Isolation of friedelin from black condensate of cork.

PubMed

Pires, Ricardo A; Aroso, Ivo; Silva, Susana P; Mano, João F; Reis, Rui L

2011-11-01

Black condensates (BC) are wastes of the insulation corkboard industry that contain several valuable chemicals, including friedelin, a terpene exhibiting biological activity. Herein, we report a straightforward procedure to extract friedelin from BC. Using this procedure, we were able to extract friedelin with yields between 0.4% and 2.9% and to further purify it obtaining purities from 77.0% to 99.3% (HPLC). The initial BC (2 batches), extracted raw product and purified friedelin were analyzed using FTIR. The extraction yields and purities were found to be directly related to the intensity of the carbonyl vibration at 1713 cm(-1) in the FTIR spectrum of the used BC batch. Therefore, these spectra can be used to screen and select BC batches suitable for friedelin extraction.

Enzyme-assisted supercritical carbon dioxide extraction of black pepper oleoresin for enhanced yield of piperine-rich extract.

PubMed

Dutta, Sayantani; Bhattacharjee, Paramita

2015-07-01

Black pepper (Piper nigrum L.), the King of Spices is the most popular spice globally and its active ingredient, piperine, is reportedly known for its therapeutic potency. In this work, enzyme-assisted supercritical carbon dioxide (SC-CO2) extraction of black pepper oleoresin was investigated using α-amylase (from Bacillus licheniformis) for enhanced yield of piperine-rich extract possessing good combination of phytochemical properties. Optimization of the extraction parameters (without enzyme), mainly temperature and pressure, was conducted in both batch and continuous modes and the optimized conditions that provided the maximum yield of piperine was in the batch mode, with a sample size of 20 g of black pepper powder (particle diameter 0.42 ± 0.02 mm) at 60 °C and 300 bar at 2 L/min of CO2 flow. Studies on activity of α-amylase were conducted under these optimized conditions in both batch and continuous modes, with varying amounts of lyophilized enzyme (2 mg, 5 mg and 10 mg) and time of exposure of the enzyme to SC-CO2 (2.25 h and 4.25 h). The specific activity of the enzyme increased by 2.13 times when treated in the continuous mode than in the batch mode (1.25 times increase). The structural changes of the treated enzymes were studied by (1)H NMR analyses. In case of α-amylase assisted extractions of black pepper, both batch and continuous modes significantly increased the yields and phytochemical properties of piperine-rich extracts; with higher increase in batch mode than in continuous. Copyright © 2014 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

An approach to optimize the batch mixing process for improving the quality consistency of the products made from traditional Chinese medicines*

PubMed Central

Yan, Bin-jun; Qu, Hai-bin

2013-01-01

The efficacy of traditional Chinese medicine (TCM) is based on the combined effects of its constituents. Variation in chemical composition between batches of TCM has always been the deterring factor in achieving consistency in efficacy. The batch mixing process can significantly reduce the batch-to-batch quality variation in TCM extracts by mixing them in a well-designed proportion. However, reducing the quality variation without sacrificing too much of the production efficiency is one of the challenges. Accordingly, an innovative and practical batch mixing method aimed at providing acceptable efficiency for industrial production of TCM products is proposed in this work, which uses a minimum number of batches of extracts to meet the content limits. The important factors affecting the utilization ratio of the extracts (URE) were studied by simulations. The results have shown that URE was affected by the correlation between the contents of constituents, and URE decreased with the increase in the number of targets and the relative standard deviations of the contents. URE could be increased by increasing the number of storage tanks. The results have provided a reference for designing the batch mixing process. The proposed method has possible application value in reducing the quality variation in TCM and providing acceptable production efficiency simultaneously. PMID:24190450

An approach to optimize the batch mixing process for improving the quality consistency of the products made from traditional Chinese medicines.

PubMed

Yan, Bin-jun; Qu, Hai-bin

2013-11-01

The efficacy of traditional Chinese medicine (TCM) is based on the combined effects of its constituents. Variation in chemical composition between batches of TCM has always been the deterring factor in achieving consistency in efficacy. The batch mixing process can significantly reduce the batch-to-batch quality variation in TCM extracts by mixing them in a well-designed proportion. However, reducing the quality variation without sacrificing too much of the production efficiency is one of the challenges. Accordingly, an innovative and practical batch mixing method aimed at providing acceptable efficiency for industrial production of TCM products is proposed in this work, which uses a minimum number of batches of extracts to meet the content limits. The important factors affecting the utilization ratio of the extracts (URE) were studied by simulations. The results have shown that URE was affected by the correlation between the contents of constituents, and URE decreased with the increase in the number of targets and the relative standard deviations of the contents. URE could be increased by increasing the number of storage tanks. The results have provided a reference for designing the batch mixing process. The proposed method has possible application value in reducing the quality variation in TCM and providing acceptable production efficiency simultaneously.

Are allergen batch differences and the use of double skin prick test important?

PubMed

Thomsen, Gert F; Schlünssen, Vivi; Skadhauge, Lars R; Malling, Tine Halsen; Sherson, David L; Omland, Øyvind; Sigsgaard, Torben

2015-04-09

Skin prick tests (SPT) are widely used both in clinical diagnostics and in research. The standardization of allergen extracts is well documented to be crucial for the validity of SPT, whereas less emphasis has been placed on reproducibility and the SPT procedure itself. The objectives of this study are to clarify how the double skin prick test procedure influence the sensitivity and specificity of the test and to analyse the differences in weal size in skin prick tests between two batches of allergen extracts from the same vendor. The association between rhinitis and SPT was assessed among 1135 persons from a general population sample. SPT was performed twice with 10 common aeroallergens. In a subsample of 90 persons SPT was performed simultaneously with five of the allergens using different batches. Thirty percent had at least one positive SPT. Among asthmatics this number was 62%. Only minor differences were seen between the sizes of two weals from the same batch. A second SPT with the same batch did not change the association between rhinitis and sensitization. When performing SPT with two different batches disagreement was observed in 2% (Birch) to 11% (Cat) of the subjects. Performing SPT twice with the same allergen batch does not enhance the validity of the test, and value of double testing can be questioned. Considerable differences in SPT response with different batches from the same manufacturer were observed. Thus inter batch differences in allergen extracts might be a source of variability.

Microwave superheated water extraction of polysaccharides from spent coffee grounds.

PubMed

Passos, Cláudia P; Coimbra, Manuel A

2013-04-15

The spent coffee grounds (SCG) are a food industry by-product that can be used as a rich source of polysaccharides. In the present work, the feasibility of microwave superheated water extraction of polysaccharides from SCG was studied. Different ratios of mass of SCG to water, from 1:30 to 1:5 (g:mL) were used for a total volume of 80 mL. Although the amount of material extracted/batch (MAE1) increased with the increase of the concentration of the sample, the amount of polysaccharides achieved a maximum of 0.57 g/batch for 1:10. Glycosidic-linkage composition showed that all extraction conditions allowed to obtain mainly arabinogalactans. When the unextracted insoluble material was re-extracted under the same conditions (MAE2), a further extraction of polysaccharides was observed (0.34 g/batch for 1:10), mainly galactomannans. Also, a high amount of oligosaccharides, mainly derived from galactomannans, can be obtained in MAE2 (0.96 g/batch for 1:10). This technology allows to obtain galactomannans and arabinogalactans in proportions that are dependent on the operating conditions. Copyright © 2013 Elsevier Ltd. All rights reserved.

Tracing Injection Fluids in Engineered Geothermal Systems

NASA Astrophysics Data System (ADS)

Rose, P. E.; Leecaster, K.; Mella, M.; Ayling, B.; Bartl, M. H.

2011-12-01

The reinjection of produced fluids is crucial to the effective management of geothermal reservoirs, since it provides a mechanism for maintaining reservoir pressures while allowing for the disposal of a toxic byproduct. Tracers are essential to the proper location of injection wells since they are the only known tool for reliably characterizing the flow patterns of recirculated fluids. If injection wells are placed too close to production wells, then reinjected fluids do not have sufficient residence time to extract heat from the reservoir and premature thermal breakthrough results. If injection wells are placed too far away, then the reservoir risks unacceptable pressure loss. Several thermally stable compounds from a family of very detectable fluorescent organic compounds (the naphthalene sulfonates) were characterized and found to be effective for use as geothermal tracers. Through batch-autoclave reactions, their Arrhenius pseudo-first-order decay-rate constants were determined. An analytical method was developed that allows for the laboratory determination of concentrations in the low parts-per-trillion range. Field experiments in numerous geothermal reservoirs throughout the world have confirmed the laboratory findings. Whereas conservative tracers such as the naphthalene sulfonates are effective tools for indicating interwell flow patterns and for measuring reservoir pore volumes, 'reactive' tracers can be used to constrain fracture surface area, which is the effective area for heat extraction. This is especially important for engineered geothermal system (EGS) wells, since reactive tracers can be used to measure fracture surface area immediately after drilling and while the well stimulation equipment is still on site. The reactive properties of these tracers that can be exploited to constrain fracture surface area are reversible sorption, contrasting diffusivity, and thermal decay. Laboratory batch- and flow-reactor experiments in combination with numerical simulation studies have served to identify candidate compounds for use as reactive tracers. An emerging class of materials that show promise for use as geothermal and EGS tracers are colloidal nanocrystals (quantum dots). These are semiconductor particles that fluoresce as a function of particle size. Preliminary laboratory experimentation has demonstrated that these thermally stable, water-soluble particles can serve as conservative tracers for geothermal applications. Likewise, they show promise as potential reactive tracers, since their surfaces can be modified to be reversibly sorptive and their diameters are sufficiently large to allow for contrasts in diffusivity with solute tracers.

[Study of blending method for the extracts of herbal plants].

PubMed

Liu, Yongsuo; Cao, Min; Chen, Yuying; Hu, Yuzhu; Wang, Yiming; Luo, Guoan

2006-03-01

The irregularity in herbal plant composition is influenced by multiple factors. As for quality control of traditional Chinese medicine, the most critical challenge is to ensure the dosage content uniformity. This content uniformity can be improved by blending different batches of the extracts of herbal plants. Nonlinear least-squares regression was used to calculate the blending coefficient, which means no great absolute differences allowed for all ingredients. For traditional Chinese medicines, even relatively smaller differences could present to be very important for all the ingredients. The auto-scaling pretreatment was used prior to the calculation of the blending coefficients. The pretreatment buffered the characteristics of individual data for the ingredients in different batches, so an improved auto-scaling pretreatment method was proposed. With the improved auto-scaling pretreatment, the relative. differences decreased after blending different batches of extracts of herbal plants according to the reference samples. And the content uniformity control of the specific ingredients could be achieved by the error control coefficient. In the studies for the extracts of fructus gardeniae, the relative differences of all the ingredients is less than 3% after blending different batches of the extracts. The results showed that nonlinear least-squares regression can be used to calculate the blending coefficient of the herbal plant extracts.

[Application of genetic algorithm in blending technology for extractions of Cortex Fraxini].

PubMed

Yang, Ming; Zhou, Yinmin; Chen, Jialei; Yu, Minying; Shi, Xiufeng; Gu, Xijun

2009-10-01

To explore the feasibility of genetic algorithm (GA) on multiple objective blending technology for extractions of Cortex Fraxini. According to that the optimization objective was the combination of fingerprint similarity and the root-mean-square error of multiple key constituents, a new multiple objective optimization model of 10 batches extractions of Cortex Fraxini was built. The blending coefficient was obtained by genetic algorithm. The quality of 10 batches extractions of Cortex Fraxini that after blending was evaluated with the finger print similarity and root-mean-square error as indexes. The quality of 10 batches extractions of Cortex Fraxini that after blending was well improved. Comparing with the fingerprint of the control sample, the similarity was up, but the degree of variation is down. The relative deviation of the key constituents was less than 10%. It is proved that genetic algorithm works well on multiple objective blending technology for extractions of Cortex Fraxini. This method can be a reference to control the quality of extractions of Cortex Fraxini. Genetic algorithm in blending technology for extractions of Chinese medicines is advisable.

CONVERTING FROM BATCH TO CONTINUOUS INTENSIFIED PROCESSING IN THE STT? REACTOR

EPA Science Inventory

The fluid dynamics, the physical dimensions and characteristics of the reaction zones of continuous process intensification reactors are often quite different from those of the batch reactors they replace. Understanding these differences is critical to the successful transit...

Real-time imaging as an emerging process analytical technology tool for monitoring of fluid bed coating process.

PubMed

Naidu, Venkata Ramana; Deshpande, Rucha S; Syed, Moinuddin R; Wakte, Pravin S

2018-07-01

A direct imaging system (Eyecon TM ) was used as a Process Analytical Technology (PAT) tool to monitor fluid bed coating process. Eyecon TM generated real-time onscreen images, particle size and shape information of two identically manufactured laboratory-scale batches. Eyecon TM has accuracy of measuring the particle size increase of ±1 μm on particles in the size range of 50-3000 μm. Eyecon TM captured data every 2 s during the entire process. The moving average of D90 particle size values recorded by Eyecon TM were calculated for every 30 min to calculate the radial coating thickness of coated particles. After the completion of coating process, the radial coating thickness was found to be 11.3 and 9.11 μm, with a standard deviation of ±0.68 and 1.8 μm for Batch 1 and Batch 2, respectively. The coating thickness was also correlated with percent weight build-up by gel permeation chromatography (GPC) and dissolution. GPC indicated weight build-up of 10.6% and 9.27% for Batch 1 and Batch 2, respectively. In conclusion, weight build-up of 10% can also be correlated with 10 ± 2 μm increase in the coating thickness of pellets, indicating the potential applicability of real-time imaging as an endpoint determination tool for fluid bed coating process.

Phosphate-Induced Immobilization of Uranium in Hanford Sediments.

PubMed

Pan, Zezhen; Giammar, Daniel E; Mehta, Vrajesh; Troyer, Lyndsay D; Catalano, Jeffrey G; Wang, Zheming

2016-12-20

Phosphate can be added to subsurface environments to immobilize U(VI) contamination. The efficacy of immobilization depends on the site-specific groundwater chemistry and aquifer sediment properties. Batch and column experiments were performed with sediments from the Hanford 300 Area in Washington State and artificial groundwater prepared to emulate the conditions at the site. Batch experiments revealed enhanced U(VI) sorption with increasing phosphate addition. X-ray absorption spectroscopy measurements of samples from the batch experiments found that U(VI) was predominantly adsorbed at conditions relevant to the column experiments and most field sites (low U(VI) loadings, <25 μM), and U(VI) phosphate precipitation occurred only at high initial U(VI) (>25 μM) and phosphate loadings. While batch experiments showed the transition of U(VI) uptake from adsorption to precipitation, the column study was more directly relevant to the subsurface environment because of the high solid:water ratio in the column and the advective flow of water. In column experiments, nearly six times more U(VI) was retained in sediments when phosphate-containing groundwater was introduced to U(VI)-loaded sediments than when the groundwater did not contain phosphate. This enhanced retention persisted for at least one month after cessation of phosphate addition to the influent fluid. Sequential extractions and laser-induced fluorescence spectroscopy of sediments from the columns suggested that the retained U(VI) was primarily in adsorbed forms. These results indicate that in situ remediation of groundwater by phosphate addition provides lasting benefit beyond the treatment period via enhanced U(VI) adsorption to sediments.

Phosphate-Induced Immobilization of Uranium in Hanford Sediments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan, Zezhen; Giammar, Daniel E.; Mehta, Vrajesh

2016-12-20

Phosphate can be added to subsurface environments to immobilize U(VI) contamination. The efficacy of immobilization depends on the site-specific groundwater chemistry and aquifer sediment properties. Batch and column experiments were performed with sediments from the Hanford 300 Area in Washington State and artificial groundwater prepared to emulate the conditions at the site. Batch experiments revealed enhanced U(VI) sorption with increasing phosphate addition. X-ray absorption spectroscopy measurements of samples from the batch experiments found that U(VI) was predominantly adsorbed at conditions relevant to the column experiments and most field sites (low U(VI) loadings, <25 μM), and U(VI) phosphate precipitation occurred onlymore » at high initial U(VI) (>25 μM) and phosphate loadings. While batch experiments showed the transition of U(VI) uptake from adsorption to precipitation, the column study was more directly relevant to the subsurface environment because of the high solid:water ratio in the column and the advective flow of water. In column experiments, nearly six times more U(VI) was retained in sediments when phosphate-containing groundwater was introduced to U(VI)-loaded sediments than when the groundwater did not contain phosphate. This enhanced retention persisted for at least one month after cessation of phosphate addition to the influent fluid. Sequential extractions and laser-induced fluorescence spectroscopy of sediments from the columns suggested that the retained U(VI) was primarily in adsorbed forms. These results indicate that in situ remediation of groundwater by phosphate addition provides lasting benefit beyond the treatment period via enhanced U(VI) adsorption to sediments.« less

Phosphate-Induced Immobilization of Uranium in Hanford Sediments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan, Zezhen; Giammar, Daniel E.; Mehta, Vrajesh

2016-12-20

Phosphate can be added to subsurface environments to immobilize U(VI) contamination. The efficacy of immobilization depends on the site-specific groundwater chemistry and aquifer sediment properties. Batch and column experiments were performed with sediments from the Hanford 300 Area in Washington State and artificial groundwater prepared to emulate the conditions at the site. Batch experiments revealed enhanced U(VI) sorption with increasing phosphate addition. X-ray absorption spectroscopy measurements of samples from the batch experiments found that U(VI) was predominantly adsorbed at conditions relevant to the column experiments and most field sites (low U(VI) loadings, <25 μM), and U(VI) phosphate precipitation occurred onlymore » at high initial U(VI) (>25μM) and phosphate loadings. While batch experiments showed the transition of U(VI) uptake from adsorption to precipitation, the column study was more directly relevant to the subsurface environment because of the high solid:water ratio in the column and the advective flow of water. In column experiments, nearly six times more U(VI) was retained in sediments when phosphate-containing groundwater was introduced to U(VI)-loaded sediments than when the groundwater did not contain phosphate. This enhanced retention persisted for at least one month after cessation of phosphate addition to the influent fluid. Sequential extractions and laser-induced fluorescence spectroscopy of sediments from the columns suggested that the retained U(VI) was primarily in adsorbed forms. These results indicate that in situ remediation of groundwater by phosphate addition provides lasting benefit beyond the treatment period via enhanced U(VI) adsorption to sediments.« less

Batch process fault detection and identification based on discriminant global preserving kernel slow feature analysis.

PubMed

Zhang, Hanyuan; Tian, Xuemin; Deng, Xiaogang; Cao, Yuping

2018-05-16

As an attractive nonlinear dynamic data analysis tool, global preserving kernel slow feature analysis (GKSFA) has achieved great success in extracting the high nonlinearity and inherently time-varying dynamics of batch process. However, GKSFA is an unsupervised feature extraction method and lacks the ability to utilize batch process class label information, which may not offer the most effective means for dealing with batch process monitoring. To overcome this problem, we propose a novel batch process monitoring method based on the modified GKSFA, referred to as discriminant global preserving kernel slow feature analysis (DGKSFA), by closely integrating discriminant analysis and GKSFA. The proposed DGKSFA method can extract discriminant feature of batch process as well as preserve global and local geometrical structure information of observed data. For the purpose of fault detection, a monitoring statistic is constructed based on the distance between the optimal kernel feature vectors of test data and normal data. To tackle the challenging issue of nonlinear fault variable identification, a new nonlinear contribution plot method is also developed to help identifying the fault variable after a fault is detected, which is derived from the idea of variable pseudo-sample trajectory projection in DGKSFA nonlinear biplot. Simulation results conducted on a numerical nonlinear dynamic system and the benchmark fed-batch penicillin fermentation process demonstrate that the proposed process monitoring and fault diagnosis approach can effectively detect fault and distinguish fault variables from normal variables. Copyright © 2018 ISA. Published by Elsevier Ltd. All rights reserved.

Ginkgo fruit extract as an additive to modify rumen microbiota and fermentation and to mitigate methane production.

PubMed

Oh, S; Shintani, R; Koike, S; Kobayashi, Y

2017-03-01

Ginkgo fruit, an unused byproduct of the ginkgo nut industry, contains antimicrobial compounds known as anacardic acids. Two major cultivars of ginkgo, Kyuju (K) and Tokuro (T), were evaluated for their potential as a feed additive for ruminants. In batch culture, we incubated a mixture of hay and concentrate in diluted rumen fluid with or without 1.6% (fruit equivalent) ginkgo fruit extract. We conducted another series of batch culture studies to determine the dose response of fermentation. We also conducted continuous culture using the rumen simulation technique (RUSITEC) with cultivar K and carried out a pure culture study to monitor the sensitivity of 17 representative rumen bacterial species to ginkgo extract and component phenolics. Although both K and T extracts led to decreased methane and increased propionate production, changes were more apparent with K extract, and were dose-dependent. Total gas production was depressed at doses ≥3.2%, suggesting that 1.6% was the optimal supplementation level. In RUSITEC fermentation supplemented with 1.6% ginkgo K, methane decreased by 53% without affecting total gas or total VFA production, but with decreased acetate and increased propionate. Disappearance of dry matter, neutral detergent fiber, and acid detergent fiber were not affected by ginkgo, but ammonia levels were decreased. Quantitative PCR indicated that the abundance of protozoa, fungi, methanogens, and bacteria related to hydrogen and formate production decreased, but the abundance of bacteria related to propionate production increased. MiSeq analysis (Illumina Inc., San Diego, CA) confirmed these bacterial changes and identified archaeal community changes, including a decrease in Methanobrevibacter and Methanomassiliicoccaceae and an increase in Methanoplanus. Pure culture study results supported the findings for the above bacterial community changes. These results demonstrate that ginkgo fruit can modulate rumen fermentation toward methane mitigation and propionate enhancement via microbial selection. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Preparation of a novel sorptive stir bar based on vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer for the simultaneous extraction of diazepam and nordazepam from human plasma.

PubMed

Torabizadeh, Mahsa; Talebpour, Zahra; Adib, Nuoshin; Aboul-Enein, Hassan Y

2016-04-01

A new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The polymerization step was performed using different contents of monomer, cross-linker and porogenic solvent, and the best formulation was selected. The quality of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate stir bars was satisfactory, demonstrating good repeatability within batch (relative standard deviation < 3.5%) and acceptable reproducibility between batches (relative standard deviation < 6.0%). The prepared stir bar was utilized in combination with ultrasound-assisted liquid desorption, followed by high-performance liquid chromatography with ultraviolet detection for the simultaneous determination of diazepam and nordazepam in human plasma samples. To optimize the extraction step, a three-level, four-factor, three-block Box-Behnken design was applied. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for diazepam (36-1200 ng/mL) and nordazepam (25-1200 ng/mL), with correlation coefficients of 0.9986 and 0.9968 and detection limits of 12 and 10 ng/mL, respectively. The intra- and interday recovery ranged from 93 to 106%, and the relative standard deviations were less than 6%. Finally, the proposed method was successfully applied to the analysis of diazepam and nordazepam at their therapeutic levels in human plasma. The novelty of this study is the improved polarity of the stir bar coating and its application for the simultaneous extraction of diazepam and its active metabolite, nordazepam in human plasma sample. The method was more rapid than previously reported stir bar sorptive extraction techniques based on monolithic coatings, and exhibited lower detection limits in comparison with similar methods for the determination of diazepam and nordazepam in biological fluids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Enhanced ε-poly-L-lysine production through pH regulation and organic nitrogen addition in fed-batch fermentation].

PubMed

Sun, Qixing; Chen, Xusheng; Ren, Xidong; Zheng, Gencheng; Mao, Zhonggui

2015-05-01

During the production of ε-poly-L-lysine (ε-PL) in fed-batch fermentation, the decline of ε-PL synthesis often occurs at middle or late phase of the fermentation. To solve the problem, we adopted two strategies, namely pH shift and feeding yeast extract, to improve the productivity of ε-PL. ε-PL productivity in fermentation by pH shift and feeding yeast extract achieved 4.62 g/(L x d) and 5.16 g/(L x d), which were increased by 27.3% and 42.2% compared with the control ε-PL fed-batch fermentation, respectively. Meanwhile, ε-PL production enhanced 36.95 g/L and 41.32 g/L in 192 h with these two strategies, increased by 27.4% and 42.48% compared to the control, respectively. ε-PL production could be improved at middle or late phase of fed-batch fermentation by pH shift or feeding yeast extract.

Root Cause Analysis of Quality Defects Using HPLC-MS Fingerprint Knowledgebase for Batch-to-batch Quality Control of Herbal Drugs.

PubMed

Yan, Binjun; Fang, Zhonghua; Shen, Lijuan; Qu, Haibin

2015-01-01

The batch-to-batch quality consistency of herbal drugs has always been an important issue. To propose a methodology for batch-to-batch quality control based on HPLC-MS fingerprints and process knowledgebase. The extraction process of Compound E-jiao Oral Liquid was taken as a case study. After establishing the HPLC-MS fingerprint analysis method, the fingerprints of the extract solutions produced under normal and abnormal operation conditions were obtained. Multivariate statistical models were built for fault detection and a discriminant analysis model was built using the probabilistic discriminant partial-least-squares method for fault diagnosis. Based on multivariate statistical analysis, process knowledge was acquired and the cause-effect relationship between process deviations and quality defects was revealed. The quality defects were detected successfully by multivariate statistical control charts and the type of process deviations were diagnosed correctly by discriminant analysis. This work has demonstrated the benefits of combining HPLC-MS fingerprints, process knowledge and multivariate analysis for the quality control of herbal drugs. Copyright © 2015 John Wiley & Sons, Ltd.

Reynolds number effects on mixing due to topological chaos.

PubMed

Smith, Spencer A; Warrier, Sangeeta

2016-03-01

Topological chaos has emerged as a powerful tool to investigate fluid mixing. While this theory can guarantee a lower bound on the stretching rate of certain material lines, it does not indicate what fraction of the fluid actually participates in this minimally mandated mixing. Indeed, the area in which effective mixing takes place depends on physical parameters such as the Reynolds number. To help clarify this dependency, we numerically simulate the effects of a batch stirring device on a 2D incompressible Newtonian fluid in the laminar regime. In particular, we calculate the finite time Lyapunov exponent (FTLE) field for three different stirring protocols, one topologically complex (pseudo-Anosov) and two simple (finite-order), over a range of viscosities. After extracting appropriate measures indicative of both the amount of mixing and the area of effective mixing from the FTLE field, we see a clearly defined Reynolds number range in which the relative efficacy of the pseudo-Anosov protocol over the finite-order protocols justifies the application of topological chaos. More unexpectedly, we see that while the measures of effective mixing area increase with increasing Reynolds number for the finite-order protocols, they actually exhibit non-monotonic behavior for the pseudo-Anosov protocol.

Determining gold in water by anion-exchange batch extraction

USGS Publications Warehouse

McHugh, J.B.

1986-01-01

This paper describes a batch procedure for determining gold in natural waters. It is completely adaptable to field operations. The water samples are filtered and acidified before they are equilibrated with an anion-exchange resin by shaking. The gold is then eluted with acetone-nitric acid solution, and the eluate evaporated to dryness. The residue is taken up in hydrobromic acid-bromine solution and the gold is extracted with methyl isobutyl ketone. The extract is electrothermally atomized in an atomic-absorption spectrophotometer. The limit of determination is 1 ng 1. ?? 1986.

Manifold free multiple sheet superplastic forming

DOEpatents

Elmer, John W.; Bridges, Robert L.

2001-01-01

Fluid-forming compositions in a container attached to enclosed adjacent sheets are heated to relatively high temperatures to generate fluids (gases) that effect inflation of the sheets. Fluid rates to the enclosed space between the sheets can be regulated by the canal from the container. Inflated articles can be produced by a continuous, rather than batch-type, process.

Manifold free multiple sheet superplastic forming

DOEpatents

Elmer, John W.; Bridges, Robert L.

2004-01-13

Fluid-forming compositions in a container attached to enclosed adjacent sheets are heated to relatively high temperatures to generate fluids (gases) that effect inflation of the sheets. Fluid rates to the enclosed space between the sheets can be regulated by the canal from the container. Inflated articles can be produced by a continuous, rather than batch-type, process.

Extraction-Scrub-Strip test results from the interim Salt Disposition Program Macrobatch 9 Tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T.

2016-02-23

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 9 for the Interim Salt Disposition Program (ISDP). The Salt Batch 9 characterization results were previously reported. An Extraction-Scrub-Strip (ESS) test was performed to determine cesium distribution ratios (D (Cs)) and cesium concentration in the strip effluent and decontaminated salt solution (DSS) streams; this data will be used by Tank Farm Engineering to project a cesium decontamination factor (DF). This test used actual Tank 21H material, and a blend solvent prepared by SRNL that mimics the solvent composition currently being used atmore » the Modular Caustic-Side Solvent Extraction Unit (MCU). The ESS test showed acceptable performance with an extraction D (Cs) value of 52.4. This value is consistent with results from previous salt batch ESS tests using similar solvent formulations. This compares well against the predicted value of 56.5 from a recently created D (Cs) model« less

Extraction, -scrub, -strip test results from the interim salt disposition program macrobatch 10 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 10 for the Interim Salt Disposition Program (ISDP). The Salt Batch 10 characterization results were previously reported.ii,iii An Extraction, -Scrub, -Strip (ESS) test was performed to determine cesium distribution ratios (D(Cs)) and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams; this data will be used by Tank Farm Engineering to project a cesium decontamination factor (DF). This test used actual Tank 21H material, and a sample of the NGS Blend solvent currently being used at the Modularmore » Caustic-Side Solvent Extraction Unit (MCU). The ESS test showed acceptable performance with an extraction D(Cs) value of 110. This value is consistent with results from previous salt batch ESS tests using similar solvent formulations. This is better than the predicted value of 39.8 from a recently created D(Cs) model.« less

An in vitro study of anti-inflammatory activity of standardised Andrographis paniculata extracts and pure andrographolide.

PubMed

Low, Mitchell; Khoo, Cheang S; Münch, Gerald; Govindaraghavan, Suresh; Sucher, Nikolaus J

2015-02-07

The anti-inflammatory activity of Andrographis paniculata (Acanthaceae), a traditional medicine widely used in Asia, is commonly attributed to andrographolide, its main secondary metabolite. Commercial A. paniculata extracts are standardised to andrographolide content. We undertook the present study to investigate 1) how selective enrichment of andrographolide in commercial A. paniculata extracts affects the variability of non-standardised phytochemical components and 2) if variability in the non-standardised components of the extract affects the pharmacological activity of andrographolide itself. We characterized 12 commercial, standardised (≥30% andrographolide) batches of A. paniculata extracts from India by HPLC profiling. We determined the antioxidant capacity of the extracts using 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging, oxygen radical antioxidant capacity (ORAC) and a Folin-Ciocalteu (FC) antioxidant assays. Their anti-inflammatory activity was assessed by assaying their inhibitory effect on the release of tumor necrosis factor alpha (TNF-α) in the human monocytic cell line THP-1. The andrographolide content in the samples was close to the claimed value (32.2 ± 2.1%, range 27.5 to 35.9%). Twenty-one non-standardised constituents exhibited more than 2-fold variation in HPLC peak intensities in the tested batches. The chlorogenic acid content of the batches varied more than 30-fold. The DPPH free radical scavenging activity varied ~3-fold, the ORAC and FC antioxidant capacity varied ~1.5 fold among batches. In contrast, the TNF-α inhibitory activity of the extracts exhibited little variation and comparison with pure andrographolide indicated that it was mostly due to their andrographolide content. Standardised A. paniculata extracts contained the claimed amount of andrographolide but exhibited considerable phytochemical background variation. DPPH radical scavenging activity of the extracts was mostly due to the flavonoid/phenlycarboxylic acid compounds in the extracts. The inhibitory effect of andrographolide on the release of TNF-α was little affected by the quantitative variation of the non-standardised constituents.

Fuzzy clustering evaluation of the discrimination power of UV-Vis and (±) ESI-MS detection system in individual or coupled RPLC for characterization of Ginkgo Biloba standardized extracts.

PubMed

Medvedovici, Andrei; Albu, Florin; Naşcu-Briciu, Rodica Domnica; Sârbu, Costel

2014-02-01

Discrimination power evaluation of UV-Vis and (±) electrospray ionization/mass spectrometric techniques, (ESI-MS) individually considered or coupled as detectors to reversed phase liquid chromatography (RPLC) in the characterization of Ginkgo Biloba standardized extracts, is used in herbal medicines and/or dietary supplements with the help of Fuzzy hierarchical clustering (FHC). Seventeen batches of Ginkgo Biloba commercially available standardized extracts from seven manufacturers were measured during experiments. All extracts were within the criteria of the official monograph dedicated to dried refined and quantified Ginkgo extracts, in the European Pharmacopoeia. UV-Vis and (±) ESI-MS spectra of the bulk standardized extracts in methanol were acquired. Additionally, an RPLC separation based on a simple gradient elution profile was applied to the standardized extracts. Detection was made through monitoring UV absorption at 220 nm wavelength or the total ion current (TIC) produced through (±) ESI-MS analysis. FHC was applied to raw, centered and scaled data sets, for evaluating the discrimination power of the method with respect to the origins of the extracts and to the batch to batch variability. The discrimination power increases with the increase of the intrinsic selectivity of the spectral technique being used: UV-Vis

Effects of plants and essential oils on ruminal in vitro batch culture methane production and fermentation

USDA-ARS?s Scientific Manuscript database

In this study, plants (14) and essential oils (EO; 88) from plants that are naturalized to, or can be successfully grown in North America were evaluated in a batch culture in vitro screening experiments with ruminal fluid as potential anti-methanogenic additives for ruminant diets. Essential oils we...

Combining microwave resonance technology to multivariate data analysis as a novel PAT tool to improve process understanding in fluid bed granulation.

PubMed

Lourenço, Vera; Herdling, Thorsten; Reich, Gabriele; Menezes, José C; Lochmann, Dirk

2011-08-01

A set of 192 fluid bed granulation batches at industrial scale were in-line monitored using microwave resonance technology (MRT) to determine moisture, temperature and density of the granules. Multivariate data analysis techniques such as multiway partial least squares (PLS), multiway principal component analysis (PCA) and multivariate batch control charts were applied onto collected batch data sets. The combination of all these techniques, along with off-line particle size measurements, led to significantly increased process understanding. A seasonality effect could be put into evidence that impacted further processing through its influence on the final granule size. Moreover, it was demonstrated by means of a PLS that a relation between the particle size and the MRT measurements can be quantitatively defined, highlighting a potential ability of the MRT sensor to predict information about the final granule size. This study has contributed to improve a fluid bed granulation process, and the process knowledge obtained shows that the product quality can be built in process design, following Quality by Design (QbD) and Process Analytical Technology (PAT) principles. Copyright © 2011. Published by Elsevier B.V.

Extraction of Antioxidant Phenolic Compounds from Brewer’s Spent Grain: Optimization and Kinetics Modeling

PubMed Central

Sologubik, Carlos A.; Fernández, María B.; Manrique, Guillermo D.

2018-01-01

The kinetics of polyphenol extraction from brewer’s spent grain (BSG), using a batch system, ultrasound assistance, and microwave assistance and the evolution of antioxidant capacity of these extracts over time, were studied. The main parameters of extraction employed in the batch system were evaluated, and, by applying response surface analysis, the following optimal conditions were obtained: Liquid/solid ratio of 30:1 mL/g at 80 °C, using 72% (v/v) ethanol:water as the solvent system. Under these optimized conditions, ultrasound assistance demonstrated the highest extraction rate and equilibrium yield, as well as shortest extraction times, followed by microwave assistance. Among the mathematical models used, Patricelli’s model proved the most suitable for describing the extraction kinetics for each method tested, and is therefore able to predict the response values and estimate the extraction rates and potential maximum yields in each case. PMID:29570683

System for monitoring physical characteristics of fluids

NASA Technical Reports Server (NTRS)

Trinh, E. H.; Wang, T. G. (Inventor)

1983-01-01

An apparatus and method are described for measuring physical characteristics of fluid, by placing a drop of the fluid in a batch of a second fluid and passing acoustic waves through the bath. The applied frequency of the acoustic waves is varied, to determine the precise value of a frequency at which the drop undergoes resonant oscillations. The resonant frequency indicates the interfacial tension of the drop in the bath, and the interfacial tension can indicate physical properties of the fluid in the drop.

Design and application of PDF model for extracting

NASA Astrophysics Data System (ADS)

Xiong, Lei

2013-07-01

In order to change the steps of contributions in editorial department system from two steps to one, this paper advocates that the technology of extracting the information of PDF files should be transplanted from PDF reader into IEEE Xplore contribution system and that it should be combined with uploading in batch skillfully to enable editors to upload PDF files about 1GB in batch for once. Computers will extract the information of the title, author, address, mailbox, abstract and key words of thesis voluntarily for later retrieval so as to save plenty of labor, material and finance for editorial department.

Enhancing tablet disintegration characteristics of a highly water-soluble high-drug-loading formulation by granulation process.

PubMed

Pandey, Preetanshu; Levins, Christopher; Pafiakis, Steve; Zacour, Brian; Bindra, Dilbir S; Trinh, Jade; Buckley, David; Gour, Shruti; Sharif, Shasad; Stamato, Howard

2018-07-01

The objective of this study was to improve the disintegration and dissolution characteristics of a highly water-soluble tablet matrix by altering the manufacturing process. A high disintegration time along with high dependence of the disintegration time on tablet hardness was observed for a high drug loading (70% w/w) API when formulated using a high-shear wet granulation (HSWG) process. Keeping the formulation composition mostly constant, a fluid-bed granulation (FBG) process was explored as an alternate granulation method using a 2 (4-1) fractional factorial design with two center points. FBG batches (10 batches) were manufactured using varying disingtegrant amount, spray rate, inlet temperature (T) and atomization air pressure. The resultant final blend particle size was affected significantly by spray rate (p = .0009), inlet T (p = .0062), atomization air pressure (p = .0134) and the interaction effect between inlet T*spray rate (p = .0241). The compactibility of the final blend was affected significantly by disintegrant amount (p < .0001), atomization air pressure (p = .0013) and spray rate (p = .05). It was observed that the fluid-bed batches gave significantly lower disintegration times than the HSWG batches, and mercury intrusion porosimetry data revealed that this was caused by the higher internal pore structure of tablets manufactured using the FBG batches.

Semiautomated Device for Batch Extraction of Metabolites from Tissue Samples

PubMed Central

2012-01-01

Metabolomics has become a mainstream analytical strategy for investigating metabolism. The quality of data derived from these studies is proportional to the consistency of the sample preparation. Although considerable research has been devoted to finding optimal extraction protocols, most of the established methods require extensive sample handling. Manual sample preparation can be highly effective in the hands of skilled technicians, but an automated tool for purifying metabolites from complex biological tissues would be of obvious utility to the field. Here, we introduce the semiautomated metabolite batch extraction device (SAMBED), a new tool designed to simplify metabolomics sample preparation. We discuss SAMBED’s design and show that SAMBED-based extractions are of comparable quality to extracts produced through traditional methods (13% mean coefficient of variation from SAMBED versus 16% from manual extractions). Moreover, we show that aqueous SAMBED-based methods can be completed in less than a quarter of the time required for manual extractions. PMID:22292466

Near infrared spectroscopy based monitoring of extraction processes of raw material with the help of dynamic predictive modeling

NASA Astrophysics Data System (ADS)

Wang, Haixia; Suo, Tongchuan; Wu, Xiaolin; Zhang, Yue; Wang, Chunhua; Yu, Heshui; Li, Zheng

2018-03-01

The control of batch-to-batch quality variations remains a challenging task for pharmaceutical industries, e.g., traditional Chinese medicine (TCM) manufacturing. One difficult problem is to produce pharmaceutical products with consistent quality from raw material of large quality variations. In this paper, an integrated methodology combining the near infrared spectroscopy (NIRS) and dynamic predictive modeling is developed for the monitoring and control of the batch extraction process of licorice. With the spectra data in hand, the initial state of the process is firstly estimated with a state-space model to construct a process monitoring strategy for the early detection of variations induced by the initial process inputs such as raw materials. Secondly, the quality property of the end product is predicted at the mid-course during the extraction process with a partial least squares (PLS) model. The batch-end-time (BET) is then adjusted accordingly to minimize the quality variations. In conclusion, our study shows that with the help of the dynamic predictive modeling, NIRS can offer the past and future information of the process, which enables more accurate monitoring and control of process performance and product quality.

Strategy for large-scale isolation of enantiomers in drug discovery.

PubMed

Leek, Hanna; Thunberg, Linda; Jonson, Anna C; Öhlén, Kristina; Klarqvist, Magnus

2017-01-01

A strategy for large-scale chiral resolution is illustrated by the isolation of pure enantiomer from a 5kg batch. Results from supercritical fluid chromatography will be presented and compared with normal phase liquid chromatography. Solubility of the compound in the supercritical mobile phase was shown to be the limiting factor. To circumvent this, extraction injection was used but shown not to be efficient for this compound. Finally, a method for chiral resolution by crystallization was developed and applied to give diastereomeric salt with an enantiomeric excess of 99% at a 91% yield. Direct access to a diverse separation tool box will be shown to be essential for solving separation problems in the most cost and time efficient way. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography-negative chemical ion/mass spectrometry].

PubMed

Xing, Yuanna; Lin, Zhihui; Feng, Anhong; Wang, Xin; Gong, Yemeng; Chen, Zeyong

2015-02-01

A novel method was established to determine short chain chlorinated paraffins (SC-CPs) in polyvinyl chloride (PVC) plastics by gas chromatography-negative chemical ion/mass spectrometry (GC-NCI/MS). Ultrasonic extraction was used to extract SCCPs from PVC plastics. The optimal extraction time was 1.5 h, and concentrated sulfuric acid was adopted to purify the extracted solution. Finally, SCCPs in a sample were detected by GC-NCI/MS at 160 C and with methane reagent gas at 1. 5 mL/min. This method was not influenced by medium chain chlorinated paraffins (MCCPs) in the sample, and accurate quantitation was made for SCCPs. Twelve batches of samples were analyzed and SCCPs were detected in each batch with the contents from 0. 3 x 10(2)mg/kg to 3. 5 x 10(4)mg/kg. With respect to European limitation of SC-CPs (1%), four batches of samples did not comply with the European regulation, and they accounted for 33. 3%. Obviously, high SCCPs risk was presented in PVC plastics.

Silicon microneedle array for minimally invasive human health monitoring

NASA Astrophysics Data System (ADS)

Smith, Rosemary L.; Collins, Scott D.; Duy, Janice; Minogue, Timothy D.

2018-02-01

A silicon microneedle array with integrated microfluidic channels is presented, which is designed to extract dermal interstitial fluid (ISF) for biochemical analysis. ISF is a cell-free biofluid that is known to contain many of the same constituents as blood plasma, but the scope and dynamics of biomarker similarities are known for only a few components, most notably glucose. Dermal ISF is accessible just below the outer skin layer (epidermis), which can be reached and extracted with minimal sensation and tissue trauma by using a microneedle array. The microneedle arrays presented here are being developed to extract dermal ISF for off-chip profiling of nucleic acid constituents in order to identify potential biomarkers of disease. In order to assess sample volume requirements, preliminary RNA profiling was performed with suction blister ISF. The microneedles are batch fabricated using established silicon technology (low cost), are small in size, and can be integrated with sensors for on-chip analysis. This approach portends a more rapid, less expensive, self-administered assessment of human health than is currently achievable with blood sampling, especially in non-clinical and austere settings. Ultimately, a wearable device for monitoring a person's health in any setting is envisioned.

Synthesis of high generation thermo-sensitive dendrimers for extraction of rivaroxaban from human fluid and pharmaceutic samples.

PubMed

Parham, Negin; Panahi, Homayon Ahmad; Feizbakhsh, Alireza; Moniri, Elham

2018-04-13

In this present study, poly (N-isopropylacrylamide) as a thermo-sensitive agent was grafted onto magnetic nanoparticles, then ethylenediamine and methylmethacrylate were used to synthesize the first generation of poly amidoamine (PAMAM) dendrimers successively and the process continued alternatively until the ten generations of dendrimers. The synthesized nanocomposite was investigated using Fourier transform infrared spectrometry, thermalgravimetry analysis, X-ray diffractometry, elemental analysis and vibrating-sample magnetometer. The particle size and morphology were characterized using dynamic light scattering, field emission scanning electron microscopy and transmission electron microscopy. Batch experiments were conducted to investigate the parameters affecting adsorption and desorption of rivaroxaban by synthesized nanocomposite. The maximum sorption of rivaroxaban by the synthesized nanocomposite was obtained at pH of 8. The resulting grafted magnetic nanoparticle dendrimers were applied for extraction of rivaroxaban from biologic human liquids and medicinal samples. The specifications of rivaroxaban sorbed by a magnetic nanoparticle dendrimer showed good accessibility and high capacity of the active sites within the dendrimers. Urine and drug matrix extraction recoveries of more than 92.5 and 99.8 were obtained, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

Supercritical extraction of lycopene from tomato industrial wastes with ethane.

PubMed

Nobre, Beatriz P; Gouveia, Luisa; Matos, Patricia G S; Cristino, Ana F; Palavra, António F; Mendes, Rui L

2012-07-11

Supercritical fluid extraction of all-E-lycopene from tomato industrial wastes (mixture of skins and seeds) was carried out in a semi-continuous flow apparatus using ethane as supercritical solvent. The effect of pressure, temperature, feed particle size, solvent superficial velocity and matrix initial composition was evaluated. Moreover, the yield of the extraction was compared with that obtained with other supercritical solvents (supercritical CO₂ and a near critical mixture of ethane and propane). The recovery of all-E-lycopene increased with pressure, decreased with the increase of the particle size in the initial stages of the extraction and was not practically affected by the solvent superficial velocity. The effect of the temperature was more complex. When the temperature increased from 40 to 60 °C the recovery of all-E-lycopene increased from 80 to 90%. However, for a further increase to 80 °C, the recovery remained almost the same, indicating that some E-Z isomerization could have occurred, as well as some degradation of lycopene. The recovery of all-E-lycopene was almost the same for feed samples with different all-E-lycopene content. Furthermore, when a batch with a higher all-E-lycopene content was used, supercritical ethane and a near critical mixture of ethane and propane showed to be better solvents than supercritical CO₂ leading to a faster extraction with a higher recovery of the carotenoid.

The Impact of Mineralogy on the Geochemical Alteration of Shales During Hydraulic Fracturing Operations

NASA Astrophysics Data System (ADS)

Maher, K.; Harrison, A. L.; Jew, A. D.; Dustin, M. K.; Kiss, A. M.; Kohli, A. H.; Thomas, D.; Joe-Wong, C. M.; Brown, G. E.; Bargar, J.

2016-12-01

The extraction of oil and gas resources from low permeability shale reservoirs using hydraulic fracturing techniques has increased significantly in recent years. During hydraulic fracturing, large volumes of fluid are injected into subsurface shale formations, which drives substantial fluid-rock interaction that can release contaminants and alter rock permeability. Here, a combined experimental, imaging, and modeling approach was employed to systematically evaluate the impact of shale mineralogy on its physical and chemical alteration when exposed to fracturing fluids of different composition. Batch reactor experiments contained different shales with unique mineralogical compositions that were exposed to simulated hydraulic fracturing fluid. Experiments revealed that the balance between fluid acidity and acid neutralizing capacity of the rock was the strongest control on the evolution of fluid and rock chemistry. Carbonate mineral-rich shales rapidly recovered solution pH to circum-neutral conditions, whereas fluids in contact with carbonate mineral-poor shales remained acidic. The dissolution of shale minerals released metal contaminants, yet the precipitation of Fe(III)-bearing secondary phases helped to attenuate their release via co-precipitation or sorption. Post-reaction imaging illustrated that selective dissolution of carbonate minerals generated secondary porosity, the connectivity of which was dictated by initial carbonate distribution. Conversely, the precipitation of secondary Al- and Fe-bearing phases may occlude porosity, potentially inhibiting transport of water, contaminants, and hydrocarbons. The maturation of secondary Fe-bearing phases from amorphous to crystalline over time suggests that porosity will continue to evolve even after oxidation reactions have effectively ceased. These experiments reveal that the relative abundance and distribution of carbonate minerals is the master variable dictating both porosity alteration and contaminant release from shale formations, implying that the response of a reservoir to hydraulic fracturing can be better assessed using robust mineralogical data.

Reynolds number effects on mixing due to topological chaos

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Spencer A.; Warrier, Sangeeta

2016-03-15

Topological chaos has emerged as a powerful tool to investigate fluid mixing. While this theory can guarantee a lower bound on the stretching rate of certain material lines, it does not indicate what fraction of the fluid actually participates in this minimally mandated mixing. Indeed, the area in which effective mixing takes place depends on physical parameters such as the Reynolds number. To help clarify this dependency, we numerically simulate the effects of a batch stirring device on a 2D incompressible Newtonian fluid in the laminar regime. In particular, we calculate the finite time Lyapunov exponent (FTLE) field for threemore » different stirring protocols, one topologically complex (pseudo-Anosov) and two simple (finite-order), over a range of viscosities. After extracting appropriate measures indicative of both the amount of mixing and the area of effective mixing from the FTLE field, we see a clearly defined Reynolds number range in which the relative efficacy of the pseudo-Anosov protocol over the finite-order protocols justifies the application of topological chaos. More unexpectedly, we see that while the measures of effective mixing area increase with increasing Reynolds number for the finite-order protocols, they actually exhibit non-monotonic behavior for the pseudo-Anosov protocol.« less

Bioherbicidal activity of Sinapis alba seed meal extracts

USDA-ARS?s Scientific Manuscript database

Although seed meal from yellow mustard (Sinapis alba L.) is a potential tool for controlling weeds as a consequence of contained glucosinolate substrates that are enzymatically hydrolyzed to produce phytotoxic products, use is limited by batch-to-batch variability and logistical constraints. Our obj...

A rapid and efficient assay for extracting DNA from fungi

USGS Publications Warehouse

Griffin, Dale W.; Kellogg, C.A.; Peak, K.K.; Shinn, E.A.

2002-01-01

Aims: A method for the rapid extraction of fungal DNA from small quantities of tissue in a batch-processing format was investigated. Methods and Results: Tissue (< 3.0 mg) was scraped from freshly-grown fungal isolates. The tissue was suspended in buffer AP1 and subjected to seven rounds of freeze/thaw using a crushed dry ice/ethanol bath and a boiling water bath. After a 30 min boiling step, the tissue was quickly ground against the wall of the microfuge tube using a sterile pipette tip. The Qiagen DNeasy Plant Tissue Kit protocol was then used to purify the DNA for PCR/ sequencing applications. Conclusions: The method allowed batch DNA extraction from multiple fungal isolates using a simple yet rapid and reliable assay. Significance and Impact of the Study: Use of this assay will allow researchers to obtain DNA from fungi quickly for use in molecular assays that previously required specialized instrumentation, was time-consuming or was not conducive to batch processing.

A reproducible and scalable procedure for preparing bacterial extracts for cell-free protein synthesis.

PubMed

Katsura, Kazushige; Matsuda, Takayoshi; Tomabechi, Yuri; Yonemochi, Mayumi; Hanada, Kazuharu; Ohsawa, Noboru; Sakamoto, Kensaku; Takemoto, Chie; Shirouzu, Mikako

2017-11-01

Cell-free protein synthesis is a useful method for preparing proteins for functional or structural analyses. However, batch-to-batch variability with regard to protein synthesis activity remains a problem for large-scale production of cell extract in the laboratory. To address this issue, we have developed a novel procedure for large-scale preparation of bacterial cell extract with high protein synthesis activity. The developed procedure comprises cell cultivation using a fermentor, harvesting and washing of cells by tangential flow filtration, cell disruption with high-pressure homogenizer and continuous diafiltration. By optimizing and combining these methods, ∼100 ml of the cell extract was prepared from 150 g of Escherichia coli cells. The protein synthesis activities, defined as the yield of protein per unit of absorbance at 260 nm of the cell extract, were shown to be reproducible, and the average activity of several batches was twice that obtained using a previously reported method. In addition, combinatorial use of the high-pressure homogenizer and diafiltration increased the scalability, indicating that the cell concentration at disruption varies from 0.04 to 1 g/ml. Furthermore, addition of Gam protein and examinations of the N-terminal sequence rendered the extract prepared here useful for rapid screening with linear DNA templates. © The Authors 2017. Published by Oxford University Press on behalf of the Japanese Biochemical Society. All rights reserved.

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.

Planar solid-phase microextraction-ion mobility spectrometry: a diethoxydiphenylsilane-based coating for the detection of explosives and explosive taggants.

PubMed

Mattarozzi, M; Bianchi, F; Bisceglie, F; Careri, M; Mangia, A; Mori, G; Gregori, A

2011-03-01

A novel diethoxydiphenylsilane-based coating for planar solid-phase microextraction was developed using sol-gel technology and used for ion mobility spectrometric detection of the explosives 2,4,6-trinitrotoluene, 2,4-dinitrotoluene, and of the explosive taggant ethylene glycol dinitrate. The trap was characterized in terms of coating thickness, morphology, inter-batch repeatability, and extraction efficiency. An average thickness of 143 ± 13 μm with a uniform distribution of the coating was obtained. Good performances of the developed procedure in terms of both intra-batch and inter-batch repeatability with relative standard deviations <7% were obtained. Experimental design and desirability function were used to find the optimal conditions for simultaneous headspace extraction of the investigated compounds: the optimal values were found in correspondence of a time and a temperature of extraction of 45 min and 40 °C, respectively. Detection and quantitation limits in low nanogram levels were achieved proving the superior extraction capability of the developed coating, obtaining ion mobility spectrometric responses at least two times higher than those achieved using commercial teflon and paper traps.

The comparison of anti-oxidative kinetics in vitro of the fluid extract from maidenhair tree, motherwort and hawthorn.

PubMed

Bernatoniene, Jurga; Kucinskaite, Agne; Masteikova, Ruta; Kalveniene, Zenona; Kasparaviciene, Giedre; Savickas, Arunas

2009-01-01

The aim of the study was to perform a quantitative analysis of fluid extracts of maidenhair tree (Ginkgo biloba L.), motherwort (Leonurus cardiaca L.) and hawthorn (Crataegus monogyna Jacq.), to evaluate their antioxidant activity and to compare their ability to inactivate free radicals. The antioxidant activity was measured using the DPPH*and the ABTS*+ radical scavenging reaction systems. The study showed that the manifestation of the radical scavenging capacity in the DPPH* reaction system was in the following order: the fluid extract of hawthorn (70.37 +/- 0.80%) > the fluid extract of maidenhair tree (82.63 +/- 0.23%) > the fluid extract of motherwort (84.89 +/- 0.18%), while in the ABTS*+ reaction system, the manifestation of the radical scavenging capacity was in the following order: the fluid extract of hawthorn (87.09 +/- 0.55%) > the fluid extract of motherwort (88.28 +/- 1.06%) > the fluid extract of maidenhair tree (88.39 +/- 0.72%). The results showed that in the DPPH* reaction system, fluid extract of motherwort manifested higher antioxidant activity, compared to the fluid extracts of maidenhair tree and hawthorn. By contrast, in the ABTS*+ reaction system, higher antioxidant activity was found in the fluid extract of maidenhair tree, compared to the fluid extracts of motherwort and hawthorn. This would suggest that preparations manufactured from these herbal raw materials could be used as effective preventive means and valuable additional remedies in the treatment of diseases caused by oxidative stress.

Products derived from olive leaves and fruits can alter in vitro ruminal fermentation and methane production.

PubMed

Shakeri, Pirouz; Durmic, Zoey; Vadhanabhuti, Joy; Vercoe, Philip E

2017-03-01

The industrial processing of olive generates a high quantity of by-products. The objective of this study was to examine the effects of products derived from olive trees, i.e. leaves, fruits or kernels as a sole substrate (part A), and crude extract from leaves combined with a substrate (part B) on rumen microbial fermentation in an in vitro batch fermentation system. In this study, total gas production, methane production, and concentrations of volatile fatty acids (VFA) and ammonia in ruminal fluid were measured. In part A, in vitro fermentation of leaves or fruits yielded a gas and total VFA production that were comparable with control substrate, while most of them produced significantly less methane (up to 55.6%) when compared to control substrate. In part B, amongst leaf extracts, only addition of chloroform extract reduced methane production, which was also associated with a decrease (P < 0.01) in gas production. This effect was associated with a significant reduction (P < 0.01) in acetate to propionate ratio and ammonia production, but not in reduction in VFA concentrations. Olive leaf and olive leaf chloroform extract reduced ammonia production and increased the molar proportion of propionate in the rumen and can assist in developing novel feed additives for methane mitigation from the rumen. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Metabolomics study of Saw palmetto extracts based on 1H NMR spectroscopy.

PubMed

de Combarieu, Eric; Martinelli, Ernesto Marco; Pace, Roberto; Sardone, Nicola

2015-04-01

Preparations containing Saw palmetto extracts are used in traditional medicine to treat benign prostatic hyperplasia. According to the European and the American Pharmacopoeias, the extract is obtained from comminuted Saw palmetto berries by a suitable extracting procedure using ethanol or supercritical carbon dioxide or a mixture of n-hexane and methylpentanes. In the present study an approach to metabolomics profiling using nuclear magnetic resonance (NMR) has been used as a finger-printing tool to assess the overall composition of the extracts. The phytochemical analysis coupled with principal component analysis (PCA) showed the same composition of the Saw palmetto extracts obtained with carbon dioxide and hexane with minor not significant differences for extracts obtained with ethanol. In fact these differences are anyhow lower than the batch-to-batch variability ascribable to the natural-occurring variability in the Saw palmetto fruits' phytochemical composition. The fingerprinting analysis combined with chemometric method, is a technique, which would provide a tool to comprehensively assess the quality control of Saw palmetto extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

Traditionally used medicinal plants against uncomplicated urinary tract infections: Are unusual, flavan-4-ol- and derhamnosylmaysin derivatives responsible for the antiadhesive activity of extracts obtained from stigmata of Zea mays L. against uropathogenic E. coli and Benzethonium chloride as frequent contaminant faking potential antibacterial activities?

PubMed

Rafsanjany, Nasli; Sendker, Jandirk; Lechtenberg, Matthias; Petereit, Frank; Scharf, Birte; Hensel, Andreas

2015-09-01

The dried stigmata from Zea mays L. are used traditionally for the treatment of uncomplicated urinary tract infections. A recent screening has indicated that hydroalcoholic extract of the herbal material inhibits the adhesion of uropathogenic Escherichia coli (UPEC) to T24 bladder cells. For verification of these data EtOH-water (1:1) extracts from 4 different batches of Maydis stigmata were investigated. Within an in vitro adhesion assay (UPEC strain 2980 and human T24 bladder cells) a dose-dependent antiadhesive activity against UPEC was verified (IC50 1040μg/mL). Bioassay guided fractionation of M. stigmata, batch S1, by EtOH-water extraction, followed by chromatography on Sephadex LH20 revealed two active fractions (I and XI). Further purification of fraction I and structure elucidation of the isolated compound revealed the presence of significant amounts of the biocide benzethonium chloride as contaminant. Benzethonium chloride was also identified in subsequent investigations in 2 different batches of M. stigmata. The presence of such nondeclared and illegal contaminants in the herbal raw material market has to be discussed intensively. From benzethonium-free raw material (batch S2) as well as from batch S1 fraction XI was further fractionated by MPLC and preparative HPLC, leading to a still complex subfraction XIG, which was analyzed by UHPLC/+ESI-QTOF-MS analysis. Advanced data processing and species-metabolite relationship database revealed the tentatively existence of the unusual C-glycosidic flavones derhamnosylmaysin (6), 3'-deoxyrhamnosylmaysin (4), 3'-O-methylderhamnosylmaysin (3), apiferol (2) and alternanthin (8) which might be related to the antiadhesive activity of this subfraction against UPEC. Copyright © 2015 Elsevier B.V. All rights reserved.

Bio-based extraction and stabilization of anthocyanins.

PubMed

Roy, Anirban; Mukherjee, Rudra Palash; Howard, Luke; Beitle, Robert

2016-05-01

This work reports a novel method of recovering anthocyanin compounds from highly-pigmented grapes via a fermentation based approach. It was hypothesized that batch growth of Zymomonas mobilis on simple medium would produce both ethanol and enzymes/biomass-acting materials, the combination of which will provide a superior extraction when compared to simple alcohol extraction. To examine this hypothesis, Z. mobilis was fermented in a batch consisting of mashed Vitis vinifera and glucose, and the recovered anthocyanin pool was compared to that recovered via extraction with ethanol. Data indicated higher amounts of anthocyanins were recovered when compared to simple solvent addition. Additionally, the percent polymeric form of the anthocyanins could be manipulated by the level of aeration maintained in the fermentation. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:601-605, 2016. © 2016 American Institute of Chemical Engineers.

Extraction of organic contaminants from marine sediments and tissues using microwave energy.

PubMed

Jayaraman, S; Pruell, R J; McKinney, R

2001-07-01

In this study, we compared microwave solvent extraction (MSE) to conventional methods for extracting organic contaminants from marine sediments and tissues with high and varying moisture content. The organic contaminants measured were polychlorinated biphenyl (PCB) congeners, chlorinated pesticides, and polycyclic aromatic hydrocarbons (PAHs). Initial experiments were conducted on dry standard reference materials (SRMs) and field collected marine sediments. Moisture content in samples greatly influenced the recovery of the analytes of interest. When wet sediments were included in a sample batch, low recoveries were often encountered in other samples in the batch, including the dry SRM. Experiments were conducted to test the effect of standardizing the moisture content in all samples in a batch prior to extraction. SRM1941a (marine sediment). SRM1974a (mussel tissue), as well as QA96SED6 (marine sediment), and QA96TIS7 (marine tissue), both from 1996 NIST Intercalibration Exercise were extracted using microwave and conventional methods. Moisture levels were adjusted in SRMs to match those of marine sediment and tissue samples before microwave extraction. The results demonstrated that it is crucial to standardize the moisture content in all samples, including dry reference material to ensure good recovery of organic contaminants. MSE yielded equivalent or superior recoveries compared to conventional methods for the majority of the compounds evaluated. The advantages of MSE over conventional methods are reduced solvent usage, higher sample throughput and the elimination of halogenated solvent usage.

Short-term Influence of Two Types of Drilling Fluids on Wastewater Treatment Rate and Eukaryotic Organisms of Activated Sludge in Sequencing Batch Reactors.

PubMed

Babko, Roman; Jaromin-Gleń, Katarzyna; Łagód, Grzegorz; Danko, Yaroslav; Kuzmina, Tatiana; Pawłowska, Małgorzata; Pawłowski, Artur

2017-07-01

This work presents the results of studies on the impact of spent drilling fluids cotreated with municipal wastewater on the rate of the wastewater treatment process and the structure of the community of eukaryotic organisms inhabiting an activated sludge. The studies were conducted under laboratory conditions in sequencing batch reactors. The effect of added polymer-potassium drilling fluid (DF1) and polymer drilling fluid (DF2) at dosages of 1 and 3% of wastewater volume on the rate of removal of total suspended solids, turbidity, chemical oxygen demand, and the content of total and ammonium nitrogen were analyzed, taking into account the values of these parameters measured at the end of each operating cycle. In addition to the impacts on the aforementioned physicochemical indices, the influence of drilling fluid on the biomass of various groups of eukaryotes in activated sludge was analyzed. The impact of the drilling fluid was highly dependent on its type and dosage. A noticeable slowdown in the rate of the wastewater treatment process and a negative effect on the organisms were observed after the addition of DF2. This effect intensified after an increase in fluid dose. However, no statistically significant negative changes were observed after the introduction of DF1. Conversely, the removal rate of some of the analyzed pollutant increased. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Sol-gel polydimethylsiloxane/poly(vinylalcohol)-coated stir bar sorptive extraction of organophosphorus pesticides in honey and their determination by large volume injection GC.

PubMed

Yu, Chunhe; Hu, Bin

2009-01-01

A PDMS/poly(vinylalcohol) (PDMS/PVA) film prepared through a sol-gel process was coated on stir bars for sorptive extraction, followed by liquid desorption and large volume injection-GC-flame photometric detector (LVI-GC-FPD) for the determination of five organophosphorus pesticides (OPPs) (phorate, fenitrothion, malathion, parathion, and quinalphos) in honey. The preparation reproducibility of PDMS/PVA-coated stir bar ranged from 4.3 to 13.4% (n = 4) in one batch, and from 6.0 to 12.6% (n = 4) in batch to batch. And one prepared stir bar can be used for more than 50 times without apparent coating loss. The significant parameters affecting stir bar sorptive extraction (SBSE) were investigated and optimized. The LODs for five OPPs ranged from 0.013 (parathion) to 0.081 microg/L (phorate) with the RSDs ranging from 5.3 to 14.2% (c = 1 microg/L, n = 6). The proposed method was successfully applied to the analysis of five OPPs in honey.

Degassing of different magma batches as the main controlling factor for fumarolic fluid chemistry at the Planchón-Peteroa-Azufre Volcanic Complex (Argentina-Chile) in 2010-2015

NASA Astrophysics Data System (ADS)

Tassi, Franco; Aguilera, Felipe; Benavente, Oscar; Paonita, Antonio; Chiodini, Giovanni; Caliro, Stefano; Agusto, Mariano; Gutierrez, Francisco; Capaccioni, Bruno; Vaselli, Orlando; Caselli, Alberto

2016-04-01

This study presents the first geochemical data of gas discharges collected during five sampling campaigns (February 2010 to March 2015), from the NNE-oriented Planchón-Peteroa-Azufre Volcanic Complex (PPAVC), located in the Transitional Southern Volcanic Zone (TSVZ) at the border between Argentina and Chile. In 2012, the acidic gas species of the low temperature (up to 102 °C) fumaroles from the Peteroa summit showed a huge increase (SO2>CO2) with respect to the 2010-2011 period, whereas the typical hydrothermal compounds (CH4 and light hydrocarbons) decreased. Such a dramatic compositional change was apparently indicating a pulse of magmatic fluids. By contrast, the temporal evolution of the δ18O-H2O, δD-H2O, R/Ra and 13C-CO2 values suggested an enhanced fluid contribution from a shallow source. In 2014-2015, the dominant hydrothermal signature characterizing the 2010-2011 fumaroles was almost completely restored. The temporary decoupling of the chemical and isotopic parameters can only be reconciled by admitting the occurrence of a double source of magmatic fluids: a basaltic batch, controlling the fumarolic chemistry in 2010-2011 and 2014-2015, and a small, shallower dacitic batch, likely affected by a significant crustal contamination, whose contribution to the fumarolic fluid emissions achieved its maximum in 2012. It cannot be ruled out that the phreatic to phreatomagmatic eruptions (VEI ≤2) that have affected Peteroa volcano from January 2010 to July 2011 have played a significant role for the modification of the deep feeding source of the fumarolic gases. The disturbance created by the volcanic events and the related seismic activity (MW<3), possibly related to the devastating Maule earthquake occurred on February 27 2010, could have activated a silent dacitic magma batch that in 2012 imposed over that of basaltic composition. Although this scenario provides a reliable explanation for the peculiar compositional changes that affected the Peteroa fumaroles in 2010-2015 and is consistent with the volcanic products of PPAVC, such an intriguing hypothesis is expected to be supported by geophysical investigations aimed to locate the two magma sources invoked to construct the proposed degassing model.

Extraction of Peace River bitumen using supercritical ethane

NASA Astrophysics Data System (ADS)

Rose, Jeffrey Lawrence

2000-10-01

As the supply of conventional crude oil continues to decline, petroleum companies are looking for alternative hydrocarbon sources. The vast reserves of heavy oil and bitumen located in northern Alberta are among the alternatives. The challenge facing engineers is to develop a process for recovering this oil which is economic, efficient and environmentally acceptable. Supercritical fluid extraction is one method being investigated which could potentially meet all of these criteria. In this study, Peace River bitumen was extracted using supercritical ethane. The bitumen was mixed with sand and packed into a semi-batch extractor. Ethane contacted the bitumen/sand mixture and the fraction of the bitumen soluble in the ethane was removed and subsequently collected in a two phase separator. The flow of ethane was such that the experiments were governed by equilibrium and not mass transfer. Experimental temperatures and pressures were varied in order to observe the effect of these parameters on the mass and composition of the extracted material. The extraction yields increased as the temperature decreased and pressure increased. Samples were collected at various time intervals to measure changes in the properties of the extracted bitumen over the duration of the process. As the extraction proceeded, the samples became heavier and more viscous. The bitumen feed was characterised and the experimental data was then modelled using the Peng-Robinson equation of state. The characterisation process involved the distillation of the bitumen into five fractions. The distillation curve and density of each fraction was measured and this data was used in conjunction with correlations to determine the critical properties of the bitumen. Interaction parameters in the equation of state were then optimised until the predicted composition of extracted bitumen matched the experimental results.

Terra-Kleen Response Group, Inc. Solvent Extraction Technology Rapid Commercialization Initiative Report

EPA Science Inventory

Terra-Kleen Response Group Inc. (Terra-Kleen), has commercialized a solvent extraction technology that uses a proprietary extraction solvent to transfer organic constituents from soil to a liquid phase in a batch process at ambient temperatures. The proprietary solvent has a rel...

Antioxidant and Antilipid Peroxidation Potential of Supercritical Fluid Extract and Ethanol Extract of Leaves of Vitex Negundo Linn.

PubMed Central

Nagarsekar, K. S.; Nagarsenker, M. S.; Kulkarni, S. R.

2011-01-01

Supercritical fluid extract and ethanol extract of Vitex negundo Linn. were subjected to the chromatographic evaluation for identification of their constituents. Free radical scavenging activity of both extracts was studied by subjecting them to DPPH assay. IC50 values of ethanol and supercritical fluid extract of Vitex negundo indicate that ethanol extract has stronger reducing potential and ability to scavenge free radicals as compared to the supercritical fluid extract. The in vivo effect of extracts on lipid peroxidation was studied using ethanol induced oxidative stress model in rat. Ingestion of extracts for 14 days exhibited significant reduction in plasma MDA level of stressed animals. Ethanol extract exhibited higher in vivo antilipid peroxidation potential as compared to supercritical fluid extract which correlated well with radical scavenging potential of extract. PMID:22707827

An innovative approach to the safety evaluation of natural products: cranberry (Vaccinium macrocarpon Aiton) leaf aqueous extract as a case study.

PubMed

Booth, Nancy L; Kruger, Claire L; Wallace Hayes, A; Clemens, Roger

2012-09-01

Assessment of safety for a food or dietary ingredient requires determination of a safe level of ingestion compared to the estimated daily intake from its proposed uses. The nature of the assessment may require the use of different approaches, determined on a case-by-case basis. Natural products are chemically complex and challenging to characterize for the purpose of carrying out a safety evaluation. For example, a botanical extract contains numerous compounds, many of which vary across batches due to changes in environmental conditions and handling. Key components integral to the safety evaluation must be identified and their variability established to assure that specifications are representative of a commercial product over time and protective of the consumer; one can then extrapolate the results of safety studies on a single batch of product to other batches that are produced under similar conditions. Safety of a well-characterized extract may be established based on the safety of its various components. When sufficient information is available from the public literature, additional toxicology testing is not necessary for a safety determination on the food or dietary ingredient. This approach is demonstrated in a case study of an aqueous extract of cranberry (Vaccinium macrocarpon Aiton) leaves. Copyright © 2012. Published by Elsevier Ltd.

On-line coupling of supercritical fluid extraction and chromatographic techniques.

PubMed

Sánchez-Camargo, Andrea Del Pilar; Parada-Alfonso, Fabián; Ibáñez, Elena; Cifuentes, Alejandro

2017-01-01

This review summarizes and discusses recent advances and applications of on-line supercritical fluid extraction coupled to liquid chromatography, gas chromatography, and supercritical fluid chromatographic techniques. Supercritical fluids, due to their exceptional physical properties, provide unique opportunities not only during the extraction step but also in the separation process. Although supercritical fluid extraction is especially suitable for recovery of non-polar organic compounds, this technique can also be successfully applied to the extraction of polar analytes by the aid of modifiers. Supercritical fluid extraction process can be performed following "off-line" or "on-line" approaches and their main features are contrasted herein. Besides, the parameters affecting the supercritical fluid extraction process are explained and a "decision tree" is for the first time presented in this review work as a guide tool for method development. The general principles (instrumental and methodological) of the different on-line couplings of supercritical fluid extraction with chromatographic techniques are described. Advantages and shortcomings of supercritical fluid extraction as hyphenated technique are discussed. Besides, an update of the most recent applications (from 2005 up to now) of the mentioned couplings is also presented in this review. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Intensification of extraction of curcumin from Curcuma amada using ultrasound assisted approach: Effect of different operating parameters.

PubMed

Shirsath, S R; Sable, S S; Gaikwad, S G; Sonawane, S H; Saini, D R; Gogate, P R

2017-09-01

Curcumin, a dietary phytochemical, has been extracted from rhizomes of Curcuma amada using ultrasound assisted extraction (UAE) and the results compared with the conventional extraction approach to establish the process intensification benefits. The effect of operating parameters such as type of solvent, extraction time, extraction temperature, solid to solvent ratio, particle size and ultrasonic power on the extraction yield have been investigated in details for the approach UAE. The maximum extraction yield as 72% was obtained in 1h under optimized conditions of 35°C temperature, solid to solvent ratio of 1:25, particle size of 0.09mm, ultrasonic power of 250W and ultrasound frequency of 22kHz with ethanol as the solvent. The obtained yield was significantly higher as compared to the batch extraction where only about 62% yield was achieved in 8h of treatment. Peleg's model was used to describe the kinetics of UAE and the model showed a good agreement with the experimental results. Overall, ultrasound has been established to be a green process for extraction of curcumin with benefits of reduction in time as compared to batch extraction and the operating temperature as compared to Soxhlet extraction. Copyright © 2017. Published by Elsevier B.V.

Production of nattokinase by batch and fed-batch culture of Bacillus subtilis.

PubMed

Cho, Young-Han; Song, Jae Yong; Kim, Kyung Mi; Kim, Mi Kyoung; Lee, In Young; Kim, Sang Bum; Kim, Hyeon Shup; Han, Nam Soo; Lee, Bong Hee; Kim, Beom Soo

2010-09-30

Nattokinase was produced by batch and fed-batch culture of Bacillus subtilis in flask and fermentor. Effect of supplementing complex media (peptone, yeast extract, or tryptone) was investigated on the production of nattokinase. In flask culture, the highest cell growth and nattokinase activity were obtained with 50 g/L of peptone supplementation. In this condition, nattokinase activity was 630 unit/ml at 12 h. In batch culture of B. subtilis in fermentor, the highest nattokinase activity of 3400 unit/ml was obtained at 10h with 50 g/L of peptone supplementation. From the batch kinetics data, it was shown that nattokinase production was growth-associated and culture should be harvested before stationary phase for maximum nattokinase production. In fed-batch culture of B. subtilis using pH-stat feeding strategy, cell growth (optical density monitored at 600 nm) increased to ca. 100 at 22 h, which was 2.5 times higher than that in batch culture. The highest nattokinase activity was 7100 unit/ml at 19 h, which was also 2.1 times higher than that in batch culture. Copyright 2010 Elsevier B.V. All rights reserved.

Incorporation of additives into polymers

DOEpatents

McCleskey, T. Mark; Yates, Matthew Z.

2003-07-29

There has been invented a method for incorporating additives into polymers comprising: (a) forming an aqueous or alcohol-based colloidal system of the polymer; (b) emulsifying the colloidal system with a compressed fluid; and (c) contacting the colloidal polymer with the additive in the presence of the compressed fluid. The colloidal polymer can be contacted with the additive by having the additive in the compressed fluid used for emulsification or by adding the additive to the colloidal system before or after emulsification with the compressed fluid. The invention process can be carried out either as a batch process or as a continuous on-line process.

Changes in copper sulfate crystal habit during cooling crystallization

NASA Astrophysics Data System (ADS)

Giulietti, M.; Seckler, M. M.; Derenzo, S.; Valarelli, J. V.

1996-09-01

The morphology of technical grade copper(II) sulfate pentahydrate crystals produced from batch cooling experiments in the temperature range of 70 to 30°C is described and correlated with the process conditions. A slow linear cooling rate (batch time of 90 min) predominantly caused the appearance of well-formed crystals. Exponential cooling (120 min) resulted in the additional formation of agglomerates and twins. The presence of seeds for both cooling modes led to round crystals, agglomerates and twins. Fast linear cooling (15 min) gave rise to a mixture of the former types. Broken crystals and adhering fragments were often found. Growth zoning was pronounced in seeded and linear cooling experiments. Fluid inclusions were always found and were more pronounced for larger particles. The occurrence of twinning, zoning and fluid inclusions was qualitatively explained in terms of fundamental principles.

Effects of high-pressure process on kinetics of leaching oil from soybean powder using hexane in batch systems.

PubMed

Uhm, Joo Tae; Yoon, Won Byong

2011-08-01

Mass transfer models of leaching oil from soybean (Glycine max) flour with hexane after high-pressure process (HPP) treatment were developed. High pressure (450 MPa) was applied to the soybean flour (mean diameter of flour particle: 365 μm) for 30 min before leaching the oil components in the solvent. The ratio of solvent (volume, mL) to soybean flour (mass, g), such as 1:10 and 1:20, was employed to characterize the effect of solvent ratio on the leaching rate in the batch type of extraction process. Ultraviolet absorbance at 300 nm was used to monitor the extraction rate. Saturation solubility (C(AS)) was determined to be 21.73 kg/m³. The mass transfer coefficients (k) were determined based on the 1st- and 2nd-order kinetic models. The 2nd kinetic model showed better fit. The HPP treatment showed a higher extraction rate and yield compared to the control, while the amount of solvent did not affect the extraction rate and yield. The scanning electron microscope showed that HPP-treated soybean particles included more pores than the untreated. The pores observed in the HPP-treated soybean flours might help increase the mass transfer rate of solvent and solute in the solid matrix. High-pressure processing can help increase the extraction rate of oil from the soybean flour operated in batch systems. The conventional solid to solvent ratio (1:20) used to extract oil composition from the plant seed did not help increase the amount of oil extracted from the soybean flour. © 2011 Institute of Food Technologists®

Potential effect of the medicinal plants Calotropis procera, Ficus elastica and Zingiber officinale against Schistosoma mansoni in mice.

PubMed

Seif el-Din, Sayed H; El-Lakkany, Naglaa M; Mohamed, Mona A; Hamed, Manal M; Sterner, Olov; Botros, Sanaa S

2014-02-01

Calotropis procera (Ait.) R. Br. (Asclepiadaceae), Ficus elastica Roxb. (Moraceae) and Zingiber officinale Roscoe (Zingiberaceae) have been traditionally used to treat many diseases. The antischistosomal activity of these plant extracts was evaluated against Schistosoma mansoni. Male mice exposed to 80 ± 10 cercariae per mouse were divided into two batches. The first was divided into five groups: (I) infected untreated, while groups from (II-V) were treated orally (500 mg/kg for three consecutive days) by aqueous stem latex and flowers of C. procera, latex of F. elastica and ether extract of Z. officinale, respectively. The second batch was divided into four comparable groups (except Z. officinale-treated group) similarly treated as the first batch in addition to the antacid ranitidine (30 mg/kg) 1 h before extract administration. Safety, worm recovery, tissues egg load and oogram pattern were assessed. Calotropis procera latex and flower extracts are toxic (50-70% mortality) even in a small dose (250 mg/kg) before washing off their toxic rubber. Zingiber officinale extract insignificantly decrease (7.26%) S. mansoni worms. When toxic rubber was washed off and ranitidine was used, C. procera (stem latex and flowers) and F. elastica extracts revealed significant S. mansoni worm reductions by 45.31, 53.7 and 16.71%, respectively. Moreover, C. procera extracts produced significant reductions in tissue egg load (∼34-38.5%) and positively affected oogram pattern. The present study may be useful to supplement information with regard to C. procera and F. elastica antischistosomal activity and provide a basis for further experimental trials.

Removal of zearalenone toxin from synthetics gastric and body fluids using talc and diatomite: a batch kinetic study.

PubMed

Sprynskyy, Myroslav; Gadzała-Kopciuch, Renata; Nowak, Karolina; Buszewski, Bogusław

2012-06-01

Adsorption kinetics of zearalenone (ZEA) toxin from synthetic gastric fluid (SGF) and synthetic body fluid (SBF) by talc and diatomite was studied in the batch experiments. Chemical composition, morphology and structure of the used adsorbents were examined by scanning electron microscopy, FTIR spectroscopy and low-temperature nitrogen adsorption/desorption method. High performance liquid chromatography (HPLC) method was used for ZEA determining. The study results showed that ZEA is more effectively adsorbed on the talc (73% and 54% from SGF and SBF respectively). The efficiency on the diatomite was lower (53% and 42% from SGF and SBF respectively). The first order kinetics model was applied to describe the adsorption process. Rate of the ZEA adsorption from SGF is very rapid initially with about 95% of amount of the toxin adsorbed during first 5 min, while ZEA is adsorbed from SBF in two steps. The values of determined Gibbs free energy of adsorption (from -13 to -17 kJ/mol) indicated that adsorption of ZEA toxin by the both adsorbents are spontaneous and exothermic. Copyright © 2012 Elsevier B.V. All rights reserved.

Bioconversion of waste office paper to hydrogen using pretreated rumen fluid inoculum.

PubMed

Botta, Lívia Silva; Ratti, Regiane Priscila; Sakamoto, Isabel Kimiko; Ramos, Lucas Rodrigues; Silva, Edson Luiz; Varesche, Maria Bernadete Amâncio

2016-12-01

In this study, a microbial consortium from an acid-treated rumen fluid was used to improve the yields of H 2 production from paper residues in batch reactors. The anaerobic batch reactors, which contained paper and cellulose, were operated under three conditions: (1) 0.5 g paper/L, (2) 2 g paper/L, and (3) 4 g paper/L. Cellulase was added to promote the hydrolysis of paper to soluble sugars. The H 2 yields were 5.51, 4.65, and 3.96 mmol H 2 /g COD, respectively, with substrate degradation ranging from 56 to 65.4 %. Butyric acid was the primary soluble metabolite in the three reactors, but pronounced solventogenesis was detected in the reactors incubated with increased paper concentrations (2.0 and 4.0 g/L). A substantial prevalence of Clostridium acetobutylicum (99 % similarity) was observed in the acid-treated rumen fluid, which has been recognized as an efficient H 2 -producing strain in addition to ethanol and n-butanol which were also detected in the reactors.

Qualitative and Quantitative Assessment of Four Marketed Formulations of Brahmi

PubMed Central

Saini, Neeti; Mathur, Rajani; Agrawal, S. S.

2012-01-01

This study was conducted with the aim to compare two batches each of four popular commercial formulations of Bacopa monnieri (Brahmi), and report, if any, inter-batch variations. The formulations were procured from local market and analyzed for label specifications, uniformity of weight of capsule, identity, purity and strength parameters (total ash content test, acid insoluble ash content, water soluble extractive, alcohol soluble extractive, loss on drying). Bacoside A, one of the pharmacologically active saponin present in B. monnieri, was quantified in all the formulations using UV-spectrophotometer. In addition each formulation was assessed and compared for variation in biological activity using in vitro test for hemolytic activity using human erythrocytes. The results of the study show that there is a wide variation in the quality and content of herbal drugs marketed by different manufacturers. More importantly this study demonstrates that there exists a bigger challenge of batch-to-batch variation in the quality and content of herbal formulations of the same manufacturer. This challenge of providing standardized formulations is being faced by not any one manufacturing house but by all, and may be attributed firstly to, lack of stringent regulations and secondly to high variability in raw material quality. PMID:23204618

Qualitative and quantitative assessment of four marketed formulations of brahmi.

PubMed

Saini, Neeti; Mathur, Rajani; Agrawal, S S

2012-01-01

This study was conducted with the aim to compare two batches each of four popular commercial formulations of Bacopa monnieri (Brahmi), and report, if any, inter-batch variations. The formulations were procured from local market and analyzed for label specifications, uniformity of weight of capsule, identity, purity and strength parameters (total ash content test, acid insoluble ash content, water soluble extractive, alcohol soluble extractive, loss on drying). Bacoside A, one of the pharmacologically active saponin present in B. monnieri, was quantified in all the formulations using UV-spectrophotometer. In addition each formulation was assessed and compared for variation in biological activity using in vitro test for hemolytic activity using human erythrocytes. The results of the study show that there is a wide variation in the quality and content of herbal drugs marketed by different manufacturers. More importantly this study demonstrates that there exists a bigger challenge of batch-to-batch variation in the quality and content of herbal formulations of the same manufacturer. This challenge of providing standardized formulations is being faced by not any one manufacturing house but by all, and may be attributed firstly to, lack of stringent regulations and secondly to high variability in raw material quality.

Probing the interaction of U (VI) with phosphonate-functionalized mesoporous silica using solid-state NMR spectroscopy

DOE PAGES

Uribe, Eva C.; Mason, Harris E.; Shusterman, Jennifer A.; ...

2016-05-30

The fundamental interaction of U (VI) with diethylphosphatoethyl triethoxysilane functionalized SBA-15 mesoporous silica is studied by macroscopic batch experiments and solid-state NMR spectroscopy. DPTS-functionalized silica has been shown to extract U (VI) from nitric acid solutions at or above pH 3. Extraction is dependent on pH and ionic strength. Single-pulse 31P NMR on U (VI) contacted samples revealed that U (VI)only interacts with a fraction of the ligands present on the surface. At pH 4 the U (VI) extraction capacity of the material is limited to 27–37% of the theoretical capacity, based on ligand loading. We combined single pulse 31Pmore » NMR on U (VI)-contacted samples with batch studies to measure a ligand-to-metal ratio of approximately 2 : 1 at pH 3 and 4. Batch studies and cross-polarization NMR measurements reveal that U (VI) binds to deprotonated phosphonate and/or silanol sites. We use 31P– 31P DQ-DRENAR NMR studies to compare the average dipolar coupling between phosphorus spins for both U (VI)-complexed and non-complexed ligand environments. Furthermore, these measurements reveal that U (VI) extraction is not limited by inadequate surface distribution of ligands, but rather by low stability of the surface phosphonate complex.« less

Probing the interaction of U (VI) with phosphonate-functionalized mesoporous silica using solid-state NMR spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Uribe, Eva C.; Mason, Harris E.; Shusterman, Jennifer A.

The fundamental interaction of U (VI) with diethylphosphatoethyl triethoxysilane functionalized SBA-15 mesoporous silica is studied by macroscopic batch experiments and solid-state NMR spectroscopy. DPTS-functionalized silica has been shown to extract U (VI) from nitric acid solutions at or above pH 3. Extraction is dependent on pH and ionic strength. Single-pulse 31P NMR on U (VI) contacted samples revealed that U (VI)only interacts with a fraction of the ligands present on the surface. At pH 4 the U (VI) extraction capacity of the material is limited to 27–37% of the theoretical capacity, based on ligand loading. We combined single pulse 31Pmore » NMR on U (VI)-contacted samples with batch studies to measure a ligand-to-metal ratio of approximately 2 : 1 at pH 3 and 4. Batch studies and cross-polarization NMR measurements reveal that U (VI) binds to deprotonated phosphonate and/or silanol sites. We use 31P– 31P DQ-DRENAR NMR studies to compare the average dipolar coupling between phosphorus spins for both U (VI)-complexed and non-complexed ligand environments. Furthermore, these measurements reveal that U (VI) extraction is not limited by inadequate surface distribution of ligands, but rather by low stability of the surface phosphonate complex.« less

Method and apparatus for continuous flow injection extraction analysis

DOEpatents

Hartenstein, Steven D.; Siemer, Darryl D.

1992-01-01

A method and apparatus for a continuous flow injection batch extraction aysis system is disclosed employing extraction of a component of a first liquid into a second liquid which is a solvent for a component of the first liquid, and is immiscible with the first liquid, and for separating the first liquid from the second liquid subsequent to extraction of the component of the first liquid.

Comparison of the potency of different brands of Serenoa repens extract on 5alpha-reductase types I and II in prostatic co-cultured epithelial and fibroblast cells.

PubMed

Scaglione, Francesco; Lucini, Valeria; Pannacci, Marilou; Caronno, Alessia; Leone, Claude

2008-01-01

Serenoa repens extract is the phytotherapeutic agent most frequently used for the treatment of the urological symptoms caused by benign prostatic hyperplasia. There are many extracts in the market and each manufacturer uses different extraction processes; for this reason, it's possible that one product is not equivalent to another. The aim of this study was to compare the activity of different extracts of Serenoa repens marketed in Italy. The following extracts were tested on 10 day co-cultured epithelial and fibroblast cells by a 5alpha-reductase activity assay: Permixon, Saba, Serpens, Idiprost, Prostamev, Profluss and Prostil. In order to assess the variability in Serenoa repens products, 2 different batches for each brand were evaluated. All extracts tested, albeit variably, are able to inhibit both isoforms of 5alpha-reductase. However, the potency of the extracts appears to be very different, as well as the potencies of 2 different batches of the same extract. This is probably due to qualitative and quantitative differences in the active ingredients. So, the product of each company must be tested to evaluate the clinical efficacy and bioactivity. Copyright 2008 S. Karger AG, Basel.

Results Of Initial Analyses Of The Salt (Macro) Batch 9 Tank 21H Qualification Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T.

2015-10-08

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Interim Salt Disposition Project (ISDP) Salt (Macro) Batch 9 for processing through the Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU). This document reports the initial results of the analyses of samples of Tank 21H. Analysis of the Tank 21H Salt (Macro) Batch 9 composite sample indicates that the material does not display any unusual characteristics. Further results on the chemistry and other tests will be issued in the future.

DEMONSTRATION BULLETIN: TERRA KLEEN SOLVENT EXTRACTION TECHNOLOGY - TERRA-KLEEN RESPONSE GROUP, INC.

EPA Science Inventory

The Terra-Kleen Solvent Extraction Technology was developed by Terra-Kleen Response Group, Inc., to remove polychlorinated biphenyls (PCB) and other organic constituents from contaminated soil. This batch process system uses a proprietary solvent at ambient temperatures to treat ...

Inorganic fouling mitigation by salinity cycling in batch reverse osmosis.

PubMed

Warsinger, David M; Tow, Emily W; Maswadeh, Laith A; Connors, Grace B; Swaminathan, Jaichander; Lienhard V, John H

2018-06-15

Enhanced fouling resistance has been observed in recent variants of reverse osmosis (RO) desalination which use time-varying batch or semi-batch processes, such as closed-circuit RO (CCRO) and pulse flow RO (PFRO). However, the mechanisms of batch processes' fouling resistance are not well-understood, and models have not been developed for prediction of their fouling performance. Here, a framework for predicting reverse osmosis fouling is developed by comparing the fluid residence time in batch and continuous (conventional) reverse osmosis systems to the nucleation induction times for crystallization of sparingly soluble salts. This study considers the inorganic foulants calcium sulfate (gypsum), calcium carbonate (calcite), and silica, and the work predicts maximum recovery ratios for the treatment of typical water sources using batch reverse osmosis (BRO) and continuous reverse osmosis. The prediction method is validated through comparisons to the measured time delay for CaSO 4 membrane scaling in a bench-scale, recirculating reverse osmosis unit. The maximum recovery ratio for each salt solution (CaCO 3 , CaSO 4 ) is individually predicted as a function of inlet salinity, as shown in contour plots. Next, the maximum recovery ratios of batch and conventional RO are compared across several water sources, including seawater, brackish groundwater, and RO brine. Batch RO's shorter residence times, associated with cycling from low to high salinity during each batch, enable significantly higher recovery ratios and higher salinity than in continuous RO for all cases examined. Finally, representative brackish RO brine samples were analyzed to determine the maximum possible recovery with batch RO. Overall, the induction time modeling methodology provided here can be used to allow batch RO to operate at high salinity and high recovery, while controlling scaling. The results show that, in addition to its known energy efficiency improvement, batch RO has superior inorganic fouling resistance relative to conventional RO. Copyright © 2018 Elsevier Ltd. All rights reserved.

[Monitoring method of extraction process for Schisandrae Chinensis Fructus based on near infrared spectroscopy and multivariate statistical process control].

PubMed

Xu, Min; Zhang, Lei; Yue, Hong-Shui; Pang, Hong-Wei; Ye, Zheng-Liang; Ding, Li

2017-10-01

To establish an on-line monitoring method for extraction process of Schisandrae Chinensis Fructus, the formula medicinal material of Yiqi Fumai lyophilized injection by combining near infrared spectroscopy with multi-variable data analysis technology. The multivariate statistical process control (MSPC) model was established based on 5 normal batches in production and 2 test batches were monitored by PC scores, DModX and Hotelling T2 control charts. The results showed that MSPC model had a good monitoring ability for the extraction process. The application of the MSPC model to actual production process could effectively achieve on-line monitoring for extraction process of Schisandrae Chinensis Fructus, and can reflect the change of material properties in the production process in real time. This established process monitoring method could provide reference for the application of process analysis technology in the process quality control of traditional Chinese medicine injections. Copyright© by the Chinese Pharmaceutical Association.

Feasibility of biogas production from anaerobic co-digestion of herbal-extraction residues with swine manure.

PubMed

Li, Yan; Yan, Xi-Luan; Fan, Jie-Ping; Zhu, Jian-Hang; Zhou, Wen-Bin

2011-06-01

The objective of this work was to examine the feasibility of biogas production from the anaerobic co-digestion of herbal-extraction residues with swine manure. Batch and semi-continuous experiments were carried out under mesophilic anaerobic conditions. Batch experiments revealed that the highest specific biogas yield was 294 mL CH(4) g(-1) volatile solids added, obtained at 50% of herbal-extraction residues and 3.50 g volatile solids g(-1) mixed liquor suspended solids. Specific methane yield from swine manure alone was 207 mL CH(4) g(-1) volatile solid added d(-1) at 3.50 g volatile solids g(-1) mixed liquor suspended solids. Furthermore, specific methane yields were 162, 180 and 220 mL CH(4) g (-1) volatile solids added d(-1) for the reactors co-digesting mixtures with 10%, 25% and 50% herbal-extraction residues, respectively. These results suggested that biogas production could be enhanced efficiently by the anaerobic co-digestion of herbal-extraction residues with swine manure. Copyright © 2011 Elsevier Ltd. All rights reserved.

Total amino acid stabilization during cell-free protein synthesis reactions.

PubMed

Calhoun, Kara A; Swartz, James R

2006-05-17

Limitations in amino acid supply have been recognized as a substantial problem in cell-free protein synthesis reactions. Although enzymatic inhibitors and fed-batch techniques have been beneficial, the most robust way to stabilize amino acids is to remove the responsible enzymatic activities by genetically modifying the source strain used for cell extract preparation. Previous work showed this was possible for arginine, serine, and tryptophan, but cysteine degradation remained a major limitation in obtaining high protein synthesis yields. Through radiolabel techniques, we confirmed that cysteine degradation was caused by the activity of glutamate-cysteine ligase (gene gshA) in the cell extract. Next, we created Escherichia coli strain KC6 that combines a gshA deletion with previously described deletions for arginine, serine, and tryptophan stabilization. Strain KC6 grows well, and active cell extract can be produced from it for cell-free protein synthesis reactions. The extract from strain KC6 maintains stable amino acid concentrations of all 20 amino acids in a 3-h batch reaction. Yields for three different proteins improved 75-250% relative to cell-free expression using the control extract.

Oxidation Stability of Pig Liver Pâté with Increasing Levels of Natural Antioxidants (Grape and Tea)

PubMed Central

Pateiro, Mirian; Lorenzo, José M.; Vázquez, José A.; Franco, Daniel

2015-01-01

The present study investigated the effect of the addition of increasing levels of the natural antioxidants tea (TEA) and grape seed extracts (GRA) on the physiochemical and oxidative stability of refrigerated stored pig pâtés. In addition, a synthetic antioxidant and a control batch were used, thus a total of eight batches of liver pâté were prepared: CON, BHT, TEA (TEA50, TEA200 and TEA1000) and GRA (GRA50, GRA200 and GRA1000). Pâté samples were analyzed following 0, 4, 8 and 24 weeks of storage. Color parameters were affected by storage period and level of antioxidant extract. Samples with TEA200 and GRA1000 levels of extracts showed lower total color difference between 0 and 24 weeks. At the end of storage period, the lower TBARs values were obtained in samples with the highest concentration on natural extract. Overall, the evolution of volatile compounds showed an increase in those ones that arise from the lipid oxidation and samples with TEA1000 extract showed the lowest values. PMID:26785340

Optimization of L-(+)-lactic acid production by ring and disc plastic composite supports through repeated-batch biofilm fermentation.

PubMed Central

Ho, K L; Pometto, A L; Hinz, P N

1997-01-01

Four customized bioreactors, three with plastic composite supports (PCS) and one with suspended cells (control), were operated as repeated-batch fermentors for 66 days at pH 5 and 37 degrees C. The working volume of each customized reactor was 600 ml, and each reactor's medium was changed every 2 to 5 days for 17 batches. The performance of PCS bioreactors in long-term biofilm repeated-batch fermentation was compared with that of suspended-cell bioreactors in this research. PCS could stimulate biofilm formation, supply nutrients to attached and free suspended cells, and reduce medium channelling for lactic acid production. Compared with conventional repeated-batch fermentation, PCS bioreactors shortened the lag time by threefold (control, 11 h; PCS, 3.5 h) and sixfold (control, 9 h; PCS, 1.5 h) at yeast extract concentrations of 0.4 and 0.8% (wt/vol), respectively. They also increased the lactic acid productivity of Lactobacillus casei subsp. rhamnosus (ATCC 11443) by 40 to 70% and shortened the total fermentation time by 28 to 61% at all yeast extract concentrations. The fastest productivity of the PCS bioreactors (4.26 g/liter/h) was at a starting glucose concentration of 10% (wt/vol), whereas that of the control (2.78 g/liter/h) was at 8% (wt/vol). PCS biofilm lactic acid fermentation can drastically improve the fermentation rate with reduced complex-nutrient addition. PMID:9212403

Improved productivity of poly (3-hydroxybutyrate) (PHB) in thermophilic Chelatococcus daeguensis TAD1 using glycerol as the growth substrate in a fed-batch culture.

PubMed

Cui, Bin; Huang, Shaobin; Xu, Fuqian; Zhang, Ruijian; Zhang, Yongqing

2015-07-01

A particularly successful polyhydroxyalkanoate (PHA) in industrial applications is poly (3-hydroxybutyrate) (PHB). However, one of the major obstacles for wider application of PHB is the cost of its production and purification. Therefore, it is desirable to discover a method for producing PHB in large quantities at a competitive price. Glycerol is a cheap and widely used carbon source that can be applied in PHB production process. There are numerous advantages to operating fermentation at elevated temperatures; only several thermophilic bacteria are able to accumulate PHB when glycerol is the growth substrate. Here, we report on the possibility of increasing PHB production at low cost using thermophilic Chelatococcus daeguensis TAD1 when glycerol is the growth substrate in a fed-batch culture. We found that (1) excess glycerol inhibited PHB accumulation and (2) organic nitrogen sources, such as tryptone and yeast extract, promoted the growth of C. daeguensis TAD1. In the batch fermentation experiments, we found that using glycerol at low concentrations as the sole carbon source, along with the addition of mixed nitrate (NH4Cl, tryptone, and yeast extract), stimulated PHB accumulation in C. daeguensis TAD1. The results showed that the PHB productivity decreased in the following order: two-stage fed-batch fermentation > fed-batch fermentation > batch fermentation. In optimized culture conditions, a PHB amount of 17.4 g l(-1) was obtained using a two-stage feeding regimen, leading to a productivity rate of 0.434 g l(-1) h(-1), which is the highest productivity rate reported for PHB to date. This high PHB biosynthetic productivity could decrease the total production cost, allowing for further development of industrial applications of PHB.

Sulfur Speciation and Extraction in Jet A (Briefing Charts)

DTIC Science & Technology

2015-08-16

Extraction fluid: denatured ethanol from Fisher Scientific and deionized water – Jet A fuel , approximately 500-800 ppm sulfur by weight – Data...Outline • Background • Experimental Setup – Extraction of sulfur compounds from fuel to alcohol/water extraction fluid – Each rinse is...Hydrophobic / Oleophillic Membrane Oleophobic / Hydrophillic Membrane Emulsion Phase Fuel Phase Water (Extraction Fluid) Phase DISTRIBUTION A

Electrochemical treatment of tannery effluent using a battery integrated DC-DC converter and solar PV power supply--an approach towards environment and energy management.

PubMed

Iyappan, K; Basha, C Ahmed; Saravanathamizhan, R; Vedaraman, N; Tahiyah Nou Shene, C A; Begum, S Nathira

2014-01-01

Electrochemical oxidation of tannery effluent was carried out in batch, batch recirculation and continuous reactor configurations under different conditions using a battery-integrated DC-DC converter and solar PV power supply. The effect of current density, electrolysis time and fluid flow rate on chemical oxygen demand (COD) removal and energy consumption has been evaluated. The results of batch reactor show that a COD reduction of 80.85% to 96.67% could be obtained. The results showed that after 7 h of operation at a current density of 2.5 A dm(-2) and flow rate of 100 L h(-1) in batch recirculation reactor, the removal of COD is 82.14% and the specific energy consumption was found to be 5.871 kWh (kg COD)(-1) for tannery effluent. In addition, the performance of single pass flow reactors (single and multiple reactors) system of various configurations are analyzed.

Analysis of microbiota involved in the aged natural fermentation of indigo.

PubMed

Okamoto, Takahiro; Aino, Kenichi; Narihiro, Takashi; Matsuyama, Hidetoshi; Yumoto, Isao

2017-04-01

Although the indigo reduction process is performed via natural fermentation and maintained under open-air condition, the indigo-reducing reactions continue for 6 months (on average) or longer. Identifying the mechanism underlying the maintenance of this process could lead to the development of a novel, long-lasting, unsterilized bioprocesses. To determine the mechanisms underlying the maintenance of the indigo fermentation system microbiota for more than 6 months in a reduced state in an anaerobic alkaline environment, we examined changes in the microbiota in one early-phase batch and two aged batches of indigo fermentation fluid. The microbiota in the aged fermentation fluid consisted mainly of the genera Alkalibacterium, Amphibacillus, Anaerobacillus and Polygonibacillus and the family Proteinivoraceae. The genera Alkalibacterium, Amphibacillus and Polygonibacillus are known to include indigo-reducing bacteria. Although the transition speed was slower in the aged fermentation fluid than in the early-stage fluid, the microbiota in the aged fermentation fluid maintained for more than 6 months was drastically changed within a period of 3 months. The results of this study indicate that the bacterial consortia consisted of various indigo-reducing species that replace the previous group of indigo-reducing bacteria. The notable transitional changes may be concomitant with changes in the environmental conditions, such as the nutritional conditions, observed over 3 months. This flexibility may lead to important changes in the microbiota that allow for the maintenance of a fermentation-reducing state over a long period.

Sequential injection analysis with chemiluminescence detection for rapid monitoring of commercial Calendula officinalis extractions.

PubMed

Hughes, Rachel R; Scown, David; Lenehan, Claire E

2015-01-01

Plant extracts containing high levels of antioxidants are desirable due to their reported health benefits. Most techniques capable of determining the antioxidant activity of plant extracts are unsuitable for rapid at-line analysis as they require extensive sample preparation and/or long analysis times. Therefore, analytical techniques capable of real-time or pseudo real-time at-line monitoring of plant extractions, and determination of extraction endpoints, would be useful to manufacturers of antioxidant-rich plant extracts. To develop a reliable method for the rapid at-line extraction monitoring of antioxidants in plant extracts. Calendula officinalis extracts were prepared from dried flowers and analysed for antioxidant activity using sequential injection analysis (SIA) with chemiluminescence (CL) detection. The intensity of CL emission from the reaction of acidic potassium permanganate with antioxidants within the extract was used as the analytical signal. The SIA-CL method was applied to monitor the extraction of C. officinalis over the course of a batch extraction to determine the extraction endpoint. Results were compared with those from ultra high performance liquid chromatography (UHPLC). Pseudo real-time, at-line monitoring showed the level of antioxidants in a batch extract of Calendula officinalis plateaued after 100 min of extraction. These results correlated well with those of an offline UHPLC study. SIA-CL was found to be a suitable method for pseudo real-time monitoring of plant extractions and determination of extraction endpoints with respect to antioxidant concentrations. The method was applied at-line in the manufacturing industry. Copyright © 2015 John Wiley & Sons, Ltd.

CLEANING UP PESTICIDE CONTAMINATED SOILS: COMPARING EFFECTIVENESS OF SUPERCRITICAL FLUID EXTRACTION WITH SOLVENT EXTRACTION AND LOW TEMPERATURE THERMAL DESORPTION

EPA Science Inventory

Bench-scale supercritical fluid extraction (SFE) studies were performed on soil samples obtained from a Superfund site that is contaminated with high levels of p,p,-DDT, p,p,-DDD, p,p,-DDE, toxaphene and hexachlorocyclohexane. The effectiveness of supercritical fluid extraction ...

High-titer and productivity of l-(+)-lactic acid using exponential fed-batch fermentation with Bacillus coagulans arr4, a new thermotolerant bacterial strain.

PubMed

Coelho, Luciana Fontes; Beitel, Susan Michelz; Sass, Daiane Cristina; Neto, Paulo Marcelo Avila; Contiero, Jonas

2018-04-01

Bacillus coagulans arr4 is a thermotolerant microorganism with great biotechnological potential for l-(+)-lactic acid production from granulated sugar and yeast extract. The highest l-(+)-lactic acid production was obtained with Ca(OH) 2 . The maximum production of l-(+)-lactic acid (206.81 g/L) was observed in exponential feeding using granulated sugar solution (900 g/L) and yeast extract (1%) at 50 °C, pH 6.5, and initial granulated sugar concentration of 100 g/L at 39 h. 5.3 g/L h productivity and 97% yield were observed, and no sugar remained. Comparing the simple batch with exponential fed-batch fermentation, the l(+) lactic acid production was improved in 133.22% and dry cell weight was improved in 83.29%, using granulated sugar and yeast extract. This study presents the highest productivity of lactic acid ever observed in the literature, on the fermentation of thermotolerant Bacillus sp. as well as an innovative and high-efficiency purification technology, using low-cost substances as Celite and charcoal. The recovery of lactic acid was 86%, with 100% protein removal, and the fermentation medium (brown color) became a colorless solution.

Methylamphetamine synthesized from cold medication as precursor source via two different routes show significantly different stable isotope signatures

NASA Astrophysics Data System (ADS)

Jayaram, S.; Daeid, N. Nic; Kerr, W. J.; Kemp, H. F.; Meier-Augenstein, W.

2012-04-01

This work exposes the variation in light element stable isotopic abundance values of 13C, 2H and 15N) derived from the analysis of methylamphetamine synthesized via 2 different synthetic routes popular with clandestine laboraties, the Hypophosphorous and the Moscow route. We repeatedly prepared the final product using known clandestine synthetic methods where the precursors, catalysts and reducing agents have themselves been derived from house hold products and commonly available cold medications. Methylamphetamine was prepared from both lab grade pseudoephedrine and pseudoephedrine extracted (using three different solvent systems) from Sudafed®, an over-the-counter cold medication widely available in the United Kingdom. Six repetitive batches of the final product were produced in each case to provide within and between batch variations thus yielding a total of 48 samples (24 for each route). We have demonstrated that stable isotope analysis by Isotope Ratio Mass Spectrometry (IRMS) is potentially useful in the comparison and discrimination of batches of methylamphetamine produced for each route and for each precursor depending on the solvent used for extracting the pseudoephedrine starting material. To our knowledge this is the first time multivariate stable isotope analysis has been applied to methylamphetamine samples synthesized from pseudoephedrine extracted from over-the-counter cold medications.

Extraction chromatography of the Rf homologs, Zr and Hf, using TEVA and UTEVA resins in HCl, HNO3, and H2SO4 media

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alfonso, M. C.; Bennett, M. E.; Folden, C. M.

2015-06-20

The extraction behavior of the Rf homologs, Zr and Hf, has been studied in HCl, HNO3, and H2SO4 media using TEVA (R) (a trioctyl and tridecyl methyl ammonium-based resin) and UTEVA (R) (a diamyl amylphosphonate-based resin). All six systems were considered for the future chemical characterization of Rf. Batch uptake studies were first performed to determine which systems could separate Zr and Hf and these results were used to determine what acid concentration range to focus on for the column studies. The batch uptake studies showed that UTEVA separates Zr and Hf in all media, while the intergroup separation wasmore » only observed in HCl media with TEVA. Both HCl systems showed viability for potential extraction chromatographic studies of Rf.« less

Headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

PubMed

Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

2008-11-20

Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

Can Chlamydia abortus be transmitted by embryo transfer in goats?

PubMed

Oseikria, M; Pellerin, J L; Rodolakis, A; Vorimore, F; Laroucau, K; Bruyas, J F; Roux, C; Michaud, S; Larrat, M; Fieni, F

2016-10-01

The objectives of this study were to determine (i) whether Chlamydia abortus would adhere to or penetrate the intact zona pellucida (ZP-intact) of early in vivo-derived caprine embryos, after in vitro infection; and (ii) the efficacy of the International Embryo Transfer Society (IETS) washing protocol for bovine embryos. Fifty-two ZP-intact embryos (8-16 cells), obtained from 14 donors were used in this experiment. The embryos were randomly divided into 12 batches. Nine batches (ZP-intact) of five embryos were incubated in a medium containing 4 × 10(7)Chlamydia/mL of AB7 strain. After incubation for 18 hours at 37 °C in an atmosphere of 5% CO2, the embryos were washed in batches in 10 successive baths of a phosphate buffer saline and 5% fetal calf serum solution in accordance with IETS guidelines. In parallel, three batches of ZP-intact embryos were used as controls by being subjected to similar procedures but without exposure to C. abortus. The 10 wash baths were collected separately and centrifuged for 1 hour at 13,000 × g. The washed embryos and the pellets of the 10 centrifuged wash baths were frozen at -20 °C before examination for evidence of C. abortus using polymerase chain reaction. C. abortus DNA was found in all of the infected batches of ZP-intact embryos (9/9) after 10 successive washes. It was also detected in the 10th wash fluid for seven batches of embryos, whereas for the two other batches, the last positive wash bath was the eighth and the ninth, respectively. In contrast, none of the embryos or their washing fluids in the control batches were DNA positive. These results report that C. abortus adheres to and/or penetrates the ZP of in vivo caprine embryos after in vitro infection, and that the standard washing protocol recommended by the IETS for bovine embryos, failed to remove it. The persistence of these bacteria after washing makes the embryo a potential means of transmission of the bacterium during embryo transfer from infected donor goats to healthy recipients and/or their offspring. Nevertheless, the detection of C. abortus DNA by polymerase chain reaction does not prove that the bacteria found was infectious. Further studies are required to investigate whether enzymatic and/or antibiotic treatment of caprine embryos infected by C. abortus would eliminate the bacteria from the ZP. Copyright © 2016 Elsevier Inc. All rights reserved.

Assessment of critical-fluid extractions in the process industries

NASA Technical Reports Server (NTRS)

1982-01-01

The potential for critical-fluid extraction as a separation process for improving the productive use of energy in the process industries is assessed. Critical-fluid extraction involves the use of fluids, normally gaseous at ambient conditions, as extraction solvents at temperatures and pressures around the critical point. Equilibrium and kinetic properties in this regime are very favorable for solvent applications, and generally allow major reductions in the energy requirements for separating and purifying chemical component of a mixture.

Antioxidant properties of mushroom mycelia obtained by batch cultivation and tocopherol content affected by extraction procedures.

PubMed

Vamanu, Emanuel

2014-01-01

The determination of the antioxidant potential of lyophilized mushroom mycelia from 5 strains of the species Pleurotus ostreatus and Coprinus comatus (obtained by submerged cultivation in batch system) was analyzed as ethanolic extracts by evaluating ABTS and the hydroxyl scavenging activity, FRAP method, the chelating capacity, the inhibition of human erythrocyte hemolysis, and the inhibition of xanthine oxidase activity. The main compounds present in all extracts were determined by HPLC chromatography. Overall, results demonstrated that the biologically active substances content is modulated by the extraction method used. The most beneficial extract, characterized by determining the EC50 value, was that of C. comatus M8102, followed by P. ostreatus PQMZ91109. Significant amount of α-tocopherol (179.51 ± 1.51 mg/100 g extract) was determined as well as flavones such as rutin and apigenin. In the P. ostreatus PQMZ91109 extract, 4.8 ± 0.05 mg/100 g extract of tocopherol acetate known to play a significant role as an antioxidant in skin protection against oxidative stress generated by UV rays was determined. The various correlations (r (2) = 0.7665-0.9426 for tocopherol content) assessed and the composition of extracts in fluidized bed from the mycelia of the tested species depicted a significant pharmacological potential as well as the possibility of usage in the development of new functional products.

Combining Experiments and Simulations of Extraction Kinetics and Thermodynamics in Advanced Separation Processes for Used Nuclear Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nilsson, Mikael

This 3-year project was a collaboration between University of California Irvine (UC Irvine), Pacific Northwest National Laboratory (PNNL), Idaho National Laboratory (INL), Argonne National Laboratory (ANL) and with an international collaborator at ForschungZentrum Jülich (FZJ). The project was led from UC Irvine under the direction of Profs. Mikael Nilsson and Hung Nguyen. The leads at PNNL, INL, ANL and FZJ were Dr. Liem Dang, Dr. Peter Zalupski, Dr. Nathaniel Hoyt and Dr. Giuseppe Modolo, respectively. Involved in this project at UC Irvine were three full time PhD graduate students, Tro Babikian, Ted Yoo, and Quynh Vo, and one MS student,more » Alba Font Bosch. The overall objective of this project was to study how the kinetics and thermodynamics of metal ion extraction can be described by molecular dynamic (MD) simulations and how the simulations can be validated by experimental data. Furthermore, the project includes the applied separation by testing the extraction systems in a single stage annular centrifugal contactor and coupling the experimental data with computational fluid dynamic (CFD) simulations. Specific objectives of the proposed research were: Study and establish a rigorous connection between MD simulations based on polarizable force fields and extraction thermodynamic and kinetic data. Compare and validate CFD simulations of extraction processes for An/Ln separation using different sizes (and types) of annular centrifugal contactors. Provide a theoretical/simulation and experimental base for scale-up of batch-wise extraction to continuous contactors. We approached objective 1 and 2 in parallel. For objective 1 we started by studying a well established extraction system with a relatively simple extraction mechanism, namely tributyl phosphate. What we found was that well optimized simulations can inform experiments and new information on TBP behavior was presented in this project, as well be discussed below. The second objective proved a larger challenge and most of the efforts were devoted to experimental studies.« less

METHOD FOR THE SUPERCRITICAL FLUID EXTRACTION OF SOILS/SEDIMENTS

EPA Science Inventory

Supercritical fluid extraction has been publicized as an extraction method which has several advantages over conventional methods, and it is expected to result in substantial cost and labor savings. This study was designed to evaluate the feasibility of using supercritical fluid ...

Biotransformation of sweet lime pulp waste into high-quality nanocellulose with an excellent productivity using Komagataeibacter europaeus SGP37 under static intermittent fed-batch cultivation.

PubMed

Dubey, Swati; Singh, Jyoti; Singh, R P

2018-01-01

Herein, sweet lime pulp waste (SLPW) was utilized as a low- or no-cost feedstock for the production of bacterial nanocellulose (BNC) alone and in amalgamation with other nutritional supplements by the isolate K. europaeus SGP37 under static batch and static intermittent fed-batch cultivation. The highest yield (26.2±1.50gL -1 ) was obtained in the hot water extract of SLPW supplemented with the components of HS medium, which got further boosted to 38±0.85gL -1 as the cultivation strategy was shifted from static batch to static intermittent fed-batch. BNC obtained from various SLPW medium was similar or even superior to that obtained with standard HS medium in terms of its physicochemical properties. The production yields of BNC thus obtained are significantly higher and fit well in terms of industrial scale production. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of major aromatic constituents in vanilla using an on-line supercritical fluid extraction coupled with supercritical fluid chromatography.

PubMed

Liang, Yanshan; Liu, Jiaqi; Zhong, Qisheng; Shen, Lingling; Yao, Jinting; Huang, Taohong; Zhou, Ting

2018-04-01

An on-line supercritical fluid extraction coupled with supercritical fluid chromatography method was developed for the determination of four major aromatic constituents in vanilla. The parameters of supercritical fluid extraction were systematically investigated using single factor optimization experiments and response surface methodology by a Box-Behnken design. The modifier ratio, split ratio, and the extraction temperature and pressure were the major parameters which have significant effects on the extraction. While the static extraction time, dynamic extraction time, and recycle time had little influence on the compounds with low polarity. Under the optimized conditions, the relative extraction efficiencies of all the constituents reached 89.0-95.1%. The limits of quantification were in the range of 1.123-4.747 μg. The limits of detection were in the range of 0.3368-1.424 μg. The recoveries of the four analytes were in the range of 76.1-88.9%. The relative standard deviations of intra- and interday precision ranged from 4.2 to 7.6%. Compared with other off-line methods, the present method obtained higher extraction yields for all four aromatic constituents. Finally, this method has been applied to the analysis of vanilla from different sources. On the basis of the results, the on-line supercritical fluid extraction-supercritical fluid chromatography method shows great promise in the analysis of aromatic constituents in natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In-syringe extraction using dissolvable layered double hydroxide-polymer sponges templated from hierarchically porous coordination polymers.

PubMed

Ghani, Milad; Frizzarin, Rejane M; Maya, Fernando; Cerdà, Víctor

2016-07-01

Herein we report the use of cobalt porous coordination polymers (PCP) as intermediates to prepare advanced extraction media based on layered double hydroxides (LDH) supported on melamine polymer foam. The obtained dissolvable Ni-Co LDH composite sponges can be molded and used as sorbent for the in-syringe solid-phase extraction (SPE) of phenolic acids from fruit juices. The proposed sorbent is obtained due to the surfactant-assisted self-assembly of Co(II)/imidazolate PCPs on commercially available melamine foam, followed by the in situ conversion of the PCP into the final dissolvable LDH coating. Advantageous features for SPE are obtained by using PCPs with hierarchical porosity (HPCPs). The LDH-sponge prepared using intermediate HPCPs (HLDH-sponge) is placed in the headspace of a glass syringe, enabling flow-through extraction followed by analyte elution by the dissolution of the LDH coating in acidic conditions. Three phenolic acids (gallic acid, p-hydroxybenzoic acid and caffeic acid) were extracted and quantified using high performance liquid chromatography. Using a 5mL sample volume, the obtained detection limits were 0.15-0.35μgL(-1). The proposed method for the preparation of HLDH-sponges showed a good reproducibility as observed from the intra- and inter-day RSD's, which were <10% for all analytes. The batch-to-batch reproducibility for three different batches of HLDH-sponges was 10.6-11.2%. Enrichment factors of 15-21 were obtained. The HLDH-sponges were applied satisfactorily to the determination of phenolic acids in natural and commercial fruit juices, obtaining relative recoveries among 89.7-95.3%. Copyright © 2016 Elsevier B.V. All rights reserved.

Application of supercritical fluid carbon dioxide to the extraction and analysis of lipids.

PubMed

Lee, Jae Won; Fukusaki, Eiichiro; Bamba, Takeshi

2012-10-01

Supercritical carbon dioxide (SCCO(2)) is an ecofriendly supercritical fluid that is chemically inert, nontoxic, noninflammable and nonpolluting. As a green material, SCCO(2) has desirable properties such as high density, low viscosity and high diffusivity that make it suitable for use as a solvent in supercritical fluid extraction, an effective and environment-friendly analytical method, and as a mobile phase for supercritical fluid chromatography, which facilitates high-throughput, high-resolution analysis. Furthermore, the low polarity of SCCO(2) is suitable for the extraction and analysis of hydrophobic compounds. The growing concern surrounding environmental pollution has triggered the development of green analysis methods based on the use of SCCO(2) in various laboratories and industries. SCCO(2) is becoming an effective alternative to conventional organic solvents. In this review, the usefulness of SCCO(2) in supercritical fluid extraction and supercritical fluid chromatography for the extraction and analysis of lipids is described.

Extracting surface diffusion coefficients from batch adsorption measurement data: application of the classic Langmuir kinetics model.

PubMed

Chu, Khim Hoong

2017-11-09

Surface diffusion coefficients may be estimated by fitting solutions of a diffusion model to batch kinetic data. For non-linear systems, a numerical solution of the diffusion model's governing equations is generally required. We report here the application of the classic Langmuir kinetics model to extract surface diffusion coefficients from batch kinetic data. The use of the Langmuir kinetics model in lieu of the conventional surface diffusion model allows derivation of an analytical expression. The parameter estimation procedure requires determining the Langmuir rate coefficient from which the pertinent surface diffusion coefficient is calculated. Surface diffusion coefficients within the 10 -9 to 10 -6  cm 2 /s range obtained by fitting the Langmuir kinetics model to experimental kinetic data taken from the literature are found to be consistent with the corresponding values obtained from the traditional surface diffusion model. The virtue of this simplified parameter estimation method is that it reduces the computational complexity as the analytical expression involves only an algebraic equation in closed form which is easily evaluated by spreadsheet computation.

Acetone-butanol-ethanol (ABE) fermentation using Clostridium acetobutylicum XY16 and in situ recovery by PDMS/ceramic composite membrane.

PubMed

Wu, Hao; Chen, Xiao-Peng; Liu, Gong-Ping; Jiang, Min; Guo, Ting; Jin, Wan-Qin; Wei, Ping; Zhu, Da-Wei

2012-09-01

PDMS/ceramic composite membrane was directly integrated with acetone-butanol-ethanol (ABE) fermentation using Clostridium acetobutylicum XY16 at 37 °C and in situ removing ABE from fermentation broth. The membrane was integrated with batch fermentation, and approximately 46 % solvent was extracted. The solvent in permeates was 118 g/L, and solvent productivity was 0.303 g/(L/h), which was approximately 33 % higher compared with the batch fermentation without in situ recovery. The fed-batch fermentation with in situ recovery by pervaporation continued for more than 200 h, 61 % solvent was extracted, and the solvent in penetration was 96.2 g/L. The total flux ranged from 0.338 to 0.847 kg/(m(2)/h) and the separation factor of butanol ranged from 5.1 to 27.1 in this process. The membrane was fouled by the active fermentation broth, nevertheless the separation performances were partially recovered by offline membrane cleaning, and the solvent productivity was increased to 0.252 g/(L/h), which was 19 % higher compared with that in situ recovery process without membrane cleaning.

[Optimization of supercritical fluid extraction of bioactive components in Ligusticum chuanxiong by orthogonal array design].

PubMed

Hu, Li-Cui; Wu, Xun; Yang, Xue-Dong

2013-10-01

With the yields of ferulic acid, coniferylferulate, Z-ligustilide, senkyunolide A, butylidenephthalide, butylphthalide, senkyunolide I, senkyunolide H, riligustilide, levistolide A, and total pharmacologically active ingredient as evaluation indexes, the extraction of Ligusticum chuanxiong by supercritical fluid technology was investigated through an orthogonal experiment L9 (3(4)). Four factors, namely temperature, pressure, flow rate of carbon dioxide, co-solvent concentration of the supercritical fluid, were investigated and optimized. Under the optimized conditions, namely 65 degrees C of temperature, 35 MPa of pressure, 1 L x min(-1) of CO2 flow rate, 8% of co-solvent concetration, supercritical fluid extraction could achieve a better yield than the conventional reflux extraction using methanol. And the supercritical fluid extraction process was validated to be stable and reliable.

Growth of the extremophilic Deinococcus geothermalis DSM 11302 using co-substrate fed-batch culture.

PubMed

Bornot, Julie; Molina-Jouve, Carole; Uribelarrea, Jean-Louis; Gorret, Nathalie

2014-02-01

Deinococcus geothermalis metabolism has been scarcely studied to date, although new developments on its utilization for bioremediation have been carried out. So, large-scale production of this strain and a better understanding of its physiology are required. A fed-batch experiment was conducted to achieve a high cell density non-limiting culture of D. geothermalis DSM 11302. A co-substrate nutritional strategy using glucose and yeast extract was carried out in a 20-L bioreactor in order to maintain a non-limited growth at a maximal growth rate of 1 h(-1) at 45 °C. Substrate supplies were adjusted by monitoring online culture parameters and physiological data (dissolved oxygen, gas analyses, respiratory quotient, biomass concentration). The results showed that yeast extract could serve as both carbon and nitrogen sources, although glucose and ammonia were consumed too. Yeast extract carbon-specific uptake rate reached a value 4.5 times higher than glucose carbon-specific uptake rate. Cell concentration of 9.6 g L(-1) dry cell weight corresponding to 99 g of biomass was obtained using glucose and yeast extract as carbon and nitrogen sources.

Effect of bioaugmentation by cellulolytic bacteria enriched from sheep rumen on methane production from wheat straw.

PubMed

Ozbayram, E Gozde; Kleinsteuber, Sabine; Nikolausz, Marcell; Ince, Bahar; Ince, Orhan

2017-08-01

The aim of this study was to determine the potential of bioaugmentation with cellulolytic rumen microbiota to enhance the anaerobic digestion of lignocellulosic feedstock. An anaerobic cellulolytic culture was enriched from sheep rumen fluid using wheat straw as substrate under mesophilic conditions. To investigate the effects of bioaugmentation on methane production from straw, the enrichment culture was added to batch reactors in proportions of 2% (Set-1) and 4% (Set-2) of the microbial cell number of the standard inoculum slurry. The methane production in the bioaugmented reactors was higher than in the control reactors. After 30 days of batch incubation, the average methane yield was 154 mL N CH 4 g VS -1 in the control reactors. Addition of 2% enrichment culture did not enhance methane production, whereas in Set-2 the methane yield was increased by 27%. The bacterial communities were examined by 454 amplicon sequencing of 16S rRNA genes, while terminal restriction fragment length polymorphism (T-RFLP) fingerprinting of mcrA genes was applied to analyze the methanogenic communities. The results highlighted that relative abundances of Ruminococcaceae and Lachnospiraceae increased during the enrichment. However, Cloacamonaceae, which were abundant in the standard inoculum, dominated the bacterial communities of all batch reactors. T-RFLP profiles revealed that Methanobacteriales were predominant in the rumen fluid, whereas the enrichment culture was dominated by Methanosarcinales. In the batch rectors, the most abundant methanogens were affiliated to Methanobacteriales and Methanomicrobiales. Our results suggest that bioaugmentation with sheep rumen enrichment cultures can enhance the performance of digesters treating lignocellulosic feedstock. Copyright © 2017 Elsevier Ltd. All rights reserved.

Mixed Carboxylic Acid Production by Megasphaera elsdenii from Glucose and Lignocellulosic Hydrolysate

DOE PAGES

Nelson, Robert S.; Peterson, Darren J.; Karp, Eric M.; ...

2017-03-01

Here, volatile fatty acids (VFAs) can be readily produced from many anaerobic microbes and subsequently utilized as precursors to renewable biofuels and biochemicals. Megasphaera elsdenii represents a promising host for production of VFAs, butyric acid (BA) and hexanoic acid (HA). However, due to the toxicity of these acids, product removal via an extractive fermentation system is required to achieve high titers and productivities. Here, we examine multiple aspects of extractive separations to produce BA and HA from glucose and lignocellulosic hydrolysate with M. elsdenii. A mixture of oleyl alcohol and 10% (v/v) trioctylamine was selected as an extraction solvent duemore » to its insignificant inhibitory effect on the bacteria. Batch extractive fermentations were conducted in the pH range of 5.0 to 6.5 to select the best cell growth rate and extraction efficiency combination. Subsequently, fed-batch pertractive fermentations were run over 230 h, demonstrating high BA and HA concentrations in the extracted fraction (57.2 g/L from ~190 g/L glucose) and productivity (0.26 g/L/h). To our knowledge, these are the highest combined acid titers and productivity values reported for M. elsdenii and bacterial mono-cultures from sugars. Lastly, the production of BA and HA (up to 17 g/L) from lignocellulosic sugars was demonstrated.« less

Mixed Carboxylic Acid Production by Megasphaera elsdenii from Glucose and Lignocellulosic Hydrolysate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nelson, Robert S.; Peterson, Darren J.; Karp, Eric M.

Here, volatile fatty acids (VFAs) can be readily produced from many anaerobic microbes and subsequently utilized as precursors to renewable biofuels and biochemicals. Megasphaera elsdenii represents a promising host for production of VFAs, butyric acid (BA) and hexanoic acid (HA). However, due to the toxicity of these acids, product removal via an extractive fermentation system is required to achieve high titers and productivities. Here, we examine multiple aspects of extractive separations to produce BA and HA from glucose and lignocellulosic hydrolysate with M. elsdenii. A mixture of oleyl alcohol and 10% (v/v) trioctylamine was selected as an extraction solvent duemore » to its insignificant inhibitory effect on the bacteria. Batch extractive fermentations were conducted in the pH range of 5.0 to 6.5 to select the best cell growth rate and extraction efficiency combination. Subsequently, fed-batch pertractive fermentations were run over 230 h, demonstrating high BA and HA concentrations in the extracted fraction (57.2 g/L from ~190 g/L glucose) and productivity (0.26 g/L/h). To our knowledge, these are the highest combined acid titers and productivity values reported for M. elsdenii and bacterial mono-cultures from sugars. Lastly, the production of BA and HA (up to 17 g/L) from lignocellulosic sugars was demonstrated.« less

Pressurized fluid extraction of essential oil from Lavandula hybrida using a modified supercritical fluid extractor and a central composite design for optimization.

PubMed

Kamali, Hossein; Jalilvand, Mohammad Reza; Aminimoghadamfarouj, Noushin

2012-06-01

Essential oil components were extracted from lavandin (Lavandula hybrida) flowers using pressurized fluid extraction. A central composite design was used to optimize the effective extraction variables. The chemical composition of extracted samples was analyzed by a gas chromatograph-flame ionization detector column. For achieving 100% extraction yield, the temperature, pressure, extraction time, and the solvent flow rate were adjusted at 90.6°C, 63 bar, 30.4 min, and 0.2 mL/min, respectively. The results showed that pressurized fluid extraction is a practical technique for separation of constituents such as 1,8-cineole (8.1%), linalool (34.1%), linalyl acetate (30.5%), and camphor (7.3%) from lavandin to be applied in the food, fragrance, pharmaceutical, and natural biocides industries. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Kinetics of sugars consumption and ethanol inhibition in carob pulp fermentation by Saccharomyces cerevisiae in batch and fed-batch cultures.

PubMed

Lima-Costa, Maria Emília; Tavares, Catarina; Raposo, Sara; Rodrigues, Brígida; Peinado, José M

2012-05-01

The waste materials from the carob processing industry are a potential resource for second-generation bioethanol production. These by-products are small carob kibbles with a high content of soluble sugars (45-50%). Batch and fed-batch Saccharomyces cerevisiae fermentations of high density sugar from carob pods were analyzed in terms of the kinetics of sugars consumption and ethanol inhibition. In all the batch runs, 90-95% of the total sugar was consumed and transformed into ethanol with a yield close to the theoretical maximum (0.47-0.50 g/g), and a final ethanol concentration of 100-110 g/l. In fed-batch runs, fresh carob extract was added when glucose had been consumed. This addition and the subsequent decrease of ethanol concentrations by dilution increased the final ethanol production up to 130 g/l. It seems that invertase activity and yeast tolerance to ethanol are the main factors to be controlled in carob fermentations. The efficiency of highly concentrated carob fermentation makes it a very promising process for use in a second-generation ethanol biorefinery.

A FLUID SORBENT RECYCLING DEVICE FOR INDUSTRIAL FLUID USERS

EPA Science Inventory

A roller compression Extractor® that extracts fluids from reusable sorbent pads was evaluated as a method of waste reduction. The extraction device, evaluated for industrial fluid users in New Jersey, was found to be effective in recycling unpleated sorbent pads, especially ...

Batch experiments versus soil pore water extraction--what makes the difference in isoproturon (bio-)availability?

PubMed

Folberth, Christian; Suhadolc, Metka; Scherb, Hagen; Munch, Jean Charles; Schroll, Reiner

2009-10-01

Two approaches to determine pesticide (bio-)availability in soils (i) batch experiments with "extraction with an excess of water" (EEW) and (ii) the recently introduced "soil pore water (PW) extraction" of pesticide incubated soil samples have been compared with regard to the sorption behavior of the model compound isoproturon in soils. A significant correlation between TOC and adsorbed pesticide amount was found when using the EEW approach. In contrast, there was no correlation between TOC and adsorbed isoproturon when using the in situ PW extraction method. Furthermore, sorption was higher at all concentrations in the EEW method when comparing the distribution coefficients (K(d)) for both methods. Over all, sorption in incubated soil samples at an identical water tension (-15 kPa) and soil density (1.3 g cm(-3)) appears to be controlled by a complex combination of sorption driving soil parameters. Isoproturon bioavailability was found to be governed in different soils by binding strength and availability of sorption sites as well as water content, whereas the dominance of either one of these factors seems to depend on the individual composition and characteristics of the respective soil sample. Using multiple linear regression analysis we obtained furthermore indications that the soil pore structure is affected by the EEW method due to disaggregation, resulting in a higher availability of pesticide sorption sites than in undisturbed soil samples. Therefore, it can be concluded that isoproturon sorption is overestimated when using the EEW method, which should be taken into account when using data from this approach or similar batch techniques for risk assessment analysis.

Extracts of Morus nigra L. Leaves Standardized in Chlorogenic Acid, Rutin and Isoquercitrin: Tyrosinase Inhibition and Cytotoxicity

PubMed Central

Fontes, Pedro Ribeiro; Souza, Paula Monteiro; William Fagg, Christopher; Neves Silva Guerra, Eliete; de Medeiros Nóbrega, Yanna Karla; Silveira, Damaris; Fonseca-Bazzo, Yris; Simeoni, Luiz Alberto; Homem-de-Mello, Maurício; Oliveira Magalhães, Pérola

2016-01-01

Melanogenesis is a process responsible for melanin production, which is stored in melanocytes containing tyrosinase. Inhibition of this enzyme is a target in the cosmetics industry, since it controls undesirable skin conditions such as hyperpigmentation due to the overproduction of melanin. Species of the Morus genus are known for the beneficial uses offered in different parts of its plants, including tyrosinase inhibition. Thus, this project aimed to study the inhibitory activity of tyrosinase by extracts from Morus nigra leaves as well as the characterization of its chromatographic profile and cytotoxicity in order to become a new therapeutic option from a natural source. M. nigra leaves were collected, pulverized, equally divided into five batches and the standardized extract was obtained by passive maceration. There was no significant difference between batches for total solids content, yield and moisture content, which shows good reproducibility of the extraction process. Tyrosinase enzymatic activity was determined for each batch, providing the percentage of enzyme inhibition and IC50 values obtained by constructing dose-response curves and compared to kojic acid, a well-known tyrosinase inhibitor. High inhibition of tyrosinase activity was observed (above 90% at 15.625 μg/mL). The obtained IC50 values ranged from 5.00 μg/mL ± 0.23 to 8.49 μg/mL ± 0.59 and were compared to kojic acid (3.37 μg/mL ± 0.65). High Performance Liquid Chromatography analysis revealed the presence of chlorogenic acid, rutin and, its major compound, isoquercitrin. The chromatographic method employed was validated according to ICH guidelines and the extract was standardized using these polyphenols as markers. Cytotoxicity, assessed by MTT assay, was not observed on murine melanomas, human keratinocytes and mouse fibroblasts in tyrosinase IC50 values. This study demonstrated the potential of M. nigra leaf extract as a promising whitening agent of natural source against skin hyperpigmentation. PMID:27655047

A comparison of accelerated solvent extraction, Soxhlet extraction, and ultrasonic-assisted extraction for analysis of terpenoids and sterols in tobacco.

PubMed

Shen, Jinchao; Shao, Xueguang

2005-11-01

The performance of accelerated solvent extraction in the analysis of terpenoids and sterols in tobacco samples was investigated and compared with those of Soxhlet extraction and ultrasonically assisted extraction with respect to yield, extraction time, reproducibility and solvent consumption. The results indicate that although the highest yield was achieved by Soxhlet extraction, ASE appears to be a promising alternative to classical methods since it is faster and uses less solvent, especially when applied to the investigation of large batch tobacco samples. However, Soxhlet extraction is still the preferred method for analyzing sterols since it gives a higher extraction efficiency than other methods.

COMPARISONS OF SOXHLET EXTRACTION, PRESSURIZED LIQUID EXTRACTION, SUPERCRITICAL FLUID EXTRACTION, AND SUBCRITICAL WATER EXTRACTION FOR ENVIRONMENTAL SOLIDS: RECOVERY, SELECTIVITY, AND EFFECTS ON SAMPLE MATRIX. (R825394)

EPA Science Inventory

Extractions of a polycyclic aromatic hydrocarbon (PAH)-contaminated soil from a former manufactured gas plant site were performed with a Soxhlet apparatus (18 h), by pressurized liquid extraction (PLE) (50 min at 100°C), supercritical fluid extraction (SFE) (1 h at 150°...

Application of response surface methodology to optimise supercritical carbon dioxide extraction of volatile compounds from Crocus sativus.

PubMed

Shao, Qingsong; Huang, Yuqiu; Zhou, Aicun; Guo, Haipeng; Zhang, Ailian; Wang, Yong

2014-05-01

Crocus sativus has been used as a traditional Chinese medicine for a long time. The volatile compounds of C. sativus appear biologically active and may act as antioxidants as well as anticonvulsants, antidepressants and antitumour agents. In order to obtain the highest possible yield of essential oils from C. sativus, response surface methodology was employed to optimise the conditions of supercritical fluid carbon dioxide extraction of the volatile compounds from C. sativus. Four factorswere investigated: temperature, pressure, extraction time and carbon dioxide flow rate. Furthermore, the chemical compositions of the volatile compounds extracted by supercritical fluid extraction were compared with those obtained by hydro-distillation and Soxhlet extraction. The optimum extraction conditions were found to be: optimised temperature 44.9°C, pressure 34.9 MPa, extraction time 150.2 min and CO₂ flow rate 10.1 L h⁻¹. Under these conditions, the mean extraction yield was 10.94 g kg⁻¹. The volatile compounds extracted by supercritical fluid extraction and Soxhlet extraction contained a large amount of unsaturated fatty acids. Response surface methodology was successfully applied for supercritical fluid CO₂ extraction optimisation of the volatile compounds from C. sativus. The study showed that pressure and CO₂ flow rate had significant effect on volatile compounds yield produced by supercritical fluid extraction. This study is beneficial for the further research operating on a large scale. © 2013 Society of Chemical Industry.

Characterising and correcting batch variation in an automated direct infusion mass spectrometry (DIMS) metabolomics workflow.

PubMed

Kirwan, J A; Broadhurst, D I; Davidson, R L; Viant, M R

2013-06-01

Direct infusion mass spectrometry (DIMS)-based untargeted metabolomics measures many hundreds of metabolites in a single experiment. While every effort is made to reduce within-experiment analytical variation in untargeted metabolomics, unavoidable sources of measurement error are introduced. This is particularly true for large-scale multi-batch experiments, necessitating the development of robust workflows that minimise batch-to-batch variation. Here, we conducted a purpose-designed, eight-batch DIMS metabolomics study using nanoelectrospray (nESI) Fourier transform ion cyclotron resonance mass spectrometric analyses of mammalian heart extracts. First, we characterised the intrinsic analytical variation of this approach to determine whether our existing workflows are fit for purpose when applied to a multi-batch investigation. Batch-to-batch variation was readily observed across the 7-day experiment, both in terms of its absolute measurement using quality control (QC) and biological replicate samples, as well as its adverse impact on our ability to discover significant metabolic information within the data. Subsequently, we developed and implemented a computational workflow that includes total-ion-current filtering, QC-robust spline batch correction and spectral cleaning, and provide conclusive evidence that this workflow reduces analytical variation and increases the proportion of significant peaks. We report an overall analytical precision of 15.9%, measured as the median relative standard deviation (RSD) for the technical replicates of the biological samples, across eight batches and 7 days of measurements. When compared against the FDA guidelines for biomarker studies, which specify an RSD of <20% as an acceptable level of precision, we conclude that our new workflows are fit for purpose for large-scale, high-throughput nESI DIMS metabolomics studies.

Effects of process parameters on solid self-microemulsifying particles in a laboratory scale fluid bed.

PubMed

Mukherjee, Tusharmouli; Plakogiannis, Fotios M

2012-01-01

The purpose of this study was to select the critical process parameters of the fluid bed processes impacting the quality attribute of a solid self-microemulsifying (SME) system of albendazole (ABZ). A fractional factorial design (2(4-1)) with four parameters (spray rate, inlet air temperature, inlet air flow, and atomization air pressure) was created by MINITAB software. Batches were manufactured in a laboratory top-spray fluid bed at 625-g scale. Loss on drying (LOD) samples were taken throughout each batch to build the entire moisture profiles. All dried granulation were sieved using mesh 20 and analyzed for particle size distribution (PSD), morphology, density, and flow. It was found that as spray rate increased, sauter-mean diameter (D(s)) also increased. The effect of inlet air temperature on the peak moisture which is directly related to the mean particle size was found to be significant. There were two-way interactions between studied process parameters. The main effects of inlet air flow rate and atomization air pressure could not be found as the data were inconclusive. The partial least square (PLS) regression model was found significant (P < 0.01) and predictive for optimization. This study established a design space for the parameters for solid SME manufacturing process.

Biodiesel production from Nannochloropsis gaditana lipids through transesterification catalyzed by Rhizopus oryzae lipase.

PubMed

Navarro López, Elvira; Robles Medina, Alfonso; González Moreno, Pedro Antonio; Esteban Cerdán, Luis; Martín Valverde, Lorena; Molina Grima, Emilio

2016-03-01

Biodiesel (fatty acid methyl esters, FAMEs) was produced from saponifiable lipids (SLs) extracted from wet Nannochloropsis gaditana biomass using methanolysis catalyzed by Rhizopus oryzae intracellular lipase. SLs were firstly extracted with ethanol to obtain 31 wt% pure SLs. But this low SL purity also gave a low biodiesel conversion (58%). This conversion increased up to 80% using SLs purified by crystallization in acetone (95 wt% purity). Polar lipids play an important role in decreasing the reaction velocity - using SLs extracted with hexane, which have lower polar lipid content (37.4% versus 49.0% using ethanol), we obtained higher reaction velocities and less FAME conversion decrease when the same lipase batch was reused. 83% of SLs were transformed to biodiesel using a 70 wt% lipase/SL ratio, 11:1 methanol/SL molar ratio, 10 mL t-butanol/g SLs after 72 h. The FAME conversion decreased to 71% after catalyzing three reactions with the same lipase batch. Copyright © 2015 Elsevier Ltd. All rights reserved.

[Study on the dynamic model with supercritical CO2 fluid extracting the lipophilic components in Panax notoginseng].

PubMed

Duan, Xian-Chun; Wang, Yong-Zhong; Zhang, Jun-Ru; Luo, Huan; Zhang, Heng; Xia, Lun-Zhu

2011-08-01

To establish a dynamics model for extracting the lipophilic components in Panax notoginseng with supercritical carbon dioxide (CO2). Based on the theory of counter-flow mass transfer and the molecular mass transfer between the material and the supercritical CO2 fluid under differential mass-conservation equation, a dynamics model was established and computed to compare forecasting result with the experiment process. A dynamics model has been established for supercritical CO2 to extract the lipophilic components in Panax notoginseng, the computed result of this model was consistent with the experiment process basically. The supercritical fluid extract dynamics model established in this research can expound the mechanism in the extract process of which lipophilic components of Panax notoginseng dissolve the mass transfer and is tallied with the actual extract process. This provides certain instruction for the supercritical CO2 fluid extract' s industrialization enlargement.

Removal of common organic solvents from aqueous waste streams via supercritical C02 extraction: a potential green approach to sustainable waste management in the pharmaceutical industry.

PubMed

Leazer, Johnnie L; Gant, Sean; Houck, Anthony; Leonard, William; Welch, Christopher J

2009-03-15

Supercritical CO2 extraction of aqueous streams is a convenient and effective method to remove commonly used solvents of varying polarities from aqueous waste streams. The resulting aqueous layers can potentially be sewered; whereas the organic layer can be recovered for potential reuse. Supercritical fluid extraction (SFE) is a technology that is increasingly being used in commercial processes (1). Supercritical fluids are well suited for extraction of a variety of media, including solids, natural products, and liquid products. Many supercritical fluids have low critical temperatures, allowing for extractions to be done at modestly low temperatures, thus avoiding any potential thermal decomposition of the solutes under study (2). Furthermore, the CO2 solvent strength is easily tuned by adjusting the density of the supercritical fluid (The density is proportional to the pressure of the extraction process). Since many supercritical fluids are gases at ambient temperature, the extract can be concentrated by simply venting the reaction mixture to a cyclone collection vessel, using appropriate safety protocols.

Results of initial analyses of the salt (macro) batch 9 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

2015-10-01

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Interim Salt Disposition Project (ISDP) Salt (Macro) Batch 9 for processing through the Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU). This document reports the initial results of the analyses of samples of Tank 21H. Analysis of the Tank 21H Salt (Macro) Batch 9 composite sample indicates that the material does not display any unusual characteristics or observations, such as floating solids, the presence of large amount of solids, or unusual colors. Further results on the chemistry and other tests willmore » be issued in the future.« less

Effect temperature of supercritical CO2 fluid extraction on phytochemical analysis and antioxidant activity of Zingiber officinale Roscoe

NASA Astrophysics Data System (ADS)

Sondari, Dewi; Irawadi, Tun Tedja; Setyaningsih, Dwi; Tursiloadi, Silvester

2017-11-01

Supercritical fluid extraction of Zingiber officinale Roscoe has been carried out at a pressure of 16 MPa, with temperatures between 20-40 °C, during extraction time of 6 hours and the flow rate of CO2 fluid 5.5 ml/min. The result of supercritical method was compared with the extraction maceration using a mixture of water and ethanol (70% v/v) for 24 hours. The main content in ginger that has a main role as an antioxidant is a gingerol compound that can help neutralize the damaging effects caused by free radicals in the body, as anti-coagulant, and inhibit the occurrence of blood clots. This study aims to determine the effect of temperature on chemical components contained in rough extract of Zingiber officinale Roscoe and its antioxidant activity, total phenol and total flavonoid content. To determine the chemical components contained in the crude extract of Zingiber officinale Roscoe extracted by supercritical fluid and maceration extraction, GC-MS analysis was performed. Meanwhile, the antioxidant activity of the extract was evaluated based on a 2.2-diphenyl-1-picrylhydrazyl (DPPH) free radical damping method. The results of the analysis show that the result of ginger extract by using the supercritical CO2 extraction method has high antioxidant activity than by using maceration method. The highest total phenol content and total flavonoids were obtained on ginger extraction using supercritical CO2 fluid extraction, indicating that phenol and flavonoid compounds contribute to antioxidant activity. Chromatographic analysis showed that the chemical profile of ginger extract containing oxygenated monoterpenes, monoterpene hydrocarbons, sesquiterpene hydrocarbons, oxygenated monoterpene gingerol and esters. In supercritical fluid extraction, the compounds that can be identified at a temperature of 20-40 °C contain 27 compounds, and 11 compounds from the result of maceration extract. The main component of Zingiber officinale Roscoe extracted using supercritical fluid at a temperature of 40 °C is Hexanal (6.04%), Butan-2-one, 4-(3-hydroxy-2-methoxyphenyl) (27.95%), [6]-Paradol (0.73%), Gingerol (8.22%), Bis (2-ethylhexyl) phthalate (1.62%), α-Citral (12.14%) and α-zingiberene (2.90%). The main component extracts of Zingiber officinale Roscoe by maceration is Hexanal (10.71%), Decanal (3.74%), Butan-2-one, 4-(3-hydroxy-2-methoxyphenyl) (38.33%), Gingerol (4.56%) and Zingiberene (0.99).

MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

EPA Science Inventory

The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

Influence of Excipients and Spray Drying on the Physical and Chemical Properties of Nutraceutical Capsules Containing Phytochemicals from Black Bean Extract.

PubMed

Guajardo-Flores, Daniel; Rempel, Curtis; Gutiérrez-Uribe, Janet A; Serna-Saldívar, Sergio O

2015-12-03

Black beans (Phaseolus vulgaris L.) are a rich source of flavonoids and saponins with proven health benefits. Spray dried black bean extract powders were used in different formulations for the production of nutraceutical capsules with reduced batch-to-batch weight variability. Factorial designs were used to find an adequate maltodextrin-extract ratio for the spray-drying process to produce black bean extract powders. Several flowability properties were used to determine composite flow index of produced powders. Powder containing 6% maltodextrin had the highest yield (78.6%) and the best recovery of flavonoids and saponins (>56% and >73%, respectively). The new complexes formed by the interaction of black bean powder with maltodextrin, microcrystalline cellulose 50 and starch exhibited not only bigger particles, but also a rougher structure than using only maltodextrin and starch as excipients. A drying process prior to capsule production improved powder flowability, increasing capsule weight and reducing variability. The formulation containing 25.0% of maltodextrin, 24.1% of microcrystalline cellulose 50, 50% of starch and 0.9% of magnesium stearate produced capsules with less than 2.5% weight variability. The spray drying technique is a feasible technique to produce good flow extract powders containing valuable phytochemicals and low cost excipients to reduce the end-product variability.

Optimization of the Ethanol Recycling Reflux Extraction Process for Saponins Using a Design Space Approach

PubMed Central

Gong, Xingchu; Zhang, Ying; Pan, Jianyang; Qu, Haibin

2014-01-01

A solvent recycling reflux extraction process for Panax notoginseng was optimized using a design space approach to improve the batch-to-batch consistency of the extract. Saponin yields, total saponin purity, and pigment yield were defined as the process critical quality attributes (CQAs). Ethanol content, extraction time, and the ratio of the recycling ethanol flow rate and initial solvent volume in the extraction tank (RES) were identified as the critical process parameters (CPPs) via quantitative risk assessment. Box-Behnken design experiments were performed. Quadratic models between CPPs and process CQAs were developed, with determination coefficients higher than 0.88. As the ethanol concentration decreases, saponin yields first increase and then decrease. A longer extraction time leads to higher yields of the ginsenosides Rb1 and Rd. The total saponin purity increases as the ethanol concentration increases. The pigment yield increases as the ethanol concentration decreases or extraction time increases. The design space was calculated using a Monte-Carlo simulation method with an acceptable probability of 0.90. Normal operation ranges to attain process CQA criteria with a probability of more than 0.914 are recommended as follows: ethanol content of 79–82%, extraction time of 6.1–7.1 h, and RES of 0.039–0.040 min−1. Most of the results of the verification experiments agreed well with the predictions. The verification experiment results showed that the selection of proper operating ethanol content, extraction time, and RES within the design space can ensure that the CQA criteria are met. PMID:25470598

Sample preparation and detection device for infectious agents

DOEpatents

Miles, Robin R.; Wang, Amy W.; Fuller, Christopher K.; Lemoff, Asuncion V.; Bettencourt, Kerry A.; Yu, June

2003-06-10

A sample preparation and analysis device which incorporates both immunoassays and PCR assays in one compact, field-portable microchip. The device provides new capabilities in fluid and particle control which allows the building of a fluidic chip with no moving parts, thus decreasing fabrication cost and increasing the robustness of the device. The device can operate in a true continuous (not batch) mode. The device incorporates magnetohydrodynamic (MHD) pumps to move the fluid through the system, acoustic mixing and fractionation, dielectropheretic (DEP) sample concentration and purification, and on-chip optical detection capabilities.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 Tankmore » 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 D Cs 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 D Cs 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.« less

Transfer of a three step mAb chromatography process from batch to continuous: Optimizing productivity to minimize consumable requirements.

PubMed

Gjoka, Xhorxhi; Gantier, Rene; Schofield, Mark

2017-01-20

The goal of this study was to adapt a batch mAb purification chromatography platform for continuous operation. The experiments and rationale used to convert from batch to continuous operation are described. Experimental data was used to design chromatography methods for continuous operation that would exceed the threshold for critical quality attributes and minimize the consumables required as compared to batch mode of operation. Four unit operations comprising of Protein A capture, viral inactivation, flow-through anion exchange (AEX), and mixed-mode cation exchange chromatography (MMCEX) were integrated across two Cadence BioSMB PD multi-column chromatography systems in order to process a 25L volume of harvested cell culture fluid (HCCF) in less than 12h. Transfer from batch to continuous resulted in an increase in productivity of the Protein A step from 13 to 50g/L/h and of the MMCEX step from 10 to 60g/L/h with no impact on the purification process performance in term of contaminant removal (4.5 log reduction of host cell proteins, 50% reduction in soluble product aggregates) and overall chromatography process yield of recovery (75%). The increase in productivity, combined with continuous operation, reduced the resin volume required for Protein A and MMCEX chromatography by more than 95% compared to batch. The volume of AEX membrane required for flow through operation was reduced by 74%. Moreover, the continuous process required 44% less buffer than an equivalent batch process. This significant reduction in consumables enables cost-effective, disposable, single-use manufacturing. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Effect of natural antioxidants in Spanish salchichón elaborated with encapsulated n-3 long chain fatty acids in konjac glucomannan matrix.

PubMed

Munekata, P E S; Domínguez, R; Franco, D; Bermúdez, R; Trindade, M A; Lorenzo, Jose M

2017-02-01

The effect of natural antioxidants on physicochemical properties, lipid and protein oxidation, volatile compounds and free fatty acids (FFA) were determined in Spanish salchichón enriched with n-3 fatty acids encapsulated and stabilized in konjac matrix. Phenolic compounds of beer residue extract (BRE), chestnut leaves extract (CLE) and peanut skin extract (PSE) were also identified and quantified. Five batches of salchichón were prepared: control (CON, without antioxidants), butylated hydroxytoluene (BHT), BRE, CLE and PSE. The main phenolic compounds were catechin and benzoic acid for BRE, gallic acid and catechin for CLE and catechin and protocatechuic acid for PSE. Statistical analysis did not show significant differences on chemical composition among treatments. Reductions in luminosity (P<0.05) and pH (P<0.001) were observed with the CLE batch, whereas the other colour parameters were not affected by the addition of natural antioxidants. Finally, the inclusion of antioxidants (P<0.001) decreased the hexanal content, whereas the FFA content increased by the addition of natural extracts. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microbial production of mannitol by Lactobacillus brevis 3-A5 from concentrated extract of Jerusalem artichoke tubers.

PubMed

Cao, Hailong; Yue, Min; Liu, Gang; Du, Yuguang; Yin, Heng

2018-05-01

In the present study, the conversion of the extract of Jerusalem artichoke tubers for mannitol production by Lactobacillus brevis 3-A5 was investigated. When the bacterium utilized enzymatic hydrolysates of Jerusalem artichoke extract as the main substrates in batch fermentation, the significant decrease in mannitol productivity was observed when the initial concentration of reducing sugar increased. Then, a strategy of continuous fed-batch fermentation was adopted for improving mannitol production with enzymatic hydrolysates of Jerusalem artichoke extract as main substrates. Although the concentration of mannitol could reach 199.86 g/L at the end of the fermentation, the productivity for the overall process of the fermentation was only 1.67 g/L/H. To improve the mannitol productivity with both higher yield and concentration, the simultaneous enzymatic saccharification and fermentation (SSF) was studied. In SSF, the mannitol production reached 176.50 g/L in 28 H with a productivity of 6.30 g/L/H and a yield of 0.68 g/g total sugar. Our study provides a cost-effective and eco-friendly method for mannitol production from a cheap biomass. © 2017 International Union of Biochemistry and Molecular Biology, Inc.

Manganese uptake of imprinted polymers

DOE Data Explorer

Susanna Ventura

2015-09-30

Batch tests of manganese imprinted polymers of variable composition to assess their ability to extract lithium and manganese from synthetic brines at T=45C . Data on manganese uptake for two consecutive cycles are included.

Application of continuous substrate feeding to the ABE fermentation: Relief of product inhibition using extraction, perstraction, stripping, and pervaporation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qureshi, N.; Maddox, I.S.; Friedl, A.

1992-09-01

The technique of continuous substrate feeding has been applied to the batch fermentation process using freely suspended cells, for ABE (acetone-butanol-ethanol) production. To avoid the product inhibition which normally restricts ABE production to less than 20 g/L and sugar utilization to 60 g/L, a product removal technique has been integrated into the fermentation process. The techniques investigated were liquid-liquid extraction, perstraction, gas-stripping, and pervaporation. By using a substrate of whey permeate, the reactor productivity has been improved over that observed in a traditional batch fermentation, while equivalent lactose utilization and ABE production values of 180 g and 69 g, respectively,more » have been achieved in a 1-L culture volume. 17 refs., 14 figs., 5 tabs.« less

Characterization of solids deposited on the modular caustic-side solvent extraction unit (MCU) coalescer media removed in May and October 2014

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.

During routine maintenance, the coalescers utilized in the Modular Caustic-Side Solvent Extraction Unit (MCU) processing of Salt Batch 6 and a portion of Salt Batch 7 were sampled and submitted to the Savannah River National Laboratory (SRNL) for characterization, for the purpose of identifying solid phase constituents that may be accumulating in these coalescers. Specifically, two samples were received and characterized: A decontaminated salt solution (DSS) coalescer sample and a strip effluent (SE) coalescer sample. Aliquots of the samples were analyzed by XRD, Fourier Transform Infrared (FTIR) Spectroscopy, SEM, and EDS. Other aliquots of the samples were leached in acidmore » solution, and the leachates were analyzed by ICP-AES. In addition, modeling was performed to provide a basis for comparison of the analytical results.« less

Application of Taguchi optimisation of electro metal - electro winning (EMEW) for nickel metal from laterite

NASA Astrophysics Data System (ADS)

Sudibyo, Hermida, L.; Junaedi, A.; Putra, F. A.

2017-11-01

Nickel and cobalt metal able to process from low grade laterite using solvent extraction and electrowinning. One of electrowinning methods which has good performance to produce pure metal is electrometal-electrowinninge(EMEW). In this work, solventextraction was used to separate nickel and cobalt which useCyanex-Versatic Acid in toluene as an organic phase. An aqueous phase of extraction was processed using EMEW in order to deposit the nickel metal in Cathode electrode. The parameters which used in this work were batch temperature, operation time, voltage, and boric acid concentration. Those parameters were studied and optimized using the design of experiment of Taguchi. The Taguchi analysis result shows that the optimum result of EMEW was at 60°C of batch temperature, 2 Voltage, 6 hours operation and 0.5 M of boric acid.

Extracting metalworking fluid aerosol samples in cassettes by provisional ASTM and NIOSH methods.

PubMed

Harper, Martin

2002-01-01

Recent provisional methods for the determination of metalworking fluid aerosol in workplace air involve a solvent extraction procedure to separate the nonvolatile fraction of the fluid from insoluble material such as metal turnings and dirt. The procedure calls for preweighing a filter (W1) and assembling it into a cassette and taking a sample. In the laboratory the filter is removed from the cassette, desiccated to remove any collected water or other volatile substances, and weighed again (W2). The filter is then extracted in an organic solvent blend, allowed to dry, and weighed a final time (W3). The total weight collected by the filter is given by (W2-W1), and the weight of (nonvolatile) metalworking fluid collected is given by (W2-W3). The extraction step can take place within a cassette housing if it is relatively inert to the solvent blend used. The extraction of four metalworking fluids (straight oil, soluble oil, synthetic and semisynthetic) within disposable polypropylene cassettes was investigated using the same protocol used to evaluate the original method. For all fluids the extraction efficiency was greater than 95% with a precision better than 5%. The mean blank contribution to the extraction step was 16 micrograms. Blanks were also evaluated after storage, and after transport and storage. A small additional blank contribution could be removed by desiccation. The limits of detection and quantitation of the extraction step were calculated to be 28 and 94 micrograms, respectively.

The use of high pressure CO2 -facilitated pH swings to enhance in situ product recovery of butyric acid in a two-phase partitioning bioreactor.

PubMed

Peterson, Eric C; Daugulis, Andrew J

2014-11-01

Through the use of high partial pressures of CO2 (pCO2 ) to facilitate temporary pH reductions in two-phase partitioning bioreactors (TPPBs), improved pH dependent partitioning of butyric acid was observed which achieved in situ product recovery (ISPR), alleviating end-product inhibition (EPI) during the production of butyric acid by Clostridium tyrobutyricum (ATCC 25755). Through high pressure pCO2 studies, media buffering effects were shown to be substantially overcome at 60 bar pCO2 , resulting in effective extraction of the organic acid by the absorptive polymer Pebax® 2533, yielding a distribution coefficient (D) of 2.4 ± 0.1 after 1 h of contact at this pressure. Importantly, it was also found that C. tyrobutyricum cultures were able to withstand 60 bar pCO2 for 1 h with no decrease in growth ability when returned to atmospheric pressure in batch reactors after several extraction cycles. A fed-batch reactor with cyclic high pCO2 polymer extraction recovered 92 g of butyric acid to produce a total of 213 g compared to 121 g generated in a control reactor. This recovery reduced EPI in the TPPB, resulting in both higher productivity (0.65 vs. 0.33 g L(-1)  h(-1) ) and yield (0.54 vs. 0.40). Fortuitously, it was also found that repeated high pCO2 -facilitated polymer extractions of butyric acid during batch growth of C. tyrobutyricum lessened the need for pH control, and reduced base requirements by approximately 50%. Thus, high pCO2 -mediated absorptive polymer extraction presents a novel method for improving process performance in butyric acid fermentation, and this technique could be applied to the bioproduction of other organic acids as well. © 2014 Wiley Periodicals, Inc.

Discovery of Newer Therapeutic Leads for Prostate Cancer

DTIC Science & Technology

2009-06-01

promising plant extracts and then prepare large-scale quantities of the plant extracts using supercritical fluid extraction techniques and use this...quantities of the plant extracts using supercritical fluid extraction techniques. Large scale plant collections were conducted for 14 of the top 20...material for bioassay-guided fractionation of the biologically active constituents using modern chromatography techniques. The chemical structures of

Investigation of extractable organic compounds in deep-sea hydrothermal vent fluids along the Mid-Atlantic Ridge

NASA Astrophysics Data System (ADS)

McCollom, Thomas M.; Seewald, Jeffrey S.; German, Christopher R.

2015-05-01

The possibility that deep-sea hydrothermal vents may contain organic compounds produced by abiotic synthesis or by microbial communities living deep beneath the surface has led to numerous studies of the organic composition of vent fluids. Most of these studies have focused on methane and other light hydrocarbons, while the possible occurrence of more complex organic compounds in the fluids has remained largely unstudied. To address this issue, the presence of higher molecular weight organic compounds in deep-sea hydrothermal fluids was assessed at three sites along the Mid-Atlantic Ridge that span a range of temperatures (51 to >360 °C), fluid compositions, and host-rock lithologies (mafic to ultramafic). Samples were obtained at several sites within the Lucky Strike, Rainbow, and Lost City hydrothermal fields. Three methods were employed to extract organic compounds for analysis, including liquid:liquid extraction, cold trapping on the walls of a coil of titanium tubing, and pumping fluids through cartridges filled with solid phase extraction (SPE) sorbents. The only samples to consistently yield high amounts of extractable organic compounds were the warm (51-91 °C), highly alkaline fluids from Lost City, which contained elevated concentrations of C8, C10, and C12n-alkanoic acids and, in some cases, trithiolane, hexadecanol, squalene, and cholesterol. Collectively, the C8-C12 acids can account for about 15% of the total dissolved organic carbon in the Lost City fluids. The even-carbon-number predominance of the alkanoic acids indicates a biological origin, but it is unclear whether these compounds are derived from microbial activity occurring within the hydrothermal chimney proximal to the site of fluid discharge or are transported from deeper within the system. Hydrothermal fluids from the Lucky Strike and Rainbow fields were characterized by an overall scarcity of extractable dissolved organic compounds. Trace amounts of aromatic hydrocarbons including phenanthrenes and benzothiophene were the only compounds that could be identified as indigenous components of these fluids. Although hydrocarbons and fatty acids were observed in some samples, those compounds were likely derived from particulate matter or biomass entrained during fluid collection. In addition, extracts of some fluid samples from the Rainbow field were found to contain an unresolved complex mixture (UCM) of organic compounds. This UCM shared some characteristics with organic matter extracted from bottom seawater, suggesting that the organic matter observed in these samples might represent seawater-derived compounds that had persisted, albeit with partial alteration, during circulation through the hydrothermal system. While there is considerable evidence that Rainbow and Lost City vent fluids contain methane and other light hydrocarbons produced through abiotic reduction of inorganic carbon, we found no evidence for more complex organic compounds with an abiotic origin in the same fluids.

Results of initial analyses of the salt (macro) batch 10 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

2017-01-01

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Interim Salt Disposition Project (ISDP) Salt (Macro) Batch 10 for processing through the Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU). This document reports the initial results of the analyses of samples of Tank 21H. Analysis of the Tank 21H Salt (Macro) Batch 10 composite sample indicates that the material does not display any unusual characteristics or observations, such as floating solids, the presence of large amount of solids, or unusual colors. Further sample results will be reported in a futuremore » document. This memo satisfies part of Deliverable 3 of the Technical Task Request (TTR).« less

Results of initial analyses of the salt (macro) batch 11 Tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Interim Salt Disposition Project (ISDP) Salt (Macro) Batch 11 for processing through the Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU). This document reports the initial results of the analyses of samples of Tank 21H. Analysis of the Tank 21H Salt (Macro) Batch 11 composite sample indicates that the material does not display any unusual characteristics or observations, such as floating solids, the presence of large amounts of solids, or unusual colors. Further sample results will be reported in a futuremore » document. This memo satisfies part of Deliverable 3 of the Technical Task Request (TTR).« less

Determination of As concentration in earthworm coelomic fluid extracts by total-reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Allegretta, Ignazio; Porfido, Carlo; Panzarino, Onofrio; Fontanella, Maria Chiara; Beone, Gian Maria; Spagnuolo, Matteo; Terzano, Roberto

2017-04-01

Earthworms are often used as sentinel organisms to study As bioavailability in polluted soils. Arsenic in earthworms is mainly sequestrated in the coelomic fluids whose As content can therefore be used to asses As bioavalability. In this work, a method for determining As concentration in coelomic fluid extracts using total-reflection X-ray fluorescence spectrometry (TXRF) is presented. For this purpose coelomic fluid extracts from earthworms living in three polluted soils and one non-polluted (control) soil have been collected and analysed. A very simple sample preparation was implemented, consisting of a dilution of the extracts with polyvinyl alcohol (PVA) using a 1:8 ratio and dropwise deposition of the sample on the reflector. A detection limit of 0.2 μg/l and quantification limit of 0.6 μg/l was obtained in the diluted samples, corresponding to 2 μg/l and 6 μg/l in the coelomic fluid extracts, respectively. This allowed to quantify As concentration in coelomic fluids extracted from earthworms living in soils polluted with As at concentrations higher than 20 mg/kg (considered as a pollution threshold for agricultural soils). The TXRF method has been validated by comparison with As concentrations in standards and by analysing the same samples by ICP-MS, after acid digestion of the sample. The low limit of detection, the proven reliability of the method and the little sample preparation make TXRF a suitable, cost-efficient and "green" technique for the analysis of As in earthworm coelomic fluid extracts for bioavailability studies.

Investigation of effect of particle size and rumen fluid addition on specific methane yields of high lignocellulose grass silage.

PubMed

Wall, D M; Straccialini, B; Allen, E; Nolan, P; Herrmann, C; O'Kiely, P; Murphy, J D

2015-09-01

This work examines the digestion of advanced growth stage grass silage. Two variables were investigated: particle size (greater than 3 cm and less than 1cm) and rumen fluid addition. Batch studies indicated particle size and rumen fluid addition had little effect on specific methane yields (SMYs). In continuous digestion of 3 cm silage the SMY was 342 and 343 L CH4 kg(-1)VS, respectively, with and without rumen fluid addition. However, digester operation was significantly affected through silage floating on the liquor surface and its entanglement in the mixing system. Digestion of 1cm silage with no rumen fluid addition struggled; volatile fatty acid concentrations rose and SMYs dropped. The best case was 1cm silage with rumen fluid addition, offering higher SMYs of 371 L CH4 kg(-1)VS and stable operation throughout. Thus, physical and biological treatments benefited continuous digestion of high fibre grass silage. Copyright © 2015 Elsevier Ltd. All rights reserved.

Supercritical Fluid Extraction of Aflatoxin B 1 from Soil

EPA Science Inventory

This research describes the development of a Supercritical Fluid Extraction (SFE) method to recover aflatoxin B1 from fortified soil. The effects of temperature, pressure, modifier (identity and percentage), and extraction type were assessed. Using the optimized SFE conditions, ...

ENGINEERING BULLETIN: IN SITU SOIL FLUSHING

EPA Science Inventory

In situ soil flushing is the extraction of contaminants from the soil with water or other suitable aqueous solutions. Soil flushing is accomplished by passing the extraction fluid through in-place soils using an injection or infiltration process. Extraction fluids must be recover...

Continuous production of ethanol with Zymomonas mobilis growing on Jerusalem artichoke juice

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allais, J.J.; Torres, E.F.; Baratti, J.

1987-04-01

Recent work from the authors laboratory has shown that, compared to yeasts, much higher ethanol productivity and yield can be obtained in batch or continuous cultures using the bacterium Zymomonas mobilis grown on fructose media. In batch culture, hydrolyzed Jerusalem artichoke juice with sugar concentrations ranging from 100 to 250 g/L can be converted efficiently to ethanol. The present work describes the conversion of the hydrolyzed juice to ethanol in continuous culture. The extraction and enzymatic hydrolysis of inulin from the tubers of Jerusalem artichoke is also reported.

Steel slag carbonation in a flow-through reactor system: the role of fluid-flux.

PubMed

Berryman, Eleanor J; Williams-Jones, Anthony E; Migdisov, Artashes A

2015-01-01

Steel production is currently the largest industrial source of atmospheric CO2. As annual steel production continues to grow, the need for effective methods of reducing its carbon footprint increases correspondingly. The carbonation of the calcium-bearing phases in steel slag generated during basic oxygen furnace (BOF) steel production, in particular its major constituent, larnite {Ca2SiO4}, which is a structural analogue of olivine {(MgFe)2SiO4}, the main mineral subjected to natural carbonation in peridotites, offers the potential to offset some of these emissions. However, the controls on the nature and efficiency of steel slag carbonation are yet to be completely understood. Experiments were conducted exposing steel slag grains to a CO2-H2O mixture in both batch and flow-through reactors to investigate the impact of temperature, fluid flux, and reaction gradient on the dissolution and carbonation of steel slag. The results of these experiments show that dissolution and carbonation of BOF steel slag are more efficient in a flow-through reactor than in the batch reactors used in most previous studies. Moreover, they show that fluid flux needs to be optimized in addition to grain size, pressure, and temperature, in order to maximize the efficiency of carbonation. Based on these results, a two-stage reactor consisting of a high and a low fluid-flux chamber is proposed for CO2 sequestration by steel slag carbonation, allowing dissolution of the slag and precipitation of calcium carbonate to occur within a single flow-through system. Copyright © 2014. Published by Elsevier B.V.

Determination of the bioaccessible fraction of metals in urban aerosol using simulated lung fluids

NASA Astrophysics Data System (ADS)

Coufalík, Pavel; Mikuška, Pavel; Matoušek, Tomáš; Večeřa, Zbyněk

2016-09-01

Determination of the bioaccessible fraction of metals in atmospheric aerosol is a significant issue with respect to air pollution in the urban environment. The aim of this work was to compare of metal bioaccessibility determined according to the extraction yields of six simulated lung fluids. Aerosol samples of the PM1 fraction were collected in Brno, Czech Republic. The total contents of Cd, Ce, Cr, Cu, Fe, Mn, Ni, Pb, V, and Zn in the samples were determined and their enrichment factors were calculated. The bioaccessible proportions of elements were determined by means of extraction in Gamble's solution, Gamble's solution with dipalmitoyl phosphatidyl choline (DPPC), artificial lysosomal fluid, saline, water, and in a newly proposed solution based on DPPC, referred to as "Simulated Alveoli Fluid" (SAF). The chemical composition and surface tension of the simulated lung fluids were the main parameters influencing extraction yields. Gamble's solutions and the newly designed solution of SAF exhibited the lowest extraction efficiency, and also had the lowest surface tensions. The bioaccessibility of particulate metals should be assessed by synthetic lung fluids with a low surface tension, which simulate better the behavior and composition of native lung surfactant. The bioaccessibility of metals in aerosol assessed by means of the extraction in water or artificial lysosomal fluid can be overestimated.

Feasibility of ion-pair/supercritical fluid extraction of an ionic compound--pseudoephedrine hydrochloride.

PubMed

Eckard, P R; Taylor, L T

1997-02-01

The supercritical fluid extraction (SFE) of an ionic compound, pseudoephedrine hydrochloride, from a spiked-sand surface was successfully demonstrated. The effect of carbon dioxide density (CO2), supercritical fluid composition (pure vs. methanol modified), and the addition of a commonly used reversed-phase liquid chromatographic ion-pairing reagent, 1-heptanesulfonic acid, sodium salt, on extraction efficiency was examined. The extraction recoveries of pseudoephedrine hydrochloride with the addition of the ion-pairing reagent from a spiked-sand surface were shown to be statistically greater than the extraction recoveries without the ion-pairing reagent with both pure and methanol-modified carbon dioxide.

Visualization of Computational Fluid Dynamics

NASA Technical Reports Server (NTRS)

Gerald-Yamasaki, Michael; Hultquist, Jeff; Bryson, Steve; Kenwright, David; Lane, David; Walatka, Pamela; Clucas, Jean; Watson, Velvin; Lasinski, T. A. (Technical Monitor)

1995-01-01

Scientific visualization serves the dual purpose of exploration and exposition of the results of numerical simulations of fluid flow. Along with the basic visualization process which transforms source data into images, there are four additional components to a complete visualization system: Source Data Processing, User Interface and Control, Presentation, and Information Management. The requirements imposed by the desired mode of operation (i.e. real-time, interactive, or batch) and the source data have their effect on each of these visualization system components. The special requirements imposed by the wide variety and size of the source data provided by the numerical simulation of fluid flow presents an enormous challenge to the visualization system designer. We describe the visualization system components including specific visualization techniques and how the mode of operation and source data requirements effect the construction of computational fluid dynamics visualization systems.

Quantification of concentrated Chinese medicine granules by quantitative polymerase chain reaction.

PubMed

Lo, Yat-Tung; Shaw, Pang-Chui

2017-10-25

Determination of the amount of constituent in a multi-herb product is important for quality control. In concentrated Chinese medicine granules (CCMG), no dregs are left after dissolution of the CCMG. This study is the first to examine the feasibility of using quantitative polymerase chain reaction (qPCR) to find the amount of CCMG in solution form. DNA was extracted from Hirudo and Zaocys CCMG mixed at different ratios and amplified in qPCR using species-specific primers. The threshold cycle (C T ) obtained was compared with the respective standard curves. Results showed that reproducible quantification results could be obtained (1) for 5-50mg CCMG using a modified DNA extraction protocol, (2) amongst DNA extracted from the same batch of CCMG and (3) amongst different batches of CCMG from the same company. This study demonstrated the constitute amount of CCMG in a mixture could be determined using qPCR. This work has extended the application of DNA techniques for the quantification of herbal products and this approach may be developed for quality assurance in the CCMG industry. Copyright © 2017 Elsevier B.V. All rights reserved.

[Study on quality standard of Sophora flavescens root extract].

PubMed

Zhao, Feng-chun; Li, Hao; Chen, Liang-mian; Gao, Hui-min; Zhang, Qi-wei; Wang, Zhi-min; Wu, Pi-e

2015-01-01

As a part of the project for the Chinese Pharmacopoeia (2015 edition), the quality standard of Sophora flavescens root extract was investigated and established. According to the methods described in the Appendix of Chinese Pharmacopoeia (2010 edition), the water and ash inspections were carried out. The marker components trifolirhizin, sophoraflavanone G, oxymatrine and oxysophocarpine in the samples were identified by qualitative TLC. The determination of oxymatrine, matrine, oxysophocarpine and sophocarpine was conducted by HPLC and the total flavonoids were measured by ultraviolet spectrophotometry, using sophoraflavanone G as reference substance. The results indicated the spots on the plate were clear with good resolution and the contents of oxymatrine, matrine, oxysophocarpine and sophocarpine in the 13 batches of the samples were 3.87% - 11.1%, 0.970% - 4.33%, 1.30% - 2.59% and 0.260% - 1.14%, respectively. The total flavoids in the 13 batches of the samples were 3.88% - 7.93%. In the study, the validated methods were reproducible and the established quality standard was feasible, which could be used for the quality control of S. flavescens root extract and related preparations.

SUPERCRITICAL FLUID EXTRACTION OF POLYCYCLIC AROMATIC HYDROCARBON MIXTURES FROM CONTAMINATED SOILS

EPA Science Inventory

Highly contaminated (with PAHs) topsoils were extracted with supercritical CO₂ to determine the feasibility and mechanism of supercritical fluid extraction (SFE). Effect of SCF density, temperature, cosolvent type and amount, and of slurrying the soil with water were ...

Fuel ethanol production from Jerusalem artichoke stalks using different yeasts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Margaritis, A.; Bajpai, P.; Bajpai, P.K.

1983-01-01

The inulin-type sugars present in the stalks of Jerusalem artichoke (Helianthus tuberosus) were extracted with hot water and were used as a substrate to produce fuel EtOH. Seven different yeasts were used to obtain batch kinetic data. The medium consisted of stalk extract from Jerusalem artichoke containing 7.3% total sugars, supplemented with 0.01% oleic acid, 0.01% corn steep liquor, and 0.05% Tween 80. All batch fermentations were carried out in a 1-L bioreactor at 35 degrees and pH 4.6, and the following parameters were measured as a function of time: total sugars, EtOH and biomass concentration, maximum specific growth rate,more » and biomass and EtOH yields. The best EtOH producer was Kluyveromyces marxianus UCD (FST) 55-82 which gave an EtOH-to-sugar yield 97% of the theoretical maximum value, with almost 100% sugar utilization.« less

In-situ transesterification of seeds of invasive Chinese tallow trees (Triadica sebifera L.) in a microwave batch system (GREEN(3)) using hexane as co-solvent: Biodiesel production and process optimization.

PubMed

Barekati-Goudarzi, Mohamad; Boldor, Dorin; Nde, Divine B

2016-02-01

In-situ transesterification (simultaneous extraction and transesterification) of Chinese tallow tree seeds into methyl esters using a batch microwave system was investigated in this study. A high degree of oil extraction and efficient conversion of oil to biodiesel were found in the proposed range. The process was further optimized in terms of product yields and conversion rates using Doehlert optimization methodology. Based on the experimental results and statistical analysis, the optimal production yield conditions for this process were determined as: catalyst concentration of 1.74wt.%, solvent ratio about 3 (v/w), reaction time of 20min and temperature of 58.1°C. H(+)NMR was used to calculate reaction conversion. All methyl esters produced using this method met ASTM biodiesel quality specifications. Copyright © 2015 Elsevier Ltd. All rights reserved.

Field Testing of Rapid Electrokinetic Nanoparticle Treatment for Corrosion Control of Steel in Concrete

NASA Technical Reports Server (NTRS)

Cardenas, Henry E.; Alexander, Joshua B.; Kupwade-Patil,Kunal; Calle, Luz Marina

2009-01-01

This work field tested the use of electrokinetics for delivery of concrete sealing nanoparticles concurrent with the extraction of chlorides. Several cylinders of concrete were batched and placed in immersion at the Kennedy Space Center Beach Corrosion Test Site. The specimens were batched with steel reinforcement and a 4.5 wt.% (weight percent) content of sodium chloride. Upon arrival at Kennedy Space Center, the specimens were placed in the saltwater immersion pool at the Beach Corrosion Test Site. Following 30 days of saltwater exposure, the specimens were subjected to rapid chloride extraction concurrent with electrokinetic nanoparticle treatment. The treatments were operated at up to eight times the typical current density in order to complete the treatment in 7 days. The findings indicated that the short-term corrosion resistance of the concrete specimens was significantly enhanced as was the strength of the concrete.

Dextran Utilization During Its Synthesis by Weissella cibaria RBA12 Can Be Overcome by Fed-Batch Fermentation in a Bioreactor.

PubMed

Baruah, Rwivoo; Deka, Barsha; Kashyap, Niharika; Goyal, Arun

2018-01-01

Weissella cibaria RBA12 produced a maximum of 9 mg/ml dextran (with 90% efficiency) using shake flask culture under the optimized concentration of medium components viz. 2% (w/v) of each sucrose, yeast extract, and K 2 HPO 4 after incubation at optimized conditions of 20 °C and 180 rpm for 24 h. The optimized medium and conditions were used for scale-up of dextran production from Weissella cibaria RBA12 in 2.5-l working volume under batch fermentation in a bioreactor that yielded a maximum of 9.3 mg/ml dextran (with 93% efficiency) at 14 h. After 14 h, dextran produced was utilized by the bacterium till 18 h in its stationary phase under sucrose depleted conditions. Dextran utilization was further studied by fed-batch fermentation using sucrose feed. Dextran on production under fed-batch fermentation in bioreactor gave 35.8 mg/ml after 32 h. In fed-batch mode, there was no decrease in dextran concentration as observed in the batch mode. This showed that the utilization of dextran by Weissella cibaria RBA12 is initiated when there is sucrose depletion and therefore the presence of sucrose can possibly overcome the dextran hydrolysis. This is the first report of utilization of dextran, post-sucrose depletion by Weissella sp. studied in bioreactor.

Kinetic characterization and fed-batch fermentation for maximal simultaneous production of esterase and protease from Lysinibacillus fusiformis AU01.

PubMed

Divakar, K; Suryia Prabha, M; Nandhinidevi, G; Gautam, P

2017-04-21

The simultaneous production of intracellular esterase and extracellular protease from the strain Lysinibacillus fusiformis AU01 was studied in detail. The production was performed both under batch and fed-batch modes. The maximum yield of intracellular esterase and protease was obtained under full oxygen saturation at the beginning of the fermentation. The data were fitted to the Luedeking-Piret model and it was shown that the enzyme (both esterase and protease) production was growth associated. A decrease in intracellular esterase and increase in the extracellular esterase were observed during late stationary phase. The appearance of intracellular proteins in extracellular media and decrease in viable cell count and biomass during late stationary phase confirmed that the presence of extracellular esterase is due to cell lysis. Even though the fed-batch fermentation with different feeding strategies showed improved productivity, feeding yeast extract under DO-stat fermentation conditions showed highest intracellular esterase and protease production. Under DO-stat fed-batch cultivation, maximum intracellular esterase activity of 820 × 10 3 U/L and extracellular protease activity of 172 × 10 3 U/L were obtained at the 16th hr. Intracellular esterase and extracellular protease production were increased fivefold and fourfold, respectively, when compared to batch fermentation performed under shake flask conditions.

Fluid extraction

DOEpatents

Wai, Chien M.; Laintz, Kenneth E.

1999-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated .beta.-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated .beta.-diketone and a trialkyl phosphate, or a fluorinated .beta.-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated .beta.-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

The extraction of liquid, protein molecules and yeast cells from paper through surface acoustic wave atomization.

PubMed

Qi, Aisha; Yeo, Leslie; Friend, James; Ho, Jenny

2010-02-21

Paper has been proposed as an inexpensive and versatile carrier for microfluidics devices with abilities well beyond simple capillary action for pregnancy tests and the like. Unlike standard microfluidics devices, extracting a fluid from the paper is a challenge and a drawback to its broader use. Here, we extract fluid from narrow paper strips using surface acoustic wave (SAW) irradiation that subsequently atomizes the extracted fluid into a monodisperse aerosol for use in mass spectroscopy, medical diagnostics, and drug delivery applications. Two protein molecules, ovalbumin and bovine serum albumin (BSA), have been preserved in paper and then extracted using atomized mist through SAW excitation; protein electrophoresis shows there is less than 1% degradation of either protein molecule in this process. Finally, a solution of live yeast cells was infused into paper, which was subsequently dried for preservation then remoistened to extract the cells via SAW atomization, yielding live cells at the completion of the process. The successful preservation and extraction of fluids, proteins and yeast cells significantly expands the usefulness of paper in microfluidics.

Applications of supercritical fluid extraction (SFE) of palm oil and oil from natural sources.

PubMed

Akanda, Mohammed Jahurul Haque; Sarker, Mohammed Zaidul Islam; Ferdosh, Sahena; Manap, Mohd Yazid Abdul; Ab Rahman, Nik Norulaini Nik; Ab Kadir, Mohd Omar

2012-02-10

Supercritical fluid extraction (SFE), which has received much interest in its use and further development for industrial applications, is a method that offers some advantages over conventional methods, especially for the palm oil industry. SC-CO₂ refers to supercritical fluid extraction (SFE) that uses carbon dioxide (CO₂) as a solvent which is a nontoxic, inexpensive, nonflammable, and nonpolluting supercritical fluid solvent for the extraction of natural products. Almost 100% oil can be extracted and it is regarded as safe, with organic solvent-free extracts having superior organoleptic profiles. The palm oil industry is one of the major industries in Malaysia that provides a major contribution to the national income. Malaysia is the second largest palm oil and palm kernel oil producer in the World. This paper reviews advances in applications of supercritical carbon dioxide (SC-CO₂) extraction of oils from natural sources, in particular palm oil, minor constituents in palm oil, producing fractionated, refined, bleached, and deodorized palm oil, palm kernel oil and purified fatty acid fractions commendable for downstream uses as in toiletries and confectionaries.

Novel combined stir bar sorptive extraction coupled with ultrasonic assisted extraction for the determination of brominated flame retardants in environmental samples using high performance liquid chromatography.

PubMed

Yu, Chunhe; Hu, Bin

2007-08-10

A combined stir bar coated with poly (dimethysiloxane)-beta-cyclodextrin (PDMS-beta-CD) on single side has been prepared for the first time by sol-gel method and was coupled with ultrasonic assisted extraction (UAE) for the determination of some brominated flame-retardant compounds (BFRs) in soil and dust samples by high performance liquid chromatography (HPLC). Four different kinds of coatings including PDMS-beta-CD, PDMS, carbowax (CW)-PDMS-poly (vinyl alcohol) (PVA) and PDMS-PVA were evaluated for stir bar sorptive extraction of BFRs by orthogonal experiment design. The experimental results reveal that the PDMS-beta-CD combined stir bar exhibited the best extraction efficiency for the target analytes. The reproducibility for the preparation of PDMS-beta-CD combined stir bar ranged from 1.3% to 15.7% in one batch, and 7.2% to 15.1% among batches. Extraction time, desorption solvent, concentration of methanol and NaCl in the matrix, pH, temperature and stirring speed were optimized. The combined stir bar can avoid direct friction of the coating with the bottom of the vessel, and could be used for more than 100 times. Linearity (>0.993), repeatability (<10.5%), reproducibility (<16.5%), recovery (56-118%) and detection limits (2.9-4.2 microg L(-1)) were proper to determine the seven BFRs. The developed method was applied to the determination of BFRs in soil and dust with satisfactory results.

[Physical fingerprint for quality control of traditional Chinese medicine extract powders].

PubMed

Zhang, Yi; Xu, Bing; Sun, Fei; Wang, Xin; Zhang, Na; Shi, Xin-Yuan; Qiao, Yan-Jiang

2016-06-01

The physical properties of both raw materials and excipients are closely correlated with the quality of traditional Chinese medicine preparations in oral solid dosage forms. In this paper, based on the concept of the chemical fingerprint for quality control of traditional Chinese medicine products, the method of physical fingerprint for quality evaluation of traditional Chinese medicine extract powders was proposed. This novel physical fingerprint was built by the radar map, and consisted of five primary indexes (i.e. stackablity, homogeneity, flowability, compressibility and stability) and 12 secondary indexes (i.e. bulk density, tap density, particle size<50 μm percentage, relative homogeneity index, hausner ratio, angle of repose, powder flow time, inter-particle porosity, Carr index, cohesion index, loss on drying, hygroscopicity). Panax notoginseng saponins (PNS) extract was taken for an example. This paper introduced the application of physical fingerprint in the evaluation of source-to-source and batch-to-batch quality consistence of PNS extract powders. Moreover, the physical fingerprint of PNS was built by calculating the index of parameters, the index of parametric profile and the index of good compressibility, in order to successfully predict the compressibility of the PNS extract powder and relevant formulations containing PNS extract powder and conventional pharmaceutical excipients. The results demonstrated that the proposed method could not only provide new insights into the development and process control of traditional Chinese medicine solid dosage forms. Copyright© by the Chinese Pharmaceutical Association.

Extractive Fermentation of Sugarcane Juice to Produce High Yield and Productivity of Bioethanol

NASA Astrophysics Data System (ADS)

Rofiqah, U.; Widjaja, T.; Altway, A.; Bramantyo, A.

2017-04-01

Ethanol production by batch fermentation requires a simple process and it is widely used. Batch fermentation produces ethanol with low yield and productivity due to the accumulation of ethanol in which poisons microorganisms in the fermenter. Extractive fermentation technique is applied to solve the microorganism inhibition problem by ethanol. Extractive fermentation technique can produce ethanol with high yield and productivity. In this process raffinate still, contains much sugar because conversion in the fermentation process is not perfect. Thus, to enhance ethanol yield and productivity, recycle system is applied by returning the raffinate from the extraction process to the fermentation process. This raffinate also contains ethanol which would inhibit the performance of microorganisms in producing ethanol during the fermentation process. Therefore, this study aims to find the optimum condition for the amount of solvent to broth ratio (S: B) and recycle to fresh feed ratio (R: F) which enter the fermenter to produce high yield and productivity. This research was carried out by experiment. In the experiment, sugarcane juice was fermented using Zymomonasmobilis mutant. The fermentation broth was extracted using amyl alcohol. The process was integrated with the recycle system by varying the recycle ratio. The highest yield and productivity is 22.3901% and 103.115 g / L.h respectively, obtained in a process that uses recycle to fresh feed ratio (R: F) of 50:50 and solvents to both ratio of 1.

Bioconversion of glycerol to 1,3-propanediol in thin stillage-based media by engineered Lactobacillus panis PM1.

PubMed

Kang, Tae Sun; Korber, Darren R; Tanaka, Takuji

2014-04-01

Thin stillage (TS) is a waste residue that remains after bioethanol production, and its disposal reflects the high costs of bioethanol production. Thus, the development of cost-effective ways to process TS is a pending issue in bioethanol plants. The aim of this study was to evaluate the utilization of TS for the production of the valuable chemical, 1,3-propanediol (1,3-PDO), by Lactobacillus panis PM1. Different fermentation parameters, including temperature, pH and strains [wild-type and a recombinant strain expressing a NADPH-dependent aldehyde reductase (YqhD) gene] were tested in batch and fed-batch cultivations. The highest 1,3-PDO concentration (12.85 g/L) and yield (0.84 g/g) were achieved by batch fermentation at pH-4.5/30 °C by the YqhD recombinant strain. Furthermore, pH-controlled batch fermentation reduced the total fermentation period, resulting in the maximal 1,3-PDO concentration of 16.23 g/L and yield of 0.72 g/g in TS without an expensive nutrient or nitrogen (e.g., yeast extract, beef extract, and peptone) supplementation. The addition of two trace elements, Mg(2+) and Mn(2+), in TS increased 1,3-PDO yield (0.74 g/g) without 3-hydroxypropionaldehyde production, the only intermediate of 1,3-PDO biosynthetic pathway in L. panis PM1. Our results suggest that L. panis PM1 can offer a cost-effective process that utilizes the TS to produce a value-added chemical, 1,3-PDO.

Theoretical models for supercritical fluid extraction.

PubMed

Huang, Zhen; Shi, Xiao-Han; Jiang, Wei-Juan

2012-08-10

For the proper design of supercritical fluid extraction processes, it is essential to have a sound knowledge of the mass transfer mechanism of the extraction process and the appropriate mathematical representation. In this paper, the advances and applications of kinetic models for describing supercritical fluid extraction from various solid matrices have been presented. The theoretical models overviewed here include the hot ball diffusion, broken and intact cell, shrinking core and some relatively simple models. Mathematical representations of these models have been in detail interpreted as well as their assumptions, parameter identifications and application examples. Extraction process of the analyte solute from the solid matrix by means of supercritical fluid includes the dissolution of the analyte from the solid, the analyte diffusion in the matrix and its transport to the bulk supercritical fluid. Mechanisms involved in a mass transfer model are discussed in terms of external mass transfer resistance, internal mass transfer resistance, solute-solid interactions and axial dispersion. The correlations of the external mass transfer coefficient and axial dispersion coefficient with certain dimensionless numbers are also discussed. Among these models, the broken and intact cell model seems to be the most relevant mathematical model as it is able to provide realistic description of the plant material structure for better understanding the mass-transfer kinetics and thus it has been widely employed for modeling supercritical fluid extraction of natural matters. Copyright © 2012 Elsevier B.V. All rights reserved.

Evaluation of the essential oil of Foeniculum vulgare Mill (fennel) fruits extracted by three different extraction methods by GC/MS.

PubMed

Hammouda, Faiza M; Saleh, Mahmoud A; Abdel-Azim, Nahla S; Shams, Khaled A; Ismail, Shams I; Shahat, Abdelaaty A; Saleh, Ibrahim A

2014-01-01

Hydrodistillation (HD) and steam-distillation, or solvent extraction methods of essential oils have some disadvantages like thermal decomposition of extracts, its contamination with solvent or solvent residues and the pollution of residual vegetal material with solvent which can be also an environmental problem. Thus, new green techniques, such as supercritical fluid extraction and microwave assisted techniques, are potential solutions to overcome these disadvantages. The aim of this study was to evaluate the essential oil of Foeniculum vulgare subsp. Piperitum fruits extracted by three different extraction methods viz. Supercritical fluid extraction (SFE) using CO2, microwave-assisted extraction (MAE) and hydro-distillation (HD) using gas chromatography-mass spectrometry (GC/MS). The results revealed that both MAE and SFE enhanced the extraction efficiency of the interested components. MAE gave the highest yield of oil as well as higher percentage of Fenchone (28%), whereas SFE gave the highest percentage of anethol (72%). Microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) not only enhanced the essential oil extraction but also saved time, reduced the solvents use and produced, ecologically, green technologies.

Influence of extraction technique on the anti-oxidative potential of hawthorn (Crataegus monogyna) extracts in bovine muscle homogenates.

PubMed

Shortle, E; O'Grady, M N; Gilroy, D; Furey, A; Quinn, N; Kerry, J P

2014-12-01

Six extracts were prepared from hawthorn (Crataegus monogyna) leaves and flowers (HLF) and berries (HB) using solid-liquid [traditional (T) (HLFT, HBT), sonicated (S) (HLFS, HBS)] and supercritical fluid (C) extraction (HLFC, HBC) techniques. The antioxidant activities of HLF and HB extracts were characterised using in vitro antioxidant assays (TPC, DPPH, FRAP) and in 25% bovine muscle (longissimus lumborum) homogenates (lipid oxidation (TBARS), oxymyoglobin (% of total myoglobin)) after 24h storage at 4°C. Hawthorn extracts exhibited varying degrees of antioxidant potency. In vitro and muscle homogenate (TBARS) antioxidant activity followed the order: HLFS>HLFT and HBT>HBS. In supercritical fluid extracts, HLFC>HBC (in vitro antioxidant activity) and HLFC≈HBC (TBARS). All extracts (except HBS) reduced oxymyoglobin oxidation. The HLFS extract had the highest antioxidant activity in all test systems. Supercritical fluid extraction (SFE) exhibited potential as a technique for the manufacture of functional ingredients (antioxidants) from hawthorn for use in muscle foods. Copyright © 2014 Elsevier Ltd. All rights reserved.

Comparison study of moisture content, colour properties and essential oil compounds extracted by hydrodistillation and supercritical fluid extraction between stem and leaves of lemongrass (Cymbopogun citratus)

NASA Astrophysics Data System (ADS)

Kamaruddin, Shazlin; Mustapha, Wan Aida Wan; Haiyee, Zaibunnisa Abdul

2018-04-01

The objectives of this study were to compare the properties of moisture content, colour and essential oil compounds between stem and leaves of lemongrass (Cymbopogun citratus). The essential oil was extracted using two different methods which are hydrodistillation and supercritical fluid extraction (SFE). There was no significant difference of moisture content between stem and leaves of lemongrass. The lightness (L) and yellowness (+b) values of the stems were significantly higher (p<0.05) compared to the leaves. The highest yield of essential oil was obtained by extraction using supercritical fluid extraction (SFE) in leaves (˜ 0.7%) by treatment at 1700psi and 50°C. The main compound of extracted essential oil was citral (geranial and neral).

Montmorillonite Dissolution in Simulated Lung Fluids

NASA Astrophysics Data System (ADS)

Schmidt, M.; Wendlandt, R. F.

2008-12-01

Because lung fluids" first interaction is with the surface of inhaled grains, the surface properties of inhaled mineral dusts may have a generally mitigating effect on cytotoxicity and carcinogenicity. Wendlandt et al. (Appl. Geochem. 22, 2007) investigated the surface properties of respirable-sized quartz grains in bentonites and recognized pervasive montmorillonite surface coatings on silica grains. The purpose of this study was to determine the dissolution rate and biodurability of montmorillonite in simulated lung fluids and to assess its potential to mitigate silica cytotoxicity. Modified batch reaction experiments were conducted on purified and size fractionated calcic (SAz-2; 0.4-5 μm) and sodic (DC-2; 0.4-2 μm) montmorillonites for 120 to 160 days of reaction time at 37°C in both simulated extracellular lung fluid (Lu) and simulated lysosomal fluid (Ly). Modified batch experiments simulated a flow-through setup and minimized sample handling difficulties. Reacted Lu and Ly fluid was analyzed for Mg, Al, and Si on an ICP-OE spectrometer. Steady state dissolution was reached 90-100 days after the start of the experiment and maintained for 40-60 days. Measured montmorillonite dissolution rates based on BET surface areas and Si steady state release range from 4.1x10-15 mol/m2/s at the slowest to 1.0x10-14 mol/m2/s at the fastest with relative uncertainties of less than 10%. Samples reacting in Ly (pH = 4.55) dissolved faster than those in Lu (pH = 7.40), and DC-2 dissolved faster than SAz-2. The measured range of biodurabilities was 1,300 to 3,400 years for a 1 μm grain assuming a spherical volume and a molar volume equal to that of illite. The difference in salinities of the two fluids was too slight to draw conclusions about the relationship of ionic strength to dissolution rate. Results indicate that montmorillonite dissolution is incongruent and edge controlled. Dissolution rates for DC- 2 and SAz-2 clays were comparable to those reported in the literature. Biodurability results fall well beyond the lifespan of humans confirming montmorillonite's potential to mitigate silica cytotoxicity.

Cytotoxicity evaluation of Curcuma zedoaria (Christm.) Roscoe fluid extract used in oral hygiene products.

PubMed

Fernandes, Joao Paulo Dos Santos; Mello-Moura, Anna Carolina Volpi; Marques, Marcia Martins; Nicoletti, Maria Aparecida

2012-12-01

This in vitro study evaluated the cytotoxic effects of the Curcuma zedoaria (Christm.) Roscoe (popular name: zedoary) fluid extract, as used in preparations for oral hygiene, mostly for anti-septic purposes. The cell viability and cell growth were assessed by Trypan blue dye exclusion assay using the LMF cell line derived from oral mucosa. Cell viability (short-term assay) was measured 0, 6, 12 and 24 h after contact with the fluid extract. Cell growth (long-term assay) was analyzed in 1, 3, 5 and 7 days. The experimental groups were those testing the fluid extract obtained from the zedoary rhizome and the extractor liquid (ethanol 70° GL) in the concentrations of 0.01-0.0001% v/v. Fresh DMEM were used in the control cultures. Short-term assay-all studied cultures maintained stable cell viability; Long-term assay-there was progressive cell growth in all studied cultures. According to the results, the zedoary fluid extract presents low cytotoxicity and probably can be used in the oral hygiene products.

Supercritical fluid extraction and direct fluid injection mass spectrometry for the determination of trichothecene mycotoxins in wheat samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kalinoski, H.T.; Udseth, H.R.; Wright, B.W.

1986-10-01

The application of on-line supercritical fluid extraction with chemical ionization mass spectrometry and collision induced dissociation tandem mass spectrometry for the rapid identification of parts-per-million levels of several trichothecene mycotoxins is demonstrated. Supercritical carbon dioxide is shown to allow identification of mycotoxins with minimum sample handling in complex natural matrices (e.g., wheat). Tandem mass spectrometry techniques are employed for unambiguous identification of compounds of varying polarity, and false positives from isobaric compounds are avoided. Capillary column supercritical fluid chromatography-mass spectrometry of a supercritical fluid extract of the same sample was also performed and detection limits in the parts-per-billion range appearmore » feasible.« less

[Study on condition for extraction of arctiin from fruits of Arctium lappa using supercritical fluid extraction].

PubMed

Dong, Wen-hong; Liu, Ben

2006-08-01

To study the feasibility of supercritical fluid extraction (SFE) for arctiin from the fruits of Arctium lappa. The extracts were analyzed by HPLC, optimum extraction conditions were studied by orthogonal tests. The optimal extraction conditions were: pressure 40 MPa, temperature 70 degrees C, using methanol as modifier carrier at the rate of 0.55 mL x min(-1), static extraction time 5 min, dynamic extraction 30 min, flow rate of CO2 2 L x min(-1). SFE has the superiority of adjustable polarity, and has the ability of extracting arctiin.

Engineering design and prototype development of a full scale ultrasound system for virgin olive oil by means of numerical and experimental analysis.

PubMed

Clodoveo, Maria Lisa; Moramarco, Vito; Paduano, Antonello; Sacchi, Raffaele; Di Palmo, Tiziana; Crupi, Pasquale; Corbo, Filomena; Pesce, Vito; Distaso, Elia; Tamburrano, Paolo; Amirante, Riccardo

2017-07-01

The aim of the virgin olive oil extraction process is mainly to obtain the best quality oil from fruits, by only applying mechanical actions while guaranteeing the highest overall efficiency. Currently, the mechanical methods used to extract virgin oils from olives are basically of two types: the discontinuous system (obsolete) and the continuous one. Anyway the system defined as "continuous" is composed of several steps which are not all completely continuous, due to the presence of the malaxer, a device that works in batch. The aim of the paper was to design, realize and test the first full scale sono-exchanger for the virgin olive oil industry, to be placed immediately after the crusher and before the malaxer. The innovative device is mainly composed of a triple concentric pipe heat exchanger combined with three ultrasound probes. This mechanical solution allows both the cell walls (which release the oil droplets) along with the minor compounds to be destroyed more effectively and the heat exchange between the olive paste and the process water to be accelerated. This strategy represents the first step towards the transformation of the malaxing step from a batch operation into a real continuous process, thus improving the working capacity of the industrial plants. Considering the heterogeneity of the olive paste, which is composed of different tissues, the design of the sono-exchanger required a thorough fluid dynamic analysis. The thermal effects of the sono-exchanger were monitored by measuring the temperature of the product at the inlet and the outlet of the device; in addition, the measurement of the pigments concentration in the product allowed monitoring the mechanical effects of the sono-exchanger. The effects of the innovative process were also evaluated in terms of extra virgin olive oil yields and quality, evaluating the main legal parameters, the polyphenol and tocopherol content. Moreover, the activity of the polyphenol oxidase enzyme in the olive paste was measured. Copyright © 2017 Elsevier B.V. All rights reserved.

Bio-oil production from biomass via supercritical fluid extraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Durak, Halil, E-mail: halildurak@yyu.edu.tr

2016-04-18

Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds weremore » identified by GC-MS obtained in acetone and ethanol respectively.« less

High-Temperature Lubricant Analyses Using the System for Thermal Diagnostic Studies (STDS). A Feasibility Study

DTIC Science & Technology

1990-07-01

permeation chromatography (GPC) have been applied to lubricant type samples. 8 Most recently the newly introduced supercritical fluid chromatography (SFC... fluids , such as lubricants and hydraulic fluids can also be examined using various inverse chromatography procedures. Another mode, known as reaction...introduction of new gaseous extraction techniques, e.g., supercritical fluid extraction, procedures such as IGC will probably be developed for vastly

Nitrous Oxide Explosive Hazards

DTIC Science & Technology

2008-05-01

Supercritical Fluid Extraction- Capillary Gas Chromatography (SFE-GC) With a Conventional Split/Splitless Injection Port”, Journal of Chromatographic...Aromatic Hydrocarbons from Environmental Solids Using Supercritical Fluids ”, Steven B. Hawthorne and David J. Miller, Anal. Chem. 59, pp 1705-1708, 1987...Katayama, T., J. Supercrit . Fluids , 1990, 3, 78-84. 30. “ Supercritical Fluid Extraction of Fungal Oil Using CO2, N2O, CHF3, and SF6”, Keiji Sakaki

Chemical Composition Analysis of Extracts from Ficus Hirta Using Supercritical Fluid

NASA Astrophysics Data System (ADS)

Deng, S. B.; Chen, J. P.; Chen, Y. Z.; Yu, C. Q.; Yang, Y.; Wu, S. H.; Chen, C. Z.

2018-05-01

Ficus hirta was extracted by supercritical carbon dioxide. The volatile chemical components of extracts were analyzed using gas chromatography-mass spectrometry (GC-MS). The percentage of products extracted by Supercritical Fluid Extraction(SFE) was 2.5%. Nineteen volatile compounds were identified. The main volatile components were Elemicin, Psoralen, Palmitic acid, Bergapten, α-Linolenic acid, Medicarpin, Retinoic Acid, Maackiain, and Squalene. The method is simple and quick, and can be used for the preliminary analysis of chemical constituents of supercritical extracts of Ficus hirta.

[Automatic Extraction and Analysis of Dosimetry Data in Radiotherapy Plans].

PubMed

Song, Wei; Zhao, Di; Lu, Hong; Zhang, Biyun; Ma, Jun; Yu, Dahai

To improve the efficiency and accuracy of extraction and analysis of dosimetry data in radiotherapy plans for a batch of patients. With the interface function provided in Matlab platform, a program was written to extract the dosimetry data exported from treatment planning system in DICOM RT format and exported the dose-volume data to an Excel file with the SPSS compatible format. This method was compared with manual operation for 14 gastric carcinoma patients to validate the efficiency and accuracy. The output Excel data were compatible with SPSS in format, the dosimetry data error for PTV dose interval of 90%-98%, PTV dose interval of 99%-106% and all OARs were -3.48E-5 ± 3.01E-5, -1.11E-3 ± 7.68E-4, -7.85E-5 ± 9.91E-5 respectively. Compared with manual operation, the time required was reduced from 5.3 h to 0.19 h and input error was reduced from 0.002 to 0. The automatic extraction of dosimetry data in DICOM RT format for batch patients, the SPSS compatible data exportation, quick analysis were achieved in this paper. The efficiency of clinical researches based on dosimetry data analysis of large number of patients will be improved with this methods.

Metal-organic framework mixed-matrix disks: Versatile supports for automated solid-phase extraction prior to chromatographic separation.

PubMed

Ghani, Milad; Font Picó, Maria Francesca; Salehinia, Shima; Palomino Cabello, Carlos; Maya, Fernando; Berlier, Gloria; Saraji, Mohammad; Cerdà, Víctor; Turnes Palomino, Gemma

2017-03-10

We present for the first time the application of metal-organic framework (MOF) mixed-matrix disks (MMD) for the automated flow-through solid-phase extraction (SPE) of environmental pollutants. Zirconium terephthalate UiO-66 and UiO-66-NH 2 MOFs with different size (90, 200 and 300nm) have been incorporated into mechanically stable polyvinylidene difluoride (PVDF) disks. The performance of the MOF-MMDs for automated SPE of seven substituted phenols prior to HPLC analysis has been evaluated using the sequential injection analysis technique. MOF-MMDs enabled the simultaneous extraction of phenols with the concomitant size exclusion of molecules of larger size. The best extraction performance was obtained using a MOF-MMD containing 90nm UiO-66-NH 2 crystals. Using the selected MOF-MMD, detection limits ranging from 0.1 to 0.2μgL -1 were obtained. Relative standard deviations ranged from 3.9 to 5.3% intra-day, and 4.7-5.7% inter-day. Membrane batch-to-batch reproducibility was from 5.2 to 6.4%. Three different groundwater samples were analyzed with the proposed method using MOF-MMDs, obtaining recoveries ranging from 90 to 98% for all tested analytes. Copyright © 2017 Elsevier B.V. All rights reserved.

Etude de production et de caracterisation de biocharbons de panic erige (Panicum virgatum L.) obtenus par pyrolyse

NASA Astrophysics Data System (ADS)

Pilon, Guillaume

This research aimed at the production of biomass char under pyrolytic conditions, targeting biochar as soil amendment, while also considering its application as biocoal, either for bioenergy or subsequent upgrading. The production of biomass char was performed using two bench-scale, batch-type, fixed-bed reactors, each with an operating capacity of 1 and 25 gw.b. /batch, respectively. Switchgrass (Panicum virgatum) has been used for the tests. Production conditions studied implied temperatures of 300, 400 and 500 °C with short residence times (2.5 and 5 min). As well, the effect of using CO2 as vector gas has been compared to a common inert environment of N2. The effects of the previously mentioned parameters were correlated with some important physicochemical characteristics of biomass char. Analyses were also performed on complementary pyrolytic products (bio-oil and gas). The biomass char extraction was performed using a Soxhlet and dichloromethane was used as extracting solvent. The extracts were then characterized by GC-MS thus allowing the identification of several compounds. Specific pyrolysis conditions used at 300 °C - N2 with the 1 g/batch reactor, such as high heating rates as well as high convection conditions, presented advantegeous biomass char yields and properties, and, possible torrefaction process productivity improvement (in comparison to reported literature, such as Gilbert et al. [2009]). The char extracts as well as the bio-oils analysis (also performed using GC-MS), all generated from the 25 g/batch reactor, showed major differences among the compounds obtained from the CO2 and N2 environments, respectively. Several compounds observed in the char extracts appeared less concentrated in the CO2 environment vs N2, for the same reaction temperatures. As an example, at 400 °C, furfural was found only in char extracts from N2 environment as compared to the CO2 environment. Among all studied conditions (for both reactors), only naphthalene and naphthalene derivatives constituted the PAHs content, which was only detected for the chars produced at 500 °C. The use of CO2 as pyrolysis vector gas led to a significant difference for every temperature conditions studied for the biomass char as well as for the liquid and gas products. At 300 °C, in CO 2 environment, it is possible to observe a bio-oil production significantly lower than within a N2 environment (18.0 vs 24.6 %; CO2 vs N2 for P<0.002), a result consistent with the biomass char volatile content that was shown to be significantly higher under the same conditions (0.29 vs 0.35 gchar volatiles content/graw biomass; P=0.1). In addition, at 500 °C, the char ash content was observed to be significantly lower in CO 2 than in N2 (P<0.06). Keywords: Pyrolysis, torrefaction, char, biochar, biocoal, CO 2, Soxhlet extractions, characterization.

Effective alkaline metal-catalyzed oxidative delignification of hybrid poplar

DOE PAGES

Bhalla, Aditya; Bansal, Namita; Stoklosa, Ryan J.; ...

2016-02-09

Background: Strategies to improve copper-catalyzed alkaline hydrogen peroxide (Cu-AHP) pretreatment of hybrid poplar were investigated. These improvements included a combination of increasing hydrolysis yields, while simultaneously decreasing process inputs through (i) more efficient utilization of H 2O 2 and (ii) the addition of an alkaline extraction step prior to the metal-catalyzed AHP pretreatment. We hypothesized that utilizing this improved process could substantially lower the chemical inputs needed during pretreatment. Results: Hybrid poplar was pretreated utilizing a modified process in which an alkaline extraction step was incorporated prior to the Cu-AHP treatment step and H 2O 2 was added batch-wise overmore » the course of 10 h. Our results revealed that the alkaline pre-extraction step improved both lignin and xylan solubilization, which ultimately led to improved glucose (86 %) and xylose (95 %) yields following enzymatic hydrolysis. An increase in the lignin solubilization was also observed with fed-batch H 2O 2 addition relative to batch-only addition, which again resulted in increased glucose and xylose yields (77 and 93 % versus 63 and 74 %, respectively). Importantly, combining these strategies led to significantly improved sugar yields (96 % glucose and 94 % xylose) following enzymatic hydrolysis. In addition, we found that we could substantially lower the chemical inputs (enzyme, H 2O 2, and catalyst), while still maintaining high product yields utilizing the improved Cu-AHP process. This pretreatment also provided a relatively pure lignin stream consisting of ≥90 % Klason lignin and only 3 % xylan and 2 % ash following precipitation. Two-dimensional heteronuclear single-quantum coherence (2D HSQC) NMR and size-exclusion chromatography demonstrated that the solubilized lignin was high molecular weight (Mw ≈ 22,000 Da) and only slightly oxidized relative to lignin from untreated poplar. In conclusion: This study demonstrated that the fed-batch, two-stage Cu-AHP pretreatment process was effective in pretreating hybrid poplar for its conversion into fermentable sugars. Results showed sugar yields near the theoretical maximum were achieved from enzymatically hydrolyzed hybrid poplar by incorporating an alkaline extraction step prior to pretreatment and by efficiently utilizing H 2O 2 during the Cu-AHP process. Significantly, this study reports high sugar yields from woody biomass treated with an AHP pretreatment under mild reaction conditions.« less

Supercritical Fluid Extraction of Metal Chelate: A Review.

PubMed

Ding, Xin; Liu, Qinli; Hou, Xiongpo; Fang, Tao

2017-03-04

Supercritical fluid extraction (SFE), as a new green extraction technology, has been used in extracting various metal species. The solubilities of chelating agents and corresponding metal chelates are the key factors which influence the efficiency of SFE. Other main properties of them such as stability and selectivity are also reviewed. The extraction mechanisms of mainly used chelating agents are explained by typical examples in this paper. This is the important aspect of SFE of metal ions. Moreover, the extraction efficiencies of metal species also depend on other factors such as temperature, pressure, extraction time and matrix effect. The two main complexation methods namely in-situ and on-line chelating SFE are described in detail. As an efficient chelating agent, tributyl phosphate-nitric acid (TBP-HNO 3 ) complex attracts much attention. The SFE of metal ions, lanthanides and actinides as well as organometallic compounds are also summarized. With the proper selection of ligands, high efficient extraction of metal species can be obtained. As an efficient sample analysis method, supercritical fluid chromatography (SFC) is introduced in this paper. Recently, the extraction method combining ionic liquids (ILs) with supercritical fluid has been becoming a novel technology for treating metal ions. The kinetics related to SFE of metal species is discussed with some specific examples.

Supercritical fluid extraction

DOEpatents

Wai, Chien M.; Laintz, Kenneth

1994-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated or lipophilic crown ether or fluorinated dithiocarbamate. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

21 CFR 310.531 - Drug products containing active ingredients offered over-the-counter (OTC) for the treatment of...

Code of Federal Regulations, 2013 CFR

2013-04-01

... subnitrate, calomel, camphor, cholesterol, ergot fluid extract, hexachlorophene, ichthammol, isobutamben... aminacrine hydrochloride, bismuth subnitrate, calomel, camphor, cholesterol, ergot fluid extract...

21 CFR 310.531 - Drug products containing active ingredients offered over-the-counter (OTC) for the treatment of...

Code of Federal Regulations, 2011 CFR

2011-04-01

... subnitrate, calomel, camphor, cholesterol, ergot fluid extract, hexachlorophene, ichthammol, isobutamben... aminacrine hydrochloride, bismuth subnitrate, calomel, camphor, cholesterol, ergot fluid extract...

21 CFR 310.531 - Drug products containing active ingredients offered over-the-counter (OTC) for the treatment of...

Code of Federal Regulations, 2010 CFR

2010-04-01

... subnitrate, calomel, camphor, cholesterol, ergot fluid extract, hexachlorophene, ichthammol, isobutamben... aminacrine hydrochloride, bismuth subnitrate, calomel, camphor, cholesterol, ergot fluid extract...

21 CFR 310.531 - Drug products containing active ingredients offered over-the-counter (OTC) for the treatment of...

Code of Federal Regulations, 2012 CFR

2012-04-01

... subnitrate, calomel, camphor, cholesterol, ergot fluid extract, hexachlorophene, ichthammol, isobutamben... aminacrine hydrochloride, bismuth subnitrate, calomel, camphor, cholesterol, ergot fluid extract...

21 CFR 310.531 - Drug products containing active ingredients offered over-the-counter (OTC) for the treatment of...

Code of Federal Regulations, 2014 CFR

2014-04-01

... subnitrate, calomel, camphor, cholesterol, ergot fluid extract, hexachlorophene, ichthammol, isobutamben... aminacrine hydrochloride, bismuth subnitrate, calomel, camphor, cholesterol, ergot fluid extract...

Digestive solubilization of sediment-associated pollutants: In vitro extraction vs. in vivo bioavailability

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weston, D.P.; Mayer, L.M.

1995-12-31

A method using polychaete digestive fluids as a more biologically realistic extractant has recent been proposed as a means to quantify this bioavailable fraction. This work was intended to evaluate this approach with polynuclear aromatic hydrocarbons (PAH), and, in particular, to relate in vitro measures of PAH solubilization by digestive fluids to bioavailability as perceived by the whole animal. In tests with a variety of PAH-contaminated sediments, there were dramatic differences among the sediments in the amounts of PAH extracted by digestive fluids. About 50% of a PAH spike was extracted from a low organic carbon sediment during digestive fluidmore » extraction, while only 20% was extracted from a high organic carbon sediment. The relationships between these differences in PAH solubilization and true bioavailability were evaluated in polychaete bioaccumulation tests measuring PAH uptake rate coefficients and steady state body burdens. The work has also shown that desorption of PAH from ingested sediments in the whole animal approximated the quantities extracted in the in vitro tests. Moreover, desorption of PAH from ingested sediments was found to be greatest in that portion of the polychaete gut with the highest enzymatic activity and from which the digestive fluids had been collected. The digestive fluid extraction approach provides a new tool to examine digestive uptake of contaminants by manipulations that would be impossible in vivo, and may help to quantify a bioavailable contaminant fraction.« less

Results from the interim salt disposition program macrobatch 10 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.; Bannochie, C. J.

2017-02-23

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 10 for the Interim Salt Disposition Program (ISDP). This document reports characterization data on the samples of Tank 21H and fulfills the requirements of Deliverable 3 of the Technical Task Request (TTR). Further work will report the results of the Extraction-Scrub-Strip (ESS) testing (Task 5 of the TTR) using the Tank 21H material. Task 4 of the TTR (MST Strike) will not be completed for Salt Batch 10.

Lack of evidence in vivo for a remote effect of Escherichia coli heat stable enterotoxin on jejunal fluid absorption.

PubMed

Lucas, M L; Duncan, N W; o'reilly, N F; McIlvenny, T J; Nelson, Y B

2008-05-01

On contact with the mucosa, heat stable (STa) enterotoxin from Escherichia coli reduces fluid absorption in vivo in the perfused jejunum of the anaesthetized rat. The question of whether it also has a vagally mediated remote action on jejunal absorption, when instilled into the ileum, was re-examined, given contradictory findings in the literature. A standard perfused loop preparation was used to measure luminal uptake of fluid in vivo by means of volume recovery. STa in the ileum was found to have no effect on jejunal absorption, regardless of cervical or sub-diaphragmatic vagotomy and also regardless of the nature of the perfusate anion. The batches of toxin were shown in parallel experiments to reduce fluid absorption directly in the jejunum and also in the ileum. Similarly, vagal nerves prior to section had demonstrable in vivo physiological function. There was therefore no evidence for an indirect, vagally mediated ileal effect of STa on proximal fluid absorption.

Direct infusion mass spectrometry metabolomics dataset: a benchmark for data processing and quality control

PubMed Central

Kirwan, Jennifer A; Weber, Ralf J M; Broadhurst, David I; Viant, Mark R

2014-01-01

Direct-infusion mass spectrometry (DIMS) metabolomics is an important approach for characterising molecular responses of organisms to disease, drugs and the environment. Increasingly large-scale metabolomics studies are being conducted, necessitating improvements in both bioanalytical and computational workflows to maintain data quality. This dataset represents a systematic evaluation of the reproducibility of a multi-batch DIMS metabolomics study of cardiac tissue extracts. It comprises of twenty biological samples (cow vs. sheep) that were analysed repeatedly, in 8 batches across 7 days, together with a concurrent set of quality control (QC) samples. Data are presented from each step of the workflow and are available in MetaboLights. The strength of the dataset is that intra- and inter-batch variation can be corrected using QC spectra and the quality of this correction assessed independently using the repeatedly-measured biological samples. Originally designed to test the efficacy of a batch-correction algorithm, it will enable others to evaluate novel data processing algorithms. Furthermore, this dataset serves as a benchmark for DIMS metabolomics, derived using best-practice workflows and rigorous quality assessment. PMID:25977770

Assessing the use of food coloring as an appropriate visual guide for homogenously mixed capsule powders in extemporaneous compounding.

PubMed

Hoffmann, Brittany; Carlson, Christie; Rao, Deepa A

2014-01-01

The purpose of this work was to assess the use of food colors as a visual aid to determine homogeneous mixing in the extemporaneous preparation of capsules. Six different batches of progesterone slow-release 200-mg capsules were prepared by different mixing methods until visually determined as homogeneous based on yellow food coloring distribution in the preparation by the Central Iowa Compounding Pharmacy, Des Moines, Iowa. UV-Vis spectrophotometry was used to extract and evaluate yellow food coloring content in each of these batches and compared to an in-house, small-batch geometric dilution preparation of progesterone slow- release 200-mg capsules. Of the 6 batches tested, only one, which followed the principles of additive dilution and an appropriate mixing time, was both visually and quantitatively homogeneous in the detection of yellow food coloring. The use of food coloring alone is not a valid quality-assurance tool in determining homogeneous mixing. Principles of geometric and/or additive dilution and appropriate mixing times along with the food color can serve as a quality-assurance tool.

Physicochemical Characteristics of Transferon™ Batches.

PubMed

Medina-Rivero, Emilio; Vallejo-Castillo, Luis; Vázquez-Leyva, Said; Pérez-Sánchez, Gilberto; Favari, Liliana; Velasco-Velázquez, Marco; Estrada-Parra, Sergio; Pavón, Lenin; Pérez-Tapia, Sonia Mayra

2016-01-01

Transferon, a biotherapeutic agent that has been used for the past 2 decades for diseases with an inflammatory component, has been approved by regulatory authorities in Mexico (COFEPRIS) for the treatment of patients with herpes infection. The active pharmaceutical ingredient (API) of Transferon is based on polydispersion of peptides that have been extracted from lysed human leukocytes by a dialysis process and a subsequent ultrafiltration step to select molecules below 10 kDa. To physicochemically characterize the drug product, we developed chromatographic methods and an SDS-PAGE approach to analyze the composition and the overall variability of Transferon. Reversed-phase chromatographic profiles of peptide populations demonstrated batch-to-batch consistency from 10 representative batches that harbored 4 primary peaks with a relative standard deviation (RSD) of less than 7%. Aminogram profiles exhibited 17 proteinogenic amino acids and showed that glycine was the most abundant amino acid, with a relative content of approximately 18%. Further, based on their electrophoretic migration, the peptide populations exhibited a molecular mass of about 10 kDa. Finally, we determined the Transferon fingerprint using a mass spectrometry tool. Because each batch was produced from independent pooled buffy coat samples from healthy donors, supplied by a local blood bank, our results support the consistency of the production of Transferon and reveal its peptide identity with regard to its physicochemical attributes.

[Study on new extraction technology of astragaloside IV].

PubMed

Sun, Haiyan; Guan, Su; Huang, Min

2005-08-01

To explore the possibility and the optimal extraction technology of astragaloside IV by SFE-CO2. According the content of astragaloside IV, the optimum extraction technology parameters such as extraction temperature, pressure, extraction time, velocity of fluid and co-solvent were investigated and the result was compared with that of water extraction. The optimum technical parameters were as follows: Extracting pressure 40 Mpa, temperature 45 degrees C, extracting time 2h, co-solvent was 95% ethanol and its dosage was 4ml/g, the ratio of CO2 fluid was 10 kg/kg x h. Extraction technology of astragaloside IV by SFE-CO2 is reliable, stable.

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

DOEpatents

Wai, Chien M.; Smart, Neil G.; Lin, Yuehe

1998-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent is described. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

Justification of Drug Product Dissolution Rate and Drug Substance Particle Size Specifications Based on Absorption PBPK Modeling for Lesinurad Immediate Release Tablets.

PubMed

Pepin, Xavier J H; Flanagan, Talia R; Holt, David J; Eidelman, Anna; Treacy, Don; Rowlings, Colin E

2016-09-06

In silico absorption modeling has been performed, to assess the impact of in vitro dissolution on in vivo performance for ZURAMPIC (lesinurad) tablets. The dissolution profiles of lesinurad tablets generated using the quality control method were used as an input to a GastroPlus model to estimate in vivo dissolution in the various parts of the GI tract and predict human exposure. A model was set up, which accounts for differences of dosage form transit, dissolution, local pH in the GI tract, and fluid volumes available for dissolution. The predictive ability of the model was demonstrated by confirming that it can reproduce the Cmax observed for independent clinical trial. The model also indicated that drug product batches that pass the proposed dissolution specification of Q = 80% in 30 min are anticipated to be bioequivalent to the clinical reference batch. To further explore the dissolution space, additional simulations were performed using a theoretical dissolution profile below the proposed specification. The GastroPlus modeling indicates that such a batch will also be bioequivalent to standard clinical batches despite having a dissolution profile, which would fail the proposed dissolution specification of Q = 80% in 30 min. This demonstrates that the proposed dissolution specification sits comfortably within a region of dissolution performance where bioequivalence is anticipated and is not near an edge of failure for dissolution, providing additional confidence to the proposed specifications. Finally, simulations were performed using a virtual drug substance batch with a particle size distribution at the limit of the proposed specification for particle size. Based on these simulations, such a batch is also anticipated to be bioequivalent to clinical reference, demonstrating that the proposed specification limits for particle size distribution would give products bioequivalent to the pivotal clinical batches.

Extraction of metals using supercritical fluid and chelate forming legand

DOEpatents

Wai, Chien M.; Laintz, Kenneth E.

1998-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated .beta.-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated .beta.-diketone and a trialkyl phosphate, or a fluorinated .beta.-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated .beta.-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

Extraction of metals using supercritical fluid and chelate forming ligand

DOEpatents

Wai, C.M.; Laintz, K.E.

1998-03-24

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated {beta}-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated {beta}-diketone and a trialkyl phosphate, or a fluorinated {beta}-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated {beta}-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process. 7 figs.

Noble gases fingerprint a metasedimentary fluid source in the Macraes orogenic gold deposit, New Zealand

NASA Astrophysics Data System (ADS)

Goodwin, Nicholas R. J.; Burgess, Ray; Craw, Dave; Teagle, Damon A. H.; Ballentine, Chris J.

2017-02-01

The world-class Macraes orogenic gold deposit (˜10 Moz resource) formed during the late metamorphic uplift of a metasedimentary schist belt in southern New Zealand. Mineralising fluids, metals and metalloids were derived from within the metasedimentary host. Helium and argon extracted from fluid inclusions in sulphide mineral grains (three crush extractions from one sample) have crustal signatures, with no evidence for mantle input (R/Ra = 0.03). Xenon extracted from mineralised quartz samples provides evidence for extensive interaction between fluid and maturing organic material within the metasedimentary host rocks, with 132Xe/36Ar ratios up to 200 times greater than air. Similarly, I/Cl ratios for fluids extracted from mineralised quartz are similar to those of brines from marine sediments that have interacted with organic matter and are ten times higher than typical magmatic/mantle fluids. The Macraes mineralising fluids were compositionally variable, reflecting either mixing of two different crustal fluids in the metasedimentary pile or a single fluid type that has had varying degrees of interaction with the host metasediments. Evidence for additional input of meteoric water is equivocal, but minor meteoric incursion cannot be discounted. The Macraes deposit formed in a metasedimentary belt without associated coeval magmatism, and therefore represents a purely crustal metamorphogenic end member in a spectrum of orogenic hydrothermal processes that can include magmatic and/or mantle fluid input elsewhere in the world. There is no evidence for involvement of minor intercalated metabasic rocks in the Macraes mineralising system. Hydrothermal fluids that formed other, smaller, orogenic deposits in the same metamorphic belt have less pronounced noble gas and halogen evidence for crustal fluid-rock interaction than at Macraes, but these deposits also formed from broadly similar metamorphogenic processes.

A method for determining the phosphorus sorption capacity and amorphous aluminum of aluminum-based drinking water treatment residuals.

PubMed

Dayton, E A; Basta, N T

2005-01-01

A high amorphous aluminum or iron oxide content in drinking water treatment residuals (WTRs) can result in a high phosphorus (P) sorption capacity. Therefore, WTR may be used beneficially to adsorb P and reduce P loss to surface or ground water. The strong relationship between acid ammonium oxalate-extractable aluminum (Al(ox)) and Langmuir phosphorus adsorption maximum (P(max)) in WTR could provide a useful tool for determining P(max) without the onus of the multipoint batch equilibrations necessary for the Langmuir model. The objectives of this study were to evaluate and/or modify an acid ammonium oxalate extraction of Al(ox) and the experimental conditions used to generate P adsorption isotherms to strengthen the relationship between Al(ox) and P(max). The oxalate extraction solution to WTR ratio varied from 40:1, 100:1, and 200:1. Batch equilibration conditions were also varied. The WTR particle size was reduced from <2 mm to <150 microm, and batch equilibration was extended from 17 h to 6 d. Increasing the solution to WTR ratio to 100:1 extracted significantly greater Al(ox) at levels of >50 mg Al kg(-1). No additional increase was found at 200:1. Reducing WTR particle size from <2 mm to <150 microm increased P(max) 2.46-fold. Extending the equilibration time from 17 h to 6 d increased P(max) by a mean of 5.83-fold. The resulting empirical regression equation between the optimized Al(ox) and P(max) (r(2) = 0.91, significant at the 0.001 probability level) may provide a tool to estimate the P(max) of Al-based WTR simply by measuring Al(ox). The accurate determination of WTR P(max) and Al(ox) is essential in using WTR effectively to reduce P loss in runoff or to reduce the solubility of P in agricultural soils or organic waste materials (biosolids, manure).

Flow-batch analysis of clenbuterol based on analyte extraction on molecularly imprinted polymers coupled to an in-system chromogenic reaction. Application to human urine and milk substitute samples.

PubMed

González, Natalia; Grünhut, Marcos; Šrámková, Ivana; Lista, Adriana G; Horstkotte, Burkhard; Solich, Petr; Sklenářová, Hana; Acebal, Carolina C

2018-02-01

A fully automated spectrophotometric method based on flow-batch analysis has been developed for the determination of clenbuterol including an on-line solid phase extraction using a molecularly imprinted polymer (MIP) as the sorbent. The molecularly imprinted solid phase extraction (MISPE) procedure allowed analyte extraction from complex matrices at low concentration levels and with high selectivity towards the analyte. The MISPE procedure was performed using a commercial MIP cartridge that was introduced into a guard column holder and integrated in the analyzer system. Optimized parameters included the volume of the sample, the type and volume of the conditioning and washing solutions, and the type and volume of the eluent. Quantification of clenbuterol was carried out by spectrophotometry after in-system post-elution analyte derivatization based on azo-coupling using N- (1-Naphthyl) ethylenediamine as the coupling agent to yield a red-colored compound with maximum absorbance at 500nm. Both the chromogenic reaction and spectrophotometric detection were performed in a lab-made flow-batch mixing chamber that replaced the cuvette holder of the spectrophotometer. The calibration curve was linear in the 0.075-0.500mgL -1 range with a correlation coefficient of 0.998. The precision of the proposed method was evaluated in terms of the relative standard deviation obtaining 1.1% and 3.0% for intra-day precision and inter-day precision, respectively. The detection limit was 0.021mgL -1 and the sample throughput for the entire process was 3.4h -1 . The proposed method was applied for the determination of CLB in human urine and milk substitute samples obtaining recoveries values within a range of 94.0-100.0%. Copyright © 2017 Elsevier B.V. All rights reserved.

Rumen bacteria at work: bioaugmentation strategies to enhance biogas production from cow manure.

PubMed

Ozbayram, E G; Akyol, Ç; Ince, B; Karakoç, C; Ince, O

2018-02-01

To investigate the effects of different bioaugmentation strategies for enhancing the biogas production from cow manure and evaluate microbial community patterns. Co-inoculation with cow rumen fluid and cow rumen-derived enriched microbial consortia was evaluated in anaerobic batch tests at 36°C and 41°C. Singular addition of both rumen fluid and enriched bioaugmentation culture had a promising enhancement on methane yields; however, the highest methane yield (311 ml CH 4 per gram VS at 41°C) was achieved when the anaerobic seed sludge was co-inoculated together with rumen fluid and enriched bioaugmentation culture. Bacterial community profiles were investigated by Ion PGM Platform, and specific lignocellulolytic bacteria dynamics in batch tests were assessed by qPCR. The temperature had minor effects on the abundance of bacterial community; in which Bacteroidetes and Firmicutes were the most abundant phyla in all digesters. Furthermore, Rikenellaceae, Clostridiaceae, Porphyromonadaceae, Bacteroidaceae and Ruminococcaceae played a crucial role during the anaerobic degradation of cow manure. There was an important impact of Firmicutes flavefaciens and Ruminococcus albus at 41°C, which in turn positively affected the methane production. The degree of enhancement in biogas production can be upgraded by the co-inoculation of rumen-derived bioaugmentation culture with anaerobic seed sludge with high methanogenic activity. A close look at the biotic interactions and their associations with abiotic factors might be valuable for evaluating rumen-related bioaugmentation applications. © 2017 The Society for Applied Microbiology.

Impact of Nisin-Activated Packaging on Microbiota of Beef Burgers during Storage

PubMed Central

Ferrocino, Ilario; Greppi, Anna; La Storia, Antonietta; Rantsiou, Kalliopi; Ercolini, Danilo

2015-01-01

Beef burgers were stored at 4°C in a vacuum in nisin-activated antimicrobial packaging. Microbial ecology analyses were performed on samples collected between days 0 and 21 of storage to discover the population diversity. Two batches were analyzed using RNA-based denaturing gradient gel electrophoresis (DGGE) and pyrosequencing. The active packaging retarded the growth of the total viable bacteria and lactic acid bacteria. Culture-independent analysis by pyrosequencing of RNA extracted directly from meat showed that Photobacterium phosphoreum, Lactococcus piscium, Lactobacillus sakei, and Leuconostoc carnosum were the major operational taxonomic units (OTUs) shared between control and treated samples. Beta diversity analysis of the 16S rRNA sequence data and RNA-DGGE showed a clear separation between two batches based on the microbiota. Control samples from batch B showed a significant high abundance of some taxa sensitive to nisin, such as Kocuria rhizophila, Staphylococcus xylosus, Leuconostoc carnosum, and Carnobacterium divergens, compared to control samples from batch A. However, only from batch B was it possible to find a significant difference between controls and treated samples during storage due to the active packaging. Predicted metagenomes confirmed differences between the two batches and indicated that the use of nisin-based antimicrobial packaging can determine a reduction in the abundance of specific metabolic pathways related to spoilage. The present study aimed to assess the viable bacterial communities in beef burgers stored in nisin-based antimicrobial packaging, and it highlights the efficacy of this strategy to prolong beef burger shelf life. PMID:26546424

Laboratory-scale integrated ARP filter test

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poirier, M.; Burket, P.

2016-03-01

The Savannah River Site (SRS) is currently treating radioactive liquid waste with the Actinide Removal Process (ARP) and the Modular Caustic Side Solvent Extraction Unit (MCU). Recently, the low filter flux through the ARP of approximately 5 gallons per minute has limited the rate at which radioactive liquid waste can be treated. Salt Batch 6 had a lower processing rate and required frequent filter cleaning. There is a desire to understand the causes of the low filter flux and to increase ARP/MCU throughput. This task attempted to simulate the entire ARP process, including multiple batches (5), washing, chemical cleaning, andmore » blending the feed with heels and recycle streams. The objective of the tests was to determine whether one of these processes is causing excessive fouling of the crossflow or secondary filter. The authors conducted the tests with feed solutions containing 6.6 M sodium Salt Batch 6 simulant supernate with no MST.« less

Aerobic biodegradability of methyldiethanolamine (MDEA) used in natural gas sweetening plants in batch tests and continuous flow experiments.

PubMed

Fürhacker, M; Pressl, A; Allabashi, R

2003-09-01

Mixtures of different amines including tertiary amines (methyldiethanolamine, MDEA) are commonly used for the removal of CO2 from gas mixtures or in gas sweetening processes for the extraction of CO2 and H2S. The absorber solutions used can be released into the industrial waste water due to continuous substitution of degraded MDEA, periodically cleaning processes or an accidental spill. In this study, the aerobic biodegradability of MDEA was investigated in a standardised batch test and a continuous flow experiment (40 l/d). The results of the batch test indicated that the MDEA-solution was non-biodegradable during the test period of 28 days, whereas the continuous flow experiments showed biodegradation of more than 96% based on TOC-measurements. This was probably due to the adaptation of the microorganisms to this particular waste water contamination during continuous flow experiment.

Combined Application of UHPLC-QTOF/MS, HPLC-ELSD and 1 H-NMR Spectroscopy for Quality Assessment of DA-9801, A Standardised Dioscorea Extract.

PubMed

Kang, Kyo Bin; Ryu, Jayoung; Cho, Youngwoong; Choi, Sang-Zin; Son, Miwon; Sung, Sang Hyun

2017-05-01

DA-9801, a standardised 50% aqueous ethanolic extract of a mixture of Dioscorea japonica and D. nipponica, is a botanical drug candidate for the treatment of diabetic neuropathy, which finished its US phase II clinical trials recently. An advanced quality control method is needed for further development of DA-9801, considering its high contents of both primary and secondary metabolites. Development of a quality assessment strategy for DA-9801, based on the combination of UHPLC-QTOF/MS, HPLC-ELSD, and 1 H-NMR spectroscopy. The method was developed and tested with 15 batch products of DA-9801. The steroidal saponins of DA-9801 were tentatively identified by UHPLC-QTOF/MS and were quantified with the validated HPLC-ELSD method. Primary metabolites of DA-9801 were identified and profiled using 1 H-NMR spectrometry. The batch-to-batch equivalence of DA-9801 was tested with the 1 H-NMR spectra using spectral binning, correlation analysis, and principal component analysis. Six major saponins of DA-9801 were tentatively identified by UHPLC-QTOF/MS. Among them, protodioscin and dioscin were quantified by the validated HPLC-ELSD method. Twenty-six metabolites were identified in 1 H-NMR spectra. The similarity between DA-9801 batches could be evaluated with the NMR spectra of DA-9801. The 1 H-NMR method also revealed that two Dioscorea species contributed distinct amino acids to the contents of DA-9801. This study validates the effectiveness of UHPLC-QTOF/MS, HPLC-ELSD, and 1 H NMR-combined method for quality control of DA-9801 and its crude materials. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

32 CFR 634.38 - Involuntary extraction of bodily fluids in traffic cases.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 32 National Defense 4 2010-07-01 2010-07-01 true Involuntary extraction of bodily fluids in traffic cases. 634.38 Section 634.38 National Defense Department of Defense (Continued) DEPARTMENT OF THE ARMY (CONTINUED) LAW ENFORCEMENT AND CRIMINAL INVESTIGATIONS MOTOR VEHICLE TRAFFIC SUPERVISION Traffic Supervision § 634.38 Involuntary extraction of...

Iodine speciation in coastal and inland bathing waters and seaweeds extracts using a sequential injection standard addition flow-batch method.

PubMed

Santos, Inês C; Mesquita, Raquel B R; Bordalo, Adriano A; Rangel, António O S S

2015-02-01

The present work describes the development of a sequential injection standard addition method for iodine speciation in bathing waters and seaweeds extracts without prior sample treatment. Iodine speciation was obtained by assessing the iodide and iodate content, the two inorganic forms of iodine in waters. For the determination of iodide, an iodide ion selective electrode (ISE) was used. The indirect determination of iodate was based on the spectrophotometric determination of nitrite (Griess reaction). For the iodate measurement, a mixing chamber was employed (flow batch approach) to explore the inherent efficient mixing, essential for the indirect determination of iodate. The application of the standard addition method enabled detection limits of 0.14 µM for iodide and 0.02 µM for iodate, together with the direct introduction of the target water samples, coastal and inland bathing waters. The results obtained were in agreement with those obtained by ICP-MS and a colorimetric reference procedure. Recovery tests also confirmed the accuracy of the developed method which was effectively applied to bathing waters and seaweed extracts. Copyright © 2014 Elsevier B.V. All rights reserved.

Optical detection of tracer species in strongly scattering media.

PubMed

Brauser, Eric M; Rose, Peter E; McLennan, John D; Bartl, Michael H

2015-03-01

A combination of optical absorption and scattering is used to detect tracer species in a strongly scattering medium. An optical setup was developed, consisting of a dual-beam scattering detection scheme in which sample scattering beam overlaps with the characteristic absorption feature of quantum dot tracer species, while the reference scattering beam is outside any absorption features of the tracer. This scheme was successfully tested in engineered breakthrough tests typical of wastewater and subsurface fluid analysis, as well as in batch analysis of oil and gas reservoir fluids and biological samples. Tracers were detected even under highly scattering conditions, conditions in which conventional absorption or fluorescence methods failed.

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

DOEpatents

Wai, C.M.; Smart, N.G.; Lin, Y.

1998-06-23

A method is described for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process. 7 figs.

Systems and methods for multi-fluid geothermal energy systems

DOEpatents

Buscheck, Thomas A.

2017-09-19

A method for extracting geothermal energy from a geothermal reservoir formation. A production well is used to extract brine from the reservoir formation. At least one of nitrogen (N.sub.2) and carbon dioxide (CO.sub.2) may be used to form a supplemental working fluid which may be injected into a supplemental working fluid injection well. The supplemental working fluid may be used to augment a pressure of the reservoir formation, to thus drive a flow of the brine out from the reservoir formation.

Measurement of polychlorinated biphenyls in solid waste such as transformer insulation paper by supercritical fluid extraction and gas chromatography electron capture detection.

PubMed

Chikushi, Hiroaki; Fujii, Yuka; Toda, Kei

2012-09-21

In this work, a method for measuring polychlorinated biphenyls (PCBs) in contaminated solid waste was investigated. This waste includes paper that is used in electric transformers to insulate electric components. The PCBs in paper sample were extracted by supercritical fluid extraction and analyzed by gas chromatography-electron capture detection. The recoveries with this method (84-101%) were much higher than those with conventional water extraction (0.08-14%), and were comparable to those with conventional organic solvent extraction. Limit of detection was 0.0074 mg kg(-1) and measurable up to 2.5 mg kg(-1) for 0.5 g of paper sample. Data for real insulation paper by the proposed method agreed well with those by the conventional organic solvent extraction. Extraction from wood and concrete was also investigated and good performance was obtained as well as for paper samples. The supercritical fluid extraction is simpler, faster, and greener than conventional organic solvent extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

Extraction fatty acid as a source to produce biofuel in microalgae Chlorella sp. and Spirulina sp. using supercritical carbon dioxide

NASA Astrophysics Data System (ADS)

Tai, Do Chiem; Hai, Dam Thi Thanh; Vinh, Nguyen Hanh; Phung, Le Thi Kim

2016-06-01

In this research, the fatty acids of isolated microalgae were extracted by some technologies such as maceration, Soxhlet, ultrasonic-assisted extraction and supercritical fluid extraction; and analyzed for biodiesel production using GC-MS. This work deals with the extraction of microalgae oil from dry biomass by using supercritical fluid extraction method. A complete study at laboratory of the influence of some parameters on the extraction kinetics and yields and on the composition of the oil in terms of lipid classes and profiles is proposed. Two types of microalgae were studied: Chlorella sp. and Spirulina sp. For the extraction of oil from microalgae, supercritical CO2 (SC-CO2) is regarded with interest, being safer than n-hexane and offering a negligible environmental impact, a short extraction time and a high-quality final product. Whilst some experimental papers are available on the supercritical fluid extraction (SFE) of oil from microalgae, only limited information exists on the kinetics of the process. These results demonstrate that supercritical CO2 extraction is an efficient method for the complete recovery of the neutral lipid phase.

Conversion of Aqueous Ammonia-Treated Corn Stover to Lactic Acid by Simultaneous Saccharification and Cofermentation

NASA Astrophysics Data System (ADS)

Zhu, Yongming; Lee, Y. Y.; Elander, Richard T.

Treatment of corn stover with aqueous ammonia removes most of the structural lignin, whereas retaining the majority of the carbohydrates in the solids. After treatment, both the cellulose and hemicellulose in corn stover become highly susceptible to enzymatic digestion. In this study, corn stover treated by aqueous ammonia was investigated as the substrate for lactic acid production by simultaneous saccharification and cofermentation (SSCF). A commercial cellulase (Spezyme-CP) and Lactobacillus pentosus American Type Culture Collection (ATCC) 8041 (Spanish Type Culture Collection [CECT]-4023) were used for hydrolysis and fermentation, respectively. In batch SSCF operation, the carbohydrates in the treated corn stover were converted to lactic acid with high yields, the maximum lactic acid yield reaching 92% of the stoichiometric maximum based on total fermentable carbohydrates (glucose, xylose, and arabinose). A small amount of acetic acid was also produced from pentoses through the phosphoketolase pathway. Among the major process variables for batch SSCF, enzyme loading and the amount of yeast extract were found to be the key factors affecting lactic acid production. Further tests on nutrients indicated that corn steep liquor could be substituted for yeast extract as a nitrogen source to achieve the same lactic acid yield. Fed-batch operation of the SSCF was beneficial in raising the concentration of lactic acid to a maximum value of 75.0 g/L.

Selective Recovery of Metals from Geothermal Brines

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ventura, Susanna; Bhamidi, Srinivas; Hornbostel, Marc

The objective of this project was to determine the feasibility of developing a new generation of highly selective low-cost ion-exchange resins based on metal-ion imprinted polymers for the separation of metals from geothermal fluids. Expansion of geothermal energy production over the entire U.S. will involve exploitation of low-to-medium temperature thermal waters. Creating value streams from the recovery of critical and near-critical metals from these thermal waters will encourage geothermal expansion. Selective extraction of metals from geothermal fluids is needed to design a cost-effective process for the recovery of lithium and manganese-two near-critical metals with well-known application in the growing lithiummore » battery industry. We have prepared new lithium- and manganese-imprinted polymers in the form of beads by crosslinking polymerization of a metal polymerizable chelate, where the metal acts as a template. Upon leaching out the metal template, the crosslinked polymer is expected to leave cavities defined by the ligand functional group with enhanced selectivity for binding the template metal. We have demonstrated that lithium- and manganese-imprinted polymer beads can be used as selective solid sorbents for the extraction of lithium and manganese from brines. The polymers were tested both in batch extractions and packed bed lab-scale columns at temperatures of 45-100°C. Lithium-imprinted polymers were found to have Li + adsorption capacity as high as 2.8 mg Li +/g polymer at 45°C. Manganese-imprinted polymers were found to have a Mn 2+ adsorption capacity of more than 23 mg Mn 2+/g polymer at 75°C. The Li + extraction efficiency of the Li-imprinted polymer was found to be more that 95% when a brine containing 390 ppm Li +, 410 ppm Na +, and 390 ppm K + was passed through a packed bed of the polymer in a lab-scale column at 45°C. In brines containing 360 ppm Li +, 10,000 ppm Na +, and 3,000 ppm K +, the Li separation efficiency of the imprinted sorbent was found to be about 30% at 45°C. The Mn extraction efficiency of the Mn-imprinted polymer from a synthetic brine containing competing cations such as Li +, Na +, K +, Ca 2+, Mg 2+, and Ba 2+ was found to be 72% at 75°C in a lab-scale column. A preliminary process cost assessment for the recovery of lithium and production of lithium carbonate from geothermal brines was performed. We concluded that the total cost of a plant designed to process 6000 gal of brine/min is 20,456,265 with a total annual operating costs of $11,057,048 based on 300 days/year uptime. Assuming a conservative sale price of 2000/ton for Li 2CO 3, the annual revenue from the sale of Li 2CO 3 produced by this plant would exceed $40,000,000 at a production rate of 49Kg/min for geothermal fluids containing 400 ppm Li +.« less

Pore Fluid Extraction by Reactive Solitary Waves in 3-D

NASA Astrophysics Data System (ADS)

Omlin, Samuel; Malvoisin, Benjamin; Podladchikov, Yury Y.

2017-09-01

In the lower crust, viscous compaction is known to produce solitary porosity and fluid pressure waves. Metamorphic (de)volatilization reactions can also induce porosity changes in response to the propagating fluid pressure anomalies. Here we present results from high-resolution simulations using Graphic Processing Unit parallel processing with a model that includes both viscous (de)compaction and reaction-induced porosity changes. Reactive porosity waves propagate in a manner similar to viscous porosity waves, but through a different mechanism involving fluid release and trap in the solid by reaction. These waves self-generate from red noise or an ellipsoidal porosity anomaly with the same characteristic size and abandon their source region to propagate at constant velocity. Two waves traveling at different velocities pass through each other in a soliton-like fashion. Reactive porosity waves thus provide an additional mechanism for fluid extraction at shallow depths with implications for ore formation, diagenesis, metamorphic veins formation, and fluid extraction from subduction zones.

Isotopic characterisation of 3,4-methylenedioxyamphetamine and 3,4-methylenedioxymethylamphetamine (ecstasy).

PubMed

Carter, James F; Titterton, a Emma L; Murray, Martin; Sleeman, Richard

2002-06-01

Combined delta2H, delta13C and delta15N isotopic analysis of MDA and MDMA extracted from seized "ecstasy" tablets provides an isotopic "fingerprint" of the active ingredient allowing individual tablets to be linked to a common batch. Correlating these data with 2H NMR analysis of the extracts has the potential to study both the natural precursor materials and synthetic pathways used in the preparation of MDA and N-substituted homologues.

Automated multisyringe stir bar sorptive extraction using robust montmorillonite/epoxy-coated stir bars.

PubMed

Ghani, Milad; Saraji, Mohammad; Maya, Fernando; Cerdà, Víctor

2016-05-06

Herein we present a simple, rapid and low cost strategy for the preparation of robust stir bar coatings based on the combination of montmorillonite with epoxy resin. The composite stir bar was implemented in a novel automated multisyringe stir bar sorptive extraction system (MS-SBSE), and applied to the extraction of four chlorophenols (4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) as model compounds, followed by high performance liquid chromatography-diode array detection. The different experimental parameters of the MS-SBSE, such as sample volume, selection of the desorption solvent, desorption volume, desorption time, sample solution pH, salt effect and extraction time were studied. Under the optimum conditions, the detection limits were between 0.02 and 0.34μgL(-1). Relative standard deviations (RSD) of the method for the analytes at 10μgL(-1) concentration level ranged from 3.5% to 4.1% (as intra-day RSD) and from 3.9% to 4.3% (as inter-day RSD at 50μgL(-1) concentration level). Batch-to-batch reproducibility for three different stir bars was 4.6-5.1%. The enrichment factors were between 30 and 49. In order to investigate the capability of the developed technique for real sample analysis, well water, wastewater and leachates from a solid waste treatment plant were satisfactorily analyzed. Copyright © 2016 Elsevier B.V. All rights reserved.

Antioxidant effects of supercritical fluid garlic extracts in sunflower oil.

PubMed

Bravi, Elisabetta; Perretti, Giuseppe; Falconi, Caterina; Marconi, Ombretta; Fantozzi, Paolo

2017-01-01

Lipid oxidation causes changes in quality attributes of vegetable oils. Synthetic antioxidants have been used to preserve oils; however, there is interest in replacing them with natural ones. Garlic and its thiosulfinate compound allicin are known for their antioxidant activities. This study assesses a novel formulation, the supercritical fluid extract of garlic, on sunflower oil oxidation during an accelerated shelf-life test. Three quality parameters (free acidity, peroxide values, and p-anisidine values) were evaluated in each of the six oil samples. The samples included sunflower oil alone, sunflower oil supplemented with BHT, the undiluted supercritical fluid extract of garlic, and sunflower oils supplemented with three levels of garlic extract. The oils were also investigated for their antioxidant properties using the DPPH and the FRAP assays. The results were compared with the effect of the synthetic BHT. Our results underlined that the highest level of garlic extract may be superior, or at least comparable, with BHT in preserving sunflower oil. The oxidative degradation of oily samples can be limited by using supercritical fluid extract of garlic as it is a safe and an effective natural antioxidant formulation. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Coal fly ash interaction with environmental fluids: Geochemical and strontium isotope results from combined column and batch leaching experiments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brubaker, Tonya M; Stewart, Brian W; Capo, Rosemary C

2013-05-01

The major element and Sr isotope systematics and geochemistry of coal fly ash and its interactions with environmental waters were investigated using laboratory flow-through column leaching experiments (sodium carbonate, acetic acid, nitric acid) and sequential batch leaching experiments (water, acetic acid, hydrochloric acid). Column leaching of Class F fly ash samples shows rapid release of most major elements early in the leaching procedure, suggesting an association of these elements with soluble and surface bound phases. Delayed release of certain elements (e.g., Al, Fe, Si) signals gradual dissolution of more resistant silicate or glass phases as leaching continues. Strontium isotope resultsmore » from both column and batch leaching experiments show a marked increase in {sup 87}Sr/{sup 86}Sr ratio with continued leaching, yielding a total range of values from 0.7107 to 0.7138. For comparison, the isotopic composition of fluid output from a fly ash impoundment in West Virginia falls in a narrow range around 0.7124. The experimental data suggest the presence of a more resistant, highly radiogenic silicate phase that survives the combustion process and is leached after the more soluble minerals are removed. Strontium isotopic homogenization of minerals in coal does not always occur during the combustion process, despite the high temperatures encountered in the boiler. Early-released Sr tends to be isotopically uniform; thus the Sr isotopic composition of fly ash could be distinguishable from other sources and is a useful tool for quantifying the possible contribution of fly ash leaching to the total dissolved load in natural surface and ground waters.« less

CO 2-induced chemo-mechanical alteration in reservoir rocks assessed via batch reaction experiments and scratch testing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aman, Michael; Espinoza, D. Nicolas; Ilgen, Anastasia G.

Here, the injection of carbon dioxide (CO 2) into geological formations results in a chemical re-equilibration between the mineral assemblage and the pore fluid, with ensuing mineral dissolution and re-precipitation. Hence, target rock formations may exhibit changes of mechanical and petrophysical properties due to CO 2 exposure. We conducted batch reaction experiments with Entrada Sandstone and Summerville Siltstone exposed to de-ionized water and synthetic brine under reservoir pressure (9–10 MPa) and temperature (80°C) for up to four weeks. Samples originate from the Crystal Geyser field site, where a naturally occurring CO 2 seepage alters portions of these geologic formations. Wemore » conducted micro-scratch tests on rock samples without alteration, altered under laboratory conditions, and naturally altered over geologic time. Scratch toughness and hardness decrease as a function of exposure time and water salinity up to 52% in the case of Entrada and 87% in the case of Summerville after CO 2-induced alteration in the laboratory. Imaging of altered cores with SEM-EDS and X-ray microCT methods show dissolution of carbonate and silica cements and matrix accompanied by minor dissolution of Fe-oxides, clays, and other silicates. Parallel experiments using powdered samples confirm that dissolution of carbonate and silica are the primary reactions. The batch reaction experiments in the autoclave utilize a high fluid to rock volume ratio and represent an end member of possible alteration associated with CO 2 storage systems. These types of tests serve as a pre-screening tool to identify the susceptibility of rock facies to CO 2-related chemical-mechanical alteration during long-term CO 2 storage.« less

IN-PACKAGE CHEMISTRY ABSTRACTION

DOE Office of Scientific and Technical Information (OSTI.GOV)

E. Thomas

2005-07-14

This report was developed in accordance with the requirements in ''Technical Work Plan for Postclosure Waste Form Modeling'' (BSC 2005 [DIRS 173246]). The purpose of the in-package chemistry model is to predict the bulk chemistry inside of a breached waste package and to provide simplified expressions of that chemistry as a function of time after breach to Total Systems Performance Assessment for the License Application (TSPA-LA). The scope of this report is to describe the development and validation of the in-package chemistry model. The in-package model is a combination of two models, a batch reactor model, which uses the EQ3/6more » geochemistry-modeling tool, and a surface complexation model, which is applied to the results of the batch reactor model. The batch reactor model considers chemical interactions of water with the waste package materials, and the waste form for commercial spent nuclear fuel (CSNF) waste packages and codisposed (CDSP) waste packages containing high-level waste glass (HLWG) and DOE spent fuel. The surface complexation model includes the impact of fluid-surface interactions (i.e., surface complexation) on the resulting fluid composition. The model examines two types of water influx: (1) the condensation of water vapor diffusing into the waste package, and (2) seepage water entering the waste package as a liquid from the drift. (1) Vapor-Influx Case: The condensation of vapor onto the waste package internals is simulated as pure H{sub 2}O and enters at a rate determined by the water vapor pressure for representative temperature and relative humidity conditions. (2) Liquid-Influx Case: The water entering a waste package from the drift is simulated as typical groundwater and enters at a rate determined by the amount of seepage available to flow through openings in a breached waste package.« less

CO 2-induced chemo-mechanical alteration in reservoir rocks assessed via batch reaction experiments and scratch testing

DOE PAGES

Aman, Michael; Espinoza, D. Nicolas; Ilgen, Anastasia G.; ...

2017-09-22

Here, the injection of carbon dioxide (CO 2) into geological formations results in a chemical re-equilibration between the mineral assemblage and the pore fluid, with ensuing mineral dissolution and re-precipitation. Hence, target rock formations may exhibit changes of mechanical and petrophysical properties due to CO 2 exposure. We conducted batch reaction experiments with Entrada Sandstone and Summerville Siltstone exposed to de-ionized water and synthetic brine under reservoir pressure (9–10 MPa) and temperature (80°C) for up to four weeks. Samples originate from the Crystal Geyser field site, where a naturally occurring CO 2 seepage alters portions of these geologic formations. Wemore » conducted micro-scratch tests on rock samples without alteration, altered under laboratory conditions, and naturally altered over geologic time. Scratch toughness and hardness decrease as a function of exposure time and water salinity up to 52% in the case of Entrada and 87% in the case of Summerville after CO 2-induced alteration in the laboratory. Imaging of altered cores with SEM-EDS and X-ray microCT methods show dissolution of carbonate and silica cements and matrix accompanied by minor dissolution of Fe-oxides, clays, and other silicates. Parallel experiments using powdered samples confirm that dissolution of carbonate and silica are the primary reactions. The batch reaction experiments in the autoclave utilize a high fluid to rock volume ratio and represent an end member of possible alteration associated with CO 2 storage systems. These types of tests serve as a pre-screening tool to identify the susceptibility of rock facies to CO 2-related chemical-mechanical alteration during long-term CO 2 storage.« less

Quantitative determination of methamphetamine in oral fluid by liquid-liquid extraction and gas chromatography/mass spectrometry.

PubMed

Bahmanabadi, L; Akhgari, M; Jokar, F; Sadeghi, H B

2017-02-01

Methamphetamine abuse is one of the most medical and social problems many countries face. In spite of the ban on the use of methamphetamine, it is widely available in Iran's drug black market. There are many analytical methods for the detection of methamphetamine in biological specimen. Oral fluid has become a popular specimen to test for the presence of methamphetamine. The purpose of the present study was to develop a method for the extraction and detection of methamphetamine in oral fluid samples using liquid-liquid extraction (LLE) and gas chromatography/mass spectrometry (GC/MS) methods. An analytical study was designed in that blank and 50 authentic oral fluid samples were collected to be first extracted by LLE and subsequently analysed by GC/MS. The method was fully validated and showed an excellent intra- and inter-assay precision (reflex sympathetic dystrophy ˂ 10%) for external quality control samples. Recovery with LLE methods was 96%. Limit of detection and limit of quantitation were 5 and 15 ng/mL, respectively. The method showed high selectivity, no additional peak due to interfering substances in samples was observed. The introduced method was sensitive, accurate and precise enough for the extraction of methamphetamine from oral fluid samples in forensic toxicology laboratories.

Evaluation of activated sludge for biodegradation of propylene glycol as an aircraft deicing fluid.

PubMed

Delorit, Justin D; Racz, LeeAnn

2014-04-01

Aircraft deicing fluid used at airport facilities is often collected for treatment or disposal in order to prevent serious ecological threats to nearby surface waters. This study investigated lab scale degradation of propylene glycol, the active ingredient in a common aircraft deicing fluid, by way of a laboratory-scale sequencing batch reactor containing municipal waste water treatment facility activated sludge performing simultaneous organic carbon oxidation and nitrification. The ability of activated sludge to remove propylene glycol was evaluated by studying the biodegradation and sorption characteristics of propylene glycol in an activated sludge medium. The results indicate sorption may play a role in the fate of propylene glycol in AS, and the heterotrophic bacteria readily degrade this compound. Therefore, a field deployable bioreactor may be appropriate for use in flight line applications.

Metal speciation of environmental samples using SPE and SFC-AED analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mitchell, S.C.; Burford, M.D.; Robson, M.

1995-12-31

Due to growing public concern over heavy metals in the environment, soil, water and air particulate samples azre now routinely screened for their metal content. Conventional metal analysis typically involves acid digestion extraction and results in the generation of large aqueous and organic solvent waste. This harsh extraction process is usually used to obtain the total metal content of the sample, the extract being analysed by atomic emission or absorption spectroscoply techniques. A more selective method of metal extraction has been investigated which uses a supercritical fluid modified with a complexing agent. The relatively mild extraction method enables both organometallicmore » and inorganic metal species to be recovered intact. The various components from the supercritical fluid extract can be chromatographically separated using supercritical fluid chromatography (SFC) and positive identification of the metals achieved using atomic emission detection (AED). The aim of the study is to develop an analytical extraction procedure which enables a rapid, sensitive and quantitative analysis of metals in environmental samples, using just one extraction (eg SFE) and one analysis (eg SFC-AED) procedure.« less

Recovery of Oil with Unsaturated Fatty Acids and Polyphenols from Chaenomelessinensis (Thouin) Koehne: Process Optimization of Pilot-Scale Subcritical Fluid Assisted Extraction.

PubMed

Zhu, Zhenzhou; Zhang, Rui; Zhan, Shaoying; He, Jingren; Barba, Francisco J; Cravotto, Giancarlo; Wu, Weizhong; Li, Shuyi

2017-10-22

The potential effects of three modern extraction technologies (cold-pressing, microwaves and subcritical fluids) on the recovery of oil from Chaenomelessinensis (Thouin) Koehne seeds have been evaluated and compared to those of conventional chemical extraction methods (Soxhlet extraction). This oil contains unsaturated fatty acids and polyphenols. Subcritical fluid extraction (SbFE) provided the highest yield-25.79 g oil/100 g dry seeds-of the three methods. Moreover, the fatty acid composition in the oil samples was analysed using gas chromatography-mass spectrometry. This analysis showed that the percentages of monounsaturated (46.61%), and polyunsaturated fatty acids (42.14%), after applying SbFE were higher than those obtained by Soxhlet, cold-pressing or microwave-assisted extraction. In addition, the oil obtained under optimized SbFE conditions (35 min extraction at 35 °C with four extraction cycles), showed significant polyphenol (527.36 mg GAE/kg oil), and flavonoid (15.32 mg RE/kg oil), content, had a good appearance and was of high quality.

L-Lactic Acid Production by Lactobacillus rhamnosus ATCC 10863

PubMed Central

Senedese, Ana Lívia Chemeli; Maciel Filho, Rubens; Maciel, Maria Regina Wolf

2015-01-01

Lactic acid has been shown to have the most promising application in biomaterials as poly(lactic acid). L. rhamnosus ATCC 10863 that produces L-lactic acid was used to perform the fermentation and molasses was used as substrate. A solution containing 27.6 g/L of sucrose (main composition of molasses) and 3.0 g/L of yeast extract was prepared, considering the final volume of 3,571 mL (14.0% (v/v) inoculum). Batch and fed batch fermentations were performed with temperature of 43.4°C and pH of 5.0. At the fed batch, three molasses feed were applied at 12, 24, and 36 hours. Samples were taken every two hours and the amounts of lactic acid, sucrose, glucose, and fructose were determined by HPLC. The sucrose was barely consumed at both processes; otherwise the glucose and fructose were almost entirely consumed. 16.5 g/L of lactic acid was produced at batch and 22.0 g/L at fed batch. Considering that lactic acid was produced due to the low concentration of the well consumed sugars, the final amount was considerable. The cell growth was checked and no substrate inhibition was observed. A sucrose molasses hydrolysis is suggested to better avail the molasses fermentation with this strain, surely increasing the L-lactic acid. PMID:25922852

Physicochemical Characteristics of Transferon™ Batches

PubMed Central

Pérez-Sánchez, Gilberto; Favari, Liliana; Estrada-Parra, Sergio

2016-01-01

Transferon, a biotherapeutic agent that has been used for the past 2 decades for diseases with an inflammatory component, has been approved by regulatory authorities in Mexico (COFEPRIS) for the treatment of patients with herpes infection. The active pharmaceutical ingredient (API) of Transferon is based on polydispersion of peptides that have been extracted from lysed human leukocytes by a dialysis process and a subsequent ultrafiltration step to select molecules below 10 kDa. To physicochemically characterize the drug product, we developed chromatographic methods and an SDS-PAGE approach to analyze the composition and the overall variability of Transferon. Reversed-phase chromatographic profiles of peptide populations demonstrated batch-to-batch consistency from 10 representative batches that harbored 4 primary peaks with a relative standard deviation (RSD) of less than 7%. Aminogram profiles exhibited 17 proteinogenic amino acids and showed that glycine was the most abundant amino acid, with a relative content of approximately 18%. Further, based on their electrophoretic migration, the peptide populations exhibited a molecular mass of about 10 kDa. Finally, we determined the Transferon fingerprint using a mass spectrometry tool. Because each batch was produced from independent pooled buffy coat samples from healthy donors, supplied by a local blood bank, our results support the consistency of the production of Transferon and reveal its peptide identity with regard to its physicochemical attributes. PMID:27525277

Fluid sampling system for a nuclear reactor

DOEpatents

Lau, Louis K.; Alper, Naum I.

1994-01-01

A system of extracting fluid samples, either liquid or gas, from the interior of a nuclear reactor containment utilizes a jet pump. To extract the sample fluid, a nonradioactive motive fluid is forced through the inlet and discharge ports of a jet pump located outside the containment, creating a suction that draws the sample fluid from the containment through a sample conduit connected to the pump suction port. The mixture of motive fluid and sample fluid is discharged through a return conduit to the interior of the containment. The jet pump and means for removing a portion of the sample fluid from the sample conduit can be located in a shielded sample grab station located next to the containment. A non-nuclear grade active pump can be located outside the grab sampling station and the containment to pump the nonradioactive motive fluid through the jet pump.

Fluid sampling system for a nuclear reactor

DOEpatents

Lau, L.K.; Alper, N.I.

1994-11-22

A system of extracting fluid samples, either liquid or gas, from the interior of a nuclear reactor containment utilizes a jet pump. To extract the sample fluid, a nonradioactive motive fluid is forced through the inlet and discharge ports of a jet pump located outside the containment, creating a suction that draws the sample fluid from the containment through a sample conduit connected to the pump suction port. The mixture of motive fluid and sample fluid is discharged through a return conduit to the interior of the containment. The jet pump and means for removing a portion of the sample fluid from the sample conduit can be located in a shielded sample grab station located next to the containment. A non-nuclear grade active pump can be located outside the grab sampling station and the containment to pump the nonradioactive motive fluid through the jet pump. 1 fig.

[Study on supercritical CO2 extraction of xiaoyaosan and its GC-MS fingerprint].

PubMed

Zuo, Ya-Mei; Tian, Jun-Sheng; Guo, Xiao-Qing; Zhou, Yu-Zhi; Gao, Xiao-Xia; Qin, Xue-Mei

2014-02-01

To determine the optimum conditions of supercritical CO2 extraction of Xiaoyaosan, and establish its fingerprint by gas chromatography-mass spectrometry (GC-MS), the yield of extract were investigated, an orthogonal test was used to quantify the effects of extraction temperature, pressure, CO2 flow rate and time, and fingerprint analysis of different batches of extracts were by GC-MS. The optimal extraction conditions were determined as follows: extraction pressure 20 MPa, extraction temperature 50 degrees C, CO2 flow rate 25 kg x h(-1), extraction time 3 h, and average yield 2.2%. The GC-MS fingerprint was established and 27 common peaks were found, whose contents add up to 81.89% of the total peak area. Among them, 21 compounds were identified, accounting for 53.20% of the total extract. The extraction process is reasonable and favorable for industrial production. The GC-MS method is accurate, reliable, reproducible, and can be used for quality control of supercritical CO2 extract from Xiaoyaosan.

Automated Fluid Feature Extraction from Transient Simulations

NASA Technical Reports Server (NTRS)

Haimes, Robert; Lovely, David

1999-01-01

In the past, feature extraction and identification were interesting concepts, but not required to understand the underlying physics of a steady flow field. This is because the results of the more traditional tools like iso-surfaces, cuts and streamlines were more interactive and easily abstracted so they could be represented to the investigator. These tools worked and properly conveyed the collected information at the expense of much interaction. For unsteady flow-fields, the investigator does not have the luxury of spending time scanning only one "snap-shot" of the simulation. Automated assistance is required in pointing out areas of potential interest contained within the flow. This must not require a heavy compute burden (the visualization should not significantly slow down the solution procedure for co-processing environments like pV3). And methods must be developed to abstract the feature and display it in a manner that physically makes sense. The following is a list of the important physical phenomena found in transient (and steady-state) fluid flow: (1) Shocks, (2) Vortex cores, (3) Regions of recirculation, (4) Boundary layers, (5) Wakes. Three papers and an initial specification for the (The Fluid eXtraction tool kit) FX Programmer's guide were included. The papers, submitted to the AIAA Computational Fluid Dynamics Conference, are entitled : (1) Using Residence Time for the Extraction of Recirculation Regions, (2) Shock Detection from Computational Fluid Dynamics results and (3) On the Velocity Gradient Tensor and Fluid Feature Extraction.

Development of new critical fluid-based processing methods for nutraceuticals and natural products

DOE Office of Scientific and Technical Information (OSTI.GOV)

King, J. W.

2004-01-01

The development of new supercritical fluid processing technology as applied to nutraceuticals and natural products is no longer confined to using just supercritical fluid extraction (SFE) and supercritical carbon dioxide (SC-CO{sub 2}). Recently reported advances have been focused on modifying natural products and improving functionality of an end product using newer experimental techniques and fluid phases. In this presentation four focus areas will be emphasized: (1) control of particle size/morphology and encapsulation of the nutraceutical ingredients, (2) the use of combinatorial methodology to optimize critical fluid processing, (3) application of sub-critical water as a complementary medium for processing natural products,more » and (4) an assessment of the current state of products and processing which use critical fluid to produce nutraceutical and natural products for the food and cosmetic marketplace. Application of the various particle fomiation processes conducted in the presence of critical fluid media, such as: CPF, SAS, DELOS, RESS, PGSS, and GAS, can be used to produce particles of small and uniform distribution, having unique morphologies, that facilitate rapid dissolution or sustained release of many nutraceutical ingredients. These substances have included: therapeutic spices, phystosterols, vitamins, phospholpids, and carotenoids. Accelerating the development of critical fluid processing has been the application of combinatorial methodology to optimize extraction, fractionation, and/or reactions in near-, SC-, or subcritical fluid media. This is frequently accomplished by using sequential or multichannel automated instrumentation that was originally designed for analytical purposes. Several examples will be provided of rapidly assessing the extraction of anthocyanins with sub-critical water and the SFE of natural products. However, differences do exist in conducting experiments on the above instrumentation vs. scaled-up continuous processes, which will be noted. Sub-critical water is finding increase use as an extraction/fractionation or reaction medium. The literature reports applications for the extraction spices, natural antioxidants (rosemary, anthocyanins, etc.), and herbal components (tea and coffee ingredients), Our studies and the literature provide adequate correlations of solute solubility in sub-critical water as well as models for the kinetics of extraction in this medium. Finally, the current state of critical fluid technology as applied to natural products and nutraceuticals will be assessed; noting specific processes, organizations, and products that exist.« less

Efficient production of l-lactic acid from hydrolysate of Jerusalem artichoke with immobilized cells of Lactococcus lactis in fibrous bed bioreactors.

PubMed

Shi, Zhouming; Wei, Peilian; Zhu, Xiangcheng; Cai, Jin; Huang, Lei; Xu, Zhinan

2012-10-10

Hydrolysate of Jerusalem artichoke was applied for the production of l-lactic acid by immobilized Lactococcus lactis cells in a fibrous bed bioreactor system. Preliminary experiments had indicated that the high quality hydrolysate, which was derived from the 40 min acid treatment at 95 °C and pH 1.8, was sufficient to support the cell growth and synthesis of l-lactic acid. With the addition of 5 g/l yeast extract, the fermentative performance of free cell system was evidently improved. After the basal settlement of hydrolysate based fermentation, the batch mode and the fed-batch mode fermentation were carried out in the free cell system and the fibrous bed bioreactor system, respectively. In all cases the immobilized cells presented the superior ability to produce l-lactic acid. The comparison of batch mode and fed-batch mode also indicated that the growth-limiting feeding strategy could reduce the lag phase of fermentation process and enhance the production of l-lactic acid. The achieved maximum concentration of l-lactic acid was 142 g/l in the fed-batch mode. Subsequent repeated-batch fermentation of the fibrous bed bioreactor system had further exhibited the persistence and stability of this system for the high production of l-lactic acid in a long term. Our work suggested the great potential of the fibrous bed bioreactor system and hydrolysate of J. artichoke in the economical production of l-lactic acid at industrial scale. Copyright © 2012 Elsevier Inc. All rights reserved.

A short term quality control tool for biodegradable microspheres.

PubMed

D'Souza, Susan; Faraj, Jabar A; Dorati, Rossella; DeLuca, Patrick P

2014-06-01

Accelerated in vitro release testing methodology has been developed as an indicator of product performance to be used as a discriminatory quality control (QC) technique for the release of clinical and commercial batches of biodegradable microspheres. While product performance of biodegradable microspheres can be verified by in vivo and/or in vitro experiments, such evaluation can be particularly challenging because of slow polymer degradation, resulting in extended study times, labor, and expense. Three batches of Leuprolide poly(lactic-co-glycolic acid) (PLGA) microspheres having varying morphology (process variants having different particle size and specific surface area) were manufactured by the solvent extraction/evaporation technique. Tests involving in vitro release, polymer degradation and hydration of the microspheres were performed on the three batches at 55°C. In vitro peptide release at 55°C was analyzed using a previously derived modification of the Weibull function termed the modified Weibull equation (MWE). Experimental observations and data analysis confirm excellent reproducibility studies within and between batches of the microsphere formulations demonstrating the predictability of the accelerated experiments at 55°C. The accelerated test method was also successfully able to distinguish the in vitro product performance between the three batches having varying morphology (process variants), indicating that it is a suitable QC tool to discriminate product or process variants in clinical or commercial batches of microspheres. Additionally, data analysis utilized the MWE to further quantify the differences obtained from the accelerated in vitro product performance test between process variants, thereby enhancing the discriminatory power of the accelerated methodology at 55°C.

Impact of Nisin-Activated Packaging on Microbiota of Beef Burgers during Storage.

PubMed

Ferrocino, Ilario; Greppi, Anna; La Storia, Antonietta; Rantsiou, Kalliopi; Ercolini, Danilo; Cocolin, Luca

2016-01-15

Beef burgers were stored at 4°C in a vacuum in nisin-activated antimicrobial packaging. Microbial ecology analyses were performed on samples collected between days 0 and 21 of storage to discover the population diversity. Two batches were analyzed using RNA-based denaturing gradient gel electrophoresis (DGGE) and pyrosequencing. The active packaging retarded the growth of the total viable bacteria and lactic acid bacteria. Culture-independent analysis by pyrosequencing of RNA extracted directly from meat showed that Photobacterium phosphoreum, Lactococcus piscium, Lactobacillus sakei, and Leuconostoc carnosum were the major operational taxonomic units (OTUs) shared between control and treated samples. Beta diversity analysis of the 16S rRNA sequence data and RNA-DGGE showed a clear separation between two batches based on the microbiota. Control samples from batch B showed a significant high abundance of some taxa sensitive to nisin, such as Kocuria rhizophila, Staphylococcus xylosus, Leuconostoc carnosum, and Carnobacterium divergens, compared to control samples from batch A. However, only from batch B was it possible to find a significant difference between controls and treated samples during storage due to the active packaging. Predicted metagenomes confirmed differences between the two batches and indicated that the use of nisin-based antimicrobial packaging can determine a reduction in the abundance of specific metabolic pathways related to spoilage. The present study aimed to assess the viable bacterial communities in beef burgers stored in nisin-based antimicrobial packaging, and it highlights the efficacy of this strategy to prolong beef burger shelf life. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Batch and fixed-bed column studies for biosorption of Zn(II) ions onto pongamia oil cake (Pongamia pinnata) from biodiesel oil extraction.

PubMed

Shanmugaprakash, M; Sivakumar, V

2015-12-01

The present work, analyzes the potential of defatted pongamia oil cake (DPOC) for the biosorption of Zn(II) ions from aqueous solutions in the both batch and column mode. Batch experiments were conducted to evaluate the optimal pH, effect of adsorbent dosage, initial Zn(II) ions concentration and contact time. The biosorption equilibrium and kinetics data for Zn(II) ions onto the DPOC were studied in detail, using several models, among all it was found to be that, Freundlich and the second-order model explained the equilibrium data well. The calculated thermodynamic parameters had shown that the biosorption of Zn(II) ions was exothermic and spontaneous in nature. Batch desorption studies showed that the maximum Zn(II) recovery occurred, using 0.1 M EDTA. The Bed Depth Service Time (BDST) and the Thomas model was successfully employed to evaluate the model parameters in the column mode. The results indicated that the DPOC can be applied as an effective and eco-friendly biosorbent for the removal of Zn(II) ions in polluted wastewater. Copyright © 2015 Elsevier Ltd. All rights reserved.

Determination of gas volume trapped in a closed fluid system

NASA Technical Reports Server (NTRS)

Hunter, W. F.; Jolley, J. E.

1971-01-01

Technique involves extracting known volume of fluid and measuring system before and after extraction, volume of entrapped gas is then computed. Formula derived from ideal gas laws is basis of this method. Technique is applicable to thermodynamic cycles and hydraulic systems.

Supercritical Fluid Extraction versus Traditional Solvent Extraction of Caffeine from Tea Leaves: A Laboratory-Based Case Study for an Organic Chemistry Course

ERIC Educational Resources Information Center

Schaber, Peter M.; Larkin, Judith E.; Pines, Harvey A.; Berchou, Kelly; Wierchowski, Elizabeth; Marconi, Andrew; Suriani, Allison

2012-01-01

In this case-based laboratory, an instrument sales person attempts to convince an analysis laboratory of the virtues of supercritical fluid extraction (SFE). The sales person deals directly with the laboratory technicians who will make the decision. Arrangements are made to have SFE instrumentation brought into the laboratory for a comparative…

Pressurised fluid extraction of bupirimate and ethirimol from aged soils.

PubMed

Fitzpatrick, L J; Dean, J R

2001-05-25

This paper assesses the effect of pressurised fluid extraction (PFE) on the recovery of bupirimate and its degradation product, ethirimol from a range of soil types. The analytes were extracted under standard conditions (pressure, 2000 p.s.i.; temperature, 100 degrees C; and, three static flush cycles of 5 min static extraction time each) using a variety of individual and combined solvents. It was found that the recovery of bupirimate was dependent upon the organic matter content of soil.

Submersible pumping system with heat transfer mechanism

DOEpatents

Hunt, Daniel Francis Alan; Prenger, F. Coyne; Hill, Dallas D; Jankowski, Todd Andrew

2014-04-15

A submersible pumping system for downhole use in extracting fluids containing hydrocarbons from a well. In one embodiment, the pumping system comprises a rotary induction motor, a motor casing, one or more pump stages, and a cooling system. The rotary induction motor rotates a shaft about a longitudinal axis of rotation. The motor casing houses the rotary induction motor such that the rotary induction motor is held in fluid isolation from the fluid being extracted. The pump stages are attached to the shaft outside of the motor casing, and are configured to impart fluid being extracted from the well with an increased pressure. The cooling system is disposed at least partially within the motor casing, and transfers heat generated by operation of the rotary induction motor out of the motor casing.

Insights Gained from the Dehalococcoides ethenogenes Strain 195’s Transcriptome Responding to a Wide Range of Respiration Rates and Substrate Types

DTIC Science & Technology

2012-04-01

fermented yeast , pure hydrogen, or endogenous biomass decay). When similarly respiring (~120 ?eeq PCE/(L-hr)) batch and PSS cultures were contrasted, the...electron equivalence (eeq) basis), and electron donor type (butyrate, lactate, yeast extract, fermented yeast , pure hydrogen, or endogenous biomass...acceptor ratios (0.7 to 17 on an electron equivalence (eeq) basis), and 12 electron donor type (butyrate, lactate, yeast extract, fermented yeast , pure

Parameters optimization of supercritical fluid-CO2 extracts of frankincense using response surface methodology and its pharmacodynamics effects.

PubMed

Zhou, Jing; Ma, Xing-miao; Qiu, Bi-Han; Chen, Jun-xia; Bian, Lin; Pan, Lin-mei

2013-01-01

The volatile oil parts of frankincense (Boswellia carterii Birdw.) were extracted with supercritical carbon dioxide under constant pressure (15, 20, or 25 MPa) and fixed temperature (40, 50, or 60°C), given time (60, 90, or 120 min) aiming at the acquisition of enriched fractions containing octyl acetate, compounds of pharmaceutical interest. A mathematical model was created by Box-Behnken design, a popular template for response surface methodology, for the extraction process. The response value was characterized by synthetical score, which comprised yields accounting for 20% and content of octyl acetate for 80%. The content of octyl acetate was determined by GC. The supercritical fluid extraction showed higher selectivity than conventional steam distillation. Supercritical fluid-CO(2) for extracting frankincense under optimum condition was of great validity, which was also successfully verified by the pharmacological experiments. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

9 CFR 319.721 - Fluid extract of meat.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 9 Animals and Animal Products 2 2010-01-01 2010-01-01 false Fluid extract of meat. 319.721 Section 319.721 Animals and Animal Products FOOD SAFETY AND INSPECTION SERVICE, DEPARTMENT OF AGRICULTURE... Beef”) shall contain not more than 50 percent of moisture. ...

9 CFR 319.721 - Fluid extract of meat.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 9 Animals and Animal Products 2 2012-01-01 2012-01-01 false Fluid extract of meat. 319.721 Section 319.721 Animals and Animal Products FOOD SAFETY AND INSPECTION SERVICE, DEPARTMENT OF AGRICULTURE... Beef”) shall contain not more than 50 percent of moisture. ...

9 CFR 319.721 - Fluid extract of meat.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 9 Animals and Animal Products 2 2014-01-01 2014-01-01 false Fluid extract of meat. 319.721 Section 319.721 Animals and Animal Products FOOD SAFETY AND INSPECTION SERVICE, DEPARTMENT OF AGRICULTURE... Beef”) shall contain not more than 50 percent of moisture. ...

9 CFR 319.721 - Fluid extract of meat.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 9 Animals and Animal Products 2 2013-01-01 2013-01-01 false Fluid extract of meat. 319.721 Section 319.721 Animals and Animal Products FOOD SAFETY AND INSPECTION SERVICE, DEPARTMENT OF AGRICULTURE... Beef”) shall contain not more than 50 percent of moisture. ...

9 CFR 319.721 - Fluid extract of meat.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 9 Animals and Animal Products 2 2011-01-01 2011-01-01 false Fluid extract of meat. 319.721 Section 319.721 Animals and Animal Products FOOD SAFETY AND INSPECTION SERVICE, DEPARTMENT OF AGRICULTURE... Beef”) shall contain not more than 50 percent of moisture. ...

Assessment of Supercritical Fluid Extraction Use in Whole Sediment Toxicity Identification Evaluations

EPA Science Inventory

In this investigation, supercritical fluid extraction (SFE) with pure CO2 was assessed as a confirmatory tool in Phase III of whole sediment toxicity identification evaluations (TIEs). The SFE procedure was assessed on two reference sediments and three contaminated sediments usi...

Application of FTA technology to extraction of sperm DNA from mixed body fluids containing semen.

PubMed

Fujita, Yoshihiko; Kubo, Shin-ichi

2006-01-01

FTA technology is a novel method designed to simplify the collection, shipment, archiving and purification of nucleic acids from a wide variety of biological sources. In this study, we report a rapid and simple method of extracting DNA from sperm when body fluids mixed with semen were collected using FTA cards. After proteinase K digestion of the sperm and body fluid mixture, the washed pellet suspension as the sperm fraction and the concentrated supernatant as the epithelial cell fraction were respectively applied to FTA cards containing DTT. The FTA cards were dried, then directly added to a polymerase chain reaction (PCR) mix and processed by PCR. The time required from separation of the mixed fluid into sperm and epithelial origin DNA extractions was only about 2.5-3h. Furthermore, the procedure was extremely simple. It is considered that our designed DNA extraction procedure using an FTA card is available for application to routine work.

Actinide and lanthanide separation process (ALSEP)

DOEpatents

Guelis, Artem V.

2013-01-15

The process of the invention is the separation of minor actinides from lanthanides in a fluid mixture comprising, fission products, lanthanides, minor actinides, rare earth elements, nitric acid and water by addition of an organic chelating aid to the fluid; extracting the fluid with a solvent comprising a first extractant, a second extractant and an organic diluent to form an organic extractant stream and an aqueous raffinate. Scrubbing the organic stream with a dicarboxylic acid and a chelating agent to form a scrubber discharge. The scrubber discharge is stripped with a simple buffering agent and a second chelating agent in the pH range of 2.5 to 6.1 to produce actinide and lanthanide streams and spent organic diluents. The first extractant is selected from bis(2-ethylhexyl)hydrogen phosphate (HDEHP) and mono(2-ethylhexyl)2-ethylhexyl phosphonate (HEH(EHP)) and the second extractant is selected from N,N,N,N-tetra-2-ethylhexyl diglycol amide (TEHDGA) and N,N,N',N'-tetraoctyl-3-oxapentanediamide (TODGA).

Genetic significance of the 867 cm- 1 out-of-plane Raman mode in graphite associated with V-bearing green grossular

NASA Astrophysics Data System (ADS)

Thomas, Rainer; Rericha, Adolf; Pohl, Walter L.; Davidson, Paul

2018-03-01

SE Kenya is the world's largest producer of green vanadium grossular gemstones (tsavorite). Samples from one of the mines near Mwatate, and of occurrences in Tanzania yielded remarkable new insights into the genesis of tsavorite. Graphite is intimately associated with V-grossular and is one of the keys to understanding its origin. In the course of this study we found five different types of graphite. Surprisingly, in one graphite type the "Raman-forbidden" and IR-active 867 cm- 1 band was observed. In this communication, we attempt to find an explanation for this unusual phenomenon. Additionally, our observations also address some of the issues pertaining to the origin of the green grossular-dominated rocks (grossularites), as well as the gem quality tsavorite crystals, since we propose that the anomalous spectroscopic behavior of the graphite is related to the unusual conditions during crystallization of both the grossular and graphite from a near-supercritical volatile- and sulfur-rich silicate melt. The massive green vanadium grossular contains abundant unequivocal crystallized melt inclusions, while the transparent gem quality grossular (tsavorite) displays only fluid inclusions. On the basis of inclusion studies we suggest that anatectic melts originated in the peculiar evaporitic host lithology of the tsavorite deposits. Near peak metamorphic temperatures ( 700 °C) these liquids occurred as a supercritical volatile-rich "fluid/melt phase" characterized by complete miscibility between H2O and silicate liquid. Relatively dry liquid batches precipitated non-transparent green grossular, whereas wet batches segregated fluids that formed transparent tsavorite.

Supercritical Fluid Extraction of Toxic Heavy Metals and Uranium from Acidic Solutions with Sulfur-Containing Organophosphorus Reagents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Yuehe; Liu, Chongxuan; Wu, Hong

2003-03-02

The feasibility of using sulfur-containing organophosphorus reagents for the chelation-supercritical fluid extraction (SFE) of toxic heavy metals and uranium from acidic media was investigated. The SFE experiments were conducted in a specially-designed flow-through liquid extractor. Effective extraction of the metal ions from various acidic media was demonstrated. The effect of ligand concentration in supercritical CO{sub 2} on the kinetics of metal extraction was studied. A simplified model is used to describe the extraction kinetics and the good agreement of experimental data with the equilibrium-based model is achieved.

Sorptive extraction using polydimethylsiloxane/metal-organic framework coated stir bars coupled with high performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

PubMed

Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

2014-08-22

In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

CO2-assisted phosphorus extraction from poultry litter and selective recovery of struvite and potassium struvite.

PubMed

Shashvatt, Utsav; Benoit, Josh; Aris, Hannah; Blaney, Lee

2018-06-18

Phosphorus recovery from industrialized poultry operations is necessary to ensure sustainable waste management and resource consumption. To realize these goals, an innovative, two-stage process chemistry has been developed to extract nutrients from poultry litter and recover value-added products. Over 75% phosphorus extraction was achieved by bubbling carbon dioxide into poultry litter slurries and adding strong acid to reach pH 4.5-5.5. After separating the nutrient-deficient poultry litter solids and the nutrient-rich liquid, the extract pH was increased through aeration and strong base addition. Over 95% of the extracted phosphorus was recovered as solid precipitate at pH 8.5-9.0. High-purity struvite and potassium struvite products were selectively recovered through pH control, introduction of a calcium-complexing agent, and addition of magnesium chloride. The nitrogen-to-phosphorus-to-potassium (NPK) ratio of the recovered solids was controlled through aeration and pH adjustment. Precipitation at pH 8.5-9.0 and 10.5-11.0 resulted in NPK ratios of 2.0:1.0:0.1 and 0.9:1.0:0.2, respectively. The process effluent was effectively recycled as makeup water for the subsequent batch of poultry litter, thereby decreasing water consumption and increasing overall nutrient recovery. Sequencing batch operation yielded greater than 70% phosphorus recovery within a 45-min process, demonstrating the potential for this technology to alleviate nutrient pollution in agricultural settings and generate an alternative supply of phosphorus fertilizers. Copyright © 2018. Published by Elsevier Ltd.

Flow-through dynamic microextraction system for automatic in vitro assessment of chyme bioaccessibility in food commodities.

PubMed

Souza, Lais A; Rosende, María; Korn, Maria Graças A; Miró, Manuel

2018-10-05

An automatic flow-through dynamic extraction method is proposed for the first time for in vitro exploration, with high temporal resolution, of the transit of the chyme from the gastric to the duodenal compartment using the Versantvoort's fed-state physiologically relevant extraction test. The flow manifold was coupled on-line to an inductively coupled plasma optical emission spectrometer (ICP OES) for real-time elucidation of the bioaccessible elemental fraction of micronutrients (viz., Cu, Fe and Mn) in food commodities across the gastrointestinal tract. The simulated intestinal and bile biofluid (added to the gastric phase) was successively pumped at 1.0 mL min -1 through a large-bore column (maintained at 37.0 ± 2.0 °C) initially loaded with a weighed amount of linseed (250 mg) using a PVDF filter membrane (5.0 μm pore size) for retaining of the solid sample and in-line filtration of the extracts. The lack of bias (trueness) of the on-line gastrointestinal extraction method coupled to ICP OES was confirmed using mass balance validation following microwave assisted digestion of the residual (non-bioaccessible) elemental fraction. Mass balance validation yielded absolute recoveries spanning from 79 to 121% for the overall analytes and samples. On-line dynamic extraction was critically appraised against batch counterparts for both gastric and gastrointestinal compartments. Due to the lack of consensus in the literature regarding the agitation method for batch oral bioaccessibility testing, several extraction approaches (viz., magnetic stirring, end-over-end rotation and orbital shaking) were evaluated. Improved gastric extractability of Fe along with bioaccessible data comparable to the dynamic counterpart based on the continuous displacement of the extraction equilibrium was obtained with batchwise magnetic stirring, which is deemed most appropriate for ascertaining worst-case/maximum bioaccessibility scenarios. Copyright © 2018 Elsevier B.V. All rights reserved.

Novel method for screening of enteric film coatings properties with magnetic resonance imaging.

PubMed

Dorożyński, Przemysław; Jamróz, Witold; Niwiński, Krzysztof; Kurek, Mateusz; Węglarz, Władysław P; Jachowicz, Renata; Kulinowski, Piotr

2013-11-18

The aim of the study is to present the concept of novel method for fast screening of enteric coating compositions properties without the need of preparation of tablets batches for fluid bed coating. Proposed method involves evaluation of enteric coated model tablets in specially designed testing cell with application of MRI technique. The results obtained in the testing cell were compared with results of dissolution studies of mini-tablets coated in fluid bed apparatus. The method could be useful in early stage of formulation development for screening of film coating properties that will shorten and simplify the development works. Copyright © 2013 Elsevier B.V. All rights reserved.

Potential Transport and Degradation of “Aged” Pesticide Residues in Soil

USDA-ARS?s Scientific Manuscript database

Increased pesticide residence time in soil, or “aging”, has been shown to affect the sorption-desorption of pesticides in the soil, which in turn can control transport and degradation processes. Aging effects have been characterized by batch sequential extraction methods, in which sorption coefficie...

Potential transport and degradation of “Aged” pesticide residues in soil

USDA-ARS?s Scientific Manuscript database

“Aging” has been shown to affect the sorption-desorption of pesticides in the soil, which in turn can control transport and degradation processes. Aging effects have been characterized by batch sequential extraction methods, in which sorption coefficients (i.e. Kd) are determined for the chemical re...

EMERGING TECHNOLOGY BULLETIN: PROCESS FOR THE TREATMENT OF VOLATILE ORGANIC CARBON AND HEAVY-METAL- CONTAMINATED SOIL - INTERNATIONAL TECHNOLOGY CORPORATION

EPA Science Inventory

The batch steam distillation and metal extraction treatment process is a two-stage system that treats soils contaminated with organics and inorganics. This system uses conventional, readily available process equipment, and does not produce hazardous combustion products. Hazar...

SigmaPlot 2000, Version 6.00, SPSS Inc. Computer Software Test Plan

DOE Office of Scientific and Technical Information (OSTI.GOV)

HURLBUT, S.T.

2000-10-24

SigmaPlot is a vendor software product used in conjunction with the supercritical fluid extraction Fourier transform infrared spectrometer (SFE-FTIR) system. This product converts the raw spectral data to useful area numbers. SigmaPlot will be used in conjunction with procedure ZA-565-301, ''Determination of Moisture by Supercritical Fluid Extraction and Infrared Detection.'' This test plan will be performed in conjunction with or prior to HNF-6936, ''HA-53 Supercritical Fluid Extraction System Acceptance Test Plan'', to perform analyses for water. The test will ensure that the software can be installed properly and will manipulate the analytical data correctly.

Supercritical CO(2) fluid extraction of crystal water from trehalose dihydrate. Efficient production of form II (T(alpha)) phase.

PubMed

Akao, Ken-ichi; Okubo, Yusei; Inoue, Yoshio; Sakurai, Minoru

2002-10-11

Form II is a kind of metastable crystalline form of trehalose anhydrate, and it is easily converted to the dihydrate crystal by absorbing water in moist atmosphere at room temperature (Akao et al., Carbohydr. Res. 2001, 334, 233-241). It can be utilized as an edible and nontoxic desiccant, and thus its efficient production from the dihydrate is significant from a viewpoint of industrial applications. In this study, we attempt to extract crystal water from the dihydrate using supercritical CO(2). We examine the dependence of extraction efficiency on the extraction time, the temperature and pressure of the fluid. Then, FTIR measurements are carried out to detect the extracted water and to identify the polymorphic phase of the sugar sample after the extraction treatment. In particular, the so-called first derivative euclidean distance analysis for IR spectra is shown to be quite useful for the structural identification. Consequently, we demonstrate that form II is produced from the dihydrate through supercritical CO(2) fluid extraction if appropriate temperature and pressure conditions (around 80 degrees C and 20 MPa) are maintained.

The use of tannin from chestnut (Castanea vesca).

PubMed

Krisper, P; Tisler, V; Skubic, V; Rupnik, I; Kobal, S

1992-01-01

After mimosa and quebracho extracts, chestnut extract is the third most important vegetable tannin used for leather production. It is produced only in Europe on the northern side of the Mediterranean sea. The extract is prepared by hot water extraction of the bark and timber, followed by spray-drying of the solution. Analysis shows that there are insignificant variations in extract quality between batches, so the extract can be used with modern automated leather production systems. The extract contains approximately 75 percent active tanning substances. The primary component is castalagin, along with smaller amounts of vescalagin, castalin, and vescalin. A castalagin-based pharmaceutical product is currently in use for prevention and treatment of diarrhea in pigs and cattle that is caused by changes in diet. The beneficial effect is due to prevention of water losses through mucous membranes. The castalagin may also form chelates with iron, which influences the reabsorption of the metal in the animal digestive tract.

Effect of saliva stabilisers on detection of porcine reproductive and respiratory syndrome virus in oral fluid by quantitative reverse transcriptase real-time PCR.

PubMed

Decorte, Inge; Van der Stede, Yves; Nauwynck, Hans; De Regge, Nick; Cay, Ann Brigitte

2013-08-01

This study evaluated the effect of extraction-amplification methods, storage temperature and saliva stabilisers on detection of porcine reproductive and respiratory syndrome virus (PRRSV) RNA by quantitative reverse transcriptase real-time PCR (qRT-PCR) in porcine oral fluid. The diagnostic performance of different extraction-amplification methods was examined using a dilution series of oral fluid spiked with PRRSV. To determine RNA stability, porcine oral fluid, with or without commercially available saliva stabilisers, was spiked with PRRSV, stored at 4°C or room temperature and tested for the presence of PRRSV RNA by qRT-PCR. PRRSV RNA could be detected in oral fluid using all extraction-amplification combinations, but the limit of detection varied amongst different combinations. Storage temperature and saliva stabilisers had an effect on the stability of PRRSV RNA, which could only be detected for 7 days when PRRSV spiked oral fluid was kept at 4°C or stabilised at room temperature with a commercial mRNA stabiliser. Copyright © 2013 Elsevier Ltd. All rights reserved.

Supercritical fluid extraction and processing of foods

USDA-ARS?s Scientific Manuscript database

Consumers are aware of the processing techniques used to manufacture food and health supplements and are concerned about the impact of those processes on their health and the environment. Processes that use supercritical fluids as an alternative to solvents that are used to extract nutrients and bio...

Environmentally safe fluid extractor

DOEpatents

Sungaila, Zenon F.

1993-01-01

An environmentally safe fluid extraction device for use in mobile laboratory and industrial settings comprising a pump, compressor, valving system, waste recovery tank, fluid tank, and a exhaust filtering system.

Environmentally safe fluid extractor

DOEpatents

Sungaila, Zenon F.

1993-07-06

An environmentally safe fluid extraction device for use in mobile laboratory and industrial settings comprising a pump, compressor, valving system, waste recovery tank, fluid tank, and a exhaust filtering system.

Impacts of Extraction Methods in the Rapid Determination of Atrazine Residues in Foods using Supercritical Fluid Chromatography and Enzyme-Linked Immunosorbent Assay: Microwave Solvent vs. Supercritical Fluid Extractions

PubMed Central

El-Saeid, Mohamed H.; Kanu, Ijeoma; Anyanwu, Ebere C.; Saleh, Mahmoud A.

2005-01-01

It is an accepted fact that many food products that we eat today have the possibility of being contaminated by various chemicals used from planting to processing. These chemicals have been shown to cause illnesses for which some concerned government agencies have instituted regulatory mechanisms to minimize the risks and the effects on humans. It is for these concerns that reliable and accurate rapid determination techniques are needed to effect proper regulatory standards for the protection of people's nutritional health. This paper, therefore, reports the comparative evaluation of the extraction methods in the determination of atrazine (commonly used in agricultural as a herbicide) residues in foods using supercritical fluid chromatography (SFC) and enzyme-linked immunosorbent assay (ELISA) techniques. Supercritical fluid extraction (SFE) and microwave solvent extraction (MSE) methods were used to test samples of frozen vegetables, fruit juice, and jam from local food markets in Houston. Results showed a high recovery percentage of atrazine residues using supercritical fluid coupled with ELISA and SFC than with MSE. Comparatively, however, atrazine was detected 90.9 and 54.5% using SFC and ELISA techniques, respectively. ELISA technique was, however, less time consuming, lower in cost, and more sensitive with low detection limit of atrazine residues than SFC technique. PMID:15674445

The mechanism of improved pullulan production by nitrogen limitation in batch culture of Aureobasidium pullulans.

PubMed

Wang, Dahui; Chen, Feifei; Wei, Gongyuan; Jiang, Min; Dong, Mingsheng

2015-08-20

Batch culture of Aureobasidium pullulans CCTCC M 2012259 for pullulan production at different concentrations of ammonium sulfate and yeast extract was investigated. Increased pullulan production was obtained under nitrogen-limiting conditions, as compared to that without nitrogen limitation. The mechanism of nitrogen limitation favoring to pullulan overproduction was revealed by determining the activity as well as gene expression of key enzymes, and energy supply for pullulan biosynthesis. Results indicated that nitrogen limitation increased the activities of α-phosphoglucose mutase and glucosyltransferase, up-regulated the transcriptional levels of pgm1 and fks genes, and supplied more ATP intracellularly, which were propitious to further pullulan biosynthesis. The economic analysis of batch pullulan production indicated that nitrogen limitation could reduce more than one third of the cost of raw materials when glucose was supplemented to a total concentration of 70 g/L. This study also helps to understand the mechanism of other polysaccharide overproduction by nitrogen limitation. Copyright © 2015 Elsevier Ltd. All rights reserved.

Improving succinic acid production by Actinobacillus succinogenes from raw industrial carob pods.

PubMed

Carvalho, Margarida; Roca, Christophe; Reis, Maria A M

2016-10-01

Carob pods are an inexpensive by-product of locust bean gum industry that can be used as renewable feedstock for bio-based succinic acid. Here, for the first time, unprocessed raw carob pods were used to extract a highly enriched sugar solution, afterwards used as substrate to produce succinic acid using Actinobacillus succinogenes. Batch fermentations containing 30g/L sugars resulted in a production rate of 1.67gSA/L.h and a yield of 0.39gSA/g sugars. Taking advantage of A. succinogenes' metabolism, uncoupling cell growth from succinic acid production, a fed-batch mode was implemented to increase succinic acid yield and reduce by-products formation. This strategy resulted in a succinic acid yield of 0.94gSA/g sugars, the highest yield reported in the literature for fed-batch and continuous experiments, while maintaining by-products at residual values. Results demonstrate that raw carob pods are a highly efficient feedstock for bio-based succinic acid production. Copyright © 2016 Elsevier Ltd. All rights reserved.

Patulin Production by Penicillium urticae Bainier in Batch Culture1

PubMed Central

Norstadt, Fred A.; McCalla, T. M.

1969-01-01

A still, batch-culture method, with potato dextrose medium and Penicillium urticae Bainier, produced patulin yields of 1.2 to 1.7 g/liter of medium. Incubation was at 25 C for 14 days. Ethyl acetate extraction of condensed culture filtrate and drying with anhydrous MgSO4, followed by solvent change to dry ethyl ether and purification on alumina (pH 4.5), produced pure crystalline patulin. The use of 2-liter, round-bottom flasks and a rotating vacuum evaporator provided versatile equipment and easy manipulation in the operations. Soil from wheat fields provided a convenient natural P. urticae source. Potato dextrose medium was superior to potato sucrose or Raulin-Thom media. Images PMID:5775903

Supercritical-fluid extraction and chromatography-mass spectrometry for analysis of mycotoxins

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, R.D.; Udseth, H.R.

1982-07-01

The use of direct supercritical-fluid injection-mass spectrometry for the rapid analysis of mycotoxins of the tricothecene group is demonstrated. A solution containing diacetoxyscirpenol or T-2 toxin is injected into a fluid consisting primarily of pentane or carbon dioxide and is rapidly brought to supercritical conditions. Direct injection of the fluid stream into a chemical ionization source allows thermally labile compounds to be analyzed. Under these conditions trichothecene mass spectra showing significant (M + 1)/sup +/ ions and distinctive fragmentation patterns are obtained. Detection limits are in the subnanogram range. Direct analysis from complex substrates using selective supercritical-fluid extraction is proposed.more » 4 figures.« less

On-line supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry of polycyclic aromatic hydrocarbons in soil.

PubMed

Wicker, A Paige; Carlton, Doug D; Tanaka, Kenichiro; Nishimura, Masayuki; Chen, Vivian; Ogura, Tairo; Hedgepeth, William; Schug, Kevin A

2018-06-01

On-line supercritical fluid extraction - supercritical fluid chromatography - mass spectrometry (SFE-SFC-MS) has been applied for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil. The purpose of this study was to develop and validate the first on-line SFE-SFC-MS method for the quantification of PAHs in various types of soil. By coupling the sample extraction on-line with chromatography and detection, sample preparation is minimized, diminishing sample loss and contamination, and significantly decreasing the required extraction time. Parameters for on-line extraction coupled to chromatographic analysis were optimized. The method was validated for concentrations of 10-1500 ng of PAHs per gram of soil in Certified Reference Material (CRM) sediment, clay, and sand with R 2  ≥ 0.99. Limits of detection (LOD) were found in the range of 0.001-5 ng/g, and limits of quantification (LOQ) in the range of 5-15 ng/g. The method developed in this study can be effectively applied to the study of PAHs in the environment, and may lay the foundation for further applications of on-line SFE-SFC-MS. Copyright © 2018 Elsevier B.V. All rights reserved.

Characterization of the homologs of flerovium with crown ether based extraction chromatography resins: studies in nitric acid

DOE PAGES

Despotopulos, John D.; Kmak, Kelly N.; Gharibyan, Narek; ...

2016-09-17

Eichrom’s Pb resin, a crown-ether-based extraction chromatography resin, was characterized for separation of the flerovium (Fl) homologs, Pb and Sn. Batch uptake of Pb(II) and Sn(IV) radionuclides was determined from an HNO 3 matrix. Pb(II) was strongly retained on the resin at all HNO 3 concentrations, while Sn(IV) showed no uptake. Extraction kinetics for Pb(II) were examined and show suitable uptake on the second time scale. Here, separation methods for the isolation of individual homologs, Pb(II) and Sn(IV), have been established using 2 mL pre-packed vacuum flow Pb resin columns.

Human Metabolite Lamotrigine-N(2)-glucuronide Is the Principal Source of Lamotrigine-Derived Compounds in Wastewater Treatment Plants and Surface Water.

PubMed

Zonja, Bozo; Pérez, Sandra; Barceló, Damià

2016-01-05

Wastewater and surface water samples, extracted with four solid-phase extraction cartridges of different chemistries, were suspect-screened for the anticonvulsant lamotrigine (LMG), its metabolites, and related compounds. LMG, three human metabolites, and a LMG synthetic impurity (OXO-LMG) were detected. Preliminary results showed significantly higher concentrations of OXO-LMG in wastewater effluent, suggesting its formation in the wastewater treatment plants (WWTPs). However, biodegradation experiments with activated sludge demonstrated that LMG is resistant to degradation and that its human metabolite lamotrigine-N(2)-glucuronide (LMG-N2-G) is the actual source of OXO-LMG in WWTPs. In batch reactors, LMG-N2-G was transformed, following pseudo-first-order kinetics to OXO-LMG and LMG, but kinetic experiments suggested an incomplete mass balance. A fragment ion search applied to batch-reactor and environmental samples revealed another transformation product (TP), formed by LMG-N2-G oxidation, which was identified by high-resolution mass spectrometry. Accounting for all TPs detected, a total mass balance at two concentration levels in batch reactors was closed at 86% and 102%, respectively. In three WWTPs, the total mass balance of LMG-N2-G ranged from 71 to 102%. Finally, LMG-N2-G and its TPs were detected in surface water samples with median concentration ranges of 23-139 ng L(-1). The results of this study suggest that glucuronides of pharmaceuticals might also be sources of yet undiscovered, but environmentally relevant, transformation products.

Supercritical CO2 impregnation of PLA/PCL films with natural substances for bacterial growth control in food packaging.

PubMed

Milovanovic, Stoja; Hollermann, Gesa; Errenst, Cornelia; Pajnik, Jelena; Frerich, Sulamith; Kroll, Stephen; Rezwan, Kurosch; Ivanovic, Jasna

2018-05-01

Biodegradable polymers with antibacterial properties are highly desirable materials for active food packaging applications. Thymol, a dietary monoterpene phenol with a strong antibacterial activity is abundant in plants belonging to the genus Thymus. This study presents two approaches for supercritical CO 2 impregnation of poly(lactic acid)(PLA)/poly(ε-caprolactone)(PCL) blended films to induce antibacterial properties of the material: (i) a batch impregnation process for loading pure thymol, and (ii) an integrated supercritical extraction-impregnation process for isolation of thyme extract and its incorporation into the films, operated in both batch or semi-continuous modes with supercritical solution circulation. The PCL content in films, impregnation time and CO 2 flow regime were varied to maximize loading of the films with thymol or thyme extract with preserving films' structure and thermal stability. Representative film samples impregnated with thymol and thyme extract were tested against Gram (-) (Escherichia coli) and Gram(+) (Bacillus subtilis) model strains, by measuring their metabolic activity and re-cultivation after exposure to the films. The film containing thymol (35.8 wt%) showed a strong antibacterial activity leading to a total reduction of bacterial cell viability. Proposed processes enable fast, controlled and organic solvent-free fabrication of the PLA/PCL films containing natural antibacterial substances at moderately low temperature, with a compact structure and a good thermal stability, for potential use as active food packaging materials. Copyright © 2018 Elsevier Ltd. All rights reserved.

Optimization of conditions for supercritical fluid extraction of flavonoids from hops (Humulus lupulus L.)*

PubMed Central

He, Guo-qing; Xiong, Hao-ping; Chen, Qi-he; Ruan, Hui; Wang, Zhao-yue; Traoré, Lonseny

2005-01-01

Waste hops are good sources of flavonoids. Extraction of flavonoids from waste hops (SC-CO2 extracted hops) using supercritical fluids technology was investigated. Various temperatures, pressures and concentrations of ethanol (modifier) and the ratio (w/w) of solvent to material were tested in this study. The results of single factor and orthogonal experiments showed that at 50 °C, 25 MPa, the ratio of solvent to material (50%), ethanol concentration (80%) resulted in maximum extraction yield flavonoids (7.8 mg/g). HPLC-MS analysis of the extracts indicated that flavonoids obtained were xanthohumol, the principal prenylflavonoid in hops. PMID:16187413

Phytochemical profile and anticholinesterase and antimicrobial activities of supercritical versus conventional extracts of Satureja montana.

PubMed

Silva, Filipa V M; Martins, Alice; Salta, Joana; Neng, Nuno R; Nogueira, José M F; Mira, Delfina; Gaspar, Natália; Justino, Jorge; Grosso, Clara; Urieta, José S; Palavra, António M S; Rauter, Amélia P

2009-12-23

Winter savory Satureja montana is a medicinal herb used in traditional gastronomy for seasoning meats and salads. This study reports a comparison between conventional (hydrodistillation, HD, and Soxhlet extraction, SE) and alternative (supercritical fluid extraction, SFE) extraction methods to assess the best option to obtain bioactive compounds. Two different types of extracts were tested, the volatile (SFE-90 bar, second separator vs HD) and the nonvolatile fractions (SFE-250 bar, first and second separator vs SE). The inhibitory activity over acetyl- and butyrylcholinesterase by S. montana extracts was assessed as a potential indicator for the control of Alzheimer's disease. The supercritical nonvolatile fractions, which showed the highest content of (+)-catechin, chlorogenic, vanillic, and protocatechuic acids, also inhibited selectively and significantly butyrylcholinesterase, whereas the nonvolatile conventional extract did not affect this enzyme. Microbial susceptibility tests revealed the great potential of S. montana volatile supercritical fluid extract for the growth control and inactivation of Bacillus subtilis and Bacillus cereus, showing some activity against Botrytis spp. and Pyricularia oryzae. Although some studies were carried out on S. montana, the phytochemical analysis together with the biological properties, namely, the anticholinesterase and antimicrobial activities of the plant nonvolatile and volatile supercritical fluid extracts, are described herein for the first time.

Process And Apparatus To Accomplish Autothermal Or Steam Reforming Via A Reciprocating Compression Device

DOEpatents

Lyons, K. David; James, Robert; Berry, David A.; Gardner, Todd

2004-09-21

The invention provides a method and apparatus for producing a synthesis gas from a variety of hydrocarbons. The apparatus (device) consists of a semi-batch, non-constant volume reactor to generate a synthesis gas. While the apparatus feeds mixtures of air, steam, and hydrocarbons into a cylinder where work is performed on the fluid by a piston to adiabatically raise its temperature without heat transfer from an external source.

Unraveling the Fate and Transport of SrEDTA-2 and Sr+2 in Hanford Sediments

NASA Astrophysics Data System (ADS)

Pace, M. N.; Mayes, M. A.; Jardine, P. M.; Mehlhorn, T. L.; Liu, Q. G.; Yin, X. L.

2004-12-01

Accelerated migration of strontium-90 has been observed in the vadose zone beneath the Hanford tank farm. The goal of this paper is to provide an improved understanding of the hydrogeochemical processes that contribute to strontium transport in the far-field Hanford vadose zone. Laboratory scale batch, saturated packed column experiments, and an unsaturated transport experiment in an undisturbed core were conducted to quantify geochemical and hydrological processes controlling Sr+2 and SrEDTA-2 sorption to Hanford flood deposits. After experimentation, the undisturbed core was disassembled and samples were collected from different bedding units as a function of depth. Sequential extractions were then performed on the samples. It has been suggested that organic chelates such as EDTA may be responsible for the accelerated transport of strontium due to the formation of stable anionic complexes. Duplicate batch and column experiments performed with Sr+2 and SrEDTA-2 suggested that the SrEDTA-2 complex was not stable in the presence of soil and rapid dissociation allowed strontium to be transported as a divalent cation. Batch experiments indicated a decrease in sorption with increasing rock:water ratios, whereas saturated packed column experiments indicated equal retardation in columns of different lengths. This difference between the batch and column experiments is primarily due to the difference between equilibrium conditions where dissolution of cations may compete for sorption sites versus flowing conditions where any dissolved cations are flushed through the system minimizing competition for sorption sites. Unsaturated transport in the undisturbed core resulted in significant Sr+2 retardation despite the presence of physical nonequilibrium. Core disassembly and sequential extractions revealed the mass wetness distribution and reactive mineral phases associated with strontium in the core. Overall, results indicated that strontium will most likely be transported through the Hanford far-field vadose zone as a divalent cation.

Quality evaluation of Yin Chen Hao Tang extract based on fingerprint chromatogram and simultaneous determination of five bioactive constituents.

PubMed

Wang, Xijun; Lv, Haitao; Sun, Hui; Jiang, Xingang; Wu, Zeming; Sun, Wenjun; Wang, Ping; Liu, Lian; Bi, Kaishun

2008-01-01

A completely validated method based on HPLC coupled with photodiode array detector (HPLC-UV) was described for evaluating and controlling quality of Yin Chen Hao Tang extract (YCHTE). First, HPLC-UV fingerprint chromatogram of YCHTE was established for preliminarily elucidating amount and chromatographic trajectory of chemical constituents in YCHTE. Second, for the first time, five mainly bioactive constituents in YCHTE were simultaneously determined based on fingerprint chromatogram for furthermore controlling the quality of YCHTE quantitatively. The developed method was applied to analyze 12 batches of YCHTE samples which consisted of herbal drugs from different places of production, showed acceptable linearity, intraday (RSD <5%), interday precision (RSD <4.80%), and accuracy (RSD <2.80%). As a result, fingerprint chromatogram determined 15 representative general fingerprint peaks, and the fingerprint chromatogram resemblances are all better than 0.9996. The contents of five analytes in different batches of YCHTE samples do not indicate significant difference. So, it is concluded that the developed HPLC-UV method is a more fully validated and complete method for evaluating and controlling the quality of YCHTE.

Ethanol production from lignocellulosic byproducts of olive oil extraction.

PubMed

Ballesteros, I; Oliva, J M; Saez, F; Ballesteros, M

2001-01-01

The recent implementation of a new two-step centrifugation process for extracting olive oil in Spain has substantially reduced water consumption, thereby eliminating oil mill wastewater. However, a new high sugar content residue is still generated. In this work the two fractions present in the residue (olive pulp and fragmented stones) were assayed as substrate for ethanol production by the simultaneous saccharification and fermentation (SSF) process. Pretreatment of fragmented olive stones by sulfuric acid-catalyzed steam explosion was the most effective treatment for increasing enzymatic digestibility; however, a pretreatment step was not necessary to bioconvert the olive pulp into ethanol. The olive pulp and fragmented olive stones were tested by the SSF process using a fed-batch procedure. By adding the pulp three times at 24-h intervals, 76% of the theoretical SSF yield was obtained. Experiments with fed-batch pretreated olive stones provided SSF yields significantly lower than those obtained at standard SSF procedure. The preferred SSF conditions to obtain ethanol from olives stones (61% of theoretical yield) were 10% substrate and addition of cellulases at 15 filter paper units/g of substrate.

Establishment and assessment of an integrated citric acid-methane production process.

PubMed

Xu, Jian; Chen, Yang-Qiu; Zhang, Hong-Jian; Bao, Jia-Wei; Tang, Lei; Wang, Ke; Zhang, Jian-Hua; Chen, Xu-Sheng; Mao, Zhong-Gui

2015-01-01

To solve the problem of extraction wastewater in citric acid industrial production, an improved integrated citric acid-methane production process was established in this study. Extraction wastewater was treated by anaerobic digestion and then the anaerobic digestion effluent (ADE) was stripped by air to remove ammonia. Followed by solid-liquid separation to remove metal ion precipitation, the supernatant was recycled for the next batch of citric acid fermentation, thus eliminating wastewater discharge and reducing water consumption. 130U/g glucoamylase was added to medium after inoculation and the recycling process performed for 10 batches. Fermentation time decreased by 20% in recycling and the average citric acid production (2nd-10th) was 145.9±3.4g/L, only 2.5% lower than that with tap water (149.6g/L). The average methane production was 292.3±25.1mL/g CODremoved and stable in operation. Excessive Na(+) concentration in ADE was confirmed to be the major challenge for the proposed process. Copyright © 2014 Elsevier Ltd. All rights reserved.

Degradation pathway of 2-chloroethanol in Pseudomonas stutzeri strain JJ under denitrifying conditions.

PubMed

Dijk, John A; Gerritse, Jan; Schraa, Gosse; Stams, Alfons J M

2004-12-01

The pathway of 2-chloroethanol degradation in the denitrifying Pseudomonas stutzeri strain JJ was investigated. In cell-free extracts, activities of a phenazine methosulfate (PMS)-dependent chloroethanol dehydrogenase, an NAD-dependent chloroacetaldehyde dehydrogenase, and a chloroacetate dehalogenase were detected. This suggested that the 2-chloroethanol degradation pathway in this denitrifying strain is the same as found in aerobic bacteria that degrade chloroethanol. Activity towards primary alcohols, secondary alcohols, diols, and other chlorinated alcohols could be measured in cell-free extracts with chloroethanol dehydrogenase (CE-DH) activity. PMS and phenazine ethosulfate (PES) were used as primary electron acceptors, but not NAD, NADP or ferricyanide. Cells of strain JJ cultured in a continuous culture under nitrate limitation exhibited chloroethanol dehydrogenase activity that was a 12 times higher than in cells grown in batch culture. However, under chloroethanol-limiting conditions, CE-DH activity was in the same range as in batch culture. Cells grown on ethanol did not exhibit CE-DH activity. Instead, NAD-dependent ethanol dehydrogenase (E-DH) activity and PMS-dependent E-DH activity were detected.

Biosynthesis of highly enriched 13C-lycopene for human metabolic studies using repeated batch tomato cell culturing with 13C-glucose

PubMed Central

Moran, Nancy E.; Rogers, Randy B.; Lu, Chi-Hua; Conlon, Lauren E.; Lila, Mary Ann; Clinton, Steven K.; Erdman, John W.

2013-01-01

While putative disease-preventing lycopene metabolites are found in both tomato (Solanum lycopersicum) products and in their consumers, mammalian lycopene metabolism is poorly understood. Advances in tomato cell culturing techniques offer an economical tool for generation of highly-enriched 13C-lycopene for human bioavailability and metabolism studies. To enhance the 13C-enrichment and yields of labeled lycopene from the hp-1 tomato cell line, cultures were first grown in 13C-glucose media for three serial batches and produced increasing proportions of uniformly labeled lycopene (14.3 +/− 1.2 %, 39.6 +/− 0.5 %, and 48.9 +/− 1.5% with consistent yields (from 5.8 to 9 mg/L). An optimized 9-day-long 13C-loading and 18-day-long labeling strategy developed based on glucose utilization and lycopene yields, yielded 13C-lycopene with 93% 13C isotopic purity, and 55% of isotopomers were uniformly labeled. Furthermore, an optimized acetone and hexane extraction led to a four-fold increase in lycopene recovery from cultures compared to a standard extraction. PMID:23561155

Kinetic models for batch ethanol production from sweet sorghum juice under normal and high gravity fermentations: Logistic and modified Gompertz models.

PubMed

Phukoetphim, Niphaphat; Salakkam, Apilak; Laopaiboon, Pattana; Laopaiboon, Lakkana

2017-02-10

The aim of this study was to model batch ethanol production from sweet sorghum juice (SSJ), under normal gravity (NG, 160g/L of total sugar) and high gravity (HG, 240g/L of total sugar) conditions with and without nutrient supplementation (9g/L of yeast extract), by Saccharomyces cerevisiae NP 01. Growth and ethanol production increased with increasing initial sugar concentration, and the addition of yeast extract enhanced both cell growth and ethanol production. From the results, either logistic or a modified Gompertz equation could be used to describe yeast growth, depending on information required. Furthermore, the modified Gompertz model was suitable for modeling ethanol production. Both the models fitted the data very well with coefficients of determination exceeding 0.98. The results clearly showed that these models can be employed in the development of ethanol production processes using SSJ under both NG and HG conditions. The models were also shown to be applicable to other ethanol fermentation systems employing pure and mixed sugars as carbon sources. Copyright © 2016 Elsevier B.V. All rights reserved.

An Analytical Model for Assessing Stability of Pre-Existing Faults in Caprock Caused by Fluid Injection and Extraction in a Reservoir

NASA Astrophysics Data System (ADS)

Wang, Lei; Bai, Bing; Li, Xiaochun; Liu, Mingze; Wu, Haiqing; Hu, Shaobin

2016-07-01

Induced seismicity and fault reactivation associated with fluid injection and depletion were reported in hydrocarbon, geothermal, and waste fluid injection fields worldwide. Here, we establish an analytical model to assess fault reactivation surrounding a reservoir during fluid injection and extraction that considers the stress concentrations at the fault tips and the effects of fault length. In this model, induced stress analysis in a full-space under the plane strain condition is implemented based on Eshelby's theory of inclusions in terms of a homogeneous, isotropic, and poroelastic medium. The stress intensity factor concept in linear elastic fracture mechanics is adopted as an instability criterion for pre-existing faults in surrounding rocks. To characterize the fault reactivation caused by fluid injection and extraction, we define a new index, the "fault reactivation factor" η, which can be interpreted as an index of fault stability in response to fluid pressure changes per unit within a reservoir resulting from injection or extraction. The critical fluid pressure change within a reservoir is also determined by the superposition principle using the in situ stress surrounding a fault. Our parameter sensitivity analyses show that the fault reactivation tendency is strongly sensitive to fault location, fault length, fault dip angle, and Poisson's ratio of the surrounding rock. Our case study demonstrates that the proposed model focuses on the mechanical behavior of the whole fault, unlike the conventional methodologies. The proposed method can be applied to engineering cases related to injection and depletion within a reservoir owing to its efficient computational codes implementation.

Fluid extraction using carbon dioxide and organophosphorus chelating agents

DOEpatents

Smart, N.G.; Wai, C.M.; Lin, Y.; Kwang, Y.H.

1998-11-24

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO{sub 2}, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO{sub 2} and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process. 1 fig.

Fluid extraction using carbon dioxide and organophosphorus chelating agents

DOEpatents

Smart, Neil G.; Wai, Chien M.; Lin, Yuehe; Kwang, Yak Hwa

1998-01-01

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO.sub.2, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO.sub.2 and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process.

In-situ remediation system and method for contaminated groundwater

DOEpatents

Corey, John C.; Looney, Brian B.; Kaback, Dawn S.

1989-01-01

A system for removing volatile contaminants from a subsurface plume of contamination comprising two sets of wells, a well for injecting a fluid into a saturated zone on one side of the plume and an extracting well for collecting the fluid together with volatilized contaminants from the plume on the other side of the plume. The fluid enables the volatile contaminants to be volatilized and carried therewith through the ground to the extracting well. Injecting and extracting wells are preferably horizontal wells positioned below the plume in the saturated zone and above the plume in the vadose zone, respectively. The fluid may be air or other gas or a gas and liquid mixture depending on the type of contaminant to be removed and may be preheated to facilitate volatilization. Treatment of the volatilized contamination may be by filtration, incineration, atmospheric dispersion or the like.

In-situ remediation system and method for contaminated groundwater

DOEpatents

Corey, J.C.; Looney, B.B.; Kaback, D.S.

1989-05-23

A system for removing volatile contaminants from a subsurface plume of contamination comprising two sets of wells, a well for injecting a fluid into a saturated zone on one side of the plume and an extracting well for collecting the fluid together with volatilized contaminants from the plume on the other side of the plume. The fluid enables the volatile contaminants to be volatilized and carried therewith through the ground to the extracting well. Injecting and extracting wells are preferably horizontal wells positioned below the plume in the saturated zone and above the plume in the vadose zone, respectively. The fluid may be air or other gas or a gas and liquid mixture depending on the type of contaminant to be removed and may be preheated to facilitate volatilization. Treatment of the volatilized contamination may be by filtration, incineration, atmospheric dispersion or the like. 3 figs.

Fed batch fermentation and purification strategy for high yield production of Brucella melitensis recombinant Omp 28 kDa protein and its application in disease diagnosis.

PubMed

Karothia, B S; Athmaram, T N; D, Thavaselvam; Ashu, Kumar; Tiwari, Sapna; Singh, Anil K; Sathyaseelan, K; Gopalan, N

2013-07-01

Brucellosis is a disease caused by bacteria belonging to the genus Brucella. It affects cattle, goat, sheep, dog and humans. The serodiagnosis of brucellosis involves detection of antibodies generated against the LPS or whole cell bacterial extracts, however these tests lack sensitivity and specificity. The present study was performed to optimize the culture condition for the production of recombinant Brucella melitensis outer membrane protein 28 kDa protein in E.coli via fed batch fermentation. Expression was induced with 1.5mM isopropyl β thiogalactoside and the expressed recombinant protein was purified using Ni-NTA affinity chromatography. After fed-batch fermentation the dry cell weight of 17.81 g/L and a purified protein yield of 210.10 mg/L was obtained. The purified Brucella melitensis recombinant Omp 28 kDa protein was analyzed through SDS- poly acrylamide gel electrophoresis and western blotting. The obtained recombinant protein was evaluated for its diagnostic application through Indirect ELISA using brucellosis suspected human sera samples. Our results clearly indicate that recombinant Omp28 produced via fed batch fermentation has immense potential as a diagnostic reagent that could be employed in sero monitoring of brucellosis.

Heater Validation for the NEXT-C Hollow Cathodes

NASA Technical Reports Server (NTRS)

Verhey, Timothy R.; Soulas, George C.; Mackey, Jonathan A.

2018-01-01

Swaged cathode heaters whose design was successfully demonstrated under a prior flight project are to be provided by the NASA Glenn Research Center for the NEXT-C ion thruster being fabricated by Aerojet Rocketdyne. Extensive requalification activities were performed to validate process controls that had to be re-established or revised because systemic changes prevented reuse of the past approaches. A development batch of heaters was successfully fabricated based on the new process controls. Acceptance and cyclic life testing of multiple discharge and neutralizer sized heaters extracted from the development batch was initiated in August, 2016, with the last heater completing testing in April, 2017. Cyclic life testing results substantially exceeded the NEXT-C thruster requirement as well as all past experience for GRC-fabricated units. The heaters demonstrated ultimate cyclic life capability of 19050 to 33500 cycles. A qualification batch of heaters is now being fabricated using the finalized process controls. A set of six heaters will be acceptance and cyclic tested to verify conformance to the behavior observed with the development heaters. The heaters for flight use will be then be provided to the contractor from the remainder of the qualification batch. This paper summarizes the fabrication process control activities and the acceptance and life testing of the development heater units.

A GPU-Accelerated Approach for Feature Tracking in Time-Varying Imagery Datasets.

PubMed

Peng, Chao; Sahani, Sandip; Rushing, John

2017-10-01

We propose a novel parallel connected component labeling (CCL) algorithm along with efficient out-of-core data management to detect and track feature regions of large time-varying imagery datasets. Our approach contributes to the big data field with parallel algorithms tailored for GPU architectures. We remove the data dependency between frames and achieve pixel-level parallelism. Due to the large size, the entire dataset cannot fit into cached memory. Frames have to be streamed through the memory hierarchy (disk to CPU main memory and then to GPU memory), partitioned, and processed as batches, where each batch is small enough to fit into the GPU. To reconnect the feature regions that are separated due to data partitioning, we present a novel batch merging algorithm to extract the region connection information across multiple batches in a parallel fashion. The information is organized in a memory-efficient structure and supports fast indexing on the GPU. Our experiment uses a commodity workstation equipped with a single GPU. The results show that our approach can efficiently process a weather dataset composed of terabytes of time-varying radar images. The advantages of our approach are demonstrated by comparing to the performance of an efficient CPU cluster implementation which is being used by the weather scientists.

EVALUATION OF ANALYTICAL METHODS FOR DETERMINING PESTICIDES IN BABY FOOD

EPA Science Inventory

Three extraction methods and two detection techniques for determining pesticides in baby food were evaluated. The extraction techniques examined were supercritical fluid extraction (SFE), enhanced solvent extraction (ESE), and solid phase extraction (SPE). The detection techni...

Comparison of two different solvents employed for pressurised fluid extraction of stevioside from Stevia rebaudiana: methanol versus water.

PubMed

Pól, Jaroslav; Varadová Ostrá, Elena; Karásek, Pavel; Roth, Michal; Benesová, Karolínka; Kotlaríková, Pavla; Cáslavský, Josef

2007-08-01

Pressurised fluid extraction using water or methanol was employed for the extraction of stevioside from Stevia rebaudiana Bertoni. The extraction method was optimised in terms of temperature and duration of the static or the dynamic step. Extracts were analysed by liquid chromatography followed by UV and mass-spectrometric (MS) detections. Thermal degradation of stevioside was the same in both solvents within the range 70-160 degrees C. Methanol showed better extraction ability for isolation of stevioside from Stevia rebaudiana leaves than water within the range 110-160 degrees C. However, water represents the green alternative to methanol. The limit of detection of stevioside in the extract analysed was 30 ng for UV detection and 2 ng for MS detection.

Determination of fluid extraction and osmotic conductance sigma K in the lung with hypertonic NaCl infusion. I. Theory.

PubMed

Hunter, M; Lee, J

1992-11-01

A dispersion and extraction model of the lung is developed to assess how the infusion of hypertonic saline into the pulmonary artery changes the gravimetric density of pulmonary venous blood. The dispersion analysis is built on the indicator dilution curve measured for the pulmonary circulation. The extraction model consists of microvascular and interstitial compartments separated by a permeable pulmonary endothelium. Because the density of fluid extracted by the hypertonic disturbance is lower than the blood density, the extraction leads to a decrease in blood density. Two cases of fluid extraction are analyzed, a hypertonic infusion to elevate the osmotic pressure in the pulmonary arterial blood in the form of a step function and an infusion performed over a period of 1 sec. Both cases show that the dispersion significantly attenuates the changes in osmotic pressure and density as they are transported by the blood along the pulmonary vasculature. Because the model has taken into account the effect of dispersion and pulmonary blood flow, the equations developed here provide the basis to calculate from the density change in pulmonary venous blood the characteristics of osmotic extraction intrinsic to the lung.

Numerical simulation of stress distribution in Inconel 718 components realized by metal injection molding during supercritical debinding

NASA Astrophysics Data System (ADS)

Agne, Aboubakry; Barrière, Thierry

2018-05-01

Metal injection molding (MIM) is a process combining advantages of thermoplastic injection molding and powder metallurgy process in order to manufacture components with complex and near net-shape geometries. The debinding of a green component can be performed in two steps, first by using solvent debinding in order to extract the organic part of the binder and then by thermal degradation of the rest of the binder. A shorter and innovative method for extracting an organic binder involves the use of supercritical fluid instead of a regular solvent. The debinding via a supercritical fluid was recently investigated to extract organic binders contained in components obtained by Metal Injection Molding. It consists to put the component in an enclosure subjected to high pressure and temperature. The supercritical fluid has various properties depending on these two conditions, e.g., density and viscosity. The high-pressure combined with the high temperature during the process affect the component structure. Three mechanisms contributing to the deformation of the component can been differentiated: thermal expansion, binder extraction and supercritical fluid effect on the outer surfaces of the component. If one supposes that, the deformation due to binder extraction is negligible, thermal expansion and the fluid effect are probably the main mechanisms that can produce several stress. A finite-element model, which couples fluid-structures interaction and structural mechanics, has been developed and performed on the Comsol Multiphysics® finite-element software platform allowed to estimate the stress distribution during the supercritical debinding of MIM component composed of Inconel 718 powders, polypropylene, polyethylene glycol and stearic acid as binder. The proposed numerical simulations allow the estimation of the stress distribution with respect to the processing parameters for MIM components during the supercritical debinding process using a stationary solver.

In vitro digestive fluid extraction as a measure of the bioavailability of sediment-associated polycyclic aromatic hydrocarbons: Sources of variation and implications for partitioning models

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weston, D.P.; Mayer, L.M.

1998-05-01

In vitro extraction of contaminated sediments using the digestive fluid of a deposit-feeding polychaete has recently been proposed to study contaminant bioaccumulation mechanisms and perhaps to better quantify the bioavailable contaminant fraction. This approach was evaluated using digestive fluid from the polychaete Arenicola brasiliensis and six marine sediments containing both spiked radiolabeled polycyclic aromatic hydrocarbons (PAHs) and in situ-contaminated unlabeled PAHs. The proportion of total contaminant extracted by digestive fluid from each sediment varied from 22 to 71% and 13 to 52%, for phenanthrene and benzo[a]pyrene, respectively. The proportions of contaminant solubilized were inversely correlated with the sediments` organic carbonmore » content. The extent of PAH solubilization among sediments by A. brasiliensis digestive fluid was highly correlated with that of digestive fluid from the echiuran Urechis caupo and appears to be a consequence of surfactant properties of the fluids rather than of their enzymatic activity. The proportion of PAHs solubilized in vitro was similar to in vivo measurements of solubilization for contaminant exposures lasting about 24 h. However, with continued exposure, in vivo PAH concentrations in the digestive fluid increased fivefold, suggesting that digestive fluid is retained in the gut longer than sediment and thus accumulates PAHs through sequential digestion of many gut volumes. This phenomenon may enhance contaminant fugacity in the gut and increase the potential for bioaccumulation or toxicity.« less

Supercritical fluid processing: opportunities for new resist materials and processes

NASA Astrophysics Data System (ADS)

Gallagher-Wetmore, Paula M.; Ober, Christopher K.; Gabor, Allen H.; Allen, Robert D.

1996-05-01

Over the past two decades supercritical fluids have been utilized as solvents for carrying out separations of materials as diverse as foods, polymers, pharmaceuticals, petrochemicals, natural products, and explosives. More recently they have been used for non-extractive applications such as recrystallization, deposition, impregnation, surface modification, and as a solvent alternative for precision parts cleaning. Today, supercritical fluid extraction is being practiced in the foods and beverage industries; there are commercial plants for decaffeinating coffee and tea, extracting beer flavoring agents from hops, and separating oils and oleoresins from spices. Interest in supercritical fluid processing of polymers has grown over the last ten years, and many new purification, fractionation, and even polymerization techniques have emerged. One of the most significant motivations for applying this technology to polymers has been increased performance demands. More recently, with increasing scrutiny of traditional solvents, supercritical fluids, and in particular carbon dioxide, are receiving widespread attention as 'environmentally conscious' solvents. This paper describes several examples of polymers applications, including a few involving photoresists, which demonstrate that as next- generation advanced polymer systems emerge, supercritical fluids are certain to offer advantages as cutting edge processing tools.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Despotopulos, John D.; Kmak, Kelly N.; Gharibyan, Narek

Eichrom’s Pb resin, a crown-ether-based extraction chromatography resin, was characterized for separation of the flerovium (Fl) homologs, Pb and Sn. Batch uptake of Pb(II) and Sn(IV) radionuclides was determined from an HNO 3 matrix. Pb(II) was strongly retained on the resin at all HNO 3 concentrations, while Sn(IV) showed no uptake. Extraction kinetics for Pb(II) were examined and show suitable uptake on the second time scale. Here, separation methods for the isolation of individual homologs, Pb(II) and Sn(IV), have been established using 2 mL pre-packed vacuum flow Pb resin columns.

Polydimethylsiloxane/MIL-100(Fe) coated stir bar sorptive extraction-high performance liquid chromatography for the determination of triazines in environmental water samples.

PubMed

Lei, Yun; Chen, Beibei; You, Linna; He, Man; Hu, Bin

2017-12-01

Polydimethylsiloxane (PDMS)/MIL-100(Fe) coated stir bar was prepared by sol gel technique, and good preparation reproducibility was achieved with relative standard deviations (RSDs) ranging from 2.6% to 7.5% (n=7) and 3.6% to 10.8% (n=7) for bar-to-bar and batch-to-batch, respectively. Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/MIL-100(Fe) stir bar showed better extraction efficiency for target triazines compounds. It also exhibited relatively fast extraction/desorption kinetics and long lifespan. Based on it, a method of PDMS/MIL-100(Fe) coated stir bar sorptive extraction (SBSE)-high performance liquid chromatography-ultraviolet detector (HPLC-UV) was developed for the determination of six triazines (simazine, atrazine, prometon, ametryn, prometryne and prebane) in environmental water samples. Several parameters affecting SBSE of six target triazines including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.021-0.079μgL -1 . The repeatability RSDs were in the range of 2.3-6.3% (n=7, c=0.5μgL -1 ) and the enrichment factors (EFs) ranged from 51.1 to 102-fold (theoretical EF was 200-fold). The proposed method was applied to the analysis of target triazines in environmental water samples, with recoveries of 98.0-118% and 94.0-107% for spiked East Lake water and local pond water samples, respectively. Copyright © 2017. Published by Elsevier B.V.

Development and Evaluation of Naproxen Sodium Gel Using Piper cubeba for Enhanced Transdermal Drug Delivery and Therapeutic Facilitation.

PubMed

Patwardhan, Sunetra; Patil, Manohar; Sockalingam, Anbazhagan

2017-01-01

The absorption of drug through skin avoids many side effects of oral route like gastric irritation, nausea, systemic toxicity etc and thus improves patient compliance. Naproxen sodium (NPRS) is one of the potent NSAID agents. The present study was aimed to develop and evaluate the gel formulation containing NPRS for transdermal drug delivery reducing the side effects and improving patient compliance. The patents on topical delivery of NSAIDS (US 9012402 B1, US 9072659 B2, US 20150258196 A1) and patents indicating use of herbal penetration enhancers (US 20100273746A1, WO 2005009510 A2, US 6004969 A) helped in selecting the drug, excipients. Current protocol employs various extracts of Piper cubeba fruit to evaluate its role in absorption of NPRS. Various batches containing 1% NPRS and varying concentrations of synthetic permeation enhancers or the extracts were formulated in carbopol gel. Gel was evaluated for parameters like organoleptic parameters, pH, viscosity and spreadability. An ex-vivo percutaneous absorption of NPRS from gel was investigated and compared with best performing synthetic enhancer, transcutol P (TP). The batch containing 2% n-hexane extract (NHE) of Piper cubeba showed higher permeation than TP and Chloroform (CE), Methanolic (ME) and aqueous (AE) extracts as well. It showed improved % cumulative release (85.09%) and flux (278.61μg/cm2.h), as compared to TP and other extracts. Histopathology indicated the formulation safer as compared to that with synthetic enhancer. It suggests P. cubeba as effective and safer tool for transdermal delivery and acts as therapeutic facilitator for naproxen. GC-MS analysis indicates lignans & terpenes in NHE to which this permeation enhancement activity may be attributed. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Influence of indigenous and added iron on copper extraction from soil.

PubMed

Di Palma, Luca

2009-10-15

Experimental tests of copper leaching from a low permeability soil are presented and discussed. The objective of the experiments was to investigate the influence of indigenous and added iron in the soil towards copper mobilization. Metals' leaching was performed by flushing (column tests) or washing (batch tests) the soil with an aqueous solution of ethylenediaminetetraacetic acid, EDTA. An excess of EDTA was used in flushing tests (up to a EDTA:Cu molar ratio of about 26.2:1), while, in washing tests, the investigated EDTA vs. copper molar ratios were in the range between 1 (equimolar tests) and 8. Copper extraction yield in flushing tests (up to about 85%) was found to depend upon contact time between the soil and the leaching solution and the characteristics of the conditioning solution. The saturation of the soil with a NaNO(3) solution before the treatment, favoured the flushing process reducing the time of percolation, but resulted in a lower metal extraction during the following percolation of EDTA. The indigenous iron was competitive with copper to form EDTA complexes only when it was present in the organic and oxides-hydroxides fractions. Artificial iron addition to the soil resulted in an increase of both the exchangeable iron and the iron bonded to the organic fraction of the soil, thus increasing the overall amount of iron available to extraction. In both batch and continuous tests, the mechanism of copper extraction was found to involve the former dissolution of metal salts, that lead to an initial high concentration of both copper and selected competitive cations (essentially Ca(2+)), and the following EDTA exchange reaction between calcium and copper complexes. The initial metal salts dissolution was found to be pH-dependant.

Method and apparatus for back-extracting metal chelates

DOEpatents

Wai, Chien M.; Smart, Neil G.; Lin, Yuehe

1998-01-01

A method of extracting metal and metalloid species from a solid or liquid substrate using a supercritical fluid solvent containing one or more chelating agents followed by back-extracting the metal and metalloid species from the metal and metalloid chelates formed thereby. The back-extraction acidic solution is performed utilizing an acidic solution. Upon sufficient exposure of the metal and metalloid chelates to the acidic solution, the metal and metalloid species are released from the chelates into the acid solution, while the chelating agent remains in the supercritical fluid solvent. The chelating agent is thereby regenerated and the metal and metalloid species recovered.

Selective enrichment in bioactive compound from Kniphofia uvaria by super/subcritical fluid extraction and centrifugal partition chromatography.

PubMed

Duval, Johanna; Destandau, Emilie; Pecher, Virginie; Poujol, Marion; Tranchant, Jean-François; Lesellier, Eric

2016-05-20

Nowadays, a large portion of synthetic products (active cosmetic and therapeutic ingredients) have their origin in natural products. Kniphofia uvaria is a plant from Africa which has proved in the past by in-vivo tests an antioxidant activity due to compounds present in roots. Recently, we have observed anthraquinones in K. uvaria seeds extracts. These derivatives are natural colorants which could have interesting bioactive potential. The aim of this study was to obtain an extract enriched in anthraquinones from K. uvaria seeds which mainly contains glycerides. First, the separation of the seed compounds was studied by using supercritical fluid chromatography (SFC) in the goal to provide a rapid quantification method of these bioactive compounds. A screening of numerous polar stationary phases was achieved for selecting the most suited phase to the separation of the four anthraquinones founded in the seeds. A gradient elution was optimized for improving the separation of the bioactive compounds from the numerous other families of major compounds of the extracts (fatty acids, di- and triglycerides). Besides, a non-selective and green Supercritical Fluid Extraction (SFE) with pure CO2 was applied to seeds followed by a Centrifugal Partition Chromatography (CPC). The CPC system was optimized by using the Arizona phase system, to enrich the extract in anthraquinones. Two systems were selected to isolate the bioactive compounds from the oily extract with varied purity target. The effect of the injection mode for these very viscous samples was also studied. Finally, in order to directly apply a selective process of extraction to the seeds, the super/subcritical fluid extraction was optimized to increase the anthraquinone yield in the final extract, by studying varied modifier compositions and nature, as well as different temperatures and backpressures. Conditions suited to favour an enrichment factor bases on the ratio of anthraquinone and trilycerides extracted are described. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid and quantitative determination of 10 major active components in Lonicera japonica Thunb. by ultrahigh pressure extraction-HPLC/DAD

NASA Astrophysics Data System (ADS)

Fan, Li; Lin, Changhu; Duan, Wenjuan; Wang, Xiao; Liu, Jianhua; Liu, Feng

2015-01-01

An ultrahigh pressure extraction (UPE)-high performance liquid chromatography (HPLC)/diode array detector (DAD) method was established to evaluate the quality of Lonicera japonica Thunb. Ten active components, including neochlorogenic acid, chlorogenic acid, 4-dicaffeoylquinic acid, caffeic acid, rutin, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and quercetin, were qualitatively evaluated and quantitatively determined. Scanning electron microscope images elucidated the bud surface microstructure and extraction mechanism. The optimal extraction conditions of the UPE were 60% methanol solution, 400 MPa of extraction pressure, 3 min of extraction time, and 1:30 (g/mL) solid:liquid ratio. Under the optimized conditions, the total extraction yield of 10 active components was 57.62 mg/g. All the components showed good linearity (r2 ≥ 0.9994) and recoveries. This method was successfully applied to quantify 10 components in 22 batches of L. japonica samples from different areas. Compared with heat reflux extraction and ultrasonic-assisted extraction, UPE can be considered as an alternative extraction technique for fast extraction of active ingredient from L. japonica.

Supercritical carbon dioxide extraction of 2,4-dichlorophenol from food crop tissues.

PubMed

Thomson, C A; Chesney, D J

1992-04-15

Supercritical fluid extraction with carbon dioxide has been found to be effective for the isolation of residue levels (0.1-1 ppm) of 2,4-dichlorophenol from selected plant tissues. The 2,4-dichlorophenol residues were incompletely extracted with supercritical CO2 alone, since a substantial fraction of the 2,4-dichlorophenol was covalently attached to the plant matrix. An acid pretreatment procedure was developed to partially hydrolyze the plant tissue prior to extraction, releasing the bound 2,4-dichlorophenol residues. Steam distillation showed higher residue levels for field-treated straw samples. This is attributed to the greater degree of hydrolysis inherent in the steam distillation procedure. Supercritical CO2 extraction of field-treated seed samples showed higher levels of 2,4-dichlorophenol residues than did steam distillation. The supercritical fluid extractant was able to solvate 2,4-dichlorophenol residues in the interior of the seed and transport them to the surface for collection. The aqueous medium used in steam distillation was unable to penetrate the hydrophobic seed matrix to the same degree. While the actual extraction time experienced in supercritical fluid extraction was far less than that of steam distillation (45 min vs 6 h, respectively), the total sample preparation time was similar in both methods.

Analysis of Supercritical-Extracted Chelated Metal Ions From Mixed Organic-Inorganic Samples

NASA Technical Reports Server (NTRS)

Sinha, Mahadeva P. (Inventor)

1996-01-01

Organic and inorganic contaminants of an environmental sample are analyzed by the same GC-MS instrument by adding an oxidizing agent to the sample to oxidize metal or metal compounds to form metal ions. The metal ions are converted to chelate complexes and the chelate complexes are extracted into a supercritical fluid such as CO2. The metal chelate extract after flowing through a restrictor tube is directly injected into the ionization chamber of a mass spectrometer, preferably containing a refractory metal filament such as rhenium to fragment the complex to release metal ions which are detected. This provides a fast, economical method for the analysis of metal contaminants in a sample and can be automated. An organic extract of the sample in conventional or supercritical fluid solvents can be detected in the same mass spectrometer, preferably after separation in a supercritical fluid chromatograph.

Diethylstilbestrol in fish tissue determined through subcritical fluid extraction and with GC-MS

NASA Astrophysics Data System (ADS)

Qiao, Qinghui; Shi, Nianrong; Feng, Xiaomei; Lu, Jie; Han, Yuqian; Xue, Changhu

2016-06-01

As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol (DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane (R134a) extraction in combination with gas chromatography-mass spectrometry (GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C18 and NH2 solid phase extraction (SPE). Finally, the analyte was derived by heptafluorobutyric anhydride (HFBA), followed by GC-MS analysis. Response surface methodology (RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26°C; amount of co-solvent volume, 4.7 mL. Under this condition, at a spiked level of 1, 5, 10 μg kg-1, the mean recovery of DES was more than 90% with relative standard deviations (RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.

A New Method of Obtaining High-Resolution Paleoclimate Records from Speleothem Fluid Inclusions

NASA Astrophysics Data System (ADS)

Logan, A. J.; Horton, T. W.

2010-12-01

We present a new method for stable hydrogen and oxygen isotope analysis of ancient drip water trapped within cave speleothems. Our method improves on existing fluid inclusion isotopic analytical techniques in that it decreases the sample size by a factor of ten or more, dramatically improving the spatial and temporal precision of fluid inclusion-based paleoclimatology. Published thermal extraction methods require large samples (c. 150 mg) and temperatures high enough (c. 500-900°C) to cause calcite decomposition, which is also associated with isotopic fractionation of the trapped fluids. Extraction by crushing faces similar challenges, where the failure to extract all the trapped fluid can result in isotopic fractionation, and samples in excess of 500 mg are required. Our new method combines the strengths of these published thermal and crushing methods using continuous-flow isotope ratio analytical techniques. Our method combines relatively low-temperature (~250°C) thermal decrepitation with cryogenic trapping across a switching valve sample loop. In brief, ~20 mg carbonate samples are dried (75°C for >1 hour) and heated (250°C for >1 hour) in a quartz sample chamber under a continuously flowing stream of ultra-high purity helium. Heating of the sample chamber is achieved by use of a tube furnace. Fluids released during the heating step are trapped in a coiled stainless steel cold trap (~ -98°C) serving as the sample loop in a 6-way switching valve. Trapped fluids are subsequently injected into a high-temperature conversion elemental analyzer by switching the valve and rapidly thawing the trap. This approach yielded accurate and precise measurements of injected liquid water IAEA reference materials (GISP; SMOW2; SLAP2) for both hydrogen and oxygen isotopic compositions. Blanking tests performed on the extraction line demonstrate extremely low line-blank peak heights (<50mv). Our tests also demonstrate that complete recovery of liquid water is possible and that a minimum quantity of ~100nL water was required. In contrast to liquid water analyses, carbonate inclusion waters gave highly variable results. As plenty of signal was produced from relatively small sample sizes (~20 mg), the observed isotopic variation most likely reflects fractionation during fluid extraction, or natural isotopic variability. Additional tests and modifications to the extraction procedure are in progress, using a recently collected New Zealand stalagmite from a West Coast cave (DOC collection permit WC-27462-GEO). U-Th age data will accompany a paleoclimate record from this stalagmite obtained using standard carbonate analytical techniques, and compared to the results from our new fluid inclusion analyses.

Antimicrobial activity and composition profile of grape (Vitis vinifera) pomace extracts obtained by supercritical fluids.

PubMed

Oliveira, Daniela A; Salvador, Ana Augusta; Smânia, Artur; Smânia, Elza F A; Maraschin, Marcelo; Ferreira, Sandra R S

2013-04-10

The possibility of increasing the aggregated value of the huge amount of residues generated by wineries around the world foment studies using the grape pomace - the residue from the wine production, composed by seed, skin and stems - to obtain functional ingredients. Nowadays, consumers in general prefer natural and safe products mainly for food and cosmetic fields, where the supercritical fluid extraction is of great importance due to the purity of the extracts provided. Therefore, the objective of this work is to evaluate the global extraction yield, the antimicrobial activity and the composition profile of Merlot and Syrah grape pomace extracts obtained by supercritical CO2 (SC-CO2) and CO2 added with co-solvent at pressures up to 300 bar and temperatures of 50 and 60 °C. The results were compared with the ones obtained by Soxhlet and by ultrasound-assisted leaching extraction methods. The main components from the extracts, identified by HPLC, were gallic acid, p-OH-benzoic acid, vanillic acid and epicatechin. The antibacterial and antifungal activities of the extracts were evaluated using four strains of bacteria (Staphylococcus aureus, Bacillus cereus, Escherichia coli and Pseudomonas aeruginosa) and three fungi strains (Candida albicans, Candida parapsilosis, Candida krusei). Despite lower extraction yield results, the supercritical fluid extracts presented the highest antimicrobial effectiveness compared to the other grape pomace extracts due to the presence of antimicrobial active compounds. Syrah extracts were less efficient against the microorganisms tested and Merlot extracts were more active against Gram-positive bacteria. Copyright © 2012 Elsevier B.V. All rights reserved.

Development of the Fray-Farthing-Chen Cambridge Process: Towards the Sustainable Production of Titanium and Its Alloys

NASA Astrophysics Data System (ADS)

Hu, Di; Dolganov, Aleksei; Ma, Mingchan; Bhattacharya, Biyash; Bishop, Matthew T.; Chen, George Z.

2018-02-01

The Kroll process has been employed for titanium extraction since the 1950s. It is a labour and energy intensive multi-step semi-batch process. The post-extraction processes for making the raw titanium into alloys and products are also excessive, including multiple remelting steps. Invented in the late 1990s, the Fray-Farthing-Chen (FFC) Cambridge process extracts titanium from solid oxides at lower energy consumption via electrochemical reduction in molten salts. Its ability to produce alloys and powders, while retaining the cathode shape also promises energy and material efficient manufacturing. Focusing on titanium and its alloys, this article reviews the recent development of the FFC-Cambridge process in two aspects, (1) resource and process sustainability and (2) advanced post-extraction processing.

Modeling of the Kinetics of Supercritical Fluid Extraction of Lipids from Microalgae with Emphasis on Extract Desorption

PubMed Central

Sovová, Helena; Nobre, Beatriz P.; Palavra, António

2016-01-01

Microalgae contain valuable biologically active lipophilic substances such as omega-3 fatty acids and carotenoids. In contrast to the recovery of vegetable oils from seeds, where the extraction with supercritical CO2 is used as a mild and selective method, economically viable application of this method on similarly soluble oils from microalgae requires, in most cases, much higher pressure. This paper presents and verifies hypothesis that this difference is caused by high adsorption capacity of microalgae. Under the pressures usually applied in supercritical fluid extraction from plants, microalgae bind a large fraction of the extracted oil, while under extremely high CO2 pressures their adsorption capacity diminishes and the extraction rate depends on oil solubility in supercritical CO2. A mathematical model for the extraction from microalgae was derived and applied to literature data on the extraction kinetics in order to determine model parameters. PMID:28773546

Antioxidant activity and sensory evaluation of a rosmarinic acid-enriched extract of Salvia officinalis

USDA-ARS?s Scientific Manuscript database

An extract of S. officinalis (garden sage) was developed using supercritical fluid extraction, followed by hot water extraction. The resulting extract was enriched in polyphenols, including rosmarinic acid (RA), which has shown promising health benefits in animals. The extract contained RA at a conc...

Feasibility/treatability studies for removal of heavy metals from training range soils at the Grafenwoehr Training Area, Germany

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, R.W.

1995-05-01

A feasibility/treatability study was performed to investigate the leaching potential of heavy metals (particularly lead) from soils at the Grafenw6hr Training Area (GTA) in Germany. The study included an evaluation of the effectiveness of chelant extraction to remediate the heavy-metal-contarninated soils. Batch shaker tests indicated that ethylenediaminetetraacetic acid (EDTA) (0.01M) was more effective than citric acid (0.01M) at removing cadmium, copper, lead, and zinc. EDTA and citric acid were equally effective in mobilizing chromium and barium from the soil. The batch shaker technique with chelant extraction offers promise as a remediation technique for heavy-metal-contaninated soil at the GTA. Columnar floodingmore » tests conducted as part of the study revealed that deionized water was the least effective leaching solution for mobilization of the heavy metals; the maximum solubilization obtained was 3.72% for cadmium. EDTA (0.05M) achieved the greatest removal of lead (average removal of 17.6%). The difficulty of extraction using deionized water indicates that all of the heavy metals are very tightly bound to the soil; therefore, they are very stable in the GTA soils and do not pose a serious threat to the groundwater system. Columnar flooding probably does not represent a viable remediation technique for in-situ cleanup of heavy-metal-contaminated soils at the GTA.« less

Method and turbine for extracting kinetic energy from a stream of two-phase fluid

NASA Technical Reports Server (NTRS)

Elliott, D. G. (Inventor)

1979-01-01

An axial flow separator turbine is described which includes a number of nozzles for delivering streams of a two-phase fluid along linear paths. A phase separator which responsively separates the vapor and liquid is characterized by concentrically related annuli supported for rotation within the paths. The separator has endless channels for confining the liquid under the influence of centrifugal forces. A vapor turbine fan extracts kinetic energy from the liquid. Angular momentum of both the liquid phase and the vapor phase of the fluid is converted to torque.

Properties of structural panels fabricated from bioremediated CCA-treated wood: pilot scale

Treesearch

Carol A. Clausen; James H. Muehl; Andrzej M. Krzysik

2006-01-01

Particleboard and flakeboard panels were fabricated from remediated CCA-treated southern yellow pine. Treated wood, flaked or comminuted into particles, was remediated in 12-kg batches using oxalic acid extraction, followed by bioleaching with the metal-tolerant bacterium Bacillus licheniformis. Remediation resulted in removal of 80 percent Cu, 71 percent Cr, and 89...

Supercritical fluid extraction and analysis of compounds from Clivia miniata for uterotonic activity.

PubMed

Sewram, V; Raynor, M W; Mulholland, D A; Raidoo, D M

2001-07-01

In this descriptive study, the superciritical fluid extract of the roots of Clivia miniata L. was tested for uterotonic activity using guinea pig uterine smooth muscle in vitro. Extraction was performed with water modified supercritical carbon dioxide at 400 atm and 80 degrees C. The uterine contractions induced by this extract were compared to those induced by the aqueous extract and found to be active at lower doses. The active compounds were isolated and the structures elucidated by spectroscopic and chromatographic techniques. Both linoleic acid and 5-hydroxymethyl-2-furancarboxaldehyde isolated from the extract were found to induce muscle contractions individually. The pharmacological mode of action of 5-hydroxymethyl-2-furancarboxaldehyde was assessed using two receptor agonists and antagonists. This compound was found to mediate its effect through cholinergic receptors.

The Application of Chinese High-Spatial Remote Sensing Satellite Image in Land Law Enforcement Information Extraction

NASA Astrophysics Data System (ADS)

Wang, N.; Yang, R.

2018-04-01

Chinese high -resolution (HR) remote sensing satellites have made huge leap in the past decade. Commercial satellite datasets, such as GF-1, GF-2 and ZY-3 images, the panchromatic images (PAN) resolution of them are 2 m, 1 m and 2.1 m and the multispectral images (MS) resolution are 8 m, 4 m, 5.8 m respectively have been emerged in recent years. Chinese HR satellite imagery has been free downloaded for public welfare purposes using. Local government began to employ more professional technician to improve traditional land management technology. This paper focused on analysing the actual requirements of the applications in government land law enforcement in Guangxi Autonomous Region. 66 counties in Guangxi Autonomous Region were selected for illegal land utilization spot extraction with fusion Chinese HR images. The procedure contains: A. Defines illegal land utilization spot type. B. Data collection, GF-1, GF-2, and ZY-3 datasets were acquired in the first half year of 2016 and other auxiliary data were collected in 2015. C. Batch process, HR images were collected for batch preprocessing through ENVI/IDL tool. D. Illegal land utilization spot extraction by visual interpretation. E. Obtaining attribute data with ArcGIS Geoprocessor (GP) model. F. Thematic mapping and surveying. Through analysing 42 counties results, law enforcement officials found 1092 illegal land using spots and 16 suspicious illegal mining spots. The results show that Chinese HR satellite images have great potential for feature information extraction and the processing procedure appears robust.

Influence of the soil/solution ratio, interaction time, and extractant on the evaluation of iron chelate sorption/desorption by soils.

PubMed

Hernández-Apaolaza, Lourdes; Lucena, Juan J

2011-03-23

Synthetic Fe chelates are the most efficient agricultural practice to control Fe deficiency in crops, EDTA/Fe3+ and o,o-EDDHA/Fe3+ being the most commonly used. Their efficacy as Fe sources and carriers in soils can be severely limited by their retention on it. The aim of this work is to evaluate the possible bias introduced in the studies of the iron chelate retention by soils. For that purpose, results obtained for EDTA and EDDHA iron chelates from two batch studies with different soil/solution ratios were compared with data obtained for a leaching column experiment. Moreover, different extractants were tested to study the o,o-EDDHA/Fe3+ and o,p-EDDHA/Fe3+ desorption from a calcareous soil, and also the effect of the interaction time in their retention process has been evaluated. In summary, the mobility through a calcareous soil of the studied iron chelates differs greatly depending on the type of iron chelate and also on the procedure used to evaluate the retention and the soil/solution ratio used. In general, the leaching column method is preferred because the achieved conclusions are more representative of the natural conditions, but batch methods are very useful as a preliminary experiment, especially one with a high soil/solution ratio. The iron chelate desorption could be quantified by using a sequential extraction with water, sodium sulfate, and DTPA as extractants. Under the experimental conditions used in this study, o,o-EDDHA/Fe3+ retention increased with interaction time.

Methodology for extracting local constants from petroleum cracking flows

DOEpatents

Chang, Shen-Lin; Lottes, Steven A.; Zhou, Chenn Q.

2000-01-01

A methodology provides for the extraction of local chemical kinetic model constants for use in a reacting flow computational fluid dynamics (CFD) computer code with chemical kinetic computations to optimize the operating conditions or design of the system, including retrofit design improvements to existing systems. The coupled CFD and kinetic computer code are used in combination with data obtained from a matrix of experimental tests to extract the kinetic constants. Local fluid dynamic effects are implicitly included in the extracted local kinetic constants for each particular application system to which the methodology is applied. The extracted local kinetic model constants work well over a fairly broad range of operating conditions for specific and complex reaction sets in specific and complex reactor systems. While disclosed in terms of use in a Fluid Catalytic Cracking (FCC) riser, the inventive methodology has application in virtually any reaction set to extract constants for any particular application and reaction set formulation. The methodology includes the step of: (1) selecting the test data sets for various conditions; (2) establishing the general trend of the parametric effect on the measured product yields; (3) calculating product yields for the selected test conditions using coupled computational fluid dynamics and chemical kinetics; (4) adjusting the local kinetic constants to match calculated product yields with experimental data; and (5) validating the determined set of local kinetic constants by comparing the calculated results with experimental data from additional test runs at different operating conditions.

High throughput screening and antioxidant assay of dibenzo[a,c]cyclooctadiene lignans in modified-ultrasonic and supercritical fluid extracts of Schisandra chinensis Baill by liquid chromatography--mass spectrometry and a free radical-scavenging method.

PubMed

Wang, Ming-Chih; Lai, Yih-Cherng; Chang, Chia-Lin

2008-05-01

Dibenzo[a,c]cyclooctadiene lignans of Schisandra chinensis Baill are well known because of their hepatoprotective activity, antioxidant activity, and anticancer effect. For the isolation of the dibenzo[a,c]cyclooctadiene lignans of Schisandra chinensis Baill two extraction methods were used: modified-ultrasonic extraction and supercritical fluid extraction. A specific and fast analytical method for structure identification is established for quality control because structure elucidation could be accomplished by means of liquid chromatography-mass spectrometry (LC-MS) technologies. The separation and identification of the compounds were completed by: (i) a water-acetonitrile gradient system using a C18 reversed-phase column; (ii) UV detection at 225 nm; (iii) MS/MS experiments with electrospray ionization interface (ESI) ion trap mass spectrometry in the positive mode. Normalized collision energy was used to obtain fragment ions of structural relevance in the LC-MS/MS. These results provided a reliable LC-MS/MS method for the determination of the dibenzo[a,c]cyclooctadiene lignans from Schisandra chinensis Baill. Finally, we also detected 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging effects (%) of the modified-ultrasonic and supercritical fluid extracts of Schisandra chinensis Baill compared with 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (Trolox). The antioxidant activities of the modified-ultrasonic and supercritical fluid extracts were lower than that of trolox.

Helium measurements of pore fluids obtained from the San Andreas Fault Observatory at Depth (SAFOD, USA) drill cores

NASA Astrophysics Data System (ADS)

Ali, S.; Stute, M.; Torgersen, T.; Winckler, G.; Kennedy, B. M.

2011-02-01

4He accumulated in fluids is a well established geochemical tracer used to study crustal fluid dynamics. Direct fluid samples are not always collectable; therefore, a method to extract rare gases from matrix fluids of whole rocks by diffusion has been adapted. Helium was measured on matrix fluids extracted from sandstones and mudstones recovered during the San Andreas Fault Observatory at Depth (SAFOD) drilling in California, USA. Samples were typically collected as subcores or from drillcore fragments. Helium concentration and isotope ratios were measured 4-6 times on each sample, and indicate a bulk 4He diffusion coefficient of 3.5 ± 1.3 × 10-8 cm2 s-1 at 21°C, compared to previously published diffusion coefficients of 1.2 × 10-18 cm2 s-1 (21°C) to 3.0 × 10-15 cm2 s-1 (150°C) in the sands and clays. Correcting the diffusion coefficient of 4Hewater for matrix porosity (˜3%) and tortuosity (˜6-13) produces effective diffusion coefficients of 1 × 10-8 cm2 s-1 (21°C) and 1 × 10-7 (120°C), effectively isolating pore fluid 4He from the 4He contained in the rock matrix. Model calculations indicate that <6% of helium initially dissolved in pore fluids was lost during the sampling process. Complete and quantitative extraction of the pore fluids provide minimum in situ porosity values for sandstones 2.8 ± 0.4% (SD, n = 4) and mudstones 3.1 ± 0.8% (SD, n = 4).

Activity and immunodetection of lysozyme in earthworm Dendrobaena veneta (Annelida).

PubMed

Fiołka, Marta J; Zagaja, Mirosław P; Hułas-Stasiak, Monika; Wielbo, Jerzy

2012-01-01

In the present study, lysozyme-like activity against Micrococcus luteus was detected in the coelomic fluid, the extract from coelomocytes, intestine and in the homogenates from cocoons of Dendrobaena veneta. Four hours after immunization with Escherichia coli, the lysozyme activity in the coelomic fluid increased about three times and in the extract of coelomocytes - four times, in comparison to the control. In three cases: of the coelomic fluid, the homogenates from cocoons and the extract from coelomocytes, the antibody against HEWL (hen egg white lysozyme) recognized only one protein with a molecular mass of about 14.4 kDa. In the coelomic fluid, apart from the protein with molecular mass of 14.4 kDa the antibody directed against human lysozyme recognized an additional protein of 22 kDa. Using the bioautography technique after electrophoretic resolution of native proteins in acidic polyacrylamide gels, two lytic zones of M. luteus were observed in the case of the coelomic fluid and three after the analysis of the extract of coelomocytes and the egg homogenates. The results indicated the existence of several forms of lysozyme with a different electric charge in the analyzed D. veneta samples. The highest lysozyme activity in the intestine of D. veneta was observed in the midgut. The antibody directed against human lysozyme indicated a strong positive signal in epidermal and midgut cells of earthworm. Copyright © 2011 Elsevier Inc. All rights reserved.

Determination of in vitro isoflavone degradation in rumen fluid.

PubMed

Trnková, Andrea; Šancová, Kateřina; Zapletalová, Martina; Kašparovská, Jitka; Dadáková, Kateřina; Křížová, Ludmila; Lochman, Jan; Hadrová, Sylvie; Ihnatová, Ivana; Kašparovský, Tomáš

2018-06-01

The aim of this study was to determine the degradation of dietary isoflavones in rumen fluid under 2 feeding regimens. The experiments were performed in vitro using a rumen fluid buffer system. The rumen fluid was taken from cows fed either a hay diet or a concentrate-rich diet (the diet consisted of 34.6% maize silage, 17.6% haylage, 12.8% alfalfa hay, and 35.0% supplemental mixture on a dry matter basis). As a source of isoflavones, 40% soybean extract (Biomedica, Prague, Czech Republic) at levels of 5, 25, 50, and 75 mg per 40 mL of rumen fluid was used. Samples of soybean extract were incubated in triplicate at 39°C for 0, 3.0, 6.0, 12.0, and 24.0 h in incubation solution. The metabolism of daidzein and genistein was faster under concentrate-rich diet conditions. In general, production of equol started after 3 to 6 h of incubation and reached the highest rate after approximately 12 h of incubation regardless of the type of diet or concentration of extract. In most of the experiments, production of equol continued after 24 h of incubation. Generally, equol production was greater under the hay diet conditions. Furthermore, experiments with higher amounts of added soybean extract revealed possible inhibitory effects of high levels of isoflavones on the rumen microflora. Copyright © 2018 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Method and apparatus for back-extracting metal chelates

DOEpatents

Wai, C.M.; Smart, N.G.; Lin, Y.

1998-08-11

A method is described for extracting metal and metalloid species from a solid or liquid substrate using a supercritical fluid solvent containing one or more chelating agents followed by back-extracting the metal and metalloid species from the metal and metalloid chelates formed thereby. The back-extraction acidic solution is performed utilizing an acidic solution. Upon sufficient exposure of the metal and metalloid chelates to the acidic solution, the metal and metalloid species are released from the chelates into the acid solution, while the chelating agent remains in the supercritical fluid solvent. The chelating agent is thereby regenerated and the metal and metalloid species recovered. 3 figs.

A Comprehensive Strategy to Construct In-house Database for Accurate and Batch Identification of Small Molecular Metabolites.

PubMed

Zhao, Xinjie; Zeng, Zhongda; Chen, Aiming; Lu, Xin; Zhao, Chunxia; Hu, Chunxiu; Zhou, Lina; Liu, Xinyu; Wang, Xiaolin; Hou, Xiaoli; Ye, Yaorui; Xu, Guowang

2018-05-29

Identification of the metabolites is an essential step in metabolomics study to interpret regulatory mechanism of pathological and physiological processes. However, it is still a big headache in LC-MSn-based studies because of the complexity of mass spectrometry, chemical diversity of metabolites, and deficiency of standards database. In this work, a comprehensive strategy is developed for accurate and batch metabolite identification in non-targeted metabolomics studies. First, a well defined procedure was applied to generate reliable and standard LC-MS2 data including tR, MS1 and MS2 information at a standard operational procedure (SOP). An in-house database including about 2000 metabolites was constructed and used to identify the metabolites in non-targeted metabolic profiling by retention time calibration using internal standards, precursor ion alignment and ion fusion, auto-MS2 information extraction and selection, and database batch searching and scoring. As an application example, a pooled serum sample was analyzed to deliver the strategy, 202 metabolites were identified in the positive ion mode. It shows our strategy is useful for LC-MSn-based non-targeted metabolomics study.

Fermentation Kinetics and Continuous Process of L-Asparaginase Production

PubMed Central

Liu, F. S.; Zajic, J. E.

1973-01-01

For the purpose of obtaining L-asparaginase in quantities from Erwinia aroideae, cell growth and enzyme formation were investigated in both batch and continuous fermentation. Using yeast extract as a growth-limiting substrate, the relationship between specific growth rate and substrate concentration was found to fit the Monod equation. The optimum temperature for enzyme production was 24 C, although cell growth was higher at 28 C. The enzyme yield reached its maximum of 4 IU/ml during the negative acceleration growth phase which occurs just prior to stationary growth. Compared to batch fermentations, the continuous fermentation process gave a lower enzyme yield except when the fermentation was conducted at a dilution rate of 0.1 hr-1. The graphical method frequently used for prediction of continuous fermentation does not apply to L-asparaginase production by E. aroideae. The optimum temperature for enzyme production in continuous process was 24 C, which was the same as in batch process. Increasing the temperature from 24 to 28 C resulted in a 20% loss of enzyme yield. PMID:4568894

Production of acetone butanol (AB) from liquefied corn starch, a commercial substrate, using Clostridium beijerinckii coupled with product recovery by gas stripping.

PubMed

Ezeji, Thaddeus C; Qureshi, Nasib; Blaschek, Hans P

2007-12-01

A potential industrial substrate (liquefied corn starch; LCS) has been employed for successful acetone butanol ethanol (ABE) production. Fermentation of LCS (60 g l(-1)) in a batch process resulted in the production of 18.4 g l(-1) ABE, comparable to glucose: yeast extract based medium (control experiment, 18.6 g l(-1) ABE). A batch fermentation of LCS integrated with product recovery resulted in 92% utilization of sugars present in the feed. When ABE was recovered by gas stripping (to relieve inhibition) from the fed-batch reactor fed with saccharified liquefied cornstarch (SLCS), 81.3 g l(-1) ABE was produced compared to 18.6 g l(-1) (control). In this integrated system, 225.8 g l(-1) SLCS sugar (487 % of control) was consumed. In the absence of product removal, it is not possible for C. beijerinckii BA101 to utilize more than 46 g l(-1) glucose. A combination of fermentation of this novel substrate (LCS) to butanol together with product recovery by gas stripping may economically benefit this fermentation.

Development and application of computer assisted optimal method for treatment of femoral neck fracture.

PubMed

Wang, Monan; Zhang, Kai; Yang, Ning

2018-04-09

To help doctors decide their treatment from the aspect of mechanical analysis, the work built a computer assisted optimal system for treatment of femoral neck fracture oriented to clinical application. The whole system encompassed the following three parts: Preprocessing module, finite element mechanical analysis module, post processing module. Preprocessing module included parametric modeling of bone, parametric modeling of fracture face, parametric modeling of fixed screw and fixed position and input and transmission of model parameters. Finite element mechanical analysis module included grid division, element type setting, material property setting, contact setting, constraint and load setting, analysis method setting and batch processing operation. Post processing module included extraction and display of batch processing operation results, image generation of batch processing operation, optimal program operation and optimal result display. The system implemented the whole operations from input of fracture parameters to output of the optimal fixed plan according to specific patient real fracture parameter and optimal rules, which demonstrated the effectiveness of the system. Meanwhile, the system had a friendly interface, simple operation and could improve the system function quickly through modifying single module.

Bi-directionally draining pore fluid extraction vessel

DOEpatents

Prizio, Joseph; Ritt, Alexander; Mower, Timothy E.; Rodine, Lonn

1991-01-01

The invention is used to extract pore fluid from porous solids through a combination of mechanical compression and inert-gas injection and comprises a piston for axially compressing samples to force water out, and top and bottom drainage plates for capturing the exuded water and using inert gas to force water to exit when the limits of mechanical compression have been reached.

Integration of phase separation with ultrasound-assisted salt-induced liquid-liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography.

PubMed

Wang, Huili; Gao, Ming; Wang, Mei; Zhang, Rongbo; Wang, Wenwei; Dahlgren, Randy A; Wang, Xuedong

2015-03-15

Herein, we developed a novel integrated device to perform phase separation based on ultrasound-assisted salt-induced liquid-liquid microextraction for determination of five fluoroquinones (FQs) in human body fluids. The integrated device consisted of three simple HDPE components used to separate the extraction solvent from the aqueous phase prior to retrieving the extractant. A series of extraction parameters were optimized using the response surface method based on central composite design. Optimal conditions consisted of 945μL acetone extraction solvent, pH 2.1, 4.1min stir time, 5.9g Na2SO4, and 4.0min centrifugation. Under optimized conditions, the limits of detection (at S/N=3) were 0.12-0.66μgL(-1), the linear range was 0.5-500μgL(-1) and recoveries were 92.6-110.9% for the five FQs extracted from plasma and urine. The proposed method has several advantages, such as easy construction from inexpensive materials, high extraction efficiency, short extraction time, and compatibility with HPLC analysis. Thus, this method shows excellent prospects for sample pretreatment and analysis of FQs in human body fluids. Copyright © 2015 Elsevier B.V. All rights reserved.

Instrument for Analysis of Organic Compounds on Other Planets

NASA Technical Reports Server (NTRS)

Daulton, Riley M.; Hintze, Paul E.

2016-01-01

The goal of this project is to develop the Instrument for Solvent Extraction and Analysis of Extraterrestrial Bodies using In Situ Resources (ISEE). Specifically, ISEE will extract and characterize organic compounds from regolith which is found on the surface of other planets or asteroids. The techniques this instrument will use are supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC). ISEE aligns with NASA's goal to expand the frontiers of knowledge, capability, and opportunities in space in addition to supporting NASA's aim to search for life elsewhere by characterizing organic compounds. The outcome of this project will be conceptual designs of 2 components of the ISEE instrument as well as the completion of proof-of-concept extraction experiments to demonstrate the capabilities of SFE. The first conceptual design is a pressure vessel to be used for the extraction of the organic compounds from the regolith. This includes a comparison of different materials, geometry's, and a proposition of how to insert the regolith into the vessel. The second conceptual design identifies commercially available fluid pumps based on the requirements needed to generate supercritical CO2. The proof-of-concept extraction results show the percent mass lost during standard solvent extractions of regolith with organic compounds. This data will be compared to SFE results to demonstrate the capabilities of ISEE's approach.

Mechanistic study of lead desorption during the leaching process of ion-absorbed rare earths: pH effect and the column experiment

NASA Astrophysics Data System (ADS)

Xue, Q.; Tang, J., Sr.; Chen, H.

2017-12-01

High concentrations of ammonium sulfate, often used in the in-situ mining process, can result in a decrease of pH in the environment and dissolution of rare earth metals. Ammonium sulfate can also cause desorption of toxic heavy metals, leading to environmental and human health implications. In this study, the desorption behavior and fraction changes of lead in the ion-absorbed rare earth ore were studied using batch desorption experiments and column leaching tests. Results from batch desorption experiments showed that the desorption process of lead included fast and slow stages, and followed an Elovich model well. The desorption rate and the proportion of lead content in the solution to the total lead in the soil were observed to increase with a decrease in the initial pH of the ammonium sulfate solution. The lead in soil included an acid extractable fraction, reducible fraction, oxidizable fraction, and a residual fraction, with the predominant fractions being the reducible and acid extractable fractions. 96% of the extractable fraction in soil were desorbed into solution at pH=3.0, and the content of the reducible fraction was observed to initially increase (when pH>4.0) and then decrease (when pH<4.0) with a decrease in pH. Column leaching tests indicated that the content of lead in the different fractions of soil followed the trend of reducible fraction > oxidizable fraction > acid extractable fraction > residual fraction after the simulating leaching mining process. The change in pH was also found to have a larger influence on the acid extractable and reducible fractions than the other two fractions. The proportion of the extractable fraction being leached was ca. 86%, and the reducible fraction was enriched along the migration direction of the leaching liquid. These results suggest that certain lead fractions may desorb again and contaminate the environment via acid rain, which provides significant information for environmental assessment and remediation after mining process.

Efficient production of ε-poly-L-lysine by Streptomyces ahygroscopicus using one-stage pH control fed-batch fermentation coupled with nutrient feeding.

PubMed

Liu, Sheng-Rong; Wu, Qing-Ping; Zhang, Ju-Mei; Mo, Shu-Ping

2015-03-01

ε-Poly-L-lysine (ε-PL) is a homopolymer of L-lysine molecules connected between the ε amino and alpha carboxyl groups. This polymer is currently used as a natural preservative in food. Insufficient biomass is a major problem in ε-PL fermentation. Here, to improve cell growth and ε-PL productivity, various nitrogen-rich nutrients were supplemented into flask cultures after 16 h cultivation, marking the onset of ε-PL biosynthesis. Yeast extract, soybean powder, corn powder, and beef extract significantly improved cell growth. In terms of ε-PL productivity, yeast extract at 0.5% (w/v) gave the maximum yield (2.24 g/l), 115.4% higher than the control (1.04 g/l), followed by soybean powder (1.86 g/l) at 1% (w/v) and corn powder (1.72 g/l) at 1% (w/v). However, supplementation with beef extract inhibited ε-PL production. The optimal time for supplementation for all nutrients examined was at 16 h cultivation. The kinetics of yeast-extract-supplemented cultures showed enhanced cell growth and production duration. Thus, the most commonly used two-stage pH control fed-batch fermentation method was modified by omitting the pH 5.0-controlled period, and coupling the procedure with nutrient feeding in the pH 3.9-controlled phase. Using this process, by continuously feeding 0.5 g/h of yeast extract, soybean powder, or corn powder into cultures in a 30 L fermenter, the final ε-PL titer reached 28.2 g/l, 23.7 g/l, and 21.4 g/l, respectively, 91.8%, 61.2%, and 45.6% higher than that of the control (14.7 g/l). This describes a promising option for the mass production of ε-PL.

Off-flavors removal and storage improvement of mackerel viscera by supercritical carbon dioxide extraction.

PubMed

Lee, Min Kyung; Uddin, M Salim; Chun, Byung Soo

2008-07-01

The oil in mackerel viscera was extracted by supercritical carbon dioxide (SCO2) at a semi-batch flow extraction process and the fatty acids composition in the oil was identified. Also the off-flavors removal in mackerel viscera and the storage improvement of the oils were carried out. As results obtained, by increasing pressure and temperature, quantity was increased. The maximum yield of oils obtained from mackerel viscera by SCO, extraction was 118 mgg(-1) (base on dry weight of freeze-dried raw anchovy) at 50 degrees C, 350 bar And the extracted oil contained high concentration of EPA and DHA. Also it was found that the autoxidation of the oils using SCO2 extraction occurred very slowly compared to the oils by organic solvent extraction. The off-flavors in the powder after SCO2 extraction were significantly removed. Especially complete removal of the trimethylamine which influences a negative compound to the products showed. Also other significant off-flavors such as aldehydes, sulfur-containing compounds, ketones, acids or alcohols were removed by the extraction.

Effects of dissolved CO2 on Shallow Freshwater Microbial Communities simulating a CO2 Leakage Scenario

NASA Astrophysics Data System (ADS)

Gulliver, D. M.; Lowry, G. V.; Gregory, K.

2013-12-01

Geological carbon sequestration is likely to be part of a comprehensive strategy to minimize the atmospheric release of greenhouse gasses, establishing a concern of sequestered CO2 leakage into overlying potable aquifers. Leaking CO2 may affect existing biogeochemical processes and therefore water quality. There is a critical need to understand the evolution of CO2 exposed microbial communities that influence the biogeochemistry in these freshwater aquifers. The evolution of microbial ecology for different CO2 exposure concentrations was investigated using fluid-slurry samples obtained from a shallow freshwater aquifer (55 m depth, 0.5 MPa, 22 °C, Escatawpa, MS). The microbial community of well samples upstream and downstream of CO2 injection was characterized. In addition, batch vessel experiments were conducted with the upstream aquifer samples exposed to varying pCO2 from 0% to 100% under reservoir temperature and pressure for up to 56 days. The microbial community of the in situ experiment and the batch reactor experiment were analyzed with 16S rRNA clone libraries and qPCR. In both the in situ experiment and the batch reactor experiment, DNA concentration did not correlate with CO2 exposure. Both the in situ experiment and the batch reactors displayed a changing microbial community with increased CO2 exposure. The well water isolate, Curvibacter, appeared to be the most tolerant genus to high CO2 concentrations in the in situ experiments and to mid-CO2 concentrations in the batch reactors. In batch reactors with pCO2 concentrations higher than experienced in situ (pCO2 = 0.5 MPa), Pseudomonas appeared to be the most tolerant genus. Findings provide insight into a dynamic biogeochemical system that will alter with CO2 exposure. Adapted microbial populations will eventually give rise to the community that will impact the metal mobility and water quality. Knowledge of the surviving microbial populations will enable improved models for predicting the fate of CO2 following leakage and lead to better strategies for ensuring the quality of potable aquifer water.

Mathematical model of simple spalling formation during coal cutting with extracting machine

NASA Astrophysics Data System (ADS)

Gabov, V. V.; Zadkov, D. A.

2018-05-01

A single-mass model of a rotor shearer is analyzed. It is shown that rotor mining machines has large inertia moments and load dynamics. An extraction module model with selective movement of the cutting tool is represented. The peculiar feature of such extracting machines is fluid power drive cutter mechanism. They can steadily operate at large shear thickness, and locking modes are not an emergency for them. Comparing with shearers they have less inertional mass, but slower average cutting speed, and its momentary values depend on load. Basing on the equation of hydraulic fuel consumption balance the work of fluid power drive of extracting module cutter mechanism together with hydro pneumatic accumulator is analyzed. Spalling formation model during coal cutting with fluid power drive cutter mechanism and potential energy stores are suggested. Matching cutter speed with the speed of main crack expansion and amount of potential energy consumption, cutter load is determined only by ultimate stress at crack pole and friction. Tests of an extracting module cutter in real size model proved the stated theory.

Software Aids Visualization of Computed Unsteady Flow

NASA Technical Reports Server (NTRS)

Kao, David; Kenwright, David

2003-01-01

Unsteady Flow Analysis Toolkit (UFAT) is a computer program that synthesizes motions of time-dependent flows represented by very large sets of data generated in computational fluid dynamics simulations. Prior to the development of UFAT, it was necessary to rely on static, single-snapshot depictions of time-dependent flows generated by flow-visualization software designed for steady flows. Whereas it typically takes weeks to analyze the results of a largescale unsteady-flow simulation by use of steady-flow visualization software, the analysis time is reduced to hours when UFAT is used. UFAT can be used to generate graphical objects of flow visualization results using multi-block curvilinear grids in the format of a previously developed NASA data-visualization program, PLOT3D. These graphical objects can be rendered using FAST, another popular flow visualization software developed at NASA. Flow-visualization techniques that can be exploited by use of UFAT include time-dependent tracking of particles, detection of vortex cores, extractions of stream ribbons and surfaces, and tetrahedral decomposition for optimal particle tracking. Unique computational features of UFAT include capabilities for automatic (batch) processing, restart, memory mapping, and parallel processing. These capabilities significantly reduce analysis time and storage requirements, relative to those of prior flow-visualization software. UFAT can be executed on a variety of supercomputers.

Fluid extraction across pumping and permeable walls in the viscous limit

NASA Astrophysics Data System (ADS)

Herschlag, G.; Liu, J.-G.; Layton, A. T.

2016-04-01

In biological transport mechanisms such as insect respiration and renal filtration, fluid travels along a leaky channel allowing material exchange with systems exterior to the channel. The channels in these systems may undergo peristaltic pumping which is thought to enhance the material exchange. To date, little analytic work has been done to study the effect of pumping on material extraction across the channel walls. In this paper, we examine a fluid extraction model in which fluid flowing through a leaky channel is exchanged with fluid in a reservoir. The channel walls are allowed to contract and expand uniformly, simulating a pumping mechanism. In order to efficiently determine solutions of the model, we derive a formal power series solution for the Stokes equations in a finite channel with uniformly contracting/expanding permeable walls. This flow has been well studied in the case in which the normal velocity at the channel walls is proportional to the wall velocity. In contrast we do not assume flow that is proportional to the wall velocity, but flow that is driven by hydrostatic pressure, and we use Darcy's law to close our system for normal wall velocity. We incorporate our flow solution into a model that tracks the material pressure exterior to the channel. We use this model to examine flux across the channel-reservoir barrier and demonstrate that pumping can either enhance or impede fluid extraction across channel walls. We find that associated with each set of physical flow and pumping parameters, there are optimal reservoir conditions that maximize the amount of material flowing from the channel into the reservoir.

Characterization via liquid chromatography coupled to diode array detector and tandem mass spectrometry of supercritical fluid antioxidant extracts of Spirulina platensis microalga.

PubMed

Mendiola, Jose A; Marín, Francisco R; Hernández, S Francisco; Arredondo, Bertha O; Señoráns, F Javier; Ibañez, Elena; Reglero, Guillermo

2005-06-01

Spirulina platensis microalga has been extracted on a pilot scale plant using supercritical fluid extraction (SFE) under various extraction conditions. The extraction yield and the antioxidant activity of the extracts were evaluated in order to select those extracts with both the highest antioxidant capacity and a good extraction yield. These extracts were characterized using LC coupled to diode array detection (DAD) and LC coupled to mass spectrometry (MS) with two different interfaces, atmospheric pressure chemical ionization (APCI) and electrospray (ESI) which allowed us to perform tandem MS by using an ion trap analyzer. The best extraction conditions were as follows: CO2 with 10% of modifier (ethanol) as extraction solvent, 55 degrees C (extraction temperature) and 220 bar (extraction pressure). Fractionation was achieved by cascade depressurization providing two extracts with different activity and chemical composition. Several compounds have been identified in the extracts, corresponding to different carotenoids previously identified in Spirulina platensis microalga along with chlorophyll a and some degradation products. Also, the structure of some phenolic compounds could be tentatively identified. The antioxidant activity of the extracts could be attributed to some of the above mentioned compounds.

Functional Ginger Extracts from Supercritical Fluid Carbon Dioxide Extraction via In Vitro and In Vivo Assays: Antioxidation, Antimicroorganism, and Mice Xenografts Models

PubMed Central

Lee, Chih-Chen; Chiou, Li-Yu; Wang, Jheng-Yang; Chou, Sin-You; Lan, John Chi-Wei; Huang, Tsi-Shu; Huang, Kuo-Chuan

2013-01-01

Supercritical fluid carbon dioxide extraction technology was developed to gain the active components from a Taiwan native plant, Zingiber officinale (ginger). We studied the biological effects of ginger extracts via multiple assays and demonstrated the biofunctions in each platform. Investigations of ginger extracts indicated antioxidative properties in dose-dependant manners on radical scavenging activities, reducing powers and metal chelating powers. We found that ginger extracts processed moderate scavenging values, middle metal chelating levels, and slight ferric reducing powers. The antibacterial susceptibility of ginger extracts on Staphylococcus aureus, Streptococcus sobrinus, S. mutans, and Escherichia coli was determined with the broth microdilution method technique. The ginger extracts had operative antimicroorganism potentials against both Gram-positive and Gram-negative bacteria. We further discovered the strong inhibitions of ginger extracts on lethal carcinogenic melanoma through in vivo xenograft model. To sum up, the data confirmed the possible applications as medical cosmetology agents, pharmaceutical antibiotics, and food supplements. PMID:23983624

Comparison of the bioavailability of elemental waste laden soils using in vivo and in vitro analytical methodology and refinement of exposure/dose models. 1998 annual progress report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lioy, P.J.; Gallo, M.; Georgopoulos, P.

1998-06-01

'The authors hypotheses are: (1) the more closely the synthetic, in vitro, extractant mimics the extraction properties of the human digestive bio-fluids, the more accurate will be the estimate of an internal dose; (2) performance can be evaluated by in vivo studies with a rat model and quantitative examination of a mass balance, calculation and dose estimates from model simulations for the in vitro and in vivo system; and (3) the concentration of the elements Pb, Cd, Cr and selected Radionuclides present in the bioavailable fraction obtained with a synthetic extraction system will be a better indicator of contaminant ingestionmore » from a contaminated soil because it represents the portion of the mass which can yield exposure, uptake and then the internal dose to an individual. As of April 15, 1998, they have made significant progress in the development of a unified approach to the examination of bioavailability and bioaccessibility of elemental contamination of soils for the ingestion route of exposure. This includes the initial characterization of the soil, in vitro measurements of bioaccessibility, and in vivo measurements of bioavailability. They have identified the basic chemical and microbiological characteristics of waste laden soils. These have been used to prioritize the soils for potential mobility of the trace elements present in the soil. Subsequently they have employed a mass balance technique, which for the first time tracked the movement and distribution of elements through an in vitro or in vivo experimental protocol to define the bioaccessible and the bioavailable fractions of digested soil. The basic mass balance equation for the in vitro system is: MT = MSGJ + MIJ + MR. where MT is the total mass extractable by a specific method, MSGJ, is the mass extracted by the saliva and the gastric juices, MIJ is the mass extracted by the intestinal fluid, and MR is the unextractable portion of the initial mass. The above is based upon the use of a synthetic digestive bio-fluids model that includes the saliva, gastric juices, and intestinal fluids. The system has been devised to sequentially extract elements from soil by starting with an extraction by the saliva and carrying the entire mixture to the subsequent bio-fluids for further extraction. The residence time of the soil in each extractant and the liquid to mass ratio in the gastric juices are based upon typical values known for the human digestive system. Experiments were conducted to examine the sensitivity of the extractions to changes in these major variables. The results indicated the lack of significant extraction after 2 h of residence in gastric fluid. The range of variation of the liquid to mass ratio was element dependent over the interval 100:1 and 5,000:1. The final values used for the extraction protocol were: 2 h residence time , and a ratio of 1,000:1. Details of the chemical composition of the extraction protocol are found in Hamel, 1998.'« less

Supercritical Fluid Extraction of Bioactive Compounds from Plant Materials.

PubMed

Wrona, Olga; Rafińska, Katarzyna; Możeński, Cezary; Buszewski, Bogusław

2017-11-01

There has been growing interest in the application of supercritical solvents over the last several years, many of the applications industrial in nature. The purpose of plant material extraction is to obtain large amounts of extract rich in the desired active compounds in a time-sensitive and cost-effective manner. The productivity and profitability of a supercritical fluid extraction (SFE) process largely depends on the selection of process parameters, which are elaborated upon in this paper. Carbon dioxide (CO2) is the most desirable solvent for the supercritical extraction of natural products. Its near-ambient critical temperature makes it suitable for the extraction of thermolabile components without degradation. A new approach has been adopted for SFE in which the solubility of nonpolar supercritical CO2 can be enhanced by the addition of small amounts of cosolvent.

Effects of Moringa oleifera seed extract on rumen fermentation in vitro.

PubMed

Hoffmann, E M; Muetzel, S; Becker, K

2003-02-01

Moringa oleifera is a pantropical tree of the family Moringaceae. A previously undescribed property of an aqueous extract from the seeds of this plant is the modulation of ruminal fermentation patterns, especially protein degradation, as demonstrated in a short-term batch incubation system. Gas, short chain fatty acids (SCFA) and cellulolytic enzyme activities were determined as general fermentation parameters. A dot blot assay able to directly detect true protein in rumen fluid samples was used to quantify protein degradation. For complex substrates the interpretation of protein degradation profiles was amended by polyacrylamide gel electrophoresis (PAGE) of the samples. When incubated with pure carbohydrates at a concentration of 1 mg ml(-1), the extract reduced microbial degradation of the model protein, bovine serum albumin (BSA), such that its concentration was at least 40% above the control after 12 h of incubation. Total protein degradation was thus delayed by approximately 9 h. When fermented along with wheat straw, leaf protein (Rubisco) was almost entirely protected during 12 h of fermentation. The degradation of soy proteins was retarded by at least 4-6 h, depending on the protein band. There were strong side effects on the fermentation of pure cellulose (SCFA yield-60% after 12 h), whereas cellobiose and starch fermentation were less affected (-18 and -8%, respectively). When the complex substrates were fermented, SCFA yield was reduced by approximately 30% after 12 h. In our work we clearly demonstrate the efficacy of the new substance, which is neither a tannin nor a saponin, in an in vitro system, using pure as well as complex substrates. The properties shown in vitro for the crude extract suggest that it could have a positive effect on the protein metabolism of ruminants under intensive management and that negative side effects can be overcome by an optimized dosage. If the chemical nature of the active substance and its mechanism of action can be clarified, it may provide an alternative to replace critical synthetic feed additives (such as antibiotics) for high yielding dairy cows.

Scrap tyre recycling process with molten zinc as direct heat transfer and solids separation fluid: A new reactor concept.

PubMed

Riedewald, Frank; Goode, Kieran; Sexton, Aidan; Sousa-Gallagher, Maria J

2016-01-01

Every year about 1.5 billion tyres are discarded worldwide representing a large amount of solid waste, but also a largely untapped source of raw materials. The objective of the method was to prove the concept of a novel scrap tyre recycling process which uses molten zinc as the direct heat transfer fluid and, simultaneously, uses this media to separate the solids products (i.e. steel and rCB) in a sink-float separation at an operating temperature of 450-470 °C. This methodology involved: •construction of the laboratory scale batch reactor,•separation of floating rCB from the zinc,•recovery of the steel from the bottom of the reactor following pyrolysis.

[Study on quality standards of decoction pieces of salt Alpinia].

PubMed

Li, Wenbing; Hu, Changjiang; Long, Lanyan; Huang, Qinwan; Xie, Xiuqiong

2010-12-01

To establish the quality criteria for decoction pieces of salt Alpinia. Decoction pieces of salt Alpinia were measured with moisture, total ash, acid-insoluble ash, water-extract and volatile oils according to the procedures recorded in the Chinese Pharmacopoeia 2010. The content of Nootkatone was determined by HPLC, and NaCl, by chloridion electrode method. We obtained results of total ash, acid-insoluble ash, water-extract and volatile oils of 10 batches of decoction pieces of salt Alpinia moisture; Meanwhile we set the HPLC and chloridion electrode method. This research established a fine quality standard for decoction pieces of salt Alpinia.

The Molecular Design of High-Performance Carbon Materials

DTIC Science & Technology

2008-06-30

Thies MC. Control of mesophase pitch properties by supercritical fluid extraction. Carbon 1998; 36(7-8):953-61. 7] Zhuang M, Gast K, Thies MC...pitch with supercritical toluene. J Supercrit Fluids 1991; 4(1):7-14. 16] Herod AA, Bartle KD, Kandiyoti R. Characterization of heavy...MALDI, mass spectrometry, mesophase, extraction, supercritical , fractionation. 16. SECURITY CLASSIFICATION OF: a. REPORT u b. ABSTRACT u c. THIS

Image data-processing system for solar astronomy

NASA Technical Reports Server (NTRS)

Wilson, R. M.; Teuber, D. L.; Watkins, J. R.; Thomas, D. T.; Cooper, C. M.

1977-01-01

The paper describes an image data processing system (IDAPS), its hardware/software configuration, and interactive and batch modes of operation for the analysis of the Skylab/Apollo Telescope Mount S056 X-Ray Telescope experiment data. Interactive IDAPS is primarily designed to provide on-line interactive user control of image processing operations for image familiarization, sequence and parameter optimization, and selective feature extraction and analysis. Batch IDAPS follows the normal conventions of card control and data input and output, and is best suited where the desired parameters and sequence of operations are known and when long image-processing times are required. Particular attention is given to the way in which this system has been used in solar astronomy and other investigations. Some recent results obtained by means of IDAPS are presented.

Study of sulfur bonding on gallium arsenide (100) surfaces using supercritical fluid extraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cabauy, P.; Darici, Y.; Furton, K.G.

1995-12-01

In the last decades Gallium Arsenide (GaAs) has been considered the semiconductor that will replace silicon because of its direct band gap and high electron mobility. Problems with GaAs Fermi level pinning has halted its widespread use in the electronics industry. The formation of oxides on GaAs results in a high density of surface states that effectively pin the surface Fermi level at the midgap. Studies on sulfur passivation have eliminated oxidation and virtually unpinned the Fermi level on the GaAs surface. This has given rise to interest in sulfur-GaAs bonds. In this presentation, we will discuss the types ofmore » sulfur bonds extracted from a sulfur passivated GaAs (100) using Supercritical Fluid (CO2) Extraction (SFE). SFE can be a valuable tool in the study of chemical speciations on semiconductor surfaces. The variables evaluated to effectively study the sulfur species from the GaAs surface include passivation techniques, supercritical fluid temperatures, densities, and extraction times.« less

Mass balance of metal species in supercritical fluid extraction using sodium diethyldithiocarbamate and dibutylammonium dibutyldithiocarbamate.

PubMed

Wang, Joanna Shaofen; Chiu, Kong-Hwa

2006-03-01

The objective of this work is to track the amount of metal complexes distributed in the extraction cell, collection vial, and tubing used in supercritical fluid extraction (SFE) systems after progressive removal of metal ions in supercritical carbon dioxide (SC-CO2). Sodium diethyldithiocarbamate (NaDDC) and dibutylammonium dibutyldithiocarbamate (DBDC) ligands were used to form complexes with Cd, Cu, Pb, and Zn and CO(2)/5% methanol as a supercritical fluid. The mass balance of metal complexes were obtained before and after extraction, and metals in different locations in the system were flushed out using an organic solvent and nitric acid (HNO3). These results infer that the stability constant (beta) of the metal-ligand complex has a strong correlation with SFE. Because of the composition of the stainless-steel cell, Fe, Cr, and Ni or other trace elements in the cell might interfere with the mass balance of metal complexes in SFE due to an exchange mechanism taking place between the cell and the sample.

Multi-fluid renewable geo-energy systems and methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buscheck, Thomas A.

A geo-energy production method for extracting thermal energy from a reservoir formation. A production well extracts brine from the reservoir formation. A plurality of working fluid injection ("WFI") wells may be arranged proximate to the production well to at least partially circumscribe the production well. A plurality of brine production ("BP") wells may be arranged in a vicinity of the WFI wells to at least partially circumscribe the WFI wells. A working fluid is injected into the WFI wells to help drive a flow of the brine up through the production and BP wells, together with at least a portionmore » of the injected working fluid. Parasitic-load time-shifting and to storing of excess solar thermal energy may also be performed.« less

Comparison of various extraction methods for policosanol from rice bran wax and establishment of chromatographic fingerprint of policosanol.

PubMed

Wang, Mei-Fei; Lian, Hong-Zhen; Mao, Li; Zhou, Jing-Ping; Gong, Hui-Juan; Qian, Bao-Yong; Fang, Yan; Li, Jie

2007-07-11

A capillary gas chromatographic (GC) method has been developed for the separation and determination of policosanol components extracted from rice bran wax. A Varian CP-sil 8 CB column was employed, and an oven temperature was programmed. Gas chromatography-mass spectrometry (GC-MS) was used to identify the composition of policosanol. Quantitative analysis was carried out by means of hydrogen flame ionization detector (FID) with dinonyl phthalate (DNP) as internal standard. The results indicated that the extract obtained by dry saponification has the highest contents of octacosanol and triacontanol among extracts by all used extraction methods including dry saponification, saponification in alcohol, saponification in water (neutralized and non-neutralized), and transesterification. Meanwhile, the GC-MS fingerprint of policosanol extracted by dry saponification has been established. Euclidean distance similarity calculation showed remarkable consistency of compositions and contents among 12 batches of policosanol from a rice bran wax variety. This protocol provided a rapid and feasible method for quality control of policosanol products.

Production of Oxygen from Lunar Regolith using Molten Oxide Electrolysis

NASA Technical Reports Server (NTRS)

Sibille, Laurent; Sadoway, Donald R.; Sirk, Aislinn; Tripathy, Prabhat; Melendez, Orlando; Standish, Evan; Dominquez, Jesus A.; Stefanescu, Doru M.; Curreri, Peter A.; Poizeau, Sophie

2009-01-01

This slide presentation reviews the possible use of molten oxide electrolysis to extract oxygen from the Lunar Regolith. The presentation asserts that molten regolith electrolysis has advanced to be a useful method for production of oxygen and metals in situ on the Moon. The work has demonstrated an 8 hour batch of electrolysis at 5 amps using Iridium inert anodes.

Intracellular nucleotide and nucleotide sugar contents of cultured CHO cells determined by a fast, sensitive, and high-resolution ion-pair RP-HPLC.

PubMed

Kochanowski, N; Blanchard, F; Cacan, R; Chirat, F; Guedon, E; Marc, A; Goergen, J-L

2006-01-15

Analysis of intracellular nucleotide and nucleotide sugar contents is essential in studying protein glycosylation of mammalian cells. Nucleotides and nucleotide sugars are the donor substrates of glycosyltransferases, and nucleotides are involved in cellular energy metabolism and its regulation. A sensitive and reproducible ion-pair reverse-phase high-performance liquid chromatography (RP-HPLC) method has been developed, allowing the direct and simultaneous detection and quantification of some essential nucleotides and nucleotide sugars. After a perchloric acid extraction, 13 molecules (8 nucleotides and 5 nucleotide sugars) were separated, including activated sugars such as UDP-glucose, UDP-galactose, GDP-mannose, UDP-N-acetylglucosamine, and UDP-N-acetylgalactosamine. To validate the analytical parameters, the reproducibility, linearity of calibration curves, detection limits, and recovery were evaluated for standard mixtures and cell extracts. The developed method is capable of resolving picomolar quantities of nucleotides and nucleotide sugars in a single chromatographic run. The HPLC method was then applied to quantify intracellular levels of nucleotides and nucleotide sugars of Chinese hamster ovary (CHO) cells cultivated in a bioreactor batch process. Evolutions of the titers of nucleotides and nucleotide sugars during the batch process are discussed.

Removing tannins from medicinal plant extracts using an alkaline ethanol precipitation process: a case study of Danshen injection.

PubMed

Gong, Xingchu; Li, Yao; Qu, Haibin

2014-11-14

The alkaline ethanol precipitation process is investigated as an example of a technique for the removal of tannins extracted from Salviae miltiorrhizae Radix et Rhizoma for the manufacture of Danshen injection. More than 90% of the tannins can be removed. However, the recoveries of danshensu, rosmarinic acid, and salvianolic acid B were less than 60%. Total tannin removal increased as the refrigeration temperature decreased or the amount of NaOH solution added increased. Phenolic compound recoveries increased as refrigeration temperature increased or the amount of NaOH solution added decreased. When operated at a low refrigeration temperature, a relative high separation selectivity can be realized. Phenolic compound losses and tannin removal were mainly caused by precipitation. The formation of phenol salts, whose solubility is small in the mixture of ethanol and water used, is probably the reason for the precipitation. A model considering dissociation equilibrium and dissolution equilibrium was established. Satisfactory correlation results were obtained for phenolic compound recoveries and total tannin removal. Two important parameters in the model, which are the water content and pH value of alkaline supernatant, are suggested to be monitored and controlled to obtain high batch-to-batch consistency.

Optimization of Banana Juice Fermentation for the Production of Microbial Oil †

PubMed Central

Vega, Esther Z.; Glatz, Bonita A.; Hammond, Earl G.

1988-01-01

Apiotrichum curvatum ATCC 20509 (formerly Candida curvata D), a lipid-accumulating yeast, was grown in banana juice. The optimum conditions for biomass production in shake flasks were 30°C growth temperature, efficient aeration, a juice concentration of 25%, and preliminary heat treatment at less than sterilization conditions. Under controlled conditions in a fermentor, 20% banana juice was optimum. High concentrations of yeast extract (0.3%) increased biomass production by 40% but decreased oil production by 30%. A lower yeast extract concentration (0.05%) increased biomass production by 2% and oil production by 25%. The best growth and oil production were observed when asparagine (1.4 g/liter) and mineral salts were added to the banana juice. The addition of minerals seemed to improve the utilization of carbon. Growth inhibition was observed when the fermentor was aerated with pure oxygen, even when additional nutrients were present. A fed-batch process permitted the juice concentration to be increased from 15 to 82%; biomass accumulation was three times higher than in batch fermentations. However, the cellular lipid content was only 30% of dry weight, and chemical oxygen demand reduction was slow and inefficient. PMID:16347584

Effect of animal products and extracts on wound healing promotion in topical applications: a review.

PubMed

Napavichayanun, Supamas; Aramwit, Pornanong

2017-06-01

Wound healing is a natural process of body reaction to repair itself after injury. Nonetheless, many internal and external factors such as aging, comorbidity, stress, smoking, alcohol drinking, infections, malnutrition, or wound environment significantly affect the quality and speed of wound healing. The unsuitable conditions may delay wound healing process and cause chronic wound or scar formation. Therefore, many researches have attempted to search for agents that can accelerate wound healing with safety and biocompatibility to human body. Widely studied wound healing agents are those derived from either natural sources including plants and animals or chemical synthesis. The natural products seem to be safer and more biocompatible to human tissue. This review paper demonstrated various kinds of the animal-derived products including chitosan, collagen, honey, anabolic steroids, silk sericin, peptides, and proteoglycan in term of mechanisms of action, advantages, and disadvantages when applied as wound healing accelerator. The benefits of these animal-derived products are wound healing promotion, anti-inflammatory, antimicrobial activity, moisturizing effect, biocompatibility, and safety. However, the drawbacks such as allergy, low stability, batch-to-batch variability, and high extraction and purification costs could not be avoided in some products.

Biotechnological transformation of hydrocortisone to 16α-hydroxy hydrocortisone by Streptomyces roseochromogenes.

PubMed

Restaino, Odile Francesca; Marseglia, Mariacarmela; De Castro, Cristina; Diana, Paola; Forni, Pasquale; Parrilli, Michelangelo; De Rosa, Mario; Schiraldi, Chiara

2014-02-01

Streptomyces roseochromogenes is able to hydroxylate steroid compounds in different positions of their cycloalkane rings thanks to a cytochrome P-450 multi-enzyme complex. In this paper, the hydroxylation of the hydrocortisone in the 16α position, performed by bacterial whole cells, was investigated in both shake flask and fermentation conditions; the best settings for both cellular growth and transformation reaction were studied by investigating the optimal medium composition, the kinetic of conversion, the most suitable substrate concentration and the preferred addition timing. Using newly formulated malt extract- and yeast extract-based media, a 16α-hydrohydrocortisone concentration of 0.2 ± 0.01 g L(-1) was reached in shake flasks. Batch experiments in a 2-L fermentor established the reproducibility and robustness of the biotransformation, while a pulsed batch fermentation strategy allowed the production to increase up to 0.508 ± 0.01 g L(-1). By-product formation was investigated, and two new derivates of the hydrocortisone obtained during the bacterial transformation reaction and unknown so far, a C-20 hydroxy derivate and a C-21 N-acetamide one, were determined by NMR analyses.

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

PubMed Central

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85%) and oleic acid (1.64%–18.97%). Thymoquinone (0.72%–21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. PMID:28814830

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

PubMed

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P <0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

Batch and Continuous Ultrasound Assisted Extraction of Boldo Leaves (Peumus boldus Mol.).

PubMed

Petigny, Loïc; Périno-Issartier, Sandrine; Wajsman, Joël; Chemat, Farid

2013-03-12

Vegetal extracts are widely used as primary ingredients for various products from creams to perfumes in the pharmaceutical, nutraceutic and cosmetic industries. Having concentrated and active extract is essential, as the process must extract as much soluble material as possible in a minimum time, using the least possible volume of solvent. The boldo leaves extract is of great interest for the industry as it holds a great anti-oxidant activity due to high levels of flavonoids and alkaloids such as boldine. Ultrasound Assisted Extraction (UAE) has been used to improve the efficiency of the plant extraction, reducing extraction time, increasing the concentration of the extract with the same amount of solvent and plant material. After a preliminary study, a response surface method has been used to optimize the extraction of soluble material from the plant. The results provided by the statistical analysis revealed that the optimized conditions were: sonication power 23 W/cm2 for 40 min and a temperature of 36 °C. The optimized parameters of the UAE provide a better extraction compared to a conventional maceration in terms of process time (30 min instead of 120 min), higher yield, more energy saving, cleanliness, safety and product quality.

Batch and Continuous Ultrasound Assisted Extraction of Boldo Leaves (Peumus boldus Mol.)

PubMed Central

Petigny, Loïc; Périno-Issartier, Sandrine; Wajsman, Joël; Chemat, Farid

2013-01-01

Vegetal extracts are widely used as primary ingredients for various products from creams to perfumes in the pharmaceutical, nutraceutic and cosmetic industries. Having concentrated and active extract is essential, as the process must extract as much soluble material as possible in a minimum time, using the least possible volume of solvent. The boldo leaves extract is of great interest for the industry as it holds a great anti-oxidant activity due to high levels of flavonoids and alkaloids such as boldine. Ultrasound Assisted Extraction (UAE) has been used to improve the efficiency of the plant extraction, reducing extraction time, increasing the concentration of the extract with the same amount of solvent and plant material. After a preliminary study, a response surface method has been used to optimize the extraction of soluble material from the plant. The results provided by the statistical analysis revealed that the optimized conditions were: sonication power 23 W/cm2 for 40 min and a temperature of 36 °C. The optimized parameters of the UAE provide a better extraction compared to a conventional maceration in terms of process time (30 min instead of 120 min), higher yield, more energy saving, cleanliness, safety and product quality. PMID:23481637

[Application of microwave technology in extraction process of Guizhi Fuling capsule].

PubMed

Wang, Zheng-kuan; Zhou, Mao; Liu, Yuan; Bi, Yu-an; Wang, Zhen-zhong; Xiao, Wei

2015-06-01

In this paper, optimization of the conditions of microwave technique in extraction process of Guizhi Fuling capsule in the condition of a pilot scale was carried out. First of all, through the single factor experiment investigation of various factors, the overall impact tendency and range of each factor were determined. Secondly, L9 (3(4)) orthogonal test optimization was used, and the contents of gallic acid in liquid, paeoniflorin, benzoic acid, cinnamic acid, benzoyl paeoniflorin, amygdalin of the liquid medicine were detected. The extraction rate and comprehensive evaluation were calculated with the extraction effect, as the judgment basis. Theoptimum extraction process of Guizhi Fuling capsule by microwave technology was as follows: the ratio of liquid to solid was 6: 1 added to drinking water, the microwave power was 6 kW, extraction time was 20 min for 3 times. The process of the three batch of amplification through verification, the results are stable, and compared with conventional water extraction has the advantages of energy saving, time saving, high efficiency advantages. The above results show the optimum extracting technology of high efficiency, stable and feasible.

High resolution melt curve analysis based on methylation status for human semen identification.

PubMed

Fachet, Caitlyn; Quarino, Lawrence; Karnas, K Joy

2017-03-01

A high resolution melt curve assay to differentiate semen from blood, saliva, urine, and vaginal fluid based on methylation status at the Dapper Isoform 1 (DACT1) gene was developed. Stains made from blood, saliva, urine, semen, and vaginal fluid were obtained from volunteers and DNA was isolated using either organic extraction (saliva, urine, and vaginal fluid) or Chelex ® 100 extraction (blood and semen). Extracts were then subjected to bisulfite modification in order to convert unmethylated cytosines to uracil, consequently creating sequences whose amplicons have melt curves that vary depending on their initial methylation status. When primers designed to amplify the promoter region of the DACT1 gene were used, DNA from semen samples was distinguishable from other fluids by a having a statistically significant lower melting temperature. The assay was found to be sperm-significant since semen from a vasectomized man produced a melting temperature similar to the non-semen body fluids. Blood and semen stains stored up to 5 months and tested at various intervals showed little variation in melt temperature indicating the methylation status was stable during the course of the study. The assay is a more viable method for forensic science practice than most molecular-based methods for body fluid stain identification since it is time efficient and utilizes instrumentation common to forensic biology laboratories. In addition, the assay is advantageous over traditional presumptive chemical methods for body fluid identification since results are confirmatory and the assay offers the possibility of multiplexing which may test for multiple body fluids simultaneously.

Evaluation of CO 2 -Fluid-Rock Interaction in Enhanced Geothermal Systems: Field-Scale Geochemical Simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan, Feng; McPherson, Brian J.; Kaszuba, John

Recent studies suggest that using supercritical CO 2 (scCO 2 ) instead of water as a heat transmission fluid in Enhanced Geothermal Systems (EGS) may improve energy extraction. While CO 2 -fluid-rock interactions at “typical” temperatures and pressures of subsurface reservoirs are fairly well known, such understanding for the elevated conditions of EGS is relatively unresolved. Geochemical impacts of CO 2 as a working fluid (“CO 2 -EGS”) compared to those for water as a working fluid (H 2 O-EGS) are needed. The primary objectives of this study are (1) constraining geochemical processes associated with CO 2 -fluid-rock interactions undermore » the high pressures and temperatures of a typical CO 2 -EGS site and (2) comparing geochemical impacts of CO 2 -EGS to geochemical impacts of H 2 O-EGS. The St. John’s Dome CO 2 -EGS research site in Arizona was adopted as a case study. A 3D model of the site was developed. Net heat extraction and mass flow production rates for CO 2 -EGS were larger compared to H 2 O-EGS, suggesting that using scCO 2 as a working fluid may enhance EGS heat extraction. More aqueous CO 2 accumulates within upper- and lower-lying layers than in the injection/production layers, reducing pH values and leading to increased dissolution and precipitation of minerals in those upper and lower layers. Dissolution of oligoclase for water as a working fluid shows smaller magnitude in rates and different distributions in profile than those for scCO 2 as a working fluid. It indicates that geochemical processes of scCO 2 -rock interaction have significant effects on mineral dissolution and precipitation in magnitudes and distributions.« less

The effect of pigeon yolk sac fluid on the growth behavior of calcium carbonate crystals.

PubMed

Song, Juan; Cheng, Haixia; Shen, Xinyu; Tong, Hua

2015-03-01

Previous experiments have proved that thermodynamically unstable calcium carbonate vaterite can exist for long periods in the yolk sac of a pigeon embryo. The aim of this article was to demonstrate the effect of in vitro mineralization of yolk sac fluid on calcium carbonate by direct precipitation. Experiments were conducted using pigeon yolk sac fluid and using lecithin extracted from pigeon yolk sac fluid as a control to investigate the regulating effects of the organic components in the embryo on the formation of the calcium carbonate precipitate. Multiple characterization methods were employed to study the various morphological patterns, sizes, crystal growth, and crystal phase transformations of the calcium carbonate precipitates as regulated by the yolk sac fluid extracted at different stages of incubation. The experimental results demonstrate that as the incubation proceeds towards the later stages, the composition and environmental features of the yolk sac fluid become more favorable for the formation of relatively unstable calcium carbonate phases with high energies of the vaterite state. The experiments conducted with extracted lecithin as the template for crystal growth yielded similar results. A large amount of organic molecules with polar functional groups carried by the yolk sac fluid have strong effects and can both initially induce the crystallization and regulate the aggregation of calcium carbonate. Furthermore, this regulation process is found to be closely related to the lecithin contained in yolk sac fluid. These observations confirm the changes in yolk sac fluid composition during incubation have significant effects on the production of vaterite, which implicates the calcium transport during embryo growth. © 2015 Poultry Science Association Inc.

Evaluation of CO 2 -Fluid-Rock Interaction in Enhanced Geothermal Systems: Field-Scale Geochemical Simulations

DOE PAGES

Pan, Feng; McPherson, Brian J.; Kaszuba, John

2017-01-01

Recent studies suggest that using supercritical CO 2 (scCO 2 ) instead of water as a heat transmission fluid in Enhanced Geothermal Systems (EGS) may improve energy extraction. While CO 2 -fluid-rock interactions at “typical” temperatures and pressures of subsurface reservoirs are fairly well known, such understanding for the elevated conditions of EGS is relatively unresolved. Geochemical impacts of CO 2 as a working fluid (“CO 2 -EGS”) compared to those for water as a working fluid (H 2 O-EGS) are needed. The primary objectives of this study are (1) constraining geochemical processes associated with CO 2 -fluid-rock interactions undermore » the high pressures and temperatures of a typical CO 2 -EGS site and (2) comparing geochemical impacts of CO 2 -EGS to geochemical impacts of H 2 O-EGS. The St. John’s Dome CO 2 -EGS research site in Arizona was adopted as a case study. A 3D model of the site was developed. Net heat extraction and mass flow production rates for CO 2 -EGS were larger compared to H 2 O-EGS, suggesting that using scCO 2 as a working fluid may enhance EGS heat extraction. More aqueous CO 2 accumulates within upper- and lower-lying layers than in the injection/production layers, reducing pH values and leading to increased dissolution and precipitation of minerals in those upper and lower layers. Dissolution of oligoclase for water as a working fluid shows smaller magnitude in rates and different distributions in profile than those for scCO 2 as a working fluid. It indicates that geochemical processes of scCO 2 -rock interaction have significant effects on mineral dissolution and precipitation in magnitudes and distributions.« less

Subcritical Fluid Extraction of Chinese Quince Seed: Optimization and Product Characterization.

PubMed

Wang, Li; Wu, Min; Liu, Hua-Min; Ma, Yu-Xiang; Wang, Xue-De; Qin, Guang-Yong

2017-03-25

Chinese quince seed (CQS) is an underutilized oil source and a potential source of unsaturated fatty acids and α-tocopherol-rich oil. Subcritical fluid (SCF) extraction is executed at lower pressures and temperatures than the pressures and temperatures used in supercritical fluid extraction. However, no studies on the SCF extraction of CQS oil are reported. Therefore, the objective of this study was to evaluate the use of SCF for the extraction of CQS oil and to compare the use of SCF with the classical Soxhlet (CS) and supercritical CO₂ (SC-CO₂) extraction methods. Response surface methodology (RSM) was used to investigate the extraction conditions: temperature (45-65 °C), time (30-50 min), and solvent/solid ratio (5-15 mL/g). The optimization results showed that the highest yield (27.78%) was obtained at 56.18 °C, 40.20 min, and 12.57 mL/g. The oil extracted by SCF had a higher unsaturated fatty acid content (86.37%-86.75%), higher α-tocopherol content (576.0-847.6 mg/kg), lower acid value (3.97 mg/g), and lower peroxide value (0.02 meq O₂/kg) than extractions using CS and SC-CO 2 methods. The SCF-defatted meal of oilseed exhibited the highest nitrogen solubility index (49.64%) and protein dispersibility index (50.80%), demonstrating that SCF extraction was a promising and efficient technique as an alternative to CS and SC-CO 2 methods, as very mild operating conditions and an eco-friendly solvent can be used in the process with maximum preservation of the quality of the meal.

Single-step preparation of selected biological fluids for the high performance liquid chromatographic analysis of fat-soluble vitamins and antioxidants.

PubMed

Lazzarino, Giacomo; Longo, Salvatore; Amorini, Angela Maria; Di Pietro, Valentina; D'Urso, Serafina; Lazzarino, Giuseppe; Belli, Antonio; Tavazzi, Barbara

2017-12-08

Fat-soluble vitamins and antioxidants are of relevance in health and disease. Current methods to extract these compounds from biological fluids mainly need use of multi-steps and multi organic solvents. They are time-consuming and difficult to apply to treat simultaneously large sample number. We here describe a single-step, one solvent extraction of fat-soluble vitamins and antioxidants from biological fluids, and the chromatographic separation of all-trans-retinoic acid, 25-hydroxycholecalciferol, all-trans-retinol, astaxanthin, lutein, zeaxanthin, trans-β-apo-8'-carotenal, γ-tocopherol, β-cryptoxanthin, α-tocopherol, phylloquinone, lycopene, α-carotene, β-carotene and coenzyme Q 10 . Extraction is obtained by adding one volume of biological fluid to two acetonitrile volumes, vortexing for 60s and incubating for 60min at 37°C under agitation. HPLC separation occurs in 30min using Hypersil C18, 100×4.6mm, 5μm particle size column, gradient from 70% methanol+30% H 2 O to 100% acetonitrile, flow rate of 1.0ml/min and 37°C column temperature. Compounds are revealed using highly sensitive UV-VIS diode array detector. The HPLC method suitability was assessed in terms of sensitivity, reproducibility and recovery. Using the present extraction and chromatographic conditions we obtained values of the fat-soluble vitamins and antioxidants in serum from 50 healthy controls similar to those found in literature. Additionally, the profile of these compounds was also measured in seminal plasma from 20 healthy fertile donors. Results indicate that this simple, rapid and low cost sample processing is suitable to extract fat-soluble vitamins and antioxidants from biological fluids and can be applied in clinical and nutritional studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Oral bioaccessibility and human exposure to anthropogenic and geogenic mercury in urban, industrial and mining areas.

PubMed

Rodrigues, S M; Coelho, C; Cruz, N; Monteiro, R J R; Henriques, B; Duarte, A C; Römkens, P F A M; Pereira, E

2014-10-15

The objective of this study was to characterize the link between bioaccessibility and fractionation of mercury (Hg) in soils and to provide insight into human exposure to Hg due to inhalation of airborne soil particles and hand-to-mouth ingestion of Hg-bearing soil. Mercury in soils from mining, urban and industrial areas was fractionated in organometallic forms; mobile; semi-mobile; and non-mobile forms as well as HCl-extractable Hg. The in vitro bioaccessibility of Hg was obtained by extracting soils with (1) a simulated human gastric fluid (pH1.5), and (2) a simulated human lung fluid (pH7.4). Total soil Hg concentrations ranged from 0.72 to 1.8 mg kg(-1) (urban areas), 0.28 to 94 mg kg(-1) (industrial area) and 0.92 to 37 mg kg(-1) (mining areas). Both organometallic Hg as well as 0.1M HCl extractable Hg were lower (<0.5% of total Hg) than Hg extracted by gastric fluid (up to 1.8% of total Hg) and lung fluid (up to 12% of total Hg). In addition, Hg extracted by lung fluid was significantly higher in urban and industrial soils (average 5.0-6.6% of total Hg) compared to mining soils. Such differences were related to levels of mobile Hg species in urban and industrial soils compared to mining soils. These results strengthen the need to measure site-specific Hg fractionation when determining Hg bioaccessibility. Results also show that ingestion and/or inhalation of Hg from soil particles can contribute up to 8% of adult total Hg intake when compared to total Hg intake via consumption of contaminated fish and animal products from contaminated areas. Copyright © 2014 Elsevier B.V. All rights reserved.

Effects of process parameters on peanut skins extract and CO2 diffusivity by supercritical fluid extraction

NASA Astrophysics Data System (ADS)

Putra, N. R.; Yian, L. N.; Nasir, H. M.; Idham, Z. Binti; Yunus, M. A. C.

2018-03-01

Peanut skins (Arachis hypogea) are an agricultural waste product which has received much attention because they contain high nutritional values and can be potentially utilized in difference industries. At present, only a few studies have been conducted to study the effects of parameters on the peanut skins oil extraction. Therefore, this study aimed to determine the best extraction condition in order to obtain the highest extract yield using supercritical carbon dioxide (SC-CO2) with co-solvent Ethanol as compared to Soxhlet extraction method. Diffusivity of carbon dioxide in supercritical fluid extraction was determined using Crank model. The mean particle size used in this study was 425 µm. The supercritical carbon dioxide was performed at temperature (40 – 70 °C), flow rate of co-solvent ethanol (0 - 7.5% Vethanol/Vtotal), and extraction pressure (10 – 30 MPa) were used in this studies. The results showed that the percentage of oil yields and effective diffusivity increase as the pressure, rate of co-solvent, and temperature increased.

Application of response surface methodology for the optimization of supercritical fluid extraction of essential oil from pomegranate (Punica granatum L.) peel.

PubMed

Ara, Katayoun Mahdavi; Raofie, Farhad

2016-07-01

Essential oils and volatile components of pomegranate ( Punica granatum L.) peel of the Malas variety from Meybod, Iran, were extracted using supercritical fluid extraction (SFE) and hydro-distillation methods. The experimental parameters of SFE that is pressure, temperature, extraction time, and modifier (methanol) volume were optimized using a central composite design after a (2 4-1 ) fractional factorial design. Detailed chemical composition of the essential oils and volatile components obtained by hydro-distillation and optimum condition of the supercritical CO 2 extraction were analyzed by GC-MS, and seventy-three and forty-six compounds were identified according to their retention indices and mass spectra, respectively. The optimum SFE conditions were 350 atm pressure, 55 °C temperature, 30 min extraction time, and 150 µL methanol. Results showed that oleic acid, palmitic acid and (-)-Borneol were major compounds in both extracts. The optimum extraction yield was 1.18 % (w/w) for SFE and 0.21 % (v/w) for hydro-distillation.

Remediation of Contaminated Soils By Supercritical Carbon Dioxide Extraction

NASA Astrophysics Data System (ADS)

Ferri, A.; Zanetti, M. C.; Banchero, M.; Fiore, S.; Manna, L.

The contaminants that can be found in soils are many, inorganic, like heavy metals, as well as organic. Among the organic contaminants, oil and coal refineries are responsi- ble for several cases of soil contamination with PAHs (Polycyclic Aromatic Hydrocar- bons). Polynuclear aromatic hydrocarbons (PAHs) have toxic, carcinogenic and mu- tagenic effects. Limits have been set on the concentration of most contaminants, and growing concern is focusing on soil contamination issues. USA regulations set the maximum acceptable level of contamination by PAHs equal to 40 ppm at residential sites and 270 ppm at industrial sites. Stricter values are usually adopted in European Countries. Supercritical carbon dioxide extraction is a possible alternative technology to remove volatile organic compounds from contaminated soils. Supercritical fluid extraction (SFE) offers many advantages over conventional solvent extraction. Super- critical fluids combine gaseous properties as a high diffusion coefficient, and liquid properties as a high solvent power. The solvent power is strongly pressure-dependent near supercritical conditions: selective extractions are possible without changing the solvent. Solute can be separate from the solvent depressurising the system; therefore, it is possible to recycle the solvent and recover the contaminant. Carbon dioxide is frequently used as supercritical fluid, because it has moderate critical conditions, it is inert and available in pure form. In this work, supercritical fluid extraction technology has been used to remove a polynuclear aromatic hydrocarbon from contaminated soils. The contaminant choice for the experiment has been naphthalene since several data are available in literature. G. A. Montero et al. [1] studied soil remediation with supercrit- ical carbon dioxide extraction technology; these Authors have found that there was a mass-transfer limitation. In the extraction vessel, the mass transfer coefficient in- creases with the superficial velocity of the supercritical carbon dioxide; therefore, the mass transfer resistance can be reduced increasing such velocity. In this work, higher values of superficial velocity were investigated. The experimental apparatus includes a pump, an extraction vessel, an adjustable restrictor and a trap to collect the extracted substance. Liquid carbon dioxide coming from a cylinder with a dip-tube is cooled by a cryostatic bath and then it is compressed by a pneumatic drive pump (the max- imum available pressure is 69 MPa). Subsequently, the pressurised current flows into 1 a heating coil and then into the extraction vessel, which is contained in a stove; the outlet flow is depressurised in an adjustable restrictor and the extracted substance is collected in a trap by dissolution into a solvent. The extracted naphthalene quantity was obtained by weighting the solvent and measuring the naphthalene concentration with a gas chromatograph. The soil sample is a sandy soil geologically representative of the North of Italy that was sampled and physically and chemically characterized: particle-size distribution analysis, diffractometric analysis, Cation Exchange Capac- ity, Total Organic Carbon, iron content and manganese content in order to evaluate the potential sorption degree. The soil was artificially polluted by means of a naphta- lene and methylene chloride solution. The experimental work consists in a number of naphthalene extractions from the spiked soil, that were carried out at different operat- ing conditions, temperature, pressure and flow rate by means of supercritical carbon dioxide evaluating the corresponding recovery efficiencies. The results obtained were analysed and compared in order to determine which parameters influence the system. [1] G. A. Montero, T.D. Giorgio, and K. B. Schnelle, Jr..Removal of Hazardous ,1994, Contaminants form Soils by Supercritical Fluid Extraction. Innovations in Supercriti- cal Fluids. ACS Symposium Series, 608, 280-197. 2

Enhancing methane production from U. lactuca using combined anaerobically digested sludge (ADS) and rumen fluid pre-treatment and the effect on the solubilization of microbial community structures.

PubMed

Zou, Yu; Xu, Xiaochen; Li, Liang; Yang, Fenglin; Zhang, Shushen

2018-04-01

Methane production by the anaerobic digestion of seaweed is restricted by the slow degradation caused by the influence of the rigid algal cell wall. At the present time, there has been no study focusing on the anaerobic digestion of U. lactuca by co-fermentation and pre-treatment with rumen fluid. Rumen fluid can favor methane production from algal biomass by utilizing the diversity and quantity of bacterial and archaeal communities in the rumen fluid. This research presents a novel method based on combined ADS and rumen fluid pre-treatment to improve the production of methane from seaweed. Biochemical methane potential (BMP) tests were performed to investigate the biogas production using combined ADS and rumen fluid pre-treatment at varied inoculum ratios on the performance of methane production from U. lactuca biomass. Compared to the control (no rumen fluid pre-treatment), the highest BMP yields of U. lactuca increased from 3%, 27.5% and 39.5% to 31.1%, 73% and 85.6%, respectively, for three different types of treatment. Microbial community analysis revealed that the Methanobrevibacter species, known to accept electrons to form methane, were only detected when rumen fluid was added. Together with the significant increase in species of Methanoculleus, Methanospirillum and Methanosaeta, rumen fluid improved the fermentation and degradation of the microalgae biomass not only by pre-treatment to foster cell-wall degradation but also by relying on methane production within itself during anaerobic processes. Batch experiments further indicated that rumen fluid applied to the co-fermentation and pre-treatment could increase the economic value and hold promise for enhancing biogas production from different seaweed species. Copyright © 2017 Elsevier Ltd. All rights reserved.

Variability in Bioreactivity Linked to Changes in Size and Zeta Potential of Diesel Exhaust Particles in Human Immune Cells

PubMed Central

Sarkar, Srijata; Zhang, Lin; Subramaniam, Prasad; Lee, Ki-Bum; Garfunkel, Eric; Strickland, Pamela A. Ohman.; Mainelis, Gediminas; Lioy, Paul J.; Tetley, Teresa D.; Chung, Kian Fan; Zhang, Junfeng; Ryan, Mary; Porter, Alex; Schwander, Stephan

2014-01-01

Acting as fuel combustion catalysts to increase fuel economy, cerium dioxide (ceria, CeO2) nanoparticles have been used in Europe as diesel fuel additives (Envirox™). We attempted to examine the effects of particles emitted from a diesel engine burning either diesel (diesel exhaust particles, DEP) or diesel doped with various concentrations of CeO2 (DEP-Env) on innate immune responses in THP-1 and primary human peripheral blood mononuclear cells (PBMC). Batches of DEP and DEP-Env were obtained on three separate occasions using identical collection and extraction protocols with the aim of determining the reproducibility of particles generated at different times. However, we observed significant differences in size and surface charge (zeta potential) of the DEP and DEP-Env across the three batches. We also observed that exposure of THP-1 cells and PBMC to identical concentrations of DEP and DEP-Env from the three batches resulted in statistically significant differences in bioreactivity as determined by IL-1β, TNF-α, IL-6, IFN-γ, and IL-12p40 mRNA (by qRT-PCR) and protein expression (by ELISPOT assays). Importantly, bioreactivity was noted in very tight ranges of DEP size (60 to 120 nm) and zeta potential (−37 to −41 mV). Thus, these physical properties of DEP and DEP-Env were found to be the primary determinants of the bioreactivity measured in this study. Our findings also point to the potential risk of over- or under- estimation of expected bioreactivity effects (and by inference of public health risks) from bulk DEP use without taking into account potential batch-to-batch variations in physical (and possibly chemical) properties. PMID:24825358

Improvement and automation of a real-time PCR assay for vaginal fluids.

PubMed

De Vittori, E; Giampaoli, S; Barni, F; Baldi, M; Berti, A; Ripani, L; Romano Spica, V

2016-05-01

The identification of vaginal fluids is crucial in forensic science. Several molecular protocols based on PCR amplification of mfDNA (microflora DNA) specific for vaginal bacteria are now available. Unfortunately mfDNA extraction and PCR reactions require manual optimization of several steps. The aim of present study was the verification of a partial automatization of vaginal fluids identification through two instruments widely diffused in forensic laboratories: EZ1 Advanced robot and Rotor Gene Q 5Plex HRM. Moreover, taking advantage of 5-plex thermocycler technology, the ForFluid kit performances were improved by expanding the mfDNA characterization panel with a new bacterial target for vaginal fluids and with an internal positive control (IPC) to monitor PCR inhibition. Results underlined the feasibility of a semi-automated extraction of mfDNA using a BioRobot and demonstrated the analytical improvements of the kit. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Generation of monoclonal antibodies and development of an immunofluorometric assay for the detection of CUZD1 in tissues and biological fluids.

PubMed

Farkona, Sofia; Soosaipillai, Antoninus; Filippou, Panagiota; Korbakis, Dimitrios; Serra, Stefano; Rückert, Felix; Diamandis, Eleftherios P; Blasutig, Ivan M

2017-12-01

CUB and zona pellucida-like domain-containing protein 1 (CUZD1) was identified as a pancreas-specific protein and was proposed as a candidate biomarker for pancreatic related disorders. CUZD1 protein levels in tissues and biological fluids have not been extensively examined. The purpose of the present study was to generate specific antibodies targeting CUZD1 to assess CUZD1 expression within tissues and biological fluids. Mouse monoclonal antibodies against CUZD1 were generated and used to perform immunohistochemical analyses and to develop a sensitive and specific enzyme-linked immunosorbent assay (ELISA). CUZD1 protein expression was assessed in various human tissue extracts and biological fluids and in gel filtration chromatography-derived fractions of pancreatic tissue extract, pancreatic juice and recombinant protein. Immunohistochemical staining of CUZD1 in pancreatic tissue showed that the protein is localized to the acinar cells and the lumen of the acini. Western blot analysis detected the protein in pancreatic tissue extract and pancreatic juice. The newly developed ELISA measured CUZD1 in high levels in pancreas and in much lower but detectable levels in several other tissues. In the biological fluids tested, CUZD1 expression was detected exclusively in pancreatic juice. The analysis of gel filtration chromatography-derived fractions of pancreatic tissue extract, pancreatic juice and recombinant CUZD1 suggested that the protein exists in high molecular weight protein complexes. This study describes the development of tools targeting CUZD1 protein, its tissue expression pattern and levels in several biological fluids. These new tools will facilitate future investigations aiming to delineate the role of CUZD1 in physiology and pathobiology. Copyright © 2017 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Determination of vitamin K1 in powdered infant formulas, using supercritical fluid extraction and liquid chromatography with electrochemical detection.

PubMed

Schneiderman, M A; Sharma, A K; Mahanama, K R; Locke, D C

1988-01-01

Vitamin K1 (phylloquinone) is extracted from commercial soy protein-based and milk-based powdered infant formulas by using supercritical fluid extraction with CO2 at 8000 psi and 60 degrees C. Quantitative extraction requires only 15 min, and does not suffer from the problems associated with conventional solvent extraction of lipophilic materials from media such as formulas. Vitamin K1 is determined in the extracts by using reverse-phase liquid chromatography (LC) with reductive mode electrochemical detection at a silver electrode polarized at -1.1 V vs SCE. LC run time is 9 min. The minimum detectable quantity is 80 pg, and response is linear over at least 5 orders of magnitude. Recovery of vitamin K1 from a milk-based powdered formula was 95.6% with RSD of 7.4%, and from a soy protein-based product, 94.4% recovery with RSD of 6.5%.

DEVELOPMENTS IN THE SUPERCRITICAL FLUID EXTRACTION OF CHLOROPHENOXY ACID HERBICIDES FROM SOIL SAMPLES

EPA Science Inventory

Extraction of chlorophenoxy acid herbicides from soil samples with supercritical carbon dioxide as extractant and tetrabutylammonium hydroxide and methyl iodide as derivatization agents was investigated. The extraction was carried out at 400 atm and 80 C for 15 min static, follow...

Nocardia globerula NHB-2 nitrilase catalysed biotransformation of 4-cyanopyridine to isonicotinic acid

PubMed Central

2012-01-01

Isonicotinic acid (INA) is an important pyridine derivative used in the manufacture of isoniazid (antituberculosatic drug) and other pharmaceutically important drugs. Nitrilase catalysed processes for the synthesis of pharmaceutically important acids from their corresponding nitriles are promising alternative over the cumbersome, hazardous, and energy demanding chemical processes. Nitrilase of Nocardia globerula NHB-2 (NitNHB2) is expressed in presence of isobutyronitrile in the growth medium (1.0% glucose, 0.5% peptone, 0.3% beef extract, and 0.1 % yeast extract, pH 7.5). NitNHB2 hydrolyses 4-cyanopyridine (4-CP) to INA without accumulation of isonicotinamide, which is common in the reaction catalysed via fungal nitrilases. The NitNHB2 suffers from substrate inhibition effect and hydrolysing activity up to 250 mM 4-CP was recorded. Complete conversion of 200 mM 4-CP to INA was achieved in 40 min using resting cell concentration corresponding to 10 U mL-1 nitrilase activity in the reaction. Substrate inhibition effect in the fed batch reaction (200 mM substrate feed/40min) led to formation of only 729 mM INA. In a fed batch reaction (100 mM 4-CP/20min), substrate inhibition effect was encountered after 7th feed and a total of 958 mM INA was produced in 400 min. The fed batch reaction scaled up to 1 L and 100% hydrolysis of 700 mM of 4-CP to INA at 35°C achieved in 140 min. The rate of INA production was 21.1 g h-1 mgDCW-1. This is the fastest biotransformation process ever reported for INA production with time and space productivity of 36 g L-1 h-1 using a bacterial nitrilase. PMID:22537922

Ultrasensitive quantification of the CYP2E1 probe chlorzoxazone and its main metabolite 6-hydroxychlorzoxazone in human plasma using ultra performance liquid chromatography coupled to tandem mass spectrometry after chlorzoxazone microdosing.

PubMed

Witt, Lukas; Suzuki, Yosuke; Hohmann, Nicolas; Mikus, Gerd; Haefeli, Walter E; Burhenne, Jürgen

2016-08-01

Chlorzoxazone is a probe drug to assess cytochrome P450 (CYP) 2E1 activity (phenotyping). If the pharmacokinetics of the probe drug is linear, pharmacologically ineffective doses are sufficient for the purpose of phenotyping and adverse effects can thus be avoided. For this reason, we developed and validated an assay for the ultrasensitive quantification of chlorzoxazone and 6-hydroxychlorzoxazone in human plasma. Plasma (0.5mL) and liquid/liquid partitioning were used for sample preparation. Extraction recoveries ranged between 76 and 93% for both analytes. Extracts were separated within 3min on a Waters BEH C18 Shield 1.7μm UPLC column with a fast gradient consisting of aqueous formic acid and acetonitrile. Quantification was achieved using internal standards labeled with deuterium or (13)C and tandem mass spectrometry in the multiple reaction monitoring mode using negative electrospray ionization, which yielded lower limits of quantification of 2.5pgmL(-1), while maintaining a precision always below 15%. The calibrated concentration ranges were linear for both analytes (2.5-1000pgmL(-1)) with correlation coefficients of >0.99. Within-batch and batch-to-batch precision in the calibrated ranges for both analytes were <15% and <11% and plasma matrix effects always were below 50%. The assay was successfully applied to assess the pharmacokinetics of chlorzoxazone in two human volunteers after administration of single oral doses (2.5-5000μg). This ultrasensitive assay allowed the determination of chlorzoxazone pharmacokinetics for 8h after microdosing of 25μg chlorzoxazone. Copyright © 2016 Elsevier B.V. All rights reserved.

Complete automation of solid-phase extraction with subsequent liquid chromatography-tandem mass spectrometry for the quantification of benzoylecgonine, m-hydroxybenzoylecgonine, p-hydroxybenzoylecgonine, and norbenzoylecgonine in urine--application to a high-throughput urine analysis laboratory.

PubMed

Robandt, Paul P; Reda, Louis J; Klette, Kevin L

2008-10-01

A fully automated system utilizing a liquid handler and an online solid-phase extraction (SPE) device coupled with liquid chromatography-tandem mass spectrometry (LC-MS-MS) was designed to process, detect, and quantify benzoylecgonine (BZE), meta-hydroxybenzoylecgonine (m-OH BZE), para-hydroxybenzoylecgonine (p-OH BZE), and norbenzoylecgonine (nor-BZE) metabolites in human urine. The method was linear for BZE, m-OH BZE, and p-OH BZE from 1.2 to 10,000 ng/mL with limits of detection (LOD) and quantification (LOQ) of 1.2 ng/mL. Nor-BZE was linear from 5 to 10,000 ng/mL with an LOD and LOQ of 1.2 and 5 ng/mL, respectively. The intrarun precision measured as the coefficient of variation of 10 replicates of a 100 ng/mL control was less than 2.6%, and the interrun precision for 5 replicates of the same control across 8 batches was less than 4.8% for all analytes. No assay interference was noted from controls containing cocaine, cocaethylene, and ecgonine methyl ester. Excellent data concordance (R2 > 0.994) was found for direct comparison of the automated SPE-LC-MS-MS procedure and an existing gas chromatography-MS procedure using 94 human urine samples previously determined to be positive for BZE. The automated specimen handling and SPE procedure, when compared to the traditional extraction schema, eliminates the human factors of specimen handling, processing, extraction, and derivatization, thereby reducing labor costs and rework resulting from batch handling issues, and may reduce the number of fume hoods required in the laboratory.

Simultaneous determination of five bioactive components in radix glycyrrhizae by pressurised liquid extraction combined with UPLC-PDA and UPLC/ESI-QTOF-MS confirmation.

PubMed

Zhou, Shujun; Cao, Jiliang; Qiu, Feng; Kong, Weijun; Yang, Shihai; Yang, Meihua

2013-01-01

Glycyrrhizae species are popular ingredients of herbal medicine in most traditional Chinese medicine prescriptions, and they mainly contain flavonoids and triterpene saponins. The contents of these bioactive compounds may vary in different batches and affect the therapeutic effects. Thus comprehensive quality control and monitoring of their herbal formulation are of paramount concern. To establish a rapid, effective pressurised liquid extraction (PLE) and ultra-performance liquid chromatography coupled with photodiode array (UPLC-PDA) method to evaluate the quality of Glycyrrhizae species. Radix Glycyrrhizae was extracted by PLE using 70% ethanol at 100°C for 15 min during three static extraction cycles. Separation was performed using an UPLC system to quantify five bioactive compounds, namely liquiritin apioside, liquiritin, liquiritigenin, glycyrrhizic acid and glycyrrhetinic acid, in 12 batches of samples of different origins in China. Furthermore, the samples were analysed using an ultra-performance liquid chromatography coupled with electrospray ionisation and time-of-flight mass spectrometry (UPLC/ESI-QTOF-MS) system to confirm the results. The calibration curves of all five analytes showed good linearity (R(2)  > 0.9997). Accuracy, precision and repeatability were all within required limits. The mean recoveries measured at the three concentrations were higher than 93.7% with RSDs lower than < 3.33% for the targets. The established PLE and UPLC-PDA method could serve as a rapid and effective method for quality evaluation of Radix Glycyrrhizae. The UPLC technique can be considered as an attractive alternative to HPLC in routine quality control of Chinese medicine, especially in situations where high sample throughput and fast analytical speed are required. Copyright © 2013 John Wiley & Sons, Ltd.

Polyaniline/cyclodextrin composite coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the analysis of trace polychlorinated biphenyls in environmental waters.

PubMed

Lei, Yun; He, Man; Chen, Beibei; Hu, Bin

2016-04-01

A novel polyaniline/α-cyclodextrin (PANI/α-CD) composite coated stir bar was prepared by sol-gel process for the analysis of polychlorinated biphenyls (PCBs) in this work. The preparation reproducibility of the PANI/α-CD-coated stir bar was good, with relative standard deviations (RSDs) ranging from 2.3% to 3.7% (n=7) and 2.0% to 3.8% (n=7) for bar to bar and batch to batch, respectively. Based on it, a novel method of PANI/α-CD-coated stir bar sorptive extraction (SBSE) followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for the determination of trace PCBs in environmental waters. To obtain the best extraction performance for target PCBs, several parameters affecting SBSE, such as extraction time, stirring rate, and ionic strength were investigated. Under optimal experimental conditions, the limits of detection (LODs) of the proposed method for seven PCBs were in the range of 0.048-0.22 μg/L, and the RSDs were 5.3-9.8% (n=7, c=1 μg/L). Enrichment factors (EFs) ranging from 39.8 to 68.4-fold (theoretical EF, 83.3-fold) for target analytes were achieved. The proposed method was successfully applied for the determination of seven target PCBs in Yangtze River water and East Lake water, and the recoveries were in the range of 73.0-120% for the spiked East Lake water samples and 82.7-121% for the spiked Yangtze River water samples, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Sodium-dependent transport of sugars and iodide from the cerebral venticles of the rabbit.

PubMed

Bradbury, M W; Brondsted, H E

1973-10-01

1. The objective was to discover whether the extraction of sugars and iodide from the perfused cerebral ventricles is Na(+)-dependent.2. In the ventriculo-aqueductal and ventriculo-cisternal perfusion systems in the rabbit the extraction of (14)C-labelled D-hexoses (glucose, 3-O-methyl-glucose, alpha-methyl-glucoside and galactose), (131)I(-) and (24)Na was inhibited when 82% of the Na(+) in the perfusion fluid was replaced by choline. The extraction returned to control levels when the Na(+) concentration in the perfusion fluid was returned to normal.3. Ouabain, 5 x 10(-5)M in the perfusion fluid inhibited the extraction of the above (14)C sugars and (131)I(-), but hardly affected that of [(3)H]2-deoxy-D-glucose. It enhanced the extraction of (24)Na. C.s.f. production was usually totally inhibited.4. The extraction of [(14)C]urea remained unchanged during perfusion with low Na(+) fluid or ouabain.5. Recovery from brain of [(14)C]3-O-methyl-glucose, [(3)H]2-deoxy-glucose and (131)I(-) was low while recovery of [(14)C]alpha-methyl-glucoside and (24)Na was high. On an equal weight basis recovery of [(14)C]3-O-methyl-glucose was about twelve times higher from the choroid plexus than from the brain.6. Part of the movement of (14)C sugars may be explained on basis of a Na(+)-gradient hypothesis with involvement of the Na(+) pump at the blood-c.s.f. or blood-brain barriers.7. The rate of c.s.f. production from the first three ventricles comprised about 40% of the rate from all four ventricles. The extraction of sugars, urea and cations was similar in both perfusion systems while the extraction of (131)I(-) was higher in the ventriculo-cisternal system than in the ventriculo-aqueductal system.

A sensitive and specific liquid chromatography mass spectrometry method for simultaneous determination of berberine, palmatine, coptisine, epiberberine and jatrorrhizine from Coptidis Rhizoma in rat plasma

NASA Astrophysics Data System (ADS)

Yu, Sen; Pang, Xiaoyan; Deng, Yuanxiong; Liu, Li; Liang, Yan; Liu, Xiaodong; Xie, Lin; Wang, Guangji; Wang, Xinting

2007-11-01

A sensitive and specific liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and quantification of five protoberberine alkaloids, which are berberine, palmatine, coptisine, epiberberine and jatrorrhizine, in rat plasma using tetrahydroberberine as an internal standard. Following solid-phase extraction, the analytes were separated by linear gradient elution on a Shim-pack ODS (4.6 [mu]m, 150 mm × 2.0 mm i.d.) column and analyzed in selected ion monitoring (SIM) mode with a positive electrospray ionization (ESI) interface using the respective [M]+ and [M + H]+ ions, [M]+ = 336 for berberine; 320 for coptisine; 336 for epiberberine; 338 for jatrorrhizine; 352 for palmatine and [M + H]+ = 340 for the internal standard. The method was validated over the concentration range of 0.31-20 ng mL-1 for all the five protoberberine alkaloids. Within-batch and between-batch precisions (R.S.D.%) were all within 15% and accuracy (%Er) ranged from -5 to 5%. The lower limits of quantification were 0.31 ng mL-1 for all analytes. The extraction recoveries were on average 80.8% for berberine, 67E0% for coptisine, 66.2% for epiberberine, 71.8% for jatrorrhizine and 73E2% for palmatine. The validated method was used to study the pharmacokinetic profile of the five protoberberine alkaloids in rat plasma after oral administration of Coptidis Rhizoma extract.

Biodegradable microfabricated plug-filters for glaucoma drainage devices.

PubMed

Maleki, Teimour; Chitnis, Girish; Park, Jun Hyeong; Cantor, Louis B; Ziaie, Babak

2012-06-01

We report on the development of a batch fabricated biodegradable truncated-cone-shaped plug filter to overcome the postoperative hypotony in nonvalved glaucoma drainage devices. Plug filters are composed of biodegradable polymers that disappear once wound healing and bleb formation has progressed past the stage where hypotony from overfiltration may cause complications in the human eye. The biodegradable nature of device eliminates the risks associated with permanent valves that may become blocked or influence the aqueous fluid flow rate in the long term. The plug-filter geometry simplifies its integration with commercial shunts. Aqueous humor outflow regulation is achieved by controlling the diameter of a laser-drilled through-hole. The batch compatible fabrication involves a modified SU-8 molding to achieve truncated-cone-shaped pillars, polydimethylsiloxane micromolding, and hot embossing of biodegradable polymers. The developed plug filter is 500 μm long with base and apex plane diameters of 500 and 300 μm, respectively, and incorporates a laser-drilled through-hole with 44-μm effective diameter in the center.

Silica extraction from geothermal water

DOEpatents

Bourcier, William L; Bruton, Carol J

2014-09-23

A method of producing silica from geothermal fluid containing low concentration of the silica of less than 275 ppm includes the steps of treating the geothermal fluid containing the silica by reverse osmosis treatment thereby producing a concentrated fluid containing the silica, seasoning the concentrated fluid thereby producing a slurry having precipitated colloids containing the silica, and separating the silica from the slurry.

Mineral displacement and -dissolution processes and their relevance to rock porosity and permeability in Rotliegend sandstones of the Altmark natural gas field (central Germany) - results from CO2 laboratory batch experiments

NASA Astrophysics Data System (ADS)

Pudlo, Dieter; Enzmann, Frieder; Heister, Katja; Werner, Lars; Ganzer, Leonhard; Reitenbach, Viktor; Henkel, Steven; Albrecht, Daniel; Gaupp, Reinhard

2014-05-01

The Rotliegend reservoir sandstones of the Altmark area (central Germany) comprise the second largest natural gas field of Europe. These sandstones were deposited on a playa-like continental platform with braided river systems, ephemeral lakes and aeolian dunes under semi-arid conditions. Some of the pristine, red coloured deposits suffered intensive late diagenetic alteration and are now preserved as bleached, high porous and permeable sandstones. To evaluate the relevance of distinct fluids and their fluid-rock alteration reactions on such bleaching processes we performed laboratory static batch experiments on the Altmark sandstones. These 4-6 week lasting runs were conducted with CO2 saturated synthetic brines under typical Altmark reservoir conditions (p= 20 MPa, T= 125°C). Thereby mineralogical, petrophysical and (hydro- and geo-) chemical rock features were maintained prior and after the experiments. Chemical data proved the dissolution of carbonate and sulphate minerals during the runs, whereas the variation in abundance of further elements was within the detection limit of analytical accuracy. However, FE-SEM investigations on used, evaporated brines reveal the presence of illite and chlorite minerals within a matrix of Ca-, Si-, Fe, Al-, Na- and S components (carbonate, anhydrite, albite and Fe-(hydr-) oxides ?). By porosity and relative permeability measurements an increase in both rock features was observed after the runs, indicating that mineral dissolution and/or (clay) fine migration/detachment occurred during the experiments. Mineral dissolution, especially of pore-filling cements (e.g. carbonate-, sulphate minerals) is also deduced by BET analysis, in determining the specific surface of the sandstones. The size of these reactive surfaces increased after the experiments, suggesting that after the dissolution of pore-filling cements, formerly armoured grain rimming clay cutans were exposed to potential migrating fluids. These findings are also supported by µ-CT investigations. Here, the achieved 3D modelling data indicate an increase in reactive surface areas exposed to the pore space (which is in accord to the BET observations), as well as an enhancement in rock porosity and permeability after the runs. Moreover, these simulations showed that a remarkable mass (mineral) transfer was induced by the experiments, which led to a displacement of the porosity and permeability distribution in the sandstones and therefore a change in the fluid flow characteristics within the rocks - a parameter most important for every fluid-rock process. These observations are quite astonishing because they suggest that not only fluid velocity (e.g. during fluid flow experiments) might detach and transport grain rimming (clay) minerals, but also that physico-chemical reactions may enforce the release of such solids, even during almost static p-/T-/Xfluid conditions, as used in our experiments.

Survey of 800+ data sets from human tissue and body fluid reveals xenomiRs are likely artifacts

PubMed Central

Kang, Wenjing; Bang-Berthelsen, Claus Heiner; Holm, Anja; Houben, Anna J.S.; Müller, Anne Holt; Thymann, Thomas; Pociot, Flemming; Estivill, Xavier; Friedländer, Marc R.

2017-01-01

miRNAs are small 22-nucleotide RNAs that can post-transcriptionally regulate gene expression. It has been proposed that dietary plant miRNAs can enter the human bloodstream and regulate host transcripts; however, these findings have been widely disputed. We here conduct the first comprehensive meta-study in the field, surveying the presence and abundances of cross-species miRNAs (xenomiRs) in 824 sequencing data sets from various human tissues and body fluids. We find that xenomiRs are commonly present in tissues (17%) and body fluids (69%); however, the abundances are low, comprising 0.001% of host human miRNA counts. Further, we do not detect a significant enrichment of xenomiRs in sequencing data originating from tissues and body fluids that are exposed to dietary intake (such as liver). Likewise, there is no significant depletion of xenomiRs in tissues and body fluids that are relatively separated from the main bloodstream (such as brain and cerebro-spinal fluids). Interestingly, the majority (81%) of body fluid xenomiRs stem from rodents, which are a rare human dietary contribution but common laboratory animals. Body fluid samples from the same studies tend to group together when clustered by xenomiR compositions, suggesting technical batch effects. Last, we performed carefully designed and controlled animal feeding studies, in which we detected no transfer of plant miRNAs into rat blood, or bovine milk sequences into piglet blood. In summary, our comprehensive computational and experimental results indicate that xenomiRs originate from technical artifacts rather than dietary intake. PMID:28062594

Separation of aflatoxin B1 from synthetic physiological fluids using talc and diatomite: Kinetic and isotherm aspects.

PubMed

Sprynskyy, Myroslav; Krzemień-Konieczka, Iwona; Gadzała-Kopciuch, Renata; Buszewski, Bogusław

2018-01-01

The objective of the study was to examine adsorption of the aflatoxin B1 from synthetic gastric fluid and synthetic intestinal fluid by talc, raw and calcined diatomite. The kinetic and equilibrium adsorption processes were studied in the batch adsorption experiments applying high performance liquid chromatography for the aflatoxin B1 determination. The kinetic study showed a very fast adsorption of the aflatoxin B1 onto the selected adsorbents from the both physiological fluids with reaching equilibrium within 1-15min. The aflatoxin B1 was almost completely adsorbed in initial linear step of the kinetic process that can be described well by the zero-order kinetics model. The experimental data of the equilibrium adsorption were characterized using the Langmuir and Freundlich isotherm models. The high adsorption effectiveness was found in a range of 90%-100% and 60%-100% for the diatomite samples and the talc respectively at the initial concentrations of the aflatoxin B1 as 31-300ng/mL. The possible mechanisms of the aflatoxin adsorption onto the used mineral adsorbents are also discussed in the work. Copyright © 2017 Elsevier B.V. All rights reserved.

Anthropogenic seismicity rates and operational parameters at the Salton Sea Geothermal Field.

PubMed

Brodsky, Emily E; Lajoie, Lia J

2013-08-02

Geothermal power is a growing energy source; however, efforts to increase production are tempered by concern over induced earthquakes. Although increased seismicity commonly accompanies geothermal production, induced earthquake rate cannot currently be forecast on the basis of fluid injection volumes or any other operational parameters. We show that at the Salton Sea Geothermal Field, the total volume of fluid extracted or injected tracks the long-term evolution of seismicity. After correcting for the aftershock rate, the net fluid volume (extracted-injected) provides the best correlation with seismicity in recent years. We model the background earthquake rate with a linear combination of injection and net production rates that allows us to track the secular development of the field as the number of earthquakes per fluid volume injected decreases over time.

Membrane-mediated extractive fermentation for lactic acid production from cellulosic biomass.

PubMed

Chen, R; Lee, Y Y

1997-01-01

Lactic acid production from cellulosic biomass by cellulase and Lactobacillus delbrueckii was studied in a fermenter-extractor employing a microporous hollow fiber membrane (MHF). This bioreactor system was operated under a fed-batch mode with continuous removal of lactic acid by anin situ extraction. A tertiary amine (Alamine 336) was used as an extractant for lactic acid. The extraction capacity of Alamine 336 is greatly enhanced by addition of alcohol. Long-chain alcohols serve well for this purpose since they are less toxic to micro-organism. Addition of kerosene, a diluent, was necessary to reduce the solvent viscosity. A solvent mixture of 20% Alamine 336, 40% oleyl alcohol, and 40% kerosene was found to be most effective in the extraction of lactic acid. Progressive change of pH from an initial value of 5.0 down to 4.3 has significantly improved the overall performance of the simultaneous saccharification and extractive fermentation over that of constant pH operation. The change of pH was applied to promote cell growth in the early phase, and extraction in the latter phase.

Rapid Determination of Two Triterpenoid Acids in Chaenomelis Fructus Using Supercritical Fluid Extraction On-line Coupled with Supercritical Fluid Chromatography.

PubMed

Zhang, Xiaotian; Ji, Feng; Li, Yueqi; He, Tian; Han, Ya; Wang, Daidong; Lin, Zongtao; Chen, Shizhong

2018-01-01

In this study, an on-line supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) method was developed for the rapid determination of oleanoic acid and ursolic acid in Chaenomelis Fructus. After optimization of the conditions, the two triterpenoid acids was obtained by SFE using 20% methanol as a modifier at 35°C in 8 min. They were resolved on a Shim-pack UC-X Diol column (4.6 × 150 mm, 3 μm) in 14 min (0 - 10 min, 5 - 10%; 10 - 14 min, 10% methanol in CO 2 ) with a backpressure of 15 MPa at 40°C. The on-line SFE-SFC method could be completed within 40 min (10.79 mg/g dry plant, R s = 2.36), while the ultrasound-assisted extraction and HPLC method required at least 90 min (3.55 mg/g dry plant, R s = 1.92). This on-line SFE-SFC method is powerful to simplify the pre-processing and quantitative analysis of natural products.

Supercritical Fluid Extraction of Pyrrolidine Alkaloid from Leaves of Piper amalago L.

PubMed Central

Filho, L. C.; Faiões, V. S.; Cunha-Júnior, E. F.; Torres-Santos, E. C.; Cortez, D. A. G.

2017-01-01

Supercritical fluid extraction was used to extract the alkaloid N-[7-(3′,4′-methylenedioxyphenyl)-2(Z),4(Z)-heptadienoyl]pyrrolidine from leaves of Piper amalago L. A three-level orthogonal array design matrix, OAD OA9(34), was used for optimization of the parameters of supercritical extraction of the alkaloid, employing supercritical carbon dioxide: extraction time (20, 40, and 60 min), temperature (40, 50, and 60°C), pressure (150, 200, and 250 bar), and the use of cosolvents (ethanol, methanol, and propyleneglycol). All parameters had significant effect on the alkaloid yield. The alkaloid yield after 60 min of extraction without cosolvents at 9 different conditions (32) in terms of temperature (40, 50, and 60°C) and pressure (150, 200, and 250 bar) was also evaluated. The optimal yield (≈3.8 mg g−1) was obtained with supercritical CO2 + methanol (5% v : v) at 40°C and 200 bar for 60 min of extraction. PMID:28539966

Phytosterols and their extraction from various plant matrices using supercritical carbon dioxide: a review.

PubMed

Uddin, Md Salim; Sarker, Md Zaidul Islam; Ferdosh, Sahena; Akanda, Md Jahurul Haque; Easmin, Mst Sabina; Bt Shamsudin, Siti Hadijah; Bin Yunus, Kamaruzzaman

2015-05-01

Phytosterols provide important health benefits: in particular, the lowering of cholesterol. From environmental and commercial points of view, the most appropriate technique has been searched for extracting phytosterols from plant matrices. As a green technology, supercritical fluid extraction (SFE) using carbon dioxide (CO2) is widely used to extract bioactive compounds from different plant matrices. Several studies have been performed to extract phytosterols using supercritical CO2 (SC-CO2) and this technology has clearly offered potential advantages over conventional extraction methods. However, the efficiency of SFE technology fully relies on the processing parameters, chemistry of interest compounds, nature of the plant matrices and expertise of handling. This review covers SFE technology with particular reference to phytosterol extraction using SC-CO2. Moreover, the chemistry of phytosterols, properties of supercritical fluids (SFs) and the applied experimental designs have been discussed for better understanding of phytosterol solubility in SC-CO2. © 2014 Society of Chemical Industry.

Characterization of allergoids.

PubMed

Himly, Martin; Carnés, Jerónimo; Fernández-Caldas, Enrique; Briza, Peter; Ferreira, Fatima

2009-01-01

So far it has not been possible to measure the amount of major allergens in the complexes after chemical modification. Furthermore, the presence of minor allergens remained obscure, unless antibodies were successfully generated by animal immunization with allergoids and shown to be reactive with purified natural or recombinant allergens in immunological assays. Thus, we adapted and employed a set of physicochemical methods with the aim of elucidating the molecular size and allergen composition of allergoids. Using online-HPSEC light scattering and DLS, it was shown that two thirds of depigmented allergoid prepared from birch pollen extracts adopted a MW between 1000 and 2000 kDa. The question of reproducibility of the polymerization reaction was addressed by investigating four batches of P. pratense allergoid. Three out of the four batches contained 73 to 77% of polymerized molecules in the above-mentioned range of molecular sizes. One batch showed a significantly higher content of molecules with a MW exceeding 2 MDa. Analysis of allergen composition in B. alba allergoids revealed the presence of all relevant Bet v 1 isoforms and minor allergens except for Bet v 3 and Bet v 4, which was in good agreement with the allergens detected in the native extracts. It should be noted that Bet v 3 has not been detected at the protein level before. Similarly, good agreement in allergen composition between allergoid and native extract was also found for D. pteronyssinus. Presently, the European Directorate for Quality of Medicines and Healthcare (EDQM) is committed to the application of the 3R principles (i. e. replace, reduce, refine the use of animals) for the quality control of medicines wherever possible. This is reflected by the regular review of the monographs of the European Pharmacopoeia and the introduction of alternative tests. For instance, recently it was decided to replace the rabbit pyrogen test by an in vitro test. Furthermore, through the Biological Standardisation Programme the EDQM develops, validates, and establishes alternative test methods in the field of quality control of biologicals (personal communication with Karl-Heinz Buchheit, EDQM). Therefore, the approach presented here for the characterization of allergoids relying on physicochemical methods shall also serve the growing needs for alternative methods to animal testing.

Influence of high-pressure homogenization, ultrasonication, and supercritical fluid on free astaxanthin extraction from β-glucanase-treated Phaffia rhodozyma cells.

PubMed

Hasan, Mojeer; Azhar, Mohd; Nangia, Hina; Bhatt, Prakash Chandra; Panda, Bibhu Prasad

2016-01-01

In this study astaxanthin production by Phaffia rhodozyma was enhanced by chemical mutation using ethyl methane sulfonate. The mutant produces a higher amount of astaxanthin than the wild yeast strain. In comparison to supercritical fluid technique, high-pressure homogenization is better for extracting astaxanthin from yeast cells. Ultrasonication of dimethyl sulfoxide, hexane, and acetone-treated cells yielded less astaxanthin than β-glucanase enzyme-treated cells. The combination of ultrasonication with β-glucanase enzyme is found to be the most efficient method of extraction among all the tested physical and chemical extraction methods. It gives a maximum yield of 435.71 ± 6.55 µg free astaxanthin per gram of yeast cell mass.

Preparative isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. using supercritical fluid extraction combined with consecutive high-speed countercurrent chromatography.

PubMed

Yan, Rongwei; Shen, Jie; Liu, Xiaojing; Zou, Yong; Xu, Xinjun

2018-05-01

The objective of this study was to develop a consecutive preparation method for the isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. The process involved supercritical fluid extraction with CO 2 , solvent extraction, and two-step high-speed countercurrent chromatography. Pressure, temperature, and the volume of entrainer were optimized as 27 MPa, 52°C, and 60 mL by response surface methodology in supercritical fluid extraction with CO 2 , and the yield of the crude extracts was 7.91 g from 100 g of leaves. Subsequently, 80% methanol/water was used to extract and condense the three compounds from the crude extracts, and 4.23 g of methanol/water extracts was obtained. Then, a two-step high-speed countercurrent chromatography procedure was developed for the isolation of the three target compounds from methanol/water extracts, including conventional high-speed countercurrent chromatography for further enrichment and consecutive high-speed countercurrent chromatography for purification. The yield of concentrates from high-speed countercurrent chromatography was 2.50 g from 4.23 g of methanol/water extracts. Finally, the consecutive high-speed countercurrent chromatography produced 103.2 mg of hainanmurpanin, 244.7 mg of meranzin, and 255.4 mg of phebalosin with purities up to 97.66, 99.36, and 98.64%, respectively, from 900 mg of high-speed countercurrent chromatography concentrates in one run of three consecutive sample loadings without exchanging a solvent system. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of nobiletin from Citrus Unshiu peels by supercritical fluid and its CRE-mediated transcriptional activity.

PubMed

Oba, Chisato; Ota, Masaki; Nomura, Koichiro; Fujiwara, Hironori; Takito, Jiro; Sato, Yoshiyuki; Ohizumi, Yasushi; Inomata, Hiroshi

2017-04-15

Polymethoxyflavone (PMF) is one of bioactive compounds in Citrus Unshiu and included mainly in the peels rather than the fruits, seeds and leaves. Supercritical CO 2 extraction is one candidate for selective extraction of polymethoxyflavone and in this study, supercritical CO 2 extraction with/without ethanol entrainer from Citrus Unshiu peels was examined at a temperature of 333K and a pressure of 30MPa. CRE (cyclic AMP response element)-mediated transcriptional assay was examined by using the extracts from supercritical fluid extraction. The results showed that extracts including nobiletin increased with increasing ethanol concentration in supercritical CO 2 and the elapsed extraction time. Extracts at ethanol concentration of 5 mol% showed high CRE-mediated transcription activity. This can be caused by activity of the extract including nobiletin in addition to the other methoxylated flavonoid species such as tangeretin. Extracts at ethanol concentration of 50% showed the highest CRE-mediated transcription activity, which can be attributed to flavonoid glycoside such as hesperidin. From our investigations, flavonoid glycoside can be one of promoters of CRE-mediated transcription activity. Copyright © 2017 Elsevier GmbH. All rights reserved.

Comparison of supercritical fluid and Soxhlet extractions for the quantification of hydrocarbons from Euphorbia macroclada.

PubMed

Ozcan, Adnan; Ozcan, Asiye Safa

2004-10-08

This study compares conventional Soxhlet extraction and analytical scale supercritical fluid extraction (SFE) for their yields in extracting of hydrocarbons from arid-land plant Euphorbia macroclada. The plant material was firstly sequentially extracted with supercritical carbon dioxide, modified with 10% methanol (v/v) in the optimum conditions that is a pressure of 400atm and a temperature of 50 degrees C and then it was sonicated in methylene chloride for an additional 4h. E. macroclada was secondly extracted by using a Soxhlet apparatus at 30 degrees C for 8h in methylene chloride. The validated SFE was then compared to the extraction yield of E. macroclada with a Soxhlet extraction by using the Student's t-test at the 95% confidence level. All of extracts were fractionated with silica-gel in a glass column to get better hydrocarbon yields. Thus, the highest hydrocarbons yield from E. macroclada was achieved with SFE (5.8%) when it compared with Soxhlet extractions (1.1%). Gas chromatography (GC) analysis was performed to determine the quantitative hydrocarbons from plant material. The greatest quantitative hydrocarbon recovery from GC was obtained by supercritical carbon dioxide extract (0.6mgg(-1)).

Preparation and application of the sol-gel-derived acrylate/silicone co-polymer coatings for headspace solid-phase microextraction of 2-chloroethyl ethyl sulfide in soil.

PubMed

Liu, Mingming; Zeng, Zhaorui; Fang, Huaifang

2005-05-27

Three types of novel acrylate/silicone co-polymer coatings, including co-poly(methyl acrylate/hydroxy-terminated silicone oil) (MA/OH-TSO), co-poly(methyl methacrylate/OH-TSO) (MMA/OH-TSO) and co-poly(butyl methacrylate/OH-TSO) (BMA/OH-TSO), were prepared for the first time by sol-gel method and cross-linking technology and subsequently applied to headspace solid-phase microextraction (HS-SPME) of 2-chloroethyl ethyl sulfide (CEES), a surrogate of mustard, in soil. The underlying mechanisms of the coating process were discussed and confirmed by IR spectra. The selectivity of the three types of sol-gel-derived acrylate/silicone coated fibers was studied, and the BMA/OH-TSO coated fibers exhibited the highest extraction ability to CEES. The concentration of BMA and OH-TSO in sol solution was optimized, and the BMA/OH-TSO (3:1)-coated fibers possessed the highest extraction efficiency. Compared with commercially available polyacrylate (PA) fiber, the sol-gel-derived BMA/OH-TSO (3:1) fibers showed much higher extraction efficiency to CEES. Therefore, the BMA/OH-TSO (3:1)-coated fibers were chosen for the analysis of CEES in soil matrix. The reproducibility of coating preparation was satisfactory, with the RSD 2.39% within batch and 3.52% between batches, respectively. The coatings proved to be quite stable at high temperature (to 350 degrees C) and in different solvents (organic or inorganic), thus their lifetimes (to 150 times) are longer than conventional fibers. Extraction parameters, such as the volume of water added to the soil, extraction temperature and time, and the ionic strength were optimized. The linearity was from 0.1 to 10 microg/g, the limit of detection (LOD) was 2.7 ng/g, and the RSD was 2.19%. The recovery of CEES was 88.06% in agriculture soil, 92.61% in red clay, and 101.95% in sandy soil, respectively.

Extracting metals directly from metal oxides

DOEpatents

Wai, Chien M.; Smart, Neil G.; Phelps, Cindy

1997-01-01

A method of extracting metals directly from metal oxides by exposing the oxide to a supercritical fluid solvent containing a chelating agent is described. Preferably, the metal is an actinide or a lanthanide. More preferably, the metal is uranium, thorium or plutonium. The chelating agent forms chelates that are soluble in the supercritical fluid, thereby allowing direct removal of the metal from the metal oxide. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is selected from the group consisting of .beta.-diketones, halogenated .beta.-diketones, phosphinic acids, halogenated phosphinic acids, carboxylic acids, halogenated carboxylic acids, and mixtures thereof. In especially preferred embodiments, at least one of the chelating agents is fluorinated. The method provides an environmentally benign process for removing metals from metal oxides without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the metal recovered, to provide an economic, efficient process.

Extracting metals directly from metal oxides

DOEpatents

Wai, C.M.; Smart, N.G.; Phelps, C.

1997-02-25

A method of extracting metals directly from metal oxides by exposing the oxide to a supercritical fluid solvent containing a chelating agent is described. Preferably, the metal is an actinide or a lanthanide. More preferably, the metal is uranium, thorium or plutonium. The chelating agent forms chelates that are soluble in the supercritical fluid, thereby allowing direct removal of the metal from the metal oxide. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is selected from the group consisting of {beta}-diketones, halogenated {beta}-diketones, phosphinic acids, halogenated phosphinic acids, carboxylic acids, halogenated carboxylic acids, and mixtures thereof. In especially preferred embodiments, at least one of the chelating agents is fluorinated. The method provides an environmentally benign process for removing metals from metal oxides without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the metal recovered, to provide an economic, efficient process. 4 figs.

Preliminary design of a supercritical CO2 wind tunnel

NASA Astrophysics Data System (ADS)

Re, B.; Rurale, A.; Spinelli, A.; Guardone, A.

2017-03-01

The preliminary design of a test-rig for non-ideal compressible-fluid flows of carbon dioxide is presented. The test-rig is conceived to investigate supersonic flows that are relevant to the study of non-ideal compressible-fluid flows in the close proximity of the critical point and of the liquid-vapor saturation curve, to the investigation of drop nucleation in compressors operating with supercritical carbon dioxide and and to the study of flow conditions similar to those encountered in turbines for Organic Rankine Cycle applications. Three different configurations are presented and examined: a batch-operating test-rig, a closed-loop Brayton cycle and a closed-loop Rankine cycle. The latter is preferred for its versatility and for economic reasons. A preliminary design of the main components is reported, including the heat exchangers, the chiller, the pumps and the test section.

Micromachined ultrasonic droplet generator based on a liquid horn structure

NASA Astrophysics Data System (ADS)

Meacham, J. M.; Ejimofor, C.; Kumar, S.; Degertekin, F. L.; Fedorov, A. G.

2004-05-01

A micromachined ultrasonic droplet generator is developed and demonstrated for drop-on-demand fluid atomization. The droplet generator comprises a bulk ceramic piezoelectric transducer for ultrasound generation, a reservoir for the ejection fluid, and a silicon micromachined liquid horn structure as the nozzle. The nozzles are formed using a simple batch microfabrication process that involves wet etching of (100) silicon in potassium hydroxide solution. Device operation is demonstrated by droplet ejection of water through 30 μm orifices at 1.49 and 2.30 MHz. The finite-element simulations of the acoustic fields in the cavity and electrical impedance of the device are in agreement with the measurements and indicate that the device utilizes cavity resonances in the 1-5 MHz range in conjunction with acoustic wave focusing by the pyramidally shaped nozzles to achieve low power operation.

Image processing in digital pathology: an opportunity to solve inter-batch variability of immunohistochemical staining

NASA Astrophysics Data System (ADS)

van Eycke, Yves-Rémi; Allard, Justine; Salmon, Isabelle; Debeir, Olivier; Decaestecker, Christine

2017-02-01

Immunohistochemistry (IHC) is a widely used technique in pathology to evidence protein expression in tissue samples. However, this staining technique is known for presenting inter-batch variations. Whole slide imaging in digital pathology offers a possibility to overcome this problem by means of image normalisation techniques. In the present paper we propose a methodology to objectively evaluate the need of image normalisation and to identify the best way to perform it. This methodology uses tissue microarray (TMA) materials and statistical analyses to evidence the possible variations occurring at colour and intensity levels as well as to evaluate the efficiency of image normalisation methods in correcting them. We applied our methodology to test different methods of image normalisation based on blind colour deconvolution that we adapted for IHC staining. These tests were carried out for different IHC experiments on different tissue types and targeting different proteins with different subcellular localisations. Our methodology enabled us to establish and to validate inter-batch normalization transforms which correct the non-relevant IHC staining variations. The normalised image series were then processed to extract coherent quantitative features characterising the IHC staining patterns.

Image processing in digital pathology: an opportunity to solve inter-batch variability of immunohistochemical staining

PubMed Central

Van Eycke, Yves-Rémi; Allard, Justine; Salmon, Isabelle; Debeir, Olivier; Decaestecker, Christine

2017-01-01

Immunohistochemistry (IHC) is a widely used technique in pathology to evidence protein expression in tissue samples. However, this staining technique is known for presenting inter-batch variations. Whole slide imaging in digital pathology offers a possibility to overcome this problem by means of image normalisation techniques. In the present paper we propose a methodology to objectively evaluate the need of image normalisation and to identify the best way to perform it. This methodology uses tissue microarray (TMA) materials and statistical analyses to evidence the possible variations occurring at colour and intensity levels as well as to evaluate the efficiency of image normalisation methods in correcting them. We applied our methodology to test different methods of image normalisation based on blind colour deconvolution that we adapted for IHC staining. These tests were carried out for different IHC experiments on different tissue types and targeting different proteins with different subcellular localisations. Our methodology enabled us to establish and to validate inter-batch normalization transforms which correct the non-relevant IHC staining variations. The normalised image series were then processed to extract coherent quantitative features characterising the IHC staining patterns. PMID:28220842

Suberin Fatty Acids from Outer Birch Bark: Isolation and Physical Material Characterization.

PubMed

Heinämäki, Jyrki; Pirttimaa, Minni M; Alakurtti, Sami; Pitkänen, H Pauliina; Kanerva, Heimo; Hulkko, Janne; Paaver, Urve; Aruväli, Jaan; Yliruusi, Jouko; Kogermann, Karin

2017-04-28

The isolation and physical material properties of suberin fatty acids (SFAs) were investigated with special reference to their potential applications as novel pharmaceutical excipients. SFAs were isolated from outer birch bark (OBB) with a new extractive hydrolysis method. The present simplified isolation process resulted in a moderate batch yield and chemical purity of SFAs, but further development is needed for establishing batch-to-batch variation. Cryogenic milling was the method of choice for the particle size reduction of SFAs powder. The cryogenically milled SFAs powder exhibited a semicrystalline structure with apparent microcrystalline domains within an amorphous fatty acids matrix. The thermogravimetric analysis (TGA) of SFAs samples showed a good thermal stability up to 200 °C, followed by a progressive weight loss, reaching a plateau at about 95% volatilization at about 470 °C. The binary blends of SFAs and microcrystalline cellulose (MCC; Avicel PH 101) in a ratio of 25:75 (w/w) displayed good powder flow and tablet compression properties. The corresponding theophylline-containing tablets showed sustained or prolonged-release characteristics. The physicochemical and bulk powder properties of SFAs isolated from OBB are auspicious in terms of potential pharmaceutical excipient applications.

Antigenicity and viability of Anisakis larvae infesting hake heated at different time-temperature conditions.

PubMed

Vidacek, Sanja; de las Heras, Cristina; Solas, Maria Teresa; Mendizábal, Angel; Rodriguez-Mahillo, Ana I; Tejada, Margarita

2010-01-01

Heat treatments (40 to 94 degrees Celsius, 30 s to 60 min) were applied to different batches of Anisakis simplex L3 larvae isolated from hake ovaries and viscera to study the effect of heat on the viability of the larvae measured as mobility, emission of fluorescence under UV light, and changes in color after staining with specific dyes, and on A. simplex antigenic proteins. The aim was to determine the lowest time-temperature conditions needed to kill the larvae to avoid anisakiasis in consumers, and to evaluate whether high temperature modifies the antigenicity of A. simplex extracts. Heating at 60 degrees Celsius for 10 min (recommended by some authors) was considered unsafe, as differences in viability between batches were found, with some larvae presenting spontaneous movements in one batch. At higher temperatures (> or = 70 degrees Celsius for > or = 1 min), no movement of the larvae was observed. Antigenic protein Ani s 4 and A. simplex crude antigens were detected in the larvae heated at 94 + or - 1 degrees Celsius for 3 min. This indicates that allergic symptoms could be provoked in previously sensitized consumers, even if the larvae were killed by heat treatment.

Identification of a Panax ginseng fruit fingerprint by HPLC-ESI-MS.

PubMed

Zhao, H F; Xu, F F; Guo, Y T; Mi, H

2016-03-11

Over many years, parts of Panax ginseng (root and rhizome) have been identified and applied for medical purposes as traditional Chinese herbal medicine. Recently, research has indicated that ginseng fruit also contains similar compounds and is as rich as the other parts of the ginseng. This discovery may dramatically improve the efficient of outputs derived from ginseng products. Here, a new technique combining high-performance liquid chromatography (HPLC) with electrospray ionization tandem mass spectrometry (ESI-MS) was employed to identify the fingerprint of P. ginseng fruit. Using HPLC, compounds that are important for medical purposes were extracted and purified. Combined with ESI-MS, the characteristic peaks (nine common peaks) of those compounds were identified, and the accuracy was confirmed by analysis using the Chromatographic Fingerprint Similarity Evaluation System (2004A edition). Overall, 15 batches of ginseng fruit had a similarity of more than 0.80, 13 batches of samples had a similarity between 0.97 and 0.99, and two batches had a similarity less than 0.90. The test solution and mobile phase selection was discussed. The HPLC-ESI-MS method can produce repeatable and reliable results and can be applied in the quality control of P. ginseng fruit.

Heater Validation for the NEXT-C Hollow Cathodes

NASA Technical Reports Server (NTRS)

Verhey, Timothy R.; Soulas, George C.; Mackey, Jonathan Ar.

2017-01-01

Swaged cathode heaters whose design was successfully demonstrated under a prior flight project are to be provided by the NASA Glenn Research Center for the NEXT-C ion thruster being fabricated by Aerojet Rocketdyne. Extensive requalification activities were performed to validate process controls that had to be re-established or revised because systemic changes prevented reuse of the past approaches. A development batch of heaters was successfully fabricated based on the new process controls. Acceptance and cyclic life testing of multiple discharge and neutralizer sized heaters extracted from the development batch was initiated in August, 2016, with the last heater completing testing in April, 2017. Cyclic life testing results substantially exceeded the NEXT-C thruster requirement as well as all past experience for GRC fabricated units. The heaters demonstrated ultimate cyclic life capability of 19050 to 33500 cycles. A qualification batch of heaters is now being fabricated using the finalized process controls. A set of six heaters will be acceptance and cyclic tested to verify conformance to the behavior observed with the development heaters. The heaters for flight use will be then be provided to the contractor. This paper summarizes the fabrication process control activities and the acceptance and life testing of the development heater units.

Influence of solid-liquid separation method parameters employed in soil leaching tests on apparent metal concentration.

PubMed

Imoto, Yukari; Yasutaka, Tetsuo; Someya, Masayuki; Higashino, Kazuo

2018-05-15

Soil leaching tests are commonly used to evaluate the leachability of hazardous materials, such as heavy metals, from the soil. Batch leaching tests often enhance soil colloidal mobility and may require solid-liquid separation procedures to remove excess soil particles. However, batch leaching test results depend on particles that can pass through a 0.45μm membrane filter and are influenced by test parameters such as centrifugal intensity and filtration volume per filter. To evaluate these parameters, we conducted batch leaching experiments using metal-contaminated soils and focused on the centrifugal intensity and filtration volume per filter used in solid-liquid separation methods currently employed in standard leaching tests. Our experiments showed that both centrifugal intensity and filtration volume per filter affected the reproducibility of batch leaching tests for some soil types. The results demonstrated that metal concentrations in the filtrates significantly differed according to the centrifugal intensity when it was 3000 g for 2h or less. Increased filtration volume per filter led to significant decreases in filtrate metal concentrations when filter cakes formed during filtration. Comparison of the filtration tests using 0.10 and 0.45μm membrane filters showed statistically significant differences in turbidity and metal concentration. These findings suggest that colloidal particles were not adequately removed from the extract and contributed substantially to the apparent metal concentrations in the leaching test of soil containing colloidal metals. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Improving the hardness of dry granulated tablets containing sodium lauryl sulfate.

PubMed

Moore, Francis; Okelo, Geoffrey; Colón, Ivelisse; Kushner, Joseph

2010-11-15

The impact of the addition of a wetting agent, the surfactant sodium lauryl sulfate (SLS), on the tablet hardness of a dry granulated, solid oral dosage form was investigated. In three batches, SLS was added concurrently with: (1) a poorly soluble, highly hydrophobic active pharmaceutical ingredient (API) and the other excipients prior to the initial blending step, (2) magnesium stearate prior to roller compaction, or (3) magnesium stearate prior to tableting. A fourth batch, which did not contain SLS, served as a control. The maximum hardness of 100 mg, 1/4″-SRC tablets for the four batches--SLS added initially, prior to roller compaction, prior to tableting, and no SLS--were 61±3, 71±3, 89±5, and 86±3N, respectively, suggesting reduced processing of SLS improves tablet hardness by ∼50%. Dissolution of the tablets in 900 ml of simulated gastric fluid with paddles at 75 rpm showed that: (1) there was no impact on the insertion point of SLS into the process on API dissolution, and (2) that the presence of SLS improved dissolution by 5% compared to the control tablets. Adding SLS just prior to tableting can improve tablet hardness and yield similar dissolution performance relative to SLS addition prior to the initial blending step. Copyright © 2010 Elsevier B.V. All rights reserved.

Carob pod water extracts as feedstock for succinic acid production by Actinobacillus succinogenes 130Z.

PubMed

Carvalho, Margarida; Roca, Christophe; Reis, Maria A M

2014-10-01

Carob pods are a by-product of locust bean gum industry containing more than 50% (w/w) sucrose, glucose and fructose. In this work, carob pod water extracts were used, for the first time, for succinic acid production by Actinobacillus succinogenes 130Z. Kinetic studies of glucose, fructose and sucrose consumption as individual carbon sources till 30g/L showed no inhibition on cell growth, sugar consumption and SA production rates. Sugar extraction from carob pods was optimized varying solid/liquid ratio and extraction time, maximizing sugar recovery while minimizing the extraction of polyphenols. Batch fermentations containing 10-15g/L total sugars resulted in a maximum specific SA production rate of 0.61Cmol/Cmol X.h, with a yield of 0.55Cmol SA/Cmol sugar and a volumetric productivity of 1.61g SA/L.h. Results demonstrate that carob pods can be a promising low cost feedstock for bio-based SA production. Copyright © 2014 Elsevier Ltd. All rights reserved.

[The progress in speciation analysis of trace elements by atomic spectrometry].

PubMed

Wang, Zeng-Huan; Wang, Xu-Nuo; Ke, Chang-Liang; Lin, Qin

2013-12-01

The main purpose of the present work is to review the different non-chromatographic methods for the speciation analysis of trace elements in geological, environmental, biological and medical areas. In this paper, the sample processing methods in speciation analysis were summarized, and the main strategies for non-chromatographic technique were evaluated. The basic principles of the liquid extractions proposed in the published literatures recently and their advantages and disadvantages were discussed, such as conventional solvent extraction, cloud point extraction, single droplet microextraction, and dispersive liquid-liquid microextraction. Solid phase extraction, as a non-chromatographic technique for speciation analysis, can be used in batch or in flow detection, and especially suitable for the online connection to atomic spectrometric detector. The developments and applications of sorbent materials filled in the columns of solid phase extraction were reviewed. The sorbents include chelating resins, nanometer materials, molecular and ion imprinted materials, and bio-sorbents. Other techniques, e. g. hydride generation technique and coprecipitation, were also reviewed together with their main applications.

Extraction of microalgal lipids and the influence of polar lipids on biodiesel production by lipase-catalyzed transesterification.

PubMed

Navarro López, Elvira; Robles Medina, Alfonso; González Moreno, Pedro Antonio; Esteban Cerdán, Luis; Molina Grima, Emilio

2016-09-01

In order to obtain microalgal saponifiable lipids (SLs) fractions containing different polar lipid (glycolipids and phospholipids) contents, SLs were extracted from wet Nannochloropsis gaditana microalgal biomass using seven extraction systems, and the polar lipid contents of some fractions were reduced by low temperature acetone crystallization. We observed that the polar lipid content in the extracted lipids depended on the polarity of the first solvent used in the extraction system. Lipid fractions with polar lipid contents between 75.1% and 15.3% were obtained. Some of these fractions were transformed into fatty acid methyl esters (FAMEs, biodiesel) by methanolysis, catalyzed by the lipases Novozym 435 and Rhizopus oryzae in tert-butanol medium. We observed that the reaction velocity was higher the lower the polar lipid content, and that the final FAME conversions achieved after using the same lipase batch to catalyze consecutive reactions decreased in relation to an increase in the polar lipid content. Copyright © 2016 Elsevier Ltd. All rights reserved.

A Novel CO2-Responsive Viscoelastic Amphiphilic Surfactant Fluid for Fracking in Enhanced Oil/Gas Recovery

NASA Astrophysics Data System (ADS)

Zhong, L.; Wu, X.; Dai, C.

2017-12-01

Over the past decade, the rapid rise of unconventional shale gas and tight sandstone oil development through horizontal drilling and high volume hydraulic fracturing has expanded the extraction of hydrocarbon resources. Hydraulic fracturing fluids play very important roles in enhanced oil/gas recovery. However, damage to the reservoir rock and environmental contamination caused by hydraulic fracturing flowback fluids has raised serious concerns. The development of reservoir rock friendly and environmental benign fracturing fluids is in immediate demand. Studies to improve properties of hydraulic fracturing fluids have found that viscoelastic surfactant (VES) fracturing fluid can increase the productivity of gas/oil and be efficiently extracted after fracturing. Compared to conventional polymer fracturing fluid, VES fracturing fluid has many advantages, such as few components, easy preparation, good proppant transport capacity, low damage to cracks and formations, and environment friendly. In this work, we are developing a novel CO2-responsive VES fracking fluid that can readily be reused. This fluid has a gelling-breaking process that can be easily controlled by the presence of CO2 and its pressure. We synthesized erucamidopropyl dimethylamine (EA) as a thickening agent for hydraulic fracturing fluid. The influence of temperature, presence of CO2 and pressure on the viscoelastic behavior of this fluid was then investigated through rheological measurements. The fracturing fluid performance and recycle property were lastly studied using core flooding tests. We expect this fluid finds applications not only in enhanced oil/gas recovery, but also in areas such as controlling groundwater pollution and microfluidics.

Bio-Oil Separation and Stabilization by Near-Critical Propane Fractionation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ginosar, Daniel M.; Petkovic, Lucia M.; Agblevor, Foster A.

Bio-oils produced by thermal process are promising sources of sustainable, low greenhouse gas alternative fuels. These thermal processes are also well suited to decentralized energy production due to low capital and operating costs. Algae feedstocks for bio-oil production are of particular interest, due in part to their high-energy growth yields. Further, algae can be grown in non-arable areas in fresh, brackish, salt water, or even waste water. Unfortunately, bio-oils produced by thermal processes present significant stability challenges. These oils have complex chemical compositions, are viscous, reactive, and thermally unstable. Further, the components within the oils are difficult to separate bymore » fractional distillation. By far, the most effective separation and stabilization method has been solvent extraction. However, liquid phase extraction processes pose two main obstacles to commercialization; they require a significant amount of energy to remove and recover the solvent from the product, and they have a propensity for the solvent to become contaminated with minerals from the char and ash present in the original bio-oil. Separation and fractionation of thermally produced bio-oils using supercritical fluids (SCF) offers the advantages of liquid solvent extraction while drastically reducing energy demands and the predisposition to carry over solids into the extracted phase. SCFs are dense fluids with liquid-like solvent properties and gas-like transport properties. Further, SCF density and solvent strength can be tuned with minor adjustments in pressure, co-solvent addition, or gas anti-solvent addition. Catalytic pyrolysis oils were produced from Scenedesmus dimorphus algae using a fluid catalytic cracking catalyst. Bio-oil produced from catalytic fast pyrolysis (CFP) was separated using critical fluids. Propane extraction was performed at 65 °C at a fluid reduced pressure of 2.0 (85 bar) using an eight to one solvent to feed ratio by weight. Extraction of catalytic fast pyrolysis oil with near critical propane produced an oil extract that was physically and chemically different from and more stable than the original oil. The propane extract displayed lower viscosity and lower average molecular weight. The species present in the propane extract were likely the less polar that would be expected from using a non-polar solvent (propane). Carbonyl containing species in the extract were likely ketones and esters. The raffinate contained a higher amnount of OH bonded species along with the more polar more polar acids, amides, and alcohols. The higher concentration of nitrogen in the raffinate may confirm the presence of amides. Viscosity of the propane extract increased only half as much as that of the CFP bio-oil. Further, In situ NMR aging studies showed that the propane extract was more stable than the raw oil. In conclusion, propane extraction is a promising method to decrease the nitrogen content of bio-oils and to improve the stability of bio-oils obtained by the catalytic pyrolysis of algae based biomass.« less

Developing an effective means to reduce 5-hydroxymethyl-2-furfural from caramel colour.

PubMed

Guan, Yongguang; Chen, Mingshun; Yu, Shujuan; Tang, Qiang; Yan, He

2014-01-15

Supercritical carbon dioxide fluid extraction was used to extract 5-hydroxymethyl-2-furfural from caramel colour (solid content was about 75%). The procedure was carried out by response surface methodology using a quadratic polynomial model. Extraction pressure, time, temperature and ethanol content were selected as the independent variables. Conditions to obtain the highest extraction ratio of 5-hydroxymethyl-2-furfural were determined to be an extraction pressure of 21.65MPa, time of 46.7min, temperature of 35°C and 70% ethanol content of caramel colour. The predicted 5-hydroxymethyl-2-furfural extraction ratio was 87.42%. Under the conditions stated above, the experimental value of 5-hydroxymethyl-2-furfural extraction ratio was 86.98%, which was similar to the predicted value by the model. This study indicated that supercritical carbon dioxide fluid extraction can effectively reduce 5-hydroxymethyl-2-furfural from caramel colour, which can help food industry to improve the safety of the food material, as well as provide more healthy caramel colour for human beings. Copyright © 2013 Elsevier Ltd. All rights reserved.

Isolation of essential oil from different plants and herbs by supercritical fluid extraction.

PubMed

Fornari, Tiziana; Vicente, Gonzalo; Vázquez, Erika; García-Risco, Mónica R; Reglero, Guillermo

2012-08-10

Supercritical fluid extraction (SFE) is an innovative, clean and environmental friendly technology with particular interest for the extraction of essential oil from plants and herbs. Supercritical CO(2) is selective, there is no associated waste treatment of a toxic solvent, and extraction times are moderate. Further, supercritical extracts were often recognized of superior quality when compared with those produced by hydro-distillation or liquid-solid extraction. This review provides a comprehensive and updated discussion of the developments and applications of SFE in the isolation of essential oils from plant matrices. SFE is normally performed with pure CO(2) or using a cosolvent; fractionation of the extract is commonly accomplished in order to isolate the volatile oil compounds from other co-extracted substances. In this review the effect of pressure, temperature and cosolvent on the extraction and fractionation procedure is discussed. Additionally, a comparison of the extraction yield and composition of the essential oil of several plants and herbs from Lamiaceae family, namely oregano, sage, thyme, rosemary, basil, marjoram and marigold, which were produced in our supercritical pilot-plant device, is presented and discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

Dissolution kinetics of volatile organic compound vapors in water: An integrated experimental and computational study

NASA Astrophysics Data System (ADS)

Mahmoodlu, Mojtaba G.; Pontedeiro, Elizabeth M.; Pérez Guerrero, Jesús S.; Raoof, Amir; Majid Hassanizadeh, S.; van Genuchten, Martinus Th.

2017-01-01

In this study we performed batch experiments to investigate the dissolution kinetics of trichloroethylene (TCE) and toluene vapors in water at room temperature and atmospheric pressure. The batch systems consisted of a water reservoir and a connected headspace, the latter containing a small glass cylinder filled with pure volatile organic compound (VOC). Results showed that air phase concentrations of both TCE and toluene increased relatively quickly to their maximum values and then became constant. We considered subsequent dissolution into both stirred and unstirred water reservoirs. Results of the stirred experiments showed a quick increase in the VOC concentrations with time up to their solubility limit in water. VOC vapor dissolution was found to be independent of pH. In contrast, salinity had a significant effect on the solubility of TCE and toluene vapors. VOC evaporation and vapor dissolution in the stirred water reservoirs followed first-order rate processes. Observed data could be described well using both simplified analytical solutions, which decoupled the VOC dynamics in the air and water phases, as well as using more complete coupled solutions. However, the estimated evaporation (ke) and dissolution (kd) rate constants differed by up to 70% between the coupled and uncoupled formulations. We also numerically investigated the effects of fluid withdrawal from the small water reservoir due to sampling. While decoupling the VOC air and water phase mass transfer processes produced unreliable estimates of kd, the effects of fluid withdrawal on the estimated rate constants were found to be less important. The unstirred experiments showed a much slower increase in the dissolved VOC concentrations versus time. Molecular diffusion of the VOCs within the aqueous phase became then the limiting factor for mass transfer from air to water. Fluid withdrawal during sampling likely caused some minor convection within the reservoir, which was simulated by increasing the apparent liquid diffusion coefficient.

Supercritical fluid extraction of the non-polar organic compounds in meteorites

NASA Astrophysics Data System (ADS)

Sephton, M. A.; Pillinger, C. T.; Gilmour, I.

2001-01-01

The carbonaceous chondrite meteorites contain a variety of extraterrestrial organic molecules. These organic components provide a valuable insight into the formation and evolution of the solar system. Attempts at obtaining and interpreting this information source are hampered by the small sample sizes available for study and the interferences from terrestrial contamination. Supercritical fluid extraction represents an efficient and contamination-free means of isolating extraterrestrial molecules. Gas chromatography-mass spectrometry analyses of extracts from Orgueil and Cold Bokkeveld reveal a complex mixture of free non-polar organic molecules which include normal alkanes, isoprenoid alkanes, tetrahydronaphthalenes and aromatic hydrocarbons. These organic assemblages imply contributions from both terrestrial and extraterrestrial sources.

Extraction of three-dimensional silver nanostructures with supercritical fluid

NASA Astrophysics Data System (ADS)

Taguchi, Natsuo; Takeyasu, Nobuyuki; Kawata, Satoshi

2018-02-01

In a previous report, a self-growing approach was proposed for fabricating complex silver nanostructures, where silver dendrites were grown at silver nanoseeds in silver ion solution owing to plasmonic heating with ultraviolet light. Structures were deformed or destroyed when they were extracted with acetone and dried in air. In this Letter, we discuss the use of supercritical carbon dioxide fluid for the nondestructive extraction of nanostructures. We show the experimental results and discuss the laser power dependence of resultant structures. Another experiment was performed for nanostructure growth inside an agarose gel as a matrix. Silver nanostructures were immobilized without damage in an agarose skeleton network.

SUPERCRITICAL FLUID EXTRACTION OF SEMI-VOLATILE ORGANIC COMPOUNDS FROM PARTICLES

EPA Science Inventory

A nitrogen oxide flux chamber was modified to measure the flux of semi-volatile organic compounds (SVOCs). Part of the modification involved the development of methods to extract SVOCs from polyurethane foam (PUF), sand, and soil. Breakthroughs and extraction efficiencies were ...

User's instructions for the Grodins' respiratory control model using the UNIVAC 1110 remote batch and demand processing

NASA Technical Reports Server (NTRS)

1974-01-01

The transient and steady state response of the respiratory control system for variations in volumetric fractions of inspired gases and special system parameters are modeled. The program contains the capability to change workload. The program is based on Grodins' respiratory control model and can be envisioned as a feedback control system comprised of a plant (the controlled system) and the regulating component (controlling system). The controlled system is partitioned into 3 compartments corresponding to lungs, brain, and tissue with a fluid interconnecting patch representing the blood.

The Measurement of Human Body-Fluid Volumes: Resting Fluid Volumes Before and After Heat Acclimation

DTIC Science & Technology

2001-01-01

equilibration period. Erythrocytes aliquots were haemolysed before counting with saponin . Both counts were used to correct the derived ECFV, which was...was largely in accordance with the procedures of Greenleaf et al. (1980). This technique used an extraction procedure in which the dye was first...collection. Therefore, the above extraction procedure was not used. A major limitation of using a cellulose column is the possibility of not collecting all

Environmental risks associated with unconventional gas extraction: an Australian perspective

NASA Astrophysics Data System (ADS)

Mallants, Dirk; Bekele, Elise; Schmidt, Wolfgang; Miotlinski, Konrad; Gerke Gerke, Kirill

2015-04-01

Coal seam gas is naturally occurring methane gas (CH4) formed by the degradation of organic material in coal seam layers over geological times, typically over several millions of years. Unlike conventional gas resources, which occur as discrete accumulations in traps formed by folds and other structures in sedimentary layers, coal seam gas is generally trapped in low permeable rock by adsorption of the gas molecules within the rock formation and cannot migrate to a trap and form a conventional gas deposit. Extraction of coal seam gas requires producers to de pressurise the coal measures by abstracting large amounts of groundwater through pumping. For coal measures that have too low permeabilities for gas extraction to be economical, mechanical and chemical techniques are required to increase permeability and thus gas yield. One such technique is hydraulic fracturing (HF). Hydraulic fracturing increases the rate and total amount of gas extracted from coal seam gas reservoirs. The process of hydraulic fracturing involves injecting large volumes of hydraulic fracturing fluids under high pressure into the coal seam layers to open up (i.e. fracture) the gas-containing coal layers, thus facilitating extraction of methane gas through pumping. After a hydraulic fracturing operation has been completed in a coal seam gas well, the fracturing fluid pressure is lowered and a significant proportion of the injected fluid returns to the surface as "flowback" water via coal seam gas wells. Flowback water is fluid that returns to the surface after hydraulic fracturing has occurred but before the well is put into production; whereas produced water is fluid from the coal measure that is pumped to the surface after the well is in production. This paper summarises available literature data from Australian coal seam gas practices on i) spills from hydraulic fracturing-related fluids used during coal seam gas drilling and hydraulic fracturing operations, ii) leaks to soil and shallow groundwater of flowback water and produced water from surface impoundments, iii) risks from well integrity failure, and iv) increased gas in water bores.

Evaluation of DNA extraction methods and their clinical application for direct detection of causative bacteria in continuous ambulatory peritoneal dialysis culture fluids from patients with peritonitis by using broad-range PCR.

PubMed

Kim, Si Hyun; Jeong, Haeng Soon; Kim, Yeong Hoon; Song, Sae Am; Lee, Ja Young; Oh, Seung Hwan; Kim, Hye Ran; Lee, Jeong Nyeo; Kho, Weon-Gyu; Shin, Jeong Hwan

2012-03-01

The aims of this study were to compare several DNA extraction methods and 16S rDNA primers and to evaluate the clinical utility of broad-range PCR in continuous ambulatory peritoneal dialysis (CAPD) culture fluids. Six type strains were used as model organisms in dilutions from 10(8) to 10(0) colony-forming units (CFU)/mL for the evaluation of 5 DNA extraction methods and 5 PCR primer pairs. Broad-range PCR was applied to 100 CAPD culture fluids, and the results were compared with conventional culture results. There were some differences between the various DNA extraction methods and primer sets with regard to the detection limits. The InstaGene Matrix (Bio-Rad Laboratories, USA) and Exgene Clinic SV kits (GeneAll Biotechnology Co. Ltd, Korea) seem to have higher sensitivities than the others. The results of broad-range PCR were concordant with the results from culture in 97% of all cases (97/100). Two culture-positive cases that were broad-range PCR-negative were identified as Candida albicans, and 1 PCR-positive but culture-negative sample was identified as Bacillus circulans by sequencing. Two samples among 54 broad-range PCR-positive products could not be sequenced. There were differences in the analytical sensitivity of various DNA extraction methods and primers for broad-range PCR. The broad-range PCR assay can be used to detect bacterial pathogens in CAPD culture fluid as a supplement to culture methods.

Extraction of magnesium from calcined dolomite ore using hydrochloric acid leaching

NASA Astrophysics Data System (ADS)

Royani, Ahmad; Sulistiyono, Eko; Prasetiyo, Agus Budi; Subagja, Rudi

2018-05-01

Magnesium is widely used in varieties industrial sector. Dolomite is one source of magnesium besides seawater. The extraction of magnesium from dolomite ores can be done by leaching process. In this work, the dolomite leaching to extract magnesium by hydrochloric acid was investigated. The leaching experiments were performed in a spherical glass batch reactor having a capacity of 1000 ml. The effects of the stirring speed, acid concentration, reaction temperature and liquid-solid ratio for each reaction time of 1; 2; and 3 h on the Mg leaching have been evaluated. 5 ml of solution sample were collected from the leached solutions, then it was filtered prior to analysis by ICP OES. The experimental results show that the magnesium extraction increases along with the increase of acid concentration, liquid-solid ratio and temperature. The optimum conditions for magnesium extraction were achieved at temperature 75 °C, extraction time 3 h, the HCl concentration of 2 M, the liquid-solid ratio 20 ml/g and stirring speed of 400 rpm. At this condition 98, 82 % of magnesium were extracted from dolomite. The conclusion obtained from this leaching process is that the magnesium can be extracted from dolomite by using hydrochloric acid solutions.

Use of different extracts of coffee pulp for the production of bioethanol.

PubMed

Menezes, Evandro Galvão Tavares; do Carmo, Juliana Ribeiro; Menezes, Aline Galvão Tavares; Alves, José Guilherme Lembi Ferreira; Pimenta, Carlos José; Queiroz, Fabiana

2013-01-01

Coffee is one of the most important agricultural products in Brazil. More than 50 % of the coffee fruit is not used for the production of commercial green coffee and is therefore discarded, usually ending up in the environment. The goal of this work was to select an efficient process for obtaining coffee pulp extract and to evaluate the use of this extract in bioethanol production. The effects of heat treatment and trituration on the yield and composition of the extract were investigated by measuring the amounts of reducing sugars, starch, pectin, and phenolic compounds. The extraction process was most efficient at room temperature using grinding followed by pressing. Five different fermentation media were tested: sugarcane juice or molasses diluted with water or with coffee pulp extract and a medium with only coffee pulp extract. Batch fermentations were carried out at 30 °C for 24 h, and samples were taken to obtain measurements of the total reducing sugars, cell count, and ethanol concentration. The addition of coffee pulp extract did not influence the fermentation or yeast viability, and it can thus be mixed with sugarcane juice or molasses for the production of bioethanol, with a yield of approximately 70 g/L.

Role of modifiers for analytical-scale supercritical fluid extraction of environmental samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Langenfeld, J.J.; Hawthorne, S.B.; Miller, D.J.

1994-03-15

Supercritical fluid extraction (SFE) using eight different CO[sub 2] + organic modifier mixtures and one ternary mixture (CO[sub 2] + methanol/toluene) at two different concentrations (1 and 10% v/v) was performed on two certified reference materials including polychlorinated biphenyls (PCBs) from river sediment and polycyclic aromatic hydrocarbons (PAHs) from urban air particulate matter. The modifier identity was more important than modifier concentration for increasing extraction efficiencies. Acidic/basic modifiers including methanol, acetic acid, and aniline greatly enhanced the extraction of PCBs. Low molecular weight PAHs were best extracted with modifiers including aniline, acetic acid, acetonitrile, methanol/toluene, hexane, and diethylamine. In contrast,more » modifiers capable of dipole-induced dipole interactions and [pi]-[pi] interactions such as toluene, diethylamine, and methylene chloride were the best modifiers to use for SFE of high molecular weight PAHs from air particulates. 37 refs., 6 tabs.« less

[Comparison of Chemical Components of Essential Oil from Ocimum basilicum var. pilosum Extracted by Supercritical CO2 Fluid and Steam Distillation].

PubMed

Wang, Zhao-yu; Zheng, Jia-huan; Shi, Sheng-ying; Luo, Zhi-xiong; Ni, Shun-yu; Lin, Jing-ming

2015-11-01

To compare the chemical components of essential oil prepared by steam distillation extraction (SD) and supercritical CO2 fluid extraction (SFE-CO2) from Ocimum basilicum var. pilosum whole plant. The essential oil of Ocimum basilicum var. pilosum were extracted by SD and SFE-CO2. The chemical components of essential oil were separated and analyzed by gas chromatography-mass spectrometry( GC-MS). Their relative contents were determined by normalization of peak area. 40 and 42 compounds were detected in the essential oil prepared by SD and SFE-CO2 respectively. 25 compounds were common. Thereare significant differences of the chemical components between the Ocimum basilicum var. pilosum essential oil prepared by SD and thatby SFE-CO2. Different methods showed different extraction efficiency with a special compound. It might be a good idea to unite several methods in the modern traditional Chinese medicine industry.

Geochemical modeling of fluid-fluid and fluid-mineral interactions during geological CO2 storage

NASA Astrophysics Data System (ADS)

Zhu, C.; Ji, X.; Lu, P.

2013-12-01

The long time required for effective CO2 storage makes geochemical modeling an indispensable tool for CCUS. One area of geochemical modeling research that is in urgent need is impurities in CO2 streams. Permitting impurities, such as H2S, in CO2 streams can lead to potential capital and energy savings. However, predicting the consequences of co-injection of CO2 and impurities into geological formations requires the understanding of the phase equilibrium and fluid-fluid interactions. To meet this need, we developed a statistical associating fluid theory (SAFT)-based equation of state (EOS) for the H2S-CO2-H2O-NaCl system at 373.15

Growth rate of a penny-shaped crack in hydraulic fracturing of rocks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abe, H.; Keer, L.M.; Mura, T.

1976-01-01

The deformation and growth of a crack, fractured hydraulically, is investigated when fluid is injected from an inlet into the crack at a constant flow rate. The total flow rate at the inlet is divided as follows: flow rate extracted from an outlet hole; fluid loss rate from the crack surface; and total fluid mass change in the crack. Two cases are considered: (1) inlet flow rate is initially greater than the sum of the outlet flow and fluid loss rates; and (2) the reverse holds true. Ranges are shown for which the crack attains stationary states for given inletmore » flow rate and outlet pressure. For these two cases reasonable outlet flow rates are obtained when the outlet pressure is less than or equal to the difference between the tectonic stress and the fluid head at the inlet. Results are expected to be of use in considerations of heat extraction from hot, dry rock.« less

A competitive enzyme-linked immunosorbent assay for quantification of tetrastatin in body fluids and tumor extracts.

PubMed

Dupont-Deshorgue, A; Oudart, J B; Brassart, B; Deslee, G; Perotin, J M; Diebold, M D; Monboisse, J C; Ramont, L; Brassart-Pasco, S

2015-08-01

Basement membrane collagens or derived fragments are measured in biological fluids such as blood and urine of patients and appear to be useful for diagnosis, prognostication, or treatment monitoring as proposed for endostatin, a fragment of collagen XVIII, or tumstatin, a fragment of collagen IV. Tetrastatin, the NC1 alpha 4 collagen IV domain, was previously reported to inhibit tumor growth and angiogenesis. The aim of this study was to develop and validate a method to measure tetrastatin concentrations in human fluids. We developed a competitive enzyme-linked immunosorbent assay (ELISA). It allowed measuring tetrastatin levels in human serum, bronchial aspiration and bronchoalveolar lavage fluids, and lung tissue extracts. The tetrastatin level was significantly higher in tumor tissues than in healthy lung tissues. Tetrastatin competitive ELISA could be useful to quantify tetrastatin in tissues and biological fluids for the diagnosis or prognostication of diseases in which basement membrane metabolism may be altered, especially tumor progression. Copyright © 2015 Elsevier Inc. All rights reserved.

Mechanistic study of lead desorption during the leaching process of ion-absorbed rare earths: pH effect and the column experiment.

PubMed

Tang, Jie; Xue, Qiang; Chen, Honghan; Li, Wenting

2017-05-01

High concentrations of ammonium sulfate, often used in the in situ mining process, can result in a decrease of pH in the environment and dissolution of rare earth metals. Ammonium sulfate can also cause desorption of toxic heavy metals, leading to environmental and human health implications. In this study, the desorption behavior and fraction changes of lead in the ion-absorbed rare earth ore were studied using batch desorption experiments and column leaching tests. Results from batch desorption experiments showed that the desorption process of lead included fast and slow stages and followed an Elovich model well. The desorption rate and the proportion of lead content in the solution to the total lead in the soil were observed to increase with a decrease in the initial pH of the ammonium sulfate solution. The lead in soil included an acid-extractable fraction, reducible fraction, oxidizable fraction, and a residual fraction, with the predominant fractions being the reducible and acid-extractable fractions. Ninety-six percent of the extractable fraction in soil was desorbed into solution at pH = 3.0, and the content of the reducible fraction was observed to initially increase (when pH >4.0) and then decrease (when pH <4.0) with a decrease in pH. Column leaching tests indicated that the content of lead in the different fractions of soil followed the trend of reducible fraction > oxidizable fraction > acid-extractable fraction > residual fraction after the simulating leaching mining process. The change in pH was also found to have a larger influence on the acid-extractable and reducible fractions than the other two fractions. The proportion of the extractable fraction being leached was ca. 86%, and the reducible fraction was enriched along the migration direction of the leaching liquid. These results suggest that certain lead fractions may desorb again and contaminate the environment via acid rain, which provides significant information for environmental assessment and remediation after mining process. Graphical abstract ᅟ.

Soil properties affecting wheat yields following drilling-fluid application.

PubMed

Bauder, T A; Barbarick, K A; Ippolito, J A; Shanahan, J F; Ayers, P D

2005-01-01

Oil and gas drilling operations use drilling fluids (mud) to lubricate the drill bit and stem, transport formation cuttings to the surface, and seal off porous geologic formations. Following completion of the well, waste drilling fluid is often applied to cropland. We studied potential changes in soil compaction as indicated by cone penetration resistance, pH, electrical conductivity (EC(e)), sodium adsorption ratio (SAR), extractable soil and total straw and grain trace metal and nutrient concentrations, and winter wheat (Triticum aestivum L. 'TAM 107') grain yield following water-based, bentonitic drilling-fluid application (0-94 Mg ha(-1)) to field test plots. Three methods of application (normal, splash-plate, and spreader-bar) were used to study compaction effects. We measured increasing SAR, EC(e), and pH with drilling-fluid rates, but not to levels detrimental to crop production. Field measurements revealed significantly higher compaction within areas affected by truck travel, but also not enough to affect crop yield. In three of four site years, neither drilling-fluid rate nor application method affected grain yield. Extractions representing plant availability and plant analyses results indicated that drilling fluid did not significantly increase most trace elements or nutrient concentrations. These results support land application of water-based bentonitic drilling fluids as an acceptable practice on well-drained soils using controlled rates.

Droplet-Based Segregation and Extraction of Concentrated Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buie, C R; Buckley, P; Hamilton, J

2007-02-23

Microfluidic analysis often requires sample concentration and separation techniques to isolate and detect analytes of interest. Complex or scarce samples may also require an orthogonal separation and detection method or off-chip analysis to confirm results. To perform these additional steps, the concentrated sample plug must be extracted from the primary microfluidic channel with minimal sample loss and dilution. We investigated two extraction techniques; injection of immiscible fluid droplets into the sample stream (''capping'''') and injection of the sample into an immiscible fluid stream (''extraction''). From our results we conclude that capping is the more effective partitioning technique. Furthermore, this functionalitymore » enables additional off-chip post-processing procedures such as DNA/RNA microarray analysis, realtime polymerase chain reaction (RT-PCR), and culture growth to validate chip performance.« less

Extractive fermentation for enhanced propionic acid production from lactose by Propionibacterium acidipropionici

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jin, Z.; Yang, S.T.

1998-05-01

An extractive fermentation process using an amine extractant and a hollow-fiber membrane extractor to selectively remove propionic acid from the fermentation broth was developed to produce propionate from lactose. Compared to the conventional batch fermentation, the extractive fermentation had a much higher productivity ({approximately}1 g/(L{center_dot}h) or 5-fold increase), higher propionate yield (up to 0.66 g/g or more than 20% increase), higher final product concentration (75 g/L or higher), and higher product purity ({approximately}90%). Meanwhile, acetate and succinate productions in the extractive fermentation were significantly reduced. The improved fermentation performance can be attributed to the reduced product inhibition and a possiblemore » metabolic pathway shift to favor more propionic but less acetic and succinic acid production. The process was stable and gave consistent long-term performance over the 1.5-month period studied. The effects of propionate concentration, pH, and amine content in the solvent on the extractive fermentation were also studied and are discussed in this paper.« less

Dynamic leaching and fractionation of trace elements from environmental solids exploiting a novel circulating-flow platform.

PubMed

Mori, Masanobu; Nakano, Koji; Sasaki, Masaya; Shinozaki, Haruka; Suzuki, Shiho; Okawara, Chitose; Miró, Manuel; Itabashi, Hideyuki

2016-02-01

A dynamic flow-through microcolumn extraction system based on extractant re-circulation is herein proposed as a novel analytical approach for simplification of bioaccessibility tests of trace elements in sediments. On-line metal leaching is undertaken in the format of all injection (AI) analysis, which is a sequel of flow injection analysis, but involving extraction under steady-state conditions. The minimum circulation times and flow rates required to determine the maximum bioaccessible pools of target metals (viz., Cu, Zn, Cd, and Pb) from lake and river sediment samples were estimated using Tessier's sequential extraction scheme and an acid single extraction test. The on-line AIA method was successfully validated by mass balance studies of CRM and real sediment samples. Tessier's test in on-line AI format demonstrated to be carried out by one third of extraction time (6h against more than 17 h by the conventional method), with better analytical precision (<9.2% against >15% by the conventional method) and significant decrease in blank readouts as compared with the manual batch counterpart. Copyright © 2015 Elsevier B.V. All rights reserved.

Research activities on supercritical fluid science in food biotechnology.

PubMed

Khosravi-Darani, Kianoush

2010-06-01

This article serves as an overview, introducing the currently popular area of supercritical fluids and their uses in food biotechnology. Within each application, and wherever possible, the basic principles of the technique, as well as a description of the history, instrumentation, methodology, uses, problems encountered, and advantages over the traditional, non-supercritical methods are given. Most current commercial application of the supercritical extraction involve biologically-produced materials; the technique may be particularly relevant to the extraction of biological compounds in cases where there is a requirement for low-temperature processing, high mass-transfer rates, and negligible carrying over of the solvent into the final product. Special applications to food processing include the decaffeination of green coffee beans, the production of hops extracts, the recovery of aromas and flavors from herbs and spices, the extraction and fractionation of edible oils, and the removal of contaminants, among others. New advances, in which the extraction is combined with reaction or crystallization steps, may further increase the attractiveness of supercritical fluids in the bioprocess industries. To develop and establish a novel and effective alternative to heating treatment, the lethal action of high hydrostatic pressure CO(2) on microorganisms, with none or only a minimal heating process, has recently received a great deal of attention.

An interactive multi-block grid generation system

NASA Technical Reports Server (NTRS)

Kao, T. J.; Su, T. Y.; Appleby, Ruth

1992-01-01

A grid generation procedure combining interactive and batch grid generation programs was put together to generate multi-block grids for complex aircraft configurations. The interactive section provides the tools for 3D geometry manipulation, surface grid extraction, boundary domain construction for 3D volume grid generation, and block-block relationships and boundary conditions for flow solvers. The procedure improves the flexibility and quality of grid generation to meet the design/analysis requirements.

Automatic segmentation method of pelvic floor levator hiatus in ultrasound using a self-normalizing neural network

PubMed Central

Dietz, Hans Peter; D’hooge, Jan; Barratt, Dean; Deprest, Jan

2018-01-01

Abstract. Segmentation of the levator hiatus in ultrasound allows the extraction of biometrics, which are of importance for pelvic floor disorder assessment. We present a fully automatic method using a convolutional neural network (CNN) to outline the levator hiatus in a two-dimensional image extracted from a three-dimensional ultrasound volume. In particular, our method uses a recently developed scaled exponential linear unit (SELU) as a nonlinear self-normalizing activation function, which for the first time has been applied in medical imaging with CNN. SELU has important advantages such as being parameter-free and mini-batch independent, which may help to overcome memory constraints during training. A dataset with 91 images from 35 patients during Valsalva, contraction, and rest, all labeled by three operators, is used for training and evaluation in a leave-one-patient-out cross validation. Results show a median Dice similarity coefficient of 0.90 with an interquartile range of 0.08, with equivalent performance to the three operators (with a Williams’ index of 1.03), and outperforming a U-Net architecture without the need for batch normalization. We conclude that the proposed fully automatic method achieved equivalent accuracy in segmenting the pelvic floor levator hiatus compared to a previous semiautomatic approach. PMID:29340289

Automatic segmentation method of pelvic floor levator hiatus in ultrasound using a self-normalizing neural network.

PubMed

Bonmati, Ester; Hu, Yipeng; Sindhwani, Nikhil; Dietz, Hans Peter; D'hooge, Jan; Barratt, Dean; Deprest, Jan; Vercauteren, Tom

2018-04-01

Segmentation of the levator hiatus in ultrasound allows the extraction of biometrics, which are of importance for pelvic floor disorder assessment. We present a fully automatic method using a convolutional neural network (CNN) to outline the levator hiatus in a two-dimensional image extracted from a three-dimensional ultrasound volume. In particular, our method uses a recently developed scaled exponential linear unit (SELU) as a nonlinear self-normalizing activation function, which for the first time has been applied in medical imaging with CNN. SELU has important advantages such as being parameter-free and mini-batch independent, which may help to overcome memory constraints during training. A dataset with 91 images from 35 patients during Valsalva, contraction, and rest, all labeled by three operators, is used for training and evaluation in a leave-one-patient-out cross validation. Results show a median Dice similarity coefficient of 0.90 with an interquartile range of 0.08, with equivalent performance to the three operators (with a Williams' index of 1.03), and outperforming a U-Net architecture without the need for batch normalization. We conclude that the proposed fully automatic method achieved equivalent accuracy in segmenting the pelvic floor levator hiatus compared to a previous semiautomatic approach.

Nitrogen Sources Screening for Ethanol Production Using Carob Industrial Wastes.

PubMed

Raposo, S; Constantino, A; Rodrigues, F; Rodrigues, B; Lima-Costa, M E

2017-02-01

Nowadays, bioethanol production is one of the most important technologies by the necessity to identify alternative energy resources, principally when based on inexpensive renewable resources. However, the costs of 2nd-generation bioethanol production using current biotechnologies are still high compared to fossil fuels. The feasibility of bioethanol production, by obtaining high yields and concentrations of ethanol, using low-cost medium, is the primary goal, leading the research done today. Batch Saccharomyces cerevisiae fermentation of high-density sugar from carob residues with different organic (yeast extract, peptone, urea) and inorganic nitrogen sources (ammonium sulfate, ammonium nitrate) was performed for evaluating a cost-effective ethanol production, with high ethanol yield and productivity. In STR batch fermentation, urea has proved to be a very promising nitrogen source in large-scale production of bioethanol, reaching an ethanol yield of 44 % (w/w), close to theoretical maximum yield value and an ethanol production of 115 g/l. Urea at 3 g/l as nitrogen source could be an economical alternative with a great advantage in the sustainability of ethanol production from carbohydrates extracted from carob. Simulation studies, with experimental data using SuperPro Design software, have shown that the bioethanol production biorefinery from carob wastes could be a very promising way to the valorization of an endogenous resource, with a competitive cost.

HPLC-ESI-MS/MS validated method for simultaneous quantification of zopiclone and its metabolites, N-desmethyl zopiclone and zopiclone-N-oxide in human plasma.

PubMed

Mistri, Hiren N; Jangid, Arvind G; Pudage, Ashutosh; Shrivastav, Pranav

2008-03-15

A simple, selective and sensitive isocratic HPLC method with triple quadrupole mass spectrometry detection has been developed and validated for simultaneous quantification of zopiclone and its metabolites in human plasma. The analytes were extracted using solid phase extraction, separated on Symmetry shield RP8 column (150 mm x 4.6 mm i.d., 3.5 microm particle size) and detected by tandem mass spectrometry with a turbo ion spray interface. Metaxalone was used as an internal standard. The method had a chromatographic run time of 4.5 min and linear calibration curves over the concentration range of 0.5-150 ng/mL for both zopiclone and N-desmethyl zopiclone and 1-150 ng/mL for zopiclone-N-oxide. The intra-batch and inter-batch accuracy and precision evaluated at lower limit of quantification and quality control levels were within 89.5-109.1% and 3.0-14.7%, respectively, for all the analytes. The recoveries calculated for the analytes and internal standard were > or = 90% from spiked plasma samples. The validated method was successfully employed for a comparative bioavailability study after oral administration of 7.5 mg zopiclone (test and reference) to 16 healthy volunteers under fasted condition.

CHARACTERIZATION AND EVALUATION OF CAUSTIC WASH TANK AND SOLVENT HOLD TANK SAMPLES FROM MCU FROM AUGUST TO SEPTEMBER 2011

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Fink, S.

2012-08-01

During processing of Salt Batches 3 and 4 in the Modular Caustic-Side Solvent Extraction Unit (MCU), the decontamination efficiency for cesium declined from historical values and from expectations based on laboratory testing. This report documents efforts to analyze samples of solvent and process solutions from MCU in an attempt to understand the cause of the reduced performance and to recommend mitigations. CWT Solutions from MCU from the time period of variable decontamination factor (DF) performance which covers from April 2011 to September 2011 (during processing of Salt Batch 4) were examined for impurities using chromatography and spectroscopy. The results indicatemore » that impurities were found to be of two types: aromatic containing impurities most likely from Modifier degradation and aliphatic type impurities most likely from Isopar{reg_sign} L and tri-n-octylamine (TOA) degradation. Caustic washing the Solvent Hold Tank (SHT) solution with 1M NaOH improved its extraction ability as determined from {sup 22}Na uptake tests. Evidence from this work showed that pH variance in the aqueous solutions within the range of 1M nitric acid to 1.91M NaOH that contacted the solvent samples does not influence the analytical determination of the TOA concentration by GC-MS.« less

Supercritical CO₂ extraction of volatile oils from Sardinian Foeniculum vulgare ssp. vulgare (Apiaceae): chemical composition and biological activity.

PubMed

Piras, Alessandra; Falconieri, Danilo; Porcedda, Silvia; Marongiu, Bruno; Gonçalves, Maria José; Cavaleiro, Carlos; Salgueiro, Ligia

2014-01-01

This article reports the results on the composition and antifungal effect of volatile extracts obtained from the aerial parts of Sardinian wild fennel (Foeniculum vulgare Mill.), by supercritical fluid extraction (SFE) and by hydrodistillation (HD). The extracts were analysed by gas chromatography-mass spectrometry for qualitative composition and gas chromatography-flame ionisation detector to establish the percentage of constituents. The main components were fenchone (7.1% vs. 8.8%), estragole (34.9% vs. 42.6%) and (E)-anethole (24.6% vs. 43.4%) in the SFE and HD extract, respectively. Minimum inhibitory concentrations (MICs) were measured according to the reference Clinical and Laboratory Standards Institute (CLSI) broth macrodilution protocols. Minimum lethal concentrations were determined by subsequent subculturing of the same cell suspensions in solid medium. The essential oil was more active against Candida albicans, whereas the supercritical fluid extract possesses higher activity against Candida guillermondii and Cryptococcus neoformans, with MIC values of 0.32 μL/mL.

Supercritical fluid extraction of grape seeds: extract chemical composition, antioxidant activity and inhibition of nitrite production in LPS-stimulated Raw 264.7 cells.

PubMed

Pérez, Concepción; Ruiz del Castillo, María Luisa; Gil, Carmen; Blanch, Gracia Patricia; Flores, Gema

2015-08-01

Grape by-products are a rich source of bioactive compounds having broad medicinal properties, but are usually wasted from juice/wine processing industries. The present study investigates the use of supercritical fluid extraction (SFE) for obtaining an extract rich in bioactive compounds. First, some variables involved in the extraction were applied. SFE conditions were selected based on the oil mass yield, fatty acid profile and total phenolic composition. As a result, 40 °C and 300 bar were selected as operational conditions. The phenolic composition of the grape seed oil was determined using LC-DAD. The antioxidant activity was determined by ABTS and DPPH assays. For the anti-inflammatory activity the inhibition of nitrite production was assessed. The grape seed oil extracted was rich in phenolic compounds and fatty acids with significant antioxidant and anti-inflammatory activities. From these results, added economic value to this agroindustrial residue is proposed using environmentally friendly techniques.

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth.

PubMed

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-09-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%).

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth#

PubMed Central

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-01-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%). PMID:27604860

Supercritical fluid extraction of plant flavors and fragrances.

PubMed

Capuzzo, Andrea; Maffei, Massimo E; Occhipinti, Andrea

2013-06-19

Supercritical fluid extraction (SFE) of plant material with solvents like CO₂, propane, butane, or ethylene is a topic of growing interest. SFE allows the processing of plant material at low temperatures, hence limiting thermal degradation, and avoids the use of toxic solvents. Although today SFE is mainly used for decaffeination of coffee and tea as well as production of hop extracts on a large scale, there is also a growing interest in this extraction method for other industrial applications operating at different scales. In this review we update the literature data on SFE technology, with particular reference to flavors and fragrance, by comparing traditional extraction techniques of some industrial medicinal and aromatic crops with SFE. Moreover, we describe the biological activity of SFE extracts by describing their insecticidal, acaricidal, antimycotic, antimicrobial, cytotoxic and antioxidant properties. Finally, we discuss the process modelling, mass-transfer mechanisms, kinetics parameters and thermodynamic by giving an overview of SFE potential in the flavors and fragrances arena.

Effect on Non-Newtonian Rheology on Mixing in Taylor-Couette Flow

NASA Astrophysics Data System (ADS)

Cagney, Neil; Balabani, Stavroula

2017-11-01

Mixing processes within many industry applications are strongly affected by the rheology of the working fluid. This is particularly relevant for pharmaceutical, food and waste treatment industries, where the working fluids are often strongly non-Newtonian, and significant variations in rheology between batches may occur. We approach the question of how rheology affects mixing by focussing on a the classical case of Taylor-Couette flow, which exhibits a number of instabilities and flow regimes as a function of Reynolds number. We examine Taylor-Couette flow generated for a range of aqueous solutions of xantham gum or corn starch, such that the rheology varies from shear-thinning to shear-thickening. For each case, we measure the power consumption using a torque meter and the flow field using high speed, time-resolved Particle-Image Velocimetry. The mixing characteristics are quantified using a number of Lagrangian and Eulerian approaches, including the coarse grained density method and vortex strength. By comparing these metrics to the power number, we discuss how the mixing efficiency (ratio of mixing effectiveness to power input) varies with the flow index of the fluid.

Effects of supercritical fluid extraction pressure on chemical composition, microbial population, polar lipid profile, and microstructure of goat cheese.

PubMed

Sánchez-Macías, D; Laubscher, A; Castro, N; Argüello, A; Jiménez-Flores, R

2013-03-01

The consumer trend for healthier food choices and preferences for low-fat products has increased the interest in low-fat cheese and nutraceutical dairy products. However, consumer preference is still for delicious food. Low- and reduced-fat cheeses are not completely accepted because of their unappealing properties compared with full-fat cheeses. The method reported here provides another option to the conventional cheese-making process to obtain lower fat cheese. Using CO(2) as a supercritical fluid offers an alternative to reduce fat in cheese after ripening, while maintaining the initial characteristics and flavor. The aim of this experiment was to evaluate the effect of pressure (10, 20, 30, and 40 × 10(6) Pa) of supercritical CO(2) on the amount of fat extracted, microbial population, polar lipid profile, and microstructure of 2 varieties of goat cheese: Majorero, a protected denomination of origin cheese from Spain, and goat Gouda-type cheese. The amount of fat was reduced 50 to 57% and 48 to 55% for Majorero and goat Gouda-type cheeses, respectively. Higher contents (on a fat basis) of sphingomyelin and phosphatidylcholine were found in Majorero cheese compared with control and goat Gouda-type cheeses. The microbial population was reduced after supercritical fluid extraction in both cheeses, and the lethality was higher as pressure increased in Majorero cheese, most noticeably on lactococcus and lactobacillus bacteria. The Gouda-type cheese did not contain any lactobacilli. Micrographs obtained from confocal laser scanning microscopy showed a more open matrix and whey pockets in the Majorero control cheese. This could explain the ease of extracting fat and reducing the microbial counts in this cheese after treatment with supercritical CO(2). Supercritical fluid extraction with CO(2) has great potential in the dairy industry and in commercial applications. The Majorero cheese obtained after the supercritical fluid extraction treatment was an excellent candidate as a low-fat goat cheese, lower in triglycerides and cholesterol but still with all the health benefits inherent in goat milk. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

The Influence of Lactic Acid Concentration on the Separation of Light Rare Earth Elements by Continuous Liquid-Liquid Extraction with 2-Ethylhexyl Phosphonic Acid Mono-2-ethylhexyl Ester

NASA Astrophysics Data System (ADS)

de Carvalho Gomes, Rafael; Seruff, Luciana Amaral; Scal, Maira Labanca Waineraich; Vera, Ysrael Marrero

2018-02-01

The separation of rare earth elements (REEs) using solvent extraction adding complexing agents appears to be an alternative to saponification of the extractant. We evaluated the effect of lactic acid concentration on didymium (praseodymium and neodymium) and lanthanum extraction with 2-ethylhexyl phosphonic acid mono-2-ethyl hexyl ester [HEH(EHP)] as extractant. First, we investigated in batch experiments the separation of lanthanum (La) and didymium (Pr and Nd) using McCabe-Thiele diagrams to estimate the number of extraction stages when the feed solution was or was not conditioned with lactic acid. Additionally, we conducted continuous liquid-liquid extraction experiments and evaluated the influence of lactic acid concentration on the REE extraction and separation. The tests showed that the extraction percentage of REEs and the separation factor Pr/La increased when the lactic acid concentration increased, but the didymium purity decreased. Lanthanum, praseodymium, and neodymium extraction rate were 23.0, 89.7, and 99.2 pct, respectively, with 1:1 aqueous/organic volume flow rate and feed solution doped with 0.52 mol L-1 lactic acid. The highest didymium purity reached was 92.0 pct with 0.26 mol L-1 lactic acid concentration.

Selected physical and chemical properties of Feverfew (Tanacetum parthenium) extracts important for formulated product quality and performance.

PubMed

Jin, Ping; Madieh, Shadi; Augsburger, Larry L

2008-01-01

The objectives of this research are: (1) to assess selected formulation-relevant physical properties of several commercial Feverfew extracts, including flowability, hygroscopicity, compressibility and compactibility (2) to develop and validate a suitable extraction method and HPLC assay, and (3) to determine the parthenolide content of several commercial Feverfew extracts. Carr's index, minimum orifice diameter and particle-particle interaction were used to evaluate powder flowability. Hygroscopicity was evaluated by determining the equilibrium moisture content (EMC) after storage at various % relative humidities. Heckle analysis and compression pressure-radial tensile strength relationship were used to represent compression and compaction properties of feverfew extracts. An adapted analytical method was developed based on literature methods and then validated for the determination of parthenolide in feverfew. The commercial extracts tested exhibited poor to very poor flowability. The comparatively low mean yield pressure suggested that feverfew extracts deformed mainly plastically. Hygroscopicity and compactibility varied greatly with source. No commercial feverfew extracts tested contained the label claimed parthenolide. Even different batches from the same manufacturer showed significantly different parthenolide content. Therefore, extract manufactures should commit to proper quality control procedures that ensure accurate label claims, and supplement manufacturers should take into account possible differences in physico-chemical properties when using extracts from multiple suppliers.

The temporal evolution of magnesium isotope fractionation during hydromagnesite dissolution, precipitation, and at equilibrium

NASA Astrophysics Data System (ADS)

Oelkers, Eric H.; Berninger, Ulf-Niklas; Pérez-Fernàndez, Andrea; Chmeleff, Jérôme; Mavromatis, Vasileios

2018-04-01

This study provides experimental evidence of the resetting of the magnesium (Mg) isotope signatures of hydromagnesite in the presence of an aqueous fluid during its congruent dissolution, precipitation, and at equilibrium at ambient temperatures over month-long timescales. All experiments were performed in batch reactors in aqueous sodium carbonate buffer solutions having a pH from 7.8 to 9.2. The fluid phase in all experiments attained bulk chemical equilibrium within analytical uncertainty with hydromagnesite within several days, but the experiments were allowed to continue for up to 575 days. During congruent hydromagnesite dissolution, the fluid first became enriched in isotopically light Mg compared to the dissolving hydromagnesite, but this Mg isotope composition became heavier after the fluid attained chemical equilibrium with the mineral. The δ26Mg composition of the fluid was up to ∼0.35‰ heavier than the initial dissolving hydromagnesite at the end of the dissolution experiments. Hydromagnesite precipitation was provoked during one experiment by increasing the reaction temperature from 4 to 50 °C. The δ26Mg composition of the fluid increased as hydromagnesite precipitated and continued to increase after the fluid attained bulk equilibrium with this phase. These observations are consistent with the hypothesis that mineral-fluid equilibrium is dynamic (i.e. dissolution and precipitation occur at equal, non-zero rates at equilibrium). Moreover the results presented in this study confirm (1) that the transfer of material from the solid to the fluid phase may not be conservative during stoichiometric dissolution, and (2) that the isotopic compositions of carbonate minerals can evolve even when the mineral is in bulk chemical equilibrium with its coexisting fluid. This latter observation suggests that the preservation of isotopic signatures of carbonate minerals in the geological record may require a combination of the isolation of fluid-mineral system from external chemical input and/or the existence of a yet to be defined dissolution/precipitation inhibition mechanism.

Characterization of Linum usitatissimum L. oil obtained from different extraction technique and in vitro antioxidant potential of supercritical fluid extract

PubMed Central

Chauhan, Rishika; Chester, Karishma; Khan, Yasmeen; Tamboli, Ennus Tajuddin; Ahmad, Sayeed

2015-01-01

Aim: Present investigation was aimed to characterize the fixed oil of Linum usitatissimum L. using five different extraction methods: Supercritical fluid extraction (SFE), ultrasound-assistance, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO2) were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high performance thin layer chromatography (HPTLC), gas chromatography-mass spectrometry (GC-MS), and Fourier-transformed infrared spectroscopy (FT-IR) fingerprinting. Antioxidant activity was also determined using 1,1-diphenyl-2-picrylhydrazyl and superoxide scavenging method. Result: The main fatty acids were α-linolenic acid, linoleic acid, palmitic acid, and stearic acid as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks, as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods, were superimposable. Conclusion: Analysis reported that the fixed oil of L. usitatissimum L. is a good source of n-3 fatty acid with the significant antioxidant activity of oil obtained from SFE extraction method. PMID:26681884

Survey of 800+ data sets from human tissue and body fluid reveals xenomiRs are likely artifacts.

PubMed

Kang, Wenjing; Bang-Berthelsen, Claus Heiner; Holm, Anja; Houben, Anna J S; Müller, Anne Holt; Thymann, Thomas; Pociot, Flemming; Estivill, Xavier; Friedländer, Marc R

2017-04-01

miRNAs are small 22-nucleotide RNAs that can post-transcriptionally regulate gene expression. It has been proposed that dietary plant miRNAs can enter the human bloodstream and regulate host transcripts; however, these findings have been widely disputed. We here conduct the first comprehensive meta-study in the field, surveying the presence and abundances of cross-species miRNAs (xenomiRs) in 824 sequencing data sets from various human tissues and body fluids. We find that xenomiRs are commonly present in tissues (17%) and body fluids (69%); however, the abundances are low, comprising 0.001% of host human miRNA counts. Further, we do not detect a significant enrichment of xenomiRs in sequencing data originating from tissues and body fluids that are exposed to dietary intake (such as liver). Likewise, there is no significant depletion of xenomiRs in tissues and body fluids that are relatively separated from the main bloodstream (such as brain and cerebro-spinal fluids). Interestingly, the majority (81%) of body fluid xenomiRs stem from rodents, which are a rare human dietary contribution but common laboratory animals. Body fluid samples from the same studies tend to group together when clustered by xenomiR compositions, suggesting technical batch effects. Last, we performed carefully designed and controlled animal feeding studies, in which we detected no transfer of plant miRNAs into rat blood, or bovine milk sequences into piglet blood. In summary, our comprehensive computational and experimental results indicate that xenomiRs originate from technical artifacts rather than dietary intake. © 2017 Kang et al.; Published by Cold Spring Harbor Laboratory Press for the RNA Society.

Barium isotope fractionation during witherite (BaCO3) dissolution, precipitation and at equilibrium

NASA Astrophysics Data System (ADS)

Mavromatis, Vasileios; van Zuilen, Kirsten; Purgstaller, Bettina; Baldermann, Andre; Nägler, Thomas F.; Dietzel, Martin

2016-10-01

This study examines the behavior of Ba isotope fractionation between witherite and fluid during mineral dissolution, precipitation and at chemical equilibrium. Experiments were performed in batch reactors at 25 °C in 10-2 M NaCl solution where the pH was adjusted by continuous bubbling of a water saturated gas phase of CO2 or atmospheric air. During witherite dissolution no Ba isotope fractionation was observed between solid and fluid. In contrast, during witherite precipitation, caused by a pH increase, a preferential uptake of the lighter 134Ba isotopomer in the solid phase was observed. In this case, the isotope fractionation factor αwitherite-fluid is calculated to be 0.99993 ± 0.00004 (or Δ137/134Bawitherite-fluid ≈ -0.07 ± 0.04‰, 2 sd). The most interesting feature of this study, however, is that after the attainment of chemical equilibrium, the Ba isotope composition of the aqueous phase is progressively becoming lighter, indicating a continuous exchange of Ba2+ ions between witherite and fluid. Mass balance calculations indicate that the detachment of Ba from the solid is not only restricted to the outer surface layer of the solid, but affects several (∼7 unit cells) subsurface layers of the crystal. This observation comes in excellent agreement with the concept of a dynamic system at chemical equilibrium in a mineral-fluid system, denoting that the time required for the achievement of isotopic equilibrium in the witherite-fluid system is longer compared to that observed for chemical equilibrium. Overall, these results indicate that the isotopic composition of Ba bearing carbonates in natural environments may be altered due to changes in fluid composition without a net dissolution/precipitation to be observed.

Metal release from sandstones under experimentally and numerically simulated CO2 leakage conditions.

PubMed

Kirsch, Katie; Navarre-Sitchler, Alexis K; Wunsch, Assaf; McCray, John E

2014-01-01

Leakage of CO2 from a deep storage formation into an overlying potable aquifer may adversely impact water quality and human health. Understanding CO2-water-rock interactions is therefore an important step toward the safe implementation of geologic carbon sequestration. This study targeted the geochemical response of siliclastic rock, specifically three sandstones of the Mesaverde Group in northwestern Colorado. To test the hypothesis that carbonate minerals, even when present in very low levels, would be the primary source of metals released into a CO2-impacted aquifer, two batch experiments were conducted. Samples were reacted for 27 days with water and CO2 at partial pressures of 0.01 and 1 bar, representing natural background levels and levels expected in an aquifer impacted by a small leakage, respectively. Concentrations of major (e.g., Ca, Mg) and trace (e.g., As, Ba, Cd, Fe, Mn, Pb, Sr, U) elements increased rapidly after CO2 was introduced into the system, but did not exceed primary Maximum Contaminant Levels set by the U.S. Environmental Protection Agency. Results of sequential extraction suggest that carbonate minerals, although volumetrically insignificant in the sandstone samples, are the dominant source of mobile metals. This interpretation is supported by a simple geochemical model, which could simulate observed changes in fluid composition through CO2-induced calcite and dolomite dissolution.

Rheoscopic Fluids in a Post-Kalliroscope World

NASA Astrophysics Data System (ADS)

Borrero-Echeverry, Daniel; Crowley, Christopher J.

2016-11-01

In rheoscopic flow visualization the working fluid is seeded with small plate-shaped particles, which preferentially align in the flow due to their anisotropy. This leads to preferential light scattering, which highlights qualitatively different regions of the flow. For the past four decades, the gold standard in rheoscopic flow visualization has been Kalliroscope, a commercial product consisting of crystalline guanine particles. Guanine is a shiny compound extracted from fish scales and has traditionally been used in cosmetics to provide a pearlescent effect. It stands out among other options for rheoscopic flow visualization (e.g., aluminum flakes or coated mica particles) due to its relatively good density match with water. Guanine extraction, however, is an expensive process and as the cosmetics industry has adopted less expensive alternatives, commercial guanine production has dropped, leading to the closure of the Kalliroscope Corporation in 2014. In this talk, we discuss our recent discovery of a rheoscopic fluid based on stearic acid crystals, which has an overall performance similar to, and in some cases superior to, Kalliroscope. This rheoscopic fluid can be extracted from household items making it very inexpensive and readily accessible to researchers around the world.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Goven, A.J.; Chen, S.C.; Fitzpatrick, L.C.

Lysozyme activity in earthworm (Lumbricus terrestris) coelomic fluid and coelomocytes appears sufficiently sensitive for use as a nonmammalian biomarker to detect toxic effects of sublethal body burdens of Cu[sup 2+]. Lysozyme, a phylogenetically conserved enzyme, is capable of bactericidal activity via action on peptidoglycan of gram-positive bacterial cell walls and functions as a component of an organism's innate antimicrobial defense mechanism. Coelomic fluid and coelomocyte lysozyme activities, which exhibit temperature-response patterns similar to those of human saliva, plasma, serum and leukocyte extracts, were sensitive to Cu[sup 2+] exposure. Lysozyme activity of coelomic fluid and coelomocyte extracts from earthworms exposed formore » 5 d to CuSO[sub 4], using filter paper contact exposure, decreased with increasing sublethal Cu[sup 2+] concentrations of 0.05 and 0.1 [mu]g/cm[sup 2]. Compared to controls, coelomic fluid lysozyme activity was suppressed significantly at both exposure concentrations, whereas coelomocyte extract lysozyme activity was suppressed significantly at the 0.1-[mu]g/cm[sup 2] exposure concentration. Low inherent natural variability and sensitivity to sublethal Cu[sup 2+] body burdens indicate that lysozyme activity has potential as a biomarker for assaying immunotoxicity of metals.« less

Supercritical fluid technology: concepts and pharmaceutical applications.

PubMed

Deshpande, Praful Balavant; Kumar, G Aravind; Kumar, Averineni Ranjith; Shavi, Gopal Venkatesh; Karthik, Arumugam; Reddy, Meka Sreenivasa; Udupa, Nayanabhirama

2011-01-01

In light of environmental apprehension, supercritical fluid technology (SFT) exhibits excellent opportunities to accomplish key objectives in the drug delivery sector. Supercritical fluid extraction using carbon dioxide (CO(2)) has been recognized as a green technology. It is a clean and versatile solvent with gas-like diffusivity and liquid-like density in the supercritical phase, which has provided an excellent alternative to the use of chemical solvents. The present commentary provides an overview of different techniques using supercritical fluids and their future opportunity for the drug delivery industry. Some of the emerging applications of SFT in pharmaceuticals, such as particle design, drug solubilization, inclusion complex, polymer impregnation, polymorphism, drug extraction process, and analysis, are also covered in this review. The data collection methods are based on the recent literature related to drug delivery systems using SFT platforms. SFT has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This cutting-edge technology is growing predominantly to surrogate conventional unit operations in relevance to the pharmaceutical production process. Supercritical fluid technology has recently drawn attention in the field of pharmaceuticals. It is a distinct conception that utilizes the solvent properties of supercritical fluids above their critical temperature and pressure, where they exhibit both liquid-like and gas-like properties, which can enable many pharmaceutical applications. For example, the liquid-like properties provide benefits in extraction processes of organic solvents or impurities, drug solubilization, and polymer plasticization, and the gas-like features facilitate mass transfer processes. It has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This review is focused on different techniques that use supercritical fluids and their opportunities for the pharmaceutical sector.

Methylxanthines: properties and determination in various objects

NASA Astrophysics Data System (ADS)

Andreeva, Elena Yu; Dmitrienko, Stanislava G.; Zolotov, Yurii A.

2012-05-01

Published data on the properties and determination of caffeine, theophylline, theobromine and some other methylxanthines in various objects are surveyed and described systematically. Different sample preparation procedures such as liquid extraction from solid matrices and liquid-liquid, supercritical fluid and solid-phase extraction are compared. The key methods of analysis including chromatography, electrophoresis, spectrometry and electrochemical methods are discussed. Examples of methylxanthine determination in plants, food products, energy beverages, pharmaceuticals, biological fluids and natural and waste waters are given. The bibliography includes 393 references.

Segmentation of Unstructured Datasets

NASA Technical Reports Server (NTRS)

Bhat, Smitha

1996-01-01

Datasets generated by computer simulations and experiments in Computational Fluid Dynamics tend to be extremely large and complex. It is difficult to visualize these datasets using standard techniques like Volume Rendering and Ray Casting. Object Segmentation provides a technique to extract and quantify regions of interest within these massive datasets. This thesis explores basic algorithms to extract coherent amorphous regions from two-dimensional and three-dimensional scalar unstructured grids. The techniques are applied to datasets from Computational Fluid Dynamics and from Finite Element Analysis.

A new perspective of using sequential extraction: To predict the deficiency of trace elements during anaerobic digestion.

PubMed

Cai, Yafan; Wang, Jungang; Zhao, Yubin; Zhao, Xiaoling; Zheng, Zehui; Wen, Boting; Cui, Zongjun; Wang, Xiaofen

2018-09-01

Trace elements were commonly used as additives to facilitate anaerobic digestion. However, their addition is often blind because of the complexity of reaction conditions, which has impeded their widespread application. Therefore, this study was conducted to evaluate deficiencies in trace elements during anaerobic digestion by establishing relationships between changes in trace element bioavailability (the degree to which elements are available for interaction with biological systems) and digestion performance. To accomplish this, two batch experiments were conducted. In the first, sequential extraction was used to detect changes in trace element fractions and then to evaluate trace element bioavailability in the whole digestion cycle. In the second batch experiment, trace elements (Co, Fe, Cu, Zn, Mn, Mo and Se) were added to the reaction system at three concentrations (low, medium and high) and their effects were monitored. The results showed that sequential extraction was a suitable method for assessment of the bioavailability of trace elements (appropriate coefficient of variation and recovery rate). The results revealed that Se had the highest (44.2%-70.9%) bioavailability, while Fe had the lowest (1.7%-3.0%). A lack of trace elements was not directly related to their absolute bioavailability, but was instead associated with changes in their bioavailability throughout the digestion cycle. Trace elements were insufficient when their bioavailability was steady or increased over the digestion cycle. These results indicate that changes in trace element bioavailability during the digestion cycle can be used to predict their deficiency. Copyright © 2018 Elsevier Ltd. All rights reserved.

Copper removal by algae Gelidium, agar extraction algal waste and granulated algal waste: kinetics and equilibrium.

PubMed

Vilar, Vítor J P; Botelho, Cidália M S; Boaventura, Rui A R

2008-03-01

Biosorption of copper ions by an industrial algal waste, from agar extraction industry has been studied in a batch system. This biosorbent was compared with the algae Gelidium itself, which is the raw material for agar extraction, and the industrial waste immobilized with polyacrylonitrile (composite material). The effects of contact time, pH, ionic strength (IS) and temperature on the biosorption process have been studied. Equilibrium data follow both Langmuir and Langmuir-Freundlich models. The parameters of Langmuir equilibrium model were: q(max)=33.0mgg(-1), K(L)=0.015mgl(-1); q(max)=16.7mgg(-1), K(L)=0.028mgl(-1) and q(max)=10.3mgg(-1), K(L)=0.160mgl(-1) respectively for Gelidium, algal waste and composite material at pH=5.3, T=20 degrees C and IS=0.001M. Increasing the pH, the number of deprotonated active sites increases and so the uptake capacity of copper ions. In the case of high ionic strengths, the contribution of the electrostatic component to the overall binding decreases, and so the uptake capacity. The temperature has little influence on the uptake capacity principally for low equilibrium copper concentrations. Changes in standard enthalpy, Gibbs energy and entropy during biosorption were determined. Kinetic data at different solution pH (3, 4 and 5.3) were fitted to pseudo-first-order and pseudo-second-order models. The adsorptive behaviour of biosorbent particles was modelled using a batch reactor mass transfer kinetic model, which successfully predicts Cu(II) concentration profiles.

40 CFR Appendix 8 to Subpart A of... - Reference C16-C18 Internal Olefin Drilling Fluid Formulation

Code of Federal Regulations, 2014 CFR

2014-07-01

... Drilling Fluid Formulation 8 Appendix 8 to Subpart A of Part 435 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS (CONTINUED) OIL AND GAS EXTRACTION POINT...—Reference C16-C18 Internal Olefin Drilling Fluid Formulation The reference C16-C18 internal olefin drilling...

40 CFR Appendix 8 to Subpart A of... - Reference C16-C18 Internal Olefin Drilling Fluid Formulation

Code of Federal Regulations, 2012 CFR

2012-07-01

... Drilling Fluid Formulation 8 Appendix 8 to Subpart A of Part 435 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS (CONTINUED) OIL AND GAS EXTRACTION POINT...—Reference C16-C18 Internal Olefin Drilling Fluid Formulation The reference C16-C18 internal olefin drilling...

40 CFR Appendix 8 to Subpart A of... - Reference C16-C18 Internal Olefin Drilling Fluid Formulation

Code of Federal Regulations, 2013 CFR

2013-07-01

... Drilling Fluid Formulation 8 Appendix 8 to Subpart A of Part 435 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS (CONTINUED) OIL AND GAS EXTRACTION POINT...—Reference C16-C18 Internal Olefin Drilling Fluid Formulation The reference C16-C18 internal olefin drilling...

Using Neutrons to Study Fluid-Rock Interactions in Shales

NASA Astrophysics Data System (ADS)

DiStefano, V. H.; McFarlane, J.; Anovitz, L. M.; Gordon, A.; Hale, R. E.; Hunt, R. D.; Lewis, S. A., Sr.; Littrell, K. C.; Stack, A. G.; Chipera, S.; Perfect, E.; Bilheux, H.; Kolbus, L. M.; Bingham, P. R.

2015-12-01

Recovery of hydrocarbons by hydraulic fracturing depends on complex fluid-rock interactions that we are beginning to understand using neutron imaging and scattering techniques. Organic matter is often thought to comprise the majority of porosity in a shale. In this study, correlations between the type of organic matter embedded in a shale and porosity were investigated experimentally. Selected shale cores from the Eagle Ford and Marcellus formations were subjected to pyrolysis-gas chromatography, Differential Thermal Analysis/Thermogravimetric analysis, and organic solvent extraction with the resulting affluent analyzed by gas chromatography-mass spectrometry. The pore size distribution of the microporosity (~1 nm to 2 µm) in the Eagle Ford shales was measured before and after solvent extraction using small angle neutron scattering. Organics representing mass fractions of between 0.1 to 1 wt.% were removed from the shales and porosity generally increased across the examined microporosity range, particularly at larger pore sizes, approximately 50 nm to 2 μm. This range reflects extraction of accessible organic material, including remaining gas molecules, bitumen, and kerogen derivatives, indicating where the larger amount of organic matter in shale is stored. An increase in porosity at smaller pore sizes, ~1-3 nm, was also present and could be indicative of extraction of organic material stored in the inter-particle spaces of clays. Additionally, a decrease in porosity after extraction for a sample was attributed to swelling of pores with solvent uptake. This occurred in a shale with high clay content and low thermal maturity. The extracted hydrocarbons were primarily paraffinic, although some breakdown of larger aromatic compounds was observed in toluene extractions. The amount of hydrocarbon extracted and an overall increase in porosity appeared to be primarily correlated with the clay percentage in the shale. This study complements fluid transport neutron imaging studies, to explain the physics and chemistry of fluid-rock behavior. Research supported by the U.S. Department of Energy, Office of Science, Basic Energy Sciences, Chemical Sciences, Geosciences, and Biosciences Division and the Bredesen Center at the University of Tennessee.

A fully automated liquid–liquid extraction system utilizing interface detection

PubMed Central

Maslana, Eugene; Schmitt, Robert; Pan, Jeffrey

2000-01-01

The development of the Abbott Liquid-Liquid Extraction Station was a result of the need for an automated system to perform aqueous extraction on large sets of newly synthesized organic compounds used for drug discovery. The system utilizes a cylindrical laboratory robot to shuttle sample vials between two loading racks, two identical extraction stations, and a centrifuge. Extraction is performed by detecting the phase interface (by difference in refractive index) of the moving column of fluid drawn from the bottom of each vial containing a biphasic mixture. The integration of interface detection with fluid extraction maximizes sample throughput. Abbott-developed electronics process the detector signals. Sample mixing is performed by high-speed solvent injection. Centrifuging of the samples reduces interface emulsions. Operating software permits the user to program wash protocols with any one of six solvents per wash cycle with as many cycle repeats as necessary. Station capacity is eighty, 15 ml vials. This system has proven successful with a broad spectrum of both ethyl acetate and methylene chloride based chemistries. The development and characterization of this automated extraction system will be presented. PMID:18924693