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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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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. Phase distribution visualisation in continuous counter-current extraction.

    PubMed

    van den Heuvel, Remco; Sutherland, Ian

    2009-05-01

    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. PMID:19100985

  4. Countercurrent Flow of Molten Glass and Air during Siphon Tests

    SciTech Connect

    Guerrero, H.N.

    2001-01-16

    Siphon tests of molten glass were performed to simulate potential drainage of a radioactive waste melter, the Defense Waste Processing Facility (DWPF) at the Savannah River Site. Glass is poured from the melter through a vertical downspout that is connected to the bottom of the melter through a riser. Large flow surges have the potential of completely filling the downspout and creating a siphon effect that has the potential for complete draining of the melter. Visual observations show the exiting glass stream starts as a single-phase pipe flow, constricting into a narrow glass stream. Then a half-spherical bubble forms at the exit of the downspout. The bubble grows, extending upwards into the downspout, while the liquid flows counter-currently to one side of the spout. Tests were performed to determine what are the spout geometry and glass properties that would be conducive to siphoning, conditions for terminating the siphon, and the total amount of glass drained.

  5. 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)

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  7. 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.

  8. 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.

  9. Accelerated solvent extraction and pH-zone-refining counter-current chromatographic purification of yunaconitine and 8-deacetylyunaconitine from Aconitum vilmorinianum Kom.

    PubMed

    Shu, Xi-Kai; Li, Jia; Liu, Feng; Lin, Xiao-Jing; Wang, Xiao; Song, Chun-Xia

    2013-08-01

    This study aimed to seek an efficient method to extract and purify yunaconitine and 8-deacetylyunaconitine from Aconitum vilmorinianum Kom. by accelerated solvent extraction combined with pH-zone-refining counter-current chromatography. The major extraction parameters for accelerated solvent extraction were optimized by an orthogonal test design L9 (3)(4). Then a separation and purification method was established using pH-zone-refining counter-current chromatography with a two-phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (5:5:2:8, v/v) with 10 mM triethylamine in the upper phase and 10 mM HCl in the lower phase. From 2 g crude extract, 224 mg of 8-deacetylyunaconitine (I) and 841 mg of yunaconitine (II) were obtained with a purity of over 98.0%. The chemical structures were identified by ESI-MS and (1)H and (13)C NMR spectroscopy.

  10. 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. PMID:24299786

  11. 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.

  12. Ultrasound-assisted dynamic extraction coupled with parallel countercurrent chromatography for simultaneous extraction, purification, and isolation of phytochemicals: application to isoflavones from red clover.

    PubMed

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

    2015-06-01

    A novel procedure comprising ultrasonic-assisted dynamic extraction (UADE) coupled with two countercurrent-chromatography systems (parallel countercurrent chromatography, PCCC) was developed. This technique offers the possibility for simultaneous extraction, solvent configuration, purification, and isolation of target compounds. This new approach was applied to the fractionation and purification of isoflavones from red clover. The two-phase solvent system was prepared by automating the equipment. The lower aqueous phase of the two-phase solvent system was used as the UADE solution and as the mobile phase for PCCC. After the extraction and purification steps, the purified sample was pumped into the countercurrent chromatography 1 (CCC1) column for the first isolation step. During CCC1 separation, the sample was enriched and purified and then pumped into the CCC2 column for the second isolation step. After completion of the first cycle of UADE-PCCC steps, the second-cycle experiments were performed. Using this sequence, five target compounds, daidzein, prunetin, genistein, irilone, and maackiain, with >95.31 % purity were successfully extracted and isolated using the two-phase solvent system of n-hexane-ethyl acetate-ethanol-water (0.623:1.00:0.99:1.246, v/v). With this instrumental setup, scientific and systematic extraction and isolation of natural products was achieved, and this technique has great potential for industrial application. Graphical Abstract Simplified schematic of instrumental setup of UADE combined with two HSCCC instruments.

  13. An automatic countercurrent liquid-liquid micro-extraction system coupled with atomic absorption spectrometry for metal determination.

    PubMed

    Mitani, Constantina; Anthemidis, Aristidis N

    2015-02-01

    A novel and versatile automatic sequential injection countercurrent liquid-liquid microextraction (SI-CC-LLME) system coupled with atomic absorption spectrometry (FAAS) is presented for metal determination. The extraction procedure was based on the countercurrent flow of aqueous and organic phases which takes place into a newly designed lab made microextraction chamber. A noteworthy feature of the extraction chamber is that it can be utilized for organic solvents heavier or lighter than water. The proposed method was successfully demonstrated for on-line lead determination and applied in environmental water samples using an amount of 120 μL of chloroform as extractant and ammonium diethyldithiophosphate as chelating reagent. The effect of the major experimental parameters including the volume of extractant, as well as the flow rate of aqueous and organic phases were studied and optimized. Under the optimum conditions for 6 mL sample consumption an enhancement factor of 130 was obtained. The detection limit was 1.5 μg L(-1) and the precision of the method, expressed as relative standard deviation (RSD) was 2.7% at 40.0 μg L(-1) Pb(II) concentration level. The proposed method was evaluated by analyzing certified reference materials and spiked environmental water samples. PMID:25435230

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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. PMID:26590235

  1. Combination of supercritical fluid extraction with counter-current chromatography to isolate anthocyanidins from the petals of Chaenomeles sinensis based on mathematical calculations.

    PubMed

    Li, Sainan; Guo, Liping; Liu, Chunming; Fu, Zi Ao; Zhang, Yuchi

    2013-11-01

    Supercritical fluid extraction (SFE) coupled with high-speed counter-current chromatography (HSCCC) was successfully used for the extraction and on-line isolation of the anthocyanidins from the petals of Chaenomeles sinensis in two stages. The SFE parameters were optimized by an orthogonal test, and the solvent systems of SFE and HSCCC were calculated and optimized with the help of a multiexponential function model. In the first stage, the lower phase of the solvent system of n-butanol/tert-butyl methyl ether/acetonitrile/0.1% aqueous TFA (0.715:1.0:0.134:1.592, v/v/v/v) was used as both the SFE modifier and the HSCCC stationary phase, after extraction, the extractants were pumped into HSCCC column, and then eluted with the corresponding upper phase to isolate the moderately hydrophobic compounds. In the second stage, the upper phase of the solvent system of n-butanol/ethyl acetate/acetonitrile/0.1% aqueous TFA (1.348:1.0:0.605:2.156, v/v/v/v) was used as both the SFE modifier and the HSCCC stationary phase, followed by elution with the corresponding lower phase to separate the hydrophobic compounds. With the help of two-stage SFE/HSCCC, six compounds including delphinidin-3-O-glucoside (Dp3G), cyanidin-3-O-glucoside (Cy3G), peonidin-3-O-glucoside (Pn3G), delphinidin (Dp), peonidin (Pn), and malvidin (Mv) were successfully separated within 300 min. The targeted compounds were identified by UV spectrophotometry, MS, and NMR spectroscopy. This research has opened up great prospects for the industrial application of SFE-HSCCC for the automatic extraction and separation of unstable compounds.

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

    PubMed Central

    Liang, Jinru; Ito, Yoichiro; Zhang, Xinxin; He, Jiao; Sun, Wenji

    2014-01-01

    A rapid method combining microwave-assisted extraction and high-speed counter-current chromatography was applied for preparative separation of six bioactive compounds including loganic acid (I), isoorientin-4'-O-glucoside (II), 6'-O-β-d-glucopyranosyl gentiopicroside (III), swertiamarin (IV), gentiopicroside (V), sweroside (VI) from traditional Tibetan medicine Gentiana crassicaulis Duthie ex Burk. Microwave-assisted extraction parameters were predicted by central composite design-response surface methodology. That is, 5.0 g dried roots of G. Crassicaulis was extracted with 50 mL 57.5% aqueous ethanol under 630 W for 3.39 min. The extract (gentian total glycosides) was separated by high-speed counter-current chromatography with n-butanol/ethyl acetate/methanol/1% acetic acid water (7.5:0.5:0.5:3.5, v/v/v/v) using upper phase mobile in tail-to-head elution mode. 16.3 mg, 8.8 mg, 12.8 mg, 25.1 mg, 40.7 mg and 21.8 mg of compounds I–VI were obtained with high purities in one run from 500 mg of original sample. The purities and identities of separated components were confirmed using HPCL with photo diode array detection and quadrupole time-of-flight MS and NMR spectroscopy. The study reveals that response surface methodology is convenient and highly predictive for optimizing extraction process, microwave-assisted extraction coupled with high-speed counter-current chromatography could be an expeditious method for extraction and separation of phytochemicals from ethnomedicine. PMID:24151213

  3. 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. PMID:26864462

  4. 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.

  5. An efficient new method for extraction, separation and purification of psoralen and isopsoralen from Fructus Psoraleae by supercritical fluid extraction and high-speed counter-current chromatography.

    PubMed

    Wang, Xiao; Wang, Yuqiang; Yuan, Jinpeng; Sun, Qinglei; Liu, Jianhua; Zheng, Chengchao

    2004-11-01

    Psoralen and isopsoralen were extracted from Fructus Psoraleae (Psoralea corylitolia L.) by supercritical CO2. The effect of various parameters, i.e., pressure, temperature and sample particle size on yield was investigated with an analytical-scale supercritical fluid extraction (SFE) system to find the optimal conditions. The process was then scaled up by 50 times with a preparative SFE system under the optimized conditions of pressure (26 MPa), temperature (60 degrees C) and a sample particle size of 40-60 mesh. The yield of the preparative SFE was 9.1% and the combined yield of psoralen and isopsoralen was 2.5 mg/g of dry seeds. Psoralen and isopsoralen in the extract were separated and purified by high-speed counter-current chromatography with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.7:1:0.8, v/v), and the fractions were analyzed by HPLC, MS, 1HNMR and 13C NMR. The structures of the products were further confirmed by comparison with authentic samples (National Institute of the Control of Pharmaceutical and Biological Products, Beijing, China). PMID:15560489

  6. Application of supercritical fluid extraction coupled with counter-current chromatography for extraction and online isolation of unstable chemical components from Rosa damascena.

    PubMed

    Li, Sainan; Guo, Liping; Liu, Chunming; Zhang, Yuchi

    2013-07-01

    Supercritical fluid extraction (SFE) coupled with high-speed counter-current chromatography (HSCCC) was successfully used for the extraction and online isolation of the unstable compounds from Rosa damascene in a single extraction and separation operation in two stages. The solvent systems of SFE/HSCCC were optimized with the help of multiexponential function model. At the first stage, the upper phase of the solvent system of n-butanol-tert-butyl methyl ether-acetonitrile-0.1% aqueous TFA (1.7:1.0:0.8:4.0, v/v/v/v) was used as both the SFE entrainer and the HSCCC stationary phase, and the target compounds were eluted with the corresponding lower phase to separate the hydrophobic compounds. At the second stage, the upper phase of the solvent system of n-hexane-ethyl acetate-methanol-water (3.2:1.0:2.8:2.6, v/v/v/v) was used as both the SFE entrainer and the HSCCC stationary phase, followed by elution with the corresponding lower phase to separate the moderate hydrophobic compounds. Six compounds including formononetin, delphinidin, cyaniding, 5,6,4'-trihydroxy-7,8-dimethoxy flavone, 5,3'-dihydroxy-7,8-dimethoxy flavone, and 5-hydroxy-6,7,8,3',4'-pentamethoxy flavone were successfully separated in one extraction-separation operation within 300 min. The targeted compounds were identified by MS and NMR spectroscopy. This research has opened up great prospects for industrial application of SFE/HSCCC to the extraction and separation of unstable compounds.

  7. 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

    2015-04-01

    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.

  8. Simple, quantitative method for low molecular weight dissolved organic matter extracted from natural waters based upon high performance counter-current chromatography.

    PubMed

    Rojas, Alfonso; Sandron, Sara; Wilson, Richard; Davies, Noel W; Haddad, Paul R; Shellie, Robert A; Nesterenko, Pavel N; Paull, Brett

    2016-02-25

    A simple, high-performance counter-current chromatography method with sequential UV absorbance (254 nm) and evaporative light scattering detection (ELSD) was developed for the quantification of pre-extracted low molecular weight dissolved organic matter (DOM) extracted from natural waters. The method requires solid-phase extraction (SPE) extraction of only small volumes of water samples, here using poly(styrenedivinylbenzene)-based extraction cartridges (Varian PPL). The extracted and concentrated DOM was quantified using reversed-phase high-performance counter-current chromatography (HPCCC), with a water/methanol (5:5) mobile phase and hexane/ethyl acetate (3:7) stationary phase. The critical chromatographic parameters were optimised, applying a revolution speed of 1900 rpm and a flow-rate of 1 mL min(-1). Under these conditions, 50 μL of extracted DOM solution could be injected and quantified using calibration against a reference natural dissolved material (Suwannee River), based upon UV absorbance at 254 nm and ELSD detection. Both detection methods provided excellent linearity (R(2) > 0.995) for DOM across the concentration ranges of interest, with limits of detection of 4 μg ml(-1) and 7 μg ml(-1) for ELSD and UV absorbance, respectively. The method was validated for peak area precision (<5%), and accuracy and recovery based upon spiking seawater samples prior to extraction, together with DOM solutions post-extraction (>95% recovery). The developed method was applied to the determination of the concentration of DOM in seawater, based upon initial sample volumes as small as 20 mL. PMID:26851093

  9. Studies of protein-protein interaction using countercurrent distribution in aqueous two-phase systems. Partition behaviour of six Calvin-cycle enzymes from a crude spinach (Spinacia oleracea) chloroplast extract.

    PubMed Central

    Persson, L O; Johansson, G

    1989-01-01

    The partition behaviour of six enzymes of the Calvin cycle in extracts of chloroplasts from spinach (Spinacia oleracea) between two aqueous phases has been studied by countercurrent distribution. The enzymes showed distribution patterns which indicate heterogeneity and the presence of two or three fractions of most of the enzymes. When two of the enzymes, phosphoglycerate kinase and fructose-bisphosphate aldolase, were partitioned in both purified and partially purified form, they behaved like homogeneous substances. These results indicate that countercurrent distribution of crude extracts in aqueous two-phase systems is a useful method to study protein-protein interaction. PMID:2730589

  10. 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.

  11. 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.

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

    PubMed

    Liang, Jinru; Ito, Yoichiro; Zhang, Xinxin; He, Jiao; Sun, Wenji

    2013-12-01

    A rapid method combining microwave-assisted extraction (MAE) and high-speed counter-current chromatography (HSCCC) was applied for preparative separation of six bioactive compounds including loganic acid (I), isoorientin-4'-O-glucoside (II), 6'-O-β-d-glucopyranosyl gentiopicroside (III), swertiamarin (IV), gentiopicroside (V), sweroside (VI) from traditional Tibetan medicine Gentiana crassicaulis Duthie ex Burk. MAE parameters were predicted by central composite design response surface methodology. That is, 5.0 g dried roots of G. crassicaulis were extracted with 50 mL 57.5% aqueous ethanol under 630 W for 3.39 min. The extract (gentian total glycosides) was separated by HSCCC with n-butanol/ethyl acetate/methanol/1% acetic acid water (7.5:0.5:0.5:3.5, v/v/v/v) using upper phase mobile in tail-to-head elution mode. 16.3, 8.8, 12., 25.1, 40.7, and 21.8 mg of compounds I-VI were obtained with high purities in one run from 500 mg of original sample. The purities and identities of separated components were confirmed using HPLC with photo diode array detection and quadrupole TOF-MS and NMR spectroscopy. The study reveals that response surface methodology is convenient and highly predictive for optimizing extraction process, MAE coupled with HSCCC could be an expeditious method for extraction and separation of phytochemicals from ethnomedicine.

  13. 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.

  14. Development of a method to extract and purify target compounds from medicinal plants in a single step: online hyphenation of expanded bed adsorption chromatography and countercurrent chromatography

    PubMed Central

    Li, Yang; Wang, Nan; Zhang, Min; Ito, Yoichiro; Zhang, Hongyang; Wang, Yuerong; Guo, Xin; Hu, Ping

    2014-01-01

    Pure compounds extracted and purified from natural sources are crucial to lead discovery and drug screening. This study presents a novel two-dimensional hyphenation of expanded bed adsorption chromatography (EBAC) and high-speed countercurrent chromatography (HSCCC) for extraction and purification of target compounds from medicinal plants in a single step. The EBAC and HSCCC were hyphenated via a six-port injection valve as an interface. Fractionation of ingredients of Salvia miltiorrhiza and Rhizoma coptidis was performed on the hyphenated system to verify its efficacy. An amount each of 52.9 mg of salvianolic acid B and 2.1 mg of rosmarinic acid was obtained from Salvia miltiorrhiza by the two-dimensional system in a single step. The purities of the targets were over 96% of salvianolic acid B and 74% of rosmarinic acid. An amount each of 4.6 mg of coptisine and 4.1 mg of berberine was obtained from Rhizoma coptidis each with 98% and 82% purity, respectively. The processing time was nearly 50% that of the multi-step method. These results indicate that the present method is a rapid and green way to harvest targets from medicinal plants in a single step. PMID:24588208

  15. 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.

  16. 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. PMID:25204267

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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. PMID:26847919

  3. Air stripping and emissions control technologies: Field testing of countercurrent packings, rotary air stripping, catalytic oxidation, and adsorption materials. Final report, April 1987-June 1989

    SciTech Connect

    Wilson, J.H.; Counce, R.M.; Lucero, A.J.; Jennings, H.L.; Singh, S.P.

    1992-05-01

    The objective of this activity was to field test innovative air stripping with emissions control technologies. The scale of the various components used in these tests was selected such that results would be useful for better predicting the performance of application-scale equipment. The goal of this effort was to provide managers and engineers with necessary information so that decisions relating to the application of this technology can proceed on a rational basis. Conventional countercurrent air stripping (with 4 different packing materials) were compared to a centrifugal contactor, also known as a rotary air stripper. Emissions control tests showed that the activity of the noble metal catalyst was lost before any useful abatement results were obtained. This loss in activity was attributed to poisoning by sulfur stripped from the groundwater. Control of the emissions by activated carbon was achieved. Significant quantities of lighter hydrocarbons were noted in the stripper effluent that were not effectively adsorbed by the carbon. No generally useful results ere obtained for control of emissions by molecular sieves.... Air stripping, Rotary air stripper, VOCs, Fuel contamination, Catalytic oxidations, Carbon adsorption, Molecular sieves.

  4. 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

  5. Diagnosis of cystic echinococcosis: ultrasound imaging or countercurrent immunoelectrophoresis?

    PubMed

    Sadjjadi, S M; Ardehali, S; Noman-Pour, B; Kumar, V; Izadpanah, A

    2001-11-01

    Cystic echinococcosis is a major zoonotic diseases in the Islamic Republic of Iran. This study was carried out in 3 general hospitals in Shiraz. We examined the records of all 1227 surgical patients with a surgically-proven diagnosis of cystic echinococcosis for the 20-year period 1978-98. The results of countercurrent immunoelectrophoresis were compared with pathology and ultrasound reports to determine whether serological tests could be helpful for diagnosis. Countercurrent immunoelectrophoresis could detect only 62.0% of cases, whereas the pathology and ultrasound results were positive for 96.3% of cases. This study confirms the usefulness of ultrasound and suggests that only in doubtful cases would countercurrent immunoelectrophoresis be useful for diagnosing cystic echinococcosis.

  6. Optimization of the Ultrasonic-Assisted Extraction of Bioactive Flavonoids from Ampelopsis grossedentata and Subsequent Separation and Purification of Two Flavonoid Aglycones by High-Speed Counter-Current Chromatography.

    PubMed

    Zhang, Hongbing; Xie, Guoyong; Tian, Mei; Pu, Qian; Qin, Minjian

    2016-01-01

    The fermented leaf of Ampelopsis grossedentata has been used as a beverage and folk medicine called "vine tea" in the southern region of China. In this paper, the optimum extraction conditions for the maximum recovery amounts of total flavonoids (TF), dihydromyricetin (DMY), myricitrin (MYG) and myricetin (MY) from natural Ampelopsis grossedentata leaves subjected to ultrasonic-assisted extraction (UAE) were determined and optimized by using response surface methodology. The method was employed by the Box-Behnken design (BBD) and Derringer's desirability function using methanol concentration, extraction time, liquid/solid ratio as factors and the contents of TF, DMY, MYG and MY as responses. The obtained optimum UAE conditions were as follows: a solvent of 80.87% methanol, an extraction time of 31.98 min and a liquid/solid ratio of 41.64:1 mL/g. Through analysis of the response surface, it implied that methanol concentration and the liquid/solid ratio had significant effects on TF, DMY, MYG and MY yields, whereas extraction time had relatively little effects. The established extraction and analytical methods were successfully applied to determine the contents of the total flavonoids and three individual flavonoids in 10 batches of the leaf samples of A. grossedentata from three counties in Fujian Province, China. The results suggested the variability in the quality of A. grossedentata leaves from different origins. In addition, high purities of dihydromyricetin and myricetin were simultaneously separated and purified from the extract subjected to optimized UAE, by high-speed counter-current chromatography using a solvent system of N-hexane-ethyl acetate-methanol-water (1:3:2:4; v/v/v/v). In a single operation, 200 mg of the extract were separated to yield 86.46 mg of dihydromyricetin and 3.61 mg of myricetin with the purity of 95.03% and 99.21%, respectively. The results would be beneficial for further exploiting the herbal products and controlling the quality of

  7. 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

  8. 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

  9. 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.

  10. 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.

  11. SNS EXTRACTION KICKER POWER SUPPLY PROTOTYPE TEST

    SciTech Connect

    MI,J.L.; SANDBERG,J.; SANDERS,R.; SOUKAS,A.; ZHANG,W.

    2000-06-27

    The SNS (Spallation Neutron Source) accumulator ring Extraction System consists of a Fast kicker and a Lambertson Septum magnet. The proposed design will use 14 kicker magnets powered by an Extraction Kicker Power Supply System. They will eject the high power beam from the SNS accumulator ring into RTBT (Ring to Target Beam Tunnel) through a Lambertson Septum magnet. This paper describes some test results of the SNS Extraction Kicker power supply prototype. The high repetition rate of 60 pulse per second operation is the challenging part of the design. In the prototype testing, a 3 kA damp current of 700ns pulse-width, 200 nS rise time and 60 Hz repetition rate at 32 kV PFN operation voltage has been demonstrated. An Extraction kicker power supply system design diagram is depicted.

  12. 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. PMID:25800228

  13. Extracting laboratory test information from biomedical text

    PubMed Central

    Kang, Yanna Shen; Kayaalp, Mehmet

    2013-01-01

    Background: No previous study reported the efficacy of current natural language processing (NLP) methods for extracting laboratory test information from narrative documents. This study investigates the pathology informatics question of how accurately such information can be extracted from text with the current tools and techniques, especially machine learning and symbolic NLP methods. The study data came from a text corpus maintained by the U.S. Food and Drug Administration, containing a rich set of information on laboratory tests and test devices. Methods: The authors developed a symbolic information extraction (SIE) system to extract device and test specific information about four types of laboratory test entities: Specimens, analytes, units of measures and detection limits. They compared the performance of SIE and three prominent machine learning based NLP systems, LingPipe, GATE and BANNER, each implementing a distinct supervised machine learning method, hidden Markov models, support vector machines and conditional random fields, respectively. Results: Machine learning systems recognized laboratory test entities with moderately high recall, but low precision rates. Their recall rates were relatively higher when the number of distinct entity values (e.g., the spectrum of specimens) was very limited or when lexical morphology of the entity was distinctive (as in units of measures), yet SIE outperformed them with statistically significant margins on extracting specimen, analyte and detection limit information in both precision and F-measure. Its high recall performance was statistically significant on analyte information extraction. Conclusions: Despite its shortcomings against machine learning methods, a well-tailored symbolic system may better discern relevancy among a pile of information of the same type and may outperform a machine learning system by tapping into lexically non-local contextual information such as the document structure. PMID:24083058

  14. Solvent Extraction of Tc and Cs from Alkaline Nitrate Wastes

    SciTech Connect

    Bonnesen, P.V.; Conner, C.; Delmau, L.H.; Haverlock, T.J.; Leonard, R.A.; Lumetta, G.J.; Moyer, B.A.; Sachleben, R.A.

    1999-07-11

    This paper summarizes progress at three collaborating US national laboratories on the extraction of the fission products {sup 99}Tc and {sup 137}Cs from alkaline high-level wastes (HLW). Efficient, economical processes for Tc and Cs extraction (SRTALK and alkaline-side CSEX, respectively) have been developed, and testing has progressed through batch tests on actual wastes and continuous countercurrent centrifugal-contactor tests on simulants.

  15. 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.

  16. Recent progress on countercurrent chromatography modeling

    PubMed Central

    Wang, Fengkang; Ito, Yoichiro; Wei, Yun

    2014-01-01

    As countercurrent chromatography is becoming an established method in chromatography for many kinds of products, it is becoming increasingly important to model the process and to be able to predict the peaks for a given process. The CCC industries are looking for rapid methods to analyze the processes of countercurrent chromatography and select suitable solvent system. In this paper, recent progress is reviewed in the development and demonstration of several types of models of countercurrent chromatography. Literature lists a number of countercurrent chromatography (CCC) models that can predict the retention time and to a certain extent the peak width of a solute eluting from a CCC column, such as cell model, CCD model, CSTRs model, probabilistic model, temperature dependence plate model, physical models, etc. PMID:25580072

  17. 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)

  18. 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.

  19. 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. PMID:23240206

  20. 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.

  1. 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.

  2. Universal counter-current chromatography modelling based on counter-current distribution.

    PubMed

    de Folter, Joost; Sutherland, Ian A

    2009-05-01

    There is clearly a need for a model which is versatile enough to take into account the numerous operating modes and pump out procedures that can be used with counter-current chromatography (CCC). This paper will describe a universal model for counter-current chromatography based on counter-current distribution. The model is validated with real separations from the literature and against established CCC partition theory. This universal model is proven to give good results for isocratic flow modes, as well as for co-current CCC and dual flow CCC, and will likely also give good results for other modes such as intermittent CCC. PMID:19070863

  3. Countercurrent flooding in vertical-to-inclined pipes

    SciTech Connect

    Kawaji, M.; Thomson, L.A. ); Krishnan, V.S. )

    1991-01-01

    This paper reports on countercurrent flooding data obtained using air and water for vertical-to- downwardly inclined pipes containing elbows of varying angles. Experiments were performed with six different test sections, all having an inner diameter of 51 mm and a 1-m- long vertical tube connected to an inclined or horizontal tube. The flooding data for 112.5{degrees} and 135{degrees} elbow angles were almost identical and showed that these geometries required the largest gas flow rates for flooding among all the geometries tested. The flooding gas velocities for the 157.5{degrees} elbow were slightly less than those of the 112.5{degrees} and 135{degrees} elbows but greater than those of the vertical pipe without any elbow and vertical-to- horizontal pipes at low to moderate liquid flow rates. In all vertical-to-inclined pipes, flooding was initiated in the inclined section at about 15 to 50 cm downstream of the elbow. Due to the countercurrent flow of gas, the liquid stream just downstream of the elbow became highly agitated and a frothy mixture was carried upstream by gas at flooding. At moderate to high liquid flow rates, the liquid was deflected off at the elbow to form a turbulent, jetlike stream that partially broke up into droplets. These droplets were, at the onset of flooding, entrained and carried over by the gas stream.

  4. 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

  5. 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.

  6. 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

  7. Enrichment and separation of antitumor triterpene acids from the epidermis of Poria cocos by pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography.

    PubMed

    Dong, Hongjing; Wu, Panpan; Yan, Renyi; Xu, Qihua; Li, Hua; Zhang, Fangbo; Li, Jianrong; Yang, Bin

    2015-06-01

    Triterpene acids were extracted from the epidermis of Poria cocos (Schw.) Wolf. These acids were found to inhibit the growth of lung cancer cells in vitro and in vivo. An efficient method for the preparative separation of antitumor triterpene acids was established that involves the combination of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography. We used pH-zone-refining counter-current chromatography to concentrate the triterpene acids using a two-phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (3:7:5:5, v/v/v/v), trifluoroacetic acid (10 mM) was added to the upper phase as a retainer, and ammonia (10 mM) was added to the lower phase as an eluter. As a result, 200 mg concentrate of triterpene acids was obtained from 1.0 g of crude extract. The concentrate was further separated by conventional high-speed counter-current chromatography using a solvent system composed of petroleum ether/ethyl acetate/methanol/water (0.8:1.2:1.2:0.9, v/v), yielding 50 mg of poricoic acid A and 5 mg of poricoic acid B from 120 mg concentrate, respectively. The inhibitory activity of the major compound on lung A549 cells was examined and poricoic acid A was found to significantly inhibit the growth of A 549 cells.

  8. Enrichment and separation of antitumor triterpene acids from the epidermis of Poria cocos by pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography.

    PubMed

    Dong, Hongjing; Wu, Panpan; Yan, Renyi; Xu, Qihua; Li, Hua; Zhang, Fangbo; Li, Jianrong; Yang, Bin

    2015-06-01

    Triterpene acids were extracted from the epidermis of Poria cocos (Schw.) Wolf. These acids were found to inhibit the growth of lung cancer cells in vitro and in vivo. An efficient method for the preparative separation of antitumor triterpene acids was established that involves the combination of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography. We used pH-zone-refining counter-current chromatography to concentrate the triterpene acids using a two-phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (3:7:5:5, v/v/v/v), trifluoroacetic acid (10 mM) was added to the upper phase as a retainer, and ammonia (10 mM) was added to the lower phase as an eluter. As a result, 200 mg concentrate of triterpene acids was obtained from 1.0 g of crude extract. The concentrate was further separated by conventional high-speed counter-current chromatography using a solvent system composed of petroleum ether/ethyl acetate/methanol/water (0.8:1.2:1.2:0.9, v/v), yielding 50 mg of poricoic acid A and 5 mg of poricoic acid B from 120 mg concentrate, respectively. The inhibitory activity of the major compound on lung A549 cells was examined and poricoic acid A was found to significantly inhibit the growth of A 549 cells. PMID:25821060

  9. 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

  10. Counter-current flow limited CHF in thin rectangular channels

    SciTech Connect

    Cheng, L.Y.

    1990-01-01

    An analytical expression for counter-current-flow-limitation (CCFL) was used to predict critical heat flux (CHF) for downward flow in thin vertical rectangular channels which are prototypes of coolant channels in test and research nuclear reactors. Top flooding is the mechanism for counter-current flow limited CHF. The CCFL correlation also was used to determine the circulation and flooding-limited CHF. Good agreements were observed between the period the model predictions and data on the CHF for downflow. The minimum CHF for downflow is lower than the flooding-limited CHF and it is predicted to occur at a liquid flow rate higher than that at the flooding limit. 17 refs., 7 figs.

  11. Isolation of achyrobichalcone from Achyrocline satureioides by high- speed countercurrent chromatography.

    PubMed

    Carini, Juliana P; Leitão, Gilda G; Schneider, Paulo H; Santos, Cristiane C; Costa, Fernanda N; Holzschuh, Maribete H; Klamt, Fábio; Bassani, Valquiria L

    2015-01-01

    Achyrobichalcone is a biflavonoid recently found in Achyrocline satureioides. This substance has unprecedented chemical structure and occurrence, but resembles other bioactive bichalcones, which have important pharmacological properties, such as anticancer activity. The major challenge for evaluation of the physicochemical and biological properties of this new molecule is the isolation step, which affects the purity and yield of the isolated product. Thus, the objective of this work was to develop a semi-preparative method for achyrobichalcone isolation from Achyrocline satureioides by high-speed countercurrent chromatography. The high-speed countercurrent chromatography separation was achieved in two steps. In the first step, an enriched fraction of achyrobichalcone from the freeze-dried extract was obtained, using the solvent system hexane-ethyl acetate-methanol-water 0.8:1:0.8:1, v/v. The purification of achyrobichalcone from the enriched fractions was achieved by further high-speed countercurrent chromatography fractionation with hexane-ethyl acetate-methanol-water 0.9:0.9:0.8:1, v/v. The final isolated product was obtained using preparative thin layer chromatography and crystallization procedure. A yellow semi-crystalline solid with purity close to 90% was obtained as the final product. The mass recovery of achyrobichalcone isolation was near 67%. The structural identification from spectroscopic and chromatographic techniques confirmed the achyrobichalcone structure. This is the first report of achyrobichalcone isolation on a semi-preparative scale by high-speed countercurrent chromatography. This method afforded achyrobichalcone in good yield and purity for further biopharmaceutical studies.

  12. Countercurrent-distribution studies on histones

    PubMed Central

    Butler, J. A. V.; Power, D. F.; Palau, J.

    1967-01-01

    1. The possibilities of fractionating histones and histone fractions by means of countercurrent distribution between two phases formed by water and butan-2-ol, in the presence of various concentrations of trichloroacetic acid, have been examined. 2. Although the principal histone fractions differ considerably in their partition ratios, a satisfactory resolution of the principal histone fractions from the whole histone has not been achieved. 3. The histone fractions obtained by other methods can be resolved with suitable concentrations of trichloroacetic acid. Besides the main peak several subsidiary peaks are obtained in most cases, the composition of which corresponds with others of the main fractions. 4. The method is therefore capable of removing from the principal fractions as previously prepared contamination by other fractions. 5. Except in one case, no fraction with composition unlike other fractions has been obtained. In several cases the material isolated from the principal peak behaves as a single component on running again. In two cases fractions with similar compositions were distinguished by countercurrent distribution. PMID:6029613

  13. 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.

  14. 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.

  15. 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

  16. Fishing and knockout of bioactive compounds using a combination of high-speed counter-current chromatography (HSCCC) and preparative HPLC for evaluating the holistic efficacy and interaction of the components of Herba Epimedii.

    PubMed

    Jin, Jing; Li, Yubo; Kipletting Tanui, Emmanuel; Han, Liwen; Jia, Yuan; Zhang, Lu; Wang, Yuming; Zhang, Xiuxiu; Zhang, Yanjun

    2013-05-20

    Due to the complex chemical compositions and pharmacological effects of traditional Chinese medicines, we developed a strategy based on fishing and knockout of bioactive compounds using a combination of high-speed counter-current chromatography (HSCCC) and preparative HPLC for evaluating the holistic activity and interaction of the components of Herba Epimedii. First, osteoblast target cell extraction was used for preliminary screening of the potential bioactive compounds of Herba Epimedii. Second, the bioactive compounds identified (epimedin A, epimedin B, epimedin C and icariin) were fished and knocked out using high-speed counter-current chromatography and preparative HPLC. Third, the bioactivity of resulting fractions was assessed by determining their influence on cell proliferation and differentiation, thereby allowing for an evaluation of their interaction.The pharmacodynamic contribution ratio of each bioactive compound to the efficacy of the herbal medicine could then be comprehensively and intuitively determined based on the spectra-activity correlations (VIP values) of the tested compositions using partial least-squares regression (PLS-R), through which the reliability of the screening and isolation of bioactive compounds by the target cell extraction technique were verified. The proposed strategy is a useful approach with potential application in other traditional Chinese medicines.

  17. Rapid detection of enteric fever by coagglutination and countercurrent immunoelectrophoresis.

    PubMed

    Mishra, M; Thakar, Y S; Chande, C; Tankhiwale, N S; Saoji, A M

    1998-10-01

    A total of 463 patients clinically suspected of enteric fever and 100 healthy individuals were investigated by coagglutination (COAG) and countercurrent immunoelectrophoresis (CIEP) for rapid diagnosis of enteric fever. The S. typhi was grown in blood culture in 32 (6.91%) and Widal test was positive in 126 (27.21%) cases. The serum COAG with local antiserum was positive in 165 (35.64%), serum COAG with standard antiserum in 163 (35.21%), Blood culture supernatant (BCS) COAG in 153 (33.05%), serum CIEP for antigen (Ag) in 118 (25.09%), BCS CIEP in 99 (21.39%) while serum CIEP for antibody (Ab) was positive in 34 (7.34%) cases. Only two healthy controls revealed positive COAG result with local antiserum. The sensitivity of all antigen detection tests was 100% except BCS CIEP (98.25%) in the first week of fever and declined rapidly to 75.79% for serum COAG tests, 69.47% for BCS COAG and dramatically to 37.89% for serum CIEP for Ag and 22.11% for BCS CIEP tests during the second week whereas the sensitivity of serum CIEP for Ab detection rose from 17.54% to 23.16% from first to second week of illness. In view of the resulting data, it is suggested that both COAG and CIEP may be employed for the rapid diagnosis of enteric fever in the routine clinical setup.

  18. 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.

  19. 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.

  20. 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

    2012-11-01

    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.

  1. 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.

  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. Detection of circulating antigen in amoebic liver abscess by counter-current immunoelectrophoresis.

    PubMed

    Parija, S C; Karki, B M

    1999-01-01

    Fifty serum samples from patients with amoebic liver abscess and 50 from subjects who had not suffered from the disease (25 from patients with other, chiefly parasitic, infections and 25 from healthy blood donors, staff or students) were tested for circulating amoebic antigen by counter-current immuno-electrophoresis (CIEP). Amoebic antigen was detected in 38 sera (76%) from cases of amoebic liver abscess, but in none of the other sera. Although CIEP is only moderately sensitive, the high specificity suggests that this simple test may be useful in the diagnosis of amoebic liver abscess.

  4. [In vitro chromosome aberration test and in vivo micronucleus test of Ca-type Garcinia extract].

    PubMed

    Ono, Hiromi; Tamura, Hideyuki; Yamashita, Yasuhiro; Tamura, Kouichi; Iwakura, Keiko

    2006-04-01

    The induction of chromosome aberration of Ca-type Garcinia cambogia extract containing about 65% (-)-hydroxycitric acid was investigated by use of the chromosome aberration test in cultured Chinese hamster lung cells (CHL/IU) and the micronucleus test in mice. In the chromosome aberration test, Ca-type Garcinia cambogia extract did not increase the number of cells with structural aberration and/or numerical aberrations. The micronucleus test was carried out with bone marrow cells of Slc : ddY male mice after single oral administration of up to 2,000 microg/kg. There was no significant increase in the frequency of micronucleated polychromatic erythrocytes. These results indicate that Ca-type Garcinia cambogia extract does not induce chromosome aberration. PMID:16729669

  5. 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.

  6. 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.

  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 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.

  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 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.

  9. Test plan for demonstrating plutonium extraction from 10-L solutions using EIChrom extraction chromatographic resins

    SciTech Connect

    Barney, G.S.

    1994-08-15

    Corrosive plutonium solutions stored in 10-L containers at the Plutonium Finishing Plant must be treated to convert the plutonium to a safe, solid form for storage and to remove the americium so that radiation exposure can be reduced. Extraction chromatographic resins will be tested for separating plutonium from these solutions in the laboratory. Separation parameters will be developed during the testing for large scale processing of the 10-L solutions and solutions of similar composition. Use of chromatographic resins will allow plutonium separation with minimum of chemical addition to the feed and without the need for plutonium valence adjustment. The separated plutonium will be calcined to plutonium oxide by direct solution calcination.

  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. Preparative separation of six rhynchophylla alkaloids from Uncaria macrophylla wall by pH-zone refining counter-current chromatography.

    PubMed

    Zhang, Qinghai; Lin, Changhu; Duan, Wenjuan; Wang, Xiao; Luo, Aiqin

    2013-12-12

    pH-Zone refining counter-current chromatography was successfully applied to the preparative isolation and purification of six alkaloids from the ethanol extracts of Uncaria macrophylla Wall. Because of the low content of alkaloids (about 0.2%, w/w) in U. macrophylla Wall, the target compounds were enriched by pH-zone refining counter-current chromatography using a two-phase solvent system composed of petroleum ether-ethyl acetate-isopropanol-water (2:6:3:9, v/v), adding 10 mM triethylamine in organic stationary phase and 5 mM hydrochloric acid in aqueous mobile phase. Then pH-zone refining counter-current chromatography using the other two-phase solvent system was used for final purification. Six target compounds were finally isolated and purified by following two-phase solvent system composed of methyl tert-butyl ether (MTBE)-acetonitrile-water (4:0.5:5, v/v), adding triethylamine (TEA) (10 mM) to the organic phase and HCl (5 mM) to aqueous mobile phase. The separation of 2.8 g enriched total alkaloids yielded 36 mg hirsutine, 48 mg hirsuteine, 82 mg uncarine C, 73 mg uncarine E, 163 mg rhynchophylline, and 149 mg corynoxeine, all with purities above 96% as verified by HPLC Their structures were identified by electrospray ionization-mass spectrometry (ESI-MS) and 1H-NMR spectroscopy.

  13. Isolation of α-Amylase Inhibitors from Kadsura longipedunculata Using a High-Speed Counter-Current Chromatography Target Guided by Centrifugal Ultrafiltration with LC-MS.

    PubMed

    Cen, Yin; Xiao, Aiping; Chen, Xiaoqing; Liu, Liangliang

    2016-01-01

    In this study, a high-speed counter-current chromatography (HSCCC) separation method target guided by centrifugal ultrafiltration with high-performance liquid chromatography-mass spectrometry (CU-LC-MS) was proposed. This method was used to analyze α-amylase inhibitors from Kadsura longipedunculata extract. According to previous screening with CU-LC-MS, two screened potential α-amylase inhibitors was successfully isolated from Kadsura longipedunculata extract using HSCCC under the optimized experimental conditions. The isolated two target compounds (with purities of 92.3% and 94.6%) were, respectively, identified as quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) based on the MS, UV, and ¹H-NMR spectrometry data. To verify the inhibition of screened compounds, the inhibitory activities of quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) on α-amylase were tested, and it demonstrated that the experimental IC50 values of quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) were 28.8 and 12.5 μmol/L. These results proved that the hyphenated technique using CU-LC-MS and HSCCC was a rapid, competent, and reproductive method to screen and separate potential active compounds, like enzyme inhibitors from the extract of herbal medicines.

  14. Isolation of α-Amylase Inhibitors from Kadsura longipedunculata Using a High-Speed Counter-Current Chromatography Target Guided by Centrifugal Ultrafiltration with LC-MS.

    PubMed

    Cen, Yin; Xiao, Aiping; Chen, Xiaoqing; Liu, Liangliang

    2016-01-01

    In this study, a high-speed counter-current chromatography (HSCCC) separation method target guided by centrifugal ultrafiltration with high-performance liquid chromatography-mass spectrometry (CU-LC-MS) was proposed. This method was used to analyze α-amylase inhibitors from Kadsura longipedunculata extract. According to previous screening with CU-LC-MS, two screened potential α-amylase inhibitors was successfully isolated from Kadsura longipedunculata extract using HSCCC under the optimized experimental conditions. The isolated two target compounds (with purities of 92.3% and 94.6%) were, respectively, identified as quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) based on the MS, UV, and ¹H-NMR spectrometry data. To verify the inhibition of screened compounds, the inhibitory activities of quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) on α-amylase were tested, and it demonstrated that the experimental IC50 values of quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) were 28.8 and 12.5 μmol/L. These results proved that the hyphenated technique using CU-LC-MS and HSCCC was a rapid, competent, and reproductive method to screen and separate potential active compounds, like enzyme inhibitors from the extract of herbal medicines. PMID:27617987

  15. 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.

  16. 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.

  17. Separation and purification of hydrolyzable tannin from Geranium wilfordii Maxim by reversed-phase and normal-phase high-speed counter-current chromatography.

    PubMed

    Liu, Dan; Su, Zhiguo; Wang, Changhai; Gu, Ming; Xing, Siliang

    2010-08-01

    Three hydrolyzable tannins, geraniin, corilagin and gallic acid, main active components of Geranium wilfordii Maxim, have been separated and purified in one-step by both reversed-phase and normal-phase high-speed counter-current chromatography. Gallic acid, corilagin and geraniin were purified from 70% aqueous acetone extract of G. wilfordii Maxim with solvent system n-hexane-ethyl acetate-methanol-acetic acid-water (1:10:0.2:0.2:20) by reversed-phase high-speed counter-current chromatography at purities of 94.2, 91.0 and 91.3%, at yields of 89.3, 82.9 and 91.7%, respectively. Gallic acid, corilagin and geraniin were purified with solvent system n-hexane-ethyl acetate-methanol-acetic acid-water (0.2:10:2:1:5) by normal-phase high-speed counter-current chromatography at purities of 85.9, 92.2 and 87.6%, at yields of 87.4, 94.6 and 94.3%, respectively. It was successful for both reversed-phase and normal-phase high-speed counter-current chromatography to separate high-polarity of low-molecular-weight substances.

  18. Low sensitivity of counter-current immuno-electrophoresis for serodiagnosis of typhoid fever.

    PubMed

    Sharma, M; Datta, U; Roy, P; Verma, S; Sehgal, S

    1997-12-01

    Counter-current immuno-electrophoresis was evaluated as a diagnostic test for the serodiagnosis of typhoid fever with somatic (O), flagellar (H) and capsular polysaccharide (Vi) antigens of Salmonella typhi on the sera of patients who were blood culture positive (confirmed typhoid cases) or had high Widal agglutination titres, > or = 320, (presumptive typhoid cases). Of the 37 sera from confirmed cases, 30% showed positivity with O antigen, 24% with H antigens and 51% with Vi antigen. In patients with a presumptive diagnosis, 45% were positive for O antibody, 27% for flagellar antibody and 52% for Vi antibody. When all three antigens were combined the reactivity to any of the antigens was found to be 59% in confirmed typhoid cases, 79% in presumptive typhoid cases and 93% in patients who were simultaneously positive by blood culture and Widal agglutination. However, none of the sera from 45 controls gave a positive precipitation reaction with any of the antigens. It is concluded that counter-current immuno-electrophoresis is a rapid test with low sensitivity and high specificity with Vi antigen, a panel of antigens being most effective, and is, therefore, recommended for rapid diagnosis of typhoid fever.

  19. 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. PMID:25413585

  20. 40 CFR Appendix Ix to Part 268 - Extraction Procedure (EP) Toxicity Test Method and Structural Integrity Test (Method 1310B)

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 28 2012-07-01 2012-07-01 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...

  1. 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...

  2. 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...

  3. 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...

  4. Isolation and purification of the bioactive carotenoid zeaxanthin from the microalga Microcystis aeruginosa by high-speed counter-current chromatography.

    PubMed

    Chen, Feng; Li, Hua-Bin; Wong, Ricky Ngok-Shun; Ji, Bo; Jiang, Yue

    2005-02-01

    High-speed counter-current chromatography was successfully applied for the first time to the isolation and purification of the bioactive carotenoid zeaxanthin from the cyanobacterium Microcystis aeruginosa. The crude zeaxanthin was obtained by extraction with organic solvents after the microalgal sample had been saponified. Preparative high-speed counter-current chromatography with a two-phase solvent system composed of n-hexane-ethyl acetate-ethanol-water (8:2:7:3, v/v/v/v) was successfully performed yielding zeaxanthin at 96.2% purity from 150 mg of the crude extract in a one-step separation. The recovery of zeaxanthin was 91.4%. This was also the first report that zeaxanthin was successfully separated and purified from microalgae.

  5. 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.

  6. Fractionation of Gallotannins from mango (Mangifera indica L.) kernels by high-speed counter-current chromatography and determination of their antibacterial activity.

    PubMed

    Engels, Christina; Gänzle, Michael G; Schieber, Andreas

    2010-01-27

    High-speed counter-current chromatography was applied to the separation of gallotannins from mango (Mangifera indica L.) kernels. The kernels were defatted and subsequently extracted with aqueous acetone [80% (v/v)]. The crude extract was purified by being partitioned against ethyl acetate. A hexane/ethyl acetate/methanol/water solvent system [0.5:5:1:5 (v/v/v/v)] was used in the head-to-tail mode to elute tannins according to their degree of galloylation (tetra-O-galloylglucose to deca-O-galloylglucose). The compounds were characterized using liquid chromatography and mass spectrometry in the negative ionization mode. Purities ranged from 72% (tetra-O-galloylglucose) to 100% (octa-O-galloylglucose). The iron binding capacity of gallotannins was dependent on the number of galloyl groups in the molecule, with a larger capacity at lower degrees of galloylation. The minimum inhibitory concentration against Bacillus subtilis did not change among the different gallotannins tested and was in the range of 0.05-0.1 g/L in Luria-Bertani broth but up to 20 times higher in media containing more iron and divalent cations.

  7. Preparative isolation and purification of iridoid glycosides from Fructus Corni by high-speed countercurrent chromatography

    PubMed Central

    Liang, Jinru; He, Jiao; Zhu, Sha; Zhao, Wenna; Zhang, Yongmin; Ito, Yoichiro; Sun, Wenji

    2012-01-01

    Using a two-phase solvent system composed of dichloromethane–methanol–n-butanol–water–acetic acid (5:5:3:4:0.1, v/v/v/v/v), high-speed countercurrent chromatography was successfully performed for isolation and purification of three iridoid glycosides from Fructus Corni for the first time. From 100 mg of a crude extract of Fructus Corni 7.9 mg of sweroside, 13.1 mg of morroniside, and 10.2 mg of loganin were obtained in less than 3 h with purities of 92.3, 96.3 and 94.2%, respectively. These target compounds were identified by ESI-MS, 1H NMR and 13C NMR. PMID:24899790

  8. 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.

  9. Isolation and purification of ginkgo flavonol glycosides from Ginkgo biloba leaves by high-speed counter-current chromatography.

    PubMed

    Zhang, Qiang; Chen, Li-Juan; Ye, Hao-Yu; Gao, Lei; Hou, Wenli; Tang, Minghai; Yang, Guangli; Zhong, Zhenhua; Yuan, Yuan; Peng, Aihua

    2007-08-01

    A high-speed counter-current chromatography method was developed for the separation and purification of bioactive flavonol glycosides from a crude ethanol extract of Ginkgo biloba leaves. The separation was performed with a two-phase solvent system composed of n-hexane-butanol-ethyl acetate-methanol-0.5% acetic acid (1:0.5:3.5:1:4, v/v) and three pure compounds were eluted in high purities in a one-step separation. Their purities were determined by HPLC and identified by MS,(1)H-NMR, and(13)C-NMR.

  10. 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.

  11. 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. PMID:3069856

  12. The effect of surfactant on counter-current gas-liquid flows in vertical tubes

    NASA Astrophysics Data System (ADS)

    Zadrazil, Ivan; Matar, Omar; Markides, Christos

    2015-11-01

    Counter-current gas-liquid flows in vertical tubes are often accompanied by flow reversal. This so-called ``flooding'' phenomenon could occur for at least a part of the liquid phase from a counter-current to a co-current state, against the action of gravity. This phenomenon is of central importance to the oil-and-gas and nuclear industries, and has received considerable attention experimentally. The large majority of the previous work in this area, however, has considered the case of pure fluids, in the absence of additives; the latter are used frequently in industry in an attempt to control the onset of various flow regimes with little understanding of the mechanisms underlying their influence on the interfacial dynamics. In this study, we address this issue by investigating the dynamics of flooding in the presence of surfactants in a 4 m long, 32.4 mm nominal bore polymethyl methacrylate test section using high-speed shadowgraphy, and axial-view imaging. The system parameters include the superficial gas and liquid velocities, and surfactant concentration. We show that the presence of surfactant can have a dramatic effect on the flow structures and the onset of flooding. The mechanisms responsible for these phenomena are analysed. EPSRC Programme Grant, MEMPHIS, EP/K0039761/1.

  13. 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)

  14. 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

  15. 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.

  16. Flow enhancement of deformable self-driven objects by countercurrent

    NASA Astrophysics Data System (ADS)

    Mashiko, Takashi; Fujiwara, Takashi

    2016-10-01

    We report numerical simulations of the mixed flows of two groups of deformable self-driven objects. The objects belonging to the group A (B) have drift coefficient D =DA (DB), where a positive (negative) value of D denotes the rightward (leftward) driving force. For co-current flows (DA ,DB > 0), the result is rather intuitive: the net flow of one group (QA) increases if the driving force of the other group is stronger than its own driving force (i.e., DB >DA), and decreases otherwise (DB countercurrent flows (DB < 0 countercurrent can be larger than the net flow with a weaker co-current. This phenomenon is observed only for deformable objects and results from the entanglement of objects, which in turn is caused by their deformability.

  17. Purification of rutin and nicotiflorin from the flowers of Edgeworthia chrysantha Lindl. by high-speed counter-current chromatography.

    PubMed

    Tong, Shengqiang; Yan, Jizhong; Chen, Gang; Lou, Jianzhong

    2009-01-01

    An ethanol extract of air-dried flowers of Edgeworthia chrysantha Lindl. was partitioned between water and petroleum, ethyl acetate, and n-butanol. The n-butanol extraction was initially purified by silica gel column chromatography to give a partially purified sample. The bioactive compound rutin, along with nicotiflorin, were successfully separated from the partially purified sample by high-speed counter-current chromatography. The two compounds were isolated from the plant of Edgeworthia genus for the first time. The two-phase solvent system used was composed of ethyl acetate-n-butanol-water at an optimized ratio of 4:1:5 (v/v/v). High-speed counter-current chromatography yielded, from 108 mg of the partially purified extract, 53 mg rutin and 32 mg nicotiflorin with 92.5% and 92.2% recovery, with each at over 96.5% purity by high-performance liquid chromatography analysis. Their structures were identified by 1H NMR and 13C NMR. PMID:19476699

  18. Numerical simulation of the countercurrent flow in a gas centrifuge

    SciTech Connect

    Cloutman, L.D.; Gentry, R.A.

    1981-01-01

    A finite difference method is presented for the numerical simulation of the axisymmetric countercurrent flows in gas centrifuge. A time-marching technique is used to relax an arbitrary initial condition to the desired steady-state solution. All boundary layers may be resolved, and nonlinear effects may be included. Numerical examples are presented. It is concluded that this technique is capable of accurately predicting the performance of a wide variety of machines under all operating conditions of interest.

  19. On the subsurface countercurrents in the Philippine Sea

    NASA Astrophysics Data System (ADS)

    Wang, Fan; Zang, Nan; Li, Yuanlong; Hu, Dunxin

    2015-01-01

    subsurface countercurrents in the Philippine Sea and their roles in water mass transportation have been reported in previous studies. Their existence is still controversial, and the underlying dynamics remains unclear. This study investigates the climatological structures and relationships of three subsurface countercurrents, namely the Mindanao Undercurrent (MUC), the Luzon Undercurrent (LUC), and the North Equatorial Undercurrent (NEUC), using recently available hydrographic and satellite altimeter data. The three subsurface currents below and opposite to the surface currents are confirmed by multisections analysis. The MUC, as traced at zonal sections between 6.5°N and 10.5°N, shows two northward velocity cores, both with maximum speed larger than 10 cm s-1. The LUC exhibits an obscure core with southward velocity larger than 2 cm s-1 under the Kuroshio at 18°N and 16.25°N sections. The eastward flowing NEUC also has two separated cores at 128.2°E and 130°E sections with velocity larger than 1 cm s-1. Analyses of θ-S relationship suggest that the southern part of NEUC is fed by the MUC with the South Pacific water and South/North Pacific water mixture, while the northern NEUC is likely a destiny of the North Pacific water carried by the LUC. Tightly associated with the opposite horizontal gradients between sea surface height (SSH) and the depth of thermocline (DTC), the subsurface countercurrents exist in connected zones where the baroclinic adjustment below the thermocline overcomes the barotropic forcing at the sea surface, which indicates the dynamical linkages among the three subsurface countercurrents.

  20. 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

  1. Schinus terebinthifolius scale-up countercurrent chromatography (Part I): High performance countercurrent chromatography fractionation of triterpene acids with off-line detection using atmospheric pressure chemical ionization mass spectrometry.

    PubMed

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

    2015-04-10

    'Countercurrent chromatography' (CCC) is an ideal technique for the recovery, purification and isolation of bioactive natural products, due to the liquid nature of the stationary phase, process predictability and the possibility of scale-up from analytical to preparative scale. In this work, a method developed for the fractionation of Schinus terebinthifolius Raddi berries dichloromethane extract was thoroughly optimized to achieve maximal throughput with minimal solvent and time consumption per gram of processed crude extract, using analytical, semi-preparative and preparative 'high performance countercurrent chromatography' (HPCCC) instruments. The method using the biphasic solvent system composed of n-heptane-ethyl acetate-methanol-water (6:1:6:1, v/v/v/v) was volumetrically scaled up to increase sample throughput up to 120 times, while maintaining separation efficiency and time. As a fast and specific detection alternative, the fractions collected from the CCC-separations were injected to an 'atmospheric pressure chemical ionization mass-spectrometer' (APCI-MS/MS) and reconstituted molecular weight MS-chromatograms of the APCI-ionizable compounds from S. terebinthifolius were obtained. This procedure led to the direct isolation of tirucallane type triterpenes such as masticadienonic and 3β-masticadienolic acids. Also oleanonic and moronic acids have been identified for the first time in the species. In summary, this approach can be used for other CCC scale-up processes, enabling MS-target-guided isolation procedures.

  2. Schinus terebinthifolius scale-up countercurrent chromatography (Part I): High performance countercurrent chromatography fractionation of triterpene acids with off-line detection using atmospheric pressure chemical ionization mass spectrometry.

    PubMed

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

    2015-04-10

    'Countercurrent chromatography' (CCC) is an ideal technique for the recovery, purification and isolation of bioactive natural products, due to the liquid nature of the stationary phase, process predictability and the possibility of scale-up from analytical to preparative scale. In this work, a method developed for the fractionation of Schinus terebinthifolius Raddi berries dichloromethane extract was thoroughly optimized to achieve maximal throughput with minimal solvent and time consumption per gram of processed crude extract, using analytical, semi-preparative and preparative 'high performance countercurrent chromatography' (HPCCC) instruments. The method using the biphasic solvent system composed of n-heptane-ethyl acetate-methanol-water (6:1:6:1, v/v/v/v) was volumetrically scaled up to increase sample throughput up to 120 times, while maintaining separation efficiency and time. As a fast and specific detection alternative, the fractions collected from the CCC-separations were injected to an 'atmospheric pressure chemical ionization mass-spectrometer' (APCI-MS/MS) and reconstituted molecular weight MS-chromatograms of the APCI-ionizable compounds from S. terebinthifolius were obtained. This procedure led to the direct isolation of tirucallane type triterpenes such as masticadienonic and 3β-masticadienolic acids. Also oleanonic and moronic acids have been identified for the first time in the species. In summary, this approach can be used for other CCC scale-up processes, enabling MS-target-guided isolation procedures. PMID:25757818

  3. 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.

  4. 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.

  5. 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.

  6. 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…

  7. 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.

  8. 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.

  9. Chiral ligand exchange high-speed countercurrent chromatography: mechanism, application and comparison with conventional liquid chromatography in enantioseparation of aromatic α-hydroxyl acids

    PubMed Central

    Tong, Shengqiang; Shen, Mangmang; Cheng, Dongping; Ito, Yoichiro; Yan, Jizhong

    2014-01-01

    This work concentrates on the separation mechanism and application of chiral ligand exchange high-speed countercurrent chromatography (HSCCC) in enantioseparations, and comparison with traditional chiral ligand exchange high performance liquid chromatography (HPLC). The enantioseparation of ten aromatic α-hydroxyl acids were performed by these two chromatographic methods. Results showed that five of the racemates were successfully enantioseparated by HSCCC while only three of the racemates could be enantioseparated by HPLC using a suitable chiral ligand mobile phase additive. For HSCCC, the two-phase solvent system was composed of butanol-water (1:1, v/v), to which N-n-dodecyl-L-proline was added in the organic phase as chiral ligand and cupric acetate was added in the aqueous phase as a transition metal ion. Various operation parameters in HSCCC were optimized by enantioselective liquid-liquid extraction. Based on the results of the present studies the separation mechanism for HSCCC was proposed. For HPLC, the optimized mobile phase composed of aqueous solution containing 6 mmol L−1 L-phenylalanine and 3 mmol L−1 cupric sulfate and methanol was used for enantioseparation. Among three ligands tested on a conventional reverse stationary phase column, only one was found to be effective. In the present studies HSCCC presented unique advantages due to its high versatility of two-phase solvent systems and it could be used as an alternative method for enantioseparations. PMID:25087742

  10. Isolation of a polysaccharide with anticancer activity from Auricularia polytricha using high-speed countercurrent chromatography with an aqueous two-phase system.

    PubMed

    Song, Guanglei; Du, Qizhen

    2010-09-17

    Polysaccharides from a crude extract of Auricularia polytricha were separated by high-speed countercurrent chromatography (HSCCC). The separation was performed with an aqueous two-phase system of PEG1000-K2HPO4-KH2PO4-H2O (0.5:1.25:1.25:7.0, w/w). The crude sample (2.0 g) was successfully separated into three polysaccharide components of AAPS-1 (192 mg), AAPS-2 (137 mg), and AAPS-3 (98 mg) with molecular weights of 162, 259, and 483 kDa, respectively. These compounds were tested for growth inhibition of transplanted S180 sarcoma in mice. AAPS-2 had an inhibition rate of 40.4%. The structure of AAPS-2 was elucidated from partial hydrolysis, periodate oxidation, acetylation, methylation analysis, and NMR spectroscopy (1H, 13C). These results showed AAPS-2 is a polysaccharide with a backbone of (1-->3)-linked-beta-d-glucopyranosyl and (1-->3, 6)-linked-beta-D-glucopyranosyl residues in a 2:1 ratio, and has one terminal (1-->)-beta-D-glucopyranosyl at the O-6 position of (1-->3, 6)-linked-beta-D-glucopyranosyl of the main chain. PMID:20719324

  11. Solvent extraction studies of coprocessing flowsheets: results from campaigns 3 and 4 of the Solvent-Extraction Test Facility (SETF)

    SciTech Connect

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

    1982-05-01

    Experiments on tri-n-butyl phosphate solvent extraction of uranium and plutonium at full activity levels (Campaigns 3 and 4) were conducted in the Solvent Extraction Test Facility (SETF), located in one of the heavily shielded cells of the Transuranium Processing Plant. The primary objectives were: (1) to demonstrate and evaluate the first two cycles of the Hot Engineering Facility flowsheets (codecontamination and partial partitioning), and (2) to investigate and evaluate the use of HNO{sub 2} as the reductant for tetravalent plutonium during reductive stripping operations. Secondary objectives were to determine the solvent extraction behavior of feed solutions prepared by dissolving fuel from a boiling water reactor (BWR) and to improve the solvent extraction feed clarification.

  12. 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.

  13. 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. PMID:27118320

  14. Commercially available Hypericum perforatum extracts do not decrease immobility of rats in the forced swimming test.

    PubMed

    Guilhermano, Luiz G; Ortiz, Luciana; Ferigolo, Maristela; Barros, Helena M T

    2004-01-01

    There are controversial results of clinical trials on the antidepressant effects of Hypericum perforatum, while several preclinical studies describe antidepressant properties for Hypericum extracts. This study evaluates the antidepressant effect of two commercially available hydroalcoholic extracts of H. perforatum standardized to contain 0.3% hypericin in comparison to imipramine (IMI), in the forced swimming test (FST). Wistar rats were treated with different doses of two Hypericum extracts, of hypericin or of IMI and submitted to the FST. The experiments were videotape recorded to detail immobile and active behaviors of rats during the procedures. The imported extract tested and hypericin did not modify rats' behaviors in the test, while IMI, a classical antidepressant, significantly shortened immobility and prolonged climbing behavior during forced swimming. The locally produced Hypericum extract significantly increased immobility duration as compared to the controls at the same time as climbing efforts were decreased. Therefore, the two different commercially available Brazilian hydroalcoholic H. perforatum extracts did not show the expected effects in a screening test for antidepressant agents, on the contrary, one of the extracts promoted a depressant-like effect in rats. Therefore, these extracts available to the population differ from other Hypericum extracts. At which step of the production or commercialization chain these extracts probably lost their therapeutic potential remains to be evaluated.

  15. Selective partitioning of mercury from co-extracted actinides in a simulated acidic ICPP waste stream

    SciTech Connect

    Brewer, K.N.; Herbst, R.S.; Tranter, T.J.

    1995-12-01

    The TRUEX process is being evaluated at the Idaho Chemical Processing Plant (ICPP) as a means to partition the actinides from acidic sodium-bearing waste (SBW). The mercury content of this waste averages 1 g/l. Because the chemistry of mercury has not been extensively evaluated in the TRUEX process, mercury was singled out as an element of interest. Radioactive mercury, {sup 203}Hg, was spiked into a simulated solution of SBW containing 1 g/l mercury. Successive extraction batch contacts with the mercury spiked waste simulant and successive scrubbing and stripping batch contacts of the mercury loaded TRUEX solvent (0.2 M CMPO-1.4 M TBP in dodecane) show that mercury will extract into and strip from the solvent. The extraction distribution coefficient for mercury, as HgCl{sub 2} from SBW having a nitric acid concentration of 1.4 M and a chloride concentration of 0.035 M was found to be 3. The stripping distribution coefficient was found to be 0.5 with 5 M HNO{sub 3} and 0.077 with 0.25 M Na{sub 2}CO{sub 3}. An experimental flowsheet was designed from the batch contact tests and tested counter-currently using 5.5 cm centrifugal contactors. Results from the counter-current test show that mercury can be removed from the acidic mixed SBW simulant and recovered separately from the actinides.

  16. 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. PMID:25542704

  17. An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography.

    PubMed

    Feng, Rui-Hong; Hou, Jin-Jun; Zhang, Yi-Bei; Pan, Hui-Qin; Yang, Wenzhi; Qi, Peng; Yao, Shuai; Cai, Lu-Ying; Yang, Min; Jiang, Bao-Hong; Liu, Xuan; Wu, Wan-Ying; Guo, De-An

    2015-08-28

    An efficient and target-oriented sample enrichment method was established to increase the content of the minor alkaloids in crude extract by using the corresponding two-phase solvent system applied in pH-zone-refining counter-current chromatography. The enrichment and separation of seven minor indole alkaloids from Uncaria rhynchophylla (Miq.) Miq. ex Havil(UR) were selected as an example to show the advantage of this method. An optimized two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v) was used in this study, where triethylamine (TEA) as the retainer and hydrochloric acid (HCl) as the eluter were added at the equimolar of 10mM. Crude alkaloids of UR dissolved in the corresponding upper phase (containing 10mM TEA) were extracted twice with lower phase (containing 10mM TEA) and lower phase (containing 10mM HCl), respectively, the second lower phase extract was subjected to pH-zone-refining CCC separation after alkalization and desalination. Finally, from 10g of crude alkaloids, 4g of refined alkaloids was obtained and the total content of seven target indole alkaloids was increased from 4.64% to 15.78%. Seven indole alkaloids, including 54mg isocorynoxeine, 21mg corynoxeine, 46mg isorhynchophylline, 35mg rhynchophylline, 65mg hirsutine, 51mg hirsuteine and 27mg geissoschizine methylether were all simultaneously separated from 2.5g of refined alkaloids, with the purity of 86.4%, 97.5%, 90.3%, 92.1%, 98.5%, 92.3%, and 92.8%, respectively. The total content and purities of the seven minor indole alkaloids were tested by HPLC and their chemical structures were elucidated by ESI-HRMS and (1)H NMR.

  18. 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)

  19. 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.

  20. Isolation of cyanidin 3-glucoside from blue honeysuckle fruits by high-speed counter-current chromatography.

    PubMed

    Chen, Liang; Xin, Xiulan; Lan, Rong; Yuan, Qipeng; Wang, Xiaojie; Li, Ye

    2014-01-01

    Blue honeysuckle fruits are rich in anthocyanins with many beneficial effects such as reduction of the risk of cardiovascular diseases, diabetes and cancers. High-speed counter-current chromatography (HSCCC) was used for the separation of anthocyanin on a preparative scale from blue honeysuckle fruit crude extract with a biphasic solvent system composed of tert-butyl methyl ether/n-butanol/acetonitrile/water/trifluoroacetic acid (2:2:1:5:0.01, v/v) for the first time in this paper. Each injection of 100 mg crude extract yielded 22.8 mg of cyanidin 3-glucoside (C3G) at 98.1% purity. The compound was identified by means of electro-spray ionisation mass (ESI/MS) and (1)H and (13)C nuclear magnetic resonance (NMR) spectra.

  1. ISOLATION OF GLYCOSIDES FROM THE BARKS OF ILEX ROTUNDA BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY

    PubMed Central

    Wang, Chun; Chao, Zhimao; Sun, Wen; Wu, Xiaoyi; Ito, Yoichiro

    2013-01-01

    Semi-preparative and preparative high-speed counter-current chromatography (HSCCC) were successfully used for isolation of glycosides from 50% ethanol extract of the dried barks of Ilex rotunda Thunb. (Aquifoliaceae) by using a two-phase solvent system composed of ethyl acetate-n-butanol-water (1:6:7, v/v/v). From 1.0 g of the extract, syringaresinol 4',4"-di-o-β-d-glucopyranoside (I, 20.2 mg),, syringin (II, 56.8 mg), sinapaldehyde glucoside (III, 26.2 mg),, syringaresinol 4'-o-β-d-glucopyranoside (IV, 20.4 mg), and pedunculoside (V, 45.1 mg) were obtained by one run of TBE-1000A HSCCC instrument with 1000 mL of column volume. Their structures were identified by IR, MS, and 1H and 13C NMR studies. Glycoside I was isolated from this plant for the first time. PMID:25132792

  2. ISOLATION OF GLYCOSIDES FROM THE BARKS OF ILEX ROTUNDA BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY.

    PubMed

    Wang, Chun; Chao, Zhimao; Sun, Wen; Wu, Xiaoyi; Ito, Yoichiro

    2014-04-01

    Semi-preparative and preparative high-speed counter-current chromatography (HSCCC) were successfully used for isolation of glycosides from 50% ethanol extract of the dried barks of Ilex rotunda Thunb. (Aquifoliaceae) by using a two-phase solvent system composed of ethyl acetate-n-butanol-water (1:6:7, v/v/v). From 1.0 g of the extract, syringaresinol 4',4"-di-o-β-d-glucopyranoside (I, 20.2 mg),, syringin (II, 56.8 mg), sinapaldehyde glucoside (III, 26.2 mg),, syringaresinol 4'-o-β-d-glucopyranoside (IV, 20.4 mg), and pedunculoside (V, 45.1 mg) were obtained by one run of TBE-1000A HSCCC instrument with 1000 mL of column volume. Their structures were identified by IR, MS, and (1)H and (13)C NMR studies. Glycoside I was isolated from this plant for the first time.

  3. Preparative separation and purification of gingerols from ginger (Zingiber officinale Roscoe) by high-speed counter-current chromatography.

    PubMed

    Zhan, Kunyou; Xu, Kun; Yin, Hongzong

    2011-06-15

    A novel method for purifying gingerols from ginger was developed using a high-speed counter-current chromatography (HSCCC). The two-phase solvent system such as light petroleum (bp 60-90°C)-ethyl acetate-methanol-water (5:5:6.5:3.5, v/v/v/v) was applied to the separation and purification of 6-, 8- and 10-gingerol from a crude extract of ginger. The experiment yielded 30.2mg of 6-gingerol, 40.5mg of 8-gingerol, 50.5mg of 10-gingerol from 200mg of crude extract in one-step separation. And the purity of these compounds was 99.9%, 99.9% and 99.2%, respectively, as determined by high-performance liquid chromatography (HPLC). Their structures were identified by gas chromatography-mass spectrometry (GC/MS) and (1)H, (13)C nuclear magnetic resonance (NMR). PMID:25213983

  4. Isolation and purification of canthaxanthin from the microalga Chlorella zofingiensis by high-speed counter-current chromatography.

    PubMed

    Hua-Bin, Li; Fan, King-Wai; Chen, Feng

    2006-03-01

    Certain microalgae are considered to be a potential source of canthaxanthin, which possesses strong antioxidant and anticancer activities. A high-speed counter-current chromatography (HSCCC) method was developed for the separation and purification of canthaxanthin from the microalga Chlorella zofingiensis. The crude canthaxanthin was obtained by extraction with organic solvents after the microalgal sample had been saponified. Preparative HSCCC, with a two-phase solvent system composed of n-hexane-ethanol-water (10:9:1 v/v), was successfully performed yielding canthaxanthin at 98.7% purity from 150 mg of the crude extract (2.1% canthaxanthin) in a one-step separation. The recovery of canthaxanthin was 92.3%. This was the first report that canthaxanthin was successfully separated and purified from microalgae.

  5. 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(+). PMID:26030975

  6. 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.

  7. Isolation of the Predominant Cycloartane Glycoside, Sutherlandioside B, from Sutherlandia frutescens R.Br. by Spiral Countercurrent Chromatography

    PubMed Central

    Brownstein, Korey J.; Rottinghaus, George E.; Knight, Martha; Ito, Yoichiro; Folk, William

    2014-01-01

    The introduction of spiral countercurrent chromatography in the last few years using new separation columns such as the spiral tubing support rotor has enabled the application of more polar volatile solvent systems for natural products separation. This method can be applied to water soluble compounds and their metabolites. We have used spiral countercurrent chromatography with the spiral tubing support rotor to fractionate n-butanol extracts of an African plant Sutherlandia frutescens and have determined conditions by which the predominant cycloartane glycoside (sutherlandioside B) can be purified in good yield. A solvent system of ethyl acetate, methanol, and water was modified by adding n-butanol to separate sutherlandioside B from other compounds. With the optimal amount of n-butanol in the two-phase solvent system with the lower aqueous phase mobile, the target compound was eluted well separated from the other components. The purity of sutherlandioside B was determined by high performance liquid chromatography/mass spectrometry analysis and the yield compares favorably with the content in bulk material. PMID:25646069

  8. 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. PMID:24311558

  9. Preparative isolation of seven diterpenoid alkaloids from Aconitum coreanum by pH-zone-refining counter-current chromatography.

    PubMed

    Wang, Xueyong; Shu, Xikai; Wang, Xiao; Yu, Jinqian; Jing, Feng

    2014-08-19

    The aim of this paper was to seek an efficient method to preparative separation of alkaloid compounds from Aconitum coreanum (Guanbaifu), a well-known traditional Chinese medicinal plant for heart disease. Seven alkaloid compounds were successfully purified by pH-zone-refining counter-current chromatography with two-phase solvent system of petroleum ether-ethyl acetate-methanol-water (5:5:1:9, v/v/v/v), 10 mM triethylamine in upper phase and 10 mM hydrochloric acid in lower phase. From 3.5 g of crude extract, 356 mg of Guanfu base I, 578 mg of Guanfu base A, 74 mg of atisine, 94 mg of Guanfu base F, 423 mg of Guanfu base G, 67 mg of Guanfu base R and 154 mg of Guanfu base P were obtained with the purity of 96.40%, 97.2%, 97.5%, 98.1%, 98.9%, 98.3% and 98.4%. Their chemical structures were identified by TOF-MS and 1H-NMR. This study indicated that pH-zone-refining counter-current chromatography was an efficient method for separating the kind of alkaloids with low absorbance values.

  10. 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. PMID:25686848

  11. Bubble column reactors for wastewater treatment. 1: Theory and modeling of continuous countercurrent solvent sublation

    SciTech Connect

    Smith, J.S.; Valsaraj, K.T.; Thibodeaux, L.J.

    1996-05-01

    Solvent sublation is a nonfoaming wastewater treatment process that combines the benefits of bubble fractionation and liquid-liquid extraction in a way that does not require mixers, settlers, or subsequent downstream treatment. A review of past work on small lab-scale batch columns revealed that removal efficiencies of nonvolatile and volatile organic compounds are generally higher than those observed in bubble fractionation, air stripping, and conventional liquid-liquid extraction. In this work, the first of a three-part series, the transport mechanisms in a three-phase continuous, countercurrent sublation process are presented. Two mathematical models, namely, the series CSTR model (SCM) and the two-phase axial dispersion model (ADM2), are developed. It is shown that these two models are equivalent and can be used interchangeably with the aid of a simple expression. Nondimensional correlations, based upon simulated data obtained from the SCM, are generated to predict the steady-state fractional removal, FR, and the separation factor, {Sigma} (ratio of effluent solvent concentration to effluent water concentration), for strongly hydrophobic compounds. The effects of operational, hydrodynamic, thermodynamic, and design variables on sublation performance are discussed.

  12. 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.

  13. Isolation of phenolics from Rhizophora mangle by combined counter-current chromatography and gel-filtration.

    PubMed

    Costa, Fernanda das Neves; da Silva, Marcos Daniel; Borges, Ricardo Moreira; Leitão, Gilda Guimarães

    2014-12-01

    Nine phenolic compounds, quercetin, epi-catechin, catechin, 4-hydroxybenzoic acid, kaempferol 3-O-β-glucopyranoside, quercetin 3-O-β-glucopyranoside, quercetin 3-O-6"-trans-coumaroyl-β-glucoside, kaempferol 3-O-β-rutinoside and quercetin 3-O-β-rutinoside, were isolated from the EtOAc leaf extract of Rhizophora mangle (Rhizophoraceae) combining counter-current chromatography (CCC) and gel-filtration. A solvent system of n-hexane-ethyl acetate-methanol-water (1.5:6:1.5:6) was employed at the preliminary stage of EtOAc extract fractionation as it was shown to contain compounds that differed highly in their hydrophobicity. The obtained fractions were further purified by either CCC or gel-filtration depending on their complexity. The isolated compounds were analyzed by NMR spectroscopy and the proposed structures were confirmed by HRES/ESI/TOF MS. Some of these compounds were isolated and/or identified for the first time in R. mangle. PMID:25632470

  14. [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. PMID:23342648

  15. 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...

  16. Prototype of a test bench for applied research on Extracted beams of the nuclotron accelerator complex

    NASA Astrophysics Data System (ADS)

    Baldin, A. A.; Berlev, A. I.; Bradnova, V.; Butenko, A. V.; Fedorov, A. N.; Kudashkin, I. V.

    2016-05-01

    The results of the development and testing of elements of a test bench for investigating the impact of accelerated particle beams on biological objects, electronics, and other targets are presented. The systems for beam monitoring and target positioning were tested on extracted argon beams in the framework of experiments on studying the radiation hardness of electronic components.

  17. 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...

  18. 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...

  19. Field vapor extraction test and long-term monitoring at a PCE contaminated site.

    PubMed

    Chai, J-C; Miura, N

    2004-07-01

    The results of a field investigation, vapor extraction tests, and long-term monitoring at a PCE-contaminated site in Saga, Japan, are reported. The field investigation indicated that PCE likely was trapped in a surface clayey sand layer (vadose zone), and soil vapor extraction (SVE) was adopted as the remediation approach. The field test results the effectiveness of SVE in removing volatile organic compounds (VOCs) from contaminated sites. For the case where the radius of influence for an extraction well was 15-20 m, the blower capacity had no obvious effect on the radius of influence possibly due to the short circuiting of air from the ground surface. However, the maximum negative pressure (difference between vapor pressure and ambient pressure) in the extraction well was approximately proportional to blower capacity for the range of blower capacities tested. The long-term monitoring results indicate that PCE concentration varied seasonably, and temperature and rainfall are two of the influencing factors.

  20. 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.

  1. 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.

  2. 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

  3. 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.

  4. 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

    2015-01-01

    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. PMID:26528961

  5. Heat extracted from the long term flow test in the Fenton Hill HDR reservoir

    SciTech Connect

    Kruger, Paul; Robinson, Bruce

    1994-01-20

    A long-term flow test was carried out in the Fenton Hill HDR Phase-2 reservoir for 14 months during 1992-1993 to examine the potential for supplying thermal energy at a sustained rate as a commercial demonstration of HDR technology. The test was accomplished in several segments with changes in mean flowrate due to pumping conditions. Re-test estimates of the extractable heat content above a minimum useful temperature were based on physical evidence of the size of the Fenton Hill reservoir. A numerical model was used to estimate the extent of heat extracted during the individual flow segments from the database of measured production data during the test. For a reservoir volume of 6.5x10{sup 6}m{sup 3}, the total heat content above a minimum temperature of 150{degree} C was 1.5x10{sup 15}J. For the total test period at the three sustained mean flowrates, the integrated heat extracted was 0.088x10{sup 15}J, with no discernable temperature decline of the produced fluid. The fraction of energy extracted above the abandonment temperature was 5.9%. On the basis of a constant thermal energy extraction rate, the lifetime of the reservoir (without reservoir growth) to the abandonment temperature would be 13.3 years, in good agreement with the pre-test estimate of 15.0 years for the given reservoir volume.

  6. [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.

  7. 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.

  8. Rapid separation of polysaccharides using a novel spiral coil column by high-speed countercurrent chromatography.

    PubMed

    Li, Weili; Wu, Tao

    2016-04-01

    The separation of polysaccharides is time consuming. We developed and optimized a type-J counter-current chromatography system with a novel tri-rotor spiral coil column for the rapid separation of polysaccharides. The optimal composition of an aqueous PEG1000/K2 HPO4 /KH2 PO4 system was found to be 14:16:14 w/w/w where the lower phase was the mobile phase. Optimal performance was achieved at a column rotational speed, temperature, and flow rate of 1200 rpm, 45°C, and 3.0 mL/min, respectively. The mobile phase was pumped from the inner terminal in a ''head-to-tail'' elution mode. Polysaccharide LCP-1 (10.7 mg) was successfully obtained in high purity in one step from 50.0 mg of a crude polysaccharide extracted from the lychee fruit (Litchi chinensis) within 100 min. LCP-1 possess a number-average molecular weight and weight-average molecular weight of 1.05 × 10(5) and 1.59 × 10(5) kDa, respectively. The monosaccharide composition consists of the molar ratio of glucose, galactose, and arabinose of 1.3:3.5:1.

  9. 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

  10. 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.

  11. Separation of amaranthine-type betacyanins by ion-pair high-speed countercurrent chromatography.

    PubMed

    Jerz, Gerold; Gebers, Nadine; Szot, Dominika; Szaleniec, Maciej; Winterhalter, Peter; Wybraniec, Slawomir

    2014-05-30

    Betacyanins, red-violet plant pigments, were fractionated by ion-pair high-speed countercurrent chromatography (IP-HSCCC) from leaves extract of Iresine lindenii Van Houtte, an ornamental plant of the family Amaranthaceae. An HSCCC solvent system consisting of TBME-1-BuOH-ACN-H2O (1:3:1:5, v/v/v/v) was applied using ion-pair forming heptafluorobutyric acid (HFBA). Significantly different elution profiles of betacyanin diastereomeric pairs (derivatives based on betanidin and isobetanidin) observed in the HSCCC in comparison to HPLC systems indicate a complementarity of both techniques' fractionation capabilities. The numerous diastereomeric pairs can be selectively separated from each other using the HSCCC system simplifying the pigment purification process. Apart from the three well known highly abundant pigments (amaranthine, betanin and iresinin I) together with their isoforms, three new acylated (feruloylated and sinapoylated) betacyanins as well as known pigment hylocerenin (previously isolated from cacti fruits) were characterized in the plant for the first time and they are new for the whole Amaranthaceae family.

  12. 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. PMID:27374588

  13. Flowsheet Modeling and Testing of Pseudohydroxide Extraction from Aqueous Sodium Hydroxide Solutions with 3,5-di-tert-Butylphenol in Isopar® L Modified with Exxal® 8

    SciTech Connect

    Arm, Stuart T.; Lumetta, Gregg J.; Levitskaia, Tatiana G.

    2007-09-01

    A conceptual counter-current process flowsheet was developed for sodium hydroxide recovery from alkaline solutions via pseudohydroxide extraction (PHE). PHE relies on a simple sodium ion/proton exchange mechanism at elevated pH using a weak organic acid extractant. Contact of the sodium-loaded organic phase with water results in the reconstitution of the extractant in the organic phase and sodium hydroxide in the aqueous phase. In this work, the 3,5-di-tert-butylphenol (35-DTBP) cation exchanger was used in the Isopar® L diluent modified with isooctyl alcohol Exxal® 8. Equilibrium isotherms determined for PHE from pure sodium hydroxide solutions and simulated radioactive waste leachate were used to develop a semi-empirical model that could be used for designing PHE process flowsheets. Using this model, a conceptual PHE flowsheet was developed for recovering NaOH from solutions generated by caustic leaching of radioactive tank sludges. The flowsheet consists of extraction, scrub, and strip processes, each employing four equilibrium stages. Modeling of this flowsheet indicates 97% recovery of the sodium hydroxide from the waste leachate feed solution. An experimental demonstration, performed with a simulated radioactive waste leachate using batch contacts in a co-current analog of the counter-current flowsheet, confirmed the potential for practical application of PHE technology.

  14. Preparative isolation and purification of alkaloids from Picrasma quassiodes (D. Don) Benn. by high-speed countercurrent chromatography

    PubMed Central

    Zhao, Wenna; He, Jiao; Zhang, Yongmin; Ito, Yoichiro; Su, Qi; Sun, Wenji

    2012-01-01

    By using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (2:2:2:2, v/v/v/v), a high-speed counter-current chromatography technique was successfully used for isolation and purification of three alkaloids from Picrasma quassiodes (D. Don) Benn. for the first time. A total of 22.1 mg of 3-methylcanthin-2,6-dione, 4.9 mg of 4-methoxy-5-hydroxycanthin-6-one and 1.2 mg of 1-mthoxycarbonyl-β-carboline were obtained from 100 mg of crude extract of Picrasma quassiodes (D. Don) Benn. in less than 5 h, with purities of 89.30%, 98.32% and 98.19%, respectively. The target compounds were identified by ESI-MS, 1H NMR and 13C NMR. PMID:22798720

  15. 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.

  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. 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. PMID:27433984

  18. Large-scale isolation and purification of geniposide from the fruit of Gardenia jasminoides Ellis by high-speed counter-current chromatography.

    PubMed

    Zhou, Tingting; Fan, Guorong; Hong, Zhanying; Chai, Yifeng; Wu, Yutian

    2005-12-23

    High-speed counter-current chromatography (HSCCC) was applied to the isolation and purification of geniposide from Gardenia jasminoides Ellis. Analytical HSCCC was used for the preliminary selection of a suitable solvent system composed of ethyl acetate-n-butanol-water (2:1:3, v/v/v). According to the above solvent system, preparative HSCCC was successfully performed with the optimal solvent system composed of ethyl acetate-n-butanol-water (2:1.5:3, v/v/v) yielding 389 mg of geniposide at over 98% purity from 1g of the partially purified extract with 38.9% recovery in a one-step separation.

  19. 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

  20. 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...

  1. An evaluation of acetone extracts from six plants in the Ames mutagenicity test.

    PubMed

    White, R D; Krumperman, P H; Cheeke, P R; Buhler, D R

    1983-01-01

    Acetone extracts from six plants were evaluated for mutagenic activity with the Salmonella/mammalian-microsome mutagenicity test (Ames) utilizing tester strains TA98 and TA100 and in the presence and absence of induced rat liver microsomes. Extracts from alfalfa (Medicago sativa), lettuce (Lactuca sativa) and thread-leaf groundsel (Senecio longilobus) produced only negative responses. Comfrey (Symphytum officinale) and tansy ragwort (Senecio jacobaea) extracts produced toxic responses that were abolished in the presence of the microsomal bioactivation system. Bracken (Pteridium aquilinum) and tansy ragwort extracts produced positive responses following bioactivation with the liver microsomal system. The results suggest that the Ames mutagenicity test may be of some value in initial evaluations for potential toxic effects of plants consumed by animals and man. PMID:6836587

  2. 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.

  3. 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

  4. 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

  5. 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

    2009-10-01

    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

  6. 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

  7. 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

  8. Comprehensive separation of secondary metabolites in natural products by high-speed counter-current chromatography using a three-phase solvent system.

    PubMed

    Yanagida, Akio; Yamakawa, Yutaka; Noji, Ryoko; Oda, Ako; Shindo, Heisaburo; Ito, Yoichiro; Shibusawa, Yoichi

    2007-06-01

    High-speed counter-current chromatography (HSCCC) using the three-phase solvent system n-hexane-methyl acetate-acetonitrile-water at a volume ratio of 4:4:3:4 was applied to the comprehensive separation of secondary metabolites in several natural product extracts. A wide variety of secondary metabolites in each natural product was effectively extracted with the three-phase solvent system, and the filtered extract was directly submitted to the HSCCC separation using the same three-phase system. In the HSCCC profiles of crude natural drugs listed in the Japanese Pharmacopoeia, several physiologically active compounds were clearly separated from other components in the extracts. The HSCCC profiles of several tea products, each manufactured by a different process, clearly showed their compositional difference in main compounds such as catechins, caffeine, and pigments. These HSCCC profiles also provide useful information about hydrophobic diversity of whole components present in each natural product.

  9. 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

  10. 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.

  11. 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.

  12. 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. PMID:25627599

  13. 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.

  14. 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.

  15. Design of countercurrent separation of Ginkgo biloba terpene lactones by nuclear magnetic resonance.

    PubMed

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

    2012-06-15

    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 (1)H 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.

  16. Proper use of skin tests with food extracts in diagnosis of hypersensitivity to food in children.

    PubMed

    Bock, S A; Buckley, J; Holst, A; May, C D

    1977-07-01

    This study was undertaken to determine the proper use of skin tests with food extracts in diagnosis of hypersensitivity to food in children. Cutaneous reactions evoked by graded amounts of food extracts were compared with results of double-blind food challenge and in vitro release of histamine from leucocytes. A 3 mm or greater weal reaction in skin tests by puncture technique using food extracts of 1:20 w/v concentration was found to indicate the degree of hypersensitivity likely to be associated with clinically significant hypersensitivity reactions to food. Proper use of this simple technique will facilitate accurate diagnosis of food hypersensitivity in children by identifying the group among whom all positive reactions to food challenges will be found. Nevertheless, double-blind food challenge is essential to establish a diagnosis of symptomatic hypersensitivity to food.

  17. 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.

  18. 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.

  19. 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

  20. 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.

  1. [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.

  2. 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.

  3. Vortex Counter-Current Chromatography: Performance of a New Preparative Column

    PubMed Central

    Ito, Yoichiro; Clary, Robert; Witten, Jacob J.; Zeng, Yun

    2012-01-01

    A New preparative column for the vortex counter-current chromatograph was fabricated by making many (966) cylindrical separation units to a high-dendity polyethylene disk and thenthreading them with 6-40 taps. The resulting column had a total capacity of 364 mL. The performance of this vortex column was examined with three different two-phase solvent systems each using a set of suitable test samples: hexane-ethyl acetate-methanol-0.1 M hydrochloric acid (1:1:1:1, v/v) for separation of DNP-amino acids; 1-butanol-acetic acid-water (4:1:5, v/v) for separation of dipeptides; and hexane-acetonitrile-water (20:15:2, v/v) for separation of Sudan dyes. Most of the separations show high partition efficiency of over a thousand theoretical plates, as expected based on the results previously obtained in preliminary separations with a small column. Overall, the results of the present study suggest that further improvement of the partition efficiency can be obtained by the modifying column configuration. PMID:23503931

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

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

    PubMed

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

    2013-05-01

    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.

  10. 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.

  11. Evaluation of extracts from Coccoloba mollis using the Salmonella/microsome system and in vivo tests

    PubMed Central

    2010-01-01

    The common everyday use of medicinal plants is an ancient, and still very widespread practice, whereby the need for studies on their possible toxicity and mutagenic properties. The species Coccoloba mollis has been much used in phytotherapy, mainly in cases involving loss of memory and stress. In order to investigate its genotoxic and mutagenic potential, ethanolic extracts from the leaves and roots underwent Salmonella/microsome assaying (TA98 and TA100 strains, with and without exogenous metabolism – S9), besides comet and micronucleus tests in vivo.There was no significant increase in the number of revertants/plate of Salmonella strains in any of the analyzed root-extract concentrations, although the extract itself was extremely toxic to the Salmonella TA98 strain in the tests carried out with S9 (doses varying from 0.005 to 0.5 μg/plate). On the other hand, the leaf-extract induced mutations in the TA98 strain in the absence of S9 in the highest concentration evaluated, although at very low mutagenic potency (0.004 rev/ μg). Furthermore, there was no statistically significant increase in the number of comets and micronuclei, in treatments involving Swiss mice. It was obvious that extracts of Coccoloba mollis, under the described experimental conditions, are not mutagenic. PMID:21637430

  12. Test Plan for Solvent Extraction Data Acquisition to Support Modeling Efforts

    SciTech Connect

    Veronica Rutledge; Kristi Christensen; Troy Garn; Jack Law

    2010-12-01

    This testing will support NEAMS SafeSep Modeling efforts related to droplet simulation in liquid-liquid extraction equipment. Physical characteristic determinations will be completed for the fluids being used in the experiment including viscosity, density, surface tension, distribution coefficients, and diffusion coefficients. Then, experiments will be carried out to provide data for comparison to the simulation’s calculation of mass transfer coefficients. Experiments will be conducted with solutions used in the TRansUranic EXtraction (TRUEX) process extraction section. The TRUEX process was chosen since it is one solvent extraction system currently proposed for the separation of actinides and lanthanides from used nuclear fuel, it is diffusion limited, testing can be performed using non radioactive lanthanides to evaluate mass transfer. The extraction section involves transfer of one or more lanthanide species from an aqueous solution to an organic solvent. Single droplets rising by buoyancy will be studied first. Droplet size and number of species transferred will be varied independently to provide mass transfer coefficients as a function of each variable. An apparatus has been designed specifically for these experiments. In order to get more accurate measurements of droplet size, contact time, time of droplet formation, and possibly droplet breakup and coalescence, a high speed camera will be utilized for these experiments. Other potential experiments include examining the effects of jetted droplets and shear flow on the mass transfer coefficients.

  13. Human skin safety test of green tea cell extracts in condition of allergic contact dermatitis.

    PubMed

    Kim, Hyun Kyu; Choi, Sun Young; Chang, Hui Kyoung; Baek, Seok Yun; Chung, Jin Oh; Rha, Chan Su; Kim, Beom Joon; Kim, Myeung Nam

    2012-06-01

    Various kinds of positive effects of green tea extracts had been studied for long time which included anti-inflammation, anti-aging, and cardiometabolic effects. Although topical steroid and non-steroidal calcineurin inhibitors may control clinical symptoms of allergic contact dermatitis, some of patients also present allergic reaction to these topical agents. Therefore, we have tried green tea extracts for managing this skin disorder with expectation of anti-inflammatory effect without potential side effects including skin irritation and toxic responses. The toxicity test of green tea extract also did not show any sign of irritation in the skin throughout the test period. Moderate severity of allergic contact dermatitis presented satisfactory clinical outcome at second week follow-up which was final visit of outpatient. This result mean that green tea extract has a positive effect for managing allergic contact dermatitis but its potency and efficacy seem to be so not strong enough to control moderate severity allergy skin lesion. In this pilot study, we were able to conclude that green tea cell extracts might be applied for potential anti-inflammatory soaking without skin toxicity.

  14. 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

  15. 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.

  16. Appraisal of skin tests with food extracts for diagnosis of food hypersensitivity.

    PubMed

    Bock, S A; Lee, W Y; Remigio, L; Holst, A; May, C D

    1978-11-01

    Seventy-six children aged 5 months to 15 years who exhibited a net weal of 3.0 mm or greater to a puncture skin test with one or more of fourteen foods were subjected to double-blind food challenge. Confirmed reactions to double-blind food challenge were found to occur only with peanut, milk, egg and soybean. Puncture skin tests with 1:20 w/v concentration of food extracts identified all subjects who exhibited an adverse reaction during the double-blind food challenge. Performance of intradermal skin tests did not identify any additional subjects who reacted clinically to double-blind food challenge.

  17. [Preparative isolation and purification of cinnamoyl-C-glycoside chromone from aloe vera by high-speed countercurrent chromatography].

    PubMed

    Pan, Xia; Cao, Xueli; Dong, Yinmao; Zhao, Hua

    2005-01-01

    Aloe chromone is a group of anti-inflammatory and anti-tyrosinase constituents found in aloe vera leaves. High-speed countercurrent chromatography (HSCCC) is reported for the preparative isolation and purification of a chromone from aloe vera. The crude extract was obtained by a series of pretreatment of aloe vera leaves and extracted from decolorizing active carbon with methanol. Then the extract was distributed between dichloromethane and water, and the organic part was then subjected to HSCCC for the isolation of chromone constituents. The chromone compounds with a high performance liquid chromatographic grade (>95%) was isolated through two step HSCCC separations by employing two solvent systems composed of chloroform-methanol-water and dichloromethane-methanol-water at volume ratios of 4/3/2 and 5/4/2, respectively. The chromone was finally identified as cinnamoyl-C-glycoside chromone by ultraviolet (UV), fast atom bombardment mass spectrometry (FAB-MS), nuclear magnetic resonance (1H NMR and 13C NMR).

  18. Micron-scale laser-wire scanner for the KEK Accelerator Test Facility extraction line

    NASA Astrophysics Data System (ADS)

    Boogert, Stewart T.; Blair, Grahame A.; Boorman, Gary; Bosco, Alessio; Deacon, Lawrence C.; Karataev, Pavel; Aryshev, Alexander; Fukuda, Masafumi; Terunuma, Nobihiro; Urakawa, Junji; Corner, Laura; Delerue, Nicolas; Foster, Brian; Howell, David; Newman, Myriam; Senanayake, Rohan; Walczak, Roman; Ganaway, Fred

    2010-12-01

    A laser-wire transverse electron beam size measurement system has been constructed and operated at the Accelerator Test Facility (ATF) extraction line at KEK. The construction of the system is described in detail along with the environment of the ATF related to the laser wire. A special set of electron beam optics was developed to generate an approximately 1μm vertical focus at the laser-wire location. The results of our operation at the ATF extraction line are presented, where a minimum rms electron beam size of 4.8±0.3μm was measured, and smaller electron beam sizes can be measured by developing the method further. The beam size at the laser-wire location was changed using quadrupoles and the resulting electron beam size measured, and vertical emittance extracted.

  19. Solvent-extraction studies of coprocessing flowsheets: results from campaigns 1 and 2 of the Solvent-Extraction Test Facility (SETF)

    SciTech Connect

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

    1982-07-01

    The Solvent Extraction Test Facility (SETF) was installed in one of the heavily shielded cells of the Transuranium Processing Plant during 1978. This facility contains dissolution, feed preparation, solvent extraction (three 16-stage mixer-settlers), and plutonium product handling equipment, as well as waste solution tanks. Irradiated fuel from the H.B. Robinson-2 Pressurized Water Reactor was processed in the first two campaigns of experimental work, which were completed in 1979. The objective was to test a variety of coprocessing flowsheets. Areas of the solvent extraction process that received special attention included (1) crud formation, particularly in the extraction contactor; (2) uranium and plutonium losses in the extraction raffinate; (3) fission product decontamination; (4) reduction of tetravalent plutonium, particularly by means of hydroxylamine nitrate or nitrous acid; (5) costripping of uranium and plutonium; (6) partial partitioning; and (7) solvent degradation.

  20. 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.

  1. 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.

  2. Performance optimization of continuous countercurrent tangential chromatography for antibody capture.

    PubMed

    Dutta, Amit K; Tan, Jasmine; Napadensky, Boris; Zydney, Andrew L; Shinkazh, Oleg

    2016-03-01

    Recent studies have demonstrated that continuous countercurrent tangential chromatography (CCTC) can effectively purify monoclonal antibodies from clarified cell culture fluid. CCTC has the potential to overcome many of the limitations of conventional packed bed protein A chromatography. This paper explores the optimization of CCTC in terms of product yield, impurity removal, overall productivity, and buffer usage. Modeling was based on data from bench-scale process development and CCTC experiments for protein A capture of two clarified Chinese Hamster Ovary cell culture feedstocks containing monoclonal antibodies provided by industrial partners. The impact of resin binding capacity and kinetics, as well as staging strategy and buffer recycling, was assessed. It was found that optimal staging in the binding step provides better yield and increases overall system productivity by 8-16%. Utilization of higher number of stages in the wash and elution steps can lead to significant decreases in buffer usage (∼40% reduction) as well as increased removal of impurities (∼2 log greater removal). Further reductions in buffer usage can be obtained by recycling of buffer in the wash and regeneration steps (∼35%). Preliminary results with smaller particle size resins show that the productivity of the CCTC system can be increased by 2.5-fold up to 190 g of mAb/L of resin/hr due to the reduction in mass transfer limitations in the binding step. These results provide a solid framework for designing and optimizing CCTC technology for capture applications. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:430-439, 2016. PMID:26914276

  3. 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.

  4. TNX Area Phase II Soil Vapor Extraction Test Treatability Study Report

    SciTech Connect

    Noonkester, Jay

    2000-11-01

    The Savannah River Technology Center (SRTC), at the Savannah River Site (SRS), operates a pilot scale testing facility in the TNX Area. Research conducted in the TNX Area generated wastewater that was disposed of in earthen basins until 1988. As a result of these operations, shallow groundwater and sediments beneath the TNX Area are contaminated with both dissolved and residual chlorinated volatile organic compounds (CVOCs) such as trichloroethylene (TCE), carbon tetrachloride, and perchloroethylene (PCE). In 1996, the SRS initiated an Interim Remedial Action to capture and contain the dissolved contamination that was greater that 500 {micro}g/L TCE (WSRC, 1999). The Interim Remedial Action included the installation of a recovery well network and air stripper, and a vertical recirculation well. The objective of the recovery well network and air stripper is to provide hydraulic containment of the contaminated groundwater and provide a mechanism for the treatment of purge water generated during monitoring of the Interim Remedial Action. A vertical recirculation well, TVR1A, was installed to test the in-well vapor stripping (IVS) technology. Results from the test indicated that the IVS technology was not effective in the TNX Area. A single well soil vapor extraction test was conducted during June of 1997 using well TVR1A and the existing vacuum extraction unit that was installed for the in-well vapor stripping test. The objective of the SVE test at TNX was to collect preliminary information for the design of a SVE system to remediate residual CVOCs in the sediments.

  5. Liquid-liquid/solid three-phase high-speed counter-current chromatography, a new technique for separation of polyphenols from Geranium wilfordii Maxim.

    PubMed

    Liu, Dan; Ma, Yan; Gu, Ming; Janson, Jan-Christer; Wang, Changhai; Xiao, Hongbin

    2012-08-01

    High-speed counter-current chromatography using a new liquid-liquid/solid three-phase system was used for the separation of the polyphenols corilagin and geraniin from a crude extract of Geranium wilfordii Maxim in one step. The optimized three-phase system was composed of n-hexane/ethyl acetate/methanol/acetic acid/water and to which was added 10-μm average diameter microspheres of cross-linked 12% agarose at the ratio of 0.2:10:2:1:5 and 0.1 g/mL, respectively. The purities of geraniin and corilagin were 82 and 90%, which were determined by HPLC at 280 nm. A 14.5 and 7 mg of geraniin and corilagin were purified from 160 mg crude extract with the yields of 70 and 78%, respectively.

  6. Ultrafiltration liquid chromatography combined with high-speed countercurrent chromatography for screening and isolating potential α-glucosidase and xanthine oxidase inhibitors from Cortex Phellodendri.

    PubMed

    Li, Sainan; Liu, Chunming; Guo, Liping; Zhang, Yuchi; Wang, Jing; Ma, Bing; Wang, Yueqi; Wang, Yumeng; Ren, Junqi; Yang, Xiaojing; Qin, Yao; Tang, Ying

    2014-09-01

    Cortex Phellodendri is a typical Chinese herb with a large number of alkaloids existing in all parts of it. The most common methods for screening and isolating alkaloids are mostly labor intensive and time consuming. In this study, a new assay based upon ultrafiltration liquid chromatography was developed for the rapid screening of ligands for α-glucosidase and xanthine oxidase. The C. Phellodendri extract was found to contain two alkaloids with both α-glucosidase- and xanthine oxidase binding activities and one lactone with α-glucosidase-binding activity. Subsequently, with the help of high-speed countercurrent chromatography, the specific binding ligands including palmatine, berberine, and obaculactone with purities of 97.38, 96.12, and 96.08%, respectively, were successfully separated. An optimized low-toxicity two-phase solvent system composed of ethyl acetate/n-butanol/ethanol/water (3.5:1.7:0.5:5, v/v/v/v) was used to isolate the three compounds mentioned above from C. Phellodendri. The targeted compounds were identified by liquid chromatography coupled with mass spectrometry and NMR spectroscopy. Therefore, ultrafiltration liquid chromatography combined with high-speed countercurrent chromatography is not only a powerful tool for screening and isolating α-glucosidase and xanthine oxidase inhibitors in complex samples but is also a useful platform for discovering bioactive compounds for the prevention and treatment of diabetes mellitus and gout.

  7. Assay of mutagens in aqueous fecal extracts with a modified ames Salmonella test.

    PubMed

    Shaw, R; Andrews, A W; Riggs, C W

    1985-01-01

    Mutagenicity with Salmonella strain TA 100 can be determined by an island test in which only an isolated portion of a pour plate is spotted with a sample. The magnitude of the ratio of the numbers of revertant colonies on the treated and untreated parts of the plate reflects the potency of the mutagen. Five of six chemicals tested yielded statistically significant and generally linear dose-response curves. Minimum detectable mutagenic doses for four compounds calculated from the dose-response curves showed that the island test generally required less material for detection of mutagenicity than the liquid pre-incubation procedure. The island method was primarily designed to test the mutagenicity of aqueous extracts of human stool samples. Dose-responses were obtained for six such samples, and in two samples the amount of material needed for a positive response was significantly less than that required in the liquid pre-incubation method. PMID:2859658

  8. 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…

  9. Genotoxicity testing of Plantago major extracts in somatic cells of Drosophila melanogaster.

    PubMed

    Pimenta, Vânia Maria Sartini Dutra; Nepomuceno, Júlio César

    2005-01-01

    Plantago major is used in many parts of the world for the treatment of diseases and to promote the healing of wounds. In the present study, the somatic mutation and recombination test (SMART) in Drosophila melanogaster was used to evaluate the genotoxic activity of an aqueous extract of P. major. The following Drosophila crosses were made: standard (ST) cross, in which virgin flare females (flr3/TM3, Bds) were mated with mwh/mwh males, and high-bioactivation (HB) cross, in which virgin ORR females (ORR/ORR; flr3/TM3, Bds) were mated with mwh/mwh males. Each cross produced two types of descendents, marker-transheterozygous (MH) (mwh +/+ flr3) and balancer-heterozygous (BH) (mwh +/+ TM3, Bds) flies. Three-day-old larvae of both types of descendents were treated with undiluted and diluted (1:1 and 1:2 in water) aqueous extracts of P. major. The extracts were genotoxic in both crosses, producing similar induced frequencies in ST and HB flies. Comparison of the frequencies of wing spots in the BH and MH descendents indicated that recombination was a major response. The results indicate that, under these experimental conditions, aqueous extracts of P. major are genotoxic (recombinagenic).

  10. Genotoxicity testing of Plantago major extracts in somatic cells of Drosophila melanogaster.

    PubMed

    Pimenta, Vânia Maria Sartini Dutra; Nepomuceno, Júlio César

    2005-01-01

    Plantago major is used in many parts of the world for the treatment of diseases and to promote the healing of wounds. In the present study, the somatic mutation and recombination test (SMART) in Drosophila melanogaster was used to evaluate the genotoxic activity of an aqueous extract of P. major. The following Drosophila crosses were made: standard (ST) cross, in which virgin flare females (flr3/TM3, Bds) were mated with mwh/mwh males, and high-bioactivation (HB) cross, in which virgin ORR females (ORR/ORR; flr3/TM3, Bds) were mated with mwh/mwh males. Each cross produced two types of descendents, marker-transheterozygous (MH) (mwh +/+ flr3) and balancer-heterozygous (BH) (mwh +/+ TM3, Bds) flies. Three-day-old larvae of both types of descendents were treated with undiluted and diluted (1:1 and 1:2 in water) aqueous extracts of P. major. The extracts were genotoxic in both crosses, producing similar induced frequencies in ST and HB flies. Comparison of the frequencies of wing spots in the BH and MH descendents indicated that recombination was a major response. The results indicate that, under these experimental conditions, aqueous extracts of P. major are genotoxic (recombinagenic). PMID:15612001

  11. 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.

  12. [Preparative isolation and purification of the active components from Viticis Fructus by high-speed counter-current chromatography].

    PubMed

    Guan, Renjun; Wang, Daijie; Yu, Zongyuan; Wang, Xiao; Lan, Tianfeng

    2010-11-01

    Vitex trifolia L. var. simplicifolia Cham. is widely distributed in Asia, and its fruits are used as a folk medicine for headaches, colds, migraine, eyepain, etc. In order to effectively separate high-purity active components from the seeds of Vitex trifolia L. var. simplicifolia Cham., a high-speed counter-current chromatography (HSCCC) procedure was performed to separate four components from the crude extract of the fruits. A two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water (3:6: 3.6: 3, v/v/v/ v) was used. Within 230 min, 23 mg of 4-hydroxybenzoic acid, 15 mg of 3,6,7-trimethylquercetagetin, 24 mg of casticin and 5 mg of artemetin were obtained from 250 mg of the crude extract of Viticis Fructus in one-step elution under the conditions of a flow rate of 1.5 mL/min, 800 r/min and the detection wavelength of 254 nm. The purities of the four fractions were 93.1%, 97.3%, 98.7% and 98.5%, respectively. The obtained fractions were analyzed by high performance liquid chromatography (HPLC), and identified by electrospray ionization mass spectrometry (ESI-MS), 1H-nuclear magnetic resonance (NMR) and 13C-NMR. The results indicate that HSCCC is a powerful technique for the purification of active components from Viticis Fructus.

  13. Application of preparative high-speed counter-current chromatography for separation and purification of arctiin from Fructus Arctii.

    PubMed

    Wang, Xiao; Li, Fuwei; Sun, Qinglei; Yuan, Jingpeng; Jiang, Ting; Zheng, Chengchao

    2005-01-21

    Following an initial clean-up step on the AB-8 resin (polystyrene resin, 0.3-1.25 mm: NanKai Chemical Factory, Tianjin, China), high-speed counter-current chromatography (HSCCC) was used to purify an arctiin from an extract of the fruits of the Arctium lappa L. Arctiin is a major lignan compound in the traditional Chinese medicinal herb A. lappa L. The two-phase solvent system used was composed of ethyl acetate-n-butanol-ethanol-water at an optimized volume ratio of 5:0.5:1:5 (v/v/v/v). The upper phase was used as the mobile phase in the head to tail elution mode. A total amount of 159 mg of arctiin at 98% purity was obtained from 350 mg of the crude extract (containing 49% arctiin) with 91% recovery. The preparative isolation and purification of arctiin by HSCCC was completed in 5 h in a separation. Identification of the target compound was performed by LC-electrospray ionization MS and 13C-NMR. The structure of the product was further confirmed by comparison with authentic sample (National Institute of the Control of Pharmaceutical and Biological Products, Beijing, China).

  14. [Isolation and preparation of gallic acid from Terminalia chebula Retz. with high-speed counter-current chromatography].

    PubMed

    Li, Zhongqin; Li, Qiuyun; Jiang, Xinglong; Zhang, Kun; Guan, Ruizhang

    2014-12-01

    A separation method based on high-speed counter-current chromatography (HSCCC) has been established for the isolation and preparation of gallic acid from the ethanol extract of Terminalia chebula Retz. After comparing five kinds of solvent protocols of HSCCC, the two-phase system of n-hexane-ethyl acetate-methanol-water (1:5:1:5, v/v/v/v) was finally chosen as the operating solvent of HSCCC for the separation of gallic acid, in which the lower phase was used as the mobile phase and the upper phase as stationary phase. The detection in the experiments was performed with an ultraviolet detector at 254 nm. Under the conditions of rotation speed of 850 r/min, lower phase flow rate of 2 mL/min, four peaks (I/II/III/IV) were displayed on HSCCC chromatogram. Among them, only peak III contained a large amount of gallic acid (about 96. 40%), which was confirmed by electrospray ionization mass spectrometry (ESI-MS) and high performance liquid chromatographic (HPLC) analysis. As much as 8. 6 mg of gallic acid was obtained from 100 mg of the ethanol extract of Terminalia chebula Retz., indicating the method is simple, robust and efficient for the preparation of gallic acid.

  15. Preparative separation of alkaloids from Picrasma quassioides (D. Don) Benn. by conventional and pH-zone-refining countercurrent chromatography.

    PubMed

    Zhang, Qinghai; Shu, Xikai; Jing, Feng; Wang, Xiao; Lin, Changhu; Luo, Aiqin

    2014-06-25

    Two high-speed countercurrent chromatography (HSCCC) modes were compared by separation of major alkaloids from crude extract of Picrasma quassioides. The conventional HSCCC separation was performed with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (5:5:4.5:5.5, v/v/v/v) with 200 mg loading. pH-Zone-refining CCC was performed with two-phase solvent system composed of petroleum ether-ethyl acetate-n-butanol-water (3:2:7:9, v/v/v/v) where triethylamine (10 mM) was added to the upper organic stationary phase and hydrochloric acid (5 mM) was added to the lower aqueous phase with 2 g loading. From 2 g of crude extract, 87 mg of 5-methoxycanthin-6-one (a), 38 mg of 1-methoxy-β-carboline (b), 134 mg of 1-ethyl-4,8-dimethoxy-β-carboline (c), 74 mg of 1-ethoxycarbonyl-β-carboline (d), 56 mg of 1-vinyl-4,8-dimethoxy-β-carboline (e) and 26 mg of 1-vinyl-4-dimethoxy-β-carboline (f) were obtained with purities of over 97.0%. The results indicated that pH-zone-refining CCC is an excellent separations tool at the multigram level.

  16. Large-scale separation of alkaloids from Corydalis bungeana Turcz. by pH-zone-refining counter-current chromatography.

    PubMed

    Wang, Xiao; Dong, Hongjing; Shu, Xikai; Zheng, Zhenjia; Yang, Bin; Huang, Luqi

    2012-12-17

    pH-Zone-refining counter-current chromatography (pH-zone-refining CCC) was successfully applied for the large-scale separation of alkaloids from Corydalis bungeana. The crude extract was separated by a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (5:5:2:8, v/v) 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 a displacer. As a result, 285 mg of protopine, 86 mg of corynoloxine, 430 mg of coryno1ine, and 115 mg of acetylcorynoline were obtained from 3.0 g of crude extract in a one-step separation. The purities of these compounds were 99.1%, 98.3%, 99.0% and 98.5%, respectively, as determined by HPLC. The chemical structures of these isolated compounds were confirmed by ESI-MS, ¹H-NMR and ¹³C-NMR.

  17. High Speed Countercurrent Chromatography/Fourier Transform Infrared (HSCCC/FT-IR) Spectrometry

    NASA Astrophysics Data System (ADS)

    Romanach, Rodolfo J.; de Haseth, James A.

    1985-12-01

    High Speed Countercurrent Chromatography/Fourier transform infrared (HSCCC/FT-IR) spectrometry is present-ed. High solute-to-solvent ratios can be obtained in separations performed using HSCCC. At these high solute concentrations it is possible to obtain spectra of solutes without solvent elimination, even in the presence of polar solvents, such as water and methanol.

  18. Isolation of symlandine from the roots of common comfrey (Symphytum officinale) using countercurrent chromatography.

    PubMed

    Kim, N C; Oberlies, N H; Brine, D R; Handy, R W; Wani, M C; Wall, M E

    2001-02-01

    Three pyrrolizidine alkaloids, symlandine, symphytine, and echimidine (1-3), were isolated from the roots of Symphytum officinale using a one-step countercurrent chromatography procedure. The structures of 1-3 were confirmed by several spectroscopic techniques including 2D NMR methods. This is the first description of the separation of symlandine (1) from its stereoisomer, symphytine (2). PMID:11430014

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  20. Counter-current CO2 purification of partially deacylated sunflower oil

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  1. 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

    2013-09-01

    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. PMID:24010658

  2. 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.

  3. Development and validation of a standard test method for sequential batch extraction of waste with acidic extraction fluid

    SciTech Connect

    Sorini, S.S.

    1993-08-01

    Subject is characterization of waste materials. Since acid rain is increasingly prevalent throughout the world, a sequential batch extraction method was developed which uses a dilute acid solution as the extraction fluid. A collaborative study was conducted in which the draft method was used to treat a spray dryer waste from a clean coal technology process and a composite mining waste. Effects of filter pore size and digestion vs nondigestion on analytical concentrations in extracts were also studied. Elements determined included Al, Ba, B, Ca, Cr, Si, Na, Sr, Pb, Mg, Mn, Si, Zn. The draft method will be published as ASTM Method D5284-92.

  4. Co- and counter-current rotation in Tore Supra lower hybrid current drive plasmas

    NASA Astrophysics Data System (ADS)

    Chouli, B.; Fenzi, C.; Garbet, X.; Bourdelle, C.; Decker, J.; Aniel, T.; Artaud, J.-F.; Basiuk, V.; Clairet, F.; Colledani, G.; Dumont, R.; Elbeze, D.; Gil, C.; Lotte, P.; Sarazin, Y.; the Tore Supra Team

    2014-09-01

    Observations of lower hybrid (LH) radio frequency heating effects on toroidal plasma rotation in L-mode Tore Supra plasmas are reported. A database of more than 50 plasma discharges has been analysed. Core rotation is found to increment in co- or counter-current direction depending on the plasma current (Ip). At low plasma current, the induced rotation is up to +15 km s-1 in the co-current direction, the rotation profile being affected over the whole plasma minor radius. At higher plasma current, an opposite trend is observed, the core plasma rotation incrementing up to -15 km s-1 in the counter-current direction, the profile being affected up to r/a < 0.6 only. At the zero crossing point, which is defined when the plasma rotation profile is not affected by LH power injection, Ip ˜ 0.95 MA. In both low and high Ip cases, rotation increments are found to increase with the injected power. Several mechanisms in competition which can induce co- or counter-current rotation in Tore Supra LHCD plasmas are investigated and typical order of magnitude are discussed. How those effects evolve with plasma parameters and how they compete are important issues addressed in this paper. Rotation increment increase with Ip at fixed LH power is consistent with a dominant standard momentum confinement mechanism related to Ip increase. The co-current change in rotation is consistent with a fast electron ripple loss mechanism, while thermal ripple induced neoclassical friction and absorbed LH wave momentum from resonant electrons are expected to influence the rotation in the counter-current direction. Finally, the numerical simulations show that the radial turbulent momentum transport does impact the rotation behaviour inducing increment in co- or counter-current directions, depending on the plasma current amplitude.

  5. 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

  6. Model for analysis of counter-current gas transfer in fish gills.

    PubMed

    Scheid, P; Hook, C; Piiper, J

    1986-06-01

    The validity of previously used simplified models for the analysis of gas transfer in fish gills was tested using an integrated model which includes water flow and blood flow in counter-current arrangement. The model accounts for the resistance to diffusion of O2 both in the water-blood barrier and in the interlamellar water, which is assumed to flow with a parabolic velocity profile between the secondary lamellae. The O2 diffusing capacity (transfer factor) for this model (Dint) was compared to that (Dm + w) calculated from the diffusing capacity of the water-blood barrier (Dm), and from the effective diffusive conductance of the parabolically streaming interlamellar water (Dw) as 1/Dm + w = 1/Dm + 1/Dw. These diffusing capacities were compared with that (Dadd) calculated from Dm and diffusing capacity of a water layer of 1/4 thickness of the interlamellar space (Dw) as 1/Dadd = 1/Dm + 1/Dw. Calculations with morphometric and gas exchange parameters in the elasmobranch Scyliorhinus stellaris reveal the following features: (1) In physiological conditions, Dm + w and Dint are similar to within 10%, but Dint is always higher. (2) Dint and Dm + w increase with increasing ventilation; Dint increases with decreasing perfusion, while Dm + w remains constant. (3) Both Dint and Dm + w agree reasonably well with Dadd. In other anatomical and physiological conditions, particularly for relatively high Dm, Dw, and Dw and high ventilation, greater discrepancies between Dint and Dm + w may occur but Dm + w appears to represent a reasonable approximation of the effective O2 diffusing capacity, which is best modelled as Dint. PMID:3738259

  7. 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.

  8. 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.

  9. Tests of the extraction of the Sivers, Boer-Mulders, and transversity distributions in SIDIS reactions

    NASA Astrophysics Data System (ADS)

    Christova, Ekaterina; Leader, Elliot

    2015-12-01

    A major experimental program is presently underway worldwide to determine the fundamental nonperturbative functions, the Sivers, Boer-Mulders and transversity distributions, which are vital for an understanding of the internal structure of the nucleon. However, at present, many simplifying assumptions are used in extracting these functions from the data. We demonstrate that if the binning of the data in Q2 is small enough so that Q2 evolution can be neglected inside a bin, then one can obtain stringent tests of these assumptions. Failure to satisfy these tests implies that the presently extracted nonperturbative functions are unreliable. To this end, we consider the measurement of the Sivers, Boer-Mulders and transversity difference asymmetries for hadrons with opposite charges in SIDIS reactions with unpolarized and transversely polarized deuteron and proton targets: l +N →l'+h +X , h =π± , K± , h± . Utilizing only charge and isospin invariance, and applying the above mentioned simplifying assumptions, we obtain several testable relations amongst the measured asymmetries. If these tests are satisfied, then the measured asymmetries determine two different combinations of the valence-quark transverse-momentum-dependent distributions, which can be determined separately without any contributions from the strange and other sea quarks.

  10. 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

    2008-05-01

    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.

  11. Adsorbent materials development and testing for the extraction of uranium from seawater

    SciTech Connect

    Felker, L.K.; Dai, S.; Hay, B.P.; Janke, C.J.; Mayes, R.T.; Sun, X.; Tsouris, C.

    2013-07-01

    The extraction of uranium from seawater has been the focus of a research project for the U.S. Department of Energy to develop amidoxime functional group adsorbents using radiation-induced graphing on polymer-based fiber materials and subsequent chemical conversion of the radical sites to form the desired adsorbent material. Materials with promising uranium adsorption capacities were prepared through a series of parametric studies on radiation dose, time, temperature, graphing solutions, and properties of the base polymer materials. A laboratory screening protocol was developed to determine the uranium adsorption capacity to identify the most promising candidate materials for seawater testing. (authors)

  12. 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.

  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. Sorbent Testing for Solidification of Organic Plutonium/Uranium Extraction Waste - Phase IV

    SciTech Connect

    Bickford, J.L.; Joyce, H.O.; Holmes-Burns, H.

    2006-07-01

    The U.S. Department of Energy (DOE) is evaluating various sorbents to solidify and immobilize hazardous constituents of the organic fraction of plutonium/uranium extraction (PUREX) process waste at the Savannah River Site (SRS).[5] The purpose of the solidification is to provide a cost-effective alternative to incineration of the waste. Incineration at the Consolidated Incinerator Facility (CIF) at SRS is currently identified as the treatment technology for PUREX waste. However, the CIF is not in operation at this time, so SRS is interested in pursuing alternatives to incineration for treatment of this waste. The DOE Western Environmental Technology Office in Butte, MT was designated as the facility for conducting the sorbent testing and evaluation for the organic PUREX waste surrogate. MSE Technology Applications, Inc. tested and evaluated two clay and two polymer sorbents with the capability of solidifying organic PUREX waste. A surrogate organic PUREX waste recipe was utilized, and sorbents were tested and evaluated at bench-scale, 22-liter (5-gallon) scale, and 242-liter (55-gallon) scale. This paper presents experimental results evaluating four sorbent materials including: Imbiber Beads{sup TM} IMB230301-R, Nochar A610 Petrobond{sup TM}, Petroset II{sup TM}, and Petroset II Granular{sup TM}. Previous work at SRS indicated that these products could solidify organic PUREX waste on a bench scale [1]. The sorbents were evaluated using operational criteria and final wasteform properties. Operational criteria included: sorbent capacity; sorption rate; sorbent handling; and mixing requirements. Final wasteform evaluation properties included: ignitability; thermal stability; offgas generation, leachability tests and volumetric expansion. Bench-scale tests, 22-liter (5-gallon) tests, and initial 242-liter (55-gallon) tests are complete. This paper summarizes the results of the bench-scale, 22-liter (5-gallon) scale, and 242-liter (55-gallon) scale tests performed

  15. Program plan: Testing of vacuum extraction and in-situ air stripping technologies

    SciTech Connect

    Kaback, D.S.; Looney, B.B.

    1987-07-24

    Recent hydrological investigations at the Savannah River Plant (SRP) have shown that operation of the plant has resulted in contamination of the groundwater and the vadose zone in various locations across the plant. Volatile organic solvent (VOC) contamination has been observed at a number of locations across SRP. A remedial action program consisting of above-ground air stripping of groundwater is underway to address contamination in M Area. A recent pilot study to clean up the soils above the water table was completed in M Area (for location see Figure 1). A new technique, in-situ vacuum extraction, successfully removed significant quantities of trichloroethylene and tetrachloroethylene from the soils along a portion of the abandoned process-sewer line in M Area. The vacuum-extraction test was conducted for a period of three weeks. It is calculated that almost 1500 pounds of solvents were removed from the soils during the test. The radius of influence for the vacuum process is estimated to be greater than 75 feet. 5 figs.

  16. Target-guided separation of Bougainvillea glabra betacyanins by direct coupling of preparative ion-pair high-speed countercurrent chromatography and electrospray ionization mass-spectrometry.

    PubMed

    Jerz, Gerold; Wybraniec, Sławomir; Gebers, Nadine; Winterhalter, Peter

    2010-07-01

    In this study, preparative ion-pair high-speed countercurrent chromatography was directly coupled to an electrospray ionization mass-spectrometry device (IP-HSCCC/ESI-MS-MS) for target-guided fractionation of high molecular weight acyl-oligosaccharide linked betacyanins from purple bracts of Bougainvillea glabra (Nyctaginaceae). The direct identification of six principal acyl-oligosaccharide linked betacyanins in the mass range between m/z 859 and m/z 1359 was achieved by positive ESI-MS ionization and gave access to the genuine pigment profile already during the proceeding of the preparative separation. Inclusively, all MS/MS-fragmentation data were provided during the chromatographic run for a complete analysis of substitution pattern. On-line purity evaluation of the recovered fractions is of high value in target-guided screening procedures and for immediate decisions about suitable fractions used for further structural analysis. The applied preparative hyphenation was shown to be a versatile screening method for on-line monitoring of countercurrent chromatographic separations of polar crude pigment extracts and also traced some minor concentrated compounds. For the separation of 760mg crude pigment extract the biphasic solvent system tert.-butylmethylether/n-butanol/acetonitrile/water 2:2:1:5 (v/v/v/v) was used with addition of ion-pair forming reagent trifluoroacetic acid. The preparative HSCCC-eluate had to be modified by post-column addition of a make-up solvent stream containing formic acid to reduce ion-suppression caused by trifluoroacetic acid and later significantly maximized response of ESI-MS/MS detection of target substances. A variable low-pressure split-unit guided a micro-eluate to the ESI-MS-interface for sensitive and direct on-line detection, and the major volume of the effluent stream was directed to the fraction collector for preparative sample recovery. The applied make-up solvent mixture significantly improved smoothness of the continuously

  17. 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.

  18. 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. PMID:27608619

  19. 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.

  20. 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.

  1. 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. PMID:25069743

  2. 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. PMID:24220992

  3. 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%.

  4. 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.

  5. 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.

  6. Separation of four flavonoids from Rhodiola rosea by on-line combination of sample preparation and counter-current chromatography.

    PubMed

    Ma, Chaoyang; Hu, Liming; Fu, Qianyun; Gu, Xiaohong; Tao, Guanjun; Wang, Hongxin

    2013-09-01

    Purification of four flavonoids from Rhodiola rosea was developed by on-line combination of sample preparation and counter-current chromatography (CCC). Flavonoid sample was prepared by dynamic ultrasonic-assisted and solid-phase extraction using ion liquids as extractant. The preparation conditions were optimized by D-optimal design as follows: 2mol/L of 1-ethyl-3-methylimidazolium bromide concentration, 360W of ultrasonic power, 1.5mL/min of flow rate, 35min of extraction time and 0.5mL (absorbent) per g (material) of absorbent amount. The prepared sample solution (20mL) was loaded and injected directly into CCC column for final separation. As a result, four flavonoids, herbacetin-3-O-β-d-glucopyranosyl-7-O-α-l-rhamnopyranoside 1 (40.1mg), kaempferol-3-O-β-d-glucopyranosyl-7-O-α-l-rhamn-opyranoside 2 (4.6mg), kaempferol 3-O-β-d-glucopyranoside-(2→1)-β-d-xylopyranoside 3 (20.2mg) and herbacetin-8-O-β-d-glucopyranoside 4 (22.5mg), were obtained from 20g of R. rosea material using ethyl acetate-n-butanol-H2O as solvent system at a ratio of 4:1:5 by CCC. Their structures were identified by ESI-MS/MS, NMR methods. Their purities determined by UPLC were 98.5%, 95.4%, 98.1% and 97.5%, respectively. Kaempferol-3-O-β-d-glucopyranosyl-7-O-α-l-rhamnopyranoside 2 and herbacetin-8-O-β-d-glucopyrano-side 4 were isolated for first time from R. rosea. The purification method was simple, efficient and evaded tedious sample preparation process. PMID:23890556

  7. Preparative isolation and purification of two benzoxazinoid glucosides from Acanthus ilicifolius L. by high-speed counter-current chromatography.

    PubMed

    Yin, Hao; Zhang, Si; Luo, Xiongming; Liu, Yonghong

    2008-09-26

    The first preparative separation of two benzoxazinoids, (2R)-2-O-beta-d-glucopyranosyl-2H-1,4-benzoxazin-3(4H)-one (HBOA-Glc) and (2R)-2-O-beta-d-glucopyranosyl-4-hydroxy-2H-1,4-benzoxazin-3(4H)-one (DIBOA-Glc), by means of high-speed counter-current chromatography (HSCCC) from the n-butanol extract of Acanthus ilicifolius L. is presented. The two-phase solvent system containing ethyl acetate-n-butanol-0.5%NH(4)OH (2:3:5, v/v/v, system B) was selected for the one-step HSCCC separation of HBOA-Glc and DIBOA-Glc according to the partition coefficient values (K) for target compounds and the separation factor (alpha) between the two target compounds. In the one-step HSCCC separation using solvent B, from 100mg n-butanol extract of A. ilicifolius, 6.3 mg HBOA-Glc and 6.8 mg DIBOA-Glc were isolated with purities of 90.3% and 80.2%, respectively. In order to obtain the two target compounds with higher purity, a second separation process was developed comprising two steps. In the two-step separation, the sample was first pre-purified by HSCCC using ethyl acetate-n-butanol-water (2:3:5, v/v/v, system A) solvent system and then purified using solvent system B. A 100-mg amount of the n-butanol extracts of A. ilicifolius was separated to yield 5.8 mg of HBOA-Glc and 4.8 mg of DIBOA-Glc with purities of 97.1% and 94.8%, respectively, which were directly used for NMR analyses.

  8. 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.

  9. Leach and EP (extraction procedure) toxicity tests on grouted waste from Tank 106-AN

    SciTech Connect

    Serne, R.J.; Martin, W.J.; Lokken, R.O.; LeGore, V.L.; Lindenmeier, C.W.; Martin, P.F.C.

    1989-09-01

    Pacific Northwest Laboratory is conducting laboratory experiments to produce leach rate data for various waste species that will be contained in grout at Hanford. In the work reported here, grout made from Tank 106-AN liquid waste was used to produce empirical leach rate data for several radionuclides ({sup 60}Co, {sup 90}Sr, {99}Tc, {129}I, {137}Cs, and {sup 241}Am), stable major components (NO{sub 3}{sup {minus}}, NO{sub 2}{sup {minus}}, F, Cl, and Na), and trace metals (Cr, Mo, and Ni). Two types of tests were used to produce leach rate data: an intermittent replacement leach test (ANS 16.1 leach test) and a static leach test. Measured effective diffusivities of key species are as follows: 4 to 6 {times} 10{sup {minus}8} cm{sup 2}/sec for {sup 99}Tc, 3 to 7 {times} 10{sup {minus}8} cm{sup 2}/sec for {sup 129}I, 4 to 6 {times} 10{sup {minus}9} cm{sup 2}/sec for nitrate, and 6 to 7 {times} 10{sup {minus}9} cm{sup 2}/sec for nitrite. The leach indices of all species studied are above (more favorable than) the waste form criteria. The leach indices for {sup 99}Tc and {sup 129}I are 7.4 {plus minus} 1.2 and 7.6 {plus minus} 0.4, respectively, and are being further investigated in continuing studies of double-shell slurry feed grouts. An Extraction Procedure (EP) toxicity test was also conducted and the grouted water is considered nontoxic per this test protocol. 19 refs., 9 figs., 8 tabs.

  10. 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)

  11. Chiral ligand exchange countercurrent chromatography: Equilibrium model study on enantioseparation of mandelic acid.

    PubMed

    Tong, Shengqiang; Shen, Mangmang; Xiong, Qing; Wang, Xiaoping; Lu, Mengxia; Yan, Jizhong

    2016-05-20

    The equilibrium model in enantioseparation of mandelic acid by chiral ligand exchange countercurrent chromatography was investigated using N-n-dodecyl-l-proline as chiral ligand and cupric ion as central metal. Important parameters, including physical partition coefficient and formation constants of binary and ternary coordination complexes in the two-phase solvent system, were determined. This equilibrium model could give an excellent prediction of distribution ratio and enantioseparation factor of the analyte in the biphasic solvent system, which was further verified by experiments. All the average relative deviations were less than 12%, indicating that the established model could provide a simple computational approach for optimization of enantioseparation conditions in chiral ligand exchange countercurrent chromatography.

  12. 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%.

  13. 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%. PMID:25199445

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. Comparison of two extractable nuclear antigen testing algorithms: ALBIA versus ELISA/line immunoassay.

    PubMed

    Chandratilleke, Dinusha; Silvestrini, Roger; Culican, Sue; Campbell, David; Byth-Wilson, Karen; Swaminathan, Sanjay; Lin, Ming-Wei

    2016-08-01

    Extractable nuclear antigen (ENA) antibody testing is often requested in patients with suspected connective tissue diseases. Most laboratories in Australia use a two step process involving a high sensitivity screening assay followed by a high specificity confirmation test. Multiplexing technology with Addressable Laser Bead Immunoassay (e.g., FIDIS) offers simultaneous detection of multiple antibody specificities, allowing a single step screening and confirmation. We compared our current diagnostic laboratory testing algorithm [Organtec ELISA screen / Euroimmun line immunoassay (LIA) confirmation] and the FIDIS Connective Profile. A total of 529 samples (443 consecutive+86 known autoantibody positivity) were run through both algorithms, and 479 samples (90.5%) were concordant. The same autoantibody profile was detected in 100 samples (18.9%) and 379 were concordant negative samples (71.6%). The 50 discordant samples (9.5%) were subdivided into 'likely FIDIS or current method correct' or 'unresolved' based on ancillary data. 'Unresolved' samples (n = 25) were subclassified into 'potentially' versus 'potentially not' clinically significant based on the change to clinical interpretation. Only nine samples (1.7%) were deemed to be 'potentially clinically significant'. Overall, we found that the FIDIS Connective Profile ENA kit is non-inferior to the current ELISA screen/LIA characterisation. Reagent and capital costs may be limiting factors in using the FIDIS, but potential benefits include a single step analysis and simultaneous detection of dsDNA antibodies.

  19. 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. PMID:25342478

  20. 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. PMID:27036211

  1. 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.

  2. 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.

  3. 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.

  4. Continuing assessment of the 5 day sodium carbonate-ammonium nitrate extraction assay as an indicator test for silicon fertilizers

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  5. 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

  6. Preparative Separation of Main Ustilaginoidins from Rice False Smut Balls by High-Speed Counter-Current Chromatography.

    PubMed

    Sun, Weibo; Dong, Xuejiao; Xu, Dan; Meng, Jiajia; Fu, Xiaoxiang; Wang, Xiaohan; Lai, Daowan; Zhou, Ligang; Liu, Yang

    2016-01-12

    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.

  7. Aqueous CO{sup 2} vs. aqueous extraction of soils as a preparative procedure for acute toxicity testing

    SciTech Connect

    Yates, G.W.; Burks, S.L.

    1994-12-31

    This study was to determine if contaminated soils extracted with supercritical CO{sup 2} (SFE) would yield different results from soils extracted with an aqueous media. Soil samples from an abandoned oil refinery were subjected to aqueous and SFE extraction. Uncontaminated control sites were compared with contaminated sites. Each extract was analyzed for 48 hour acute Ceriodaphnia LC50s and Microtox{reg_sign} EC50s. Comparisons were then made between the aqueous extracts and the SFE extracts. An additional study was made with HPLC chromatographs of the SFE contaminated site extracts to determine if there was a correlation between LC50 results and peak area of different sections of the chromatograph. The 48 hour Ceriodaphnia LC50 of one contaminated site showed a significant increase in toxicity with the supercritical extract compared to the aqueous extract. All contaminated sites gave toxic responses with the supercritical procedure. The Microtox{reg_sign} assay showed a toxic response with 2 of the 3 contaminated sites for both aqueous and SFE extracts. Results indicate that the Ceriodaphnia assays were more sensitive than Microtox{reg_sign} to contaminants found in the refinery soil. SFE controls did not show adverse effects with the Ceriodaphnia, but did have a slight effect with Microtox{reg_sign}. The best correlation (r{sup 2} > 0.90) between the Ceriodaphnia LC50s and the peak areas of the chromatographs was obtained for sections with an estimated log K{sub ow} of 1 to 5. SFE extraction provided a fast, efficient and inexpensive method of collecting and testing moderately non-polar to strongly non-polar organic contaminants from contaminated soils.

  8. 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. PMID:17487597

  9. 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.

  10. Characterization and testing of amidoxime-based adsorbent materials to extract uranium from natural seawater

    DOE PAGESBeta

    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)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

  11. 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.

  12. 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

  13. 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. PMID:26903487

  14. Overlapping elution-extrusion counter-current chromatography: a novel method for efficient purification of natural cytotoxic andrographolides from Andrographis paniculata.

    PubMed

    Wu, Dingfang; Cao, Xiaoji; Wu, Shihua

    2012-02-01

    Counter-current chromatography (CCC) is extremely useful for the separation, purification, and isolation of natural products. Recently, Berthod et al. established an elution-extrusion CCC method in metabolic analysis by combining regular chromatographic elution with stationary-phase extrusion, which extends the hydrophobicity window of a counter-current separation. In this study, a novel overlapping elution-extrusion CCC method was developed and applied to the preparation of natural cytotoxic andrographolides from the aerial parts of Andrographis paniculata, a well-known Traditional Chinese Medicine (TCM) with potent anti-inflammatory effect and anti-cancer activity. Its theory was first developed, and then a series of CCC experiments were performed to investigate the efficiency of the method in the separation of the ethanol extracts from A. paniculata. Results show that overlapping elution-extrusion CCC is an efficient method to prepare a cytotoxic natural diterpenoid combination of 14-deoxy-andrographolide and 14-deoxy-11,12-didehydroandrographolide with the molar ratio of 1:2 as well as andrographolide using an optimized solvent system composed of hexane-ethyl acetate-ethanol-water (5:5:4:6, v/v) with an on-demand solvent preparation mode. All components obtained showed potent cytotoxic activity against human hepatocellular liver carcinoma cells HepG2 and doxorubicin-resistant R-HepG2 cells. Molecular structures have been identified by electrospray ionization mass spectrometry (ESI-MS), electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS), one- and two-dimensional nuclear magnetic resonance (1D- and 2D-NMR). The method appears to be very useful for the high-throughput purification of natural products.

  15. 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.

  16. 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.

  17. 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. PMID:25722166

  18. Sister chromatid exchange test in river buffalo lymphocytes treated in vitro with furocoumarin extracts.

    PubMed

    Iannuzzi, Alessandra; Perucatti, Angela; Genualdo, Viviana; Pauciullo, Alfredo; Melis, Rita; Porqueddu, Claudio; Marchetti, Mauro; Usai, Marianna; Iannuzzi, Leopoldo

    2016-09-01

    Furocoumarin extracts from Psoralea morisiana, the endemic Sardinian legume species, were tested for their mutagenic potential on river buffalo blood cells. The results obtained performing the sister chromatid exchange (SCE) test in blood cultures of five river buffalo calves (exposure to furocoumarins for 72h) and five cows (exposure to furocoumarins for 3h, in the absence and presence of S9 metabolic activator) are reported. Significant differences in mean values of SCEs were observed in cells of calves compared to control cells (unexposed), but no differences in SCE mean values were found between treated and untreated cells of cows in the presence or absence of S9. SCE mean values were much higher in cells of cows (exposed and control) than in cells of calves. Indeed, in calf cells, SCE mean values/cell (±SD) were 6.66±2.45 in the control and 7.63±3.01, 9.03±3.90, 9.53±3.60 and 9.99±3.41 in treated cells at 50, 100, 200 and 400 µg/ml of furocoumarin extracts, respectively. In cow cells, grown in presence of S9, SCE mean values/cell were 11.49±4.78 and 11.65±5.19 in treated cells at 100 and 200 µg/ml of furocoumarins and 11.66±5.45 in the control. In cow cells grown in absence of S9, SCE mean values were 11.81±6.14 in the control and 12.35±7.09 and 12.01±5.43, respectively, in the presence of 100 and 200 µg/ml of furocoumarins. Despite their higher SCE values in the absence of S9, no statistically significant differences were found when these values were compared with those shown in presence of S9, suggesting no mutagenic action of furocoumarins in cows, at the doses used in this study. PMID:27180332

  19. Solvent systems for countercurrent chromatography: an aqueous two phase liquid system based on a room temperature ionic liquid.

    PubMed

    Ruiz-Angel, Maria Jose; Pino, Veronica; Carda-Broch, Samuel; Berthod, Alain

    2007-06-01

    A new aqueous two phase liquid system (ATPS) based on the ionic liquid 1-butyl-3-methyl imidazolium chloride (BMIM Cl), potassium dibasic phosphate (K(2)HPO(4)) and water was recently proposed in the literature. The full phase diagram of this ATPS was prepared and some tie lines were fully determined. It was compared to classical ATPSs based on polyethylene glycol with an average molecular mass of 1000 (PEG 1000) and 10,000 (PEG 10000) and K(2)HPO(4). Two countercurrent chromatography (CCC) columns, a hydrostatic Sanki and a J type hydrodynamic CCC columns were used to test the liquid phase retention of these ATPSs in all possible configurations. It was found that the BMIM Cl ATPS liquid phases were much easier to retain in the two CCC columns than the PEG 1000 ATPS phases. Using protein and alcohol solutes, it was established that the BMIM Cl ATPS has a polarity completely different from that of the PEG 1000 ATPS. For example, ovalbumin partitions equally between the two phases of the PEG 1000 ATPS (K(D)=1.4) when it is completely located in the BMIM Cl upper phase of the ionic liquid ATPS (K(D)=180). The discrimination factor of the ionic liquid system and its intrinsic hydrophobicity were respectively found three times higher and ten times lower than the respective values of the PEG 1000 ATPS. PMID:17166506

  20. 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.

  1. The effects of surface tension on flooding in counter-current two-phase flow in an inclined tube

    SciTech Connect

    Deendarlianto; Ousaka, Akiharu; Indarto; Kariyasaki, Akira; Lucas, Dirk; Vallee, Christophe; Vierow, Karen; Hogan, Kevin

    2010-10-15

    The purpose of the present study is to investigate the effects of surface tension on flooding phenomena in counter-current two-phase flow in an inclined tube. Previous studies by other researchers have shown that surface tension has a stabilizing effect on the falling liquid film under certain conditions and a destabilizing or unclear trend under other conditions. Experimental results are reported herein for air-water systems in which a surfactant has been added to vary the liquid surface tension without altering other liquid properties. The flooding section is a tube of 16 mm in inner diameter and 1.1 m length, inclined at 30-60 from horizontal. The flooding mechanisms were observed by using two high-speed video cameras and by measuring the time variation of liquid hold-up along the test tube. The results show that effects of surface tension are significant. The gas velocity needed to induce flooding is lower for a lower surface tension. There was no upward motion of the air-water interfacial waves upon flooding occurrence, even for lower a surface tension. Observations on the liquid film behavior after flooding occurred suggest that the entrainment of liquid droplets plays an important role in the upward transport of liquid. Finally, an empirical correlation for flooding velocities is proposed that includes functional dependencies on surface tension and tube inclination. (author)

  2. 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.

  3. 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)

  4. 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.

  5. 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

  6. 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.

  7. Post-extraction stabilization of HIV viral RNA for quantitative molecular tests.

    PubMed

    Stevens, Daniel S; Crudder, Christopher H; Domingo, Gonzalo J

    2012-06-01

    Two approaches to stabilize viral nucleic acid in processed clinical specimens were evaluated. HIV-1 RNA extracted from clinical specimens was stabilized in a dry matrix in a commercial product (RNAstable, Biomatrica, San Diego, CA, USA) and in a reverse-transcription reaction mixture in liquid form as cDNA. As few as 145 HIV-1 genome copies of viral RNA are reliably stabilized by RNAstable at 45°C for 92 days and in the cDNA format at 45°C for 7 days as determined by real-time PCR. With RNAstable the R(2) at days 1, 7, and 92 were 0.888, 0.871, and 0.943 when compared to baseline viral load values. The cDNA generated from the same clinical specimens was highly stable with an R(2) value of 0.762 when comparing viral load determinations at day 7 to baseline values. In conclusion viral RNA stabilized in a dry RNAstable matrix is highly stable for long periods of time at high temperatures across a substantial dynamic range. Viral RNA signal can also be stabilized in liquid in the form of cDNA for limited periods of time. Methods that reduce reliance on the cold chain and preserve specimen integrity are critical for extending the reach of molecular testing to low-resource settings. Products based on anhydrobiosis, such as the RNAstable should be evaluated further to support viral pathogen diagnosis. PMID:22433512

  8. Bioaccessibility of metals in dust from the indoor environment: application of a physiologically based extraction test.

    PubMed

    Turner, Andrew; Ip, Ka-Hei

    2007-11-15

    A physiologically based extraction test, simulating sequential digestion in the stomach and intestine, has been applied to dust samples collected from various domestic and working settings to define bioaccessible concentrations of metals (Al, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sn, U, Zn) in the indoor environment. With the exception of Ca, Cd, and Zn in the stomach phase, mean bioaccessibilities (relative to respective total metal concentrations) were less than 50%. For a given metal, bioaccessibility in either phase was variable among samples but, in many cases, displayed an inverse dependence on total concentration. This suggests that, to a good approximation, variations in both metal contamination and accessibility in the indoor environment arise from variable proportions of metal-rich particulates of low digestibility. Compared with accessibility in the stomach, accessibility in the more alkaline, carbonate-rich intestine was either lower (Al, Ca, Cd, Mn, Ni, Sn, Pb, Zn), similar (Co, Cu, Fe) or greater (Cr, U). We attribute these observations to precipitation and/or readsorption in the intestine, stabilization by complexation, or anion-like adsorption of negatively charged, polyatomic species, respectively.

  9. Stability Test and Quantitative and Qualitative Analyses of the Amino Acids in Pharmacopuncture Extracted from Scolopendra subspinipes mutilans

    PubMed Central

    Cho, GyeYoon; Han, KyuChul; Yoon, JinYoung

    2015-01-01

    Objectives: Scolopendra subspinipes mutilans (S. subspinipes mutilans) is known as a traditional medicine and includes various amino acids, peptides and proteins. The amino acids in the pharmacopuncture extracted from S. subspinipes mutilans by using derivatization methods were analyzed quantitatively and qualitatively by using high performance liquid chromatography (HPLC) over a 12 month period to confirm its stability. Methods: Amino acids of pharmacopuncture extracted from S. subspinipes mutilans were derived by using O-phthaldialdehyde (OPA) & 9-fluorenyl methoxy carbonyl chloride (FMOC) reagent and were analyzed using HPLC. The amino acids were detected by using a diode array detector (DAD) and a fluorescence detector (FLD) to compare a mixed amino acid standard (STD) to the pharmacopuncture from centipedes. The stability tests on the pharmacopuncture from centipedes were done using HPLC for three conditions: a room temperature test chamber, an acceleration test chamber, and a cold test chamber. Results: The pharmacopuncture from centipedes was prepared by using the method of the Korean Pharmacopuncture Institute (KPI) and through quantitative analyses was shown to contain 9 amino acids of the 16 amino acids in the mixed amino acid STD. The amounts of the amino acids in the pharmacopuncture from centipedes were 34.37 ppm of aspartate, 123.72 ppm of arginine, 170.63 ppm of alanine, 59.55 ppm of leucine and 57 ppm of lysine. The relative standard deviation (RSD %) results for the pharmacopuncture from centipedes had a maximum value of 14.95% and minimum value of 1.795% on the room temperature test chamber, the acceleration test chamber and the cold test chamber stability tests. Conclusion: Stability tests on and quantitative and qualitative analyses of the amino acids in the pharmacopuncture extracted from centipedes by using derivatization methods were performed by using HPLC. Through research, we hope to determine the relationship between time and the

  10. [Genotoxic effects of pesticide-treated vegetable extracts using the Allium cepa chromosome aberration and micronucleus tests].

    PubMed

    Biscardi, D; De Fusco, R; Feretti, D; Zerbini, I; Izzo, C; Esposito, V; Nardi, G; Monarca, S

    2003-01-01

    The presence of chemical residues in vegetables and fruit is a source of human exposure to toxic and genotoxic chemicals. The mutagenic and carcinogenic action of herbicides, insecticides and fungicides on experimental animals is already known. Several studies have shown that chronic exposure to low levels of pesticides can cause adverse health effects and that many pesticides are mutagenic/carcinogenic. In the present research we monitored concurrently the presence of pesticides and genotoxic compounds extracted from 21 treated vegetables and 8 types of grapes sampled from the markets of a region in Southern Italy. The extracts were analysed for pesticides by gas-chromatography and HPLC, and for genotoxicity with two plant tests in Allium cepa roots: the micronucleus test and the chromosomal aberration test. We found 33 pesticides, some of which are outlawed. Genotoxicity was found in some of the vegetables and grapes tested. Allium cepa tests were sensitive for monitoring genotoxicity in food extracts. The micronucleus test in interphase cells gave much higher mutagenicity than the chromosomal aberration test in anaphase-telophase cells. PMID:15049565

  11. Separation and identification of polyphenols in apple pomace by high-speed counter-current chromatography and high-performance liquid chromatography coupled with mass spectrometry.

    PubMed

    Cao, Xueli; Wang, Cong; Pei, Hairun; Sun, Baoguo

    2009-05-01

    Apple pomace, a by-product in the processing of apple juice, was investigated as a potential source of polyphenols. Two methods of separation and purification of polyphenols from apple pomace extract were established by combination of gel chromatography with high-speed counter-current chromatography (HSCCC) and solvent extraction with HSCCC, respectively. The optimal separation was performed on a Sephadex LH-20 column using gradient aqueous ethanol as eluting solvent from 0% to 100% in increments of 10%. HPLC analysis indicated that main polyphenols existed in fractions eluted between 40% and 50% aqueous ethanol. The fractions of interest from column were separated by HSCCC with the solvent system hexane-ethyl acetate-1% aqueous acetic acid (0.5:9.5:10, v/v/v). Ethyl acetate fractionation of the apple pomace extract followed by direct HSCCC separation by the same solvent system in the volume ratio of 1:9:10 also produced a good separation of the main polyphenols of interest. Six high-purity polyphenols were achieved tentatively and identified by HPLC/MS: chlorogenic acid (1, m/z 354), quercetin-3-glucoside/quercetin-3-glacaside (2, m/z 464), quercetin-3-xyloside (3, m/z 434), phloridzin (4, m/z 436), quercetin-3-arabinoside (5, m/z 434), and quercetin-3-rhamnoside (6, m/z 448). These results provided a preliminary foundation for further development and exploration of apple pomace.

  12. 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

  13. 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

  14. Differences between heat-treated raw and commercial peanut extracts by skin testing and immunoblotting

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Peanut is generally consumed in a heat-treated form, yet the commonly available extracts for diagnostic purposes are derived from raw peanuts. Raw and heat-treated samples were prepared and compared with commercially available peanut extracts regarding SPT reactivity and serum IgE reactivity. Protei...

  15. 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

  16. 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). PMID:27554028

  17. 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

  18. Plants as Sources of Antimalarial Drugs Part. 1. In vitro Test Method for the Evaluation of Crude Extracts from Plants.

    PubMed

    O'neill, M J; Bray, D H; Boardman, P; Phillipson, J D; Warhurst, D C

    1985-10-01

    An IN VITRO antimalarial test, utilising the inhibition of uptake of [G- (3)H]-hypoxanthine into PLASMODIUM FALCIPARUM cultured in human blood, has been used to assess the activity of crude extracts of ARTEMISIA ANNUA and A. VULGARIS (Compositae) and of BRUCEA JAVANICA, AILANTHUS ALTISSIMA, and SIMABA CEDRON (Simaroubaceae).

  19. 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. PMID:20563411

  20. 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)

  1. Behavioral, neurochemical and neuroendocrine effects of the ethanolic extract from Curcuma longa L. in the mouse forced swimming test.

    PubMed

    Xia, X; Cheng, G; Pan, Y; Xia, Z H; Kong, L D

    2007-03-21

    Curcuma longa L. (turmeric) has been used for centuries in traditional Chinese medicine as a treatment for mental disorders including depression. The studies described here were undertaken to determine the behavioral, neurochemical and neuroendocrine effects of the ethanolic extract from Curcuma longa using the forced swimming test (FST) in male ICR strain of mice. The ethanolic extract was found to reduce the duration of immobility in the mouse FST when orally administered for 21 days. The extract markedly attenuated swim stress-induced decreases in serotonin, 5-hydroxyindoleacetic acid, noradrenaline and dopamine concentrations, as well as increases in serotonin turnover. Furthermore, the ethanolic extract of Curcuma longa significantly reversed the swim stress-induced increases in serum corticotropin-releasing factor and cortisol levels. Under these conditions, the ethanolic extract of Curcuma longa was partly different from fluoxetine and amitriptyline. These results suggested that antidepressant properties of the ethanolic extract of Curcuma longa was mediated through regulations of neurochemical and neuroendocrine systems and it may be a useful agent against depression.

  2. Countercurrent flow-limiting characteristics of a Savannah River Plant control rod septifoil

    SciTech Connect

    Anderson, J.L.

    1992-07-01

    Experiments were performed at the Idaho National Engineering Laboratory to investigate the counter-current flow limiting characteristics of a Savannah River Plant control rod septifoil assembly. These experiments were unheated, using air and water as the working fluids. Results are presented in terms of the Wallis flooding correlation for several different control rod configurations. Flooding was observed to occur in the vicinity of the inlet slots/holes of the septifoil, rather than within the rod bundle at the location of the minimum flow area. Nearly identical flooding characteristics of the septifoil were observed for configurations with zero, three, and four rods inserted, but significantly different results occurred with 5 rods inserted.

  3. 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

  4. 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.

  5. 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.

  6. Summary report of results of the vapor vacuum extraction test at the RWMC (Radioactive Waste Management Complex)

    SciTech Connect

    Sisson, J.B.; Ellis, G.C.

    1990-11-01

    A test scale vapor vacuum extraction system was operated for four months at the Radioactive Waste Management Complex. The extraction system removed more than 65 million ft{sup 3} of soil gas containing 429 Kg of Carbon Tetrachloride and 164 Kg of TCE. Hydraulic properties of the basalts were estimated and input into a numerical transport model. The model simulations indicated that a rubble zone at 190 ft dominated the soil gas flow pattern. Refined calibration of transport models will allow enhancement of the production system design to increase operational efficiency and effectiveness. 7 refs., 18 figs.

  7. 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...

  8. 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. PMID:22059477

  9. 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. PMID:25437744

  10. 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. PMID:22082527

  11. 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.

  12. 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.

  13. 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.

  14. Bioactivity-guided isolation of antimicrobial coumarins from Heracleum mantegazzianum Sommier & Levier (Apiaceae) fruits by high-performance counter-current chromatography.

    PubMed

    Walasek, Magdalena; Grzegorczyk, Agnieszka; Malm, Anna; Skalicka-Woźniak, Krystyna

    2015-11-01

    An efficient strategy, based on bioassay-guided fractionation, high-performance liquid chromatography (HPLC), and high-performance counter-current chromatography (HPCCC), was established to purify and evaluate the bioactive compounds from the dichloromethane extract of the fruits of Heracleum mantegazzianum Sommier & Levier (Apiaceae). The quaternary solvent system n-heptane-ethyl acetate-methanol-water (6:5:6:5 v/v) was used in the reversed phase mode. Using this method, in a single run, seven fractions were isolated, among them three were the pure furanocoumarins: pimpinellin, imperatorin, and phellopterin. In order to purify xanthotoxin a more polar system (1:1:1:1 v/v) was further applied. The antimicrobial activity of extract, chromatographic fractions, and single compounds were in the range of MIC = 0.03-1 mg mL(-1). Xanthotoxin may have priority as a compound of further interest based on its antimicrobial activity. For the first time, an extensive antimicrobial study was performed for pimpinellin and phellopterin.

  15. Separation and purification of four oligostilbenes from Iris lactea Pall. var. chinensis (Fisch.) Koidz by high-speed counter-current chromatography.

    PubMed

    Lv, Huanhuan; Wang, Honglun; He, Yanfeng; Ding, Chenxu; Wang, Xiaoyan; Suo, Yourui

    2015-04-15

    A method of using high-speed counter-current chromatography (HSCCC) for preparative isolation and purification of oligostilbenes from the ethanol extracts of seed kernel of Iris lactea Pall. var. chinensis (Fisch.) Koidz was established in this study. Four oligostilbenes were successfully separated and purified by HSCCC with two sets of two-phase solvent system, n-hexane-ethyl acetate-methanol-water (3:6:4.2:5.5, v/v/v/v) in the head-to-tail elution mode for the first separation to mainly isolate vitisin A (58 mg), ɛ-viniferin (76 mg) and peak II (43 mg) from 300 mg of the crude ethanol extracts, and then light petroleum-ethyl acetate-methanol-water (5:5:3:6, v/v/v/v) in the tail-to-head elution mode for the second separation to isolate vitisin B (52 mg) and vitisin C (11 mg) from 100mg of peak II. The purities of the isolated four oligostilbenes were all over 95.0% as determined by HPLC. Vitisin A, vitisin B and vitisin C, resveratrol tetramers, were isolated from Iris lactea for the first time. The preparation of crude sample was simple and the HSCCC method for the isolation and purification of four oligostilbenes was rapid, efficient and economical.

  16. 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

    2016-01-01

    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.

  17. 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

    2016-01-01

    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. PMID:27240330

  18. 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.

  19. Screening of antioxidant phenolic compounds in Chinese rhubarb combining fast counter-current chromatography fractionation and liquid chromatography/mass spectrometry analysis.

    PubMed

    Hu, Ruilin; Lu, Yanbin; Dai, Xiaojing; Pan, Yuanjiang

    2010-06-01

    In this paper, an effective method combing fast elution-extrusion counter-current chromatography (CCC) and LC/MS for rapid screening of antioxidative phenolic compounds in Chinese Rhubarb is presented. An integrated three-coil CCC column (40 mL each coil) was used to accomplish the optimization of biphasic liquid system. In a single run (approximately 40 min), the solvent system composed of n-hexane/ethyl acetate/methanol/water (1:1:1:1, v/v) was selected as optimum CCC liquid system for fast fractionation of the crude ethanol extract. With a 140 mL-capacity CCC instrument, 100 mg Chinese Rhubarb extract was separated under the optimized conditions, producing six fractions in only 100 min. The quantities of each fraction were approximately 15 mg. In addition, each fraction was subjected to antioxidant activity assay and characterized by LC/MS analysis. Fifty compounds, including phenolic acids, phenolic glucosides and hydroxyanthraquinones, were detected by LC/MS/MS analysis. As a result, gallic acid together with Fr I showed excellent antioxidant activity, which was well consistent with previous studies and exhibited great potential for natural drug discovery program of the present method.

  20. 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. PMID:26904162

  1. 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

  2. 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.

  3. A mathematical model for counter-current multiplications in the swim-bladder.

    PubMed Central

    Sund, T

    1977-01-01

    1. A computer model for swim-bladder gas filling has been developed. Phenomenological descriptions of the Root effect (pH-dependent O2 capacity of fish haemoglobin), of the lactic acid production in the gas gland and of the geometry of the rete mirabile are incorporated in the general counter-current equations to give a comprehensive model of gas filling. 2. It is known that pH along the rete is not constant, as supposed in an earlier gas-filling model. It is also known that the Root shift reaction has a different half-time model. It is also known that the Root shift reaction has a different half-time depending on whether the haemoglobin absorbs or releases O2. These particular effects are accounted for in the present model. 3. The model gives gas filling rate and maximum swim-bladder pressure for CO2, O2 and N2. The partial pressure of these gases as well as the concentration of lactic acid and the pH along the rete are also calculated. 4. The model reproduces quite accurately experimental values for gas-filling rate in eel, together with lactic acid, CO2 and O2 concentrations measured at the rete end-points. There is also good correlation between maximum predicted stable swim-bladder pressure and maximum recorded depth for four fishes investigated (r=0-937; P=0-06). 5. The model predicts an enhancement of O2 filling rate and maximum swim-bladder pressure of at least 4 when the reaction rates of the Root shift in eel haemoglobin are 0-2 sec (Root-off) and 10 sec (Root-on), as compared to an instantaneous Root shift. 6. With a swim-bladder pressure of 1 atm and Root-shift reaction rates of equal magnitude, the po2-profile along the rete is nearly linear. When the reaction rates are such as found experimentally in eel haemoglobin, the po2 along the rete is non-linear, with a maximum of approximately 2 atm near the bladder pole of the rete. An experimental verification of this maximum will constitute a crucial test of the model. 7. The calculations show that blood

  4. 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.

  5. Recovery of butanol by counter-current carbon dioxide fractionation with its potential application to butanol fermentation

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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,...

  6. 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

    2009-05-01

    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).

  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. PMID:27649502

  8. 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.

  9. 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

  10. Extractive phase vanishing reactions with dichloromethane, perfluorohexanes, and dibromoethane: slow addition in a test tube.

    PubMed

    Curran, Dennis P; Werner, Stefan

    2004-03-18

    [reaction: see text] Partition coefficient measurements and experiments with a dye show that a new fluorous "phase vanishing reaction" described by Jana and Verkade occurs by an extractive mechanism. This mechanism is contrasted with the original diffusive phase-vanishing reactions introduced by Ryu and co-workers.

  11. Test-methods on the test-bench: a comparison of complete exhaust and exhaust particle extracts for genotoxicity/mutagenicity assessment.

    PubMed

    Steiner, Sandro; Heeb, Norbert V; Czerwinski, Jan; Comte, Pierre; Mayer, Andreas; Petri-Fink, Alke; Rothen-Rutishauser, Barbara

    2014-05-01

    With the growing number of new exhaust after-treatment systems, fuels and fuel additives for internal combustion engines, efficient and reliable methods for detecting exhaust genotoxicity and mutagenicity are needed to avoid the widespread application of technologies with undesirable effects toward public health. In a commonly used approach, organic extracts of particulates rather than complete exhaust is used for genotoxicity/mutagenicity assessment, which may reduce the reliability of the results. In the present study, we assessed the mutagenicity and the genotoxicity of complete diesel exhaust compared to an organic exhaust particle extract from the same diesel exhaust in a bacterial and a eukaryotic system, that is, a complex human lung cell model. Both, complete exhaust and organic extract were found to act mutagenic/genotoxic, but the amplitudes of the effects differed considerably. Furthermore, our data indicate that the nature of the mutagenicity may not be identical for complete exhaust and particle extracts. Because in addition, differences between the responses of the different biological systems were found, we suggest that a comprehensive assessment of exhaust toxicity is preferably performed with complete exhaust and with biological systems representative for the organisms and organs of interest (i.e., human lungs) and not only with the Ames test. PMID:24697289

  12. 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.

  13. 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.

  14. 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.

  15. 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. PMID:26268968

  16. 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

  17. 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

  18. 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.

  19. 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

  20. 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.

  1. Analytical high-speed countercurrent chromatography with photodiode array detection (HSCCC-UV)

    SciTech Connect

    Schaufelberger, D.E. )

    1989-01-01

    The use of analytical high-speed countercurrent chromatography with a photodiode array detector (HSCCC-UV) is described. Reduction of detector noise caused by non-retained stationary phase was achieved by adding an auxiliary solvent (MeOH, isoPrOH) by means of a post-column reactor. The technique was applied to the separation of aromatic compounds and natural products in Hexane-MeOH-H{sub 2} and CHCl{sub 3}-MeOH-H{sub 2}O solvent systems. On-line recorded UV spectra were almost identical to those obtained with pure standards in methanol. Spectra obtained by HSCCC-UV can be used to characterize separated compounds and facilitate peak identification.

  2. Separation of phenylsuccinic acid enantiomers using biphasic chiral recognition high-speed countercurrent chromatography.

    PubMed

    Sun, Genlin; Tang, Kewen; Zhang, Panliang; Yang, Weijun; Sui, Guoqing

    2014-07-01

    High-speed countercurrent chromatography (HSCCC) combined with biphasic chiral recognition was successfully applied to the resolution of phenylsuccinic acid enantiomers. D-Isobutyl tartrate and hydroxypropyl-β-cyclodextrin were employed as lipophilic and hydrophilic selectors dissolved in the organic stationary phase and aqueous mobile phase, respectively. The two-phase solvent system was made up of n-hexane/methyl tert-butyl ether/water (0.5:1.5:2, v/v/v). Impacts of the type and concentration of chiral selectors, the pH value of the aqueous phase solution as well as the temperature on the separation efficiency were investigated. By means of preparative HSCCC, pure enantiomer was obtained by separating 810 mg of racemate with a purity >99.5% and a recovery rate between 82 and 85%. The experimental results indicate that biphasic recognition HSCCC provide a promising means for efficient separation of racemates.

  3. The impact of advective transport by the South Indian Ocean Countercurrent on the Madagascar plankton bloom

    NASA Astrophysics Data System (ADS)

    Huhn, F.; von Kameke, A.; Pérez-Muñuzuri, V.; Olascoaga, M. J.; Beron-Vera, F. J.

    2012-03-01

    Based on ten years (1998-2007) of satellite ocean color data we analyze the spatiotemporal patterns in the seasonal Madagascar plankton bloom with respect to the advection of the recently discovered Southern Indian Ocean Countercurrent (SICC). In maps of Finite-time Lyapunov Exponents (FTLE) and Finite-Time Zonal Drift (FTZD) computed from altimetry derived velocities we observe a narrow zonal jet that starts at ˜25°S at the southern tip of Madagascar, an important upwelling region, and extends to the east further than the largest plankton blooms (˜2500 km). In bloom years, the jet coincides with large parts of the northern boundary of the plankton bloom, acting as a barrier to meridional transport. Our findings suggest that advection is an important and so far underestimated mechanism for the eastward propagation and the extent of the plankton bloom. This supports the hypothesis of a single nutrient source south of Madagascar.

  4. 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.

  5. Modeling of reflux condensation and countercurrent annular flow in a two-phase closed thermosyphon

    SciTech Connect

    Reed, J.G.; Tien, C.L.

    1985-12-01

    Reflux condensation in the steam generator tubes of a PWR is a potentially important heat removal mechanism during the cool-down phase following a small-break LOCA. This work studies reflux condensation using the two-phase closed thermosyphon as a model system. An analytical model based on control-volume formulations of mass, momentum, and energy balances for the liquid and vapor flows in each section of the device is developed. Numerical solutions to the system of governing equations are presented for both steady-state and transient operation of the device. While no data with which to compare the results of the transient analysis are currently available, the steady-state solutions compare well with available experimental data on flooding and film thickness. Thus, the analytical approach presented in this work is demonstrated to be a powerful technique for analyzing countercurrent, annular, two-phase flows. 17 refs., 17 figs.

  6. 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.

  7. 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%.

  8. EVALUATION OF THE EXTRACT-RELEASE VOLUME PHENOMENON AS A RAPID TEST FOR DETECTING SPOILAGE IN BEEF.

    PubMed

    JAY, J M; KONTOU, K S

    1964-07-01

    Ground beef of several grades, obtained fresh and held refrigerated until spoiled, was presented to a test panel for scoring on color, odor, and tactile response (tackiness) as to degree of acceptance. Panel scores were correlated with total bacterial counts, ninhydrin-reactive substances, and ERV (extract-release volume) on the same meat. ERV correlated highest with bacterial counts the largest number of times; tackiness, odor, ninhydrin, and color followed in that order. Correlation between bacterial numbers and organoleptic qualities was best, with tackiness followed closely by odor, and then by color. Correlation between tackiness and odor was high. The degree of correlation between bacterial numbers, tackiness, and ERV was high enough to warrant the use of the ERV phenomenon as a rapid test of microbial quality of beef. An ERV value of 25 under the conditions of the test was supported as a divider between acceptable and unacceptable ground beef. PMID:14201094

  9. EVALUATION OF THE EXTRACT-RELEASE VOLUME PHENOMENON AS A RAPID TEST FOR DETECTING SPOILAGE IN BEEF.

    PubMed

    JAY, J M; KONTOU, K S

    1964-07-01

    Ground beef of several grades, obtained fresh and held refrigerated until spoiled, was presented to a test panel for scoring on color, odor, and tactile response (tackiness) as to degree of acceptance. Panel scores were correlated with total bacterial counts, ninhydrin-reactive substances, and ERV (extract-release volume) on the same meat. ERV correlated highest with bacterial counts the largest number of times; tackiness, odor, ninhydrin, and color followed in that order. Correlation between bacterial numbers and organoleptic qualities was best, with tackiness followed closely by odor, and then by color. Correlation between tackiness and odor was high. The degree of correlation between bacterial numbers, tackiness, and ERV was high enough to warrant the use of the ERV phenomenon as a rapid test of microbial quality of beef. An ERV value of 25 under the conditions of the test was supported as a divider between acceptable and unacceptable ground beef.

  10. 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).

  11. 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.

  12. Efficient preparative isolation and identification of walnut bioactive components using high-speed counter-current chromatography and LC-ESI-IT-TOF-MS.

    PubMed

    Grace, Mary H; Warlick, Charles W; Neff, Scott A; Lila, Mary Ann

    2014-09-01

    Preparative isolation of complex mixtures of compounds from walnut polar extracts was established by a combination of high-speed counter-current chromatography (HSCCC) and electrospray ionization-ion trap-time of flight mass spectrometry (ESI-IT-TOF-MS). Compounds were isolated after a solvent optimisation selection based on solute distribution in a biphasic solvent system. Isolation was achieved through one or two successive HSCCC runs, and final purification on Sephadex LH-20. Isolated compounds included ellagitannins (1-11), gallic acid (12), dicarboxylic acid glucosides (13-15), hydrojuglone glucoside (16), catechin (17), procyanidin B2 (18), and megasterone glucosides (19-20). Praecoxin D (4) was isolated for the first time from walnut, while praecoxin A methyl ester (5) and glansreginin A n-butyl ester (14) are newly identified compounds. The purity and identity of isolated compounds were confirmed by NMR and HPLC-ESI-MS/MS. These results provided a foundation for in depth characterisation of walnut compounds and offered an efficient strategy for isolation of potentially health-relevant phytochemicals from walnuts.

  13. 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.

  14. Isolation of two new prenylated flavonoids from Sinopodophyllum emodi fruit by silica gel column and high-speed counter-current chromatography.

    PubMed

    Sun, Yanjun; Sun, Yinshi; Chen, Hui; Hao, Zhiyou; Wang, Junmin; Guan, Yanbin; Zhang, Yanli; Feng, Weisheng; Zheng, Xiaoke

    2014-10-15

    Two new prenylated flavonoids, sinoflavonoids A-B, were isolated from the dried fruits of Sinopodophyllum emodi by silica gel column chromatography (SGCC) and high-speed counter-current chromatography (HSCCC). The 95% ethanol extract was partitioned with petroleum ether, dichloromethane, ethyl acetate, and n-butanol in water, respectively. The ethyl acetate fraction was pre-separated by SGCC with a petroleum ether-acetone gradient. The eluates containing target compounds were further separated by HSCCC with n-hexane-ethyl acetate-methanol-water (4:6:4:4, v/v). Finally, 17.3mg of sinoflavonoid A and 25.9mg of sinoflavonoid B were obtained from 100mg of the pretreated concentrate. The purities of sinoflavonoid A and sinoflavonoid B were 98.47% and 99.38%, respectively, as determined by HPLC. Their structures were elucidated on the basis of spectroscopic evidences (HR-ESI-MS, (1)H-NMR, (13)C-NMR, HSQC, HMBC). The separation procedures proved to be efficient, especially for trace prenylated flavonoids.

  15. Analysis and determination of oestrogen-active compounds in fructus amomi by the combination of high-speed counter-current chromatography and high performance liquid chromatography.

    PubMed

    Ying, Hao; Liu, Jinpeng; Du, Qizhen

    2014-05-01

    Amomum longiligulare or Amomum villosum showed oestrogenic activity. In the present study, oestrogen-active components in fructus amomi, the seeds of A. longiligulare were separated by high-speed countercurrent chromatography (HSCCC) using stepwise elution of eight mobile phases with gradient polarity and advanced separation by high performance liquid chromatography (HPLC). The results yielded 17 compounds with the amount of 8-138mg and a purity of 94.3-99.8% from a 3g ethanolic extract of fructus amomi. The chemical structures of the compounds were identified by ESI-MS and NMR spectra, in which eight diarylheptanoids were demonstrated as the main oestrogen-active compounds in the fructus amomi. Determination of the diarylheptanoids in fructus amomi from various origins showed that fructus amomi contains more than 0.5% total diarylheptanoids. The results showed that fructus amomi is a diarylheptanoids-rich food resource possessing oestrogen-activity. The combination method of HSCCC and HPLC can be applied for the analysis of bioactive compounds by detecting the corresponding bioactivity in the HSCCC fractions and separating the target compounds with HPLC.

  16. 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.

  17. Separation and purification of five phenylpropanoid glycosides from Lamiophlomis rotata (Benth.) Kudo by a macroporous resin column combined with high-speed counter-current chromatography.

    PubMed

    Yue, Hui-Lan; Zhao, Xiao-Hui; Mei, Li-Juan; Shao, Yun

    2013-09-01

    Five phenylethanoid glycosides (PhGs), forsythoside B, verbascoside, alyssonoside, isoverbascoside, and leucosceptoside B, were isolated and purified from Lamiophlomis rotata (Benth.) Kudo by high-speed counter-current chromatography (HSCCC) combined with macroporous resin (MR) column separation. In the present study, the two-phase solvent system composed of ethyl acetate/n-butanol/water (13:3:10, v/v/v) was used for HSCCC separation. A total of 27 mg of forsythoside B, 41 mg of verbascoside, 29 mg of alyssonoside, 23 mg of isoverbascoside, and 13 mg of leucosceptoside B with purities of 97.7, 99.2, 99.5, 99.3, and 97.3%, respectively, were obtained in a one-step separation within 4 h from 150 mg of crude extract. The recoveries of the five PhGs after MR-HSCCC separation were 74.5, 76.5, 72.5, 76.4, and 77.0%, respectively. The chemical structures of all five compounds were identified by (1) H and (13) C NMR spectroscopy.

  18. Preparative isolation of alkaloids from Dactylicapnos scandens using pH-zone-refining counter-current chromatography by changing the length of the separation column.

    PubMed

    Wang, Xiao; Dong, Hongjing; Yang, Bin; Liu, Dahui; Duan, Wenjuan; Huang, Luqi

    2011-12-01

    pH-Zone-refining counter-current chromatography was successfully applied for the preparative separation of alkaloids from Dactylicapnos scandens. The two-phase solvent system was composed of petroleum ether-ethyl acetate-methanol-water (3:7:1:9, v/v), where 20 mM of triethylamine (TEA) was added to the upper phase as a retainer and 5 mM of hydrochloric acid (HCl) to the aqueous phase as an eluter. In this experiment, the apparatus with an adjustable length of the separation column was used for the separation of alkaloids from D. scandens and the resolution of the compounds can be remarkably improved by increasing the length of the separation column. As a result, 70 mg protopin, 30 mg (+) corydine, 120 mg (+) isocorydine and 40 mg (+) glaucine were obtained from 1.0 g of the crude extracts and each with 99.2%, 96.5%, 99.3%, 99.5% purity as determined by HPLC. The chemical structures of these compounds were confirmed by positive ESI-MS and (1)H NMR. PMID:22056347

  19. Isolation and purification of salvianolic acid A and salvianolic acid B from Salvia miltiorrhiza by high-speed counter-current chromatography and comparison of their antioxidant activity.

    PubMed

    Sun, Yinshi; Zhu, Haifang; Wang, Jianhua; Liu, Zhengbo; Bi, Jianjie

    2009-03-15

    Water-soluble salvianolic acid A (Sal A) and salvianolic acid B (Sal B) were successfully isolated and purified from the crude extract of Salvia miltiorrhiza by high-speed counter-current chromatography (HSCCC). The solvent system was n-hexane-ethyl acetate-methanol-water (3:6:6:10, v/v/v/v). 4.27 mg of Sal A and 32.09 mg of Sal B were obtained from 260 mg of the crude sample. The purities of Sal A and Sal B were 96.67% and 97.43%, respectively. Their structures were identified by (1)H NMR and (13)C NMR. Antioxidant activities of Sal A and Sal B were also evaluated and compared by the methods of 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay and 2,2-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS(+)) radical cation decolourisation assay. Both Sal A and Sal B showed high radical scavenging activities with their EC(50) values being 1.43+/-0.09 and 1.81+/-0.01 microg/ml in DPPH radical method. The ABTS results showed that Sal A and Sal B exhibited high total antioxidant activities, their EC(50) values were 1.35+/-0.00 and 1.43+/-0.01 microg/ml, respectively.

  20. Preparative Isolation of Two Prenylated Biflavonoids from the Roots and Rhizomes of Sinopodophyllum emodi by Sephadex LH-20 Column and High-Speed Counter-Current Chromatography.

    PubMed

    Sun, Yan-Jun; Pei, Li-Xin; Wang, Kai-Bo; Sun, Yin-Shi; Wang, Jun-Min; Zhang, Yan-Li; Gao, Mei-Ling; Ji, Bao-Yu

    2015-12-23

    Two prenylated biflavonoids, podoverines B-C, were isolated from the dried roots and rhizomes of Sinopodophyllum emodi using a Sephadex LH-20 column (SLHC) and high-speed counter-current chromatography (HSCCC). The 95% ethanol extract was partitioned with ethyl acetate in water. Target compounds from the ethyl acetate fraction were further enriched and purified by the combined application of SLHC and HSCCC. n-Hexane-ethyl acetate-methanol-water (3.5:5:3.5:5, v/v) was chosen as the two phase solvent system. The flow rate of mobile phase was optimized at 2.0 mL·min(-1). Finally, under optimized conditions, 13.8 mg of podoverine B and 16.2 mg of podoverine C were obtained from 200 mg of the enriched sample. The purities of podoverines B and C were 98.62% and 99.05%, respectively, as determined by HPLC. For the first time, podoverins B and C were found in the genus Sinopodophyllum. Their structures were determined by spectroscopic methods (HR-ESI-MS, ¹H-NMR, (13)C-NMR, HSQC, HMBC). Their absolute configurations were elucidated by comparison of their experimental and calculated ECD spectra. The cytotoxic activities were evaluated against MCF-7 and HepG2 cell lines. The separation procedures proved to be practical and economical, especially for trace prenylated biflavonoids from traditional Chinese medicine.

  1. Isolation of C-glycosylflavonoids with α-glucosidase inhibitory activity from Passiflora bogotensis Benth by gradient high-speed counter-current chromatography.

    PubMed

    Costa, Geison Modesti; Cárdenas, Paola Andrea; Gazola, Andressa Córneo; Aragón, Diana Marcela; Castellanos, Leonardo; Reginatto, Flávio Henrique; Ramos, Freddy Alejandro; Schenkel, Eloir Paulo

    2015-05-15

    In this study, we applied a gradient High-Speed Counter-Current Chromatography (HSCCC) method that allowed, by direct injection of an aqueous crude extract of the leaves of Passiflora bogotensis, the successful isolation of six flavonoids in a single run, with purity of each compound higher than 81%. This separation enabled the isolation of two new flavonoid glycosides, apigenin-6-C-α-l-rhamnopyranosyl-(1→2)-(6″-O-acetyl)-β-d-glucopyranoside (2) and luteolin-6-C-α-l-rhamnopyranosyl-(1→2)-(6″-O-acetyl)-β-d-glucopyranoside (4), and four known ones, isovitexin (1), isoorientin (3), isovitexin-2″-O-rhamnoside (5) and isoorientin-2″-O-rhamnoside (6). The structures of the isolated compounds were identified by HPLC-DAD, LC-MS, (1)H and (13)C NMR and comparison with literature data. The inhibitory activities of all of these compounds were evaluated in vitro on α-glucosidase from S. cerevisiae, and the IC50 was determinate. This is the first study concerning the chemical composition and biological activity of Passiflora bogotensis. PMID:25864011

  2. 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

    2014-10-01

    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.

  3. Preparative isolation of alkaloids from Dactylicapnos scandens using pH-zone-refining counter-current chromatography by changing the length of the separation column.

    PubMed

    Wang, Xiao; Dong, Hongjing; Yang, Bin; Liu, Dahui; Duan, Wenjuan; Huang, Luqi

    2011-12-01

    pH-Zone-refining counter-current chromatography was successfully applied for the preparative separation of alkaloids from Dactylicapnos scandens. The two-phase solvent system was composed of petroleum ether-ethyl acetate-methanol-water (3:7:1:9, v/v), where 20 mM of triethylamine (TEA) was added to the upper phase as a retainer and 5 mM of hydrochloric acid (HCl) to the aqueous phase as an eluter. In this experiment, the apparatus with an adjustable length of the separation column was used for the separation of alkaloids from D. scandens and the resolution of the compounds can be remarkably improved by increasing the length of the separation column. As a result, 70 mg protopin, 30 mg (+) corydine, 120 mg (+) isocorydine and 40 mg (+) glaucine were obtained from 1.0 g of the crude extracts and each with 99.2%, 96.5%, 99.3%, 99.5% purity as determined by HPLC. The chemical structures of these compounds were confirmed by positive ESI-MS and (1)H NMR.

  4. Clinical Efficacy Test of Polyester Containing Herbal Extract Dressings in Burn Wound Healing.

    PubMed

    Muangman, Pornprom; Praditsuktavorn, Banjerd; Chinaroonchai, Kusuma; Chuntrasakul, Chomchark

    2016-09-01

    Technological advancement has assisted in developing various availabilities of wound products that help in not only in healing and preventing infection but also in providing patients' comfort and pain reduction during application. However, most of advanced wound healing products in Thailand were imported at high costs to patients. Nowadays, there are increased numbers of local researches of herbs that could provide healing environment for successful wound care. Herbal wound products are currently being introduced as alternatives to those imported dressings. The aim of this study was to report the clinical efficacy of using polyester containing herbal extract dressings in healing of second-degree burns. The volunteers were divided by simply randomized method into the study group of patient using polyester containing herbal extract dressing and the control group of patients treating with dressings that are commercially available and common use. The standard treatment protocols were performed at every 3 days of dressing change. Comparative evaluation consisted of time of healing, length of hospital stays, pain analog score assessment, percentage of infection, and descriptive notification of unfavorable clinical symptoms or signs or side effects.

  5. Clinical Efficacy Test of Polyester Containing Herbal Extract Dressings in Burn Wound Healing.

    PubMed

    Muangman, Pornprom; Praditsuktavorn, Banjerd; Chinaroonchai, Kusuma; Chuntrasakul, Chomchark

    2016-09-01

    Technological advancement has assisted in developing various availabilities of wound products that help in not only in healing and preventing infection but also in providing patients' comfort and pain reduction during application. However, most of advanced wound healing products in Thailand were imported at high costs to patients. Nowadays, there are increased numbers of local researches of herbs that could provide healing environment for successful wound care. Herbal wound products are currently being introduced as alternatives to those imported dressings. The aim of this study was to report the clinical efficacy of using polyester containing herbal extract dressings in healing of second-degree burns. The volunteers were divided by simply randomized method into the study group of patient using polyester containing herbal extract dressing and the control group of patients treating with dressings that are commercially available and common use. The standard treatment protocols were performed at every 3 days of dressing change. Comparative evaluation consisted of time of healing, length of hospital stays, pain analog score assessment, percentage of infection, and descriptive notification of unfavorable clinical symptoms or signs or side effects. PMID:27440796

  6. A systematic approach for extracting verification patterns from an OPC test mask

    NASA Astrophysics Data System (ADS)

    Kamel, Mohammad K. A.; Al-Imam, Mohamed

    2012-06-01

    Optical Proximity Correction (OPC) is a crucial step in Semiconductor manufacturing for technology of dimensions below the exposure wavelength. Light from the exposure source is diffracted when passing through mask dimensions below the exposure wavelength causing patterns on wafer to differ from the intent patterns. During OPC the design intent layout patterns are modified to compensate for light diffractions so that the final wafer patterns match the design intent patterns. OPC achieves this by using OPC models that model the optical conditions, resist, and etch behavior; and an OPC recipe that controls the patterns modification process. The OPC models are calibrated from test mask structures that are developed, exposed and measured when starting to set up the manufacturing process. Structures chosen to be placed on the test mask have a great impact on the capability to predict future layout patterns that were not present in the original test mask, referred to as model coverage. Test masks are usually composed of patterns used in model calibration and others used for verifying the calibrated model. In advanced technology nodes, both the feature size and the error budget are being shrunk. Hence to reach the best model coverage with acceptable accuracy, we need to ensure that the test mask contains all the possible structures in the real designs, while maintaining that the number of patterns does not consume long metrology tools time, cause extra overhead cost to the process, or delay the development cycle. This paper presents a systematic approach to optimize the number of patterns to be included in the test mask and split test patterns into calibration and verification patterns. Results from using the proposed method are compared to other methods of splitting that are based either on geometrical or random methods. The approach provided a significant reduction in model calibration time, the number of needed patterns in the test mask, and the total development

  7. 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

  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).

    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.

  9. 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.

  10. 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.

  11. 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.

  12. Technology of nondestructive light gas extraction from ice tested on samples from a bore hole above Vostok Lake

    NASA Astrophysics Data System (ADS)

    Chetverikov, Yu. O.; Aruev, N. N.; Bulat, S. A.; Ezhov, V. F.; Lipenkov, V. Ya.; Solovei, V. A.; Tyukal'tsev, R. V.; Fedichkin, I. L.

    2016-07-01

    Nondestructive technology has been developed for the extraction of light gases dissolved in ice. The technology has been tested on samples of atmospheric and congealed ice of the 5-G3 bore hole of the Vostok station (East Antarctica) extracted from depths of 3457-3698 m. Down to 3539 m, ice is of an atmospheric origin, while ice deposited deeper is formed by natural water of Vostok Lake frozen on the glacier. Light gases were extracted into samplers (glass flasks) in the course of the 3-day degassing of samples freshly elevated from a bore hole. The samples were analyzed on the FT-1 time-of-flight mass spectrometer 6 months after sampling. Measurements reveal the presence of amounts of helium as well as molecular hydrogen considerably exceeding the atmospheric values. Measured values of gas ratio H2/4He = 5.4 ± 1.9 in the samples from depths of 3596-3698 m exceed the atmospheric values by more than an order of magnitude.

  13. Oxygen extraction from lunar materials - An experimental test of an ilmenite reduction process

    NASA Technical Reports Server (NTRS)

    Williams, R. J.

    1985-01-01

    The reaction of ilmenite with hydrogen to produce water has been studied experimentally in order to evaluate the effectiveness of using a cold trap to improve yields in a continuous flow process. Yields were enhanced, but not to the degree observed in batch processing systems. The terrestrial simulant used in these studies contained traces of iron sulfide, which released H2S during processing with a deleterious effect on several components of the test system. More sophisticated testing should be undertaken to obtain kinetic data and attention given to the removal of sulfides in the pre-process beneficiation.

  14. Test of a new method for seismic indices and granulation parameters extraction

    NASA Astrophysics Data System (ADS)

    Peralta, R. A.; Samadi, R.; Michel, E.

    2015-09-01

    In the framework of the data base project SSI (Stellar Seismic Indices, we have developed and tested a new method aiming at optimizing the simultaneous measurement of both the seismic indices characterizing the oscillations (Δν, νmax) and the indices characterizing the granulation signature. Here, we describe this method which is intended to take advantage of the MLE (maximum likelihood estimate) algorithm combined with the parametrized representation of the red giants pulsation spectrum following the Universal Pattern [6]. We report its performances tested on Monte Carlo simulations.

  15. The Effect of Hydro-Alcoholic Extract of Foeniculum vulgare Mill on Leukocytes and Hematological Tests in Male Rats

    PubMed Central

    Mansouri, Esrafil; Kooti, Wesam; Bazvand, Maryam; Ghasemi Boroon, Maryam; Amirzargar, Ashraf; Afrisham, Reza; Afzalzadeh, Mohammad Reza; Ashtary-Larky, Damoon; Jalali, Nasrin

    2015-01-01

    Background: Medicinal plants have a long history in treating blood disorders, which is one of the most common problems in today's advanced world. Fennel (Foeniculum vulgare) is a medicinal plant with a high content of polyphenols and has antioxidant and immunomodulatory properties. Objectives: The aim of this study was to evaluate the effect of hydro-alcoholic extract of fennel on some hematological indices in male rats. Materials and Methods: In this experimental study, thirty male Wistar rats were divided into six groups (five rats in each group). The first group (control) did not receive any dose; the second group (sham) received 1 mL normal saline (extraction solvent); and the experimental groups 1, 2, 3 and 4 respectively received 1 mL hydro alcoholic extract of fennel in four doses of 250, 500, 750 and 1000 mg/kg of body weight every 48 hours for 30 days by gavage. One day after the last gavage following induction of anesthesia and taking blood from the heart of rats, measurement of red and white blood cells, hemoglobin, hematocrit and tests of bleeding and coagulation time (CT) were performed. The data was analyzed by one-way ANOVA test using SPSS15 software. Results: Fennel increased mean RBC (7.54 ± 0.53 × 106) and WBC (5.89 ± 0.78 × 103) values, especially at a dose of 250 mg/mL and CT (2.45 ± 0.20) at a dose of 500mg/mL compared to the control group (P < 0.05). Conclusions: Fennel increased red and white blood cells probably due to the presence of polyphenols and antioxidant activity of fennel and reduced negative effects of free radicals on blood cells. PMID:25866717

  16. 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

  17. Toxicological assessment of enzyme-treated asparagus extract in rat acute and subchronic oral toxicity studies and genotoxicity tests.

    PubMed

    Ito, Tomohiro; Ono, Tomoko; Sato, Atsuya; Goto, Kazunori; Miura, Takehito; Wakame, Koji; Nishioka, Hiroshi; Maeda, Takahiro

    2014-03-01

    The safety of enzyme-treated asparagus extract (ETAS) developed as a novel anti-stress functional material was assessed in acute and subchronic studies and genotoxicity assays. In the acute oral dose toxicity study, all rats survived during the test period and ETAS did not influence clinical appearance, body weight gain and necropsy findings at a dosage of 2000mg/kg body weight. Thus, the 50% lethal dose (LD50) of ETAS was determined to be greater than 2000mg/kg. The 90-day subchronic study (500, 1000 and 2000mg/kg body weight, delivered by gavage) in rats reported no significant adverse effects in food consumption, body weight, mortality, urinalysis, hematology, biochemistry, necropsy, organ weight and histopathology. In the micronucleus test of mice, the incidence of micronuclei in ETAS-administered groups (500, 1000 and 2000mg/kg/day, injected twice) was equivalent to that of the negative control group, while the positive control group receiving mitomycin C showed a high incidence. The potential of ETAS to induce gene mutation was tested using four Salmonella typhimurium strains and Escherichia coli WP2uvrA. The test sample was not mutagenic to the test strains. These results support the safety of ETAS as food and dietary supplement.

  18. [Sub-chronic toxicity and test of eye irritability of leaf aqueous extract from Plantago major (plantaginaceae)].

    PubMed

    García González, Mildred; Coto Morales, Teresita; Soto Rodríguez, Gerardo A; Pazos, Liliana

    2003-01-01

    For the sub-chronic toxicity an aqueous preparation of Plantago major leaves was tested in 20 male NGP mice, with an average weight of 20.15 g and separated in two groups of ten individuals each. The dose used was 2000 mg/kg and the control group received 0.5 ml of distilled water. The extract administration was done daily during five days at week for a total period of 40 days. Signs of sub-chronic toxicity were observed in the days two and 12 of treatment. No significant change in corporal weight was observed. The ocular irritation was tested in five New Zeland male rabbits, with an average weight of 3.640 kg. The dose used was a 200 microliters the preparation (100 mg/ml) of Plantago major leaves, instill into the right eye and the control was used the left eye instill 200 microliters of distilled water. The administration was done daily during five days. The extract shows no significant irritation during the observation period.

  19. [Sub-chronic toxicity and test of eye irritability of leaf aqueous extract from Plantago major (plantaginaceae)].

    PubMed

    García González, Mildred; Coto Morales, Teresita; Soto Rodríguez, Gerardo A; Pazos, Liliana

    2003-01-01

    For the sub-chronic toxicity an aqueous preparation of Plantago major leaves was tested in 20 male NGP mice, with an average weight of 20.15 g and separated in two groups of ten individuals each. The dose used was 2000 mg/kg and the control group received 0.5 ml of distilled water. The extract administration was done daily during five days at week for a total period of 40 days. Signs of sub-chronic toxicity were observed in the days two and 12 of treatment. No significant change in corporal weight was observed. The ocular irritation was tested in five New Zeland male rabbits, with an average weight of 3.640 kg. The dose used was a 200 microliters the preparation (100 mg/ml) of Plantago major leaves, instill into the right eye and the control was used the left eye instill 200 microliters of distilled water. The administration was done daily during five days. The extract shows no significant irritation during the observation period. PMID:15162770

  20. In vitro physiologically based extraction test (PBET) and bioaccessibility of arsenic and lead from various mine waste materials.

    PubMed

    Bruce, Scott; Noller, Barry; Matanitobua, Vitukawalu; Ng, Jack

    2007-10-01

    In vivo models show that the bioavailability of soil contaminants varies between site and type of matrix. Studies demonstrated that assuming 100% bioavailability of arsenic (As) and lead (Pb) from soils and mine waste materials overestimates the risk associated with human exposure. In in vitro systems, the simulated bioavailability of a contaminant is referred to as the "bioaccessibility" and is used as an alternative quantitative indicator for in vivo derived bioavailability estimates. The general concept of the in vitro extraction test is to predict the bioavailability of inorganic substances from solid matrices by simulating the gastrointestinal tract (GIT) environment. The aims of this study were to: (1) investigate the bioaccessibility of As and Pb from various mine wastes, including tailings, heap leach, and waste rock, using a physiologically based extraction test (PBET); (2) validate the bioaccessibility values from PBET with in vivo bioavailability values measured using animal models; and (3) correlate PBET results with the bioavailability values measured from alternative in vivo models (rats and cattle, from Bruce, 2004). Significant correlation was observed between bioaccessibility values from PBET, and bioavailability values generated for both rats and cattle, demonstrating the potential to utilize PBET as a relatively inexpensive alternative to in vivo models for bioavailability assessment.

  1. Electromagnetic Borehole Flowmeter Testing at the H-Area Extraction Wells

    SciTech Connect

    Flach, G.P.

    2002-07-23

    The objective of the Electromagnetic Borehole Flowmeter (EBF) testing documented in this report is to expand the technology to include simultaneous characterization of conductivity, contaminant concentration, and mass flux profiles. The latter two parameters, especially mass flux, can be valuable information for remedial design.

  2. Fractionation of an anthocyanin-rich bilberry extract and in vitro antioxidative activity testing.

    PubMed

    Juadjur, A; Mohn, C; Schantz, M; Baum, M; Winterhalter, P; Richling, E

    2015-01-15

    The incidence of chronic diseases increases with advancing age of the population. A commonly discussed cause of chronic diseases is oxidative stress, which occurs in the body when there is an imbalance between the formation and inactivation of so-called reactive oxygen species (ROS). Epidemiological data suggest that a 'healthy diet', with a high content of flavonoids indicates preventive properties and correlates with an inverse effect with respect to the risk of chronic diseases. Berries (especially bilberries, Vaccinium myrtillus L.) are an important source of these flavonoids. In this study, we investigated, in vitro, the antioxidative properties of fractions obtained from a commercially available anthocyanin-rich bilberry extract (BE). As markers for antioxidative activity, the intracellularly generated ROS levels, oxidative DNA damage, and total glutathione (tGSH) levels were determined in the human colon cell lines Caco-2 and HT-29. In Caco-2 cells, the ROS levels and, in both cell lines, the oxidative DNA damage, were significantly reduced in the presence of the original BE and phenolcarbonic acid-rich fraction. Total GSH levels were slightly increased after pretreatment with BE, phenolcarbonic acid and the polymeric fractions, but not with the anthocyanin fraction. In summary, the BE and the therefrom-isolated phenolcarbonic acid-rich fraction, showed the most potent antioxidative activity whereas the polymeric and anthocyanin-rich fraction, in total, were less active.

  3. Linear two-step gradient counter-current chromatography analysis based on a recursive solution of an equilibrium stage model.

    PubMed

    Beltscheva, Daria; Hugo, Peter; Seidel-Morgenstern, Andreas

    2003-03-01

    The implementation of gradients in continuously operated chromatographic counter-current processes has recently attracted considerable interest as a method to improve the performance of this effective separation method. If liquid mobile phases are applied it is advantageous to set the solvent strength in the desorbent stream higher than that in the feed stream. As a consequence. the components to be separated are more retained in the adsorption zones and more easily eluted in the desorption zones. Due to the additional degrees of freedom the design and the optimization of such a two-step gradient counter-current process is difficult. In this paper a steady state equilibrium stage model is used to simulate the process under linear conditions. A simple solution of the underlying model equations is presented capable to describe efficiently the unit for large stage numbers typically encountered in chromatographic columns. Due to the rapidity of the algorithm developed a broad range of operating conditions can be evaluated systematically for different types of gradients. The impact of (a) the functional dependence of the adsorption equilibrium constants on the solvent composition, (b) the number of equilibrium stages and (c) the specification of purity requirements is illustrated and discussed based on results of parametric calculations. The results achieved emphasize the potential of two-step gradient counter-current chromatography. PMID:12641280

  4. 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.

  5. [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.

  6. 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

    2016-01-01

    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.

  7. 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.

  8. Preparative isolation and purification of amides from the fruits of Piper longum L. by upright counter-current chromatography and reversed-phase liquid chromatography.

    PubMed

    Wu, Shihua; Sun, Cuirong; Pei, Saifeng; Lu, Yanbin; Pan, Yuanjiang

    2004-06-25

    A versatile counter-current chromatography (CCC) with upright type-J multilayer coil planet centrifuge, named upright CCC, was applied to the isolation and purification of amides from Piper longum L., which is widely used as an anodyne and a treatment for stomach disease in China. After the saponification by KOH of the ethanol extracts solution of 15 kg of crude drug "Piper Longi Fructus", the fruits of P. longum L., the solution was extracted with light petroleum and 500 g of red crude oil was obtained. Using 2.5 g of red crude oil as sample, the preparative upright 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, which yielded nine fractions. Then these fractions were further purified by use of reversed-phase liquid chromatography (RPLC) with a glass column of 500 x 10 mm i.d. packed with reversed-phase silica gel. As a result, nine target amides with over 95% purity, i.e., 50 mg of (2E,4E)-N-isobutyl-eicosa-2,4-dienamide, 150 mg of (2E,4E,14Z)-N-isobutyl-eicosa-2,4,14-trienamide, 110 mg of (2E,4E,12Z)-N-isobutyl-ocatadeca-2,4,12-trienamide, 50 mg of guineensine, 60 mg of pipernonaline, 75 mg of pellitorine, 63 mg of piperine, 45 mg of piperanine, and 40 mg of piperlonguminine were isolated, respectively. Structures of all compounds were identified by electrospray ionization MS, electron impact ionization MS, one- and two-dimensional NMR spectra.

  9. 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.

  10. A new rapid method for Clostridium difficile DNA extraction and detection in stool: toward point-of-care diagnostic testing.

    PubMed

    Freifeld, Alison G; Simonsen, Kari A; Booth, Christine S; Zhao, Xing; Whitney, Scott E; Karre, Teresa; Iwen, Peter C; Viljoen, Hendrik J

    2012-01-01

    We describe a new method for the rapid diagnosis of Clostridium difficile infection, with stool sample preparation and DNA extraction by heat and physical disruption in a single-use lysis microreactor (LMR), followed by a rapid PCR amplification step. All steps can be accomplished in <20 minutes overall. Gel electrophoresis is currently used to detect the amplification product, pending real-time availability with an ultra-rapid thermocycler. Compared with the dual enzyme immunoassay (EIA) screening test (C. diff Quik Chek Complete; Techlab, Blacksburg, VA), the novel LMR/PCR assay showed complete concordance with all glutamate dehydrogenase (GDH) results (GDH(+)/toxin(+), n = 48; GDH(-)/toxin(-), n = 81). All 69 stool samples with discordant EIA results (GDH(+)/toxin(-)) were tested by both the LMR/PCR assay and the loop-mediated isothermal amplification test (LAMP) (Illumigene C. difficile; Meridian Bioscience, Cincinnati, OH). In 64/69 EIA-discordant samples, LAMP and LMR/PCR results matched (both positive in 29 sample and both negative in 35 samples); in the remaining 5 samples, results were discrepant between the LAMP assay (all five negative) and the LMR/PCR assay (all 5 positive). Overall, LMR/PCR testing matched the current algorithm of EIA and/or LAMP reflex testing in 193/198 (97.5%) samples. The present proof-of-concept study suggests that the novel LMR/PCR technique described here may be developed as an inexpensive, rapid, and reliable point-of-care diagnostic test for C. difficile infection and other infectious diseases.

  11. A combined cesium-strontium extraction/recovery process

    SciTech Connect

    Horwitz, E.P.; Dietz, M.L.; Jensen, M.P.

    1996-03-01

    A new solvent extraction process for the simultaneous extraction of cesium and strontium from acidic nitrate media is described. This process uses a solvent formulation comprised of 0.05 M di-t-butylcyclohexano-18-crown-6 (DtBuCH18C6), 0.1 M Crown 100{prime} (a proprietary, cesium-selective derivative of dibenzo-18-crown-6), 1.2 M tributyl phosphate (TBP), and 5% (v/v) lauryl nitrile in an isoparaffinic hydrocarbon diluent. Distribution ratios for cesium and strontium from 4 M nitric acid are 4.13 and 3.46, respectively. A benchtop batch countercurrent extraction experiment indicates that >98% of the cesium and strontium initially present in the feed solution can be removed in only four extraction stages. Through proper choice of extraction and strip conditions, extracted cesium and strontium can be recovered either together or individually.

  12. Phytochemical Screening, Physicochemical Properties, Acute Toxicity Testing and Screening of Hypoglycaemic Activity of Extracts of Eremurus himalaicus Baker in Normoglycaemic Wistar Strain Albino Rats

    PubMed Central

    Mushtaq, Ahlam; Akbar, Seema; Zargar, Mohammad A.; Wali, Adil F.; Malik, Akhtar H.; Dar, Mohammad Y.; Hamid, Rabia; Ganai, Bashir A.

    2014-01-01

    In the present study EtOAc, MeOH, and aqueous extracts of Eremurus himalaicus were evaluated for hypoglycaemic effect in normal rats using both oral glucose tolerance test and 14-day oral administration study. Phytochemical and physicochemical screening was also done. In oral glucose tolerance test the aqueous and MeOH extracts of Eremurus himalaicus at a dose level of 500 mg/kg body weight prior to glucose load resulted in a significant fall in blood glucose level within 150 min. of glucose administration. The aqueous extract at a dose level of 250 mg/kg body weight and 500 mg/kg body weight also showed good hypoglycaemic response (P < 0.001); this was followed by MeOH extract at a dose level of 500 mg/kg body weight (P < 0.05), while MeOH extract at dose level of 250 mg/kg body weight and ethyl acetate extract at dose level of 250 mg/kg body weight and 500 mg/kg body weight exhibited insignificant effect. Phytochemical screening of extracts revealed the presence of alkaloids, terpenoids, phenolics, tannins, saponins, cardiac glycosides, and flavonoids. The results indicate that aqueous extract possess significant hypoglycaemic activity in normoglycaemic rats which may be attributed to the above-mentioned chemical constituents. PMID:24864262

  13. The effect of maxillary first premolar extraction and incisor retraction on mandibular position: testing the central dogma of "functional orthodontics".

    PubMed

    Luecke, P E; Johnston, L E

    1992-01-01

    It has been argued by a vocal coterie of disaffected dentists that premolar extraction, incisor retraction, and "backward-pulling" mechanics conspire to "distalize" the condyles and, pari passu, to produce craniomandibular dysfunction. Given the gravity of this conjecture, it seemed appropriate to test the predictions it generates in a sample of patients of the type most often said to be at risk: 42 "edgewise" patients with Class II, Division 1 malocclusions, treated in conjunction with the extraction of two maxillary first premolars. Regional and anterior cranial-base cephalometric superimpositions were used to quantify the individual components of the molar and overjet corrections, to measure both at the chin and condyles the mandibular displacement seen during treatment, and to examine the extent to which this displacement is related to the correction of maxillary incisor protrusion. Although the present patients underwent marked upper incisor retraction (on average, about 5 mm), lip retraction was much less pronounced, and 70% of the sample showed a net forward displacement of mandibular basal bone. Significantly, changes in condylar position were not correlated with incisor retraction, as the "functional orthodontists" would have it, but rather with the changes in the buccal occlusion and the growth of the maxilla. Thus, 30% of the patients who showed evidence of distal displacement were generally nongrowing patients who underwent more than average anchorage loss in the mandible and less than average loss in the maxilla.(ABSTRACT TRUNCATED AT 250 WORDS)

  14. Pore-water extraction from unsaturated tuff by triaxial and one-dimensional compression methods, Nevada Test Site, Nevada

    SciTech Connect

    Mower, T.E.; Higgins, J.D.; Yang, In C.; Peters, C.A.

    1994-07-01

    The hydrologic system in the unsaturated tuff at Yucca Mountain, Nevada, is being evaluated for the US Department of Energy by the Yucca Mountain Project Branch of the US Geological Survey as a potential site for a high-level radioactive-waste repository. Part of this investigation includes a hydrochemical study that is being made to assess characteristics of the hydrologic system such as: traveltime, direction of flow, recharge and source relations, and types and magnitudes of chemical reactions in the unsaturated tuff. In addition, this hydrochemical information will be used in the study of the dispersive and corrosive effects of unsaturated-zone water on the radioactive-waste storage canisters. This report describes the design and validation of laboratory experimental procedures for extracting representative samples of uncontaminated pore water from welded and nonwelded, unsaturated tuffs from the Nevada Test Site.

  15. Test plan for single well injection/extraction characterization of DNAPL

    SciTech Connect

    Looney, B.B.; Jerome, K.M.; Burdick, S.; Rossabi, J.; Jarosch, T.R.; Eddy-Dilek, C.A.

    1995-12-01

    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 the efficient characterization or removal of DNAPL are not currently proven. For example, most DNAPL studies rely on traditional soil and water sampling and the fortuitous observation of immiscible solvent. Once DNAPL is identified, soil excavation (which is only applicable to small contained spill sites) is the only ``proven`` cleanup method. New cleanup approaches based on enhanced removal by surfactants and/or alcohols have been proposed and tested at the pilot scale. As described below, carefully designed experiments similar to the enhanced removal methods may provide important characterization information on DNAPLs.

  16. Chiral High-Speed Counter-Current Chromatography: Future Strategies for Chiral Selector Development.

    PubMed

    Ma, Ying; Ito, Yoichiro

    2014-01-01

    In conventional high-performance liquid chromatography, chiral separations are performed by chiral column with a chiral selector (CS) chemically boned to the solid support. In contrast, high-speed counter-current chromatography (HSCCC) performs chiral separations by dissolving CS in the liquid stationary phase. During the past two decades, several CSs were developed to successfully carry out chiral HSCCC which include N-dodecanoyl-L-proline-3,5-dimethylanilide, β-cyclodextrin derivatives, vancomycin, cinchona alkaloid derivatives, cellulose and amylose derivatives, tartaric acid derivatives, etc. Compared to HPLC which uses over hundred different kinds of CSs, the number of CSs effectively used in HSCCC is limited to several compounds. This may be due to the violent molecular movement of CS dissolved in the liquid stationary phase which reduces chiral selectivity based on steric affinity. Future development strategy of CS for HSCC proposed here is to suppress the molecular movement of the CS in the liquid stationary phase by the following three ways: 1) using viscous stationary phase such as aqueous-aqueous polymer phase system; 2) attaching a long hydrophobic chain to the asymmetric carbon, or 3) chemically bonding CS onto hydrophobic small particles such as carbon nanotubes, gold colloidal particles, and submicron silica particles.

  17. Chiral High-Speed Counter-Current Chromatography: Future Strategies for Chiral Selector Development

    PubMed Central

    Ma, Ying; Ito, Yoichiro

    2014-01-01

    In conventional high-performance liquid chromatography, chiral separations are performed by chiral column with a chiral selector (CS) chemically boned to the solid support. In contrast, high-speed counter-current chromatography (HSCCC) performs chiral separations by dissolving CS in the liquid stationary phase. During the past two decades, several CSs were developed to successfully carry out chiral HSCCC which include N-dodecanoyl-L-proline-3,5-dimethylanilide, β-cyclodextrin derivatives, vancomycin, cinchona alkaloid derivatives, cellulose and amylose derivatives, tartaric acid derivatives, etc. Compared to HPLC which uses over hundred different kinds of CSs, the number of CSs effectively used in HSCCC is limited to several compounds. This may be due to the violent molecular movement of CS dissolved in the liquid stationary phase which reduces chiral selectivity based on steric affinity. Future development strategy of CS for HSCC proposed here is to suppress the molecular movement of the CS in the liquid stationary phase by the following three ways: 1) using viscous stationary phase such as aqueous-aqueous polymer phase system; 2) attaching a long hydrophobic chain to the asymmetric carbon, or 3) chemically bonding CS onto hydrophobic small particles such as carbon nanotubes, gold colloidal particles, and submicron silica particles. PMID:24611132

  18. Topsy-turvy: Turning the counter-current heat exchange of leatherback turtles upside down

    USGS Publications Warehouse

    Davenport, John; Jones, T. Todd; Work, Thierry M.; Balazs, George H.

    2015-01-01

    Counter-current heat exchangers associated with appendages of endotherms feature bundles of closely applied arteriovenous vessels. The accepted paradigm is that heat from warm arterial blood travelling into the appendage crosses into cool venous blood returning to the body. High core temperature is maintained, but the appendage functions at low temperature. Leatherback turtles have elevated core temperatures in cold seawater and arteriovenous plexuses at the roots of all four limbs. We demonstrate that plexuses of the hindlimbs are situated wholly within the hip musculature, and that, at the distal ends of the plexuses, most blood vessels supply or drain the hip muscles, with little distal vascular supply to, or drainage from the limb blades. Venous blood entering a plexus will therefore be drained from active locomotory muscles that are overlaid by thick blubber when the adults are foraging in cold temperate waters. Plexuses maintain high limb muscle temperature and avoid excessive loss of heat to the core, the reverse of the accepted paradigm. Plexuses protect the core from overheating generated by muscular thermogenesis during nesting.

  19. Continuous counter-current chromatography for capture and polishing steps in biopharmaceutical production.

    PubMed

    Steinebach, Fabian; Müller-Späth, Thomas; Morbidelli, Massimo

    2016-09-01

    The economic advantages of continuous processing of biopharmaceuticals, which include smaller equipment and faster, efficient processes, have increased interest in this technology over the past decade. Continuous processes can also improve quality assurance and enable greater controllability, consistent with the quality initiatives of the FDA. Here, we discuss different continuous multi-column chromatography processes. Differences in the capture and polishing steps result in two different types of continuous processes that employ counter-current column movement. Continuous-capture processes are associated with increased productivity per cycle and decreased buffer consumption, whereas the typical purity-yield trade-off of classical batch chromatography can be surmounted by continuous processes for polishing applications. In the context of continuous manufacturing, different but complementary chromatographic columns or devices are typically combined to improve overall process performance and avoid unnecessary product storage. In the following, these various processes, their performances compared with batch processing and resulting product quality are discussed based on a review of the literature. Based on various examples of applications, primarily monoclonal antibody production processes, conclusions are drawn about the future of these continuous-manufacturing technologies. PMID:27376629

  20. Preparative separation of five flavones from flowers of Polygonum cuspidatum by high-speed countercurrent chromatography.

    PubMed

    Sun, Yinshi; Gu, Shubo; Guo, Linlin; Xia, Xue; Zhang, Hong; Wang, Jianhua

    2014-07-01

    A preparative high-speed countercurrent chromatography method was successfully used for the isolation of five minor flavones from Polygonum cuspidatum flowers. Among them, three compounds were obtained from P. cuspidatum for the first time. A twin two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/water (1:6:3:6, v/v/v/v) and petroleum ether/ethyl acetate/methanol/water (2:4:3:3, v/v/v/v) was developed. Compounds were obtained from the fraction B and fraction C prepurified by silica gel column chromatography. Five minor compositions, 6.8 mg of hesperidin, 11.2 mg of phloridzin, 4.9 mg of luteolin, 5.3 mg of hyperin, and 3.7 mg of luteoloside were obtained from 140 mg of the fraction B and 110 mg of fraction C with a purity of 95.3, 96.4, 98.0, 96.8, and 95.3%, respectively, as determined by high-performance liquid chromatography. The structures of these compounds were identified by (1) H and (13) C NMR spectroscopy.

  1. Estimates of the zonal slope and seasonal transport of the Atlantic North Equatorial Countercurrent

    NASA Technical Reports Server (NTRS)

    Carton, James A.; Katz, Eli J.

    1990-01-01

    Data from six inverted echo sounder moorings and the Geosat satellite altimeter are used to examine the seasonal variability of sea surface elevation. Monthly sea level maps are constructed using a contemporaneous subsurface temperature survey to provide a reference sea level field. The maps are then used to describe the origin and structure of the western tropical Atlantic North Equatorial Countercurrent (NECC) during a two-year period beginning in November 1987. The data reveal a zonal current which is confined between 3 deg N and 9 deg N with a typical width of 300 km. The NECC flows strongly eastward during November and December 1986 and May 1987 through January 1988. The reappearance of the current is then delayed until August, but the current flows strongly from August until the end of the record in October 1988. Volume transport is estimated for the two-year period from surface elevation by approximating the vertical structure of the ocean as a two-layer fluid. It is found that the NECC has a maximum transport of 40 x 10 to the 6th cu m/s at 38 deg W.

  2. Preparative separation of five flavones from flowers of Polygonum cuspidatum by high-speed countercurrent chromatography.

    PubMed

    Sun, Yinshi; Gu, Shubo; Guo, Linlin; Xia, Xue; Zhang, Hong; Wang, Jianhua

    2014-07-01

    A preparative high-speed countercurrent chromatography method was successfully used for the isolation of five minor flavones from Polygonum cuspidatum flowers. Among them, three compounds were obtained from P. cuspidatum for the first time. A twin two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/water (1:6:3:6, v/v/v/v) and petroleum ether/ethyl acetate/methanol/water (2:4:3:3, v/v/v/v) was developed. Compounds were obtained from the fraction B and fraction C prepurified by silica gel column chromatography. Five minor compositions, 6.8 mg of hesperidin, 11.2 mg of phloridzin, 4.9 mg of luteolin, 5.3 mg of hyperin, and 3.7 mg of luteoloside were obtained from 140 mg of the fraction B and 110 mg of fraction C with a purity of 95.3, 96.4, 98.0, 96.8, and 95.3%, respectively, as determined by high-performance liquid chromatography. The structures of these compounds were identified by (1) H and (13) C NMR spectroscopy. PMID:24753452

  3. Topsy-turvy: turning the counter-current heat exchange of leatherback turtles upside down.

    PubMed

    Davenport, John; Jones, T Todd; Work, Thierry M; Balazs, George H

    2015-10-01

    Counter-current heat exchangers associated with appendages of endotherms feature bundles of closely applied arteriovenous vessels. The accepted paradigm is that heat from warm arterial blood travelling into the appendage crosses into cool venous blood returning to the body. High core temperature is maintained, but the appendage functions at low temperature. Leatherback turtles have elevated core temperatures in cold seawater and arteriovenous plexuses at the roots of all four limbs. We demonstrate that plexuses of the hindlimbs are situated wholly within the hip musculature, and that, at the distal ends of the plexuses, most blood vessels supply or drain the hip muscles, with little distal vascular supply to, or drainage from the limb blades. Venous blood entering a plexus will therefore be drained from active locomotory muscles that are overlaid by thick blubber when the adults are foraging in cold temperate waters. Plexuses maintain high limb muscle temperature and avoid excessive loss of heat to the core, the reverse of the accepted paradigm. Plexuses protect the core from overheating generated by muscular thermogenesis during nesting. PMID:26445982

  4. Topsy-turvy: turning the counter-current heat exchange of leatherback turtles upside down

    PubMed Central

    Davenport, John; Jones, T. Todd; Work, Thierry M.; Balazs, George H.

    2015-01-01

    Counter-current heat exchangers associated with appendages of endotherms feature bundles of closely applied arteriovenous vessels. The accepted paradigm is that heat from warm arterial blood travelling into the appendage crosses into cool venous blood returning to the body. High core temperature is maintained, but the appendage functions at low temperature. Leatherback turtles have elevated core temperatures in cold seawater and arteriovenous plexuses at the roots of all four limbs. We demonstrate that plexuses of the hindlimbs are situated wholly within the hip musculature, and that, at the distal ends of the plexuses, most blood vessels supply or drain the hip muscles, with little distal vascular supply to, or drainage from the limb blades. Venous blood entering a plexus will therefore be drained from active locomotory muscles that are overlaid by thick blubber when the adults are foraging in cold temperate waters. Plexuses maintain high limb muscle temperature and avoid excessive loss of heat to the core, the reverse of the accepted paradigm. Plexuses protect the core from overheating generated by muscular thermogenesis during nesting. PMID:26445982

  5. Effect of Coriolis force on counter-current chromatographic separation by centrifugal partition chromatography.

    PubMed

    Ikehata, Jun-Ichi; Shinomiya, Kazufusa; Kobayashi, Koji; Ohshima, Hisashi; Kitanaka, Susumu; Ito, Yoichiro

    2004-02-01

    The effect of Coriolis force on the counter-current chromatographic separation was studied using centrifugal partition chromatography (CPC) with four different two-phase solvent systems including n-hexane-acetonitrile (ACN); tert-butyl methyl ether (MtBE)-aqueous 0.1% trifluoroacetic acid (TFA) (1:1); MtBE-ACN-aqueous 0.1% TFA (2:2:3); and 12.5% (w/w) polyethylene glycol (PEG) 1000-12.5% (w/w) dibasic potassium phosphate. Each separation was performed by eluting either the upper phase in the ascending mode or the lower phase in the descending mode, each in clockwise (CW) and counterclockwise column rotation. Better partition efficiencies were attained by the CW rotation in both mobile phases in all the two-phase solvent systems examined. The mathematical analysis also revealed the Coriolis force works favorably under the CW column rotation for both mobile phases. The overall results demonstrated that the Coriolis force produces substantial effects on CPC separation in both organic-aqueous and aqueous-aqueous two-phase systems.

  6. Continuous hydrolysis of oil by immobilized lipase in a countercurrent reactor.

    PubMed

    Kosugi, Y; Tanaka, H; Tomizuka, N

    1990-09-01

    Lipase from Pseudomonas fluorescens biotype I was immobilized by adsorption of anion exchange resin using glutaraldehyde to enhance the adsorption. The activity yield of the immobilized lipase was very low (below 1%) when lipase activity was measured using emulsion substrate. The activity yield was 10-70% when lipase activity was measured using non-emulsion substrate. Countercurrent reactors for hydrolysis of oil using non-emulsion substrate were studied. A fluidized bed reactor was found to be superior to a fixed bed one since in a fixed bed reactor the separation rate of the two layers was slow and the flow rate of the reactor had to be slower than the separation rate. A fluidized bed reactor system equipped with settling compartments and stirring compartments was devised. Continuous lipolysis at 60 degrees C and continuous separation of oily product and water soluble product were performed. After continuous operation for more than 3 months, 70% of the initial activity of the immobilized lipase was observed at the end of the reaction.

  7. Development and Validation of Extract the Base: An English Derivational Morphology Test for Third through Fifth Grade Monolingual Students and Spanish-Speaking English Language Learners

    ERIC Educational Resources Information Center

    Goodwin, Amanda P.; Huggins, A. Corinne; Carlo, Maria; Malabonga, Valerie; Kenyon, Dorry; Louguit, Mohammed; August, Diane

    2012-01-01

    This study describes the development and validation of the Extract the Base test (ETB), which assesses derivational morphological awareness. Scores on this test were validated for 580 monolingual students and 373 Spanish-speaking English language learners (ELLs) in third through fifth grade. As part of the validation of the internal structure,…

  8. Improving Toxicity Assessment of Pesticide Mixtures: The Use of Polar Passive Sampling Devices Extracts in Microalgae Toxicity Tests

    PubMed Central

    Kim Tiam, Sandra; Fauvelle, Vincent; Morin, Soizic; Mazzella, Nicolas

    2016-01-01

    Complexity of contaminants exposure needs to be taking in account for an appropriate evaluation of risks related to mixtures of pesticides released in the ecosystems. Toxicity assessment of such mixtures can be made through a variety of toxicity tests reflecting different level of biological complexity. This paper reviews the recent developments of passive sampling techniques for polar compounds, especially Polar Organic Chemical Integrative Samplers (POCIS) and Chemcatcher® and the principal assessment techniques using microalgae in laboratory experiments. The progresses permitted by the coupled use of such passive samplers and ecotoxicology testing as well as their limitations are presented. Case studies combining passive sampling devices (PSD) extracts and toxicity assessment toward microorganisms at different biological scales from single organisms to communities level are presented. These case studies, respectively, aimed (i) at characterizing the “toxic potential” of waters using dose-response curves, and (ii) at performing microcosm experiments with increased environmental realism in the toxicant exposure in term of cocktail composition and concentration. Finally perspectives and limitations of such approaches for future applications in the area of environmental risk assessment are discussed. PMID:27667986

  9. Improving Toxicity Assessment of Pesticide Mixtures: The Use of Polar Passive Sampling Devices Extracts in Microalgae Toxicity Tests.

    PubMed

    Kim Tiam, Sandra; Fauvelle, Vincent; Morin, Soizic; Mazzella, Nicolas

    2016-01-01

    Complexity of contaminants exposure needs to be taking in account for an appropriate evaluation of risks related to mixtures of pesticides released in the ecosystems. Toxicity assessment of such mixtures can be made through a variety of toxicity tests reflecting different level of biological complexity. This paper reviews the recent developments of passive sampling techniques for polar compounds, especially Polar Organic Chemical Integrative Samplers (POCIS) and Chemcatcher® and the principal assessment techniques using microalgae in laboratory experiments. The progresses permitted by the coupled use of such passive samplers and ecotoxicology testing as well as their limitations are presented. Case studies combining passive sampling devices (PSD) extracts and toxicity assessment toward microorganisms at different biological scales from single organisms to communities level are presented. These case studies, respectively, aimed (i) at characterizing the "toxic potential" of waters using dose-response curves, and (ii) at performing microcosm experiments with increased environmental realism in the toxicant exposure in term of cocktail composition and concentration. Finally perspectives and limitations of such approaches for future applications in the area of environmental risk assessment are discussed.

  10. Semi-Technical Cryogenic Molecular Sieve Bed for the Tritium Extraction System of the Test Blanket Module for ITER

    SciTech Connect

    Beloglazov, S.; Bekris, N.; Glugla, M.; Wagner, R.

    2005-07-15

    The tritium extraction from the ITER Helium Cooled Pebble Bed (HCPB) Test Blanket Module purge gas is proposed to be performed in a two steps process: trapping water in a cryogenic Cold Trap, and adsorption of hydrogen isotopes (H{sub 2}, HT, T{sub 2}) as well as impurities (N{sub 2}, O{sub 2}) in a Cryogenic Molecular Sieve Bed (CMSB) at 77K. A CMSB in a semi-technical scale (one-sixth of the flow rate of the ITER-HCPB) was design and constructed at the Forschungszentrum Karlsruhe. The full capacity of CMSB filled with 20 kg of MS-5A was calculated based on adsorption isotherm data to be 9.4 mol of H{sub 2} at partial pressure 120 Pa. The breakthrough tests at flow rates up to 2 Nm{sup 3}h{sup -1} of He with 110 Pa of H{sub 2} conformed with good agreement the adsorption capacity of the CMSB. The mass-transfer zone was found to be relatively narrow (12.5 % of the MS Bed height) allowing to scale up the CMSB to ITER flow rates.

  11. Improving Toxicity Assessment of Pesticide Mixtures: The Use of Polar Passive Sampling Devices Extracts in Microalgae Toxicity Tests

    PubMed Central

    Kim Tiam, Sandra; Fauvelle, Vincent; Morin, Soizic; Mazzella, Nicolas

    2016-01-01

    Complexity of contaminants exposure needs to be taking in account for an appropriate evaluation of risks related to mixtures of pesticides released in the ecosystems. Toxicity assessment of such mixtures can be made through a variety of toxicity tests reflecting different level of biological complexity. This paper reviews the recent developments of passive sampling techniques for polar compounds, especially Polar Organic Chemical Integrative Samplers (POCIS) and Chemcatcher® and the principal assessment techniques using microalgae in laboratory experiments. The progresses permitted by the coupled use of such passive samplers and ecotoxicology testing as well as their limitations are presented. Case studies combining passive sampling devices (PSD) extracts and toxicity assessment toward microorganisms at different biological scales from single organisms to communities level are presented. These case studies, respectively, aimed (i) at characterizing the “toxic potential” of waters using dose-response curves, and (ii) at performing microcosm experiments with increased environmental realism in the toxicant exposure in term of cocktail composition and concentration. Finally perspectives and limitations of such approaches for future applications in the area of environmental risk assessment are discussed.

  12. Distribution of Plasmodium species on the island of Grande Comore on the basis of DNA extracted from rapid diagnostic tests.

    PubMed

    Papa Mze, Nasserdine; Ahouidi, Ambroise D; Diedhiou, Cyrille K; Silai, Rahamatou; Diallo, Mouhamadou; Ndiaye, Daouda; Sembene, Mbacké; Mboup, Souleymane

    2016-01-01

    In the Union of Comoros, interventions for combating malaria have contributed to a spectacular decrease in the prevalence of the disease. We studied the current distribution of Plasmodium species on the island of Grande Comore using nested PCR. The rapid diagnostic tests (RDTs) currently used in the Comoros are able to identify Plasmodium falciparum but no other Plasmodium species. In this study, we tested 211 RDTs (158 positive and 53 negative). Among the 158 positive RDTs, 22 were positive for HRP2, 3 were positive only for pLDH, and 133 were positive for HRP2 and pLDH. DNA was extracted from a proximal part of the nitrocellulose membrane of RDTs. A total of 159 samples were positive by nested PCR. Of those, 156 (98.11%) were positive for P. falciparum, 2 (1.25%) were positive for P. vivaxI, and 1 (0.62%) was positive for P. malariae. None of the samples were positive for P. ovale. Our results show that P. falciparum is still the most dominant species on the island of Grande Comore, but P. vivax and P. malariae are present at a low prevalence. PMID:27561250

  13. Improving Toxicity Assessment of Pesticide Mixtures: The Use of Polar Passive Sampling Devices Extracts in Microalgae Toxicity Tests.

    PubMed

    Kim Tiam, Sandra; Fauvelle, Vincent; Morin, Soizic; Mazzella, Nicolas

    2016-01-01

    Complexity of contaminants exposure needs to be taking in account for an appropriate evaluation of risks related to mixtures of pesticides released in the ecosystems. Toxicity assessment of such mixtures can be made through a variety of toxicity tests reflecting different level of biological complexity. This paper reviews the recent developments of passive sampling techniques for polar compounds, especially Polar Organic Chemical Integrative Samplers (POCIS) and Chemcatcher® and the principal assessment techniques using microalgae in laboratory experiments. The progresses permitted by the coupled use of such passive samplers and ecotoxicology testing as well as their limitations are presented. Case studies combining passive sampling devices (PSD) extracts and toxicity assessment toward microorganisms at different biological scales from single organisms to communities level are presented. These case studies, respectively, aimed (i) at characterizing the "toxic potential" of waters using dose-response curves, and (ii) at performing microcosm experiments with increased environmental realism in the toxicant exposure in term of cocktail composition and concentration. Finally perspectives and limitations of such approaches for future applications in the area of environmental risk assessment are discussed. PMID:27667986

  14. Cost-effective monitoring for a soil vapor extraction (SVE) system: a simplified modeling and gas sensor test.

    PubMed

    Yang, J W; Cho, H J; Choi, G Y; Lee, S H

    2001-07-01

    In order to establish cost-effective monitoring strategies for soil vapor extraction (SVE), a simplified model for multi-component mass transfer of a complex liquid mixture in porous media and gas sensor are proposed and experimentally evaluated. The basic task for the cost-effective monitoring of SVE is to decide how to predict the performances of venting systems in terms of the contaminant vapor removal rate and the time required to accomplish the clean-up specification. The method includes classifying of individual components of a complex mixture on the basis of gas chromatographic (GC) profile and treating each resulting group as a pseudo-single compound. BTEX components of gasoline were selected for model input and the remainders were divided into 4 groups based on their GC retention times. The model proposed in this study is capable of predicting with accuracy volatilization behaviors of gasoline components in soil and the gas sensor (FIGARO TGS 823) was tested by GC-FID to toluene and TPH-GRO(Total Petroleum Hydrocarbon-Gasoline Range Organics) gas samples. A VOC gas sensor was developed which recognizes TPH-GRO concentrations between 250 and 50 ppm. The developed gas sensor test and proposed model can be used as a valuable tool for the cost-effective monitoring for SVE systems. PMID:11516014

  15. Distribution of Plasmodium species on the island of Grande Comore on the basis of DNA extracted from rapid diagnostic tests

    PubMed Central

    Papa Mze, Nasserdine; Ahouidi, Ambroise D.; Diedhiou, Cyrille K.; Silai, Rahamatou; Diallo, Mouhamadou; Ndiaye, Daouda; Sembene, Mbacké; Mboup, Souleymane

    2016-01-01

    In the Union of Comoros, interventions for combating malaria have contributed to a spectacular decrease in the prevalence of the disease. We studied the current distribution of Plasmodium species on the island of Grande Comore using nested PCR. The rapid diagnostic tests (RDTs) currently used in the Comoros are able to identify Plasmodium falciparum but no other Plasmodium species. In this study, we tested 211 RDTs (158 positive and 53 negative). Among the 158 positive RDTs, 22 were positive for HRP2, 3 were positive only for pLDH, and 133 were positive for HRP2 and pLDH. DNA was extracted from a proximal part of the nitrocellulose membrane of RDTs. A total of 159 samples were positive by nested PCR. Of those, 156 (98.11%) were positive for P. falciparum, 2 (1.25%) were positive for P. vivaxI, and 1 (0.62%) was positive for P. malariae. None of the samples were positive for P. ovale. Our results show that P. falciparum is still the most dominant species on the island of Grande Comore, but P. vivax and P. malariae are present at a low prevalence. PMID:27561250

  16. Green tea extract decreases starch digestion and absorption from a test meal in humans: a randomized, placebo-controlled crossover study.

    PubMed

    Lochocka, Klaudia; Bajerska, Joanna; Glapa, Aleksandra; Fidler-Witon, Ewa; Nowak, Jan K; Szczapa, Tomasz; Grebowiec, Philip; Lisowska, Aleksandra; Walkowiak, Jaroslaw

    2015-07-30

    Green tea is known worldwide for its beneficial effects on human health. However, objective data evaluating this influence in humans is scarce. The aim of the study was to assess the impact of green tea extract (GTE) on starch digestion and absorption. The study comprised of 28 healthy volunteers, aged 19 to 28 years. In all subjects, a starch (13)C breath test was performed twice. Subjects randomly ingested naturally (13)C-abundant cornflakes during the GTE test (GTE 4 g) or placebo test. The cumulative percentage dose recovery (CPDR) was significantly lower for the GTE test than for the placebo test (median [interquartile range]: 11.4% [5.5-15.5] vs. 16.1% [12.7-19.5]; p = 0.003). Likewise, CPDR expressed per hour was considerably lower in each point of the measurement. In conclusion, a single dose of green tea extract taken with a test meal decreases starch digestion and absorption.

  17. Effect of fenugreek seeds extract on cyclophosphamide-induced histomorphometrical, ultrastructural and biochemical changes in testes of albino mice.

    PubMed

    Sakr, Saber A; Mahran, Hoda A; Abo-El-Yazid, Samah M

    2012-04-01

    Cyclophosphamide (CPA) is an anticancer drug used in the treatment of a variety of neoplastic lesions. On the other hand, treatment with CPA was accompanied by different toxic effects on different body organs. The present work was conducted to study the effect of fenugreek seed extract on histomorphometrical and ultrastructural changes induced by CPA in testes of albino mice. Twenty animals were given CPA (7.0 mg/kg body weight) three times/week orally for 8 weeks and were killed after 4 and 8 weeks. Testis of CPA-treated mice showed many histological alterations including appearance of irregular seminiferous tubules, reduction in the number of all spermatogenic cells, degeneration of Leydig cells and appearance of intertubular hemorrhage. Concerning the ultrastructural changes, abnormalities in spermatogonia (A and B), spermatocytes, round and elongated spermatids were observed. Degenerated Sertoli cells and degenerated interstitial tissue with abnormal Leydig cells were also seen. Moreover, administration of CPA to animals significantly increased malondialdehyde (MDA, lipid peroxidation marker) and decreased superoxide dismutase (SOD) and catalase (CAT). These changes were time-dependent. Treating animals with CPA and fenugreek seed extract (0.4 g/kg body weight) led to an improvement in the histological and ultrastructural pictures of the testis together with reduction in the level of serum MDA and increase in the activities of serum SOD and CAT. In conclusion, the results of the present work indicated that fenugreek had ameliorative effect against testis damage induced by CPA and this may be mediated by its potent antioxidant activities.

  18. Isolation of antioxidants from Psoralea corylifolia fruits using high-speed counter-current chromatography guided by thin layer chromatography-antioxidant autographic assay.

    PubMed

    Xiao, Guodong; Li, Guowen; Chen, Liang; Zhang, Zijia; Yin, Jun-Jie; Wu, Tao; Cheng, Zhihong; Wei, Xiaohui; Wang, Zhengtao

    2010-08-20

    A combinative method using high-speed counter-current chromatography (HSCCC) and thin layer chromatography (TLC) as an antioxidant autographic assay was developed to separate antioxidant components from the fruits of Psoralea corylifolia. Under the guidance of TLC bioautography, eight compounds including five flavonoids and three coumarins were successfully separated from the fruits of P. corylifolia by HSCCC with an optimized two-phase solvent system, n-hexane-ethyl acetate-methanol-water (1:1.1:1.3:1, v/v/v/v). The separation produced 5.91mg psoralen, 6.26mg isopsoralen, 3.19mg psoralidin, 0.92mg corylifol A, and 2.43mg bavachinin with corresponding purities of 99.5, 99.8, 99.4, 96.4, and 99.0%, as well as three sub-fractions, in a single run from 250mg ethyl acetate fraction of P. corylifolia extract. Following an additional clean-up step by preparative TLC, 0.4mg 8-prenyldaidzein (purity 91.7%), 4.18mg neobavaisoflavone (purity 97.4%) and 4.36mg isobavachalcone (purity 96.8%) were separated from the three individual sub-fractions. The structures of the isolated compounds were identified by (1)H NMR and (13)C NMR. The results of antioxidant activity estimation by electron spin resonance (ESR) method showed that psoralidin was the most active antioxidant with an IC50 value of 44.7microM. This is the first report on simultaneous separation of eight compounds from P. corylifolia by HSCCC.

  19. Determination of Alternaria mycotoxins in wine and juice using ionic liquid modified countercurrent chromatography as a pretreatment method followed by high-performance liquid chromatography.

    PubMed

    Fan, Chen; Cao, Xueli; Liu, Man; Wang, Wei

    2016-03-01

    Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples.

  20. Preparative isolation and purification of flavone compounds from sophora japonica L. by high-speed counter-current chromatography combined with macroporous resin column separation.

    PubMed

    Sun, Ailing; Sun, Qinghua; Liu, Renmin

    2007-05-01

    High-speed counter-current chromatography combined with macroporous resin column separation was applied to the isolation and purification of genistein-7,4'-di-O-beta-D-glucoside (I), genistein-7-O-beta-D-glucopyranoside-4'-O-[(alpha-L-rhamnopyransoyl)-(1-2)-beta-D-glucopyranoside] (II), kaempferol-3-O-beta-D-sophoroside(III), quercetin-3-O-beta-L-ramnopyranosyl-(1 - 6)-beta-D-glucopyranoside (IV), genistein-4'-beta-L-rhamnopyransoyl-(1 - 2)-alpha-D-glucopyranoside (V), and kaempferol-3-O-beta-L-ramnopyranosyl-(1 - 6)-beta-D-glucopyranoside (VI) from the Chinese medicinal herb Sophora japonica L. The crude extracts from the pericarps of Sophora japonica L. were pre-separated on a D-101 macroporous resin column and divided into two parts as sample 1 and sample 2. An 80-mg portion of sample 1 was separated by using n-butanol-acetic acid (1%) (5:5, v/v) as the two-phase solvent system and yielded 30.1 mg of compound I, 23.3 mg of compound II. A 120 mg portion of sample 2 was separated by using ethyl acetate-n-butanol-acetic acid (1%) (5:0.8:5, v/v) as the two-phase solvent system and yielded 5.5 mg of compound III, 31.7 mg of compound IV, 37.4 mg of compound V, and 6.2 mg of compound VI. The purities of compounds I, II, III, IV, V, and VI were 98.7, 98.2, 97.8, 98.5, 99.3, and 98.9%, respectively, as determined by HPLC. The chemical structures of these components were identified by 1H-NMR and 13C-NMR. PMID:17566335

  1. Preparative isolation of novel antioxidant flavonoids of alfalfa by stop-and-go counter-current chromatography and following on-line liquid chromatography desalination.

    PubMed

    Liang, Junling; Yang, Zhi; Cao, Xiaoji; Wu, Bing; Wu, Shihua

    2011-09-01

    In this work, we have established a new stop-and-go two-dimensional chromatography coupling of counter-current chromatography and liquid chromatography (2D CCC × LC) for the preparative separation of two novel antioxidant flavonoids from the extract of alfalfa (Medicago sativa L.). The CCC column has been used as the first dimension to purify the target flavonoids using a solvent system of isopropanol and 20% sodium chloride aqueous solution (1:1, v/v) with the stop-and-go flow technique, and the LC column packed with macroporous resin has been employed as the second dimension for on-line absorption, desalination and desorption of the targeting effluents purified from the first CCC dimension. As a result, two novel flavonoids, 6,8-dihydroxy-flavone-7-O-β-D-glucuronide (15.3 mg) and 6-methoxy-8-hydroxy-flavone-7-O-β-D-glucuronide (13.7 mg), have been isolated from 126.8 mg of crude sample pre-enriched by macroporous resin column. Their structures have been identified by electrospray ionization mass spectrometry (ESI-MS), electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) and one- and two-dimensional nuclear magnetic resonance spectra (1D and 2D NMR). Further antioxidant assays showed that the first component possess a strong antioxidant activity. All the results demonstrated that the stop-and-go 2D CCC × LC method is very efficient for the separation of flavonoids of alfalfa and it can also be applied to isolate other comprehensive multi-component natural products.

  2. Preparative isolation of novel antioxidant flavonoids of alfalfa by stop-and-go counter-current chromatography and following on-line liquid chromatography desalination.

    PubMed

    Liang, Junling; Yang, Zhi; Cao, Xiaoji; Wu, Bing; Wu, Shihua

    2011-09-01

    In this work, we have established a new stop-and-go two-dimensional chromatography coupling of counter-current chromatography and liquid chromatography (2D CCC × LC) for the preparative separation of two novel antioxidant flavonoids from the extract of alfalfa (Medicago sativa L.). The CCC column has been used as the first dimension to purify the target flavonoids using a solvent system of isopropanol and 20% sodium chloride aqueous solution (1:1, v/v) with the stop-and-go flow technique, and the LC column packed with macroporous resin has been employed as the second dimension for on-line absorption, desalination and desorption of the targeting effluents purified from the first CCC dimension. As a result, two novel flavonoids, 6,8-dihydroxy-flavone-7-O-β-D-glucuronide (15.3 mg) and 6-methoxy-8-hydroxy-flavone-7-O-β-D-glucuronide (13.7 mg), have been isolated from 126.8 mg of crude sample pre-enriched by macroporous resin column. Their structures have been identified by electrospray ionization mass spectrometry (ESI-MS), electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) and one- and two-dimensional nuclear magnetic resonance spectra (1D and 2D NMR). Further antioxidant assays showed that the first component possess a strong antioxidant activity. All the results demonstrated that the stop-and-go 2D CCC × LC method is very efficient for the separation of flavonoids of alfalfa and it can also be applied to isolate other comprehensive multi-component natural products. PMID:21092976

  3. Solvent system selectivities in countercurrent chromatography using Salicornia gaudichaudiana metabolites as practical example with off-line electrospray mass-spectrometry injection profiling.

    PubMed

    Costa, Fernanda das Neves; Jerz, Gerold; Figueiredo, Fabiana de Souza; Winterhalter, Peter; Leitão, Gilda Guimarães

    2015-03-13

    For the development of an efficient two-stage isolation process for high-speed countercurrent chromatography (HSCCC) with focus on principal metabolites from the ethyl acetate extract of the halophyte plant Salicornia gaudichaudiana, separation selectivities of two different biphasic solvent systems with similar polarities were evaluated using the elution and extrusion approach. Efficiency in isolation of target compounds is determined by the solvent system selectivity and their chronological use in multiple separation steps. The system n-hexane-ethyl acetate-methanol-water (0.5:6:0.5:6, v/v/v/v) resulted in a comprehensive separation of polyphenolic glycosides. The system n-hexane-n-butanol-water (1:1:2, v/v/v) was less universal but was highly efficient in the fractionation of positional isomers such as di-substituted cinnamic acid quinic acid derivatives. Multiple metabolite detection performed on recovered HSCCC tube fractions was done with rapid mass-spectrometry profiling by sequential off-line injections to electrospray mass-spectrometry (ESI-MS/MS). Selective ion traces of metabolites delivered reconstituted preparative HSCCC runs. Molecular weight distribution of target compounds in single HSCCC tube fractions and MS/MS fragment data were available. Chromatographic areas with strong co-elution effects and fractions of pure recoverable compounds were visualized. In total 11 metabolites have been identified and monitored. Result of this approach was a fast isolation protocol for S. gaudichaudiana metabolites using two solvent systems in a strategic sequence. The process could easily be scaled-up to larger lab-scale or industrial recovery.

  4. Tests on the extracted current density of negative hydrogen ions from a single element of the matrix source

    SciTech Connect

    Lishev, St.; Yordanov, D. Shivarova, A.

    2015-04-08

    Concepts for the extraction of volume-produced negative hydrogen ions from a rf matrix source (a matrix of small-radius discharges with a planar-coil inductive driving) are presented and discussed based on experimental results for the current densities of the extracted ions and the co-extracted electrons. The experiment has been carried out in a single discharge of the source: a rf discharge with a radius of 2.25 cm inductively driven by a 3.5-turn planar coil. The length of the discharge tube, the area of the reference electrode inserted in the discharge volume, the discharge modes, the magnetic filter and its position along the discharge length, the position of the permanent magnets for the separation of the co-extracted electrons from the extracted ions in the extraction device and the bias applied to its first electrode are considered as factors influencing the extracted currents of negative ions.

  5. Use of a new enzyme extraction system to improve the sensitivity of SOS/umu test and application to environmental samples.

    PubMed

    Tian, Zhe; Oda, Yoshimitsu; Zhang, Yu; Yang, Min; Li, Hongyan

    2015-03-01

    The purpose of this study was to find a better enzyme extraction reagent for the SOS/umu test to replace the conventional one (the combination of sodium dodecyl sulfate (SDS) and Z-buffer), which has the disadvantage of denaturing β-galactosidase leading to decreased measurement sensitivity. By adopting a microplate system, the performance of the umu test using BugBuster Master Mix, a commercially available enzyme extraction reagent, was compared with that using the conventional reagent for detecting the genotoxicity of known mutagens as well as environmental samples. BugBuster Master Mix was found to increase the detection sensitivities of the selected genotoxins and environmental water samples, due to the fact that it doesn't denature β-galactosidase. The result of this study showed that BugBuster Master Mix could be a better enzyme extraction reagent for umu test. PMID:25542254

  6. Use of a new enzyme extraction system to improve the sensitivity of SOS/umu test and application to environmental samples.

    PubMed

    Tian, Zhe; Oda, Yoshimitsu; Zhang, Yu; Yang, Min; Li, Hongyan

    2015-03-01

    The purpose of this study was to find a better enzyme extraction reagent for the SOS/umu test to replace the conventional one (the combination of sodium dodecyl sulfate (SDS) and Z-buffer), which has the disadvantage of denaturing β-galactosidase leading to decreased measurement sensitivity. By adopting a microplate system, the performance of the umu test using BugBuster Master Mix, a commercially available enzyme extraction reagent, was compared with that using the conventional reagent for detecting the genotoxicity of known mutagens as well as environmental samples. BugBuster Master Mix was found to increase the detection sensitivities of the selected genotoxins and environmental water samples, due to the fact that it doesn't denature β-galactosidase. The result of this study showed that BugBuster Master Mix could be a better enzyme extraction reagent for umu test.

  7. Inhibitory Effect of Aqueous Extract of Stem Bark of Cissus populnea on Ferrous Sulphate- and Sodium Nitroprusside-Induced Oxidative Stress in Rat's Testes In Vitro

    PubMed Central

    Akomolafe, Seun F.; Oboh, Ganiyu; Akindahunsi, Afolabi A.; Akinyemi, Ayodele J.; Tade, Oluwatosin G.

    2013-01-01

    Cissus populnea are plants associated with a myriad of medicinal uses in different parts of the world and are good sources of carotenoids, triterpenoids, and ascorbic acid. The antioxidant properties and inhibitory effect of water extractible phytochemicals from stem bark of C. populnea on FeSO4 and sodium nitroprusside- (SNP-) induced lipid peroxidation in rat testes were investigated in vitro. The results revealed that the extract was able to scavenge DPPH radical, chelate Fe2+ and also had a high reducing power. Furthermore, the incubation of the testes tissue homogenate in the presence of FeSO4 and SNP, respectively, caused a significant increase in the malondialdehyde (MDA) contents of the testes. However, the aqueous extract of the stem bark of C. populnea caused a significant decrease in the MDA contents of both Fe2+ (EC50 = 0.027 mg/mL) and SNP- (EC50 = 0.22 mg/mL) induced lipid peroxidation in the rat testes homogenates in a dose-dependent manner. The water extractible phytochemicals from C. populnea protect the testes from oxidative stress and this could be attributed to their high antioxidant activity: DPPH-scavenging ability, Fe2+-chelating and -reducing power. Therefore, oxidatively stress in testes could be potentially managed/prevented by this plant. PMID:23401792

  8. In vitro induction of polyploidy and chromatid exchanges by culture medium extracts of natural rubbers compounded with 2-mercaptobenzothiazole as a positive control candidate for genotoxicity tests.

    PubMed

    Matsuoka, Atsuko; Isama, Kazuo; Tsuchiya, Toshie

    2005-11-01

    We tested extracts of custom-made natural rubber samples for cytotoxicity using V79 cells and for chromosome aberration (CA) induction using CHL cells in compliance with the Japanese guidelines for basic biological tests of medical materials and devices. The samples were formulated with a high level of 2-mercaptobenzothiazole (MBT) (A); a low level of MBT (B); or zinc dibutyldithiocarbamate (ZDBC) (C). In the CA test, MBT induced mainly polyploidy, including endoreduplication, and ZDBC induced structural CAs. In the cytotoxicity test, culture medium extracts of A, B, and C suppressed colony formation to 50% of the control value at 53.1%, 94.3%, and >100%, respectively. Culture medium extracts of sample A induced polyploidy and structural CAs in the absence of an exogenous metabolic activation system (S9 mix), but at lower concentrations in its presence, indicating the existence of other leachable promutagens. The extracts of sample B induced structural CAs at the highest concentration and only with S9 mix. Sample C was negative. The facts suggest that sample A may be a candidate for a positive control for genotoxicity tests. The high frequency of polyploidy induced by sample A was not predicted by MBT, suggesting the usefulness of the test for safety evaluation of medical devices. Numerical CAs induced by MBT and sample A are discussed. PMID:16088893

  9. Evaluation of a rat model versus a physiologically based extraction test for assessing phenanthrene bioavailability from soils.

    PubMed

    Pu, Xinzhu; Lee, Linda S; Galinsky, Raymond E; Carlson, Gary P

    2004-05-01

    The soil matrix can impact the bioavailability of soil-bound organic chemicals, and this impact is governed in part by soil properties such as organic carbon (OC) content, clay minerals, and pH. Recently, a physiologically based extraction test (PBET) was developed to predict the bioavailability of soil-bound organic chemicals. In the current study, the bioavailability of phenanthrene (PA) from laboratory-treated soils varying in OC content, clay, and pH was investigated using an in vivo rat model and an in vitro PBET. The relationship between these two approaches was also examined. In the in vivo assay, soils and corn oil containing equivalent levels of PA were administered to Sprague-Dawley rats by gavage at two dose levels: 400 and 800 mg/kg body weight. Equivalent doses were given via intravenous injection (i.v.). The areas under the blood concentration-versus-time curves (AUC) were measured, and the absolute and relative bioavailabilities of PA were determined for each soil. In the PBET tests, one g of each soil was extracted by artificial saliva, gastric juice, duodenum juice, and bile. The fraction of PA mobilized from each soil was quantified. The AUCs of PA in all soils were significantly lower than those following iv injection (p < 0.05), indicating that the soil matrix could reduce the bioavailability of PA from soil. There were obvious trends of soils with higher OC content and clay content, resulting in the lower bioavailability of PA from soil. A significant correlation (p < 0.05) was observed between the fraction of PA mobilized from soil in the PBET and its in vivo bioavailability. The data also showed that the absolute bioavailability of PA from corn oil was low: approximately 25%. These results suggest that PBET assay might be a useful alternative in predicting bioavailability of soil-bound organic chemicals. However, due to the limited soil types and use of one chemical vs. a variety of contaminants and soil properties in the environment, further

  10. Post-treatment with plant extracts used in Brazilian folk medicine caused a partial reversal of the antiproliferative effect of glyphosate in the Allium cepa test.

    PubMed

    Frescura, Viviane Dal-Souto; Kuhn, Andrielle Wouters; Laughinghouse, Haywood Dail; Paranhos, Juçara Terezinha; Tedesco, Solange Bosio

    2013-08-01

    Species of the genus Psychotria are used for multiple purposes in Brazilian folk medicine, either as water infusions, baths or poultices. This study was aimed to evaluate the genotoxic and antiproliferative effects of infusions of Psychotria brachypoda and P. birotula on the Allium cepa test. Exposure to distilled water was used as a negative control, while exposure to glyphosate was used as a positive control. The interaction of extracts (as a post-treatment) with the effects of glyphosate was also studied. Results showed that glyphosate and the extracts of both P. brachypoda and P. birotula reduced the mitotic index as compared with the negative control (distilled water). Surprisingly, however, both extracts from P. brachypoda and P. birotula caused a partial reversal of the antiproliferative effect of glyphosate when used as a post-treatment. Glyphosate also induced the highest number of cells with chromosomal alterations, which was followed by that of P. birotula extracts. However, the extracts from P. brachypoda did not show any significant genotoxic effect. Post-treatment of glyphosate-treated samples with distilled water allowed a partial recovery of the genotoxic effect of glyphosate, and some of the Psychotria extracts also did so. Notably, post-treatment of glyphosate-treated samples with P. brachypoda extracts induced a statistically significant apoptotic effect. It is concluded that P. brachypoda extracts show antiproliferative effects and are not genotoxic, while extracts of P. birotula show a less potent antiproliferative effect and may induce chromosomal abnormalities. The finding of a partial reversion of the effects of glyphosate by a post-treatment with extracts from both plants should be followed up. PMID:24392578

  11. Post-treatment with plant extracts used in Brazilian folk medicine caused a partial reversal of the antiproliferative effect of glyphosate in the Allium cepa test.

    PubMed

    Frescura, Viviane Dal-Souto; Kuhn, Andrielle Wouters; Laughinghouse, Haywood Dail; Paranhos, Juçara Terezinha; Tedesco, Solange Bosio

    2013-08-01

    Species of the genus Psychotria are used for multiple purposes in Brazilian folk medicine, either as water infusions, baths or poultices. This study was aimed to evaluate the genotoxic and antiproliferative effects of infusions of Psychotria brachypoda and P. birotula on the Allium cepa test. Exposure to distilled water was used as a negative control, while exposure to glyphosate was used as a positive control. The interaction of extracts (as a post-treatment) with the effects of glyphosate was also studied. Results showed that glyphosate and the extracts of both P. brachypoda and P. birotula reduced the mitotic index as compared with the negative control (distilled water). Surprisingly, however, both extracts from P. brachypoda and P. birotula caused a partial reversal of the antiproliferative effect of glyphosate when used as a post-treatment. Glyphosate also induced the highest number of cells with chromosomal alterations, which was followed by that of P. birotula extracts. However, the extracts from P. brachypoda did not show any significant genotoxic effect. Post-treatment of glyphosate-treated samples with distilled water allowed a partial recovery of the genotoxic effect of glyphosate, and some of the Psychotria extracts also did so. Notably, post-treatment of glyphosate-treated samples with P. brachypoda extracts induced a statistically significant apoptotic effect. It is concluded that P. brachypoda extracts show antiproliferative effects and are not genotoxic, while extracts of P. birotula show a less potent antiproliferative effect and may induce chromosomal abnormalities. The finding of a partial reversion of the effects of glyphosate by a post-treatment with extracts from both plants should be followed up.

  12. Purification of Food Color Red No. 106 (acid red) using pH-zone-refining counter-current chromatography.

    PubMed

    Oka, Hisao; Suzuki, Masanao; Harada, Ken-Ichi; Iwaya, Masato; Fujii, Kiyonaga; Goto, Tomomi; Ito, Yuko; Matsumoto, Hiroshi; Ito, Yoichiro

    2002-02-01

    pH-Zone-refining counter-current chromatography was successfully applied to the separation of the main components of Food Color Red No. 106 (R-106, acid red, Color Index No. 45100). A 300-mg quantity of sample was separated using the following two-phase solvent system: n-butanol-water, 40 mM sulfuric acid in organic stationary phase and 30 mM ammonia in aqueous mobile phase. The obtained fractions were analyzed by high-performance liquid chromatography and fast atom bombardment mass spectrometry. The separation yielded 261.9 mg of main component of acid red with purity of 99.9%.

  13. Seasonal variation of the surface North Equatorial Countercurrent (NECC) in the western Pacific Ocean

    NASA Astrophysics Data System (ADS)

    Zhao, Jun; Li, Yuanlong; Wang, Fan

    2016-11-01

    The North Equatorial Countercurrent (NECC) is an important zonal flow in the upper circulation of the tropical Pacific Ocean, which plays a vital role in the heat budget of the western Pacific warm pool. Using satellite-derived data of ocean surface currents and sea surface heights (SSHs) from 1992 to 2011, the seasonal variation of the surface NECC in the western tropical Pacific Ocean was investigated. It was found that the intensity (INT) and axis position (Y CM ) of the surface NECC exhibit strikingly different seasonal fluctuations in the upstream (128°-136°E) and downstream (145°-160°E) regions. Of the two regions, the seasonal cycle of the upstream NECC shows the greater interannual variability. Its INT and YCM are greatly influenced by variations of the Mindanao Eddy, Mindanao Dome (MD), and equatorial Rossby waves to its south. Both INT and Y CM also show semiannual signals induced by the combined effects of equatorial Rossby waves from the Central Pacific and local wind forcing in the western Pacific Ocean. In the downstream region, the variability of the NECC is affected by SSH anomalies in the MD and the central equatorial Pacific Ocean. Those in the MD region are especially important in modulating the YCM of the downstream NECC. In addition to the SSH-related geostrophic flow, zonal Ekman flow driven by meridional wind stress also plays a role, having considerable impact on INT variability of the surface NECC. The contrasting features of the variability of the NECC in the upstream and downstream regions reflect the high complexity of regional ocean dynamics.

  14. Tubing modifications for countercurrent chromatography (CCC): Stationary phase retention and separation efficiency.

    PubMed

    Englert, Michael; Vetter, Walter

    2015-07-16

    Countercurrent chromatography (CCC) is a separation technique in which two immiscible liquid phases are used for the preparative purification of synthetic and natural products. In CCC the number of repetitive mixing and de-mixing processes, the retention of the stationary phase and the mass transfer between the liquid phases are significant parameters that influence the resolution and separation efficiency. Limited mass transfer is the main reason for peak broadening and a low number of theoretical plates along with impaired peak resolution in CCC. Hence, technical improvements with regard to column design and tubing modifications is an important aspect to enhance mixing and mass transfer. In this study we constructed a crimping tool which allowed us to make reproducible, semi-automated modifications of conventional round-shaped tubing. Six crimped tubing modifications were prepared, mounted onto multilayer coils which were subsequently installed in the CCC system. The stationary phase retention of the tubing modifications were compared to the conventional system with unmodified tubing in a hydrophobic, an intermediate and a hydrophilic two-phase solvent system. Generally, the tubing modifications provided higher capabilities to retain the stationary phase depending on the solvent system and flow rates. In the intermediate solvent system the separation efficiency was evaluated with a mixture of six alkyl p-hydroxybenzoates. The peak resolution could be increased up to 50% with one of the tubing modifications compared to the unmodified tubing. Using the most convincing tubing modification at fixed values for the stationary phase retention, a reasonable comparison to the unmodified tubing was achieved. The peak width could be reduced up to 49% and a strong positive impact at increased flow rates regarding peak resolution and theoretical plate number was observed compared to unmodified tubing. It could be concluded that the tubing modification enhanced the interphase

  15. Tubing modifications for countercurrent chromatography (CCC): Stationary phase retention and separation efficiency.

    PubMed

    Englert, Michael; Vetter, Walter

    2015-07-16

    Countercurrent chromatography (CCC) is a separation technique in which two immiscible liquid phases are used for the preparative purification of synthetic and natural products. In CCC the number of repetitive mixing and de-mixing processes, the retention of the stationary phase and the mass transfer between the liquid phases are significant parameters that influence the resolution and separation efficiency. Limited mass transfer is the main reason for peak broadening and a low number of theoretical plates along with impaired peak resolution in CCC. Hence, technical improvements with regard to column design and tubing modifications is an important aspect to enhance mixing and mass transfer. In this study we constructed a crimping tool which allowed us to make reproducible, semi-automated modifications of conventional round-shaped tubing. Six crimped tubing modifications were prepared, mounted onto multilayer coils which were subsequently installed in the CCC system. The stationary phase retention of the tubing modifications were compared to the conventional system with unmodified tubing in a hydrophobic, an intermediate and a hydrophilic two-phase solvent system. Generally, the tubing modifications provided higher capabilities to retain the stationary phase depending on the solvent system and flow rates. In the intermediate solvent system the separation efficiency was evaluated with a mixture of six alkyl p-hydroxybenzoates. The peak resolution could be increased up to 50% with one of the tubing modifications compared to the unmodified tubing. Using the most convincing tubing modification at fixed values for the stationary phase retention, a reasonable comparison to the unmodified tubing was achieved. The peak width could be reduced up to 49% and a strong positive impact at increased flow rates regarding peak resolution and theoretical plate number was observed compared to unmodified tubing. It could be concluded that the tubing modification enhanced the interphase

  16. Seasonal eddy kinetic energy modulations along the North Equatorial Countercurrent in the western Pacific

    NASA Astrophysics Data System (ADS)

    Chen, Xiao; Qiu, Bo; Chen, Shuiming; Qi, Yiquan; Du, Yan

    2015-09-01

    Seasonal eddy kinetic energy (EKE) variability and its associated eddy energy conversion processes in the western tropical Pacific are investigated using satellite altimeter observations and a global, eddy-resolving, ocean general circulation model (OGCM). Both the altimeter-observed sea surface height anomalies and the OGCM simulation show an area with enhanced EKE east of the Mindanao Island centered around 133°E and 5°N. This enhanced EKE area corresponds to the location of the quasi-stationary meander of the North Equatorial Countercurrent (NECC) and is bordered to the south by the Halmahera Eddy. The mesoscale EKE in this area exhibits a clear seasonality, strong in summer (July-August) and weak in winter (November-January), and much of this seasonality is confined to the upper 200 m layer. An investigation into the upper ocean eddy energetics based on the OGCM simulation reveals that the areal barotropic eddy energy conversion rate has an annual cycle similar to the EKE variations, while the areal baroclinic eddy energy conversion is found to be much smaller that the barotropic conversion rate and exhibits no clear seasonal changes. This indicates that the EKE variations are largely controlled by barotropic conversion of the seasonally varying regional circulation. By examining the seasonal background circulation changes, we find that the amplification of the barotropic eddy energy conversion rate in July-August is related to the seasonal evolution of the Mindanao Current and the New Guinea Coastal Current that amplifies the curvature and amplitude of the quasi-stationary meander of the NECC and results in an elevated EKE level through increased regional barotropic conversion.

  17. Modeling pH-zone refining countercurrent chromatography: a dynamic approach.

    PubMed

    Kotland, Alexis; Chollet, Sébastien; Autret, Jean-Marie; Diard, Catherine; Marchal, Luc; Renault, Jean-Hugues

    2015-04-24

    A model based on mass transfer resistances and acid-base equilibriums at the liquid-liquid interface was developed for the pH-zone refining mode when it is used in countercurrent chromatography (CCC). The binary separation of catharanthine and vindoline, two alkaloids used as starting material for the semi-synthesis of chemotherapy drugs, was chosen for the model validation. Toluene/CH3CN/water (4/1/5, v/v/v) was selected as biphasic solvent system. First, hydrodynamics and mass transfer were studied by using chemical tracers. Trypan blue only present in the aqueous phase allowed the determination of the parameters τextra and Pe for hydrodynamic characterization whereas acetone, which partitioned between the two phases, allowed the determination of the transfer parameter k0a. It was shown that mass transfer was improved by increasing both flow rate and rotational speed, which is consistent with the observed mobile phase dispersion. Then, the different transfer parameters of the model (i.e. the local transfer coefficient for the different species involved in the process) were determined by fitting experimental concentration profiles. The model accurately predicted both equilibrium and dynamics factors (i.e. local mass transfer coefficients and acid-base equilibrium constant) variation with the CCC operating conditions (cell number, flow rate, rotational speed and thus stationary phase retention). The initial hypotheses (the acid-base reactions occurs instantaneously at the interface and the process is mainly governed by mass transfer) are thus validated. Finally, the model was used as a tool for catharanthine and vindoline separation prediction in the whole experimental domain that corresponded to a flow rate between 20 and 60 mL/min and rotational speeds from 900 and 2100 rotation per minutes. PMID:25795399

  18. Limonene in Arizona liquid systems used in countercurrent chromatography. I Physicochemical properties.

    PubMed

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

    2014-09-01

    Limonene is a biorenewable cycloterpene solvent derived from orange peel waste. Its potential as a "green" solvent to replace heptane was recently evaluated. Countercurrent chromatography (CCC) is a preparative separation technique using biphasic liquid systems. One liquid phase is the mobile phase; the other liquid phase is the stationary phase held in place by centrifugal fields. A particular range of special proportions of the heptane/ethyl acetate/methanol/water system is called the Arizona (AZ) liquid system when the heptane/ethyl acetate ratio is exactly the same as the methanol/water ratio. A continuous polarity decrease is obtained between the most polar A composition (ethyl acetate/water or 0/1/0/1 v/v) and the least polar Z composition (heptane/methanol or 1/0/1/0 v/v), replacing heptane by limonene and methanol by ethanol produce biphasic liquid systems much more environmentallyfriendly than the original AZ compositions. The chemical compositions of the two liquid phases of 12 AZ limonene/ethyl acetate/ethanol/water proportions were fully determined by Karl-Fisher titration of water and by gas chromatography for the organic solvents. The results were compared with the compositions of the corresponding AZ mixtures containing heptane and methanol. Significant differences in ethyl acetate and ethanol distribution between phases of the two systems with identical volume proportions were established. The ratio of the upper phase over the lower phase volumes and the phase density difference are important in CCC, there are also significant differences between the classic and "green" AZ systems that are discussed.

  19. Separation of chemical constituents from three plant medicines by counter-current chromatography using a three-phase solvent system at a novel ratio.

    PubMed

    Wu, Xiaoyi; Chao, Zhimao; Wang, Chun; Yu, Li

    2015-03-01

    A solvent system of n-hexane, methyl acetate, acetonitrile, and water at a novel volume ratio of 4:3:4:4 forms three layers, i.e. upper phase (UP), middle phase (MP), and lower phase (LP), with a volume ratio of 1:1.20:1.42 at room temperature (25°C). All three two-phases from this three-phase solvent system were successfully used to separate some chemical constituents from three plant medicines with counter-current chromatography (CCC). Eight coumarins (B1-B8) were obtained from petroleum ether extract of fresh roots of Angelica dahurica (Baizhi) with a stationary phase of UP and a mobile phase of LP. Six diarylheptanoids (L1-L6) were obtained from petroleum ether extract of dried rhizomes of Alpinia officinarum (Liangjiang) with a stationary phase of UP and a mobile phase of MP. Three chemical constituents (Z1-Z3) were obtained from ethyl acetate extract of fresh rhizomes of Anemarrhena asphodeloides (Zhimu) with a stationary phase of MP and a mobile phase of LP. Preparative HPLC was used for further purification if necessary. Seventeen chemical constituents were identified as oxypeucedanin hydrate (B1), byakangelicin (B2), byakangelicol (B3), bergapten (B4), oxypeucedanin (B5), imperatorin (B6), phellopterin (B7), isoimperatorin (B8), 5-hydroxy-7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-3-heptanone (L1), 7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-4E-en-3-heptanone (L2), 5-hydroxy-1,7-diphenyl-3-heptanone (L3), 1,7-diphenyl-4E-en-3-heptanone (L4), 5-hydroxy-1,7-diphenyl-4E,6E-dien-3-heptanone (L5), isomers of 1,7-diphenyl-3,5-heptandione and 5-hydroxy-1,7-diphenyl-4E-en-3-heptanone (L6), mangiferin (Z1), timosaponin A-III (Z2), and 2,6,4'-trihydroxy-4-methoxy-benzophenone (Z3) by means of MS, (1)H and (13)C NMR studies. Five compounds of B3, L3, L5, L6, and Z3 were isolated by CCC for the first time.

  20. Antigenotoxicity and antimutagenicity of ethanolic extracts of Brazilian green propolis and its main botanical source determined by the Allium cepa test system

    PubMed Central

    Roberto, Matheus Mantuanelli; Jamal, Cláudia Masrouah; Malaspina, Osmar; Marin-Morales, Maria Aparecida

    2016-01-01

    Abstract Brazilian green propolis is a resinous substance prepared by bees from parts of the plant Baccharis dracunculifolia. As it possess several biological properties, this work assessed the cytotoxic/anticytotoxic, genotoxic/antigenotoxic and mutagenic/antimutagenic potential of ethanolic extracts of Brazilian green propolis (EEGP) and of B. dracunculifolia (EEBD), by means of the Allium cepa test system. The effects were evaluated by assessing the chromosomal aberrations (CA) and micronuclei (MN) frequencies on meristematic and F1 generation cells from onion roots. Chemical analyses performed with the extracts showed differences in flavonoid quality and quantity. No genotoxic or mutagenic potential was detected, and both extracts were capable of inhibiting cellular damage caused by methyl methanesulfonate (MMS) treatment, reducing the frequencies of CA and MN. By these data, we can infer that, independent of their flavonoid content, the extracts presented a protective effect in A. cepa cells against the clastogenicity of MMS. PMID:27223486

  1. Antigenotoxicity and antimutagenicity of ethanolic extracts of Brazilian green propolis and its main botanical source determined by the Allium cepa test system.

    PubMed

    Roberto, Matheus Mantuanelli; Jamal, Cláudia Masrouah; Malaspina, Osmar; Marin-Morales, Maria Aparecida

    2016-05-24

    Brazilian green propolis is a resinous substance prepared by bees from parts of the plant Baccharis dracunculifolia. As it possess several biological properties, this work assessed the cytotoxic/anticytotoxic, genotoxic/antigenotoxic and mutagenic/antimutagenic potential of ethanolic extracts of Brazilian green propolis (EEGP) and of B. dracunculifolia (EEBD), by means of the Allium cepa test system. The effects were evaluated by assessing the chromosomal aberrations (CA) and micronuclei (MN) frequencies on meristematic and F1 generation cells from onion roots. Chemical analyses performed with the extracts showed differences in flavonoid quality and quantity. No genotoxic or mutagenic potential was detected, and both extracts were capable of inhibiting cellular damage caused by methyl methanesulfonate (MMS) treatment, reducing the frequencies of CA and MN. By these data, we can infer that, independent of their flavonoid content, the extracts presented a protective effect in A. cepa cells against the clastogenicity of MMS. PMID:27223486

  2. Transuranic decontamination of nitric acid solutions by the TRUEX solvent extraction process: preliminary development studies. [Octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide

    SciTech Connect

    Vandegrift, G.F.; Leonard, R.A.; Steindler, M.J.; Horwitz, E.P.; Basile, L.J.; Diamond, H.; Kalina, D.G.; Kaplan, L.

    1984-07-01

    This report summarizes the work that has been performed to date at Argonne National Laboratory on the development of the TRUEX process, a solvent extraction process employing a bifunctional organophosphorous reagent in a PUREX process solvent (tributyl phosphate-normal paraffinic hydrocarbons). The purpose of this extraction process is to separate and concentrate transuranic (TRU) elements from nuclear waste. Assessments were made of the use of two TRUEX solvents: one incorporating the well-studied dihexyl-N,N-diethylcarbamoylmethylphosphonate (DHDECMP) and a second incorporating an extractant with superior properties for a 1M HNO/sub 3/ acid feed, octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (O/sub phi/D(IB)CMPO). In this report, conceptual flowsheets for the removal of soluble TRUs from high-level nuclear wastes using these two TRUEX proces solvents are presented, and flowsheet features are discussed in detail. The conceptual flowsheet for TRU-element removal from a PUREX waste by the O/sub phi/D(IB)CMPO-TRUEX process solvent was tested in a bench-scale countercurrent experiment, and results of that experiment are presented and discussed. The conclusion of this study is that the TRUEX process is able to separate TRUs from high-level wastes so that the major portion of the solid waste (approx. 99%) can be classified as non-TRU. Areas where more experimentation is needed are listed at the end of the report. 45 references, 17 figures, 56 tables.

  3. Unsubstituted polyaromatic hydrocarbons (PAH's) in extracts of coal fly ash from the fly ash test cell in Montour, Pennsylvania

    SciTech Connect

    Applequist, M.D.

    1989-01-01

    Isotope Dilution Mass Spectrometry (IDMS) was used to identify and to quantify trace amounts of selected, unsubstituted polyaromatic hydrocarbons (PAH's) present in extracts of coal fly ash from the solid waste disposal test cell at Montour, Pennsylvania. Isotope dilution experiments using deuterated analogs of polyaromatic hydrocarbons demonstrated that the concentrations of benzo(a)pyrene and anthracene were lower than 1 ng/g of fly ash. Isotope dilution experiments demonstrated that benzo(a)pyrene could be detected at concentrations as high as 1 ng/g when an isotopic carrier was used at a concentration of 125 ng/g in the analytical method. Maximum concentrations of fluorene, fluoranthene, pyrene and chrysene were conservatively estimated to be 3 ng/g of fly ash, using a 95 percent confidence interval based on analytical precision of {+-}1 ng/g of fly ash. Concentrations of phenanthrene were found to range from 6 to 38 ng/g of fly ash with a mean concentration of 14 ng/g of fly ash. Two sources of phenanthrene were speculated: incomplete combustion of phenanthrene in the coal furnace and addition of phenanthrene to the fly ash after collection by electrostatic precipitators.

  4. Effect of organic tomato (Lycopersicon esculentum) extract on the genotoxicity of doxorubicin in the Drosophila wing spot test

    PubMed Central

    2009-01-01

    The consumption of organic tomatoes (ORTs) reduces the risk of harmful effects to humans and the environment caused by exposure to toxic agrochemicals. In this study, we used the somatic mutation and recombination test (SMART) of wing spots in Drosophila melanogaster to evaluate the genotoxicity of ORT and the effect of cotreatment with ORT on the genotoxicity of Doxorubicin® (DXR, a cancer chemotherapeutic agent) that is mediated by free radical formation. Standard (ST) cross larvae were treated chronically with solutions containing 25%, 50% or 100% of an aqueous extract of ORT, in the absence and presence of DXR (0.125 mg/mL), and the number of mutant spots on the wings of emergent flies was counted. ORT alone was not genotoxic but enhanced the toxicity of DXR when administered concomitantly with DXR. The ORT-enhanced frequency of spots induced by DXR may have resulted from the interaction of ORT with the enzymatic systems that catalyze the metabolic detoxification of this drug. PMID:21637658

  5. The bioaccessibility of soil-based mercury as determined by physiological based extraction tests and human biomonitoring in children.

    PubMed

    Safruk, Adam M; Berger, Robert G; Jackson, Blair J; Pinsent, Celine; Hair, Alan T; Sigal, Elliot A

    2015-06-15

    Environmental contaminants associated with soil particles are generally less bioavailable than contaminants associated with other exposure media where chemicals are often found in more soluble forms. In vitro methods, such as Physiological Based Extraction Tests (PBET), can provide estimates of bioaccessibility for soil-based contaminants. The results of these tests can be used to predict exposure to contaminants from soil ingestion pathways within human health risk assessment (HHRA). In the current investigation, an HHRA was conducted to examine the risks associated with elevated concentrations of mercury in soils in the northern Canadian smelter community of Flin Flon, Manitoba. A PBET was completed for residential soils and indicated mean bioaccessibilities of 1.2% and 3.0% for total mercury using gastric phase and gastric+intestinal phase methodologies, respectively. However, as many regulators only allow for the consideration of in vitro results for lead and arsenic in the HHRA process, in vitro bioaccessibility results for mercury were not utilized in the current HHRA. Based on the need to assume 100% bioaccessibility for inorganic mercury in soil, results from the HHRA indicated the need for further assessment of exposure and risk. A biomonitoring study was undertaken for children between 2 and 15 years of age in the community to examine urinary inorganic mercury concentrations. Overall, 375 children provided valid urine samples for analysis. Approximately 50% of urine samples had concentrations of urinary inorganic mercury below the limit of detection (0.1 μg/L), with an average creatinine adjusted concentration of 0.11 μg/g. Despite high variability in mercury soil concentrations within sub-communities, soil concentrations did not appear to influence urinary mercury concentrations. The results of the current investigation indicate that mercury bioaccessibility in residential soils in the Flin Flon area was likely limited and that HHRA estimates would

  6. Determination of the antimutagenicity of an aqueous extract of Rhizophora mangle L. (Rhizophoraceae), using in vivo and in vitro test systems

    PubMed Central

    2010-01-01

    An aqueous extract of Rhizophora mangle L. bark is used as raw material in pottery making in the State of Espirito Santo, Brazil. This extract presents large quantities of tannins, compounds possessing antioxidant properties. Tannin antioxidant activity, as a plant chemical defense mechanism in the process of stabilizing free radicals, has been an incentive to studies on anti-mutagenicity. The present work aimed to evaluate possible antimutagenic activity of a R. mangle aqueous extract, using the Allium cepa test-system and micronuclear (MN) assay with blockage of cytokinesis in Chinese hamster ovary cells (CHO-K1). The Allium cepa test-system indicated antimutagenic activity against the damage induced by the mutagenic agent methyl methanesulfonate. A reduction in both MN cell frequency and chromosome breaks occurred in both the pre and post-treatment protocols. The MN testing of CHO-K1 cells revealed anti-mutagenic activity of the R. mangle extract against methyl methanesulfonate and doxorubicin in pre, simultaneous and post-treatment protocols. These results suggest the presence of phyto-constituents in the extract presenting demutagenic and bio-antimutagenic activities. Since the chemical constitution of Rhizophora mangle species presents elevated tannin content, it is highly probable that these compounds are the antimutagenic promoters themselves. PMID:21637623

  7. Determination of the antimutagenicity of an aqueous extract of Rhizophora mangle L. (Rhizophoraceae), using in vivo and in vitro test systems.

    PubMed

    Malini, Maressa; Marin-Morales, Maria Aparecida; Mantovani, Mário Sérgio; Jamal, Claudia Masrouah; Nati, Natália; da Silva Passos, Tatiane; Matsumoto, Silvia Tamie

    2010-01-01

    An aqueous extract of Rhizophora mangle L. bark is used as raw material in pottery making in the State of Espirito Santo, Brazil. This extract presents large quantities of tannins, compounds possessing antioxidant properties. Tannin antioxidant activity, as a plant chemical defense mechanism in the process of stabilizing free radicals, has been an incentive to studies on anti-mutagenicity. The present work aimed to evaluate possible antimutagenic activity of a R. mangle aqueous extract, using the Allium cepa test-system and micronuclear (MN) assay with blockage of cytokinesis in Chinese hamster ovary cells (CHO-K1). The Allium cepa test-system indicated antimutagenic activity against the damage induced by the mutagenic agent methyl methanesulfonate. A reduction in both MN cell frequency and chromosome breaks occurred in both the pre and post-treatment protocols. The MN testing of CHO-K1 cells revealed anti-mutagenic activity of the R. mangle extract against methyl methanesulfonate and doxorubicin in pre, simultaneous and post-treatment protocols. These results suggest the presence of phyto-constituents in the extract presenting demutagenic and bio-antimutagenic activities. Since the chemical constitution of Rhizophora mangle species presents elevated tannin content, it is highly probable that these compounds are the antimutagenic promoters themselves. PMID:21637623

  8. TECHNOLOGY EVALUATION REPORT: SITE PROGRAM DEMONSTRATION TEST - ACCUTECH PNEUMATIC FRACTURING EXTRACTION AND HOT GAS INJECTION, PHASE 1 - VOLUME I

    EPA Science Inventory

    The Pneumatic Fracturing Extraction (PFE) process developed by Accutech Remedial Systems, Inc. makes it possible to use vapor extraction to remove volatile organics at increased rates from a broader range of vadose zones. The low permeability of silts, clays, shales, etc. would o...

  9. What Makes a Matrix so Effective? An Empirical Test of the Relative Benefits of Signaling, Extraction, and Localization

    ERIC Educational Resources Information Center

    Kauffman, Douglas F.; Kiewra, Kenneth A.

    2010-01-01

    What type of display helps students learn the most and why? This study investigated how displays differing in terms of signaling, extraction, and localization impact learning. In Experiment 1, 72 students were assigned randomly to one cell of a 4 x 2 design. Students studied a standard text, a text with key ideas extracted, an outline that…

  10. Purification of monoclonal antibodies from clarified cell culture fluid using Protein A capture continuous countercurrent tangential chromatography.

    PubMed

    Dutta, Amit K; Tran, Travis; Napadensky, Boris; Teella, Achyuta; Brookhart, Gary; Ropp, Philip A; Zhang, Ada W; Tustian, Andrew D; Zydney, Andrew L; Shinkazh, Oleg

    2015-11-10

    Recent studies using simple model systems have demonstrated that continuous countercurrent tangential chromatography (CCTC) has the potential to overcome many of the limitations of conventional Protein A chromatography using packed columns. The objective of this work was to optimize and implement a CCTC system for monoclonal antibody purification from clarified Chinese Hamster Ovary (CHO) cell culture fluid using a commercial Protein A resin. Several improvements were introduced to the previous CCTC system including the use of retentate pumps to maintain stable resin concentrations in the flowing slurry, the elimination of a slurry holding tank to improve productivity, and the introduction of an "after binder" to the binding step to increase antibody recovery. A kinetic binding model was developed to estimate the required residence times in the multi-stage binding step to optimize yield and productivity. Data were obtained by purifying two commercial antibodies from two different manufactures, one with low titer (∼ 0.67 g/L) and one with high titer (∼ 6.9 g/L), demonstrating the versatility of the CCTC system. Host cell protein removal, antibody yields and purities were similar to those obtained with conventional column chromatography; however, the CCTC system showed much higher productivity. These results clearly demonstrate the capabilities of continuous countercurrent tangential chromatography for the commercial purification of monoclonal antibody products.

  11. Direct-contact heat exchanger for swirling countercurrent flow of hot gas and finely divided solids: A parametric study

    NASA Astrophysics Data System (ADS)

    Bell, K. J.; Arman, B.

    1991-06-01

    A vertically oriented solid-to-gas direct-contact heat exchanger (DCHX) has been proposed for heat recovery in high temperature plants that process finely divided solids. The flows are countercurrent, with the inlet gas flow entering on the centerline and swirling strongly. Swirling enhances heat transfer and centrifuges the solid particles from the center to the wall in order to minimize entrainment and permit gravity separation. A computer program was written to calculate particle trajectories and heat transfer rates (and, therefore, temperature profiles) for gas and solid phases. The flow model considers interactions between the particles and the flow field of the gas. The results of the computer program showed that the introduction of swirl significantly reduced the vertical distance required to achieve a given thermal efficiency. The countercurrent flow arrangement achieves high thermal efficiency in one contacting stage, unlike existing cocurrent suspension preheater systems, which require four or five stages. The practical application of this design to the cement industry appears unlikely, because very low gas velocities and correspondingly large areas of cross-sectional flow are required to prevent elutriation of the 74 micron particles required for the chemical reactions. The computer program can be modified for spray-dryer applications by the addition of mass transfer terms and a spray-formation model. In addition, the concept of a swirling flow heat exchanger may be applicable to other processes in which larger and heavier particles are used.

  12. Isolation and purification of two antioxidant isomers of resveratrol dimer from the wine grape by counter-current chromatography.

    PubMed

    Kong, Qingjun; Ren, Xueyan; Hu, Ruilin; Yin, Xuefeng; Jiang, Guoshan; Pan, Yuanjiang

    2016-06-01

    Resveratrol dimers belong to a group of compounds called stilbenes, which along with proanthocyanidins, anthocyanins, catechins, and flavonols are natural phenolic compounds found in grapes and red wine. Stilbenes have a variety of structural isomers, all of which exhibit various biological properties. Counter-current chromatography with a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water (2:5:4:5, v/v/v/v) was applied to isolate and purify stilbene from the stems of wine grape. Two isomers of resveratrol dimers trans-ε-viniferin and trans-δ-viniferin were obtained from the crude sample in a one-step separation, with purities of 93.2 and 97.5%, respectively, as determined by high-performance liquid chromatography. The structures of these two compounds were identified by (1) H and (13) C NMR spectroscopy. In addition, their antioxidant activities were assessed by 1,1-diphenyl-2-picrylhydrazyl (DPPH) assay. The antioxidant activities of trans-δ-viniferin were higher than that of trans-ε-viniferin in this model. This work demonstrated that counter-current chromatography is a powerful and effective method for the isolation and purification of polyphenols from wine grape. Additionally, the DPPH radical assay showed that the isolated component trans-δ-viniferin exhibited stronger antioxidant activities than trans-ε-viniferin and a little bit weaker than vitamin E at the same concentration.

  13. SIMULATION OF NON-AZEOTROPIC REFRIGERANT MIXTURES FOR USE IN A DUAL-CIRCUIT REFRIGERATOR/FREEZER WITH COUNTERCURRENT HEAT EXCHANGES

    EPA Science Inventory

    The paper discusses a refrigerator/freezer (RF) system that has two complete and independent refrigeration cycles for the two compartments. It uses a non-azeotropic refrigerant mixture (NARM) in each cycle and countercurrent heat exchangers throughout. This RF is housed in a stan...

  14. Development of a method to screen and isolate potential xanthine oxidase inhibitors from Panax japlcus var via ultrafiltration liquid chromatography combined with counter-current chromatography.

    PubMed

    Li, Sainan; Tang, Ying; Liu, Chunming; Li, Jing; Guo, Liping; Zhang, Yuchi

    2015-03-01

    Panax japlcus var is a typical Chinese herb with a large number of saponins existing in all parts of it. The common methods of screening and isolating saponins are mostly labor-intensive and time-consuming. In this study, a new assay based on ultrafiltration-liquid chromatography-mass spectrometry (UF-LC-MS) was developed for the rapid screening and identifying of the ligands for xanthine oxidase from the extract of P. japlcus. Six saponins were identified as xanthine oxidase inhibitors from the extract. Subsequently, the specific binding ligands, namely, 24 (R)-majoroside R1, chikusetsusaponin IVa, oleanolic acid-28-O-β-D-glucopyranoside, notoginsenoside Fe, ginsenoside Rb2 and ginsenoside Rd (the purities of them were 95.74%, 96.12%, 93.19%, 94.83%, 95.07% and 94.62%, respectively) were separated by high-speed counter-current chromatography (HSCCC). The component ratio of the solvent system of HSCCC was calculated with the help of a multiexponential function model was optimized. The partition coefficient (K) values of the target compounds and resolutions of peaks were employed as the research indicators, and exponential function and binomial formulas were used to optimize the solvent system and flow rate of the mobile phases in a two-stage separation. An optimized two-phase solvent system composed of ethyl acetate, isopropanol, 0.1% aqueous formic acid (1.9:1.0:1.3, v/v/v, for the first-stage) and that composed of methylene chloride, acetonitrile, isopropanol, 0.1% aqueous formic acid (5.6:1.0:2.4:5.2, v/v/v/v, for the second-stage) were used to isolate the six compounds from P. japlcus. The targeted compounds isolated, collected and purified by HSCCC were analyzed by high performance liquid chromatography (UPLC), and the chemical structures of all the six compounds were identified by UV, MS and NMR. The results demonstrate that UF-LC-MS combined with HSCCC might provide not only a powerful tool for screening and isolating xanthine oxidase inhibitors in complex

  15. Preparative Separation of Phenolic Compounds from Chimonanthus praecox Flowers by High-Speed Counter-Current Chromatography Using a Stepwise Elution Mode.

    PubMed

    Li, Huaizhi; Zhang, Yongqing; Liu, Qian; Sun, Changlei; Li, Jia; Yang, Peng; Wang, Xiao

    2016-01-01

    High-speed counter-current chromatography (HSCCC) has been successfully used for the separation of eight compounds from Chimonanthus praecox flowers. Firstly, the crude extract of Chimonanthus praecox flowers was dissolved in a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-H₂O (5:5:3:7, v/v) and divided into two parts: the upper phase (part I) and the lower phase (part II). Then, HSCCC was applied to separate the phenolic acids from part I and part II, respectively. Considering the broad polarity range of target compounds in part I, a stepwise elution mode was established. Two optimal solvent systems of petroleum ether-ethyl acetate-methanol-H₂O-formic acid (FA) (5:5:3:7:0.02, 5:5:4.3:5.7:0.02, v/v) were employed in this separation. Five phenylpropanoids and two flavonoids were successfully separated from 280 mg of part I, including 8.7 mg of 3,4-dihydroxy benzoic acid (a, 95.3% purity), 10.9 mg of protocatechualdehyde (b, 96.8% purity), 11.3 mg of p-coumaric acid (c, 98.9% purity), 12.2 mg of p-hydroxybenzaldehyde (d, 95.9% purity), 24.7 mg of quercetin (e, 97.3% purity), 33.8 mg of kaempferol (f, 96.8% purity), and 24.6 mg of 4-hydroxylcinnamic aldehyde (g, 98.0% purity). From 300 mg of part II, 65.7 mg of rutin (h, 98.2% purity), 7.5 mg of 3,4-dihydroxy benzoic acid (a, 77.4% purity), and 4.7 mg of protocatechualdehyde (b, 81.6% purity) were obtained using the solvent system EtOAc-n-butanol (n-BuOH)-FA-H₂O (4:1:0.5:5, v/v). The structures of the eight pure compounds were confirmed by electrospray ionization-mass spectrometry (ESI-MS), ¹H-NMR and (13)C-NMR. To the best of our knowledge, compounds a-d and f were the first separated and reported from the Chimonanthus praecox flower extract.

  16. Preparative Separation of Phenolic Compounds from Chimonanthus praecox Flowers by High-Speed Counter-Current Chromatography Using a Stepwise Elution Mode.

    PubMed

    Li, Huaizhi; Zhang, Yongqing; Liu, Qian; Sun, Changlei; Li, Jia; Yang, Peng; Wang, Xiao

    2016-01-01

    High-speed counter-current chromatography (HSCCC) has been successfully used for the separation of eight compounds from Chimonanthus praecox flowers. Firstly, the crude extract of Chimonanthus praecox flowers was dissolved in a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-H₂O (5:5:3:7, v/v) and divided into two parts: the upper phase (part I) and the lower phase (part II). Then, HSCCC was applied to separate the phenolic acids from part I and part II, respectively. Considering the broad polarity range of target compounds in part I, a stepwise elution mode was established. Two optimal solvent systems of petroleum ether-ethyl acetate-methanol-H₂O-formic acid (FA) (5:5:3:7:0.02, 5:5:4.3:5.7:0.02, v/v) were employed in this separation. Five phenylpropanoids and two flavonoids were successfully separated from 280 mg of part I, including 8.7 mg of 3,4-dihydroxy benzoic acid (a, 95.3% purity), 10.9 mg of protocatechualdehyde (b, 96.8% purity), 11.3 mg of p-coumaric acid (c, 98.9% purity), 12.2 mg of p-hydroxybenzaldehyde (d, 95.9% purity), 24.7 mg of quercetin (e, 97.3% purity), 33.8 mg of kaempferol (f, 96.8% purity), and 24.6 mg of 4-hydroxylcinnamic aldehyde (g, 98.0% purity). From 300 mg of part II, 65.7 mg of rutin (h, 98.2% purity), 7.5 mg of 3,4-dihydroxy benzoic acid (a, 77.4% purity), and 4.7 mg of protocatechualdehyde (b, 81.6% purity) were obtained using the solvent system EtOAc-n-butanol (n-BuOH)-FA-H₂O (4:1:0.5:5, v/v). The structures of the eight pure compounds were confirmed by electrospray ionization-mass spectrometry (ESI-MS), ¹H-NMR and (13)C-NMR. To the best of our knowledge, compounds a-d and f were the first separated and reported from the Chimonanthus praecox flower extract. PMID:27527132

  17. A novel 9 × 9 map-based solvent selection strategy for targeted counter-current chromatography isolation of natural products.

    PubMed

    Liang, Junling; Meng, Jie; Wu, Dingfang; Guo, Mengzhe; Wu, Shihua

    2015-06-26

    Counter-current chromatography (CCC) is an efficient liquid-liquid chromatography technique for separation and purification of complex mixtures like natural products extracts and synthetic chemicals. However, CCC is still a challenging process requiring some special technical knowledge especially in the selection of appropriated solvent systems. In this work, we introduced a new 9 × 9 map-based solvent selection strategy for CCC isolation of targets, which permit more than 60 hexane-ethyl acetate-methanol-water (HEMWat) solvent systems as the start candidates for the selection of solvent systems. Among these solvent systems, there are clear linear correlations between partition coefficient (K) and the system numbers. Thus, an appropriate CCC solvent system (i.e., sweet spot for K = 1) may be hit by measurement of k values of the target only in two random solvent systems. Besides this, surprisingly, we found that through two sweet spots, we could get a line ("Sweet line") where there are infinite sweet solvent systems being suitable for CCC separation. In these sweet solvent systems, the target has the same partition coefficient (K) but different solubilities. Thus, the better sweet solvent system with higher sample solubility can be obtained for high capacity CCC preparation. Furthermore, we found that there is a zone ("Sweet zone") where all solvent systems have their own sweet partition coefficients values for the target in range of 0.4 < K< 2.5 or extended range of 0.25 < K < 16. All results were validated by using 14 pure GUESSmix mimic natural products as standards and further confirmed by isolation of several targets including honokiol and magnolol from the extracts of Magnolia officinalis Rehd. Et Wils and tanshinone IIA from Salvia miltiorrhiza Bunge. In practice, it is much easier to get a suitable solvent system only by making a simple screening two to four HEMWat two-phase solvent systems to obtain the sweet line or sweet zone without special knowledge

  18. Linear and nonlinear instability in vertical counter-current laminar gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Schmidt, Patrick; Ó Náraigh, Lennon; Lucquiaud, Mathieu; Valluri, Prashant

    2016-04-01

    We consider the genesis and dynamics of interfacial instability in vertical gas-liquid flows, using as a model the two-dimensional channel flow of a thin falling film sheared by counter-current gas. The methodology is linear stability theory (Orr-Sommerfeld analysis) together with direct numerical simulation of the two-phase flow in the case of nonlinear disturbances. We investigate the influence of two main flow parameters on the interfacial dynamics, namely the film thickness and pressure drop applied to drive the gas stream. To make contact with existing studies in the literature, the effect of various density contrasts is also examined. Energy budget analyses based on the Orr-Sommerfeld theory reveal various coexisting unstable modes (interfacial, shear, internal) in the case of high density contrasts, which results in mode coalescence and mode competition, but only one dynamically relevant unstable interfacial mode for low density contrast. A study of absolute and convective instability for low density contrast shows that the system is absolutely unstable for all but two narrow regions of the investigated parameter space. Direct numerical simulations of the same system (low density contrast) show that linear theory holds up remarkably well upon the onset of large-amplitude waves as well as the existence of weakly nonlinear waves. For high density contrasts, corresponding more closely to an air-water-type system, linear stability theory is also successful at determining the most-dominant features in the interfacial wave dynamics at early-to-intermediate times. Nevertheless, the short waves selected by the linear theory undergo secondary instability and the wave train is no longer regular but rather exhibits chaotic motion. The same linear stability theory predicts when the direction of travel of the waves changes — from downwards to upwards. We outline the practical implications of this change in terms of loading and flooding. The change in direction of the

  19. pH-zone-refining counter-current chromatography: Origin, mechanism, procedure and applications✩

    PubMed Central

    Ito, Yoichiro

    2012-01-01

    Since 1980, high-speed counter-current chromatography (HSCCC) has been used for separation and purification of natural and synthetic products in a standard elution mode. In 1991, a novel elution mode called pH-zone refining CCC was introduced from an incidental discovery that an organic acid in the sample solution formed the sharp peak of an acid analyte. The cause of this sharp peak formation was found to be bromoacetic acid present in the sample solution which formed a sharp trailing border to trap the acidic analyte. Further studies on the separation of DNP-amino acids with three spacer acids in the stationary phase revealed that increased sample size resulted in the formation of fused rectangular peaks, each preserving high purity and zone pH with sharp boundaries. The mechanism of this phenomenon was found to be the formation of a sharp trailing border of an acid (retainer) in the column which moves at a lower rate than that of the mobile phase. In order to facilitate the application of the method, a new method was devised using a set of retainer and eluter to form a sharp retainer rear border which moves through the column at a desired rate regardless of the composition of the two-phase solvent system. This was achieved by adding the retainer in the stationary phase and the eluter in the mobile phase at a given molar ratio. Using this new method the hydrodynamics of pH-zone-refining CCC was diagrammatically illustrated by three acidic samples. In this review paper, typical pH-zone-refining CCC separations were presented, including affinity separations with a ligand and a separation of a racemic mixture using a chiral selector in the stationary phase. Major characteristics of pH-zone-refining CCC over conventional HSCCC are as follows: the sample loading capacity is increased over 10 times; fractions are highly concentrated near saturation level; yield is improved by increasing the sample size; minute charged compounds are concentrated and detected at the peak

  20. Characterisation of coastal counter-currents on the inner shelf of the Gulf of Cadiz

    NASA Astrophysics Data System (ADS)

    Garel, E.; Laiz, I.; Drago, T.; Relvas, P.

    2016-03-01

    At the Gulf of Cadiz (GoC), poleward currents leaning along the coast alternate with coastal upwelling jets of opposite direction. Here the patterns of these coastal countercurrents (CCCs) are derived from ADCP data collected during 7 deployments at a single location on the inner shelf. The multiyear (2008-2014) time-series, constituting ~ 18 months of hourly records, are further analysed together with wind data from several sources representing local and basin-scale conditions. During one deployment, temperature sensors were also installed near the mooring site to examine the vertical thermal stratification associated with periods of poleward flow. These observations indicate that the coastal circulation is mainly alongshore and barotropic. However, a baroclinic flow is often observed shortly at the time of flow inversion to poleward. CCCs develop all year-round and exclusively control the occurrence of warm coastal water during the upwelling season. On average, one poleward flow lasting 3 days was observed every week, corresponding to CCCs during ~ 40% of the time without seasonal variability. Thus, the studied region is distinct from typical upwelling systems where equatorward coastal upwelling jets largely predominate. CCCs often start to develop near the bed and are frequently associated with 2-layer cross-shore flows characteristic of downwelling conditions (offshore near the bed). In general, the action of alongshore wind stress alone does not justify the development of CCCs. The coastal circulation is best correlated and shows the highest coherence with south-eastward wind in the basin that proceeds from the rotation of southward wind at the West coast of Portugal, hence suggesting a dominant control of large-scale wind conditions. In agreement, wavelet analyses indicate that CCCs are best correlated with alongshore wind occurring in a band period characteristic of the upwelling system (8-32 days). Furthermore, in the absence of wind coastal currents tend

  1. Study of Co-Current and Counter-Current Gas-Liquid Two-Phase Flow Through Packed Bed in Microgravity

    NASA Astrophysics Data System (ADS)

    Revankar, Shripad T.

    2002-11-01

    The main goal of the project is to obtain new experimental data and development of models on the co-current and counter-current gas-liquid two-phase flow through a packed bed in microgravity and characterize the flow regime transition, pressure drop, void and interfacial area distribution, and liquid hold up. Experimental data will be obtained for earth gravity and microgravity conditions. Models will be developed for the prediction of flow regime transition, void fraction distribution and interfacial area concentration, which are key parameters to characterize the packed bed performance. Thus the specific objectives of the proposed research are to: (1) Develop experiments for the study of the gas liquid two-phase flow through the packed bed with three different flow combinations: co-current down flow, co-current upflow and counter current flow. (2) Develop pore scale and bed scale two-phase instrumentation for measurement of flow regime transition, void distribution and gas-liquid interfacial area concentration in the packed bed. (3) Obtain database on flow regime transition, pressure drop, void distribution, interfacial area concentration and liquid hold up as a function of bed characteristics such as bed particle size, porosity, and liquid properties such as viscosity and surface tension. (4) Develop mathematical model for flow regime transition, void fraction distribution and interfacial area concentration for co-current gas-liquid flow through the porous bed in gravity and micro gravity conditions.(4) Develop mathematical model for the flooding phenomena in counter-current gas-liquid flow through the porous bed in gravity and micro gravity conditions. The present proposal addresses the most important topic of HEDS-specific microgravity fluid physics research identified by NASA 's one of the strategic enterprises, OBPR Enterprise. The proposed project is well defined and makes efficient use of the ground-based parabolic flight research aircraft facility. The

  2. SUPERFUND TREATABILITY CLEARINGHOUSE: FINAL REPORT: DEVELOPMENT OF OPTIMUM TREATMENT SYSTEM FOR WASTEWATER LAGOONS PHASE II - SOLVENT EXTRACTION LABORATORY TESTING

    EPA Science Inventory

    The U.S. Army surveyed innovative treatment techniques for restoration of hazardous waste lagoons and selected solvent extraction as cost-effective restoration for further study. This treatability study focuses on treatment of organic (explosive) contaminated lagoon sediments w...

  3. Separation of nine compounds from Salvia plebeia R.Br. using two-step high-speed counter-current chromatography with different elution modes.

    PubMed

    Ren, Da-Bing; Qin, Yan-Hua; Yun, Yong-Huan; Lu, Hong-Mei; Chen, Xiao-Qing; Liang, Yi-Zeng

    2014-08-01

    Nine compounds were successfully separated from Salvia plebeia R.Br. using two-step high-speed counter-current chromatography with three elution modes. Elution-extrusion counter-current chromatography was applied in the first step, while classical counter-current chromatography and recycling counter-current chromatography were used in the second step. Three solvent systems, n-hexane/ethyl acetate/ethanol/water (4:6.5:3:7, v/v), methyl tert-butyl ether/ethyl acetate/n-butanol/methanol/water (6:4:1:2:8, v/v) and n-hexane/ethyl acetate/methanol/water (5:5.5:5:5, v/v) were screened and optimized for the two-step separation. The separation yielded nine compounds, including caffeic acid (1), 6-hydroxyluteuolin-7-glucoside (2), 5,7,3',4'-tetrahydroxy-6-methoxyflavanone-7-glucoside (3), nepitrin (4), rosmarinic acid (5), homoplantaginin (6), nepetin (7), hispidulin (8), and 5,6,7,4'-tertrahydroxyflavone (9). To the best of our knowledge, 5,7,3',4'-tetrahydroxy-6-methoxyflavanone-7-glucoside and 5,6,7,4'-tertrahydroxyflavone have been separated from Salvia plebeia R.Br. for the first time. The purities and structures of these compounds were identified by high-performance liquid chromatography, electrospray ionization mass spectrometry, (1)H and (13)C NMR spectroscopy. This study demonstrates that high-speed counter-current chromatography is a useful and flexible tool for the separation of components from a complex sample.

  4. Proteomic Analysis of Mecistocirrus digitatus and Haemonchus contortus Intestinal Protein Extracts and Subsequent Efficacy Testing in a Vaccine Trial

    PubMed Central

    Dicker, Alison J.; Inglis, Neil F.; Manson, Erin D. T.; Subhadra, Subhra; Illangopathy, Manikkavasagan; Muthusamy, Raman; Knox, David P.

    2014-01-01

    Background Gastrointestinal nematode infections, such as Haemonchus contortus and Mecistocirrus digitatus, are ranked in the top twenty diseases affecting small-holder farmers' livestock, yet research into M. digitatus, which infects cattle and buffalo in Asia is limited. Intestine-derived native protein vaccines are effective against Haemonchus, yet the protective efficacy of intestine-derived M. digitatus proteins has yet to be determined. Methodology/Principal Findings A simplified protein extraction protocol (A) is described and compared to an established method (B) for protein extraction from H. contortus. Proteomic analysis of the H. contortus and M. digitatus protein extracts identified putative vaccine antigens including aminopeptidases (H11), zinc metallopeptidases, glutamate dehydrogenase, and apical gut membrane polyproteins. A vaccine trial compared the ability of the M. digitatus extract and two different H. contortus extracts to protect sheep against H. contortus challenge. Both Haemonchus fractions (A and B) were highly effective, reducing cumulative Faecal Egg Counts (FEC) by 99.19% and 99.89% and total worm burdens by 87.28% and 93.64% respectively, compared to the unvaccinated controls. There was no effect on H. contortus worm burdens following vaccination with the M. digitatus extract and the 28.2% reduction in cumulative FEC was not statistically significant. However, FEC were consistently lower in the M. digitatus extract vaccinates compared to the un-vaccinated controls from 25 days post-infection. Conclusions/Significance Similar, antigenically cross-reactive proteins are found in H. contortus and M. digitatus; this is the first step towards developing a multivalent native vaccine against Haemonchus species and M. digitatus. The simplified protein extraction method could form the basis for a locally produced vaccine against H. contortus and, possibly M. digitatus, in regions where effective cold chains for vaccine distribution are limited

  5. Inhibitory effects of 1alpha, 25dihydroxyvitamin D3 and Ajuga iva extract on oxidative stress, toxicity and hypo-fertility in diabetic rat testes.

    PubMed

    Hamden, K; Carreau, S; Jamoussi, K; Ayadi, F; Garmazi, F; Mezgenni, N; Elfeki, A

    2008-09-01

    The aim of the current study is to investigate the therapeutic and preventive effects of 1alpha, 25dihydroxyvitaminD3 (1,25 (OH)2 D3) and Afuga iva (AI) extract on diabetes toxicity in rats testes. Thus diabetic rats were treated with 1alpha, 25dihydroxyvitaminD3 or Ajuga iva extract as both therapeutic and preventive treatments on diabetes toxicity in rats testes. Our results showed that diabetes induced a decrease in testosterone and 17beta-estradiol levels in testes and plasma. Besides, a fall in testicular antioxidant capacity appeared by a decrease in both antioxidant (superoxide dismutase (SOD), catalase (CAT) and glutathione peroxidase (GPx) activities) and nonenzymatic antioxidant (copper (Cu), magnesium (Mg) and iron (Fe) levels). All theses changes enhanced testicular toxicity (increase in testicular aspartate amino transaminase (AST), alanine amino transaminase (ALT), lactate dehydrogenase (LDH) activities and the lipid peroxidation and triglyceride (TG) levels). In addition, a decrease in testicular total cholesterol (TCh) level was observed in diabetic rats testes. All the changes lead to a decrease in the total number and mobility of epididymal spermatozoa. The administration of 1alpha,25dihydroxyvitaminD3 and Ajuga iva extract three weeks before and after diabetes induction interfered and prevented diabetes toxicity in the reproductive system. 1,25 (OH)2 D3 and Ajuga iva extract blunted all changes observed in diabetic rats. To sum up, the data suggested that 1,25 (OH)2 D3 and Ajuga iva extract have a protective effect on alloxan-induced damage in reproductive system by enhancing the testosterone and 17beta-estradiol levels, consequently protecting from oxidative stress, cellular toxicity and maintaining the number and motility of spermatozoids.

  6. An inkjet-printed microfluidic device for liquid-liquid extraction.

    PubMed

    Watanabe, Masashi

    2011-04-01

    A microfluidic device for liquid-liquid extraction was quickly produced using an office inkjet printer. An advantage of this method is that normal end users, who are not familiar with microfabrication, can produce their original microfluidic devices by themselves. In this method, the printer draws a line on a hydrophobic and oil repellent surface using hydrophilic ink. This line directs a fluid, such as water or xylene, to form a microchannel along the printed line. Using such channels, liquid-liquid extraction was successfully performed under concurrent and countercurrent flow conditions.

  7. Development of the front end test stand and vessel for extraction and source plasma analyses negative hydrogen ion sources at the Rutherford Appleton Laboratory

    SciTech Connect

    Lawrie, S. R.; Faircloth, D. C.; Letchford, A. P.; Perkins, M.; Whitehead, M. O.; Wood, T.; Gabor, C.; Back, J.

    2014-02-15

    The ISIS pulsed spallation neutron and muon facility at the Rutherford Appleton Laboratory (RAL) in the UK uses a Penning surface plasma negative hydrogen ion source. Upgrade options for the ISIS accelerator system demand a higher current, lower emittance beam with longer pulse lengths from the injector. The Front End Test Stand is being constructed at RAL to meet the upgrade requirements using a modified ISIS ion source. A new 10% duty cycle 25 kV pulsed extraction power supply has been commissioned and the first meter of 3 MeV radio frequency quadrupole has been delivered. Simultaneously, a Vessel for Extraction and Source Plasma Analyses is under construction in a new laboratory at RAL. The detailed measurements of the plasma and extracted beam characteristics will allow a radical overhaul of the transport optics, potentially yielding a simpler source configuration with greater output and lifetime.

  8. Assessment of the influence of traffic-related particles in urban dust using sequential selective extraction and oral bioaccessibility tests.

    PubMed

    Patinha, C; Durães, N; Sousa, P; Dias, A C; Reis, A P; Noack, Y; Ferreira da Silva, E

    2015-08-01

    Urban dust is a heterogeneous mix, where traffic-related particles can combine with soil mineral compounds, forming a unique and site-specific material. These traffic-related particles are usually enriched in potentially harmful elements, enhancing the health risk for population by inhalation or ingestion. Urban dust samples from Estarreja city and traffic-related particles (brake dust and white traffic paint) were studied to understand the relative contribution of the traffic particles in the geochemical behaviour of urban dust and to evaluate the long-term impacts of the metals on an urban environment, as well as the risk to the populations. It was possible to distinguish two groups of urban dust samples according to Cu behaviour: (1) one group with low amounts of fine particles (<38 µm), low contents of organic material, high percentage of Cu in soluble phases, and low Cu bioaccessible fraction (Bf) values. This group showed similar chemical behaviour with the brake dust samples of low- to mid-range car brands (with more than 10 years old), composed by coarser wear particles; and (2) another group with greater amounts of fine particles (<38 µm), with low percentage of Cu associated with soluble phases, and with greater Cu Bf values. This group behaved similar to those found for brake dust of mid- to high-range car brands (with less than 10 years old). The results obtained showed that there is no direct correlation between the geoavailability of metals estimated by sequential selective chemical extraction (SSCE) and the in vitro oral bioaccessibility (UBM) test. Thus, oral bioaccessibility of urban dust is site specific. Geoavailability was greatly dependent on particle size, where the bioaccessibility tended to increase with a reduction in particle diameter. As anthropogenic particles showed high metal concentration and a smaller size than mineral particles, urban dusts are of major concern to the populations' health, since fine particles are easily re

  9. Assessment of the influence of traffic-related particles in urban dust using sequential selective extraction and oral bioaccessibility tests.

    PubMed

    Patinha, C; Durães, N; Sousa, P; Dias, A C; Reis, A P; Noack, Y; Ferreira da Silva, E

    2015-08-01

    Urban dust is a heterogeneous mix, where traffic-related particles can combine with soil mineral compounds, forming a unique and site-specific material. These traffic-related particles are usually enriched in potentially harmful elements, enhancing the health risk for population by inhalation or ingestion. Urban dust samples from Estarreja city and traffic-related particles (brake dust and white traffic paint) were studied to understand the relative contribution of the traffic particles in the geochemical behaviour of urban dust and to evaluate the long-term impacts of the metals on an urban environment, as well as the risk to the populations. It was possible to distinguish two groups of urban dust samples according to Cu behaviour: (1) one group with low amounts of fine particles (<38 µm), low contents of organic material, high percentage of Cu in soluble phases, and low Cu bioaccessible fraction (Bf) values. This group showed similar chemical behaviour with the brake dust samples of low- to mid-range car brands (with more than 10 years old), composed by coarser wear particles; and (2) another group with greater amounts of fine particles (<38 µm), with low percentage of Cu associated with soluble phases, and with greater Cu Bf values. This group behaved similar to those found for brake dust of mid- to high-range car brands (with less than 10 years old). The results obtained showed that there is no direct correlation between the geoavailability of metals estimated by sequential selective chemical extraction (SSCE) and the in vitro oral bioaccessibility (UBM) test. Thus, oral bioaccessibility of urban dust is site specific. Geoavailability was greatly dependent on particle size, where the bioaccessibility tended to increase with a reduction in particle diameter. As anthropogenic particles showed high metal concentration and a smaller size than mineral particles, urban dusts are of major concern to the populations' health, since fine particles are easily re

  10. Extraction and recovery of plutonium and americium from nitric acid waste solutions by the TRUEX process - continuing development studies

    SciTech Connect

    Leonard, R.A.; Vandegrift, G.F.; Kalina, D.G.; Fischer, D.F.; Bane, R.W.; Burris, L.; Horwitz, E.P.; Chiarisia, R.; Diamond, H.

    1985-09-01

    This report summarizes the work done to date on the application of the TRUEX solvent extraction process for removing and separately recovering plutonium and americium from a nitric acid waste solution containing these elements, uranium, and a complement of inert metal ions. This simulated waste stream is typical of a raffinate from a tributyl phosphate (TBP)-based solvent extraction process for removing uranium and plutonium from dissolved plutonium-containing metallurgical scrap. The TRUEX process solvent in these experiments was a solution of TBP and octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) dissolved in carbon tetrachloride. A flowsheet was designed on the basis of measured batch distribution ratios to reduce the TRU content of the solidified raffinate to less than or equal to 10 nCi/g and was tested in a countercurrent experiment performed in a 14-stage Argonne-model centrifugal contractor. The process solvent was recycled without cleanup. An unexpectedly high evaporative loss of CCl/sub 4/ resulted in concentration of the active extractant, CMPO, to nearly 0.30M in the solvent. Results are consistent with this higher CMPO concentration. The raffinate contained only 2 nCi/g of TRU, but the higher CMPO concentration resulted in reduced effectiveness in the stripping of americium from the solvent. Conditions can be easily adjusted to give high yields and good separation of americium and plutonium. Experimental studies of the hydrolytic and gamma-radiolytic degradation of the TRUEX-CCl/sub 4/ showed that solvent degradation would be (1) minimal for a year of processing this typical feed, which contained no fission products, and (2) could be explained almost entirely by hydrolytic and radiolytic damage to TBP. Even for gross amounts of solvent damage, scrubbing with aqueous sodium carbonate solution restored the original americium extraction and stripping capability of the solvent. 43 refs., 5 figs., 36 tabs.

  11. Countercurrent Chromatographic Separation of Proteins Using an Eccentric Coiled Column with Synchronous and Nonsynchronous Type-J Planetary Motions

    PubMed Central

    SHINOMIYA, Kazufusa; YOSHIDA, Kazunori; TOKURA, Koji; TSUKIDATE, Etsuhiro; YANAGIDAIRA, Kazuhiro; ITO, Yoichiro

    2015-01-01

    Protein separation was performed using the high-speed counter-current chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution. PMID:25765276

  12. Enantioseparation of racemic trans-δ-viniferin using high speed counter-current chromatography based on induced circular dichroism technology.

    PubMed

    Han, Chao; Xu, Jinfang; Wang, Xiaobing; Xu, Xiaoming; Luo, Jianguang; Kong, Lingyi

    2014-01-10

    A preparative chiral high speed counter-current chromatography (HSCCC) method based on induced circular dichroism (ICD) spectrum was developed to separate trans-δ-viniferin (TVN) enantiomers successfully. The important parameters for the chiral HSCCC separation process, including the type of chiral selector (CS), the concentration of chiral selector and the equilibrium temperature, were optimized using induced circular dichroism spectrum. The final separation procedure was established with a biphasic solvent system composed of n-hexane-ethyl acetate-25 mmol L(-1) hydroxypropyl-β-cyclodextrin aqueous solution (5:5:10, v/v/v) in the head-to-tail elution mode at 5 °C. Under optimum chiral HSCCC separation conditions, 8.2mg of (7S, 8S)-TVN (1) and 9.4 mg of (7R, 8R)-TVN (2) were successfully separated from 20mg TVN enantiomers with the purity of 99.51% and 99.36%, respectively.

  13. Preparative isolation and purification of three sesquiterpenoid lactones from Eupatorium lindleyanum DC. by high-speed counter-current chromatography.

    PubMed

    Yan, Guilong; Ji, Lilian; Luo, Yuming; Hu, Yonghong

    2012-07-27

    A high-speed counter-current chromatography (HSCCC) method was established for the preparative separation of three sesquiterpenoid lactones from Eupatorium lindleyanum DC. The two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:4:2:3, v/v/v/v) was selected. From 540 mg of the n-butanol fraction of Eupatorium lindleyanum DC., 10.8 mg of 3β-hydroxy-8β-[4'-hydroxytigloyloxy]-costunolide, 17.9 mg of eupalinolide A and 19.3 mg of eupalinolide B were obtained in a one-step HSCCC separation, with purities of 91.8%, 97.9% and 97.1%, respectively, as determined by HPLC. Their structures were further identified by ESI-MS and ¹H-NMR.

  14. Comparison of preparative reversed phase liquid chromatography and countercurrent chromatography for the kilogram scale purification of crude spinetoram insecticide.

    PubMed

    DeAmicis, Carl; Edwards, Neil A; Giles, Michael B; Harris, Guy H; Hewitson, Peter; Janaway, Lee; Ignatova, Svetlana

    2011-09-01

    Reversed phase HPLC (RP-HPLC) and high performance countercurrent chromatography (HPCCC) were compared for the pilot scale purification of two semi-synthetic spinosyns, spinetoram-J and spinetoram-L, the major components of the commercial insecticide spinetoram. Two, independently performed, 1 kg, purification campaigns were compared. Each method resulted in the isolation of both components at a purity of >97% and yields for spinetoram-J and spinetoram-L of >93% and ≥ 63% of theoretical, respectively. The HPCCC process produced a 2-fold higher throughput and consumed approximately 70% less solvent than preparative scale RP-HPLC, the volume of product containing fractions from HPCCC amounted to 7% of that produced by HPLC and so required much less post-run processing.

  15. Effects of Concept Map Extraction and a Test-Based Diagnostic Environment on Learning Achievement and Learners' Perceptions

    ERIC Educational Resources Information Center

    Lin, Yu-Shih; Chang, Yi-Chun; Liew, Keng-Hou; Chu, Chih-Ping

    2016-01-01

    Computerised testing and diagnostics are critical challenges within an e-learning environment, where the learners can assess their learning performance through tests. However, a test result based on only a single score is insufficient information to provide a full picture of learning performance. In addition, because test results implicitly…

  16. Significance of the Bohr effect for tissue oxygenation in a model with counter-current blood flow.

    PubMed

    Kobayashi, H; Pelster, B; Piiper, J; Scheid, P

    1989-06-01

    Counter-current arrangement of afferent and efferent blood flow in tissues is commonly considered to be detrimental to tissue oxygenation, since O2 diffusion would shunt O2 away from the tissue. We have investigated the combined effects of counter-current CO2 and O2 exchange in a simple model, paying particular attention to the Bohr effect. We have obtained the following main results. (1) Back-diffusion of CO2 leads to increasing CO2 partial pressure (PCO2) and CO2 content along the afferent vessel. This is enhanced when fixed acid is released by the tissue into the venous blood, e.g. during hypoxia, which leads to a further PCO2 increase therein. (2) The increasing PCO2, with concomitant decrease in pH, in the afferent blood leads to a decrease in blood O2 affinity (Bohr effect) and thus results in increased PO2. (3) The resulting O2 diffusion shunt diminishes the O2 content in afferent blood, but for most conditions its PO2 remains higher than without the Bohr effect. (4) During hypoxia, both the PO2 in blood reaching the tissue (Pta) as well as in that leaving it (Ptv) are significantly elevated above the level without the Bohr effect. Moreover, with fixed acid release both Pta and Ptv for O2 can be higher than the arterial PO2 value. (5) During hyperoxia, O2 diffusion shunt prevents the tissue PO2 levels from increasing to levels that might be regarded as toxic. It is concluded that a diffusion shunt in tissues stabilizes the O2 partial pressure at the tissue when it varies in arterial blood (hypoxia or hyperoxia).

  17. Advanced fuel hydrocarbon remediation national test location. Demonstration of hot air vapor extraction for fuel hydrocarbon cleanup

    SciTech Connect

    Heath, J.; Lory, E.

    1997-03-01

    Hot air vapor extration (HAVE) is a fast track, innovative environmental cleanup technolgy that uses a combination of thermal, heap pile, and vapor extraction techniques to remove and destroy hydrocarbon contamination in soil. This technology is very effective in cleaning soils contaminated with gasoline, diesel, heavy oil, and polycyclic aromatic hydrocarbons (PAH).

  18. On-line purity monitoring in high-speed counter-current chromatography: application of HSCCC-HPLC-DAD for the preparation of 5-HMF, neomangiferin and mangiferin from Anemarrhena asphodeloides Bunge.

    PubMed

    Zhou, Tingting; Zhu, Zhenyu; Wang, Chen; Fan, Guorong; Peng, Jinyong; Chai, Yifeng; Wu, Yutian

    2007-05-01

    An efficient on-line purity monitoring strategy based on on-line coupling of high-speed counter-current chromatography (HSCCC) with high-performance liquid chromatography-diode array detection (HPLC-DAD) was successfully applied for the first time to the isolation and purification of 5-hydroxymethyl-furancarboxaldehyde (5-HMF), mangiferin and neomangiferin from the Chinese medicinal plant Anemarrhena asphodeloides Bunge, a plant used in the traditional Chinese medicine. The introduction of on-line purity monitoring in HSCCC has greatly improved the efficiency of this technique by overcoming the drawbacks of post-purification sample handling in HSCCC isolation. The effluent from the outlet of HSCCC was split into two parts, and one was collected, while the other was introduced directly through a switch valve into a HPLC-DAD system for purity monitoring. Using this method the desired fractions with high purities could be collected. From 600 mg partially purified extract, 165.6 mg neomangiferin and 292.8 mg mangiferin with purities of 98.9 and 99.5%, respectively, were obtained with a two-phase solvent system composed of n-butanol-water (1:1, v/v) by increasing the flow-rate of the mobile phase stepwise from 1.0 to 2.2 ml min(-1) after 210 min. A 17.1mg 5-HMF with purity of 96.6% was also isolated for the first time.

  19. Separation and preparation of 6-gingerol from molecular distillation residue of Yunnan ginger rhizomes by high-speed counter-current chromatography and the antioxidant activity of ginger oils in vitro.

    PubMed

    Gan, Zhilin; Liang, Zheng; Chen, Xiaosong; Wen, Xin; Wang, Yuxiao; Li, Mo; Ni, Yuanying

    2016-02-01

    Molecular distillation residue (MD-R) from ginger had the most total phenol content of 247.6mg gallic acid equivalents per gram (GAE/g) among the ginger oils. High-speed counter-current chromatography (HSCCC) technique in semi-preparative scale was successfully performed in separation and purification of 6-gingerol from MD-R by using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (10:2:5:7, v/v/v/v). The target compound was isolated, collected, purified by HSCCC in the head-tail mode, and then analyzed by HPLC. A total of 90.38±0.53mg 6-gingerol was obtained from 600mg MD-R, with purity of 99.6%. In addition, the structural identification of 6-gingerol was performed by EI/MS, (1)H NMR and (13)C NMR. Moreover, the orders of antioxidant activity were vitamin E (VE)>supercritical fluid extraction oleoresin (SFE-O)=MD-R=6-gingerol>molecular distillation essential oil (MD-EO) and butylated hydroxytoluene (BHT)=VE>6-gingerol>MD-R=SFE-O>MD-EO, respectively in 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) scavenging and β-Carotene bleaching.

  20. Separation and preparation of 6-gingerol from molecular distillation residue of Yunnan ginger rhizomes by high-speed counter-current chromatography and the antioxidant activity of ginger oils in vitro.

    PubMed

    Gan, Zhilin; Liang, Zheng; Chen, Xiaosong; Wen, Xin; Wang, Yuxiao; Li, Mo; Ni, Yuanying

    2016-02-01

    Molecular distillation residue (MD-R) from ginger had the most total phenol content of 247.6mg gallic acid equivalents per gram (GAE/g) among the ginger oils. High-speed counter-current chromatography (HSCCC) technique in semi-preparative scale was successfully performed in separation and purification of 6-gingerol from MD-R by using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (10:2:5:7, v/v/v/v). The target compound was isolated, collected, purified by HSCCC in the head-tail mode, and then analyzed by HPLC. A total of 90.38±0.53mg 6-gingerol was obtained from 600mg MD-R, with purity of 99.6%. In addition, the structural identification of 6-gingerol was performed by EI/MS, (1)H NMR and (13)C NMR. Moreover, the orders of antioxidant activity were vitamin E (VE)>supercritical fluid extraction oleoresin (SFE-O)=MD-R=6-gingerol>molecular distillation essential oil (MD-EO) and butylated hydroxytoluene (BHT)=VE>6-gingerol>MD-R=SFE-O>MD-EO, respectively in 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) scavenging and β-Carotene bleaching. PMID:26773887