-normality. Suggestive links from atomistic simulations of foams were borrowed to formulate a physically informed hardening material input function. Motivated by a model that qualitatively captured the response of foam-type vertically aligned carbon nanotube (VACNT) pillars under uniaxial compression [2011,"Analysis of

  20. K-targeted metabolomic analysis extends chemical subtraction to DESIGNER extracts: selective depletion of extracts of hops (Humulus lupulus).

    PubMed

    Ramos Alvarenga, René F; Friesen, J Brent; Nikolić, Dejan; Simmler, Charlotte; Napolitano, José G; van Breemen, Richard; Lankin, David C; McAlpine, James B; Pauli, Guido F; Chen, Shao-Nong

    2014-12-26

    This study introduces a flexible and compound targeted approach to Deplete and Enrich Select Ingredients to Generate Normalized Extract Resources, generating DESIGNER extracts, by means of chemical subtraction or augmentation of metabolites. Targeting metabolites based on their liquid-liquid partition coefficients (K values), K targeting uses countercurrent separation methodology to remove single or multiple compounds from a chemically complex mixture, according to the following equation: DESIGNER extract = total extract ± target compound(s). Expanding the scope of the recently reported depletion of extracts by immunoaffinity or solid phase liquid chromatography, the present approach allows a more flexible, single- or multi-targeted removal of constituents from complex extracts such as botanicals. Chemical subtraction enables both chemical and biological characterization, including detection of synergism/antagonism by both the subtracted targets and the remaining metabolite mixture, as well as definition of the residual complexity of all fractions. The feasibility of the DESIGNER concept is shown by K-targeted subtraction of four bioactive prenylated phenols, isoxanthohumol (1), 8-prenylnaringenin (2), 6-prenylnaringenin (3), and xanthohumol (4), from a standardized hops (Humulus lupulus L.) extract using specific solvent systems. Conversely, adding K-targeted isolates allows enrichment of the original extract and hence provides an augmented DESIGNER material. Multiple countercurrent separation steps were used to purify each of the four compounds, and four DESIGNER extracts with varying depletions were prepared. The DESIGNER approach innovates the characterization of chemically complex extracts through integration of enabling technologies such as countercurrent separation, K-by-bioactivity, the residual complexity concepts, as well as quantitative analysis by (1)H NMR, LC-MS, and HiFSA-based NMR fingerprinting.

  1. Cytogenotoxicity of Cymbopogon citratus (DC) Stapf (lemon grass) aqueous extracts in vegetal test systems.

    PubMed

    Sousa, Saulo M; Silva, Pâmela S; Viccini, Lyderson F

    2010-06-01

    The lemon grass, Cymbopogon citratus (DC) Stapf, is an important species of Poaceae family commonly used in the folk medicine in many countries. The aim of this study was to investigate the cytotoxic and genotoxic effects of aqueous extracts from C. citratus leaves on Lactuca sativa (lettuce) root tip meristem cells by cytogenetic studies that have never been done before for lemon grass extracts. For this, lettuce seeds were treated for 72h with different concentrations of lemon grass aqueous extracts (5; 10; 20 and 30 mg/mL). The percentage of germination, root development and cellular behavior were analyzed, and the results showed that the highest concentration of aqueous extracts reduced the mitotic index, the seed germination and the root development of lettuce. The extracts have also induced chromosome aberrations and cellular death in the roots cells of L. sativa.

  2. Oscillating Hydrofoils for Tidal Energy Extraction: Experiments, Simulations and Salt Water Field Tests

    NASA Astrophysics Data System (ADS)

    Mandre, S.; Franck, J.; Breuer, K.; Fawzi, A.; Cardona, J.; Miller, M. J.; Su, Y.; Medina, A.; Loera Loera, C.; Junquera, E.; Simeski, F.; Volkmann, K.; Lorick, R.; Cowles, S.; Luiz Rocha Ribeiro, B.; Winckler, S.; Derecktor, T.

    2015-12-01

    We report on the development of a new oscillating hydrofoil technology for tidal flow energy harvesting. A series of flume experiments and computational fluid dynamics (CFD) simulations have been performed over a wide range of frequencies, f, heave amplitudes, h, and pitch angles, θ. The flume model has chord, c, of 10 cm and aspect ratio of 4.5. Mechanical power extracted is estimated from the foil trajectory, force and moment data. A robust real-time algorithm has been developed to identify the kinematics that optimizes either the total power or the Betz efficiency. Optimal efficiency is found when the pitch and heave cycles are 90 degrees out of phase, oscillating at a reduced frequency, fc/U, of approximately 0.15, with a heave amplitude of approximately 1c, and a pitch amplitude of θ=75 degrees. The high pitch amplitude and sharp leading edge of the foil generates a transient leading edge vortex on the suction side of the foil, significantly enhancing the vertical force and power. The optimal frequency ensures that the vortex generation and ultimate shedding maximize these unsteady hydrodynamic effects. The flume results, including power and efficiency, as well as flow visualization and particle image velocimetry (PIV) exhibit excellent agreement with the CFD. Furthermore, extensive CFD and physical experiments have been performed to investigate the effects of operating in confined or shallow channels. It is found that the efficiency and power generation can significantly increase in confined areas due to the acceleration of the freestream flow around the device. Finally, the Leading Edge team has designed, built, and as of this date, is currently field-testing a 1kW prototype device consisting of two foils operating in parallel. The prototype is attached to the underside of a pontoon boat, and testing is currently underway in the Narragansett Bay near Providence RI. On completion of the field tests, in October 2015, data from the prototype will be analyzed

  3. Rapid diagnostic tests for molecular surveillance of Plasmodium falciparum malaria -assessment of DNA extraction methods and field applicability.

    PubMed

    Morris, Ulrika; Aydin-Schmidt, Berit; Shakely, Delér; Mårtensson, Andreas; Jörnhagen, Louise; Ali, Abdullah S; Msellem, Mwinyi I; Petzold, Max; Gil, José P; Ferreira, Pedro E; Björkman, Anders

    2013-03-19

    The need for new malaria surveillance tools and strategies is critical, given improved global malaria control and regional elimination efforts. High quality Plasmodium falciparum DNA can reliably be extracted from malaria rapid diagnostic tests (RDTs). Together with highly sensitive molecular assays, wide scale collection of used RDTs may serve as a modern tool for improved malaria case detection and drug resistance surveillance. However, comparative studies of DNA extraction efficiency from RDTs and the field applicability are lacking. The aim of this study was to compare and evaluate different methods of DNA extraction from RDTs and to test the field applicability for the purpose of molecular epidemiological investigations. DNA was extracted from two RDT devices (Paracheck-Pf® and SD Bioline Malaria Pf/Pan®), seeded in vitro with 10-fold dilutions of cultured 3D7 P. falciparum parasites diluted in malaria negative whole blood. The level of P. falciparum detection was determined for each extraction method and RDT device with multiple nested-PCR and real-time PCR assays. The field applicability was tested on 855 paired RDT (Paracheck-Pf) and filter paper (Whatman® 3MM) blood samples (734 RDT negative and 121 RDT positive samples) collected from febrile patients in Zanzibar 2010. RDT positive samples were genotyped at four key single nucleotide polymorphisms (SNPs) in pfmdr1 and pfcrt as well as for pfmdr1 copy number, all associated with anti-malarial drug resistance. The P. falciparum DNA detection limit varied with RDT device and extraction method. Chelex-100 extraction performed best for all extraction matrixes. There was no statistically significant difference in PCR detection rates in DNA extracted from RDTs and filter paper field samples. Similarly there were no significant differences in the PCR success rates and genotyping outcomes for the respective SNPs in the 121 RDT positive samples. The results support RDTs as a valuable source of parasite DNA and

  4. Anti-hyperglycaemic activity of swietenia macrophylla king (meliaceae) seed extracts in normoglycaemic rats undergoing glucose tolerance tests

    PubMed Central

    2013-01-01

    Background Swietenia macrophylla King (Meliaceae) is used to treat diabetes mellitus in Malaysia. This study aims to evaluate the anti-hyperglycaemic potential of petroleum ether (PE), chloroform (CE) and methanol (ME) extracts of S. macrophylla seeds, in normoglycaemic and streptozotocin (STZ)-induced diabetic rats. Methods Following treatment of normoglycaemic rats with S. macrophylla seed extracts, hypoglycaemic and intraperitoneal glucose tolerance tests (IPGTT) were performed, and blood glucose concentrations were measured. Similarly, glucose concentrations were measured after 1 and 14 days of extract treatment of STZ-induced diabetic rats. Glucose absorption by isolated everted intestine and glucose uptake by isolated abdominal muscle were tested after treatment with seed extracts. Gas chromatography mass spectrometry (GC-MS) analysis was performed on PE of S. macrophylla seeds to identify the compounds responsible for its activity. Results None of the extracts had a significant effect on the blood glucose levels of 60 randomly selected normoglycaemic (normal) and diabetic rats undergoing hypoglycaemic tests. PE, however, significantly reduced blood glucose levels in 30 randomly selected normoglycaemic rats undergoing IPGTT tests 30–120 minutes after glucose administration. Repeated doses of 1000 mg/kg and 500 mg/kg PE to STZ-induced diabetic rats for 14 days did not reduce blood glucose levels significantly. PE did not significantly reduced the intestinal absorption of glucose, but significantly increased glucose uptake by abdominal muscle in the absence or presence of insulin. GC-MS analysis indicated that diterpenes, triterpenoids, fatty acid methyl esters, aldehydes and phytosterols may be responsible for the glucose lowering effects of PE. Conclusion PE extracts of S. macrophylla seeds showed anti-hyperglycaemic activity on IPGTTs . GC-MS analysis on the PE revealed that several compounds, including fucosterol and β-sitosterol, may be responsible for

  5. Validation of the LacTek test applied to spiked extracts of tissue samples: determination of performance characteristics.

    PubMed

    Mitchell, J M; Yee, A J; McNab, W B; Griffiths, M W; McEwen, S A

    1999-01-01

    LacTek tests are competitive enzyme-linked immunosorbent assays intended for rapid detection of antimicrobial residues in bovine milk. In this study, the LacTek test protocol was modified for use with extracts of bovine tissue to detect beta-lactam, tetracycline, and sulfamethazine residues. Test performance characteristics--precision, accuracy, ruggedness, practicability, and analytical specificity and sensitivity--were investigated. Results suggest that LacTek tests can be easily adapted to detect antimicrobial residues in extracts of lean ground beef. However, positive samples may not contain residues at violative concentrations (i.e., Canadian maximum residue limits), and therefore, additional analysis would be required for final confirmation and quantitation (e.g., chromatography).

  6. Effect of standardized aqueous extract of Withania somnifera on tests of cognitive and psychomotor performance in healthy human participants

    PubMed Central

    Pingali, Usharani; Pilli, Raveendranadh; Fatima, Nishat

    2014-01-01

    Background: Withania somnifera is an herbal medicine that has been known to possess memory-enhancing properties. The current study involved an assessment of cognitive and psychomotor effects of Withania somnifera extract in healthy human participants. Materials and Methods: In this prospective, double-blind, multi-dose, placebo-controlled, crossover study, 20 healthy male participants were randomized to receive 250 mg two capsules twice daily of an encapsulated dried aqueous extract of roots and leaves of Withania somnifera or a matching placebo for a period of 14 days. Cognitive and psychomotor performance was assessed pre-dose (day 1) and at 3 hrs post-dose on day 15 using a battery of computerized psychometric tests. After a washout period of 14 days, the subjects crossed-over to receive the other treatment for a further period of 14 days as per prior randomization schedule. Same battery of test procedures were performed to assess cognitive and psychomotor performance. Results: Significant improvements were observed in reaction times with simple reaction, choice discrimination, digit symbol substitution, digit vigilance, and card sorting tests with Withania somnifera extract compared to placebo. However, no effect can be seen with the finger tapping test. Conclusion: These results suggest that Withania somnifera extract can improve cognitive and psychomotor performance and may, therefore, be a valuable adjunct in the treatment of diseases associated with cognitive impairment. PMID:24497737

  7. High-speed counter-current chromatography in separation of betacyanins from flowers of red Gomphrena globosa L. cultivars.

    PubMed

    Spórna-Kucab, Aneta; Hołda, Ewelina; Wybraniec, Sławomir

    2016-10-15

    Antioxidant and possible chemopreventive properties of betacyanins, natural plant pigments, contribute to a growing interest in their chemistry and separation. Mixtures of betacyanins from fresh red Gomphrena globosa L. cultivar flowers were separated in three highly polar solvent systems by high-speed counter-current chromatography (HSCCC) for a direct comparison of their separation effectiveness. Three samples of crude extract (600mg) were run on semi-preparative scale in solvent system (NH4)2SO4soln - EtOH (2.0:1.0, v/v) (system I) and the modified systems: EtOH - ACN - 1-PrOH - (NH4)2SO4satd.soln - H2O (0.5:0.5:0.5:1.2:1.0, v/v/v/v/v) (system II) and EtOH - ACN - (NH4)2SO4satd.soln - H2O (1.0:0.5:1.2:1.0, v/v/v/v) (system III). The systems were used in the head-to-tail (system I) or tail-to-head (systems II and III) mode. The flow rate of the mobile phase was 2.0ml/min and the column rotation speed was 860rpm. The retention of the stationary phase was 52.0% (system I), 80.2% (systems II) and 82.0% (system III). The betacyanins in the crude extract as well as HSCCC fractions were analyzed by LC-MS/MS. System I was applied for the first time in HSCCC for the separation of betacyanins and was quite effective in separation of amaranthine and 17-decarboxy-amaranthine (αI=1.19) and very effective for 17-decarboxy-amaranthine and betanin (αI=2.20). Modification of system I with acetonitrile (system III) as well as acetonitrile and propanol (system II) increased their separation effectiveness. Systems II-III enable complete separation of 17-decarboxy-amaranthine (KD(II)=2.94,KD(III)=2.42) and betanin (KD(II)=2.46,KD(III)=1.10) as well as betanin and gomphrenin I (KD(II)=1.62, KD(III)=0.74). In addition, separation of amaranthine and 17-decarboxy-amaranthine is the most effective in system II, therefore, this system proved to be the most suitable for the separation of all polar betacyanins.

  8. [The diangostic value of skin tests with tissue-extracts, especially in lepra and sarcoidosis (author's transl)].

    PubMed

    Hoppe, J E; Stüttgen, G

    1975-02-01

    The immunological aspects of lepra (India, Germany) and Sarcoidosis are presented under consideration of cutaneous reaction to lepromin and Kveim-extracts. Patients with lepra, erythema nodosum, sarcoidosis and different dermatoses have been tested with lepromin, Kveim-Antigen and tuberculin. The specifity of the results has been discussed. Patients with tuberculoid lepra did not react on Kveim-test, but patients with sarcoidosis can give positive reaction on lepromin. Patients with erythema nodosum without clinical signs of sarcoidosis are Kveim negativ and a positive lepromin-test is an exception. The positive Kveim-test is bound to a histological examination. The positive lepromin-test in non lepraendemic countries should be interpreted also by histological examination. Granulomatous dermatoses can show positive lepromin-tests, but the histological picture is different from the lepromin reaction in tuberculoid lepra. The positive reactions on tissue extracts are not combined with positive immunfluorescence results. Intracutaneous injection of lepra-bacilli in lepromin extract can be presented days to weeks after intracutaneous application in biopsies.

  9. Common solvents for making extraction of allergenic proteins from plants’ pollens for prick tests and related factors: a technical review

    PubMed Central

    Mansouritorghabeh, Hassan; Jabbari-Azad, Farahzad; Varasteh, Abdolreza; Sankian, Mojtaba; Farid-Hosseini, Reza

    2017-01-01

    Collecting information on influencing factors in developing consistent and high-quality extracts results in accurate diagnosis and effective treatment of type I allergy (IgE mediated). Furthermore, considering that a large number of allergens are currently in practice, any attempt to develop a more effective procedure for preparing extract may be useful. Nowadays, different saline solvents, temperature, incubation time, and PH are being incorporated for preparing allergen extracts. The objective of the current study was to clear and address the commonest of solvent buffers and allied conditions for making extracts of pollens of grasses, trees, and weeds. The literature review was done in Jan 2016 on PubMed and Google Scholar medical search engines without any time limitation. After reading abstracts of 87 articles, finally 37 relevant papers were selected and their full texts were retrieved. In conclusion, 24 full-text papers were recognized appropriate and chosen. The extracted information for papers has been described fully in the text. On the basis of these data, PBS buffer with PH 7.4, temperature of 4 °C and with overnight incubation time, may be the optimized condition in order to have a proper extract for carrying out skin prick tests. PMID:28713519

  10. Radiolytic degradation of a new diglycol-diamide ligand for actinide and lanthanide co-extraction from spent nuclear fuel

    NASA Astrophysics Data System (ADS)

    Ossola, Annalisa; Macerata, Elena; Tinonin, Dario A.; Faroldi, Federica; Giola, Marco; Mariani, Mario; Casnati, Alessandro

    2016-07-01

    Within the Partitioning and Transmutation strategies, great efforts have been devoted in the last decades to the development of lipophilic ligands able to co-extract trivalent Lanthanides (Ln) and Actinides (An) from spent nuclear fuel. Because of the harsh working conditions these ligands undergo, it is important to prove their chemical and radiolytic stability during the counter-current multi-stage extraction process. In the present work the hydrolytic and radiolytic resistance of the freshly prepared and aged organic solutions containing the new ligand (2,6-bis[(N-methyl-N-dodecyl)carboxamide]-4-methoxy-tetrahydro-pyran) were investigated in order to evaluate the impact on the safety and efficiency of the process. Liquid-liquid extraction tests with spiked solutions showed that the ligand extracting performances are strongly impaired by storing the samples at room temperature and in the light. Moreover, the extracting efficiency of the irradiated samples resulted to be influenced by gamma irradiation, while selectivity remains unchanged. Preliminary mass spectrometric data showed that degradation is mainly due to the acid-catalysed reaction of the ligand carboxamide and ether groups with the 1-octanol present in the diluent.

  11. Testing of Perilla frutescens extract and Vicenin 2 for their antispasmodic effect.

    PubMed

    Verspohl, Eugen J; Fujii, Hajime; Homma, Kohei; Buchwald-Werner, Sybille

    2013-03-15

    Gastrointestinal discomfort is frequently observed. The effects of Perilla frutescens extract and Vicenin 2 (a compound in this extract) were assayed in rat ileum with or without stimulation with acetylcholine or Ba(2+). Both had no direct spasmolytic effect, but both decreased acetylcholine- or Ba(2+)-induced contraction of rat ileum indicating an antispasmodic effect. This is valuable because effects were only observed when spasms were induced and may disturb the patient. The extract and the compound may be used to maintain and improve gut health. Copyright © 2012 Elsevier GmbH. All rights reserved.

  12. Comparative assessment of the leprosy antibody absorption test, Mycobacterium leprae extract enzyme-linked immunosorbent assay, and gelatin particle agglutination test for serodiagnosis of lepromatous leprosy.

    PubMed Central

    Escobar-Gutiérrez, A; Amezcua, M E; Pastén, S; Pallares, F; Cázares, J V; Pulido, R M; Flores, O; Castro, E; Rodríguez, O

    1993-01-01

    A comparative assessment of three serological methods for leprosy diagnosis (the fluorescent leprosy antibody absorption [FLA-ABS] test, the Mycobacterium leprae soluble-extract enzyme-linked immunosorbent assay [ELISA], and the M. leprae particle agglutination [MLPA] test) was carried out. The objective was to identify their performance in clinical and epidemiological diagnosis of leprosy. The study group included 45 lepromatous leprosy patients under treatment. Specificity was > 95% for all three assays, and sensitivity was 95, 58, and 74% for the FLA-ABS test, the MLPA test, and the ELISA, respectively. The only cross-reactivity for M. tuberculosis-infected patients was with the soluble-extract ELISA. Although the FLA-ABS test displayed the highest specificity and sensitivity values, it can only be used in well-developed laboratories, and the patient's clinical and epidemiological background must be considered when results are interpreted because the test remains positive after therapeutic success and could be positive for some household contacts. The MLPA test is easier to perform and interpret, and it is adequate for small laboratories and epidemiological studies intended to detect active untreated or irregularly treated leprosy cases. Therefore, the FLA-ABS and MLPA tests are complementary, and both should be used for serodiagnosis of leprosy. PMID:8501238

  13. Use of hairy roots extracts for 2,4-DCP removal and toxicity evaluation by Lactuca sativa test.

    PubMed

    Angelini, Vanina A; Agostini, Elizabeth; Medina, María I; González, Paola S

    2014-02-01

    2,4-Dichlorophenol (2,4-DCP) is widely distributed in wastewaters discharged from several industries, and it is considered as a priority pollutant due to its high toxicity. In this study, the use of different peroxidase extracts for 2,4-DCP removal from aqueous solutions was investigated. Tobacco hairy roots (HRs), wild-type (WT), and double-transgenic (DT) for tomato basic peroxidases (TPX1 and TPX2) were used to obtain different peroxidase extracts: total peroxidases (TPx), soluble peroxidases (SPx), and peroxidases ionically bound to the cell wall (IBPx). All extracts derived from DT HRs exhibited higher peroxidase activity than those obtained from WT HRs. TPx and IBPx DT extracts showed the highest catalytic efficiency values. The optimal conditions for 2,4-DCP oxidation were pH 6.5, H2O2 0.5 mM, and 200 U mL(-1) of enzyme, for all extracts analyzed. Although both TPx extracts were able to oxidize different 2,4-DCP concentrations, the removal efficiency was higher for TPx DT. Polyethylene glycol addition slightly improved 2,4-DCP removal efficiency, and it showed some protective effect on TPx WT after 2,4-DCP oxidation. In addition, using Lactuca sativa test, a reduction of the toxicity of post removal solutions was observed, for both TPx extracts. The results demonstrate that TPx extracts from both tobacco HRs appear to be promising candidate for future applications in removing 2,4-DCP from wastewaters. This is particularly true considering that these peroxidase sources are associated with low costs and are readily available. However, TPx DT has increased peroxidase activity, catalytic efficiency, and higher removal efficiency than TPx WT, probably due to the expression of TPX1 and TPX2 isoenzymes.

  14. Combination of poroelasticity theory and constant strain rate test in modelling land subsidence due to groundwater extraction

    NASA Astrophysics Data System (ADS)

    Pham, Tien Hung; Rühaak, Wolfram; Sass, Ingo

    2017-04-01

    Extensive groundwater extraction leads to a drawdown of the ground water table. Consequently, soil effective stress increases and can cause land subsidence. Analysis of land subsidence generally requires a numerical model based on poroelasticity theory, which was first proposed by Biot (1941). In the review of regional land subsidence accompanying groundwater extraction, Galloway and Burbey (2011) stated that more research and application is needed in coupling of stress-dependent land subsidence process. In geotechnical field, the constant rate of strain tests (CRS) was first introduced in 1969 (Smith and Wahls 1969) and was standardized in 1982 through the designation D4186-82 by American Society for Testing and Materials. From the reading values of CRS tests, the stress-dependent parameters of poroelasticity model can be calculated. So far, there is no research to link poroelasticity theory with CRS tests in modelling land subsidence due to groundwater extraction. One dimensional CRS tests using conventional compression cell and three dimension CRS tests using Rowe cell were performed. The tests were also modelled by using finite element method with mixed elements. Back analysis technique is used to find the suitable values of hydraulic conductivity and bulk modulus that depend on the stress or void ratio. Finally, the obtained results are used in land subsidence models. Biot, M. A. (1941). "General theory of three-dimensional consolidation." Journal of applied physics 12(2): 155-164. Galloway, D. L. and T. J. Burbey (2011). "Review: Regional land subsidence accompanying groundwater extraction." Hydrogeology Journal 19(8): 1459-1486. Smith, R. E. and H. E. Wahls (1969). "Consolidation under constant rates of strain." Journal of Soil Mechanics & Foundations Div.

  15. Multistep pH-peak-focusing countercurrent chromatography with a polyethylene glycol-Na2SO4 aqueous two phase system for separation and enrichment of rare earth elements.

    PubMed

    Shimizu, Kohei; Kuribayashi, Hiroaki; Watanabe, Haruna; Shimasaki, Tomomi; Azuma, Kenzaburo; Horie, Yohei; Saitoh, Kazunori; Saito, Shingo; Shibukawa, Masami

    2013-01-15

    Multistep pH-peak-focusing countercurrent chromatography was developed for separation and enrichment of rare earth metal ions using a polyethylene glycol-Na(2)SO(4) aqueous two phase system (ATPS) and pH stepwise gradient elution. Metal ions in a sample solution are chromatographically extracted in a basic stationary phase (polymer-rich phase of the ATPS) containing a complexation ligand such as acetylacetone at the top of the countercurrent chromatography (CCC) column. After the sample solution is introduced, the mobile phases of which the pH values have been adjusted with buffer reagents are delivered into the column by stepwise gradient elution in order of decreasing pH. Each metal ion is concentrated at a pH border formed between the zones of different pH in the CCC column through extraction with a complexing agent into the stationary phase at the front side of the border (basic region) and back extraction into the mobile phase at the back side of the border (acidic region), moving toward the outlet of the column with the pH border. Mutual separations of La(III), Ce(III), Nd(III), Yb(III), and Sc(III) were achieved by the present method using five step pH gradient elution, and each rare earth metal ion was effectively enriched at each of the five pH borders. The mechanism for formation of pH profile of the column effluent and the potential of this technique for preparative scale separation are also discussed.

  16. 40 CFR 1065.1109 - Post-test sampler disassembly and sample extraction.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... methylene chloride at a cycling rate of three cycles per hour. Discard the solvent used for pre-cleaning (no... rheostat adjusted to cycle the extraction at a rate of (3.0 ±0.5) cycles per hour. Drain the water from the... for 16 hours with the rheostat adjusted to cycle the extraction at a rate of (3.0 ±0.5) cycles...

  17. Effects of Hydroalcoholic Extract of Tanacetum Sonbolii (Asteraceae) on Pain-related Behaviors during Formalin Test in Mice

    PubMed Central

    Sofiabadi, Mohammad; Azhdari-Zarmehri, Hassan; Naderi, Firouzeh; Ghalandari-Shamami, Mohadeseh; Sonboli, Ali; Haghparast, Abbas

    2014-01-01

    Introduction Tanacetum sonbolii (Asteraceae) is an endemic species in Iran. In the present study, we examined the effects of Tanacetum sonbolii hydroalcoholic extract on the formalin test in mice. Methods 126 Swiss albino mice weighing 230-280g were used as subjects. The formalin test was performed on two control groups (marked as intact and saline groups; n = 6 in each group) and an experimental group. In all groups, the formalin test was recorded for 60 min after administration of extract and drugs in mice. Results The results showed that Tanacetum sonbolii (150 and 300 mg/kg) produced significant antinociception in phase 2. In addition, different doses of Tanacetum sonbolii extract (600, 900 and 1200 mg/kg) also induced antinociceptive effects in phase1 and phase 2. On the other hand, morphine could induce antinociception in a dose-dependent manner. Diclofenac (10 mg/kg) failed to affect the pain scores compared to Tanacetum sonbolii (300 mg/kg) group. Discussion It seems that administration of hydroalcoholic extract of Tanacetum sonbolii has the potential to relieve pain through both central and peripheral mechanisms in persistent inflammatory nociception. PMID:25337375

  18. Acute effects of an Avena sativa herb extract on responses to the Stroop Color-Word test.

    PubMed

    Berry, Narelle M; Robinson, Matthew J; Bryan, Janet; Buckley, Jonathan D; Murphy, Karen J; Howe, Peter R C

    2011-07-01

    Extracts from oat (Avena sativa) herb may benefit cognitive performance. This study investigated whether Neuravena(®), an oat herb extract, could acutely improve responses to the Stroop Color-Word test, a measure of attention and concentration and the ability to maintain task focus. Elderly volunteers with below-average cognitive performance consumed single doses (0, 1600, and 2400 mg) of oat herb extract at weekly intervals in a double-blind, randomized, crossover comparison. Resting blood pressure (BP) was assessed before and after supplementation, and a Stroop test was performed. Significantly fewer errors were made during the color-naming component of the Stroop test after consuming the 1600-mg dose than after the 0-mg or 2400-mg doses (F (1,36)=18.85, p<0.001). In 7 subjects with suspected cognitive impairment, Stroop interference score was also improved by the 1600-mg dose compared to 0- and 2400-mg doses (F (1, 34)=2.40, p<0.01). Resting BP was unaffected by supplementation. Taking 1600 mg of oat herb extract may acutely improve attention and concentration and the ability to maintain task focus in older adults with differing levels of cognitive status.

  19. Separation and purification of isorhamnetin 3-sulphate from Flaveria bidentis (L.) Kuntze by counter-current chromatography comparing two kinds of solvent systems.

    PubMed

    Xie, Qianqian; Yin, Li; Zhang, Guoliang; Wei, Yun

    2012-01-01

    The first preparative separation of a flavonoid sulphate isorhamnetin 3-sulphate from Flaveria bidentis (L.) Kuntze by counter-current chromatography (CCC) was presented. Two kinds of solvent systems were used. A conventional organic/aqueous solvent system n-butanol-ethyl acetate-water (4:1:5, v/v) was used, yielding isorhamnetin 3-sulphate 2.0 mg with a purity of 93.4% from 83 mg of pre-enriched crude extract obtained from 553 mg ethanol extract by macroporous resin. A one-component organic/salt-containing system composed of n-butanol-0.25% sodium chloride aqueous solution (1:1, v/v) was also used, and the LC column packed with macroporous resin has been employed for desalination of the target compound purified from CCC. As a result, 2.1 mg of isorhamnetin 3-sulphate with a purity of over 97% has been isolated from 402 mg of crude extract without pre-enrichment. Compared with the conventional organic/aqueous system, the one-component organic/salt-containing aqueous system was more suitable for the separation of isorhamnetin 3-sulphate, and purer target compound was obtained from the crude extract without pre-enrichment using the new solvent system. The chemical structure was confirmed by ESI-MS and (1)H, (13)C NMR. In summary, our results indicated that CCC using one-component organic/salt-containing aqueous solution is very promising and powerful for high-throughput purification of isorhamnetin 3-sulphate from Flaveria bidentis (L.) Kuntze.

  20. In-house validation of PremiTest, a microbiological screening test with solvent extraction, for the detection of antimicrobial residues in poultry muscles.

    PubMed

    Magalhães, C G; De Paiva, C R; Botelho, B G; De Oliveira, A M G; De Souza, L F; Nonaka, C V; Santos, K V; Farias, L M; Carvalho, M A R

    2012-01-01

    PremiTest, a microbial inhibition test for the screening of antimicrobial residues, was validated according to the criteria established by Decision 2002/657/EC. Sensitivity, detection capability (CCβ), specificity, selectivity, robustness and applicability were evaluated. The methodology involves the technique of solvent extraction, which increases the detection capability of the test for a wider range of antibiotics. The following CCβ values in poultry muscle were found: penicillin G ≤ 12.5 µg kg(-1), total sulfonamides ≤ 75 µg kg(-1), erythromycin 75 µg kg(-1) and lincomycin 50 µg kg(-1). The detection capability of chlortetracycline was equal to its maximum residue limit (100 µg kg(-1)) and the method did not detect gentamicin (1000 µg kg(-1)), for which no MRL is established in poultry muscle. Specificity evaluated in relation to different analytes and matrices did not detect any interferences in the tests results; whilst the robustness showed that the pH neutralisation point of the extract affects the analytical results and the kits' performance. Only the screening of tetracyclines requires the analysis of extracts without pH neutralisation. The results of the validation process showed that this method is acceptable for screening β-lactam, sulfonamide and macrolide antimicrobial groups in the National Residues and Contaminants Control Programme (PNCRC), and that for this it is fit for purpose.

  1. TRU decontamination of high-level Purex waste by solvent extraction using a mixed octyl(phenyl)-N,N-diisobutyl-carbamoylmethylphosphine oxide/TBP/NPH (TRUEX) solvent

    SciTech Connect

    Horwitz, E.P.; Kalina, D.G.; Diamond, H.; Kaplan, L.; Vandegrift, G.F.; Leonard, R.A.; Steindler, M.J.; Schulz, W.W.

    1984-01-01

    The TRUEX (transuranium extraction) process was tested on a simulated high-level dissolved sludge waste (DSW). A batch counter-current extraction mode was used for seven extraction and three scrub stages. One additional extraction stage and two scrub stages and all strip stages were performed by batch extraction. The TRUEX solvent consisted of 0.20 M octyl(phenyl)-N,N-diisobutylcarbamoyl-methylphosphine oxide-1.4 M TBP in Conoco (C/sub 12/-C/sub 14/). The feed solution was 1.0 M in HNO/sub 3/, 0.3 M in H/sub 2/C/sub 2/O/sub 4/ and contained mixed (stable) fission products, U, Np, Pu, and Am, and a number of inert constituents, e.g., Fe and Al. The test showed that the process is capable of reducing the TRU concentration in the DSW by a factor of 4 x 10/sup 4/ (to <100 nCi/g of disposed form) and reducing the quantity of TRU waste by two orders of magnitude.

  2. Evaluation of the extraction efficiency for the Hypoaspis aculeifer reproduction test in the context of soil quality assessment.

    PubMed

    Pierre, Huguier; Nicolas, Manier; Pascal, Pandard

    2016-12-01

    The standardized bioassay using the predatory mite Hypoaspis aculeifer (TG 226; as reported by OECD 2008) has already proven its usefulness for the assessment of chemicals. While included in the regulatory assessment scheme of pesticides as a non-target arthropod, it has still been rarely used for the assessment of soils or complex matrices of unknown quality. For such an objective, the extraction of both adults and juveniles from soil is a necessary and crucial step to get reliable data, but may be influenced by the characteristics of the tested soils or matrices. This technical note focuses on this specific protocol point. Extraction ratios of adults and of different reproductive outputs were evaluated in soils of different textures. Recommendations on the extraction of H. aculeifer in the standardization process within ISO/TC 190 are here provided.

  3. An improved model and parameters extraction for photovoltaic cells using only three state points at standard test condition

    NASA Astrophysics Data System (ADS)

    Peng, Lele; Sun, Yize; Meng, Zhuo

    2014-02-01

    In this paper, a comprehensive modeling and parameters extraction method is proposed to describe the current-voltage and power-voltage characteristic of photovoltaic cells. This method is based on data commonly issued by commercial photovoltaic data sheet. By using Lambert W function, the improved model of solar cells is given. Meanwhile, the current-voltage and power-voltage curves of photovoltaic cells are calculated. To extract the model parameters from only three state points at standard test conditions, an optimized approach using iterative method and approximate method is presented. Compared to the popular Rp model and experimental data, the proposed method shows excellent agreement between the current-voltages points. It is found that the proposed modeling and parameters extraction method has less error at the maximum power point state. Moreover, the proposed model is more realistic when subjected to ideality factors variations.

  4. Quadriceps Muscles O2 Extraction and EMG Breakpoints during a Ramp Incremental Test.

    PubMed

    Iannetta, Danilo; Qahtani, Ahmad; Millet, Guillaume Y; Murias, Juan M

    2017-01-01

    Muscle deoxygenated breakpoint ([HHb]BP) has been found to be associated with other indices of exercise tolerance in the vastus lateralis (VL) muscle but not in the vastus medialis (VM) and rectus femoris (RF). Purpose: To investigate whether the [HHb]BP occurs also in the VM and RF muscles and whether or not it is associated with other physiological indices of exercise tolerance, such as the EMG threshold (EMGt) and the respiratory compensation point (RCP). Methods: Twelve young endurance trained participants performed maximal ramp incremental (RI) cycling tests (25-30 W·min(-1) increments). Muscle oxygen extraction and activity as well as ventilatory and gas exchange parameters were measured. After accounting for the mean response time, the oxygen uptake ([Formula: see text]O2) corresponding to the RCP, [HHb]BP, and the EMGt was determined. Results: Peak power output (POpeak) was 359 ± 48 W. Maximal oxygen consumption ([Formula: see text]O2max) was 3.87 ± 0.46 L·min(-1). The [Formula: see text]O2 at the RCP was 3.39 ± 0.41 L·min(-1). The [Formula: see text]O2 (L·min(-1)) corresponding to the [HHb]BP and EMGt were: 3.49 ± 0.46 and 3.40 ± 0.44; 3.44 ± 0.61 and 3.43 ± 0.49; 3.59 ± 0.52, and 3.48 ± 0.46 for VL, VM, and RF, respectively. Pearson's correlation between these thresholds ranged from 0.90 to 0.97 (P < 0.05). No difference was found for the absolute [Formula: see text]O2 and the normalized PO (%) at which the thresholds occurred in all three muscles investigated (P > 0.05). Although in eight out of 12 participants, the [HHb]BP in the RF led to a steeper increase instead of leading to a plateau-like response as observed in the VL and VM, the [Formula: see text]O2 at the breakpoints still coincided with that at the RCP. Conclusions: This study demonstrated that local indices of exercise tolerance derived from different portions of the quadriceps are not different to the systemic index of the RCP.

  5. Real-Time Volumetric Phase Monitoring: Advancing Chemical Analysis by Countercurrent Separation.

    PubMed

    Pauli, Guido F; Pro, Samuel M; Chadwick, Lucas R; Burdick, Thomas; Pro, Luke; Friedl, Warren; Novak, Nick; Maltby, John; Qiu, Feng; Friesen, J Brent

    2015-07-21

    Countercurrent separation (CCS) utilizes the differential partitioning behavior of analytes between two immiscible liquid phases. We introduce the first platform ("CherryOne") capable of real-time monitoring, metering, and control of the dynamic liquid-liquid CCS process. Automated phase monitoring and volumetrics are made possible with an array of sensors, including the new permittivity-based phase metering apparatus (PMA). Volumetric data for each liquid phase are converted into a dynamic real-time display of stationary phase retention (Sf) and eluent partition coefficients (K), which represent critical parameters of CCS reproducibility. When coupled with the elution-extrusion operational mode (EECCC), automated Sf and K determination empowers untargeted and targeted applications ranging from metabolomic analysis to preparative purifications.

  6. Counter-current flow in a vertical to horizontal tube with obstructions

    SciTech Connect

    Tye, P.; Matuszkiewicz, A.; Teyssedou, A.

    1995-09-01

    This paper presents experimental results on counter-current flow and flooding in an elbow between a vertical and a horizontal run. The experimental technique used allowed not only the flooding limit to be determined, but also the entire partial delivery region to be studied as well. The influence that various size orifices placed in the horizontal run have on both the delivered liquid flow rates and on the flooding limits is also examined. It is observed that both the flooding limits and the delivered liquid flow rates decrease with decreasing orifice size. Further, it is also observed that the mechanisms that govern the partial delivery of the liquid are significantly different when an orifice is present in the horizontal leg as compared to the case when no orifice is present.

  7. Mixer-settler counter-current chromatography with multiple spiral disk assembly.

    PubMed

    Ito, Yoichiro; Clary, Robert; Sharpnak, Frank; Metger, Howard; Powell, Jimmie

    2007-11-23

    A novel system for performing high-speed counter-current chromatography has been developed for separation of biopolymers using polymer phase systems. The spiral disk assembly consisting of eight units, each equipped with over 300 mixer-settler sets, was constructed and performance evaluated in terms of retention of the stationary phase and separation efficiency. A series of experiments was performed with a polymer phase system composed of polyethylene glycol 1000 (12.5%, w/w) and dibasic potassium phosphate (12.5%, w/w) using two stable protein samples of myoglobin and lysozyme at various experimental conditions of flow rates and revolution speeds. The best results were obtained with revolution speeds of 800-1000rpm at flow rates of 0.25-0.5ml/min where the partition efficiency of several 100 theoretical plates was achieved with over 50% stationary phase retention.

  8. One-step purification of proteins from chicken egg white using counter-current chromatography.

    PubMed

    Shibusawa, Y; Kihira, S; Ito, Y

    1998-05-29

    Proteins present in chicken egg white are separated by counter-current chromatography (CCC) in one step using a cross-axis coil planet centrifuge (X-axis CPC). The separation was performed with an aqueous polymer two-phase system composed of 16% (w/w) poly(ethylene glycol) 1000 and 12.5% (w/w) dibasic potassium phosphate by eluting the lower phase at a flow-rate of 1.0 ml/min. From about 20 g of the crude egg white solution, lysozyme, ovalbumin, and ovotransferrin were resolved within 5.5 h. Each component was identified by 12% SDS gel electrophoresis with Coomassie brilliant blue staining.

  9. Nonvolatiles of commercial lime and grapefruit oils separated by high-speed countercurrent chromatography.

    PubMed

    Feger, Wolfgang; Brandauer, Herbert; Gabris, Paulina; Ziegler, Herta

    2006-03-22

    The nonvolatile fractions of cold-pressed peel oils of Key and Persian lime as well as grapefruit were separated by high-speed countercurrent chromatography (HS-CCC). In addition to the isolation of the main coumarins, psoralens and polymethoxyflavones, a number of minor constituents were enriched and successfully characterized by GC-MS and HPLC-UV. 5,7,8-Trimethoxycoumarin and the cyclical acetals of oxypeucedanin hydrate with citral were determined as new nonvolatile trace constituents of lime oils and confirmed by NMR spectroscopy. The citral oxypeucedaninyl acetals were found particularly in Key lime oil type A, which as a result of the juice-oil contact, is exposed to acidic conditions during industrial processing. Some of the confirmed minor constituents, such as pabulenol, isooxypeucedanin, and oxypeucedanin methanolate in lime as well as auraptenol in grapefruit, may have been generated by hydrolysis-sensitive precursors during CCC separation or their respective industrial processing techniques.

  10. Cross-flow versus counter-current flow packed-bed scrubbers: a mathematical analysis

    SciTech Connect

    Fthenakis, V.M.

    1996-02-01

    Little is known about the mass transfer properties of packing media exposed to a crossflow of gas and liquid, whereas there is abundant information related to counter-current scrubbers. This paper presents a theoretical analysis of mass transfer and hydrodynamics in cross- flow packed bed scrubbers and compares those with information available for counter current towers, so that the first can be evaluated and/or designed based on data derived for the second. Mathematical models of mass transfer in cross-flow and counter- current packed bed scrubbers are presented. From those, one can predict the removal effectiveness of a crossflow scrubber from the number of transfer units (NTU) calculated for a similar counterflow operation; alternatively, when the removal effectiveness in counterflow is known, one can predict the corresponding NTU in crossflow.

  11. Novel Design for Centrifugal Counter-Current Chromatography: III. Saw Tooth Column

    PubMed Central

    Yang, Yi; Aisa, Haji Akber; Ito, Yoichiro

    2009-01-01

    The toroidal coil using an equilateral triangular core and zigzag pattern column have improved both retention of the stationary phase and peak resolution of the conventional toroidal coil in centrifugal counter-current chromatography. To further improve the retention of stationary phase and peak resolution, a novel saw tooth column was designed and the performance of the system was evaluated at various flow rates. The results indicated that both retention of the stationary phase and peak resolution were improved as the flow rate was decreased and at a flow rate of 0.005 ml/min the resolution is remarkably increased. Modification of the tubing called flat-twisted tubing further improved the peak resolution without increasing the column pressure. With a decreased column length at a capacity of about 0.2 ml, resolution of the saw tooth column was 1.02. PMID:20543965

  12. Novel Designs for Centrifugal Countercurrent chromatography: V. Comparative Studies on Performance of Various Column Configurations

    PubMed Central

    Yang, Yi; Gu, Dongyu; Aisa, Haji Akber; Ito, Yoichiro

    2009-01-01

    The conventional toroidal coil in centrifugal countercurrent chromatography has a low level of stationary phase retention, since a half of each helical turn is entirely occupied by the mobile phase. In order to cope with this problem, several new column designs including zigzag, saw-tooth and figure-8 patterns have been introduced and their performance was compared in terms of retention of the stationary phase (Sf), peak resolution (Rs), theoretical plate number (N) and column pressures. Overall results of experiments indicate that the figure-8 column yields the highest Rs when the lower phase is used as the mobile phase. Since the column pressure of all these new columns are much lower than that in the traditional toroidal coil column, the separation efficiency can be improved using a long separation column without a risk of column damage by high back pressure. PMID:21057664

  13. A criterion for the onset of slugging in horizontal stratified air-water countercurrent flow

    SciTech Connect

    Chun, Moon-Hyun; Lee, Byung-Ryung; Kim, Yang-Seok

    1995-09-01

    This paper presents an experimental and theoretical investigation of wave height and transition criterion from wavy to slug flow in horizontal air-water countercurrent stratified flow conditions. A theoretical formula for the wave height in a stratified wavy flow regime has been developed using the concept of total energy balance over a wave crest to consider the shear stress acting on the interface of two fluids. From the limiting condition of the formula for the wave height, a necessary criterion for transition from a stratified wavy flow to a slug flow has been derived. A series of experiments have been conducted changing the non-dimensional water depth and the flow rates of air in a horizontal pipe and a duct. Comparisons between the measured data and the predictions of the present theory show that the agreement is within {plus_minus}8%.

  14. Antioxidant and Antifatigue Properties of the Aqueous Extract of Moringa oleifera in Rats Subjected to Forced Swimming Endurance Test.

    PubMed

    Lamou, Bonoy; Taiwe, Germain Sotoing; Hamadou, André; Abene; Houlray, Justin; Atour, Mahamat Mey; Tan, Paul Vernyuy

    2016-01-01

    The effects of the aqueous extract of Moringa oleifera on swimming performance and related biochemical parameters were investigated in male Wistar rats (130-132 g). Four groups of rats (16 per group) were fed a standard laboratory diet and given distilled water, 100, 200, or 400 mg/kg of extract, respectively, for 28 days. On day 28, 8 rats from each group were subjected to the forced swimming test with tail load (10% of body weight). The remaining 8 rats per group were subjected to the 90-minute free swim. Maximum swimming time, glycemia, lactamia, uremia, triglyceridemia, hepatic and muscle glycogen, hematological parameters, and oxidative stress parameters (superoxide dismutase, catalase, reduced glutathione, and malondialdehyde) were measured. Results. M. oleifera extract increased maximum swimming time, blood hemoglobin, blood glucose, and hepatic and muscle glycogen reserves. The extract also increased the activity of antioxidant enzymes and decreased the blood concentrations of malondialdehyde. Furthermore, it decreased blood concentrations of lactate, triglycerides, and urea. In conclusion, the antifatigue properties of M. oleifera extract are demonstrated by its ability to improve body energy stores and tissue antioxidant capacity and to reduce the tissue build-up of lactic acid.

  15. Antioxidant and Antifatigue Properties of the Aqueous Extract of Moringa oleifera in Rats Subjected to Forced Swimming Endurance Test

    PubMed Central

    Lamou, Bonoy; Taiwe, Germain Sotoing; Hamadou, André; Abene; Houlray, Justin; Atour, Mahamat Mey; Tan, Paul Vernyuy

    2016-01-01

    The effects of the aqueous extract of Moringa oleifera on swimming performance and related biochemical parameters were investigated in male Wistar rats (130–132 g). Four groups of rats (16 per group) were fed a standard laboratory diet and given distilled water, 100, 200, or 400 mg/kg of extract, respectively, for 28 days. On day 28, 8 rats from each group were subjected to the forced swimming test with tail load (10% of body weight). The remaining 8 rats per group were subjected to the 90-minute free swim. Maximum swimming time, glycemia, lactamia, uremia, triglyceridemia, hepatic and muscle glycogen, hematological parameters, and oxidative stress parameters (superoxide dismutase, catalase, reduced glutathione, and malondialdehyde) were measured. Results. M. oleifera extract increased maximum swimming time, blood hemoglobin, blood glucose, and hepatic and muscle glycogen reserves. The extract also increased the activity of antioxidant enzymes and decreased the blood concentrations of malondialdehyde. Furthermore, it decreased blood concentrations of lactate, triglycerides, and urea. In conclusion, the antifatigue properties of M. oleifera extract are demonstrated by its ability to improve body energy stores and tissue antioxidant capacity and to reduce the tissue build-up of lactic acid. PMID:26904162

  16. Extraction-Scrub-Strip test results from the interim Salt Disposition Program Macrobatch 9 Tank 21H qualification samples

    SciTech Connect

    Peters, T.

    2016-02-23

    Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 9 for the Interim Salt Disposition Program (ISDP). The Salt Batch 9 characterization results were previously reported. An Extraction-Scrub-Strip (ESS) test was performed to determine cesium distribution ratios (D(Cs)) and cesium concentration in the strip effluent and decontaminated salt solution (DSS) streams; this data will be used by Tank Farm Engineering to project a cesium decontamination factor (DF). This test used actual Tank 21H material, and a blend solvent prepared by SRNL that mimics the solvent composition currently being used at the Modular Caustic-Side Solvent Extraction Unit (MCU). The ESS test showed acceptable performance with an extraction D(Cs) value of 52.4. This value is consistent with results from previous salt batch ESS tests using similar solvent formulations. This compares well against the predicted value of 56.5 from a recently created D(Cs) model

  17. GUESSmix-guided optimization of elution-extrusion counter-current separations.

    PubMed

    Friesen, J Brent; Pauli, Guido F

    2009-05-08

    Rational strategies for the optimization of separations are vital to any chromatographic technique. In counter-current separations (CS), once a suitable solvent system is selected for a given separation, the operator is faced with the task of optimizing the separation through the manipulation of those adjustable operation parameters allowed for by the current CS technology. This study employed a mixture of 21 natural products of varying polarity, molecular mass, and functionality, termed the GUESSmix, as a tool to assess the effectiveness of optimization strategies. The behavior of the GUESSmix was observed in the hexane/ethyl acetate/methanol/water 4:6:4:6 (HEMWat +3) solvent system. The effect of operation parameters on both the elution and extrusion stages of a recently introduced CS methodology, termed elution-extrusion counter-current chromatography (EECCC), was investigated. The resulting chromatograms were plotted with K-based reciprocal symmetry plots (ReS and ReSS), which allow comparison of the K values of significant peaks and assessment of resolution of eluting compounds in the interval 0< or =K< or =infinity. The operation parameters studied were: (1) the effect of temperature controlled water circulation around the centrifuge; (2) the combination of flow rate and revolution speed; (3) sample loading capacity; (4) the direction of rotation either agreeing with or opposing the direction of coil winding; (5) injection before equilibration, a practice that saves operator time and reduces solvent consumption. The GUESSmix was found to be a highly useful reference mixture to compare and contrast stationary phase retention volume ratios, resolution, K-values, peak shapes, and extrusion characteristics between CS experiments. EECCC is shown to be a robust technique that may be enhanced with appropriate temperature, rpm, flow rate, sample loading, direction of rotation, and injection timing. Plotting ReS[S] chromatograms enables systematic study of CS

  18. Identification and antioxidant activity test of bioactive compound produced from ethanol extract of temukunci (Boesenbergia rotunda)

    NASA Astrophysics Data System (ADS)

    Atun, Sri; Handayani, Sri; Frindryani, Luthfi Fitri

    2017-08-01

    The aims of this study are to identify and to analyze antioxidant activity of bioactive compounds in ethanol extract of temukunci (Boesenbergia rotunda) rhizome. This research method was carried out by maceration of 3 kg dryed powder of B. rotunda in ethanol. The extract was concentrated using a vacuum evaporator. White crystals obtained from ethanol extract further recrystallized to produce as much as 80 mg of pure compound. Identification of pure compound was obtained using UV-Vis, IR, and 1H-NMR. The antioxidant activity of ethanol extracts, pure compounds, and ascorbic acid (positive control) were obtained using DPPH (2,2-diphenyl-1-picrylhydrazyl) method. The UV-Vis spectra showed λmax 287.40 and 214.20 nm, the IR spectra showed absorption C=C aromatic group at 1571.66 cm-1, C=O carbonyl at 1639.37 cm-1 and CO at 1153.35 cm-1. 1H-NMR spectra showed a group monosubtituted benzene, benzene tetrasubstituted, proton of hydroxyl group, proton of methoxyl group, one proton oxyalkyl, and two protons alkyl. The spectroscopic data showed the compound is pinostrobin (5-hydroxy-7-metoxyiflavanone). The antioxidant activity (IC50) of the ethanol extracts from B. rotunda rhizome, pinostrobin, and ascorbic acid (positive control) were 92.6; 62.84; and 3.7 µg/mL repectively. The study showed that the ethanol extract of B. rotunda rhizome and bioactive compounds have high antioxidant activity, but their activity lower than ascorbic acid.

  19. Co- and counter-current spontaneous imbibition into groups of capillary tubes with lateral connections permitting cross-flow.

    PubMed

    Unsal, E; Mason, G; Ruth, D W; Morrow, N R

    2007-11-01

    A model for co- and counter-current imbibition through independent capillaries has already been developed and experiments conducted to verify the theory [E. Unsal, G. Mason, N.R. Morrow, D.W. Ruth, J. Colloid Interface Sci. 306 (2007) 105]. In this paper, the work is extended to capillaries which are connected laterally and in which cross-flow can take place. The fundamental pore geometry is a rod in an angled round-bottomed slot with a gap between the rod and a capping glass plate. The surfaces of the slot, rod and plate form capillaries and interconnecting passages which have non-axisymmetric cross-sections. Depending on the gap size either (i) a large single meniscus, (ii) two menisci one on each side of the rod, or (iii) three menisci, one between the rod and the glass additional to the ones on each side can be formed. A viscous refined oil was applied to one end of the capillaries and co-current and counter-current spontaneous imbibition experiments were performed. The opposite end was left open to the atmosphere for co-current experiments. When the gap between the rod and the plate was large, the imbibing oil advanced into the tubes with the meniscus in the largest capillary always lagging behind the two menisci in the other two smaller capillaries. For counter-current imbibition experiments the open end was sealed and connected to a sensitive pressure transducer. In some experiments, the oil imbibed into the smaller capillaries and expelled air as a series of bubbles from the end of the largest capillary. In other experiments, the oil was allowed to imbibe part way into the tubes before counter-current imbibition was started. The meniscus curvatures of the capillaries have been calculated using the Mayer and Stowe-Princen method for different cell slot angles and gap sizes using a value of zero for the contact angle. These values have been compared with actual values by measuring the capillary rise in the tubes; agreement was very close. A model for co

  20. Application of counter-current chromatography as a new pretreatment method for the determination of polycyclic aromatic hydrocarbons in environmental water.

    PubMed

    Cao, Xueli; Yang, Chunlei; Pei, Hairun; Li, Xinghong; Xu, Xiaobai; Ito, Yoichiro

    2012-02-01

    Counter-current chromatography (CCC) was investigated as a new sample pretreatment method for the determination of trace polycyclic aromatic hydrocarbons (PAHs) in water environmental samples. The experiment was performed with a non-aqueous binary two-phase solvent system composed of n-heptane and acetonitrile. The CCC column was first filled with the upper stationary phase, and then a large volume of water sample was pumped into the column while the CCC column was rotated at 1600 rpm. Finally, the trace amounts of PAHs extracted and enriched in the stationary phase were eluted out by the lower mobile phase and determined by gas chromatography-flame ionization detector (GC-FID) or gas chromatography-mass spectrometry (GC-MS). The enrichment and cleanup of PAHs can be fulfilled online by this method with high recoveries (84.1-103.2%) and good reproducibility (RSDs: 4.9-12.2%) for 16 EPA PAHs under the optimized CCC pretreatment conditions. This method has been successfully applied to determine PAHs in lake water where 8 PAHs were detected in the concentration of 40.9-89.9 ng/L. The present method is extremely suitable for the preparation of large volume of environmental water sample for the determination of trace amounts of organic pollutants including PAHs as studied in this paper.

  1. Separation of isorhamnetin 3-sulphate and astragalin from Flaveria bidentis (L.) Kuntze using macroporous resin and followed by high-speed countercurrent chromatography.

    PubMed

    Shaheen, Nusrat; Yin, Li; Gu, Yanxiang; Rwigimba, Eric; Xie, Qianqian; Wei, Yun

    2015-06-01

    D4020 resin offered the best dynamic adsorption and desorption capacity for total flavonoids based on the research results from ten kinds of macroporous resin. A column packed with D4020 resin was used to optimize the separation of total flavonoids from Flaveria bidentis (L.) Kuntze extracts. The content of flavonoids in the product was increased from 4.3 to 30.1% with a recovery yield of 90%. After the treatment with gradient elution on D4020 resin, the contents of isorhamnetin 3-sulfate and astragalin were increased from 0.49 to 8.70% with a recovery yield of 74.1% and 1.16 to 30.8%, with a recovery yield of 92.2%, respectively. Further purification was carried out by one-run high-speed countercurrent chromatography yielding 4.5 mg of isorhamnetin 3-sulfate at a high purity of 96.48% and yielding 24.4 mg of astragalin at a high purity of over 98.46%.

  2. Countercurrent chromatographic separation and purification of various ribonucleases using a small-scale cross-axis coil planet centrifuge with aqueous-aqueous polymer phase systems.

    PubMed

    Shinomiya, Kazufusa; Kobayashi, Hiroko; Motoyoshi, Naomi; Inokuchi, Norio; Nakagomi, Kazuya; Ito, Yoichiro

    2009-04-01

    Countercurrent chromatographic (CCC) separation and purification of various ribonucleases (RNases) was performed using the small-scale cross-axis coil planet centrifuge (X-axis CPC) with aqueous-aqueous polymer phase systems. RNases B and A were well resolved from each other with an aqueous-aqueous polymer phase system composed of 12.5% (w/w) polyethylene glycol (PEG) 1000 and 12.5% (w/w) dibasic potassium phosphate (pH 9.2) as the mobile lower phase. The commercial RNase A samples obtained from three different companies were also highly purified using the 16.0% (w/w) PEG 1000-6.3% (w/w) dibasic potassium phosphate-6.3% (w/w) monobasic potassium phosphate system (pH 6.6) using the upper phase as the mobile phase. Recombinant RNase Po(1), an RNase T(1) family enzyme, was further successfully separated from the crude extract using the same solvent system with the lower phase used as the mobile phase. The RNase activities were well preserved during the CCC separation. The overall results demonstrate that the small-scale X-axis CPC is useful for a simple and rapid purification of various RNases in a preparative-scale.

  3. Aqueous biphasic system based on low-molecular-weight polyethylene glycol for one-step separation of crude polysaccharides from Pericarpium granati using high-speed countercurrent chromatography.

    PubMed

    Zhou, Xin-Yu; Zhang, Jing; Xu, Rui-Ping; Ma, Xue; Zhang, Zhi-Qi

    2014-10-03

    The aqueous biphasic system (ABS) plays a key role in the separation of bioactive substances, and the establishment and application of a low-molecular-weight polyethylene glycol (PEG) ABS remains a challenge in high-speed countercurrent chromatography (HSCCC). In this work, an ABS of low-molecular-weight PEG, namely PEG400-Na2SO4-H2O (20%-16%-64%, w/w/w), was developed on the basis of the phase diagram, and the phase forming time and ratio, and applied to HSCCC for the separation of polysaccharides. The crude polysaccharide extracted from Pericarpium granati (PGP) was successfully separated and three purified polysaccharides were obtained: PGP-1, with an average molecular weight of 13,210Da and composed of xylose (12.4%), ribose (10.1%), and glucose (77.5%); PGP-2, which is a homogeneous polysaccharide with an average molecular weight of 2584Da and consists of mannose; and PGP-3, with an average molecular weight of 2459Da and composed of ribose (51.4%), mannose (26.7%), and glucose (21.9%). This success shows that an ABS based on low-molecular-weight PEG could be applied to HSCCC separation technology. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. PREPARATIVE ISOLATION AND PURIFICATION OF THREE GLYCINE-CONJUGATED CHOLIC ACIDS FROM PULVIS FELLIS SUIS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY COUPLED WITH ELSD DETECTION

    PubMed Central

    He, Jiao; Li, Jing; Sun, Wenji; Zhang, Tianyou; Ito, Yoichiro

    2011-01-01

    Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was developed for preparative isolation and purification of three glycine-conjugated cholic acids, glycochenodeoxycholic acid (GCDCA), glycohyodeoxycholic acid (GHDCA) and glycohyocholic acid (GHCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The separation was performed with a two-phase solvent system consisted of chloroform-methanol-water-acetic acid (65:30:10:1.5, v/v/v/v) by eluting the lower phase in the head-to-tail elution mode. The revolution speed of the separation column, flow rate of the mobile phase and separation temperature were 800 rpm, 2 ml/min and 25 °C, respectively. In a single operation, 33 mg of GCDCA, 38 mg of GHDCA and 23 mg of GHCA were obtained from 200 mg of crude extract with the purity of 95.65%, 96.72% and 96.63%, respectively, in one step separation. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the structures of the three glycine-conjugated cholic acids were identified by ESI-MS, 1H NMR and 13C NMR. PMID:23008527

  5. Changes in the mobile phase composition on a stepwise counter-current chromatography elution for the isolation of flavonoids from Siparuna glycycarpa.

    PubMed

    Costa, Fernanda das Neves; Garrard, Ian; da Silva, Antonio Jorge Ribeiro; Leitão, Gilda Guimarães

    2013-07-01

    This paper describes the isolation of flavonoids and other aromatic compounds from an ethyl acetate extract of leaves of Siparuna glycycarpa using stepwise elution counter-current chromatography (CCC). The elution profile yielded the following compounds: diglycosylated flavonoids, quercetin 3-O-rutinoside and quercetin 7-O-rutinoside, followed by monoglycosylated flavonoids, kaempferol-3-O-β-glucopyranoside, kaempferol-3-O-β-rhamnopiranoside, kaempferol-3-O-β-6''(p-coumaroyl) glucopyranoside, and quercetin-3-O-β-glucopyranoside, and then free phenolics, protocatechuic acid, and 2',6'-dihydroxy-4, 4'-dimethoxydihydrochalcone, which shows that this type of elution covers a broader range of polarity than the traditional isocratic mode. This makes it more suitable to perform separations of mixtures containing large differences in hydrophobicity. A GC analysis of a blank CCC run was performed to determine if changes in the mobile phase composition affect the chromatographic process. Results showed a gradual variation of the composition of the mobile phase emerging after the step gradient, favoring the selectivity of the solvent system.

  6. Bioassay-guided preparative separation of angiotensin-converting enzyme inhibitory C-flavone glycosides from Desmodium styracifolium by recycling complexation high-speed counter-current chromatography.

    PubMed

    Zhang, Ying-Qi; Luo, Jian-Guang; Han, Chao; Xu, Jin-Fang; Kong, Ling-Yi

    2015-01-01

    A new strategy of the convergence of high-speed counter-current chromatography (HSCCC) and bioactive assay technique was developed for rapidly screening and separating the angiotensin-converting enzyme (ACE) inhibitors from the aerial parts of Desmodium styracifolium. Bioactivity-guided fractionation of the crude extract was first established to target the bioactive fractions based on HSCCC coupled with in vitro ACE inhibitory assay. Subsequently, the bioactive fractions were further separated by the recycling complexation HSCCC respectively, using 0.10 mol/L copper sulfate in the lower phase of two-phase solvent system composed of n-butanol/water (1:1, v/v). Five C-glycosylflavones, vicenin 2 (1), carlinoside (2), vicenin 1 (3), schaftoside (4) and vicenin 3 (5), were successfully obtained. Their chemical structures were identified using ESI-MS and NMR. All the isolates showed in vitro ACE inhibitory activity with the IC50 values between 33.62 and 58.37 μM. The results demonstrated that the established method was proposed as an excellent strategy to systematically screen and purify active compounds from traditional Chinese medicines.

  7. Application of high-speed counter-current chromatography as a new pretreatment method for analysis of polycyclic aromatic hydrocarbons in environmental water samples

    PubMed Central

    Cao, Xueli; Yang, Chunlei; Pei, Hairun; Li, Xinghong; Xu, Xiaobai; Ito, Yoichiro

    2011-01-01

    High-speed counter-current chromatography (HSCCC) was investigated as a new sample pretreatment method for the analysis of trace polycyclic aromatic hydrocarbons (PAHs) in water environmental samples. The experiment was performed with a nonaqueous binary two-phase solvent system composed of heptane-acetonitrile. The HSCCC column was first entirely filled with the upper stationary phase of the and a large volume of water sample was pumped into the column while the CCC column was rotated at 1600 rpm. Finally, the trace amount of PAHs extracted and enriched in the stationary phase were eluted out by the lower mobile phase. and analyzed by gas chromatography-flame ionization detector (GC-FID) or gas chromatography-mass spectrometry (GC-MS) after concentration. The enrichment and cleanup of PAHs can be fulfilled online by this methodwithhigh recoveries (84.1%–103.2%) and good reproducibility (RSDs 4.9–12.2%) for 16 EPA PAHs under the optimized HSCCC pretreatment conditions. This method has been successfully applied to determine PAHs in lake waterwhere 8 PAHs were detected in the concentration of 40.9–89.9 ng/L. The present method is extremely suitable in the preparation of large volume of environmental water sample for the determination of a trace amount of organic pollutants including PAHs as studied in this paper. PMID:22282420

  8. Application of high-speed counter-current chromatography for isolation of triterpenes from Schisandra Chinensis (Turcz.) Baill and induction apoptosis mechanism of HSC-T6.

    PubMed

    Li, Bin; Meng, Xianjun; Zhu, Lijie; Jiao, Xinyao; Zhang, Jiachen

    2014-01-01

    Triterpenes have shown many beneficial activities in researches, but their separation and preparation usually require multiple methods. Following an initial cleaning-up step on the AB-8 macroporous resin, a preparative high-speed counter-current chromatography (HSCCC) with a two-phase solvent system comprising chloroform-n-butyl alcohol-methanol-water (10:1:7:4, v/v/v/v) was used to isolate and separate triterpenes from caculis of Schisandra Chinensis (Turcz.) baill. A total of 89 mg corosolic acid with purities of 98.5% were obtained from 400 mg crude extract in one-step elution and less than 4 h, and the structure identification was performed by UV, IR, MS, 1H NMR and 13C NMR. The inhibition on liver fibrosis activities of the triterpenes against HSC-T6 in vitro were studied by cell culture methods. The results showed that the corosolic acid have better inhibitory effects on HSC-T6 cells with the IC50 value of 5~25 μg/mL and the study also indicated that corosolic acid might be a potential Chinese medical component to inhibit liver fibrosis.

  9. Predictable and linear scale-up of four phenolic alkaloids separation from the roots of Menispermum dauricum using high-performance counter-current chromatography.

    PubMed

    Luo, Houding; Peng, Ming; Ye, Haoyu; Chen, Lijuan; Peng, Aihua; Tang, Minghai; Zhang, Fan; Shi, Jie

    2010-07-15

    This paper describes how distribution ratios were used for prediction of peak elution in analytical high-performance counter-current chromatography (HPCCC) to explore the method for separation and purification of bioactive compounds from the roots of Menispermum dauricum. Then important parameters related to HPCCC separations including solvent systems, sample concentration, sample loading volume and flow rate were optimized on an analytical Mini-DE HPCCC and finally linearly scaled up to a preparative Midi-DE HPCCC with nearly the same resolutions and separation time. Four phenolic alkaloids were for the first time obtained by HPCCC separation with a two-phase solvent system composed of petroleum ether-ethyl acetate-ethanol-water (1:2:1:2, v/v). This process produced 131.3 mg daurisolin, 197.1 mg dauricine, 32.4 mg daurinoline and 14.7 mg dauricicoline with the purity of 97.6%, 96.4%, 97.2% and 98.3%, respectively from 500 mg crude extract of the roots of M. dauricum in a one-step separation. The purities of compounds were determined by high-performance liquid chromatography (HPLC). Their structures were identified by electrospray ionization mass spectrometer (ESI-MS) and nuclear magnetic resonance (NMR).

  10. Preparative purification of bromelain (EC 3.4.22.33) from pineapple fruit by high-speed counter-current chromatography using a reverse-micelle solvent system.

    PubMed

    Yin, Lianhong; Sun, C K; Han, Xu; Xu, Lina; Xu, Youwei; Qi, Yan; Peng, Jinyong

    2011-12-01

    The crude protein of pineapple fruit was purified by high-speed counter-current chromatography (HSCCC). Excellent separation was achieved after careful investigation as follows: cetyltrimethylammonium bromide (CTAB) was selected to prepare the reverse micelle phase at the concentration of 0.10g/mL. The mobile phase was 0.05M sodium phosphate buffer solution, including mobile phase A (pH 9.5, containing 0.2M KCl) used for equilibration and mobile phase B (pH 7.0, containing 0.4M KCl) used for elution. The flow rate of the mobile phase was set at 1.5mL/min and the effluent was monitored at 280nm. Under these conditions, 127.3mg bromelain (EC 3.4.22.33) was produced from 200mg crude sample. A large-scale procedure was then carried out, and 3.01g bromelain was obtained from 5.00g crude extract in a 200min run. The separated protein was analysed by SDS-PAGE, compared with the standard and then identified by TOF/TOF-MS. Copyright © 2011 Elsevier Ltd. All rights reserved.

  11. Separation of polyphenols from leaves of Malus hupehensis (Pamp.) Rehder by off-line two-dimensional High Speed Counter-Current Chromatography combined with recycling elution mode.

    PubMed

    Liu, Qi; Zeng, Hualiang; Jiang, Shujing; Zhang, Li; Yang, Fuzhu; Chen, Xiaoqing; Yang, Hua

    2015-11-01

    In this study, off-line two-dimensional High Speed Counter-Current Chromatography (2D HSCCC) strategy combined with recycling elution mode was developed to isolate compounds from the ethyl acetate extract of a common green tea--leaves of Malus hupehensis (Pamp.) Rehder. In the orthogonal separation system, a conventional HSCCC was employed for the first dimension and two recycling HSCCCs were used for the second in parallel. Using a solvent system consisting of n-hexane-ethyl acetate-methanol-water (1:4:0.6:4.4, v/v) in the first and second dimension, four compounds including 3-hydroxy-phlorizin (1), phloretin (2), avicularin (3) and kaempferol 3-O-β-D-glucoside (4) were obtained. The purities of these four compounds were all over 95.0% as determined by HPLC. And their structures were all identified through UV, MS and (1)H NMR. It has been demonstrated that the combination of off-line 2D HSCCC with recycling elution mode is an efficient technique to isolate compounds with similar polarities in natural products.

  12. Isolation of bioactive components from Flaveria bidentis (L.) Kuntze using high-speed counter-current chromatography and time-controlled collection method.

    PubMed

    Wei, Yun; Zhang, Kai; Yin, Li; Du, Jilin; Zhang, Guoliang

    2012-04-01

    Semipreparative high-speed counter-current chromatography (HSCCC) by time-controlled collection method was successfully applied for isolation and purification of α-terthienyl, 5-(3-buten-1-ynyl)-2,2'-bithienyl, and 5-(3-penten-1-ynyl)-2,2'-bithienyl from Flaveria bidentis (L.) Kuntze for the first time. The two-phase solvent system composed of n-hexane and acetonitrile at the volume ratio of 1:1 (v/v) was used for the semipreparative HSCCC. The 5.2 mg α-terthienyl, 2.2 mg 5-(3-buten-1-ynyl)-2,2'-bithienyl, and 4.3 mg 5-(3-penten-1-ynyl)-2,2'-bithienyl with the purity of 99.9, 90.2, and 92.1% were produced from 265.6 mg crude extract, respectively, and 5-(3-penten-1-ynyl)-2,2'-bithienyl was first isolated from Flaveria bidentis (L.) Kuntze. The structures of the separated compounds were identified by electrospray-ionization mass spectrometry and proton and carbon nuclear magnetic resonance ((1)H- and (13)C-NMR).

  13. Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography.

    PubMed

    Ye, Haoyu; Chen, Lijuan; Li, Yanfang; Peng, Aihua; Fu, Afu; Song, Hang; Tang, Minghai; Luo, Houding; Luo, Youfu; Xu, Yongbin; Shi, Jianyou; Wei, Yuquan

    2008-01-18

    Both analytical and preparative high-speed counter-current chromatography (HSCCC) were used to isolate and separate chemical bioactive constituents from the seeds of Millettia pachycarpa Benth, a famous traditional Chinese medicine. Three rotenoids and one isoflavone were successfully purified for the first time by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (HEMWat) (1:0.8:1:0.6, v/v/v/v). The separation parameters were first performed on the analytical HSCCC and optimized conditions were then scaled up to preparative HSCCC. The separation produced 160.2 mg tephrosin, 14.6 mg 4',5'-dimethoxy-6,6-dimethylpyranoisoflavone, 109.4 mg deguelin, 6.7 mg 6a,12a-dehydrodeguelin with respective purities of 95, 93, 95, 95%, in one single run from 400 mg crude extract of the seeds of M. pachycarpa Benth. The purity of the isolated compounds was analyzed by high-performance liquid chromatography (HPLC) and their structures were identified by electrospray ionization mass spectrometry (ESI-MS); (1)H nuclear magnetic resonance ((1)H NMR) and (13)C nuclear magnetic resonance ((13)C NMR) analysis. This paper is an excellent example of the role that CCC is playing in isolating active compounds for pre-clinical trials of new chemical entities, even when scaling up between centrifuges from different manufacturers.

  14. Isolation of aspalathin and nothofagin from rooibos (Aspalathus linearis) using high-performance countercurrent chromatography: sample loading and compound stability considerations.

    PubMed

    de Beer, Dalene; Malherbe, Christiaan J; Beelders, Theresa; Willenburg, Elize L; Brand, D Jacobus; Joubert, Elizabeth

    2015-02-13

    Aspalathin and nothofagin, the major dihydrochalcones in rooibos (Aspalathus linearis), are valuable bioactive compounds, but their bioactivity has not been fully elucidated. Isolation of these compounds using high-performance countercurrent chromatography (HPCCC), a gentle, support-free, up-scalable technique, offers an alternative to synthesis for obtaining sufficient amounts. An HPLC-DAD method was adapted to allow rapid (16 min from injection to injection) quantification of the four major compounds (aspalathin, nothofagin, isoorientin, orientin) during development of the isolation protocol. The traditional shake-flask method, used to determine distribution constants (K(D)) for target compounds, was also adapted to obtain higher repeatability. Green rooibos leaves with a high aspalathin and nothofagin content were selected as source material. Sample loading of the polyphenol-enriched extract was limited due to constituents with emulsifying properties, but could be increased by removing ethanol-insoluble matter. Furthermore, problems with degradation of aspalathin during HPCCC separation and further processing could be limited by acidifying the HPCCC solvent system. Aspalathin was shown to be fairly stable at pH 3 (91% remaining after 29 h) compared to pH 7 (45% remaining after 29 h). Aspalathin and nothofagin with high purities (99% and 100%, respectively) were obtained from HPCCC fractions after semi-preparative HPLC.

  15. Simulating ion beam extraction from a single aperture triode acceleration column: A comparison of the beam transport codes IGUN and PBGUNS with test stand data

    SciTech Connect

    Patel, A.; Wills, J. S. C.; Diamond, W. T.

    2008-04-15

    Ion beam extraction from two different ion sources with single aperture triode extraction columns was simulated with the particle beam transport codes PBGUNS and IGUN. For each ion source, the simulation results are compared to experimental data generated on well-equipped test stands. Both codes reproduced the qualitative behavior of the extracted ion beams to incremental and scaled changes to the extraction electrode geometry observed on the test stands. Numerical values of optimum beam currents and beam emittance generated by the simulations also agree well with test stand data.

  16. Aqueous biphasic extraction of uranium and thorium from contaminated soils. Final report

    SciTech Connect

    Chaiko, D.J.; Gartelmann, J.; Henriksen, J.L.; Krause, T.R.; Deepak; Vojta, Y.; Thuillet, E.; Mertz, C.J.

    1995-07-01

    The aqueous biphasic extraction (ABE) process for soil decontamination involves the selective partitioning of solutes and fine particulates between two immiscible aqueous phases. The biphase system is generated by the appropriate combination of a water-soluble polymer (e.g., polyethlene glycol) with an inorganic salt (e.g., sodium carbonate). Selective partitioning results in 99 to 99.5% of the soil being recovered in the cleaned-soil fraction, while only 0.5 to 1% is recovered in the contaminant concentrate. The ABE process is best suited to the recovery of ultrafine, refractory material from the silt and clay fractions of soils. During continuous countercurrent extraction tests with soil samples from the Fernald Environmental Management Project site (Fernald, OH), particulate thorium was extracted and concentrated between 6- and 16-fold, while the uranium concentration was reduced from about 500 mg/kg to about 77 mg/kg. Carbonate leaching alone was able to reduce the uranium concentration only to 146 mg/kg. Preliminary estimates for treatment costs are approximately $160 per ton of dry soil. A detailed flowsheet of the ABE process is provided.

  17. ANTIFERTILITY EFFICACY OF CURCUMA LONGA (50% E to H EXTRACT) WITH SPECIAL REFERANCE TO SERUM BIOCHEMISTRY and FERTILITY TEST

    PubMed Central

    Purohit, Ashok

    1999-01-01

    Oral feeding of 50% EtOH extract of Curcuma longa to male rats at the dose of 1gm/kg body weight caused significant reduction of serum cholesterol, triglycerides and phospholipids (P≤0.01 to 0.001). Whereas the SGOT levels aware not reduced significantly. Fertility test showed 80% negative result. The negative fertility results reflects the arrest of spermatogenesis and depletion of androgen level. Further Curcuma longa reflects antispermatogenic nature. PMID:22556889

  18. Test in canine extraction site preservations by using mineralized collagen plug with or without membrane.

    PubMed

    Sun, Yi; Wang, Cheng-Yue; Wang, Zhi-Ying; Cui, Yun; Qiu, Zhi-Ye; Song, Tian-Xi; Cui, Fu-Zhai

    2016-04-01

    The aim of this study was to discuss the feasibility of porous mineralized collagen plug and bilayer mineralized collagen-guided bone regeneration membrane in site preservation in extraction sockets. The third mandibular premolars on both sides were extracted from four dogs, thus there were 16 alveolar sockets in all dogs and were randomly assigned into three groups. Group A had six alveolar sockets, and groups B and C had five alveolar sockets, respectively. Each alveolar socket of group A was immediately implanted with a porous mineralized collagen plug and covered with a bilayer mineralized collagen-guided bone regeneration membrane after tooth extraction. Alveolar sockets of group B were implanted with porous mineralized collagen plug only, and group C was set as blank control without any implantation. The healing effects of the extraction sockets were evaluated by gross observation, morphological measurements, and X-ray micro-computed tomography after twelve weeks. Twelve weeks after operation, both groups A and B had more amount of new bone formation compared with group C; in terms of the degree of alveolar bone height, group A was lower than groups B and C with significant differences; the bone mineral density in the region of interest and bone remodeling degree in group A were higher than those of groups B and C. As a result, porous mineralized collagen plug could induce the regeneration of new bone in extraction socket, and combined use of porous mineralized collagen plug and bilayer mineralized collagen guided bone regeneration membrane could further reduce the absorption of alveolar ridge and preserve the socket site.

  19. Heat production in depth up to 2500m via in situ combustion of methane using a counter-current heat-exchange reactor

    NASA Astrophysics Data System (ADS)

    Schicks, Judith Maria; Spangenberg, Erik; Giese, Ronny; Heeschen, Katja; Priegnitz, Mike; Luzi-Helbing, Manja; Thaler, Jan; Abendroth, Sven; Klump, Jens

    2014-05-01

    In situ combustion is a well-known method used for exploitation of unconventional oil deposits such as heavy oil/bitumen reservoirs where the required heat is produced directly within the oil reservoir by combustion of a small percentage of the oil. A new application of in situ combustion for the production of methane from hydrate-bearing sediments was tested at pilot plant scale within the first phase of the German national gas hydrate project SUGAR. The applied method of in situ combustion was a flameless, catalytic oxidation of CH4 in a counter-current heat-exchange reactor with no direct contact between the catalytic reaction zone and the reservoir. The catalyst permitted a flameless combustion of CH4 with air to CO2 and H2O below the auto-ignition temperature of CH4 in air (868 K) and outside the flammability limits. This led to a double secured application of the reactor. The relatively low reaction temperature allowed the use of cost-effective standard materials for the reactor and prevented NOx formation. Preliminary results were promising and showed that only 15% of the produced CH4 was needed to be catalytically burned to provide enough heat to dissociate the hydrates in the environment and release CH4. The location of the heat source right within the hydrate-bearing sediment is a major advantage for the gas production from natural gas hydrates as the heat is generated where it is needed without loss of energy due to transportation. As part of the second period of the SUGAR project the reactor prototype of the first project phase was developed further to a borehole tool. The dimensions of this counter-current heat-exchange reactor are about 540 cm in length and 9 cm in diameter. It is designed for applications up to depths of 2500 m. A functionality test and a pressure test of the reactor were successfully carried out in October 2013 at the continental deep drilling site (KTB) in Windischeschenbach, Germany, in 600 m depth and 2000 m depth, respectively

  20. Specific testing for "isolated" anti-52 kDa SSA/Ro antibodies during standard anti-extractable nuclear antigen testing is of limited clinical value.

    PubMed

    Langguth, Daman M; Morris, Samantha; Clifford, Lynette; Wilson, Robert J; Neil, John; Hogan, Patrick G; Wong, Richard C W

    2007-06-01

    To ascertain whether specific testing for "isolated" anti-52 kDa SSA/Ro antibodies (a-SSA/Ro52) during standard anti-extractable nuclear antigen (ENA) testing is clinically useful. 1438 consecutive sera submitted for anti-ENA testing over 1 year were evaluated for a-SSA/Ro52 using various assays. 7 of 1438 (0.48%) patients were found to have a-SSA/Ro52 without SSA/Ro60 antibodies. Subsequent testing detected a further five patients. Clinical follow-up was possible in 10/12 patients. 2 of these 10 patients had evidence of primary Sjögren's syndrome (SS) and one had systemic lupus erythematosus (SLE), with sicca symptoms and abnormal Schirmer's tests. Five other patients had sicca symptoms, of which four had abnormal Schirmer's tests. "Isolated" anti-52 kDa SSA/Ro antibodies were detected in approximately 0.5% of standard anti-ENA requests, in which their presence was generally not associated with underlying SS or SLE. In view of the increased testing complexity and costs in detecting and confirming these antibodies, specific testing for isolated a-SSA Ro52 antibodies during standard anti-ENA testing seems to be of limited clinical value in a non-obstetric population.

  1. Separation of epimeric aromatic acid (-)-menthol esters by countercurrent chromatography using hydroxypropyl-β-cyclodextrin as an additive.

    PubMed

    Wang, Xiaoping; Lv, Liqiong; Bu, Zhisi; Yan, Jizhong; Tong, Shengqiang

    2017-02-28

    The separation of ten epimeric aromatic acid (-)-menthol esters by countercurrent chromatography with hydroxypropyl-β-cyclodextrin as the mobile phase additive was investigated, and methods for the analysis of all the epimeric esters by reversed-phase high-performance liquid chromatography were established. A biphasic solvent system composed of n-hexane/20-70% methanol containing 50 mmol/L of hydroxypropyl-β-cyclodextrin (1:1, v/v) was selected, which provided high separation factors for five of the epimeric esters, and successful separations by countercurrent chromatography were achieved. The complete separation of five pairs of epimeric ester was obtained with the purity being over 98% for each peak fractions, as determined by high-performance liquid chromatography. The recovery of each analyte from the eluted fractions reached around 80-88%.

  2. The contribution of nasal countercurrent heat exchange to water balance in the northern elephant seal, Mirounga angustirostris.

    PubMed

    Huntley, A C; Costa, D P; Rubin, R D

    1984-11-01

    Elephant seals fast completely from food and water for 1-3 months during terrestrial breeding. Temporal countercurrent heat exchange in the nasal passage reduces expired air temperature (Te) below body temperature (Tb). At a mean ambient temperature of 13.7 degrees C, Te is 20.9 degrees C. This results in the recovery of 71.5% of the water added to inspired air. The amount of cooling of the expired air (Tb - Te) and the percentage of water recovery varies inversely with ambient temperature. Total nasal surface area available for heat and water exchange, located in the highly convoluted nasal turbinates, is estimated to be 720 cm2 in weaned pups and 3140 cm2 in an adult male. Nasal temporal countercurrent heat exchange reduces total water loss sufficiently to allow maintenance of water balance using metabolic water production alone.

  3. [Sensitivity and specificity of prick skin test with two concentrations of standardized extract of Culex quinquefasciatus in allergic children].

    PubMed

    Castro-Almarales, Raúl Lázaro; Álvarez-Castelló, Mirta; Ronquillo-Díaz, Mercedes; Rodríguez-Canosa, José S; González-León, Mayda; Navarro-Viltre, Bárbara I; Betancourt-Mesia, Daniel; Enríquez-Domínguez, Irene; Reyes-Zamora, Mary Carmen; Oliva-Díaz, Yunia; Mateo-Morejón, Maytee; Labrada-Rosado, Alexis

    2016-01-01

    Diagnostic options for immune reactions to mosquito bites are limited. In Cuba, IgE-mediated reactions are frequently related to Culex quinquefasciatus bite. To determine the sensitivity and specificity of skin prick test with two doses of standardized extract in nitrogen protein units (PNU of Culex quinquefasciatus (BIOCEN, Cuba). An analytical study was conducted on 100 children between 2 and 15 years old. Fifty atopic patients with a history of allergy to mosquito bite and positive specific serum IgE Culex quinquefasciatus and fifty atopic patients without a history of allergy to mosquito bite and negative specific serum IgE to Culex quinquefasciatus. Skin prick tests (SPT) were performed by duplicates on the forearms of the patients. Investigated doses were 100 PNU/mL and 10 PNU/mL. SPT with the highest concentration obtained a mean wheal size of 22.09 mm2 and for lower doses of 8.09 mm2, a statistically significant difference (p=0.001, Student's t test). Positive skin test correlated in 100% of patients with the presence of specific IgE. Testing with both doses showed a 94% of specificity and 88% of sensitivity. The diagnostic accuracy of SPT using both doses of standardized extract was similar, which justifies its use for diagnosis of sensitization to Culex quinquefasciatus in patients with symptoms of allergy to mosquito bite.

  4. Continuing Assessment of the 5-Day Sodium Carbonate-Ammonium Nitrate Extraction Assay as an Indicator Test for Silicon Fertilizers.

    PubMed

    Zellner, Wendy; Friedrich, Russell L; Kim, Sujin; Sturtz, Douglas; Frantz, Jonathan; Altland, James; Krause, Charles

    2015-01-01

    The 5-day sodium carbonate-ammonium nitrate extraction assay (5-day method) has been recognized by the American Association of Plant Food Control Officials as a validated test method to identify fertilizers or beneficial substances that provide plant-available silicon (Si). The test method used the molybdenum blue colorimetric assay to quantify percentage Si; however, laboratories may use inductively coupled plasma optical emission spectroscopy (ICP-OES) for elemental analysis. To examine the use of either colorimetric or ICP-OES methods for Si determination, the 5-day method was performed on the following Si-containing compounds; wollastonite, sand, biochar, and a basic oven furnace (BOF) slag. Grow-out studies using Zinnia elegans were also performed using varying rates of the wollastonite, biochar, and BOF slag. Our results show using the 5-day method, wollastonite had the highest extracted amounts of silicic acid (H4SiO4) at 4% followed by biochar (2%), BOF slag (1%), and sand (0%). Extraction values calculated using either the molybdenum blue colorimetric assay or ICP-OES for detection of the H4SiO4 had a significant correlation, supporting the application of either detection method for this type of analysis. However, when extracted values were compared to amounts of Si taken up by the plants, the 5-day method overestimated both wollastonite and biochar. While this method is a valid indicator test for determining a soluble Si source, other plant species and methods should be perused to potentially provide more quantitative analyses for plant-available Si content of all materials.

  5. Study of the genotoxicity of organic extracts from wastewater-irrigated vegetables using in vitro and in vivo biological tests.

    PubMed

    Gao, Hongxia; Cao, Yanhua; Liu, Yingli; Liu, Nan; Guan, Weijun

    2017-03-01

    The purpose of this study was to explore genotoxicity due to organic pollutants in wastewater-irrigated vegetables using biological and chemical analyses. Chinese cabbages from wastewater-irrigated farmland were taken as the research object. For the in vitro test, DNA damage was characterized in rat hepatocytes exposed to organic extracts from the cabbages using the comet assay. For the in vivo tests, mice were exposed to organic extracts from the cabbages. DNA damage was assessed in mouse peripheral blood lymphocytes (PBLs), and chromosome damage was assessed in bone marrow cells using the comet assay and micronucleus test, respectively. For the chemical analysis, gas chromatography-mass spectrometry (GC/MS) was used to analyze the organic compounds in the organic vegetable extracts. The in vitro test results showed that the comet tail lengths of the DNA in rat hepatocytes were significantly increased in the group dosed with 0.36 g/ml (P < 0.05), and the comet tailing rates of the hepatocytes were significantly increased in the groups dosed with 0.24 and 0.36 g/ml (P < 0.05). The in vivo test results indicated that the comet tail lengths of the DNA in mouse PBLs were increased in the low- and high-dose groups and that the comet tailing rate of the PBLs was increased in the high-dose group (P < 0.05). The chemical analysis results showed that the total organic content in the organic vegetable extracts from the wastewater-irrigated area (1.355 mg/kg) was significantly higher than the content in the cabbage samples from the clean-water-irrigated area (0.089 mg/kg). This finding indicated that wastewater irrigation can cause organic pollution with genetic toxicity in vegetables. This study also showed that in vivo and in vitro biological tests can reflect the joint toxicity of organic pollutants, and the test results were in accordance with the chemical analysis of the organic pollutant compositions.

  6. Toxicity of sediments potentially contaminated by coal mining and natural gas extraction to unionid mussels and commonly tested benthic invertebrates.

    PubMed

    Wang, Ning; Ingersoll, Christopher G; Kunz, James L; Brumbaugh, William G; Kane, Cindy M; Evans, R Brian; Alexander, Steven; Walker, Craig; Bakaletz, Steve

    2013-01-01

    Sediment toxicity tests were conducted to assess potential effects of contaminants associated with coal mining or natural gas extraction activities in the upper Tennessee River basin and eastern Cumberland River basin in the United States. Test species included two unionid mussels (rainbow mussel, Villosa iris, and wavy-rayed lampmussel, Lampsilis fasciola, 28-d exposures), and the commonly tested amphipod, Hyalella azteca (28-d exposure) and midge, Chironomus dilutus (10-d exposure). Sediments were collected from seven test sites with mussel communities classified as impacted and in proximity to coal mining or gas extraction activities, and from five reference sites with mussel communities classified as not impacted and no or limited coal mining or gas extraction activities. Additional samples were collected from six test sites potentially with high concentrations of polycyclic aromatic hydrocarbons (PAHs) and from a test site contaminated by a coal ash spill. Mean survival, length, or biomass of one or more test species was reduced in 10 of 14 test samples (71%) from impacted areas relative to the response of organisms in the five reference samples. A higher proportion of samples was classified as toxic to mussels (63% for rainbow mussels, 50% for wavy-rayed lampmussels) compared with amphipods (38%) or midge (38%). Concentrations of total recoverable metals and total PAHs in sediments did not exceed effects-based probable effect concentrations (PECs). However, the survival, length, or biomasses of the mussels were reduced significantly with increasing PEC quotients for metals and for total PAHs, or with increasing sum equilibrium-partitioning sediment benchmark toxic units for PAHs. The growth of the rainbow mussel also significantly decreased with increasing concentrations of a major anion (chloride) and major cations (calcium and magnesium) in sediment pore water. Results of the present study indicated that (1) the findings from laboratory tests were generally

  7. Toxicity of sediments potentially contaminated by coal mining and natural gas extraction to unionid mussels and commonly tested benthic invertebrates

    USGS Publications Warehouse

    Wang, Ning; Ingersoll, Christopher G.; Kunz, James L.; Brumbaugh, William G.; Kane, Cindy M.; Evans, R. Brian; Alexander, Steven; Walker, Craig; Bakaletz, Steve

    2013-01-01

    Sediment toxicity tests were conducted to assess potential effects of contaminants associated with coal mining or natural gas extraction activities in the upper Tennessee River basin and eastern Cumberland River basin in the United States. Test species included two unionid mussels (rainbow mussel, Villosa iris, and wavy-rayed lampmussel, Lampsilis fasciola, 28-d exposures), and the commonly tested amphipod, Hyalella azteca (28-d exposure) and midge, Chironomus dilutus (10-d exposure). Sediments were collected from seven test sites with mussel communities classified as impacted and in proximity to coal mining or gas extraction activities, and from five reference sites with mussel communities classified as not impacted and no or limited coal mining or gas extraction activities. Additional samples were collected from six test sites potentially with high concentrations of polycyclic aromatic hydrocarbons (PAHs) and from a test site contaminated by a coal ash spill. Mean survival, length, or biomass of one or more test species was reduced in 10 of 14 test samples (71%) from impacted areas relative to the response of organisms in the five reference samples. A higher proportion of samples was classified as toxic to mussels (63% for rainbow mussels, 50% for wavy-rayed lampmussels) compared with amphipods (38%) or midge (38%). Concentrations of total recoverable metals and total PAHs in sediments did not exceed effects-based probable effect concentrations (PECs). However, the survival, length, or biomasses of the mussels were reduced significantly with increasing PEC quotients for metals and for total PAHs, or with increasing sum equilibrium-partitioning sediment benchmark toxic units for PAHs. The growth of the rainbow mussel also significantly decreased with increasing concentrations of a major anion (chloride) and major cations (calcium and magnesium) in sediment pore water. Results of the present study indicated that (1) the findings from laboratory tests were generally

  8. Pore-water extraction from unsaturated tuff by triaxial and one-dimensional compression methods, Nevada Test Site, Nevada

    USGS Publications Warehouse

    Mower, Timothy E.; Higgins, Jerry D.; Yang, In C.; Peters, Charles A.

    1994-01-01

    Study of the hydrologic system at Yucca Mountain, Nevada, requires the extraction of pore-water samples from welded and nonwelded, unsaturated tuffs. Two compression methods (triaxial compression and one-dimensional compression) were examined to develop a repeatable extraction technique and to investigate the effects of the extraction method on the original pore-fluid composition. A commercially available triaxial cell was modified to collect pore water expelled from tuff cores. The triaxial cell applied a maximum axial stress of 193 MPa and a maximum confining stress of 68 MPa. Results obtained from triaxial compression testing indicated that pore-water samples could be obtained from nonwelded tuff cores that had initial moisture contents as small as 13 percent (by weight of dry soil). Injection of nitrogen gas while the test core was held at the maximum axial stress caused expulsion of additional pore water and reduced the required initial moisture content from 13 to 11 percent. Experimental calculations, together with experience gained from testing moderately welded tuff cores, indicated that the triaxial cell used in this study could not apply adequate axial or confining stress to expel pore water from cores of densely welded tuffs. This concern led to the design, fabrication, and testing of a one-dimensional compression cell. The one-dimensional compression cell used in this study was constructed from hardened 4340-alloy and nickel-alloy steels and could apply a maximum axial stress of 552 MPa. The major components of the device include a corpus ring and sample sleeve to confine the sample, a piston and base platen to apply axial load, and drainage plates to transmit expelled water from the test core out of the cell. One-dimensional compression extracted pore water from nonwelded tuff cores that had initial moisture contents as small as 7.6 percent; pore water was expelled from densely welded tuff cores that had initial moisture contents as small as 7

  9. Creating a flipbook as a medium of instruction based on the research on activity test of kencur extract

    NASA Astrophysics Data System (ADS)

    Monika, Icha; Yeni, Laili Fitri; Ariyati, Eka

    2016-02-01

    This research aimed to reveal the validity of the flipbook as a medium of learning for the sub-material of environmental pollution in the tenth grade based on the results of the activity test of kencur (Kaempferia galanga) extract to control the growth of the Fusarium oxysporum fungus. The research consisted of two stages. First, testing the validity of the medium of flipbook through validation by seven assessors and analyzed based on the total average score of all aspects. Second, testing the activity of the kencur extract against the growth of Fusarium oxysporum by using the experimental method with 10 treatments and 3 repetitions which were analyzed using one-way analysis of variance (ANOVA) test. The making of the flipbook medium was done through the stages of analysis for the potential and problems, data collection, design, validation, and revision. The validation analysis on the flipbook received an average score of 3.7 and was valid to a certain extent, so it could be used in the teaching and learning process especially in the sub-material of environmental pollution in the tenth grade of the senior high school.

  10. The agar microdilution method - a new method for antimicrobial susceptibility testing for essential oils and plant extracts.

    PubMed

    Golus, J; Sawicki, R; Widelski, J; Ginalska, G

    2016-11-01

    To develop a new agar microdilution technique suitable for the assessment of the antimicrobial activity of natural plant products such as essential oils or plant extracts as well as to evaluate the antimicrobial effect of several essential oils and plant extracts. The proposed agar microdilution method was evolved on the basis of the CLSI agar dilution method, approved for conventional antimicrobials. However, this new method combines convenience and time/cost effectiveness typical for microtitre methods with the advantages of the agar dilution of hydrophobic or coloured substances. Different concentrations of the tested agents were added to Eppendorf tubes with molten Mueller-Hinton agar, vortexed and dispensed into the 96-well microplate in a small volume of 100 μl per well which allows for rapid, easy and economical preparation of samples as well as providing a uniform and stable dispersion without separation of the oil-water phases which occurs in methods with liquid medium. Next, the agar microdilution plates were inoculated with four reference bacterial strains. The results of our study demonstrated that the minimal inhibitory concentrations (MICs) were successfully determined using the agar microdilution method even with hydrophobic essential oils or strongly coloured plant extracts. The new agar microdilution method avoids the problems associated with testing of water insoluble, oily or strongly coloured plant natural products. Moreover, it enables the reliable, cheap and easy MIC determination of such agents. In the era of increasing antibiotic resistance high hopes are associated with new drugs of plant origin. However, the lack of standardized and reliable testing methods for assessing antibacterial activity of plant natural products causes impediment to research into this area. This study demonstrated that the agar microdilution method can be used successfully for testing oily and coloured substances. © 2016 The Society for Applied Microbiology.

  11. Correlation between skin prick test using commercial extract of cow's milk protein and fresh milk and food challenges.

    PubMed

    Calvani, Mauro; Mauro, Calvani; Alessandri, Claudia; Claudia, Alessandri; Frediani, Tullio; Tullio, Frediani; Lucarelli, Sandra; Sandra, Lucarelli; Miceli Sopo, Stefano; Stefano, Miceli Sopo; Panetta, Valentina; Valentina, Panetta; Zappalã, Daniela; Daniela, Zappala'; Zicari, Anna Maria; Maria, Zicari Anna

    2007-11-01

    The skin prick test (SPT) is regarded as an important diagnostic measure in the diagnostic work-up of cow's milk protein allergy. It is not known whether commercial extracts have any advantage over fresh milk. The aims of the study were to (i) compare the diagnostic capacity of SPTs for the three main cow's milk proteins (alpha-lactalbumin, casein and beta-lactoglobulin) with fresh milk and (ii) determine a cut-off that discriminates between allergic and tolerant children in a controlled food challenge. A study was carried out on 104 children consecutively attending two paediatric allergy clinics for suspected cow's milk allergy. A clinical history, SPTs with fresh cow's milk and commercial extracts of its three main proteins and a challenge test were performed on all the children. A study of the validity of the prick test was also performed by taking different cut-off points for fresh milk and its proteins. Twenty-eight of 104 challenge tests (26.9%) were positive. At a cut-off point of 3 mm, fresh milk showed the greatest negative predictive value (98%), whereas casein showed the greatest positive predictive value (PPV, 85%). Calculation of 95% predicted probabilities using logistic regression revealed predictive decision points of 12 mm for lactalbumin, 9 mm for casein, 10 mm for beta-lactoglobulin and 15 mm for fresh cow's milk. We found that the greater the number of positive SPTs for milk proteins, the more likely the positive response to challenge. Having a positive SPT for all three milk proteins had PPV of 92.3% and would seem more clinically useful than any cut-off. Both fresh milk and cow's milk extract of the three main proteins could be useful in the diagnostic work-up of cow's milk allergy. Finding positivity to all three cow's milk proteins seems to be a simpler and more useful way of avoiding oral food challenges.

  12. K-Targeted Metabolomic Analysis Extends Chemical Subtraction to DESIGNER Extracts: Selective Depletion of Extracts of Hops (Humulus lupulus)⊥

    PubMed Central

    2015-01-01

    This study introduces a flexible and compound targeted approach to Deplete and Enrich Select Ingredients to Generate Normalized Extract Resources, generating DESIGNER extracts, by means of chemical subtraction or augmentation of metabolites. Targeting metabolites based on their liquid–liquid partition coefficients (K values), K targeting uses countercurrent separation methodology to remove single or multiple compounds from a chemically complex mixture, according to the following equation: DESIGNER extract = total extract ± target compound(s). Expanding the scope of the recently reported depletion of extracts by immunoaffinity or solid phase liquid chromatography, the present approach allows a more flexible, single- or multi-targeted removal of constituents from complex extracts such as botanicals. Chemical subtraction enables both chemical and biological characterization, including detection of synergism/antagonism by both the subtracted targets and the remaining metabolite mixture, as well as definition of the residual complexity of all fractions. The feasibility of the DESIGNER concept is shown by K-targeted subtraction of four bioactive prenylated phenols, isoxanthohumol (1), 8-prenylnaringenin (2), 6-prenylnaringenin (3), and xanthohumol (4), from a standardized hops (Humulus lupulus L.) extract using specific solvent systems. Conversely, adding K-targeted isolates allows enrichment of the original extract and hence provides an augmented DESIGNER material. Multiple countercurrent separation steps were used to purify each of the four compounds, and four DESIGNER extracts with varying depletions were prepared. The DESIGNER approach innovates the characterization of chemically complex extracts through integration of enabling technologies such as countercurrent separation, K-by-bioactivity, the residual complexity concepts, as well as quantitative analysis by 1H NMR, LC-MS, and HiFSA-based NMR fingerprinting. PMID:25437744

  13. Scale-up protein separation on stainless steel wide bore toroidal columns in the type-J counter-current chromatography.

    PubMed

    Guan, Yue Hugh; Hewitson, Peter; van den Heuvel, Remco N A M; Zhao, Yan; Siebers, Rick P G; Zhuang, Ying-Ping; Sutherland, Ian

    2015-12-11

    Manufacturing high-value added biotech biopharmaceutical products (e.g. therapeutic proteins) requires quick-to-develop, GMP-compliant, easy-to-scale and cost effective preparatory chromatography technologies. In this work, we describe the construction and testing of a set of 5-mm inner diameter stainless steel toroidal columns for use on commercially available preparatory scale synchronous J-type counter-current chromatography (CCC) machinery. We used a 20.2m long column with an aqueous two-phase system containing 14% (w/w) PEG1000 and 14% (w/w) potassium phosphate at pH 7, and tested a sample loading of 5% column volume and a mobile phase flow rate of 20ml/min. We then satisfactorily demonstrated the potential for a weekly protein separation and preparation throughput of ca. 11g based on a normal weekly routine for separating a pair of model proteins by making five stacked injections on a single portion of stationary phase with no stripping. Compared to our previous 1.6mm bore PTFE toroidal column, the present columns enlarged the nominal column processing throughput by nearly 10. For an ideal model protein injection modality, we observed a scaling up factor of at least 21. The 2 scales of protein separation and purification steps were realized on the same commercial CCC device.

  14. Investigation of urban atmospheric visibility by high-frequency extraction: Model development and field test

    NASA Astrophysics Data System (ADS)

    Luo, Chin-Hsiang; Wen, Che-Yen; Yuan, Chung-Shin; Liaw, Jiun-Jian; Lo, Cho-Ching; Chiu, Shih-Hsuan

    This work investigates atmospheric visibility by employing two statistical processes for high-frequency extraction: Sobel operator and fast Fourier transform (FFT). In replacing the traditional measurement methods for atmospheric visibility, the new approaches can provide accurate digital data urban visibility by establishing the numerical indices. The procedure is illustrated as follows. Digital images of urban areas in Kaohsiung, a city at the south of Taiwan, are analyzed according to brightness. High-frequency components of the image are extracted to calculate the index values by employing the Sobel operator and FFT. Finally, the correlation between each index and the visual range estimated by trained investigators are evaluated. A good correlation between two indices and the values obtained by visual investigation is affirmed by correlation coefficients ( R2), 0.8139 and 0.7797, respectively. Furthermore, both indices are highly correlated with each other ( R2=0.9173). Convenient transmission and the exchangeability of digital images of the real-time landscape facilitate the publication of results on the world wide web (WWW).

  15. FULL-SCALE TESTING OF A CAUSTIC SIDE SOLVENT EXTRACTION SYSTEM TO REMOVE CESIUM FROM SAVANNAH RIVER SITE RADIOACTIVE WASTE

    SciTech Connect

    Poirier, M; Thomas Peters, T; Earl Brass, E; Stanley Brown, S; Mark Geeting, M; Lcurtis Johnson, L; Charles02 Coleman, C; S Crump, S; Mark Barnes, M; Samuel Fink, S

    2007-10-15

    Savannah River Site (SRS) personnel have completed construction and assembly of the Modular Caustic Side Solvent Extraction Unit (MCU) facility. Following assembly, they conducted testing to evaluate the ability of the process to remove non-radioactive cesium and to separate the aqueous and organic phases. They conducted tests at salt solution flow rates of 3.5, 6.0, and 8.5 gpm. During testing, the MCU Facility collected samples and submitted them to Savannah River National Laboratory (SRNL) personnel for analysis of cesium, Isopar{reg_sign} L, and Modifier [1-(2,2,3,3-tetrafluoropropoxy)-3-(4-sec-butylphenoxy)-2-propanol]. SRNL personnel analyzed the aqueous samples for cesium by Inductively-Coupled Plasma Mass Spectroscopy (ICP-MS) and the solvent samples for cesium using a Parr Bomb Digestion followed by ICP-MS. They analyzed aqueous samples for Isopar{reg_sign} L and Modifier by gas chromatography (GC).

  16. Optimisation and establishment of separation conditions of organic acids from Usnea longissima Ach. by pH-zone-refining counter-current chromatography: Discussion of the eluotropic sequence.

    PubMed

    Sun, Changlei; Liu, Feng; Sun, Jie; Li, Jia; Wang, Xiao

    2016-01-04

    The major bioactive constituents of Usnea longissima Ach. are organic acids. However, few recent literatures involve the preparative separation of these organic acids. In the present study, pH zone-refining counter-current chromatography is used to separate organic acids from crude sample of U. longissima Ach. The crude extract was separated with the two-phase solvent system Pet-EtAc-MeOH-H2O (5:5:3:7, v/v) with 10mM TFA in organic stationary phase and different concentration of the eluter in aqueous mobile phase for the screening of the most suitable separation conditions. From the crude extract (1.2g), 74.0mg of orsellinic acid at 92.7% purity, 55.5mg of 4-O-methylorsellinic acid at 97.7% purity, 353.5mg of evernic acid at 93.8% purity, 102.0mg of barbatic acid at 94.8% purity, 19.4 mg of diffractaic acid at 92.2% purity, and 44.9 mg of usnic acid at 95.7% purity were obtained using the selected conditions in which the concentration of TFA in stationary phase was 10mM and the concentration of NaOH in mobile phase was 10-20mM. The purities of the separated organic acids were measured by HPLC. And the data of electrospray ionization-liquid chromatography/mass spectrometry (ESI-LC/MS), (1)H NMR, and (13)C NMR were used for confirming chemical structures.

  17. [Preparative isolation and purification of five non-volatile compounds from Fructus caryophylli and Flos caryophylli by high-speed counter-current chromatography].

    PubMed

    Gao, Lu; Yu, Bo; Yang, Hong

    2011-11-01

    A high-speed counter-current chromatographic (HSCCC) method was successfully developed for the isolation of three non-volatile compounds from Fructus Caryophylli and two chromone compounds from Flos Caryophylli. The optimum separation solution systems included system A (n-hexane-ethyl acetate-methanol-water (5:8:6: 13, v/v/v/v) and system B (n-hexane-ethyl acetate-methanol-water (5: 8: 9: 10, v/v/v/v). The upper phase of the system A was used as the stationary phase, and the lower phases of the systems A and B as the mobile phases were operated at a flow of 1.2 mL/min, while the apparatus rotated at 880 r/min. The 12.3 mg of ellagic acid, 9.6 mg of rhamnetin, 17.2 mg of quercetin were successfully purified from 70 mg of the crude extract of Fructus Caryophylli by a two-step separation. In the same way, 10.2 mg of 5,7-dimethoxy-2-methylchromone, 8.6 mg of 5,7-dimethoxy-2,6-dimethyl-chromone were purified from 50 mg of the crude extract of Flos Caryophylli. The purities of the compounds were all over 96% as determined by high performance liquid chromatography (HPLC). The five compounds were indentified by mass spectrometry (MS), 1H-nuclear magnetic resonance (NMR) and 13C-NMR. The results indicate that HSCCC is a powerful technique for the purification of non-volatile compounds from different parts of Eugenia caryophylla Thunb.

  18. Application of high-speed counter-current chromatography coupled with a reverse micelle solvent system to separate three proteins from Momordica charantia.

    PubMed

    Li, Yingnan; Yin, Lianhong; Zheng, Lingli; Xu, Lina; Xu, Youwei; Zhao, Yanyan; Qi, Yan; Yao, Jihong; Han, Xu; Liu, Kexin; Peng, Jinyong

    2012-05-01

    High-speed counter-current chromatography (HSCCC) coupled with a reverse micelle solvent system was successfully developed to separate three proteins from Momordica charantia. Suitable HSCCC conditions were carefully optimized as follows: the stationary phase was a reverse micellar phase composed of isooctane and 50mM bis-(2-ethylhexyl)-1-sulfosuccinate sodium (AOT). The mobile phase contained mobile phase A (50mM Tris-HCl buffer containing 50mM KCl at pH 7.0) for forward-extraction and mobile phase B (50mM Tris-HCl buffer containing 0.5M KCl at pH 10.0) for back-extraction. The flow rate, detection wavelength and column temperature were set at 1.5 ml/min, 280 nm and 4 °C, respectively. Under these conditions, three fractions (I, II and III) were separated, which showed high purity when analyzed by sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). The structures of these proteins were then identified by MALDI-TOF/TOF-MS/MS and compared with the NCBInr database. Fractions I and III were identified as resistance-like protein P-B and pentatricopeptide repeat-containing protein, respectively, which were found in M. charantia for the first time. However, fraction II, which is thought to be a new protein, was not identified, and further investigations on this fraction are required. The anticancer activities of these three proteins on the human gastric cancer cell line SGC-7901 were evaluated in vitro. The results indicated that fraction II has excellent anticancer activity (IC(50)=0.116 mg/ml for 48 h treatment). This is the first report on the use of HSCCC to isolate proteins from M. charantia. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Lutein in selected Canadian crops and agri-food processing by-products and purification by high-speed counter-current chromatography.

    PubMed

    Tsao, Rong; Yang, Raymond

    2006-04-21

    This study mainly focused on lutein content in several selected crops grown in southern Ontario, Canada. Marigold flower, a good rotation crop for the control of nematodes in tobacco fields was found to contain 0.77% lutein (after saponification, on dry basis). A high-speed counter-current chromatography (HSCCC) method using a two-phase solvent system consisting of hexane-ethanol-water (6:4.5:1.5, v/v/v) was developed for the purification of lutein from the saponification mixture of marigold flower extract. The purity of lutein prepared using this HSCCC method was 97%. Free lutein was found to be the predominant form in three squash varieties, and it was mostly found in the peel rather than the commonly consumed flesh. Sweet Mamma, Buttercup and Pepper squash varieties contained 25.4, 18.4 and 30.1mg/100g fresh weigh (FW) of lutein in the peels, respectively. These concentrations were significantly higher than that in spinach and kale (3.7 and 12.3 mg/100 g FW). beta-Carotene was found most in the peel of Sweet Mamma squash at 13.6 mg/100g FW, whereas it was below 2mg/100g FW in all other samples. Cooking increased extractable free lutein by 22-65% in squash peels. Lutein in Yukon Gold potato was at ca. 0.4 mg/100 g FW. Certain Yukon Gold was also found to contain violaxanthin (0.35 mg/100 g FW). Structures of lutein, beta-carotene and violaxanthin were identified by LC-atmospheric pressure chemical ionization MS in positive ion mode, and by comparing the retention time and UV-vis spectral data with standards. Results from this study suggest the selected crops and agri-food industrial processing by-products of these can be a good source of free lutein.

  20. Alternating isocratic and step gradient elution high-speed counter-current chromatography for the isolation of minor phenolics from Ormocarpum kirkii bark.

    PubMed

    Kamto, Eutrophe Le Doux; Carvalho, Tatiane S C; Mbing, Joséphine Ngo; Matene, Marie C N; Pegnyemb, Dieudonné E; Leitão, Gilda G

    2017-01-13

    A total of 14 compounds were isolated from the ethanol bark extract of O. kirkii S. Moore (Fabaceae) by alternating isocratic and step gradient elution high-speed counter-current chromatography (HSCCC) methods, using several solvent systems with reference to the polarity of compounds being purified. The extract was successively fractionated with generic solvent systems including n-hexane-ethanol-water (4:2:2) and ethyl acetate-water (1:1). Resulting fractions were further purified using the following preparative gradient elution consisting of ethyl acetate-n-butanol-water (X:Y:10), (X:Y=9:1 (I); 8:2 (II); 7:3 (III); 6:4 (IV); 5:5 (V); 4:6 (VI) 3:7 (VII) and n-hexane- ethyl acetate-methanol-water (1:X:1:1), X=1, 2, 2.5, 3 solvent systems. Two flavone glycosides, apigenin-6-C-β-d-glucopyranosyl-4'-O-[β-d-glucopyranosyl-(1→5)]-β-d-apiofuranoside (1) and apigenin-6-C-β-d-glucopyranosyl-4'-O-β-d-apiofuranoside (2), and one biflavanone diglycoside 7,7″-di-O-β-d-glucosylliquiritigeninyl-(I-3,II-3)-naringenin (4) were isolated as new compounds along with other 11 known ones. The structures of the isolated compounds were identified by HPLC-UV, ESI-MS, 1D and 2D NMR and comparison with literature data. Thus, over common traditional chromatographic methods, the present study shows that HSCCC is a useful and fast method for natural product research with no losses and lower solvent use.

  1. On-line coupling of counter-current chromatography and macroporous resin chromatography for continuous isolation of arctiin from the fruit of Arctium lappa L.

    PubMed

    Guo, Mengzhe; Liang, Junling; Wu, Shihua

    2010-08-13

    In this work, we have developed a novel hybrid two-dimensional counter-current chromatography and liquid chromatography (2D CCC x LC) system for the continuous purification of arctiin from crude extract of Arctium lappa. The first dimensional CCC column has been designed to fractionalize crude complex extract into pure arctiin effluent using a one-component organic/salt-containing system, and the second dimensional LC column has been packed with macroporous resin for on-line adsorption, desalination and desorption of arctiin which was effluent purified from the first CCC dimension. Thus, the crude arctiin mixture has been purified efficiently and conveniently by on-line CCC x LC in spite of the use of a salt-containing solvent system in CCC separation. As a result, high purity (more than 97%) of arctiin has been isolated by repeated injections both using the ethyl acetate-8% sodium chloride aqueous solution and butanol-1% sodium chloride aqueous solution. By contrast with the traditional CCC processes using multi-component organic/aqueous solvent systems, the present on-line CCC x LC process only used a one-component organic solvent and thus the solvent is easier to recover and regenerate. All of used solvents such as ethyl acetate, n-butanol and NaCl aqueous solution are low toxicity and environment-friendly. Moreover, the lower phase of salt-containing aqueous solution used as mobile phase, only contained minor organic solvent, which will save much organic solvent in continuous separation. In summary, our results indicated that the on-line hybrid 2D CCC x LC system using one-component organic/salt-containing aqueous solution is very promising and powerful tool for high-throughput purification of arctiin from fruits of A. lappa. 2010 Elsevier B.V. All rights reserved.

  2. Folding fan mode counter-current chromatography offers fast blind screening for drug discovery. Case study: finding anti-enterovirus 71 agents from Anemarrhena asphodeloides.

    PubMed

    Liu, Mengshun; Tao, Ling; Chau, Siu Leung; Wu, Rong; Zhang, Hong; Yang, Yifu; Yang, Dajian; Bian, Zhaoxiang; Lu, Aiping; Han, Quanbin; Xu, Hongxi

    2014-11-14

    A new application of counter-current chromatography (CCC) in drug discovery, called folding fan mode (FFM), is designed to eliminate the extensive and time-consuming calculation of the partition coefficients of some preset compounds in conventional CCC separation. Careful reading of reports in the literature reveals that, when two-phase solvent systems are listed in a polarity-increasing sequence, the isolates also show a similar trend in polarity. The relationship between the two-phase solvent system and the isolates is like that between the folds and the picture of a folding fan. We can directly select a two-phase solvent system to separate fractions having similar polarity, just as opening a fan reveals a picture. The solvent ratio of two-phase solvent systems can be adjusted according to the polarity and weight ratio of active fractions rather than the partition coefficients. Without preset compounds, FFM-CCC not only requires no measurement of partition coefficients, but also achieves true blind screening. This paper reports the method's first success in drug discovery: six anti-EV71 saponins were found from the mixture (9.13 g) of ethanol extract and water extract of Anemarrhena asphodeloides after a total of four CCC separations, using hexan/ethyl acetate/methanol/butanol/water as the model solvent system. Among these saponins, timosaponin B-II displayed a comparable IC50 (4.3 ± 2.1 μM) and a 40-fold higher selective index (SI=92.9) than the positive control (IC50=361.7 ± 104.6 μM, SI=2.4), ribavirin. The structure-activity relationship (SAR) of these compounds was also studied.

  3. Phase-field simulation of counter-current spontaneous imbibition in a fractured heterogeneous porous medium

    NASA Astrophysics Data System (ADS)

    Rokhforouz, M. R.; Akhlaghi Amiri, H. A.

    2017-06-01

    Spontaneous imbibition is well-known to be one of the most effective processes of oil recovery in fractured reservoirs. However, the detailed pore-scale mechanisms of the counter-current imbibition process and the effects of different fluid/rock parameters on this phenomenon have not yet been deeply addressed. This work presents the results of a new pore-level numerical study of counter-current spontaneous imbibition, using coupled Cahn-Hilliard phase field and Navier-Stokes equations, solved by a finite element method. A 2D fractured medium was constructed consisting of a nonhomogeneous porous matrix, in which the grains were represented by an equilateral triangular array of circles with different sizes and initially saturated with oil, and a fracture, adjacent to the matrix, initially saturated with water and supported by low rate water inflow. Through invasion of water into the matrix, oil drops were expelled one by one from the matrix to the fracture, and in the matrix, water progressed by forming capillary fingerings, with characteristics corresponding to the experimental observations. The effects of wettability, viscosity ratio, and interfacial tension were investigated. In strongly water-wet matrix, with grain contact angles of θ < π/8, different micro-scale mechanisms were successfully captured, including oil film thinning and rupture, fluids' contact line movement, water bridging, and oil drop detachment. It was notified that there was a specific grain contact angle for this simulated model, θ = π/4, above it, matrix oil recovery was negligible by imbibition, while below it, the imbibition rate and oil recovery were significantly increased by decreasing the contact angle. In simulated mixed wet models, water, coming from the fracture, just invaded the neighboring water-wet grains; the water front was stopped moving as it met the oil-wet grains or wide pores/throats. Increasing water-oil interfacial tension, in the range of 0.005-0.05 N/m, resulted in

  4. [Evaluation of the usefulness of the agglutination test with Mangifera indica extract for the identification of pathogenic Yersinia enterocolitica strains].

    PubMed

    Kałuzewski, S; Gierczyński, R; Szych, J; Jagielski, M

    1997-01-01

    The study was performed on 137 Y. enterocolitica strains belonging to various serological groups, including 75 03 group strains isolated form human clinical material. The agglutination test on slides was carried out on this strains using Mangifera indica extract of own production. Agglutinating preparation obtained from the seeds of M. indica agglutinated Y. enterocolitica organisms possessing the pVY plasmid and CRMOX+ phenotype in dilutions to 1.56 micrograms/ml. In identification tests conducted parallelly agglutination solution was used in concentrations of 100 and 10 micrograms/ml. All clones of Y. enterocolitica from O3 group from cultures at 37 degrees C and with CRMOX+ phenotype possessing the pVY plasmid were agglutinated by the extract. Agglutination failed to develop in the cultures of these clones incubated at 25 degrees C. Yersinia clones not containing the pVY plasmid with CRMOX- phenotype were resistant to agglutination. The virulence plasmid was found in 44 out of 75 strains of Y. enterocolitica O3 and was identified by restriction analysis after plasmid DNA digestion with Eco RI enzyme. The obtained results agreed with those of Wauters et al. in 1995 and confirmed the opinion of these authors on the usefulness of the test with M. indica agglutinin for the identification of virulent Y. enterocolitica strains.

  5. Countercurrent chromatography separation of saponins by skeleton type from Ampelozizyphus amazonicus for off-line ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry analysis and characterisation.

    PubMed

    de Souza Figueiredo, Fabiana; Celano, Rita; de Sousa Silva, Danila; das Neves Costa, Fernanda; Hewitson, Peter; Ignatova, Svetlana; Piccinelli, Anna Lisa; Rastrelli, Luca; Guimarães Leitão, Suzana; Guimarães Leitão, Gilda

    2017-01-20

    Ampelozizyphus amazonicus Ducke (Rhamnaceae), a medicinal plant used to prevent malaria, is a climbing shrub, native to the Amazonian region, with jujubogenin glycoside saponins as main compounds. The crude extract of this plant is too complex for any kind of structural identification, and HPLC separation was not sufficient to resolve this issue. Therefore, the aim of this work was to obtain saponin enriched fractions from the bark ethanol extract by countercurrent chromatography (CCC) for further isolation and identification/characterisation of the major saponins by HPLC and MS. The butanol extract was fractionated by CCC with hexane - ethyl acetate - butanol - ethanol - water (1:6:1:1:6; v/v) solvent system yielding 4 group fractions. The collected fractions were analysed by UHPLC-HRMS (ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry) and MS(n). Group 1 presented mainly oleane type saponins, and group 3 showed mainly jujubogenin glycosides, keto-dammarane type triterpene saponins and saponins with C31 skeleton. Thus, CCC separated saponins from the butanol-rich extract by skeleton type. A further purification of group 3 by CCC (ethyl acetate - ethanol - water (1:0.2:1; v/v)) and HPLC-RI was performed in order to obtain these unusual aglycones in pure form.

  6. Langmuir probes for SPIDER (source for the production of ions of deuterium extracted from radio frequency plasma) experiment: Tests in BATMAN (Bavarian test machine for negative ions)

    SciTech Connect

    Brombin, M. Spolaore, M.; Serianni, G.; Pomaro, N.; Taliercio, C.; Palma, M. Dalla; Pasqualotto, R.; Schiesko, L.

    2014-11-15

    A prototype system of the Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from RF plasma) was manufactured and experimentally qualified. The diagnostic was operated in RF (Radio Frequency) plasmas with cesium evaporation on the BATMAN (BAvarian Test MAchine for Negative ions) test facility, which can provide plasma conditions as expected in the SPIDER source. A RF passive compensation circuit was realised to operate the Langmuir probes in RF plasmas. The sensors’ holder, designed to better simulate the bias plate conditions in SPIDER, was exposed to a severe experimental campaign in BATMAN with cesium evaporation. No detrimental effect on the diagnostic due to cesium evaporation was found during the exposure to the BATMAN plasma and in particular the insulation of the electrodes was preserved. The paper presents the system prototype, the RF compensation circuit, the acquisition system (as foreseen in SPIDER), and the results obtained during the experimental campaigns.

  7. Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from Radio Frequency plasma) experiment: tests in BATMAN (BAvarian Test Machine for Negative ions).

    PubMed

    Brombin, M; Spolaore, M; Serianni, G; Pomaro, N; Taliercio, C; Dalla Palma, M; Pasqualotto, R; Schiesko, L

    2014-11-01

    A prototype system of the Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from RF plasma) was manufactured and experimentally qualified. The diagnostic was operated in RF (Radio Frequency) plasmas with cesium evaporation on the BATMAN (BAvarian Test MAchine for Negative ions) test facility, which can provide plasma conditions as expected in the SPIDER source. A RF passive compensation circuit was realised to operate the Langmuir probes in RF plasmas. The sensors' holder, designed to better simulate the bias plate conditions in SPIDER, was exposed to a severe experimental campaign in BATMAN with cesium evaporation. No detrimental effect on the diagnostic due to cesium evaporation was found during the exposure to the BATMAN plasma and in particular the insulation of the electrodes was preserved. The paper presents the system prototype, the RF compensation circuit, the acquisition system (as foreseen in SPIDER), and the results obtained during the experimental campaigns.

  8. Langmuir probes for SPIDER (source for the production of ions of deuterium extracted from radio frequency plasma) experiment: Tests in BATMAN (Bavarian test machine for negative ions)

    NASA Astrophysics Data System (ADS)

    Brombin, M.; Spolaore, M.; Serianni, G.; Pomaro, N.; Taliercio, C.; Palma, M. Dalla; Pasqualotto, R.; Schiesko, L.

    2014-11-01

    A prototype system of the Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from RF plasma) was manufactured and experimentally qualified. The diagnostic was operated in RF (Radio Frequency) plasmas with cesium evaporation on the BATMAN (BAvarian Test MAchine for Negative ions) test facility, which can provide plasma conditions as expected in the SPIDER source. A RF passive compensation circuit was realised to operate the Langmuir probes in RF plasmas. The sensors' holder, designed to better simulate the bias plate conditions in SPIDER, was exposed to a severe experimental campaign in BATMAN with cesium evaporation. No detrimental effect on the diagnostic due to cesium evaporation was found during the exposure to the BATMAN plasma and in particular the insulation of the electrodes was preserved. The paper presents the system prototype, the RF compensation circuit, the acquisition system (as foreseen in SPIDER), and the results obtained during the experimental campaigns.

  9. Pilot test of a vacuum extraction system for environmental remediation of chlorinated solvents at the Savannah River Site

    SciTech Connect

    Looney, B.B.; Pickett, J.B. ); Malot, J.J. )

    1991-12-29

    Vacuum extraction is an environmental restoration technique that is currently being applied to the remediation of soils and shallow segments that are contaminated with volatile constituents. In 1987, a h study was performed to evaluate the performance and potential applicability of this technology at the Savannah River Site (SRS). Vacuum extraction is useful when volatile constituents are present in the vadose zone. The technology has been used to remediate a number of sites across the country, including leading underground storage tanks, spill sites, landfill, and production facilities. The primary objective of the pilot study was to test the performance of the technology under the conditions specific to many of the potential areas of application at SRS. There is only a limited body of literature documenting field studiesin similar environments with in sands and clayey zones and a relatively thick vadose zone. Careful studies of this type are needed to develop full scale designs at SRS. The vacuum extraction pilot study at SRS was performed by a mm consisting of technical representatives of the Environmental Sciences Section in the Savannah River Laboratory (SRL), the Raw Materials Engineering and Technology Section of SRS, and TerraVac Inc., a subcontractor with experience in this field.

  10. Pilot test of a vacuum extraction system for environmental remediation of chlorinated solvents at the Savannah River Site

    SciTech Connect

    Looney, B.B.; Pickett, J.B.; Malot, J.J.

    1991-12-29

    Vacuum extraction is an environmental restoration technique that is currently being applied to the remediation of soils and shallow segments that are contaminated with volatile constituents. In 1987, a h study was performed to evaluate the performance and potential applicability of this technology at the Savannah River Site (SRS). Vacuum extraction is useful when volatile constituents are present in the vadose zone. The technology has been used to remediate a number of sites across the country, including leading underground storage tanks, spill sites, landfill, and production facilities. The primary objective of the pilot study was to test the performance of the technology under the conditions specific to many of the potential areas of application at SRS. There is only a limited body of literature documenting field studiesin similar environments with in sands and clayey zones and a relatively thick vadose zone. Careful studies of this type are needed to develop full scale designs at SRS. The vacuum extraction pilot study at SRS was performed by a mm consisting of technical representatives of the Environmental Sciences Section in the Savannah River Laboratory (SRL), the Raw Materials Engineering and Technology Section of SRS, and TerraVac Inc., a subcontractor with experience in this field.

  11. Formal analysis, hardness, and algorithms for extracting internal structure of test-based problems.

    PubMed

    Jaśkowski, Wojciech; Krawiec, Krzysztof

    2011-01-01

    Problems in which some elementary entities interact with each other are common in computational intelligence. This scenario, typical for coevolving artificial life agents, learning strategies for games, and machine learning from examples, can be formalized as a test-based problem and conveniently embedded in the common conceptual framework of coevolution. In test-based problems, candidate solutions are evaluated on a number of test cases (agents, opponents, examples). It has been recently shown that every test of such problem can be regarded as a separate objective, and the whole problem as multi-objective optimization. Research on reducing the number of such objectives while preserving the relations between candidate solutions and tests led to the notions of underlying objectives and internal problem structure, which can be formalized as a coordinate system that spatially arranges candidate solutions and tests. The coordinate system that spans the minimal number of axes determines the so-called dimension of a problem and, being an inherent property of every problem, is of particular interest. In this study, we investigate in-depth the formalism of a coordinate system and its properties, relate them to properties of partially ordered sets, and design an exact algorithm for finding a minimal coordinate system. We also prove that this problem is NP-hard and come up with a heuristic which is superior to the best algorithm proposed so far. Finally, we apply the algorithms to three abstract problems and demonstrate that the dimension of the problem is typically much lower than the number of tests, and for some problems converges to the intrinsic parameter of the problem--its a priori dimension.

  12. Advantages and limitations of chemical extraction tests to predict mercury soil-plant transfer in soil risk evaluations.

    PubMed

    Monteiro, R J R; Rodrigues, S M; Cruz, N; Henriques, B; Duarte, A C; Römkens, P F A M; Pereira, E

    2016-07-01

    In this study, we compared the size of the mobile Hg pool in soil to those obtained by extractions using 2 M HNO3, 5 M HNO3, and 2 M HCl. This was done to evaluate their suitability to be used as proxies in view of Hg uptake by ryegrass. Total levels of Hg in soil ranged from 0.66 to 70 mg kg(-1) (median 17 mg kg(-1)), and concentrations of Hg extracted increased in the order: mobile Hg < 2 M HNO3 < 5 M HNO3 < 2 M HCl. The percentage of Hg extracted relative to total Hg in soil varied from 0.13 to 0.79 % (for the mobile pool) to 4.8-82 % (for 2 M HCl). Levels of Hg in ryegrass ranged from 0.060 to 36 mg kg(-1) (median 0.65 mg kg(-1), in roots) and from 0.040 to 5.4 mg kg(-1) (median 0.34 mg kg(-1), in shoots). Although results from the 2 M HNO3 extraction appeared to the most comparable to the actual total Hg levels measured in plants, the 2 M HCl extraction better expressed the variation in plant pools. In general, soil tests explained between 66 and 86 % of the variability of Hg contents in ryegrass shoots. Results indicated that all methods tested here can be used to estimate the plant total Hg pool at contaminated areas and can be used in first tier soil risk evaluations. This study also indicates that a relevant part of Hg in plants is from deposition of soil particles and that splashing of soil can be more significant for plant contamination than actual uptake processes. Graphical Abstract Illustration of potential mercury soil-plant transfer routes.

  13. Extraction and isolation of phenolic compounds.

    PubMed

    Santos-Buelga, Celestino; Gonzalez-Manzano, Susana; Dueñas, Montserrat; Gonzalez-Paramas, Ana M

    2012-01-01

    Phenolic compounds constitute a major class of plant secondary metabolites that are widely distributed in the plant kingdom and show a large structural diversity. These compounds occur as aglycones or glycosides, as monomers or constituting highly polymerized structures, or as free or matrix-bound compounds. Furthermore, they are not uniformly distributed in the plant and their stability varies significantly. This greatly complicates their extraction and isolation processes, which means that a single standardized procedure cannot be recommended for all phenolics and/or plant materials; procedures have to be optimized depending on the nature of the sample and the target analytes, and also on the object of the study. In this chapter, the main techniques for sample preparation, and extraction and isolation of phenolic compounds have been reviewed-from classical solvent extraction procedures to more modern approaches, such as the use of molecularly imprinted polymers or counter-current chromatography.

  14. Isolation of terpenoids from Pimpinella anisum essential oil by high-performance counter-current chromatography.

    PubMed

    Skalicka-Woźniak, Krystyna; Walasek, Magdalena; Ludwiczuk, Agnieszka; Głowniak, Kazimierz

    2013-08-01

    High-performance counter-current chromatography was successfully used for the isolation and purification of terpenoid compounds from the essential oil of Pimpinella anisum L. A two-phase solvent system composed of n-heptane/methanol/ethyl acetate/water (5:2:5:2, v/v/v/v) was suitable for the purification of linalool, terpinen-4-ol, α-terpineol, p-anisaldehyde, while n-heptane/methanol (1:1, v/v) was used for the isolation of anethole and foeniculin. A scale-up process from analytical to preparative was developed. Additionally, a stepwise gradient elution was applied and instead of two different runs, 40 min each, one 80 min separation was performed; although the time of separation remains the same, it was possible to repeat the efficiency even if the water-containing mobile phase was changed to a nonaqueous system. The obtained essential oil, as well as purified compounds, was analyzed by GC. A total of 0.64 mg of linalool, 0.52 mg of terpinen-4-ol, 0.10 mg of α-terpineol, 0.62 mg of p-anisaldehyde, 15 mg of anethole, and 2.12 mg of foeniculin were obtained from 210 mg of the essential oil of P. anisum L. in a short time with purities of 99, 98, 94, 93.54, 93, and 93.6%, respectively. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Compact type-I coil planet centrifuge for counter-current chromatography

    PubMed Central

    Yang, Yi; Gu, Dongyu; Liu, Yongqiang; Aisa, Haji Akber; Ito, Yoichiro

    2009-01-01

    A compact type-I coil planet centrifuge has been developed for performing counter-current chromatography. It has a revolution radius of 10 cm and a column holder height of 5 cm compared with 37 cm and 50 cm in the original prototype, respectively. The reduction in the revolution radius and column length permits application of higher revolution speed and more stable balancing of the rotor which leads us to learn more about its performance and the future potential of type-I coil planet centrifuge. The chromatographic performance of this apparatus was evaluated in terms of retention of the stationary phase (Sf), peak resolution (Rs), theoretical plate (N) and peak retention time (tR). The results of the experiment indicated that increasing the revolution speed slightly improved both the retention of the stationary phase and the peak resolution while the separation time is remarkably shortened to yield an excellent peak resolution at a revolution speed of 800 rpm. With a 12 ml capacity coiled column, DNP-glu, DNP-β-ala and DNP-ala were resolved at Rs of 2.75 and 2.16 within 90 min at a flow rate of 0.4 ml/min. We believe that the compact type-I coil planet centrifuge has a high analytical potential. PMID:20060979

  16. Compact type-I coil planet centrifuge for counter-current chromatography.

    PubMed

    Yang, Yi; Gu, Dongyu; Liu, Yongqiang; Aisa, Haji Akber; Ito, Yoichiro

    2010-02-19

    A compact type-I coil planet centrifuge has been developed for performing counter-current chromatography. It has a revolution radius of 10 cm and a column holder height of 5 cm compared with 37 and 50 cm in the original prototype, respectively. The reduction in the revolution radius and column length permits application of higher revolution speed and more stable balancing of the rotor which leads us to learn more about its performance and the future potential of type-I coil planet centrifuge. The chromatographic performance of this apparatus was evaluated in terms of retention of the stationary phase (S(f)), peak resolution (R(s)), theoretical plate (N) and peak retention time (t(R)). The results of the experiment indicated that increasing the revolution speed slightly improved both the retention of the stationary phase and the peak resolution while the separation time is remarkably shortened to yield an excellent peak resolution at a revolution speed of 800 rpm. With a 12 ml capacity coiled column, DNP-DL-glu, DNP-beta-ala and DNP-l-ala were resolved at R(s) of 2.75 and 2.16 within 90 min at a flow rate of 0.4 ml/min. We believe that the compact type-I coil planet centrifuge has a high analytical potential. Published by Elsevier B.V.

  17. Powerful leverages and counter-currents in the unborn child spiritual care: a qualitative study.

    PubMed

    Heidari, Tooba; Ziaei, Saeideh; Ahmadi, Fazlollah; Mohammadi, Eesa

    2014-08-22

    In different cultures, pregnancy, birth and motherhood are perceived as spiritual events through their miraculous processes and create an ideal context for spir