Toxicity of naphthenic acids to invertebrates: Extracts from oil sands process-affected water versus commercial mixtures.

PubMed

Bartlett, Adrienne J; Frank, Richard A; Gillis, Patricia L; Parrott, Joanne L; Marentette, Julie R; Brown, Lisa R; Hooey, Tina; Vanderveen, Ruth; McInnis, Rodney; Brunswick, Pamela; Shang, Dayue; Headley, John V; Peru, Kerry M; Hewitt, L Mark

2017-08-01

The toxicity of oil sands process-affected water (OSPW) has been primarily attributed to polar organic constituents, including naphthenic acid fraction components (NAFCs). Our objective was to assess the toxicity of NAFCs derived from fresh and aged OSPW, as well as commercial naphthenic acid (NA) mixtures. Exposures were conducted with three aquatic species: Hyalella azteca (freshwater amphipod), Vibrio fischeri (marine bacterium, Microtox ® assay), and Lampsilis cardium (freshwater mussel larvae (glochidia)). Commercial NAs were more toxic than NAFCs, with differences of up to 30-, 4-, and 120-fold for H. azteca, V. fischeri, and L. cardium, respectively, demonstrating that commercial NAs are not reliable surrogates for assessing the toxicity of NAFCs. Differences in toxicity between species were striking for both commercial NAs and NAFCs. Overall, V. fischeri was the least sensitive and H. azteca was the most sensitive organism. Responses of V. fischeri and H. azteca to NAFC exposures were consistent (< 2-fold difference) regardless of source and age of OSPW; however, effects on L. cardium ranged 17-fold between NAFCs. NAFCs derived from fresh OSPW sources were similarly or less toxic to those from aged OSPW. Our results support the need to better characterize the complex mixtures associated with bitumen-influenced waters, both chemically and toxicologically. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

Diaromatic sulphur-containing 'naphthenic' acids in process waters.

PubMed

West, Charles E; Scarlett, Alan G; Tonkin, Andrew; O'Carroll-Fitzpatrick, Devon; Pureveen, Jos; Tegelaar, Erik; Gieleciak, Rafal; Hager, Darcy; Petersen, Karina; Tollefsen, Knut-Erik; Rowland, Steven J

2014-03-15

Polar organic compounds found in industrial process waters, particularly those originating from biodegraded petroleum residues, include 'naphthenic acids' (NA). Some NA have been shown to have acute toxicity to fish and also to produce sub-lethal effects. Whilst some of these toxic effects are produced by identifiable carboxylic acids, acids such as sulphur-containing acids, which have been detected, but not yet identified, may produce others. Therefore, in the present study, the sulphur-containing acids in oil sands process water were studied. A fraction (ca 12% by weight of the total NA containing ca 1.5% weight sulphur) was obtained by elution of methylated NA through an argentation solid phase extraction column with diethyl ether. This was examined by multidimensional comprehensive gas chromatography-mass spectrometry (GCxGC-MS) in both nominal and high resolution mass accuracy modes and by GCxGC-sulphur chemiluminescence detection (GCxGC-SCD). Interpretation of the mass spectra and retention behaviour of methyl esters of several synthesised sulphur acids and the unknowns allowed delimitation of the structures, but not complete identification. Diaromatic sulphur-containing alkanoic acids were suggested. Computer modelling of the toxicities of some of the possible acids suggested they would have similar toxicities to one another and to dehydroabietic acid. However, the sulphur-rich fraction was not toxic or estrogenic to trout hepatocytes, suggesting the concentrations of sulphur acids in this sample were too low to produce any such effects in vitro. Further samples should probably be examined for these compounds. Copyright © 2013 Elsevier Ltd. All rights reserved.

X-Ray Photoelectron Spectroscopy Study of the Chemisorption of Lead Naphthenate to Nucleophilic Surfaces.

DTIC Science & Technology

1980-09-10

naphthenic acid is 1-methylcyclopentane- carboxylic acid . Lead naphthenate is not one unique compound but a mixture of several naphthenates with various alkane...chain lengths and an average molecu- lar weight of 662 g/mol. It contains no free naphthenic acid . Solutions of 1% by weight lead naphthenate in...particularly on surface acidity . The influence of the pH of the pretreatment bath used for the substrate on the existence of chemi- sorbed lead naphthenate

Potential of capillary electrophoresis mass spectrometry for the characterization and monitoring of amine-derivatized naphthenic acids from oil sands process-affected water.

PubMed

MacLennan, Matthew S; Tie, Cai; Kovalchik, Kevin; Peru, Kerry M; Zhang, Xinxiang; Headley, John V; Chen, David D Y

2016-11-01

Capillary electrophoresis coupled to mass spectrometry (CE-MS) was used for the analysis of naphthenic acid fraction compounds (NAFCs) of oil sands process-affected water (OSPW). A standard mixture of amine-derivatized naphthenic acids is injected directly onto the CE column and analyzed by CE-MS in less than 15min. Time of flight MS analysis (TOFMS), optimized for high molecular weight ions, showed NAFCs between 250 and 800m/z. With a quadrupole mass analyzer, only low-molecular weight NAFCs (between 100 and 450m/z) are visible under our experimental conditions. Derivatization of NAFCs consisted of two-step amidation reactions mediated by 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC), or mediated by a mixture of EDC and N-hydroxysuccinimide, in dimethyl sulfoxide, dichloromethane or ethyl acetate. The optimum background electrolyte composition was determined to be 30% (V/V) methanol in water and 2% (V/V) formic acid. NAFCs extracted from OSPW in the Athabasca oil sands region were used to demonstrate the feasibility of CE-MS for the analysis of NAFCs in environmental samples, showing that the labeled naphthenic acids are in the mass range of 350 to 1500m/z. Copyright © 2016. Published by Elsevier B.V.

Colloidal properties of single component naphthenic acids and complex naphthenic acid mixtures.

PubMed

Mohamed, Mohamed H; Wilson, Lee D; Peru, Kerry M; Headley, John V

2013-04-01

Tensiometry was used to provide estimates of the critical micelle concentration (cmc) values for three sources of naphthenic acids (NAs) and three examples of single component NAs (S1-S3) in aqueous solution at pH 10.5 and 295 K. Two commercially available mixtures of NAs and an industrially derived mixture of NAs obtained from Alberta oil sands process water (OSPW) were investigated. The three examples of single component NAs (C(n)H(2n+z)O2) were chosen with variable z-series to represent chemical structures with 0-2 rings, as follows: 2-hexyldecanoic acid (z=0; S1), trans-4-pentylcyclohexanecarboxylic acid (z=-2; S2) and dicyclohexylacetic acid (z=-4; S3). The estimated cmc values for S1 (35.6 μM), S2 (0.545 mM), and S3 (4.71 mM) vary over a wide range according to their relative lipophile characteristics of each carboxylate anion. The cmc values for the three complex mixtures of NAs were evaluated. Two disctinct cmc values were observed (second listed in brackets) as follows: Commercial sample 1; 50.9 μM (109 μM), Commercial sample 2; 22.3 μM (52.2 μM), and Alberta derived OSPW; 154 μM (417 μM). These results provide strong support favouring two general classes of NAs in the mixtures investigated with distinct cmc values. We propose that the two groups may be linked to a recalcitrant fraction with a relatively large range of cmc values (52.2-417 μM) and a readily biodegradable fraction with a relatively low range of cmc values (22.3-154 μM) depending on the source of NAs in a given mixture. Copyright © 2013 Elsevier Inc. All rights reserved.

Toxicity of naphthenic acid fraction components extracted from fresh and aged oil sands process-affected waters, and commercial naphthenic acid mixtures, to fathead minnow (Pimephales promelas) embryos.

PubMed

Marentette, Julie R; Frank, Richard A; Bartlett, Adrienne J; Gillis, Patricia L; Hewitt, L Mark; Peru, Kerry M; Headley, John V; Brunswick, Pamela; Shang, Dayue; Parrott, Joanne L

2015-07-01

Naphthenic acids (NAs) are constituents of oil sands process-affected water (OSPW). These compounds can be both toxic and persistent and thus are a primary concern for the ultimate remediation of tailings ponds in northern Alberta's oil sands regions. Recent research has focused on the toxicity of NAs to the highly vulnerable early life-stages of fish. Here we examined fathead minnow embryonic survival, growth and deformities after exposure to extracted NA fraction components (NAFCs), from fresh and aged oil sands process-affected water (OSPW), as well as commercially available NA mixtures. Commercial NA mixtures were dominated by acyclic O2 species, while NAFCs from OSPW were dominated by bi- and tricyclic O2 species. Fathead minnow embryos less than 24h old were reared in tissue culture plates terminating at hatch. Both NAFC and commercial NA mixtures reduced hatch success, although NAFCs from OSPW were less toxic (EC50=5-12mg/L, nominal concentrations) than commercial NAs (2mg/L, nominal concentrations). The toxicities of NAFCs from aged and fresh OSPW were similar. Embryonic heart rates at 2 days post-fertilization (dpf) declined with increasing NAFC exposure, paralleling patterns of hatch success and rates of cardiovascular abnormalities (e.g., pericardial edemas) at hatch. Finfold deformities increased in exposures to commercial NA mixtures, not NAFCs. Thus, commercial NA mixtures are not appropriate surrogates for NAFC toxicity. Further work clarifying the mechanisms of action of NAFCs in OSPW, as well as comparisons with additional aged sources of OSPW, is merited. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

Photocatalytic degradation of commercially sourced naphthenic acids by TiO2-graphene composite nanomaterial.

PubMed

Liu, Juncheng; Wang, Lin; Tang, Jingchun; Ma, Jianli

2016-04-01

Naphthenic acids (NAs) are a major contributor to the toxicity in oil sands process-affected water (OSPW), which is produced by hot water extraction of bitumen. NAs are extremely difficult to be degraded due to its complex ring and side chain structure. Photocatalysis is recognized as a promising technology in the removal of refractory organic pollutants. In this work, TiO2-graphene (P25-GR) composites were synthesized by means of solvothermal method. The results showed that P25-GR composite exhibited better photocatalytic activity than pure P25. The removal efficiency of naphthenic acids in acid solution was higher than that in neutral and alkaline solutions. It was the first report ever known on the photodegradation of NAs based on graphene, and this process achieved a higher removal rate than other photocatalysis degradation of NAs in a shorter reaction time. LC/MS analysis showed that macromolecular NAs (carbon number 17-22, z value -2) were easy to be degraded than the micromolecular ones (carbon number 11-16, z value -2). Furthermore, the reactive oxygen species that play the main role in the photocatalysis system were studied. It was found that holes and ·OH were the main reactive species in the UV/P25-GR photocatalysis system. Given the high removal efficiency of refractory organic pollutants and the short degradation time, photodegradation based on composite catalysts has a broad and practical prospect. The study on the photodegradation of commercially sourced NAs may provide a guidance for the degradation of OSPW NAs by this method. Copyright © 2016 Elsevier Ltd. All rights reserved.

A traceable reference for direct comparative assessment of total naphthenic acid concentrations in commercial and acid extractable organic mixtures derived from oil sands process water.

PubMed

Brunswick, Pamela; Hewitt, L Mark; Frank, Richard A; Kim, Marcus; van Aggelen, Graham; Shang, Dayue

2017-02-23

The advantage of using naphthenic acid (NA) mixtures for the determination of total NA lies in their chemical characteristics and identification of retention times distinct from isobaric interferences. However, the differing homolog profiles and unknown chemical structures of NA mixtures do not allow them to be considered a traceable reference material. The current study provides a new tool for the comparative assessment of different NA mixtures by direct reference to a single, well-defined and traceable compound, decanoic-d 19 acid. The method employed an established liquid chromatography time-of-flight mass spectrometry (LC/QToF) procedure that was applicable both to the classic O2 NA species dominating commercial mixtures and additionally to the O4 species known to be present in acid extractable organics (AEOs) derived from oil sands process water (OSPW). Four different commercial NA mixtures and one OSPW-derived AEOs mixture were comparatively assessed. Results showed significant difference among Merichem Technical, Aldrich, Acros, and Kodak commercial NA mixtures with respect to "equivalent to decanoic-d 19 acid" concentration ratios to nominal. Furthermore, different lot numbers of single commercial NA mixtures were found to be inconsistent with respect to their homolog content by percent response. Differences in the observed homolog content varied significantly, particularly at the lower (n = 9-14) and higher (n = 20-23) carbon number ranges. Results highlighted the problem between using NA mixtures from different sources and different lot numbers but offered a solution to the problem from a concentration perspective. It is anticipated that this tool may be utilized in review of historical data in addition to future studies, such as the study of OSPW derived acid extractable organics (AEOs) and fractions employed during toxicological studies.

Biodegradation of naphthenic acid surrogates by axenic cultures.

PubMed

Yue, Siqing; Ramsay, Bruce A; Ramsay, Juliana A

2015-07-01

This is the first study to report that bacteria from the genera Ochrobactrum, Brevundimonas and Bacillus can be isolated by growth on naphthenic acids (NAs) extracted from oil sands process water (OSPW). These pure cultures were screened for their ability to use a range of aliphatic, cyclic and aromatic NA surrogates in 96-well microtiter plates using water-soluble tetrazolium redox dyes (Biolog Redox Dye H) as the indicator of metabolic activity. Of the three cultures, Ochrobactrum showed most metabolic activity on the widest range of NA surrogates. Brevundomonas and especially Ochrobactrum had higher metabolic activity on polycyclic aromatic compounds than other classes of NA surrogates. Bacillus also oxidized a wide range of NA surrogates but not as well as Ochrobactrum. Using this method to characterize NA utilisation, one can identify which NAs or NA classes in OSPW are more readily degraded. Since aromatic NAs have been shown to have an estrogenic effect and polycyclic monoaromatic compounds have been suggested to pose the greatest environmental threat among the NAs, these bacterial genera may play an important role in detoxification of OSPW. Furthermore, this study demonstrates that bacteria belonging to the genera Ochrobactrum and Bacillus can also degrade surrogates of tricyclic NAs.

Silver-Ion Solid Phase Extraction Separation of Classical, Aromatic, Oxidized, and Heteroatomic Naphthenic Acids from Oil Sands Process-Affected Water.

PubMed

Huang, Rongfu; Chen, Yuan; Gamal El-Din, Mohamed

2016-06-21

The separation of classical, aromatic, oxidized, and heteroatomic (sulfur-containing) naphthenic acid (NA) species from unprocessed and ozone-treated oil sands process-affected water (OSPW) was performed using silver-ion (Ag-ion) solid phase extraction (SPE) without the requirement of pre-methylation for NAs. OSPW samples before SPE and SPE fractions were characterized using ultra performance liquid chromatography ion mobility time-of-flight mass spectrometry (UPLC-IM-TOFMS) to corroborate the separation of distinct NA species. The mass spectrum identification applied a mass tolerance of ±1.5 mDa due to the mass errors of NAs were measured within this range, allowing the identification of O2S-NAs from O2-NAs. Moreover, separated NA species facilitated the tandem mass spectrometry (MS/MS) characterization of NA compounds due to the removal of matrix and a simplified composition. MS/MS results showed that classical, aromatic, oxidized, and sulfur-containing NA compounds were eluted into individual SPE fractions. Overall results indicated that the separation of NA species using Ag-ion SPE is a valuable method for extracting individual NA species that are of great interest for environmental toxicology and wastewater treatment research, to conduct species-specific studies. Furthermore, the separated NA species on the milligram level could be widely used as the standard materials for environmental monitoring of NAs from various contamination sites.

Solar photocatalytic degradation of naphthenic acids in oil sands process-affected water.

PubMed

Leshuk, Tim; Wong, Timothy; Linley, Stuart; Peru, Kerry M; Headley, John V; Gu, Frank

2016-02-01

Bitumen mining in the Canadian oil sands creates large volumes of oil sands process-affected water (OSPW), the toxicity of which is due in part to naphthenic acids (NAs) and other acid extractable organics (AEO). The objective of this work was to evaluate the potential of solar photocatalysis over TiO2 to remove AEO from OSPW. One day of photocatalytic treatment under natural sunlight (25 MJ/m(2) over ∼14 h daylight) eradicated AEO from raw OSPW, and acute toxicity of the OSPW toward Vibrio fischeri was eliminated. Nearly complete mineralization of organic carbon was achieved within 1-7 day equivalents of sunlight exposure, and degradation was shown to proceed through a superoxide-mediated oxidation pathway. High resolution mass spectrometry (HRMS) analysis of oxidized intermediate compounds indicated preferential degradation of the heavier and more cyclic NAs (higher number of double bond equivalents), which are the most environmentally persistent fractions. The photocatalyst was shown to be recyclable for multiple uses, and thus solar photocatalysis may be a promising "green" advanced oxidation process (AOP) for OSPW treatment. Copyright © 2015 Elsevier Ltd. All rights reserved.

Evaluation of corrosion products formed by sulfidation as inhibitors of the naphthenic corrosion of AISI-316 steel

NASA Astrophysics Data System (ADS)

Sanabria-Cala, J. A.; Montañez, N. D.; Laverde Cataño, D.; Y Peña Ballesteros, D.; Mejía, C. A.

2017-12-01

Naphthenic acids present in oil from most regions worldwide currently stand as the main responsible for the naphthenic corrosion problems, affecting the oil-refining industry. The phenomenon of sulfidation, accompanying corrosion processes brought about by naphthenic acids in high-temperature refining plant applications, takes place when the combination of sulfidic acid (H2S) with Fe forms layers of iron sulphide (FeS) on the material surface, layers with the potential to protect the material from attack by other corrosive species like naphthenic acids. This work assessed corrosion products formed by sulfidation as inhibitors of naphthenic corrosion rate in AISI-316 steel exposed to processing conditions of simulated crude oil in a dynamic autoclave. Calculation of the sulfidation and naphthenic corrosion rates were determined by gravimetry. The surfaces of the AISI-316 gravimetric coupons exposed to acid systems; were characterized morphologically by X-Ray Diffraction (XRD) and X-ray Fluorescence by Energy Dispersive Spectroscopy (EDS) combined with Scanning Electron Microscopy (SEM). One of the results obtained was the determination of an inhibiting effect of corrosion products at 250 and 300°C, where lower corrosion rate levels were detected. For the temperature of 350°C, naphthenic corrosion rates increased due to deposition of naphthenic acids on the areas where corrosion products formed by sulfidation have lower homogeneity and stability on the surface, thus accelerating the destruction of AISI-316 steel. The above provides an initial contribution to oil industry in search of new alternatives to corrosion control by the attack of naphthenic acids, from the formation of FeS layers on exposed materials in the processing of heavy crude oils with high sulphur content.

Naphthenic acids in groundwater overlying undeveloped shale gas and tight oil reservoirs.

PubMed

Ahad, Jason M E; Pakdel, Hooshang; Lavoie, Denis; Lefebvre, René; Peru, Kerry M; Headley, John V

2018-01-01

The acid extractable organics (AEOs) containing naphthenic acids (NAs) in groundwater overlying undeveloped shale gas (Saint-Édouard region) and tight oil (Haldimand sector, Gaspé) reservoirs in Québec, Canada, were analysed using high resolution Orbitrap mass spectrometry and thermal conversion/elemental analysis - isotope ratio mass spectrometry. As classically defined by C n H 2n+Z O 2 , the most abundant NAs detected in the majority of groundwater samples were straight-chain (Z = 0) or monounsaturated (Z = -2) C 16 and C 18 fatty acids. Several groundwater samples from both study areas, however, contained significant proportions of presumably alicyclic bicyclic NAs (i.e., Z = -4) in the C 10 -C 18 range. These compounds may have originated from migrated waters containing a different distribution of NAs, or are the product of in situ microbial alteration of shale organic matter and petroleum. In most groundwater samples, intramolecular carbon isotope values generated by pyrolysis (δ 13 C pyr ) of AEOs were on average around 2-3‰ heavier than those generated by bulk combustion (δ 13 C) of AEOs, providing further support for microbial reworking of subsurface organic carbon. Although concentrations of AEOs were very low (<2.0 mg/L), the detection of potentially toxic bicyclic acids in groundwater overlying unconventional hydrocarbon reservoirs points to a natural background source of organic contaminants prior to any large-scale commercial hydrocarbon development. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

Adsorption of naphthenic acids on high surface area activated carbons.

PubMed

Iranmanesh, Sobhan; Harding, Thomas; Abedi, Jalal; Seyedeyn-Azad, Fakhry; Layzell, David B

2014-01-01

In oil sands mining extraction, water is an essential component; however, the processed water becomes contaminated through contact with the bitumen at high temperature, and a portion of it cannot be recycled and ends up in tailing ponds. The removal of naphthenic acids (NAs) from tailing pond water is crucial, as they are corrosive and toxic and provide a substrate for microbial activity that can give rise to methane, which is a potent greenhouse gas. In this study, the conversion of sawdust into an activated carbon (AC) that could be used to remove NAs from tailings water was studied. After producing biochar from sawdust by a slow-pyrolysis process, the biochar was physically activated using carbon dioxide (CO2) over a range of temperatures or prior to producing biochar, and the sawdust was chemically activated using phosphoric acid (H3PO4). The physically activated carbon had a lower surface area per gram than the chemically activated carbon. The physically produced ACs had a lower surface area per gram than chemically produced AC. In the adsorption tests with NAs, up to 35 mg of NAs was removed from the water per gram of AC. The chemically treated ACs showed better uptake, which can be attributed to its higher surface area and increased mesopore size when compared with the physically treated AC. Both the chemically produced and physically produced AC provided better uptake than the commercially AC.

Structure-reactivity relationship of naphthenic acids in the photocatalytic degradation process.

PubMed

de Oliveira Livera, Diogo; Leshuk, Tim; Peru, Kerry M; Headley, John V; Gu, Frank

2018-06-01

Bitumen extraction in Canada's oil sands generates oil sands process-affected water (OSPW) as a toxic by-product. Naphthenic acids (NAs) contribute to the water's toxicity, and treatment methods may need to be implemented to enable safe discharge. Heterogeneous photocatalysis is a promising advanced oxidation process (AOP) for OSPW remediation, however, its successful implementation requires understanding of the complicated relationship between structure and reactivity of NAs. This work aimed to study the effect of various structural properties of model compounds on the photocatalytic degradation kinetics via high resolution mass spectrometry (HRMS), including diamondoid structures, heteroatomic species, and degree of unsaturation. The rate of photocatalytic treatment increased significantly with greater structural complexity, namely with carbon number, aromaticity and degree of cyclicity, properties that render particular NAs recalcitrant to biodegradation. It is hypothesized that a superoxide radical-mediated pathway explains these observations and offers additional benefits over traditional hydroxyl radical-based AOPs. Detailed structure-reactivity investigations of NAs in photocatalysis have not previously been undertaken, and the results described herein illustrate the potential benefit of combining photocatalysis and biodegradation as a complete OSPW remediation technology. Copyright © 2018 Elsevier Ltd. All rights reserved.

Impact of peroxydisulfate in the presence of zero valent iron on the oxidation of cyclohexanoic acid and naphthenic acids from oil sands process-affected water.

PubMed

Drzewicz, Przemysław; Perez-Estrada, Leonidas; Alpatova, Alla; Martin, Jonathan W; Gamal El-Din, Mohamed

2012-08-21

Large volumes of oil sands process-affected water (OSPW) are produced during the extraction of bitumen from oil sands in Alberta, Canada. The degradation of a model naphthenic acid, cyclohexanoic acid (CHA), and real naphthenic acids (NAs) from OSPW were investigated in the presence of peroxydisulfate (S(2)O(8)(2-)) and zerovalent iron (ZVI). For the model compound CHA (50 mg/L), in the presence of ZVI and 500 mg/L S(2)O(8)(2-), the concentration decreased by 45% after 6 days of treatment at 20 °C, whereas at 40, 60, and 80 °C the concentration decreased by 20, 45 and 90%, respectively, after 2 h of treatment. The formation of chloro-CHA was observed during ZVI/S(2)O(8)(2-) treatment of CHA in the presence of chloride. For OSPW NAs, in the presence of ZVI alone, a 50% removal of NAs was observed after 6 days of exposure at 20 °C. The addition of 100 mg/L S(2)O(8)(2-) to the solution increased the removal of OSPW NAs from 50 to 90%. In absence of ZVI, a complete NAs removal from OSPW was observed in presence of 2000 mg/L S(2)O(8)(2-) at 80 °C. The addition of ZVI increased the efficiency of NAs oxidation by S(2)O(8)(2-) near room temperature. Thus, ZVI/S(2)O(8)(2-) process was found to be a viable option for accelerating the degradation of NAs present in OSPW.

Chemical fingerprinting of naphthenic acids and oil sands process waters-A review of analytical methods for environmental samples.

PubMed

Headley, J V; Peru, K M; Mohamed, M H; Frank, R A; Martin, J W; Hazewinkel, R R O; Humphries, D; Gurprasad, N P; Hewitt, L M; Muir, D C G; Lindeman, D; Strub, R; Young, R F; Grewer, D M; Whittal, R M; Fedorak, P M; Birkholz, D A; Hindle, R; Reisdorph, R; Wang, X; Kasperski, K L; Hamilton, C; Woudneh, M; Wang, G; Loescher, B; Farwell, A; Dixon, D G; Ross, M; Pereira, A Dos Santos; King, E; Barrow, M P; Fahlman, B; Bailey, J; McMartin, D W; Borchers, C H; Ryan, C H; Toor, N S; Gillis, H M; Zuin, L; Bickerton, G; Mcmaster, M; Sverko, E; Shang, D; Wilson, L D; Wrona, F J

2013-01-01

This article provides a review of the routine methods currently utilized for total naphthenic acid analyses. There is a growing need to develop chemical methods that can selectively distinguish compounds found within industrially derived oil sands process affected waters (OSPW) from those derived from the natural weathering of oil sands deposits. Attention is thus given to the characterization of other OSPW components such as oil sands polar organic compounds, PAHs, and heavy metals along with characterization of chemical additives such as polyacrylamide polymers and trace levels of boron species. Environmental samples discussed cover the following matrices: OSPW containments, on-lease interceptor well systems, on- and off-lease groundwater, and river and lake surface waters. There are diverse ranges of methods available for analyses of total naphthenic acids. However, there is a need for inter-laboratory studies to compare their accuracy and precision for routine analyses. Recent advances in high- and medium-resolution mass spectrometry, concomitant with comprehensive mass spectrometry techniques following multi-dimensional chromatography or ion-mobility separations, have allowed for the speciation of monocarboxylic naphthenic acids along with a wide range of other species including humics. The distributions of oil sands polar organic compounds, particularly the sulphur containing species (i.e., OxS and OxS2) may allow for distinguishing sources of OSPW. The ratios of oxygen- (i.e., Ox) and nitrogen-containing species (i.e., NOx, and N2Ox) are useful for differentiating organic components derived from OSPW from natural components found within receiving waters. Synchronous fluorescence spectroscopy also provides a powerful screening technique capable of quickly detecting the presence of aromatic organic acids contained within oil sands naphthenic acid mixtures. Synchronous fluorescence spectroscopy provides diagnostic profiles for OSPW and potentially impacted

In situ biodegradation of naphthenic acids in oil sands tailings pond water using indigenous algae-bacteria consortium.

PubMed

Mahdavi, Hamed; Prasad, Vinay; Liu, Yang; Ulrich, Ania C

2015-01-01

In this study, the biodegradation of total acid-extractable organics (TAOs), commonly called naphthenic acids (NAs), was investigated. An indigenous microbial culture containing algae and bacteria was taken from the surface of a tailings pond and incubated over the course of 120days. The influence of light, oxygen and the presence of indigenous algae and bacteria, and a diatom (Navicula pelliculosa) on the TAO removal rate were elucidated. The highest biodegradation rate was observed with bacteria growth only (without light exposure) with a half-life (t(1/2)) of 203days. The algae-bacteria consortium enhanced the detoxification process, however, bacterial biomass played the main role in toxicity reduction. Principal component analysis (PCA) conducted on FT-IR spectra, identified functional groups and bonds (representing potential markers for biotransformation of TAOs) as follows: hydroxyl, carboxyl and amide groups along with CH, arylH, arylOH and NH bonds. Copyright © 2015 Elsevier Ltd. All rights reserved.

Aquatic plant-derived changes in oil sands naphthenic acid signatures determined by low-, high- and ultrahigh-resolution mass spectrometry.

PubMed

Headley, John V; Peru, Kerry M; Armstrong, Sarah A; Han, Xiumei; Martin, Jonathan W; Mapolelo, Mmilili M; Smith, Donald F; Rogers, Ryan P; Marshall, Alan G

2009-02-01

Mass spectrometry is a common tool for studying the fate of complex organic compound mixtures in oil sands processed water (OSPW), but a comparison of low-, high- ( approximately 10 000), and ultrahigh-resolution ( approximately 400 000) instrumentation for this purpose has not previously been made. High-resolution quadrupole time-of-flight mass spectrometry (QTOF MS) and ultrahigh-resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS), with negative-ion electrospray ionization, provided evidence for the selective dissipation of components in OSPW. Dissipation of oil sands naphthenic acids (NAs with general formula C(n)H(2n+z)O(2) where n is the number of carbon atoms, and Z is zero or a negative even number describing the number of rings) was masked (by components such as fatty acids, O(3), O(5), O(6), O(7), SO(2), SO(3), SO(4), SO(5), SO(6), and NO(4) species) at low resolution (1000) when using a triple quadrupole mass spectrometer. Changes observed in the relative composition of components in OSPW appear to be due primarily to the presence of plants, specifically cattails (Typha latifolia) and their associated microorganisms. The observed dissipation included a range of heteratomic species containing O(2), O(3), O(4), and O(5), present in Athabasca oil sands acid extracts. For the heteratomic O(2) species, namely naphthenic acids, an interesting structural relationship suggests that low and high carbon number NAs are dissipated by the plants preferentially, with a minimum around C(14)/C(15). Other heteratomic species containing O(6), O(7), SO(2), SO(3), SO(4), SO(5), SO(6), and NO(4) appear to be relatively recalcitrant to the cattails and were not dissipated to the same extent in planted systems. Copyright 2009 John Wiley & Sons, Ltd.

Comparison of four advanced oxidation processes for the removal of naphthenic acids from model oil sands process water.

PubMed

Liang, Xiaoming; Zhu, Xingdong; Butler, Elizabeth C

2011-06-15

Four advanced oxidation processes (UV/TiO(2), UV/IO(4)(-), UV/S(2)O(8)(2-), and UV/H(2)O(2)) were tested for their ability to mineralize naphthenic acids to inorganic carbon in a model oil sands process water containing high dissolved and suspended solids at pH values ranging from 8 to 12. A medium pressure mercury (Hg) lamp was used, and a Quartz immersion well surrounded the lamp. The treatment goal of 5mg/L naphthenic acids (3.4 mg/L total organic carbon (TOC)) was achieved under four conditions: UV/S(2)O(8)(2-) (20mM) at pH 8 and 10, and UV/H(2)O(2) (50mM) at pH 8 (all with the Quartz immersion well). Values of electrical energy required to meet the treatment goal were about equal for UV/S(2)O(8)(2-) (20mM) and UV/H(2)O(2) (50mM) at pH 8, but three to four times larger for treatment by UV/S(2)O(8)(2-) (20mM) at pH 10. The treatment goal was also achieved using UV/S(2)O(8)(2-) (20mM) at pH 10 when using a Vycor filter that transmits light primarily in the mid and near UV, suggesting that that treatment of naphthenic acids by UV/S(2)O(8)(2-) using low pressure Hg lamps may be feasible. Copyright © 2011 Elsevier B.V. All rights reserved.

Chemical fingerprinting of naphthenic acids at an oil sands end pit lake by comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GC×GC/TOFMS)

NASA Astrophysics Data System (ADS)

Bowman, D. T.; Arriaga, D.; Morris, P.; Risacher, F.; Warren, L. A.; McCarry, B. E.; Slater, G.

2016-12-01

Naphthenic acids (NAs) are naturally occurring in Athabasca oil sands and accumulate in tailings as a result of water-based extraction processes. NAs contribute to the toxicity of tailings and oil sands process-affected water (OSPW). NAs exist as a complex mixture, so the development of an analytical technique to characterize them has been an on-going challenge. The monitoring of individual NAs and their associated isomers through multidimensional chromatography has the potential to provide greater insight into the behavior of NAs in the environment. For NAs whose proportions do not change during environmental processing, NA ratios may provide a means to develop fingerprints characteristic of specific sources. Alternatively, relative changes in the proportions of NAs may provide a tracer of their occurrence and extent of removal. As yet, only a few studies have begun to explore these possibilities. In this study, comprehensive two dimensional gas chromatography/time-of-flight mass spectrometry was used to monitor individual naphthenic acids in an end pit lake in Alberta, Canada. NA profiles from different depths and sampling locations were compared to evaluate the spatial variations at the site.

Using ultrahigh-resolution mass spectrometry and toxicity identification techniques to characterize the toxicity of oil sands process-affected water: The case for classical naphthenic acids.

PubMed

Hughes, Sarah A; Mahaffey, Ashley; Shore, Bryon; Baker, Josh; Kilgour, Bruce; Brown, Christine; Peru, Kerry M; Headley, John V; Bailey, Howard C

2017-11-01

Previous assessments of oil sands process-affected water (OSPW) toxicity were hampered by lack of high-resolution analytical analysis, use of nonstandard toxicity methods, and variability between OSPW samples. We integrated ultrahigh-resolution mass spectrometry with a toxicity identification evaluation (TIE) approach to quantitatively identify the primary cause of acute toxicity of OSPW to rainbow trout (Oncorhynchus mykiss). The initial characterization of OSPW toxicity indicated that toxicity was associated with nonpolar organic compounds, and toxicant(s) were further isolated within a range of discrete methanol fractions that were then subjected to Orbitrap mass spectrometry to evaluate the contribution of naphthenic acid fraction compounds to toxicity. The results showed that toxicity was attributable to classical naphthenic acids, with the potency of individual compounds increasing as a function of carbon number. Notably, the mass of classical naphthenic acids present in OSPW was dominated by carbon numbers ≤16; however, toxicity was largely a function of classical naphthenic acids with ≥17 carbons. Additional experiments found that acute toxicity of the organic fraction was similar when tested at conductivities of 400 and 1800 μmhos/cm and that rainbow trout fry were more sensitive to the organic fraction than larval fathead minnows (Pimephales promelas). Collectively, the results will aid in developing treatment goals and targets for removal of OSPW toxicity in water return scenarios both during operations and on mine closure. Environ Toxicol Chem 2017;36:3148-3157. © 2017 SETAC. © 2017 SETAC.

Advances in mass spectrometric characterization of naphthenic acids fraction compounds in oil sands environmental samples and crude oil--A review.

PubMed

Headley, John V; Peru, Kerry M; Barrow, Mark P

2016-01-01

There has been a recent surge in the development of mass spectrometric methods for detailed characterization of naphthenic acid fraction compounds (all C(c)H(h)N(n)O(o)S(s), species, including heteroatomic and aromatic components in the acid-extractable fraction) in environmental samples. This surge is driven by the increased activity in oil sands environmental monitoring programs in Canada, the exponential increase in research studies on the isolation and toxicity identification of components in oil sands process water (OSPW), and the analytical requirements for development of technologies for treatment of OSPW. There has been additional impetus due to the parallel studies to control corrosion from naphthenic acids during the mining and refining of heavy bitumen and crude oils. As a result, a range of new mass spectrometry tools have been introduced since our last major review of this topic in 2009. Of particular significance are the developments of combined mass spectrometric methods that incorporate technologies such as gas chromatography, liquid chromatography, and ion mobility. There has been additional progress with respect to improved visualization methods for petroleomics and oil sands environmental forensics. For comprehensive coverage and more reliable characterization of samples, an approach based on multiple-methods that employ two or more ionization modes is recommended. On-line or off-line fractionation of isolated extracts, with or without derivatization, might also be used prior to mass spectrometric analyses. Individual ionization methods have their associated strengths and weaknesses, including biases, and thus dependence upon a single ionization method is potentially misleading. There is also a growing trend to not rely solely on low-resolution mass spectrometric methods (<20,000 resolving power at m/z 200) for characterization of complex samples. Future research is anticipated to focus upon (i) structural elucidation of components to determine

Fate and behavior of oil sands naphthenic acids in a pilot-scale treatment wetland as characterized by negative-ion electrospray ionization Orbitrap mass spectrometry.

PubMed

Ajaero, Chukwuemeka; Peru, Kerry M; Simair, Monique; Friesen, Vanessa; O'Sullivan, Gwen; Hughes, Sarah A; McMartin, Dena W; Headley, John V

2018-08-01

Large volumes of oil sands process-affected water (OSPW) are generated during the extraction of bitumen from oil sands in the Athabasca region of northeastern Alberta, Canada. As part of the development of treatment technologies, molecular characterization of naphthenic acids (NAs) and naphthenic acid fraction compounds (NAFC) in wetlands is a topic of research to better understand their fate and behavior in aquatic environments. Reported here is the application of high-resolution negative-ion electrospray Orbitrap-mass spectrometry for molecular characterization of NAs and NAFCs in a non-aerated constructed treatment wetland. The effectiveness of the wetlands to remove OSPW-NAs and NAFCs was evaluated by monitoring the changes in distributions of NAFC compounds in the untreated sample and non-aerated treatment system. After correction for measured evapotranspiration, the removal rate of the classical NAs followed approximately first-order kinetics, with higher rates observed for structures with relatively higher number of carbon atoms. These findings indicate that constructed wetland treatment is a viable method for removal of classical NAs in OSPW. Work is underway to evaluate the effects of wetland design on water quality improvement, preferential removal of different NAFC species, and reduction in toxicity. Copyright © 2018. Published by Elsevier B.V.

Characterization of naphthenic acids in oil sands wastewaters by gas chromatography-mass spectrometry.

PubMed

Holowenko, Fervone M; MacKinnon, Michael D; Fedorak, Phillip M

2002-06-01

The water produced during the extraction of bitumen from oil sands is toxic to aquatic organisms due largely to a group of naturally occurring organic acids, naphthenic acids (NAs), that are solubilized from the bitumen during processing. NAs are a complex mixture of alkyl-substituted acyclic and cycloaliphatic carboxylic acids, with the general chemical formula CnH(2n + Z)O2, where n is the carbon number and Z specifies a homologous family. Gas chromatography-electron impact mass spectrometry was used to characterize NAs in nine water samples derived from oil sands extraction processes. For each sample, the analysis provided the relative abundances for up to 156 base peaks, with each representing at least one NA structure. Plotting the relative abundances of NAs as three-dimensional bar graphs showed differences among samples. The relative abundance of NAs with carbon numbers < or = 21 to those in the "C22 + cluster" (sum of all NAs with carbon numbers > or = 22 in Z families 0 to -12) proved useful for comparing the water samples that had a range of toxicities. A decrease in toxicity of process-affected waters accompanied an increase in the proportion of NAs in the "C22 + cluster", likely caused by biodegradation of NAs with carbon numbers of < or = 21. In addition, an increase in the proportion of NAs in the "C22 + cluster" accompanied a decrease in the total NAs in the process-affected waters, again suggesting the selective removal of NAs with carbon numbers of < or = 21. This is the first investigation in which changes in the fingerprint of the NA fraction of process-affected waters from the oil sands operations has corresponded with measured toxicity in these waters.

Modified biopolymers as sorbents for the removal of naphthenic acids from oil sands process affected water (OSPW).

PubMed

Arshad, Muhammad; Khosa, M A; Siddique, Tariq; Ullah, Aman

2016-11-01

Oil sands operations consume large volumes of water in bitumen extraction process and produce tailings that express pore water to the surface of tailings ponds known as oil sands process-affected water (OSPW). The OSPW is toxic and cannot be released into the environment without treatment. In addition to metals, dissolved solids, dissolved gases, hydrocarbons and polyaromatic compounds etc., OSPW also contains a complex mixture of dissolved organic acids, referred to as naphthenic acids (NAs). The NAs are highly toxic and react with metals to develop highly corrosive functionalities which cause corrosion in the oil sands processing and refining processes. We have chemically modified keratin biopolymer using polyhedral oligomeric silsesquioxanes (POSS) nanocages and goethite dopant to unfold keratinous structure for improving functionality. The untreated neat keratin and two modified sorbents were characterized to investigate structural, morphological, dimensional and thermal properties. These sorbents were then tested for the removal of NAs from OSPW. The NAs were selectively extracted and quantified before and after sorption process. The biosorption capacity (Q), rejection percentage (R%) and isotherm models were studied to investigate NAs removal efficiency of POSS modified keratin biopolymer (PMKB) and goethite modified keratin biopolymer (GMKB) from aliquots of OSPW. Copyright © 2016 Elsevier Ltd. All rights reserved.

Evaluation of biologically mediated changes in oil sands naphthenic acid composition by Chlamydomonas reinhardtii using negative-ion electrospray orbitrap mass spectrometry.

PubMed

Goff, Kira L; Peru, Kerry; Wilson, Kenneth E; Headley, John V

2014-08-01

Industrial activity associated with oil-sands extraction in Canada's Athabasca region produces a variety of contaminants of concern, including naphthenic acid fraction components (NAFCs). NAFCs are a complex mixture of organic compounds that are poorly understood both in terms of their chemical composition and effects on the environment. NAFC toxicity in the unicellular green algae Chlamydomonas reinhardtii P.A.Dangeard was correlated with the presence of the algal cell wall. It was suggested that the toxicity of NAFCs in C. reinhardtii was due to surfactant effects. Surfactant-cell wall interactions are specific and governed by the compound class and structure, and by the nature of the biological material. Here, we investigate the effects of wildtype (WT) C. reinhardtii and two cell-wall mutants on specific classes of NAFCs when growing cultures were treated with a 100 mg · L(-1) solution of NAFCs. Changes in the NAFC composition in the media were examined using high resolution mass spectrometry over a period of 4 d. Algal mediated changes in the NAFCs were limited to specific classes of NAFCs. In particular, the removal of large, classical naphthenic acids, with a double bond equivalent of 8, was observed in WT C. reinhardtii cultures. The observed algal mediated changes in NAFC composition would have been masked by low resolution mass spectrometry and highlight the importance of this tool in examining bioremediation of complex mixtures of NAFCs. © 2014 Phycological Society of America.

Naphthenic acids speciation and removal during petroleum-coke adsorption and ozonation of oil sands process-affected water.

PubMed

Gamal El-Din, Mohamed; Fu, Hongjing; Wang, Nan; Chelme-Ayala, Pamela; Pérez-Estrada, Leonidas; Drzewicz, Przemysław; Martin, Jonathan W; Zubot, Warren; Smith, Daniel W

2011-11-01

The Athabasca Oil Sands industry produces large volumes of oil sands process-affected water (OSPW) as a result of bitumen extraction and upgrading processes. Constituents of OSPW include chloride, naphthenic acids (NAs), aromatic hydrocarbons, and trace heavy metals, among other inorganic and organic compounds. To address the environmental issues associated with the recycling and/or safe return of OSPW into the environment, water treatment technologies are required. This study examined, for the first time, the impacts of pretreatment steps, including filtration and petroleum-coke adsorption, on ozonation requirements and performance. The effect of the initial OSPW pH on treatment performance, and the evolution of ozonation and its impact on OSPW toxicity and biodegradability were also examined. The degradation of more than 76% of total acid-extractable organics was achieved using a semi-batch ozonation system at a utilized ozone dose of 150 mg/L. With a utilized ozone dose of 100 mg/L, the treated OSPW became more biodegradable and showed no toxicity towards Vibrio fischeri. Changes in the NA profiles in terms of carbon number and number of rings were observed after ozonation. The filtration of the OSPW did not improve the ozonation performance. Petroleum-coke adsorption was found to be effective in reducing total acid-extractable organics by a 91%, NA content by an 84%, and OSPW toxicity from 4.3 to 1.1 toxicity units. The results of this study indicate that the combination of petroleum-coke adsorption and ozonation is a promising treatment approach to treat OSPW. Copyright © 2011 Elsevier B.V. All rights reserved.

21 CFR 524.463 - Copper naphthenate.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 6 2011-04-01 2011-04-01 false Copper naphthenate. 524.463 Section 524.463 Food... DRUGS, FEEDS, AND RELATED PRODUCTS OPHTHALMIC AND TOPICAL DOSAGE FORM NEW ANIMAL DRUGS § 524.463 Copper naphthenate. (a) Amount. The drug is a 37.5 percent solution of copper naphthenate. (b) Sponsors. See Nos...

21 CFR 524.463 - Copper naphthenate.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Copper naphthenate. 524.463 Section 524.463 Food... DRUGS, FEEDS, AND RELATED PRODUCTS OPHTHALMIC AND TOPICAL DOSAGE FORM NEW ANIMAL DRUGS § 524.463 Copper naphthenate. (a) Amount. The drug is a 37.5 percent solution of copper naphthenate. (b) Sponsors. See Nos...

Kinetics of liquid-solid reactions in naphthenic acid conversion and Kraft pulping

NASA Astrophysics Data System (ADS)

Yang, Ling

Two liquid-solid reactions, in which the morphology of the solid changes as the reactions proceeds, were examined. One is the NA conversion in oil by decarboxylation on metal oxides and carbonates, and the other is the Kraft pulping in which lignin removal by delignification reaction. In the study of the NA conversion, CaO was chosen as the catalyst for the kinetic study from the tested catalysts based on NA conversion. Two reaction mixtures, carrier oil plus commercial naphthenic acids and heavy vacuum gas oil (HVGO) from Athabasca bitumen, were applied in the kinetic study. The influence of TAN, temperature, and catalyst loading on the NA conversion and decarboxylation were studied systematically. The results showed that the removal rate of TAN and the decarboxylation of NA were both independent of the concentration of NA over the range studied, and significantly dependent on reaction temperature. The data from analyzing the spent catalyst demonstrated that calcium naphthenate was an intermediate of the decarboxylation reaction of NA, and the decomposition of calcium naphthenate was a rate-determining step. In the study on the delignification of the Kraft pulping, a new mechanism was proposed for the heterogeneous delignification reaction during the Kraft pulping process. In particular, the chemical reaction mechanism took into account the heterogeneous nature of Kraft pulping. Lignin reacted in parallel with sodium hydroxide and sodium sulfide. The mechanism consists of three key kinetic steps: (1) adsorption of hydroxide and hydrosulfide ions on lignin; (2) surface reaction on the solid surface to produce degraded lignin products; and (3) desorption of degradation products from the solid surface. The most important step for the delignification process is the surface reaction, rather than the reactions occurring in the liquid phase. A kinetic model has, thus, been developed based on the proposed mechanism. The derived kinetic model showed that the mechanism

Comparison of methods for determination of total oil sands-derived naphthenic acids in water samples.

PubMed

Hughes, Sarah A; Huang, Rongfu; Mahaffey, Ashley; Chelme-Ayala, Pamela; Klamerth, Nikolaus; Meshref, Mohamed N A; Ibrahim, Mohamed D; Brown, Christine; Peru, Kerry M; Headley, John V; Gamal El-Din, Mohamed

2017-11-01

There are several established methods for the determination of naphthenic acids (NAs) in waters associated with oil sands mining operations. Due to their highly complex nature, measured concentration and composition of NAs vary depending on the method used. This study compared different common sample preparation techniques, analytical instrument methods, and analytical standards to measure NAs in groundwater and process water samples collected from an active oil sands operation. In general, the high- and ultrahigh-resolution methods, namely high performance liquid chromatography time-of-flight mass spectrometry (UPLC-TOF-MS) and Orbitrap mass spectrometry (Orbitrap-MS), were within an order of magnitude of the Fourier transform infrared spectroscopy (FTIR) methods. The gas chromatography mass spectrometry (GC-MS) methods consistently had the highest NA concentrations and greatest standard error. Total NAs concentration was not statistically different between sample preparation of solid phase extraction and liquid-liquid extraction. Calibration standards influenced quantitation results. This work provided a comprehensive understanding of the inherent differences in the various techniques available to measure NAs and hence the potential differences in measured amounts of NAs in samples. Results from this study will contribute to the analytical method standardization for NA analysis in oil sands related water samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of alkyl side chain location and cyclicity on the aerobic biotransformation of naphthenic acids.

PubMed

Misiti, Teresa M; Tezel, Ulas; Pavlostathis, Spyros G

2014-07-15

Aerobic biodegradation of naphthenic acids is of importance to the oil industry for the long-term management and environmental impact of process water and wastewater. The effect of structure, particularly the location of the alkyl side chain as well as cyclicity, on the aerobic biotransformation of 10 model naphthenic acids (NAs) was investigated. Using an aerobic, mixed culture, enriched with a commercial NA mixture (NA sodium salt; TCI Chemicals), batch biotransformation assays were conducted with individual model NAs, including eight 8-carbon isomers. It was shown that NAs with a quaternary carbon at the α- or β-position or a tertiary carbon at the β- and/or β'-position are recalcitrant or have limited biodegradability. In addition, branched NAs exhibited lag periods and lower degradation rates than nonbranched or simple cyclic NAs. Two NA isomers used in a closed bottle, aerobic biodegradation assay were mineralized, while 21 and 35% of the parent compound carbon was incorporated into the biomass. The NA biodegradation probability estimated by two widely used models (BIOWIN 2 and 6) and a recently developed model (OCHEM) was compared to the biodegradability of the 10 model NAs tested in this study as well as other related NAs. The biodegradation probability estimated by the OCHEM model agreed best with the experimental data and was best correlated with the measured NA biodegradation rate.

Phytotoxicity and naphthenic acid dissipation from oil sands fine tailings treatments planted with the emergent macrophyte Phragmites australis.

PubMed

Armstrong, Sarah A; Headley, John V; Peru, Kerry M; Mikula, Randy J; Germida, James J

2010-01-01

During reclamation the water associated with the runoff or groundwater flushing from dry stackable tailings technologies may become available to the reclaimed environment within an oil sands lease. Here we evaluate the performance of the emergent macrophyte, common reed (Phragmites australis), grown in chemically amended mature fine tailings (MFT) and simulated runoff/seepage water from different MFT drying treatments. The present study also investigated the phytotoxicity of the concentration of oil sands naphthenic acids (NAs) in different MFT drying chemical treatments, in both planted and unplanted systems. We demonstrate that although growth was reduced, the emergent macrophyte common reed was capable of growing in diluted unamended MFT runoff, as well as in diluted runoff from MFT amended with either 0.25% lime and gypsum or 0.5% gypsum. Common reed can thus assist in the dewatering process of oil sands MFT. However, simulated runoff or seepage waters from chemically amended and dried MFT were phytotoxic, due to combined levels of salts, naphthenic acids and pH. Phytoremediation of runoff water/ground water seepage from dry-land applied MFT will thus require pre-treatment in order to make conditions more favorable for plant growth.

Embryonic exposure to model naphthenic acids delays growth and hatching in the pond snail Lymnaea stagnalis.

PubMed

Johnston, Christina U; Clothier, Lindsay N; Quesnel, Dean M; Gieg, Lisa M; Chua, Gordon; Hermann, Petra M; Wildering, Willem C

2017-02-01

Naphthenic acids (NAs), a class of structurally diverse carboxylic acids with often complex ring structures and large aliphatic tail groups, are important by-products of many petrochemical processes including the oil sands mining activity of Northern Alberta. While it is evident that NAs have both acute and chronic harmful effects on many organisms, many aspects of their toxicity remain to be clarified. Particularly, while substantive data sets have been collected on NA toxicity in aquatic prokaryote and vertebrate model systems, to date, nothing is known about the toxic effects of these compounds on the embryonic development of aquatic invertebrate taxa, including freshwater mollusks. This study examines under laboratory conditions the toxicity of NAs extracted from oil sands process water (OSPW) and the low-molecular weight model NAs cyclohexylsuccinic acid (CHSA), cyclohexanebutyric acid (CHBA), and 4-tert-butylcyclohexane carboxylic acid (4-TBCA) on embryonic development of the snail Lymnaea stagnalis, a common freshwater gastropod with a broad Palearctic distribution. Evidence is provided for concentration-dependent teratogenic effects of both OSPW-derived and model NAs with remarkably similar nominal threshold concentrations between 15 and 20 mg/L and 28d EC 50 of 31 mg/L. In addition, the data provide evidence for substantial toxicokinetic differences between CHSA, CHBA and 4-TBCA. Together, our study introduces Lymnaea stagnalis embryonic development as an effective model to assay NA-toxicity and identifies molecular architecture as a potentially important toxicokinetic parameter in the toxicity of low-molecular weight NA in embryonic development of aquatic gastropods. Copyright © 2016 Elsevier Ltd. All rights reserved.

Photocatalytic degradation kinetics of naphthenic acids in oil sands process-affected water: Multifactorial determination of significant factors.

PubMed

Leshuk, Tim; de Oliveira Livera, Diogo; Peru, Kerry M; Headley, John V; Vijayaraghavan, Sucharita; Wong, Timothy; Gu, Frank

2016-12-01

Oil sands process-affected water (OSPW) is generated as a byproduct of bitumen extraction in Canada's oil sands. Due to the water's toxicity, associated with dissolved acid extractable organics (AEO), especially naphthenic acids (NAs), along with base-neutral organics, OSPW may require treatment to enable safe discharge to the environment. Heterogeneous photocatalysis is a promising advanced oxidation process (AOP) for OSPW remediation, however, predicting treatment efficacy can be challenging due to the unique water chemistry of OSPW from different tailings ponds. The objective of this work was to study various factors affecting the kinetics of photocatalytic AEO degradation in OSPW. The rate of photocatalytic treatment varied significantly in two different OSPW sources, which could not be accounted for by differences in AEO composition, as studied by high resolution mass spectrometry (HRMS). The effects of inorganic water constituents were investigated using factorial and response surface experiments, which revealed that hydroxyl (HO) radical scavenging by iron (Fe 3+ ) and bicarbonate (HCO 3 - ) inhibited the NA degradation rate. The effects of NA concentration and temperature on the treatment kinetics were also evaluated in terms of Langmuir-Hinshelwood and Arrhenius models; pH and temperature were identified as weak factors, while dissolved oxygen (DO) was critical to the photo-oxidation reaction. Accounting for all of these variables, a general empirical kinetic expression is proposed, enabling prediction of photocatalytic treatment performance in diverse sources of OSPW. Copyright © 2016 Elsevier Ltd. All rights reserved.

Biodegradation of naphthenic acids in oils sands process waters in an immobilized soil/sediment bioreactor.

PubMed

McKenzie, Natalie; Yue, Siqing; Liu, Xudong; Ramsay, Bruce A; Ramsay, Juliana A

2014-08-01

Aqueous extraction of bitumen in the Alberta oil sands industry produces large volumes of oil sands process water (OSPW) containing naphthenic acids (NAs), a complex mixture of carboxylic acids that are acutely toxic to aquatic organisms. Although aerobic biodegradation reduces NA concentrations and OSPW toxicity, treatment times are long, however, immobilized cell reactors have the potential to improve NA removal rates. In this study, two immobilized soil/sediment bioreactors (ISBRs) operating in series were evaluated for treatment of NAs in OSPW. A biofilm was established from microorganisms associated with sediment particles from an OSPW contaminated wetland on a non-woven textile. At 16 months of continuous operation with OSPW as the sole source of carbon and energy, 38±7% NA removal was consistently achieved at a residence time of 160 h at a removal rate of 2.32 mg NAs L(-1)d(-1). The change in NA profile measured by gas chromatography-mass spectrometry indicated that biodegradability decreased with increasing cyclicity. These results indicate that such treatment can significantly reduce NA removal rates compared to most studies, and the treatment of native process water in a bioreactor has been demonstrated. Amplification of bacterial 16S rRNA genes and sequencing using Ion Torrent sequencing characterized the reactors' biofilm populations and found as many as 235 and 198 distinct genera in the first and second bioreactor, respectively, with significant populations of ammonium- and nitrite-oxidizers. Copyright © 2014 Elsevier Ltd. All rights reserved.

Biodegradation and detoxification of naphthenic acids in oil sands process affected waters.

PubMed

Yue, Siqing; Ramsay, Bruce A; Wang, Jiaxi; Ramsay, Juliana A

2016-12-01

After oil sands process affected water (OSPW) was treated in a continuous flow biofilm reactor, about 40% of the organic compounds in the acid extractable fraction (AEF) including naphthenic acids (NAs) were degraded resulting in a reduction of 73% in the Microtox acute toxicity and of 22% in the yeast estrogenic assay. Using effect directed analysis, treated and untreated OSPW were fractionated by solid phase extraction and the fractions with the largest decrease in toxicity and estrogenicity were selected for analysis by electrospray ionization combined with linear ion trap and a high-resolution Orbitrap mass spectrometer (negative ion mode). The aim of this study was to determine whether compositional changes between the untreated and treated fractions provide insight related to biodegradation and detoxification of NAs. The O2S, O3S and O4S compounds were either not major contributors of toxicity or estrogenicity or the more toxic or estrogenic ones were biodegraded. The O3- and O4-NAs seem to be more readily metabolized than O2NAs and their degradation would contribute to detoxification. The decrease in acute toxicity may be associated with the degradation of C12 and C13 bicyclic and C12-C14 tricyclic NAs while the decrease in estrogenicity may be linked to the degradation of C16 O2-NAs with double bond equivalents (DBE)=5 and 6, C16 and 17 O2-NAs with DBE=7, and C19-O2-NAs with DBE=8. The residual acute toxicity may be caused by recalcitrant components and/or degradation products such as the O2 bicyclic and tricyclic NAs, particularly the C14 and C15 bicyclic and C14-C16 tricyclic NAs as well as the polycyclic aromatic NAs (DBE≥5 compounds). The decrease in estrogenicity may be linked to the degradation of the O3 and O4 oxidized NAs while much of the residual estrogenicity may be due to the recalcitrant polycyclic aromatic O2-NAs. Hence, treatment to further detoxify OSPW should target these compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

Impact of temperature, pH, and salinity changes on the physico-chemical properties of model naphthenic acids.

PubMed

Celsie, Alena; Parnis, J Mark; Mackay, Donald

2016-03-01

The effects of temperature, pH, and salinity change on naphthenic acids (NAs) present in oil-sands process wastewater were modeled for 55 representative NAs. COSMO-RS was used to estimate octanol-water (KOW) and octanol-air (KOA) partition ratios and Henry's law constants (H). Validation with experimental carboxylic acid data yielded log KOW and log H RMS errors of 0.45 and 0.55 respectively. Calculations of log KOW, (or log D, for pH-dependence), log KOA and log H (or log HD, for pH-dependence) were made for model NAs between -20 °C and 40 °C, pH between 0 and 14, and salinity between 0 and 3 g NaCl L(-1). Temperature increase by 60 °C resulted in 3-5 log unit increase in H and a similar magnitude decrease in KOA. pH increase above the NA pKa resulted in a dramatic decrease in both log D and log HD. Salinity increase over the 0-3 g NaCl L(-1) range resulted in a 0.3 log unit increase on average for KOW and H values. Log KOW values of the sodium salt and anion of the conjugate base were also estimated to examine their potential for contribution to the overall partitioning of NAs. Sodium salts and anions of naphthenic acids are predicted to have on average 4 log units and 6 log units lower log KOW values, respectively, with respect to the corresponding neutral NA. Partitioning properties are profoundly influenced by the by the relative prevailing pH and the substance's pKa at the relevant temperature. Copyright © 2015 Elsevier Ltd. All rights reserved.

Biodegradation of a surrogate naphthenic acid under denitrifying conditions.

PubMed

Gunawan, Yetty; Nemati, Mehdi; Dalai, Ajay

2014-03-15

Extraction of bitumen from the shallow oil sands generates extremely large volumes of waters contaminated by naphthenic acid which pose severe environmental and ecological risks. Aerobic biodegradation of NA in properly designed bioreactors has been investigated in our earlier works. In the present work, anoxic biodegradation of trans-4-methyl-1-cyclohexane carboxylic acid (trans-4MCHCA) coupled to denitrification was investigated as a potential ex situ approach for the treatment of oil sand process waters in bioreactors whereby excessive aeration cost could be eliminated, or as an in situ alternative for the treatment of these waters in anoxic stabilization ponds amended with nitrate. Using batch and continuous reactors (CSTR and biofilm), effects of NA concentration (100-750mgL(-1)), NA loading rate (up to 2607.9mgL(-1)h(-1)) and temperature (10-35°C) on biodegradation and denitrification processes were evaluated. In the batch system biodegradation of trans-4MCHCA coupled to denitrification occurred even at the highest concentration of 750mgL(-1). Consistent with the patterns reported for aerobic biodegradation, increase in initial concentration of NA led to higher biodegradation and denitrification rates and the optimum temperature was determined as 23-24°C. In the CSTR, NA removal and nitrate reduction rates passed through a maximum due to increases in NA loading rate. NA loading rate of 157.8mgL(-1)h(-1) at which maximum anoxic NA and nitrate removal rates (105.3mgL(-1)h(-1) and 144.5mgL(-1)h(-1), respectively) occurred was much higher than those reported for the aerobic alternative (NA loading and removal rates: 14.2 and 9.6mgL(-1)h(-1), respectively). In the anoxic biofilm reactor removal rates of NA and nitrate were dependent on NA loading rate in a linear fashion for the entire range of applied loading rates. The highest loading and removal rates for NA were 2607.9 and 2028.1mgL(-1)h(-1), respectively which were at least twofold higher than the values

Determination of thermodynamic and transport parameters of naphthenic acids and organic process chemicals in oil sand tailings pond water.

PubMed

Wang, Xiaomeng; Robinson, Lisa; Wen, Qing; Kasperski, Kim L

2013-07-01

Oil sand tailings pond water contains naphthenic acids and process chemicals (e.g., alkyl sulphates, quaternary ammonium compounds, and alkylphenol ethoxylates). These chemicals are toxic and can seep through the foundation of the tailings pond to the subsurface, potentially affecting the quality of groundwater. As a result, it is important to measure the thermodynamic and transport parameters of these chemicals in order to study the transport behavior of contaminants through the foundation as well as underground. In this study, batch adsorption studies and column experiments were performed. It was found that the transport parameters of these chemicals are related to their molecular structures and other properties. The computer program (CXTFIT) was used to further evaluate the transport process in the column experiments. The results from this study show that the transport of naphthenic acids in a glass column is an equilibrium process while the transport of process chemicals seems to be a non-equilibrium process. At the end of this paper we present a real-world case study in which the transport of the contaminants through the foundation of an external tailings pond is calculated using the lab-measured data. The results show that long-term groundwater monitoring of contaminant transport at the oil sand mining site may be necessary to avoid chemicals from reaching any nearby receptors.

A novel solid-state fractionation of naphthenic acid fraction components from oil sands process-affected water.

PubMed

Mohamed, Mohamed H; Wilson, Lee D; Shah, Jaimin R; Bailey, Jon; Peru, Kerry M; Headley, John V

2015-10-01

Various sorbent materials were evaluated for the fractionation of naphthenic acid fraction components (NAFCs) from oil sand process-affected water (OSPW). The solid phase materials include activated carbon (AC), cellulose, iron oxides (magnetite and goethite), polyaniline (PANI) and three types of biochar derived from biomass (BC-1; rice husks, BC-2; acacia low temperature and BC-3; acacia high temperature). NAFCs were semi-quantified using electrospray ionization high resolution Orbitrap mass spectrometry (ESI-MS) and the metals were assessed by inductively coupled plasma optical emission spectrometry (ICP-OES). The average removal efficacy of NAFCs by AC was 95%. The removal efficacy decreased in the following order: AC, BC-1>BC-2, BC-3, goethite>PANI>cellulose, magnetite. The removal of metals did not follow a clear trend; however, there was notable leaching of potassium by AC and biochar samples. The bound NAFCs by AC were desorbed efficiently with methanol. Methanol regeneration and recycling of AC revealed 88% removal on the fourth cycle; a 4.4% decrease from the first cycle. This fractionation method represents a rapid, cost-effective, efficient, and green strategy for NAFCs from OSPW, as compared with conventional solvent extraction. Copyright © 2015 Elsevier Ltd. All rights reserved.

The immunological effects of oil sands surface waters and naphthenic acids on rainbow trout (Oncorhynchus mykiss).

PubMed

Leclair, Liane A; MacDonald, Gillian Z; Phalen, Laura J; Köllner, Bernd; Hogan, Natacha S; van den Heuvel, Michael R

2013-10-15

There is concern surrounding the immunotoxic potential of naphthenic acids (NAs), a major organic constituent in waters influenced by oil sands contamination. To assess the immunological response to NAs, rainbow trout (Oncorhynchus mykiss) waterborne exposures were conducted with oil sands-influenced waters, NAs extracted and purified from oil sands tailings waters, and benzo[a]pyrene (BaP) as a positive control. After a 7d exposure, blood, spleen, head kidney, and gill samples were removed from a subset of fish in order to evaluate the distribution of thrombocytes, B-lymphocytes, myeloid cells, and T-lymphocytes using fluorescent antibodies specific for those cell types coupled with flow cytometry. The remaining trout in each experimental tank were injected with inactivated Aeromonas salmonicida and held in laboratory water for 21 d and subjected to similar lymphatic cell evaluation in addition to evaluation of antibody production. Fluorescent metabolites in bile as well as liver CYP1A induction were also determined after the 7 and 21 d exposure. Oil sands waters and extracted NAs exposures resulted in an increase in bile fluorescence at phenanthrene wavelengths, though liver CYP1A was not induced in those treatments as it was with the BaP positive control. Trout in the oil sands-influenced water exposure showed a decrease in B- and T-lymphocytes in blood as well as B-lymphocytes and myeloid cells in spleen and an increase in B-lymphocytes in head kidney. The extracted NAs exposure showed a decrease in thrombocytes in spleen at 8 mg/L and an increase in T-lymphocytes at 1mg/L in head kidney after 7d. There was a significant decrease in antibody production against A. salmonicida in both oil sands-influenced water exposures. Because oil sands-influenced waters affected multiple immune parameters, while extracted NAs impacts were limited, the NAs tested here are likely not the cause of immunotoxicity found in the oil sands-influenced water. Copyright © 2013 Elsevier

Differences in phytotoxicity and dissipation between ionized and nonionized oil sands naphthenic acids in wetland plants.

PubMed

Armstrong, Sarah A; Headley, John V; Peru, Kerry M; Germida, James J

2009-10-01

Naphthenic acids (NAs) are composed of alkyl-substituted acyclic and cycloaliphatic carboxylic acids and, because they are acutely toxic to fish, are of toxicological concern. During the caustic hot-water extraction of oil from the bitumen in oil sands deposits, NAs become concentrated in the resulting tailings pond water. The present study investigated if dissipation of NAs occurs in the presence of hydroponically grown emergent macrophytes (Typha latifolia, Phragmites australis, and Scirpus acutus) to determine the potential for phytoremediation of these compounds. Plants were grown with oil sands NAs (pKa approximately 5-6) in medium at pH 7.8 (predominantly ionized NAs) and pH 5.0 (predominantly nonionized NAs) to determine if, by altering their chemical form, NAs may be more accessible to plants and, thus, undergo increased dissipation. Whereas the oil sands NA mixture in its nonionized form was more toxic to wetland plants than its ionized form, neither form appeared to be sequestered by wetland plants. The present study demonstrated that plants may selectively enhance the dissipation of individual nonionized NA compounds, which contributes to toxicity reduction but does not translate into detectable total NA dissipation within experimental error and natural variation. Plants were able to reduce the toxicity of a NA system over 30 d, increasing the median lethal concentration (LC50; % of hydroponic solution) of the medium for Daphnia magna by 23.3% +/- 8.1% (mean +/- standard error; nonionized NAs) and 37.0% +/- 2.7% (ionized NAs) as determined by acute toxicity bioassays. This reduction in toxicity was 7.3% +/- 2.6% (nonionized NAs) and 45.0% +/- 6.8% (ionized NAs) greater than that in unplanted systems.

Kinetics study on the degradation of a model naphthenic acid by ethylenediamine-N,N'-disuccinic acid-modified Fenton process.

PubMed

Zhang, Ying; Klamerth, Nikolaus; Messele, Selamawit Ashagre; Chelme-Ayala, Pamela; Gamal El-Din, Mohamed

2016-11-15

Naphthenic acids (NAs) are reported to be the main species responsible for the oil sands process-affected water (OSPW) toxicity. In this study, the degradation of cyclohexanoic acid (CHA) as a model compound for NAs by an ethylenediamine-N,N'-disuccinic acid (EDDS)-modified Fenton process was investigated at pH 8. Optimum dose for Fe-EDDS (EDDS:Fe=2:1) was 0.45mM, and 2.94mM for hydrogen peroxide (H2O2). The time profiles of the main species in the process were studied, including CHA, H2O2, Fe(II), total Fe, and Fe-EDDS (in the main form of Fe(III)EDDS). The second-order rate constant between EDDS and hydroxyl radical (OH) at pH 8 was obtained as 2.48±0.43×10(9)M(-1)s(-1). OH was proved to be the main species responsible for the CHA degradation, while superoxide radical (O2(-)) played a minor role. The consecutive addition of H2O2 and Fe-EDDS led to a higher removal of CHA compared to that achieved by adding the reagents at a time. The half-wave potential of Fe(III/II)EDDS was measured at pH 7-9. The EDDS-modified Fenton process is a promising alternative to degrade NAs. Copyright © 2016 Elsevier B.V. All rights reserved.

The effect of oil sands process-affected water and model naphthenic acids on photosynthesis and growth in Emiliania huxleyi and Chlorella vulgaris.

PubMed

Beddow, Jessica; Johnson, Richard J; Lawson, Tracy; Breckels, Mark N; Webster, Richard J; Smith, Ben E; Rowland, Steven J; Whitby, Corinne

2016-02-01

Naphthenic acids (NAs) are among the most toxic organic pollutants present in oil sands process waters (OSPW) and enter marine and freshwater environments through natural and anthropogenic sources. We investigated the effects of the acid extractable organic (AEO) fraction of OSPW and individual surrogate NAs, on maximum photosynthetic efficiency of photosystem II (PSII) (FV/FM) and cell growth in Emiliania huxleyi and Chlorella vulgaris as representative marine and freshwater phytoplankton. Whilst FV/FM in E. huxleyi and C. vulgaris was not inhibited by AEO, exposure to two surrogate NAs: (4'-n-butylphenyl)-4-butanoic acid (n-BPBA) and (4'-tert-butylphenyl)-4-butanoic acid (tert-BPBA), caused complete inhibition of FV/FM in E. huxleyi (≥10 mg L(-1)n-BPBA; ≥50 mg L(-1)tert-BPBA) but not in C. vulgaris. Growth rates and cell abundances in E. huxleyi were also reduced when exposed to ≥10 mg L(-1)n- and tert-BPBA; however, higher concentrations of n- and tert-BPBA (100 mg L(-1)) were required to reduce cell growth in C. vulgaris. AEO at ≥10 mg L(-1) stimulated E. huxleyi growth rate (p ≤ 0.002), yet had no apparent effect on C. vulgaris. In conclusion, E. huxleyi was generally more sensitive to NAs than C. vulgaris. This report provides a better understanding of the physiological responses of phytoplankton to NAs which will enable improved monitoring of NA pollution in aquatic ecosystems in the future. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

Electrospray ionization mass spectrometry of the photodegradation of naphthenic acids mixtures irradiated with titanium dioxide.

PubMed

Headley, John V; Du, Jing-Long; Peru, Kerry M; McMartin, Dena W

2009-05-01

Electrospray ionization mass spectrometry was used to study the photodegradation of an oil sands naphthenic acid (NA) mixture, a commercial Fluka NA mixture and a candidate NA, 4-Methyl-cyclohexaneaceticic acid (4-MCHAA) irradiated with TiO(2) (P25) suspension under both fluorescent and natural sunlight. Under natural sunlight irradiation over the TiO(2) suspension, approximately 75% of compounds in the NA mixtures and 100% of 4-MCHAA were degraded in 8 h. No degradation was observed under dark conditions, regardless of the presence or absence of TiO(2). The structural formula of the NAs is given by C(n)H(2n + z)O(2), where n represents the carbon number and z specifies a homologous family with 0-6 rings (z = 0 to -12). The degree of degradation was noted to vary among the NA mixtures and the candidate NA compound with more efficient degradation achieved for molecules with -z values from 0 to 6. The difference in the efficacy of the photocatalysis was likely due to the structure and size of the compounds. In the case of -z = 6 to 12, steric constraints are a key factor what hinders photocatalysis.

Removal and toxicity reduction of naphthenic acids by ozonation and combined ozonation-aerobic biodegradation.

PubMed

Vaiopoulou, Eleni; Misiti, Teresa M; Pavlostathis, Spyros G

2015-03-01

A commercial naphthenic acids (NAs) mixture (TCI Chemicals) and five model NA compounds were ozonated in a semibatch mode. Ozonation of 25 and 35 mg/L NA mixture followed pseudo first-order kinetics (k(obs)=0.11±0.008 min(-1); r(2)=0.989) with a residual NAs concentration of about 5 mg/L. Ozone reacted preferentially with NAs of higher cyclicity and molecular weight and decreased both cyclicity and the acute Microtox® toxicity by 3.3-fold. The ozone reactivity with acyclic and monocyclic model NAs varied and depended on other structural features, such as branching and the presence of tertiary or quaternary carbons. Batch aerobic degradation of unozonated NA mixture using a NA-enriched culture resulted in 83% NA removal and a 6.7-fold decrease in toxicity, whereas a combination of ozonation-biodegradation resulted in 89% NA removal and a 15-fold decrease in toxicity. Thus, ozonation of NA-bearing waste streams coupled with biodegradation are effective treatment processes. Copyright © 2014 Elsevier Ltd. All rights reserved.

Microbial biodegradation of aromatic alkanoic naphthenic acids is affected by the degree of alkyl side chain branching

PubMed Central

Johnson, Richard J; Smith, Ben E; Sutton, Paul A; McGenity, Terry J; Rowland, Steven J; Whitby, Corinne

2011-01-01

Naphthenic acids (NAs) occur naturally in oil sands and enter the environment through natural and anthropogenic processes. NAs comprise toxic carboxylic acids that are difficult to degrade. Information on NA biodegradation mechanisms is limited, and there are no studies on alkyl branched aromatic alkanoic acid biodegradation, despite their contribution to NA toxicity and recalcitrance. Increased alkyl side chain branching has been proposed to explain NA recalcitrance. Using soil enrichments, we examined the biodegradation of four aromatic alkanoic acid isomers that differed in alkyl side chain branching: (4′-n-butylphenyl)-4-butanoic acid (n-BPBA, least branched); (4′-iso-butylphenyl)-4-butanoic acid (iso-BPBA); (4′-sec-butylphenyl)-4-butanoic acid (sec-BPBA) and (4′-tert-butylphenyl)-4-butanoic acid (tert-BPBA, most branched). n-BPBA was completely metabolized within 49 days. Mass spectral analysis confirmed that the more branched isomers iso-, sec- and tert-BPBA were transformed to their butylphenylethanoic acid (BPEA) counterparts at 14 days. The BPEA metabolites were generally less toxic than BPBAs as determined by Microtox assay. n-BPEA was further transformed to a diacid, showing that carboxylation of the alkyl side chain occurred. In each case, biodegradation of the carboxyl side chain proceeded through beta-oxidation, which depended on the degree of alkyl side chain branching, and a BPBA degradation pathway is proposed. Comparison of 16S rRNA gene sequences at days 0 and 49 showed an increase and high abundance at day 49 of Pseudomonas (sec-BPBA), Burkholderia (n-, iso-, tert-BPBA) and Sphingomonas (n-, sec-BPBA). PMID:20962873

Removal of dicyclohexyl acetic acid from aqueous solution using ultrasound, ozone and their combination.

PubMed

Kumar, Pardeep; Headley, John; Peru, Kerry; Bailey, Jon; Dalai, Ajay

2014-01-01

Naphthenic acids are a complex mixture of organic components, some of which include saturated alkyl-substituted cycloaliphatic carboxylic acids and acyclic aliphatic acids. They are naturally found in hydrocarbon deposits like oil sand, petroleum, bitumen and crude oil. In this study, the oxidation of a relatively high molecular weight naphthenic acid (Dicyclohexyl acetic acid) was investigated using ozonation, ultrasonication and hydrogen peroxide alone and their combinations. Effects on oxidation of dicyclohexyl acetic acid (DAA) were measured for different concentrations of ozone ranging between 0.7 to 3.3 mg L(-1) and pH in the range 6 to 10. Ultrasonication and hydrogen peroxide alone were not effective to oxidize dicyclohexyl acetic acid, but combining ultrasonication with H2O2 had a significant effect on oxidation of dicyclohexyl acetic acid with maximum removal reaching to 84 ± 2.2% with 81 ± 2.1% reduction in chemical oxygen demand (COD). Synergistic effects were observed for combining ultrasonication with ozonation and resulted in 100% DAA removal with 98 ± 0.8% reduction in COD within 15 min at 3.3 mg L(-1) ozone concentration and 130 Watts ultrasonication power. The reaction conditions obtained for the maximum oxidation of DAA and COD removal were used for the degradation of naphthenic acids mixture extracted from oil sands process water (OSPW). The percentage oxidation of NAs mixture extracted from OSPW was 89.3 ± 1.1% in ozonation and combined ozonation and ultrasonication, but COD removal observed was 65 ± 1.2% and 78 ± 1.4% for ozonation and combined ozonation and ultrasonication treatments, respectively.

Influence of commercial (Fluka) naphthenic acids on acid volatile sulfide (AVS) production and divalent metal precipitation.

PubMed

McQueen, Andrew D; Kinley, Ciera M; Rodgers, John H; Friesen, Vanessa; Bergsveinson, Jordyn; Haakensen, Monique C

2016-12-01

Energy-derived waters containing naphthenic acids (NAs) are complex mixtures often comprising a suite of potentially problematic constituents (e.g. organics, metals, and metalloids) that need treatment prior to beneficial use, including release to receiving aquatic systems. It has previously been suggested that NAs can have biostatic or biocidal properties that could inhibit microbially driven processes (e.g. dissimilatory sulfate reduction) used to transfer or transform metals in passive treatment systems (i.e. constructed wetlands). The overall objective of this study was to measure the effects of a commercially available (Fluka) NA on sulfate-reducing bacteria (SRB), production of sulfides (as acid-volatile sulfides [AVS]), and precipitation of divalent metals (i.e. Cu, Ni, Zn). These endpoints were assessed following 21-d aqueous exposures of NAs using bench-scale reactors. After 21-days, AVS molar concentrations were not statistically different (p<0.0001; α=0.05) among NA treatments (10, 20, 40, 60, and 80mg NA/L) and an untreated control (no NAs). Extent of AVS production was sufficient in all NA treatments to achieve ∑SEM:AVS <1, indicating that conditions were conducive for treatment of metals, with sulfide ligands in excess of SEM (Cu, Ni, and Zn). In addition, no adverse effects to SRB (in terms of density, relative abundance, and diversity) were measured following exposures of a commercial NA. In this bench-scale study, dissimilatory sulfate reduction and subsequent metal precipitation were not vulnerable to NAs, indicating passive treatment systems utilizing sulfide production (AVS) could be used to treat metals occurring in NAs affected waters. Copyright © 2016 Elsevier Inc. All rights reserved.

Estimating the in situ biodegradation of naphthenic acids in oil sands process waters by HPLC/HRMS.

PubMed

Han, Xiumei; MacKinnon, Michael D; Martin, Jonathan W

2009-06-01

The oil sands industry in Northern Alberta produces large volumes of oil sands process water (OSPW) containing high concentrations of persistent naphthenic acids (NAs; C(n)H(2n+Z)O(2)). Due to the growing volumes of OSPW that need to be reclaimed, it is important to understand the fate of NAs in aquatic systems. A recent laboratory study revealed several potential markers of microbial biodegradation for NAs; thus here we examined for these signatures in field-aged OSPW on the site of Syncrude Canada Ltd. (Fort McMurray, AB). NA concentrations were lower in older OSPW; however parent NA signatures were remarkably similar among all OSPW samples examined, with no discernible enrichment of the highly cyclic fraction as was observed in the laboratory. Comparison of NA signatures in fresh oil sands ore extracts to OSPW in active settling basins, however, suggested that the least cyclic fraction (i.e. Z=0 and Z=-2 homologues) may undergo relatively rapid biodegradation in active settling basins. Further evidence for biodegradation of NAs came from a significantly higher proportion of oxidized NAs (i.e. C(n)H(2n+Z)O(3)+C(n)H(2n+Z)O(4)) in the oldest OSPW from experimental reclamation ponds. Taken together, there is indirect evidence for rapid biodegradation of relatively labile Z=0 and Z=-2 NAs in active settling basins, but the remaining steady-state fraction of NAs in OSPW appear to be very recalcitrant, with half-lives on the order of 12.8-13.6 years. Alternative fate mechanisms to explain the slow disappearance of parent NAs from OSPW are discussed, including adsorption and atmospheric partitioning.

Electrochemical mineralization and detoxification of naphthenic acids on boron-doped diamond anodes.

PubMed

Diban, Nazely; Urtiaga, Ane

2018-01-05

Electrochemical oxidation (ELOX) with boron-doped diamond (BDD) anodes was successfully applied to degrade a model aqueous solution of a mixture of commercial naphthenic acids (NAs). The model mixture was prepared resembling the NA and salt composition of oil sands process-affected water (OSPW) as described in the literature. The initial concentration of NAs between 70 and 120 mg/L did not influence the electrooxidation kinetics. However, increasing the applied current density from 20 to 100 A/m 2 and the initial chloride concentration from 15 to 70 and 150 mg/L accelerated the rate of NA degradation. At higher chloride concentration, the formation of indirect oxidative species could contribute to the faster oxidation of NAs. Complete chemical oxygen demand removal at an initial NA concentration of 120 mg/L, 70 mg/L of chloride and applied 50 A/m 2 of current density was achieved, and 85% mineralization, defined as the decrease of the total organic carbon (TOC) content, was attained. Moreover, after 6 h of treatment and independently on the experimental conditions, the formation of more toxic species, i.e. perchlorate and organochlorinated compounds, was not detected. Finally, the use of ELOX with BDD anodes produced a 7 to 11-fold reduction of toxicity (IC 50 towards Vibrio fischeri) after 2 h of treatment.

Mechanistic investigation of industrial wastewater naphthenic acids removal using granular activated carbon (GAC) biofilm based processes.

PubMed

Islam, Md Shahinoor; Zhang, Yanyan; McPhedran, Kerry N; Liu, Yang; Gamal El-Din, Mohamed

2016-01-15

Naphthenic acids (NAs) found in oil sands process-affected waters (OSPW) have known environmental toxicity and are resistant to conventional wastewater treatments. The granular activated carbon (GAC) biofilm treatment process has been shown to effectively treat OSPW NAs via combined adsorption/biodegradation processes despite the lack of research investigating their individual contributions. Presently, the NAs removals due to the individual processes of adsorption and biodegradation in OSPW bioreactors were determined using sodium azide to inhibit biodegradation. For raw OSPW, after 28 days biodegradation and adsorption contributed 14% and 63% of NA removal, respectively. For ozonated OSPW, biodegradation removed 18% of NAs while adsorption reduced NAs by 73%. Microbial community 454-pyrosequencing of bioreactor matrices indicated the importance of biodegradation given the diverse carbon degrading families including Acidobacteriaceae, Ectothiorhodospiraceae, and Comamonadaceae. Overall, results highlight the ability to determine specific processes of NAs removals in the combined treatment process in the presence of diverse bacteria metabolic groups found in GAC bioreactors. Copyright © 2015 Elsevier B.V. All rights reserved.

Role of Naphthenic Acids in Controlling Self-Aggregation of a Polyaromatic Compound in Toluene.

PubMed

Teklebrhan, Robel B; Jian, Cuiying; Choi, Phillip; Xu, Zhenghe; Sjöblom, Johan

2016-04-14

In this work, a series of molecular dynamics simulations were performed to investigate the effect of naphthenic acids (NAs) in early stage self-assembly of polyaromatic (PA) molecules in toluene. By exploiting NA molecules of the same polar functional group but different aliphatic/cycloaliphatic nonpolar tails, it was found that irrespective of the presence of the NA molecules in the system, the dominant mode of π-π stacking is a twisted, offset parallel stacking of a slightly larger overlapping area. Unlike large NA molecules, the presence of small NA molecules enhanced the number of π-π stacked PA molecules by suppressing the hydrogen bonding interactions among the PA molecules. Smaller NA molecules were found to have a higher tendency to associate with PA molecules than larger NA molecules. Moreover, the size and distribution of π-π stacking structures were affected to different degrees by changing the size and structural features of the NA molecules in the system. It was further revealed that the association between NA and PA molecules, mainly through hydrogen bonding, creates a favorable local environment for the overlap of PA cores (i.e., π-π stacking growth) by depressing the hydrogen bonding between PA molecules, which results in the removal of some toluene molecules from the vicinity of the PA molecules.

Quantitative and qualitative analysis of naphthenic acids in natural waters surrounding the Canadian oil sands industry.

PubMed

Ross, Matthew S; Pereira, Alberto dos Santos; Fennell, Jon; Davies, Martin; Johnson, James; Sliva, Lucie; Martin, Jonathan W

2012-12-04

The Canadian oil sands industry stores toxic oil sands process-affected water (OSPW) in large tailings ponds adjacent to the Athabasca River or its tributaries, raising concerns over potential seepage. Naphthenic acids (NAs; C(n)H(2n-Z)O(2)) are toxic components of OSPW, but are also natural components of bitumen and regional groundwaters, and may enter surface waters through anthropogenic or natural sources. This study used a selective high-resolution mass spectrometry method to examine total NA concentrations and NA profiles in OSPW (n = 2), Athabasca River pore water (n = 6, representing groundwater contributions) and surface waters (n = 58) from the Lower Athabasca Region. NA concentrations in surface water (< 2-80.8 μg/L) were 100-fold lower than previously estimated. Principal components analysis (PCA) distinguished sample types based on NA profile, and correlations to water quality variables identified two sources of NAs: natural fatty acids, and bitumen-derived NAs. Analysis of NA data with water quality variables highlighted two tributaries to the Athabasca River-Beaver River and McLean Creek-as possibly receiving OSPW seepage. This study is the first comprehensive analysis of NA profiles in surface waters of the region, and demonstrates the need for highly selective analytical methods for source identification and in monitoring for potential effects of development on ambient water quality.

Petroleomic analysis of the treatment of naphthenic organics in oil sands process-affected water with buoyant photocatalysts.

PubMed

Leshuk, Tim; Peru, Kerry M; de Oliveira Livera, Diogo; Tripp, Austin; Bardo, Patrick; Headley, John V; Gu, Frank

2018-05-10

The persistence of toxicity associated with the soluble naphthenic organic compounds (NOCs) of oil sands process-affected water (OSPW) implies that a treatment solution may be necessary to enable safe return of this water to the environment. Due to recent advances in high-resolution mass spectrometry (HRMS), the majority of the toxicity of OSPW is currently understood to derive from a subset of toxic classes, comprising only a minority of the total NOCs. Herein, oxidative treatment of OSPW with buoyant photocatalysts was evaluated under a petroleomics paradigm: chemical changes across acid-, base- and neutral-extractable organic fractions were tracked throughout the treatment with both positive and negative ion mode electrospray ionization (ESI) Orbitrap MS. Elimination of detected OS + and NO + classes of concern in the earliest stages of the treatment, along with preferential degradation of high carbon-numbered O 2 - acids, suggest that photocatalysis may detoxify OSPW with higher efficiency than previously thought. Application of petroleomic level analysis offers unprecedented insights into the treatment of petroleum impacted water, allowing reaction trends to be followed across multiple fractions and thousands of compounds simultaneously. Copyright © 2018 Elsevier Ltd. All rights reserved.

Preparation of activated petroleum coke for removal of naphthenic acids model compounds: Box-Behnken design optimization of KOH activation process.

PubMed

Niasar, Hojatallah Seyedy; Li, Hanning; Das, Sreejon; Kasanneni, Tirumala Venkateswara Rao; Ray, Madhumita B; Xu, Chunbao Charles

2018-04-01

This study employed Box-Behnken design and response surface methodology to optimize activation parameters for the production of activated petroleum coke (APC) adsorbent from petroleum coke (PC) to achieve highest adsorption capacity for three model naphthenic acids. Activated petroleum coke (APC) adsorbent with a BET surface area of 1726 m 2 /g and total pore volume of 0.85 cc/g was produced at the optimum activation conditions (KOH/coke mass ratio) of 3.0, activation temperature 790 °C, and activation time 3.47 h). Effects of the activation parameters on the adsorption pefromances (adsortion capaciy and kinetics) were investigated. With the APC obtained at the optimum activation condition, the maximum adsorption capacity of 451, 362, and 320 (mg/g) was achieved for 2-naphthoic acid, diphenylacetic acid and cyclohexanepentanoic acid (CP), respectively. Although, generally APC adsorbents with a higher specific surface area and pore volume provide better adsorption capacity, the textural properties (surface areas and pore volume) are not the only parameters determining the APC adsorbents' adsorption capacity. Other parameters such as surface functionalities play effective roles on the adsorption capacity of the produced APC adsorbents for NAs. The KOH activation process, in particular the acid washing step, distinctly reduced the sulfur and metals contents in the raw PC, decreasing the leaching potential of metals from APC adsorbents during adsorption. Copyright © 2018 Elsevier Ltd. All rights reserved.

Fate and effect of naphthenic acids on oil refinery activated sludge wastewater treatment systems.

PubMed

Misiti, Teresa; Tezel, Ulas; Pavlostathis, Spyros G

2013-01-01

Naphthenic acids (NAs) are a complex group of alkyl-substituted acyclic, monocyclic and polycyclic carboxylic acids present in oil sands process waters, crude oil, refinery wastewater and petroleum products. Crude oil, desalter brine, influent, activated sludge mixed liquor and effluent refinery samples were received from six United States refineries. The total acid number (TAN) of the six crudes tested ranged from 0.12 to 1.5 mg KOH/g crude oil and correlated to the total NA concentration in the crudes. The total NA concentration in the desalter brine, influent, activated sludge mixed liquor and effluent samples ranged from 4.2 to 40.4, 4.5 to 16.6, 9.6 to 140.3 and 2.8 to 11.6 mg NA/L, respectively. The NAs in all wastewater streams accounted for less than 16% of the total COD, indicating that many other organic compounds are present and that NAs are a minor component in refinery wastewaters. Susceptibility tests showed that none of the activated sludge heterotrophic microcosms was completely inhibited by NAs up to 400 mg/L. Growth inhibition ranging from 10 to 59% was observed in all microcosms at and above 100 mg NA/L. NAs chronically-sorbed to activated sludge mixed liquor biomass and powdered activated carbon (PAC) were recalcitrant and persistent. More than 80% of the total NAs remained in the solid phase at the end of the 10-day desorption period (five successive desorption steps). Throughout a 90-day incubation period, the total NA concentration decreased by 33 and 51% in PAC-free and PAC-containing mixed liquor microcosms, respectively. The lower molecular weight fraction of NAs was preferentially degraded in both mixed liquors. The persistence of the residual, higher molecular weight NAs is likely a combination of molecular recalcitrance and decreased bioavailability when chronically-sorbed to the biomass and/or PAC. Copyright © 2012 Elsevier Ltd. All rights reserved.

Physiological effects and tissue residues from exposure of leopard frogs to commercial naphthenic acids.

PubMed

Smits, Judit E G; Hersikorn, Blair D; Young, Rozlyn F; Fedorak, Phillip M

2012-10-15

Naphthenic acids (NAs) have been cited as one of the main causes of the toxicity related to oil sands process-affected materials and have recently been measured in biological tissues (fish). However, adverse effects have not been a consistent finding in toxicology studies on vertebrates. This study set out to determine two factors: 1) whether exposure to commercial NAs (Refined Merichem) resulted in detectable tissue residues in native amphibians (northern leopard frogs, Lithobates pipiens), and 2) whether such exposure would produce clinical or subclinical toxicity. Frogs were kept in NA solutions (0, 20, or 40 mg/L) under saline conditions comparable to that on reclaimed wetlands in the Athabasca oil sands for 28 days. These exposures resulted in proportional NA concentrations in muscle tissue of the frogs, estimated by gas chromatography-mass spectrometry analyses. Detailed studies determined if the increasing concentrations of NAs, and subsequently increased tissue NA levels, caused a proportional compromise in the health of the experimental animals. Physiological investigations included innate immune function, thyroid hormone levels, and hepatic detoxification enzyme induction, none of which differed in response to increased exposures or tissue concentrations of NAs. Body mass did increase in both the salt- and NA-exposed animals, likely related to osmotic pressure and uptake of water through the skin. Our results demonstrate that commercial NAs are absorbed and deposited in muscle tissue, yet they show few negative physiological or toxicological effects on the frogs. Copyright © 2012. Published by Elsevier B.V.

The effect of naphthenic acids on physiological characteristics of the microalgae Phaeodactylum tricornutum and Platymonas helgolandica var. tsingtaoensis.

PubMed

Zhang, Huanxin; Tang, Xuexi; Shang, Jiagen; Zhao, Xinyu; Qu, Tongfei; Wang, Ying

2018-05-11

Naphthenic acids (NAs) account for 1-2% of crude oil and represent its main acidic component. However, the aquatoxic effects of NAs on marine phytoplankton and their ecological risks have remained largely unknown. Using the marine microalgae Phaeodactylum tricornutum and Platymonas helgolandica var. tsingtaoensis as the target, we studied the effects of NAs on their growth, cell morphology and physiological characteristics. The cell density decreased as the concentrations of NAs increased, indicating that they had an adverse effect on growth of the investigated algae in a concentration-dependent manner. Moreover, scanning electron microscopy revealed NAs exposure caused damage such as deformed cells, shrunken surface and ruptured cell structures. Exposure to NAs at higher concentrations for 48 h significantly increased the content of chlorophyll (Chl) a and b in P. tricornutum, but decreased their levels in P. helgolandica var. tsingtaoensis. NAs with concentrations no higher than 4 mg/L gradually enhanced the Chl fluorescence (ChlF) parameters and decreased the ChlF parameters at higher concentrations for the two marine microalgae. Additionally, NAs induced hormesis on photosynthetic efficiency of the two microalgae and also have the species difference in their aquatic toxicity. Overall, the results of this study provide a better understanding of the physiological responses of phytoplankton and will enable better risk assessments of NAs. Copyright © 2018 Elsevier Ltd. All rights reserved.

Effects of environmental conditions on aerobic degradation of a commercial naphthenic acid.

PubMed

Kinley, Ciera M; Gaspari, Daniel P; McQueen, Andrew D; Rodgers, John H; Castle, James W; Friesen, Vanessa; Haakensen, Monique

2016-10-01

Naphthenic acids (NAs) are problematic constituents in energy-derived waters, and aerobic degradation may provide a strategy for mitigating risks to aquatic organisms. The overall objective of this study was to determine the influence of concentrations of N (as ammonia) and P (as phosphate), and DO, as well as pH and temperatures on degradation of a commercial NA in bench-scale reactors. Commercial NAs provided replicable compounds necessary to compare influences of environmental conditions on degradation. NAs were quantified using high performance liquid chromatography. Microbial diversity and relative abundance were measured in treatments as explanatory parameters for potential effects of environmental conditions on microbial populations to support analytically measured NA degradation. Environmental conditions that positively influenced degradation rates of Fluka NAs included nutrients (C:N 10:1-500:1, C:P 100:1-5000:1), DO (4.76-8.43 mg L(-1)), pH (6-8), and temperature (5-25 °C). Approximately 50% removal of 61 ± 8 mg L(-1) was achieved in less than 2 d after NA introduction, achieving the method detection limit (5 mg L(-1)) by day 6 of the experiment in treatments with a C:N:P ratio of 100:10:1, DO > 8 mg L(-1), pH ∼8-9, and temperatures >23 °C. Microbial diversity was lowest in lower temperature treatments (6-16 °C), which may have resulted in observed slower NA degradation. Based on results from this study, when macro- and micronutrients were available, DO, pH, and temperature (within environmentally relevant ranges) influenced rates of aerobic degradation of Fluka NAs. This study could serve as a model for systematically evaluating environmental factors that influence NA degradation in field scenarios. Copyright © 2016 Elsevier Ltd. All rights reserved.

Enhanced characterization of oil sands acid-extractable organics fractions using electrospray ionization-high-resolution mass spectrometry and synchronous fluorescence spectroscopy.

PubMed

Bauer, Anthony E; Frank, Richard A; Headley, John V; Peru, Kerry M; Hewitt, L Mark; Dixon, D George

2015-05-01

The open pit oil sands mining operations north of Fort McMurray, Alberta, Canada, are accumulating tailings waste at a rate approximately equal to 4.9 million m(3) /d. Naphthenic acids are among the most toxic components within tailings to aquatic life, but structural components have largely remained unidentified. In the present study, electrospray ionization high-resolution mass spectrometry (ESI-HRMS) and synchronous fluorescence spectroscopy (SFS) were used to characterize fractions derived from the distillation of an acid-extractable organics (AEO) mixture isolated from oil sands process-affected water (OSPW). Mean molecular weights of each fraction, and their relative proportions to the whole AEO extract, were as follows: fraction 1: 237 Da, 8.3%; fraction 2: 240 Da, 23.8%; fraction 3: 257 Da, 26.7%; fraction 4: 308 Da, 18.9%; fraction 5: 355 Da, 10.0%. With increasing mean molecular weight of the AEO fractions, a concurrent increase occurred in the relative abundance of nitrogen-, sulfur-, and oxygen-containing ions, double-bond equivalents, and degree of aromaticity. Structures present in the higher-molecular-weight fractions (fraction 4 and fraction 5) suggested the presence of heteroatoms, dicarboxyl and dihydroxy groups, and organic acid compounds with the potential to function as estrogens. Because organic acid compositions become dominated by more recalcitrant, higher-molecular-weight acids during natural degradation, these findings are important in the context of oil sands tailings pond water remediation. © 2015 SETAC.

Beyond Naphthenic Acids: Environmental Screening of Water from Natural Sources and the Athabasca Oil Sands Industry Using Atmospheric Pressure Photoionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry.

PubMed

Barrow, Mark P; Peru, Kerry M; Fahlman, Brian; Hewitt, L Mark; Frank, Richard A; Headley, John V

2015-09-01

There is a growing need for environmental screening of natural waters in the Athabasca region of Alberta, Canada, particularly in the differentiation between anthropogenic and naturally-derived organic compounds associated with weathered bitumen deposits. Previous research has focused primarily upon characterization of naphthenic acids in water samples by negative-ion electrospray ionization methods. Atmospheric pressure photoionization is a much less widely used ionization method, but one that affords the possibility of observing low polarity compounds that cannot be readily observed by electrospray ionization. This study describes the first usage of atmospheric pressure photoionization Fourier transform ion cyclotron resonance mass spectrometry (in both positive-ion and negative-ion modes) to characterize and compare extracts of oil sands process water, river water, and groundwater samples from areas associated with oil sands mining activities. When comparing mass spectra previously obtained by electrospray ionization and data acquired by atmospheric pressure photoionization, there can be a doubling of the number of components detected. In addition to polar compounds that have previously been observed, low-polarity, sulfur-containing compounds and hydrocarbons that do not incorporate a heteroatom were detected. These latter components, which are not amenable to electrospray ionization, have potential for screening efforts within monitoring programs of the oil sands.

Removal and biodegradation of naphthenic acids by biochar and attached environmental biofilms in the presence of co-contaminating metals.

PubMed

Frankel, Mathew L; Bhuiyan, Tazul I; Veksha, Andrei; Demeter, Marc A; Layzell, David B; Helleur, Robert J; Hill, Josephine M; Turner, Raymond J

2016-09-01

This study evaluated the efficacy of using a combined biofilm-biochar approach to remove organic (naphthenic acids (NAs)) and inorganic (metals) contaminants from process water (OSPW) generated by Canada's oil sands mining operations. A microbial community sourced from an OSPW sample was cultured as biofilms on several carbonaceous materials. Two biochar samples, from softwood bark (SB) and Aspen wood (N3), facilitated the most microbial growth (measured by protein assays) and were used for NA removal studies performed with and without biofilms, and in the presence and absence of contaminating metals. Similar NA removal was seen in 6-day sterile N3 and SB assays (>30%), while biodegradation by SB-associated biofilms increased NA removal to 87% in the presence of metals. Metal sorption was also observed, with up to four times more immobilization of Fe, Al, and As on biofilm-associated biochar. These results suggest this combined approach may be a promising treatment for OSPW. Copyright © 2016 The Author(s). Published by Elsevier Ltd.. All rights reserved.

Aerobic Growth of Rhodococcus aetherivorans BCP1 Using Selected Naphthenic Acids as the Sole Carbon and Energy Sources

PubMed Central

Presentato, Alessandro; Cappelletti, Martina; Sansone, Anna; Ferreri, Carla; Piacenza, Elena; Demeter, Marc A.; Crognale, Silvia; Petruccioli, Maurizio; Milazzo, Giorgio; Fedi, Stefano; Steinbüchel, Alexander; Turner, Raymond J.; Zannoni, Davide

2018-01-01

Naphthenic acids (NAs) are an important group of toxic organic compounds naturally occurring in hydrocarbon deposits. This work shows that Rhodococcus aetherivorans BCP1 cells not only utilize a mixture of eight different NAs (8XNAs) for growth but they are also capable of marked degradation of two model NAs, cyclohexanecarboxylic acid (CHCA) and cyclopentanecarboxylic acid (CPCA) when supplied at concentrations from 50 to 500 mgL-1. The growth curves of BCP1 on 8XNAs, CHCA, and CPCA showed an initial lag phase not present in growth on glucose, which presumably was related to the toxic effects of NAs on the cell membrane permeability. BCP1 cell adaptation responses that allowed survival on NAs included changes in cell morphology, production of intracellular bodies and changes in fatty acid composition. Transmission electron microscopy (TEM) analysis of BCP1 cells grown on CHCA or CPCA showed a slight reduction in the cell size, the production of EPS-like material and intracellular electron-transparent and electron-dense inclusion bodies. The electron-transparent inclusions increased in the amount and size in NA-grown BCP1 cells under nitrogen limiting conditions and contained storage lipids as suggested by cell staining with the lipophilic Nile Blue A dye. Lipidomic analyses revealed significant changes with increases of methyl-branched (MBFA) and polyunsaturated fatty acids (PUFA) examining the fatty acid composition of NAs-growing BCP1 cells. PUFA biosynthesis is not usual in bacteria and, together with MBFA, can influence structural and functional processes with resulting effects on cell vitality. Finally, through the use of RT (Reverse Transcription)-qPCR, a gene cluster (chcpca) was found to be transcriptionally induced during the growth on CHCA and CPCA. Based on the expression and bioinformatics results, the predicted products of the chcpca gene cluster are proposed to be involved in aerobic NA degradation in R. aetherivorans BCP1. This study provides first

Occurrences and behaviors of naphthenic acids in a petroleum refinery wastewater treatment plant.

PubMed

Wang, Beili; Wan, Yi; Gao, Yingxin; Zheng, Guomao; Yang, Min; Wu, Song; Hu, Jianying

2015-05-05

Naphthenic acids (NAs) are one class of compounds in wastewaters from petroleum industries that are known to cause toxic effects, and their removal from oilfield wastewater is an important challenge for remediation of large volumes of petrochemical effluents. The present study investigated occurrences and behaviors of total NAs and aromatic NAs in a refinery wastewater treatment plant, located in north China, which combined physicochemical and biological processes. Concentrations of total NAs were semiquantified to be 113-392 μg/L in wastewater from all the treatment units, and the percentages of aromatic NAs in total NAs was estimated to be 2.1-8.8%. The mass reduction for total NAs and aromatic NAs was 15±16% and 7.5±24% after the physicochemical treatment, respectively. Great mass reduction (total NAs: 65±11%, aromatic NAs: 86±5%) was observed in the biological treatment units, and antiestrogenic activities observed in wastewater from physicochemical treatment units disappeared in the effluent of the activated sludge system. The distributions of mass fractions of NAs demonstrated that biodegradation via activated sludge was the major mechanism for removing alicyclic NAs, aromatic NAs, and related toxicities in the plant, and the polycyclic NA congener classes were relatively recalcitrant to biodegradation, which is a complete contrast to the preferential adsorption of NAs with higher cyclicity (low Z value). Removal efficiencies of total NAs were 73±17% in summer, which were higher than those in winter (53±15%), and the seasonal variation was possibly due to the relatively high microbial biotransformation activities in the activated sludge system in summer (indexed by O3-NAs/NAs). The results of the investigations indicated that biotransformation of NA mixtures by the activated sludge system were largely affected by temperature, and employing an efficient adsorbent together with biodegradation processes would help cost-effectively remove NAs in petroleum

Inert Reassessment Document for Copper Naphthenate - CAS No. 1338-02-9

EPA Pesticide Factsheets

Copper naphthenate is approved by the Food and Drug Administration (FDA) as an indirect food additive, and for use in veterinary topical applications to the surface of horse and pony hooves that have Thrush.

Adsorption of acid-extractable organics from oil sands process-affected water onto biomass-based biochar: Metal content matters.

PubMed

Bhuiyan, Tazul I; Tak, Jin K; Sessarego, Sebastian; Harfield, Don; Hill, Josephine M

2017-02-01

The impact of biochar properties on acid-extractable organics (AEO) adsorption from oil sands process-affected water (OSPW) was studied. Biochar from wheat straw with the highest ash content (14%) had the highest adsorption capacity (0.59 mg/g) followed by biochar from pulp mill sludge, switchgrass, mountain pine, hemp shives, and aspen wood. The adsorption capacity had no obvious trend with surface area, total pore volume, bulk polarity and aromaticity. The large impact of metal content was consistent with the carboxylates (i.e., naphthenate species) in the OSPW binding to the metals (mainly Al and Fe) on the carbon substrate. Although the capacity of biochar is still approximately two orders of magnitude lower than that of a commercial activated carbon, confirming the property (i.e., metal content) that most influenced AEO adsorption, may allow biochar to become competitive with activated carbon after normalizing for cost, especially if this cost includes environmental impacts. Copyright © 2016 Elsevier Ltd. All rights reserved.

Removal of naphthenic acids using adsorption process and the effect of the addition of salt.

PubMed

Azad, Fakhry Seyedeyn; Abedi, Jalal; Iranmanesh, Sobhan

2013-01-01

In this study, various types of adsorbents were examined for the removal of Naphthenic acids (NAs) in the preliminary stage of this study. Among them, activated carbon and nickel (Ni) based alumina (Ni-Al2O3) possess relatively high adsorption capacity of NAs. The removal of NAs was evaluated comparing the total organic carbon (TOC) of the solution before and after the adsorption process. The effect of Ni loading was investigated using Ni-Al2O4 with various nickel loadings. The highest adsorption capacity (20 mg of TOC/1 mg of adsorbent) was belong to Ni-Al2O4 with 10.7% Ni loading. By the addition of salt (1500 ppm NaCl) to NAs solutions having concentrations from of 15 to 38 ppm, it was observed that the adsorption decreased dramatically (up to 80%) depending on the concentration of TOC. The kinetics of the adsorption of TOC on Ni-based alumina was also investigated. The decrease of TOC was more that 40% in the first half hour, indicating that adsorption was very rapid in the beginning. The adsorption increased slightly for up to 5 h and then leveled off when the TOC reached to 50% of initial TOC concentration. However, when sodium chloride (NaCl) was added to the solution, the adsorption decreased to almost 9% within the first half hour, reaching to almost 5% after 3 h. These phenomena suggest that the effectiveness of adsorbents may be improved by decreasing the total dissolved salts in tailings pond wastewater.

Tunable polymeric sorbent materials for fractionation of model naphthenates.

PubMed

Mohamed, Mohamed H; Wilson, Lee D; Headley, John V

2013-04-04

The sorption properties are reported for several examples of single-component carboxylic acids representing naphthenic acids (NAs) with β-cyclodextrin (β-CD) based polyurethane sorbents. Seven single-component examples of NAs were chosen with variable z values, carbon number, and chemical structure as follows: 2-hexyldecanoic acid (z = 0 and C = 16; S1), n-caprylic acid (z = 0 and C = 8; S2), trans-4-pentylcyclohexanecarboxylic acid (z = -2 and C = 12; S3), 4-methylcyclohexanecarboxylic acid (z = -2 and C = 8; S4), dicyclohexylacetic acid (z = -4; C = 14; S5), 4-pentylbicyclo[2.2.2]octane-1-carboxylic acid (z = -4; C = 14; S6), and lithocholic acid (z = -6; C = 24; S7). The copolymer sorbents were synthesized at three relative β-CD:diisocyanate mole ratios (i.e., 1:1, 1:2, and 1:3) using 4,4'-dicyclohexylmethane diisocyanate (CDI) and 4,4'-diphenylmethane diisocyanate (MDI). The sorption properties of the copolymer sorbents were characterized using equilibrium sorption isotherms in aqueous solution at pH 9.00 with electrospray ionization mass spectrometry. The equilibrium fraction of the unbound carboxylate anions was monitored in the aqueous phase. The sorption properties of the copolymer sorbents (i.e., Qm) were obtained from the Sips isotherm model. The Qm values generally decrease as the number of accessible β-CD inclusion sites in the copolymer framework decreases. The chemical structure of the adsorbates played an important role in their relative uptake, as evidenced by the adsorbate lipophilic surface area (LSA) and the involvement of hydrophobic effects. The copolymers exhibit molecular selective sorption of the single-component carboxylates in mixtures which suggests their application as sorbents for fractionation of mixtures of NAs. By comparison, granular activated carbon (GAC) and chitosan sorbents did not exhibit any significant molecular selective sorption relative to the copolymer materials; however, evidence of variable sorption capacity was

Application of UV-irradiated Fe(III)-nitrilotriacetic acid (UV-Fe(III)NTA) and UV-NTA-Fenton systems to degrade model and natural occurring naphthenic acids.

PubMed

Zhang, Ying; Chelme-Ayala, Pamela; Klamerth, Nikolaus; Gamal El-Din, Mohamed

2017-07-01

Naphthenic acids (NAs) are a highly complex mixture of organic compounds naturally present in bitumen and identified as the primary toxic constituent of oil sands process-affected water (OSPW). This work investigated the degradation of cyclohexanoic acid (CHA), a model NA compound, and natural occurring NAs during the UV photolysis of Fe(III)-nitrilotriacetic acid (UV-Fe(III)NTA) and UV-NTA-Fenton processes. The results indicated that in the UV-Fe(III)NTA process at pH 8, the CHA removal increased with increasing NTA dose (0.18, 0.36 and 0.72 mM), while it was independent of the Fe(III) dose (0.09, 0.18 and 0.36 mM). Moreover, the three Fe concentrations had no influence on the photolysis of the Fe(III)NTA complex. The main responsible species for the CHA degradation was hydroxyl radical (OH), and the role of dissolved O 2 in the OH generation was found to be negligible. Real OSPW was treated with the UV-Fe(III)NTA and UV-NTA-Fenton advanced oxidation processes (AOPs). The removals of classical NAs (O 2 -NAs), oxidized NAs with one additional oxygen atom (O 3 -NAs) and with two additional oxygen atoms (O 4 -NAs) were 44.5%, 21.3%, and 25.2% in the UV-Fe(III)NTA process, respectively, and 98.4%, 86.0%, and 81.0% in the UV-NTA-Fenton process, respectively. There was no influence of O 2 on the NA removal in these two processes. The results also confirmed the high reactivity of the O 2 -NA species with more carbons and increasing number of rings or double bond equivalents. This work opens a new window for the possible treatment of OSPW at natural pH using these AOPs. Copyright © 2017 Elsevier Ltd. All rights reserved.

Culturing oil sands microbes as mixed species communities enhances ex situ model naphthenic acid degradation

PubMed Central

Demeter, Marc A.; Lemire, Joseph A.; Yue, Gordon; Ceri, Howard; Turner, Raymond J.

2015-01-01

Oil sands surface mining for bitumen results in the formation of oil sands process water (OSPW), containing acutely toxic naphthenic acids (NAs). Potential exists for OSPW toxicity to be mitigated by aerobic degradation of the NAs by microorganisms indigenous to the oil sands tailings ponds, the success of which is dependent on the methods used to exploit the metabolisms of the environmental microbial community. Having hypothesized that the xenobiotic tolerant biofilm mode-of-life may represent a feasible way to harness environmental microbes for ex situ treatment of OSPW NAs, we aerobically grew OSPW microbes as single and mixed species biofilm and planktonic cultures under various conditions for the purpose of assaying their ability to tolerate and degrade NAs. The NAs evaluated were a diverse mixture of eight commercially available model compounds. Confocal microscopy confirmed the ability of mixed and single species OSPW cultures to grow as biofilms in the presence of the NAs evaluated. qPCR enumeration demonstrated that the addition of supplemental nutrients at concentrations of 1 g L-1 resulted in a more numerous population than 0.001 g L-1 supplementation by approximately 1 order of magnitude. GC-FID analysis revealed that mixed species cultures (regardless of the mode of growth) are the most effective at degrading the NAs tested. All constituent NAs evaluated were degraded below detectable limits with the exception of 1-adamantane carboxylic acid (ACA); subsequent experimentation with ACA as the sole NA also failed to exhibit degradation of this compound. Single species cultures degraded select few NA compounds. The degradation trends highlighted many structure-persistence relationships among the eight NAs tested, demonstrating the effect of side chain configuration and alkyl branching on compound recalcitrance. Of all the isolates, the Rhodococcus spp. degraded the greatest number of NA compounds, although still less than the mixed species cultures

Characterization and determination of naphthenic acids species in oil sands process-affected water and groundwater from oil sands development area of Alberta, Canada.

PubMed

Huang, Rongfu; Chen, Yuan; Meshref, Mohamed N A; Chelme-Ayala, Pamela; Dong, Shimiao; Ibrahim, Mohamed D; Wang, Chengjin; Klamerth, Nikolaus; Hughes, Sarah A; Headley, John V; Peru, Kerry M; Brown, Christine; Mahaffey, Ashley; Gamal El-Din, Mohamed

2018-01-01

This work reports the monitoring and assessment of naphthenic acids (NAs) in oil sands process-affected water (OSPW), Pleistocene channel aquifer groundwater (PLCA), and oil sands basal aquifer groundwater (OSBA) from an active oil sands development in Alberta, Canada, using ultra performance liquid chromatography time-of-flight mass spectrometry (UPLC-TOF-MS) analysis with internal standard (ISTD) and external standard (ESTD) calibration methods and Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) for compositional analysis. PLCA was collected at 45-51 m depth and OSBA was collected at 67-144 m depth. Results of O x -NA concentrations follow an order as OSPW > OSBA > PLCA, indicating that occurrences of NAs in OSBA were likely related to natural bitumen deposits instead of OSPW. Liquid-liquid extraction (LLE) was applied to avoid the matrix effect for the ESTD method. Reduced LLE efficiency accounted for the divergence of the ISTD and ESTD calibrated results for oxidized NAs. Principle component analysis results of O 2 and O 4 species could be employed for differentiation of water types, while classical NAs with C13-15 and Z (-4)-(-6) and aromatic O 2 -NAs with C16-18 and Z (-14)-(-16) could be measured as marker compounds to characterize water sources and potential temporal variations of samples, respectively. FTICR-MS results revealed that compositions of NA species varied greatly among OSPW, PLCA, and OSBA, because of NA transfer and transformation processes. This work contributed to the understanding of the concentration and composition of NAs in various types of water, and provided a useful combination of analytical and statistical tools for monitoring studies, in support of future safe discharge of treated OSPW. Copyright © 2017 Elsevier Ltd. All rights reserved.

Growth, development and incidence of deformities in amphibian larvae exposed as embryos to naphthenic acid concentrations detected in the Canadian oil sands region.

PubMed

Melvin, Steven D; Trudeau, Vance L

2012-08-01

Naphthenic acids (NA) have been identified as harmful environmental contaminants that influence survival, growth and development of wildlife. Amphibian larvae are particularly susceptible to waterborne contaminants, but little information exists regarding exposure of amphibian embryos or tadpoles to NA. Our results demonstrate that embryos of Lithobates pipiens and Silurana tropicalis exposed to 2-4 mg/l of a commercial NA blend suffer significant reductions (32% and 25%, respectively) in growth and development upon hatching. Increased incidences of deformities were observed in exposed individuals of both species, but were only significant in L. pipiens. Embryos suffered 100% mortality following exposure to 6 mg/l NAs, and narcosis at lower concentrations. LC50 estimates were 4.10 mg/l for 72-h exposure in L. pipiens and 4.13, 3.51, and 2.95 mg/l for 24-, 48-, and 72-h exposure in S. tropicalis. These data suggest that exposure to NAs at environmentally realized concentrations may negatively affect tadpole populations. Copyright © 2012 Elsevier Ltd. All rights reserved.

Naphthenic acids removal from high TDS produced water by persulfate mediated iron oxide functionalized catalytic membrane, and by nanofiltration.

PubMed

Aher, Ashish; Papp, Joseph; Colburn, Andrew; Wan, Hongyi; Hatakeyama, Evan; Prakash, Prakhar; Weaver, Ben; Bhattacharyya, Dibakar

2017-11-01

Oil industries generate large amounts of produced water containing organic contaminants, such as naphthenic acids (NA) and very high concentrations of inorganic salts. Recovery of potable water from produced water can be highly energy intensive is some cases due to its high salt concentration, and safe discharge is more suitable. Here, we explored catalytic properties of iron oxide (Fe x O y nanoparticles) functionalized membranes in oxidizing NA from water containing high concentrations of total dissolved solids (TDS) using persulfate as an oxidizing agent. Catalytic decomposition of persulfate by Fe x O y functionalized membranes followed pseudo-first order kinetics with an apparent activation energy of 18 Kcal/mol. Fe x O y functionalized membranes were capable of lowering the NA concentrations to less than discharge limits of 10 ppm at 40 °C. Oxidation state of iron during reaction was quantified. Membrane performance was investigated for extended period of time. A coupled process of advanced oxidation catalyzed by membrane and nanofiltration was also evaluated. Commercially available nanofiltration membranes were found capable of retaining NA from water containing high concentrations of dissolved salts. Commercial NF membranes, Dow NF270 (Dow), and NF8 (Nanostone) had NA rejection of 79% and 82%, respectively. Retentate for the nanofiltration was further treated with advanced oxidation catalyzed by Fe x O y functionalized membrane for removal of NA.

Direct patterning of highly-conductive graphene@copper composites using copper naphthenate as a resist for graphene device applications.

PubMed

Bi, Kaixi; Xiang, Quan; Chen, Yiqin; Shi, Huimin; Li, Zhiqin; Lin, Jun; Zhang, Yongzhe; Wan, Qiang; Zhang, Guanhua; Qin, Shiqiao; Zhang, Xueao; Duan, Huigao

2017-11-09

We report an electron-beam lithography process to directly fabricate graphene@copper composite patterns without involving metal deposition, lift-off and etching processes using copper naphthenate as a high-resolution negative-tone resist. As a commonly used industrial painting product, copper naphthenate is extremely cheap with a long shelf time but demonstrates an unexpected patterning resolution better than 10 nm. With appropriate annealing under a hydrogen atmosphere, the produced graphene@copper composite patterns show high conductivity of ∼400 S cm -1 . X-ray diffraction, conformal Raman spectroscopy and X-ray photoelectron spectroscopy were used to analyze the chemical composition of the final patterns. With the properties of high resolution and high conductivity, the patterned graphene@copper composites could be used as conductive pads and interconnects for graphene electronic devices with ohmic contacts. Compared to common fabrication processes involving metal evaporation and lift-off steps, this pattern-transfer-free fabrication process using copper naphthenate resist is direct and simple but allows comparable device performance in practical device applications.

Microwave-Assisted Extraction of Oleanolic Acid and Ursolic Acid from Ligustrum lucidum Ait

PubMed Central

Xia, En-Qin; Wang, Bo-Wei; Xu, Xiang-Rong; Zhu, Li; Song, Yang; Li, Hua-Bin

2011-01-01

Oleanolic acid and ursolic acid are the main active components in fruit of Ligustrum lucidum Ait, and possess anticancer, antimutagenic, anti-inflammatory, antioxidative and antiprotozoal activities. In this study, microwave-assisted extraction of oleanolic acid and ursolic acid from Ligustrum lucidum was investigated with HPLC-photodiode array detection. Effects of several experimental parameters, such as type and concentration of extraction solvent, ratio of liquid to material, microwave power, extraction temperature and microwave time, on the extraction efficiencies of oleanolic acid and ursolic acid from Ligustrum lucidum were evaluated. The influence of experimental parameters on the extraction efficiency of ursolic acid was more significant than that of oleanolic acid (p < 0.05). The optimal extraction conditions were 80% ethanol aqueous solution, the ratio of material to liquid was 1:15, and extraction for 30 min at 70 °C under microwave irradiation of 500 W. Under optimal conditions, the yields of oleanolic acid and ursolic acid were 4.4 ± 0.20 mg/g and 5.8 ± 0.15 mg/g, respectively. The results obtained are helpful for the full utilization of Ligustrum lucidum, which also indicated that microwave-assisted extraction is a very useful method for extraction of oleanolic acid and ursolic acid from plant materials. PMID:21954361

Assessing spatial and temporal variability of acid-extractable organics in oil sands process-affected waters.

PubMed

Frank, Richard A; Milestone, Craig B; Rowland, Steve J; Headley, John V; Kavanagh, Richard J; Lengger, Sabine K; Scarlett, Alan G; West, Charles E; Peru, Kerry M; Hewitt, L Mark

2016-10-01

The acid-extractable organic compounds (AEOs), including naphthenic acids (NAs), present within oil sands process-affected water (OSPW) receive great attention due to their known toxicity. While recent progress in advanced separation and analytical methodologies for AEOs has improved our understanding of the composition of these mixtures, little is known regarding any variability (i.e., spatial, temporal) inherent within, or between, tailings ponds. In this study, 5 samples were collected from the same location of one tailings pond over a 2-week period. In addition, 5 samples were collected simultaneously from different locations within a tailings pond from a different mine site, as well as its associated recycling pond. In both cases, the AEOs were analyzed using SFS, ESI-MS, HRMS, GC×GC-ToF/MS, and GC- & LC-QToF/MS (GC analyses following conversion to methyl esters). Principal component analysis of HRMS data was able to distinguish the ponds from each other, while data from GC×GC-ToF/MS, and LC- and GC-QToF/MS were used to differentiate samples from within the temporal and spatial sample sets, with the greater variability associated with the latter. Spatial differences could be attributed to pond dynamics, including differences in inputs of tailings and surface run-off. Application of novel chemometric data analyses of unknown compounds detected by LC- and GC-QToF/MS allowed further differentiation of samples both within and between data sets, providing an innovative approach for future fingerprinting studies. Crown Copyright © 2016. Published by Elsevier Ltd. All rights reserved.

Impact of ozonation on naphthenic acids speciation and toxicity of oil sands process-affected water to Vibrio fischeri and mammalian immune system.

PubMed

Wang, Nan; Chelme-Ayala, Pamela; Perez-Estrada, Leonidas; Garcia-Garcia, Erick; Pun, Jonathan; Martin, Jonathan W; Belosevic, Miodrag; Gamal El-Din, Mohamed

2013-06-18

Oil sands process-affected water (OSPW) is the water contained in tailings impoundment structures in oil sands operations. There are concerns about the environmental impacts of the release of OSPW because of its toxicity. In this study, ozonation followed by biodegradation was used to remediate OSPW. The impacts of the ozone process evolution on the naphthenic acids (NAs) speciation and acute toxicity were evaluated. Ion-mobility spectrometry (IMS) was used to preliminarily separate isomeric and homologous species. The results showed limited effects of the ozone reactor size on the treatment performance in terms of contaminant removal. In terms of NAs speciation, high reactivity of NAs with higher number of carbons and rings was only observed in a region of high reactivity (i.e., utilized ozone dose lower than 50 mg/L). It was also found that nearly 0.5 mg/L total NAs was oxidized per mg/L of utilized ozone dose, at utilized ozone doses lower than 50 mg/L. IMS showed that ozonation was able to degrade NAs, oxidized NAs, and sulfur/nitrogenated NAs. Complete removal of toxicity toward Vibrio fischeri was achieved after ozonation followed by 28-day biodegradation period. In vitro and in vivo assays indicated that ozonation reduced the OSPW toxicity to mice.

Solid-phase extraction of acidic herbicides.

PubMed

Wells, M J; Yu, L Z

2000-07-14

A discussion of solid-phase extraction method development for acidic herbicides is presented that reviews sample matrix modification, extraction sorbent selection, derivatization procedures for gas chromatographic analysis, and clean-up procedures for high-performance liquid chromatographic analysis. Acidic herbicides are families of compounds that include derivatives of phenol (dinoseb, dinoterb and pentachlorophenol), benzoic acid (acifluorfen, chloramben, dicamba, 3,5-dichlorobenzoic acid and dacthal--a dibenzoic acid derivative), acetic acid [2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T)], propanoic acid [dichlorprop, fluazifop, haloxyfop, 2-(4-chloro-2-methylphenoxy)propanoic acid (MCPP) and silvex], butanoic acid [4-(2,4-dichlorophenoxy)butanoic acid (2,4-DB) and 4-(4-chloro-2-methylphenoxy)butanoic acid (MCPB)], and other miscellaneous acids such as pyridinecarboxylic acid (picloram) and thiadiazine dioxide (bentazon).

Dynamics of two methanogenic microbiomes incubated in polycyclic aromatic hydrocarbons, naphthenic acids, and oil field produced water.

PubMed

Oko, Bonahis J; Tao, Yu; Stuckey, David C

2017-01-01

Oil field produced water (OFPW) is widely produced in large volumes around the world. Transforming the organic matter in OFPW into bioenergy, such as biomethane, is one promising way to sustainability. However, OFPW is difficult to biologically degrade because it contains complex compounds such as naphthenic acids (NAs), or polycyclic aromatic hydrocarbons (PAHs). Although active microbial communities have been found in many oil reservoirs, little is known about how an exotic microbiome, e.g. the one which originates from municipal wastewater treatment plants, would evolve when incubated with OFPW. In this study, we harvested methanogenic biomass from two sources: a full-scale anaerobic digester (AD) treating oil and gas processing wastewater (named O&G sludge), and from a full-scale AD reactor treating multiple fractions of municipal solid wastes (named MS, short for mixed sludge). Both were incubated in replicate microcosms fed with PAHs, NAs, or OFPW. The results showed that the PAHs, NAs, and OFPW feeds could rapidly alter the methanogenic microbiomes, even after 14 days, while the O&G sludge adapted faster than the mixed sludge in all the incubations. Two rarely reported microorganisms, a hydrogenotrophic methanogen Candidatus methanoregula and a saccharolytic fermenter Kosmotoga , were found to be prevalent in the PAHs and OFPW microcosms, and are likely to play an important role in the syntrophic degradation of PAHs and OFPW, cooperating with methanogens such as Methanoregula, Methanosarcina, or Methanobacterium . The dominant phyla varied in certain patterns during the incubations, depending on the biomass source, feed type, and variation in nutrients. The sludge that originated from the oil and gas processing wastewater treatment (O&G) reactor adapted faster than the one from municipal solid waste reactors, almost certainly because the O&G biomass had been "pre-selected" by the environment. This study reveals the importance of biomass selection for other

Effects of aerosol formulation to amino acids and fatty acids contents in Haruan extract.

PubMed

Febriyenti; Bai-Baie, Saringat Bin; Laila, Lia

2012-01-01

Haruan (Channa striatus) extract was formulated to aerosol for wound and burn treatment. Haruan extract is containing amino acids and fatty acids that important for wound healing process. The purpose of this study is to observe the effect of formulation and other excipients in the formula to amino acids and fatty acids content in Haruan extract before and after formulated into aerosol. Precolumn derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) method is used for amino acids analysis. Fatty acids in Haruan extract were esterified using transesterification method to form FAMEs before analyzed using GC. Boron trifluoride-methanol reagent is used for transesterification. Tyrosine and methionine concentrations were different after formulated. The concentrations were decrease. There are six fatty acids have amount that significantly different after formulated into concentrate and aerosol. Contents of these fatty acids were increase. Generally, fatty acids which had content increased after formulated were the long-chain fatty acids. This might be happen because of chain extension process. Saponification and decarboxylation would give the chain extended product. Therefore contents of long-chain fatty acids were increase. Generally, the aerosol formulation did not affect the amino acids concentrations in Haruan extract while some long-chain fatty acids concentrations were increase after formulated into concentrate and aerosol.

Process for the extraction of strontium from acidic solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1994-01-01

The invention is a process for selectively extracting strontium values from aqueous nitric acid waste solutions containing these and other fission product values. The extractant solution is a macrocyclic polyether in an aliphatic hydrocarbon diluent containing a phase modifier. The process will selectively extract strontium values from nitric acid solutions which are up to 6 molar in nitric acid.

Process for the extraction of strontium from acidic solutions

DOEpatents

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

1993-01-01

The invention is a process for selectively extracting strontium values from aqueous nitric acid waste solutions containing these and other fission product values. The extractant solution is a macrocyclic polyether in an aliphatic hydrocarbon diluent containing a phase modifier. The process will selectively extract strontium values from nitric acid solutions which are up to 6 molar in nitric acid.

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Solvent extraction process for citric acid. 173... Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Solvent extraction process for citric acid. 173... Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Solvent extraction process for citric acid. 173... Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Solvent extraction process for citric acid. 173.280... extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

Process for the extraction of strontium from acidic solutions

DOEpatents

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

1994-09-06

The invention is a process for selectively extracting strontium values from aqueous nitric acid waste solutions containing these and other fission product values. The extractant solution is a macrocyclic polyether in an aliphatic hydrocarbon diluent containing a phase modifier. The process will selectively extract strontium values from nitric acid solutions which are up to 6 molar in nitric acid. 4 figs.

Ultrasound-Assisted Extraction of Carnosic Acid and Rosmarinic Acid Using Ionic Liquid Solution from Rosmarinus officinalis

PubMed Central

Zu, Ge; Zhang, Rongrui; Yang, Lei; Ma, Chunhui; Zu, Yuangang; Wang, Wenjie; Zhao, Chunjian

2012-01-01

Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C8mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid–liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential. PMID:23109836

Virus inactivation by nucleic acid extraction reagents.

PubMed

Blow, Jamie A; Dohm, David J; Negley, Diane L; Mores, Christopher N

2004-08-01

Many assume that common methods to extract viral nucleic acids are able to render a sample non-infectious. It may be that inactivation of infectious virus is incomplete during viral nucleic acid extraction methods. Accordingly, two common viral nucleic acid extraction techniques were evaluated for the ability to inactivate high viral titer specimens. In particular, the potential for TRIzol LS Reagent (Invitrogen Corp., Carlsbad, CA) and AVL Buffer (Qiagen, Valencia, CA) were examined to render suspensions of alphaviruses, flaviviruses, filoviruses and a bunyavirus non-infectious to tissue culture assay. The dilution series for both extraction reagents consistently caused cell death through a 100-fold dilution. Except for the DEN subtype 4 positive control, all viruses had titers of at least 10(6)pfu/ml. No plaques were detected in any extraction reagent plus virus combination in this study, therefore, the extraction reagents appeared to inactivate completely each of the high-titer viruses used in this study. These results support the reliance upon either TRIzol LS Reagent or AVL Buffer to render clinical or environmental samples non-infectious, which has implications for the handling and processing of samples under austere field conditions and low level containment.

Molecular profiling of naphthenic acids in technical mixtures and oil sands process-affected water using polar reversed-phase liquid chromatography-mass spectrometry.

PubMed

Han, Jun; Yi, Yi; Lin, Karen; Birks, S Jean; Gibson, John J; Borchers, Christoph H

2016-12-01

In this work, a reversed-phase ultra-HPLC (UHPLC) ultrahigh resolution MS (UHRMS) method was evaluated for the comprehensive profiling of NAs containing two O atoms in each molecule (O2NAs; general formula C n H 2n + z O 2 , where n is the number of carbon atoms and z represents hydrogen deficiency). Using a polar cyanopropyl-bonded phase column and negative-ion electrospray ionization mass spectrometric detection at 120,000 FWHM (m/z 400), 187 and 226 O2NA species were found in two naphthenic acid technical mixtures, and 424 and 198 species with molecular formulas corresponding to O2NAs were found in two oil sands process-affected water samples (one from a surface mining operation and the other from a steam-assisted gravity drainage operation), respectively. To our knowledge, these are the highest numbers of molecular compositions of O2NAs that have been profiled thus far in environmental samples. Assignments were based on accurate mass measurements (≤3 ppm) combined with rational molecular formula generation, correlation of chromatographic behavior of O2NA homologues with their elemental compositions, and confirmation with carboxyl group-specific chemical derivatization using 3-nitrophenylhydrazine. Application of this UHPLC-UHRMS method to the quantitation of O2NAs in the surface mining operation-derived water sample showed excellent linearity (R 2 = 0.9999) with external calibration, a linear range of 256-fold in concentration, and quantitation accuracies of 64.9 and 69.4% at two "standard substance" spiking levels. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Subcritical Water Extraction of Amino Acids from Atacama Desert Soils

NASA Technical Reports Server (NTRS)

Amashukeli, Xenia; Pelletier, Christine C.; Kirby, James P.; Grunthaner, Frank J.

2007-01-01

Amino acids are considered organic molecular indicators in the search for extant and extinct life in the Solar System. Extraction of these molecules from a particulate solid matrix, such as Martian regolith, will be critical to their in situ detection and analysis. The goals of this study were to optimize a laboratory amino acid extraction protocol by quantitatively measuring the yields of extracted amino acids as a function of liquid water temperature and sample extraction time and to compare the results to the standard HCl vapor- phase hydrolysis yields for the same soil samples. Soil samples from the Yungay region of the Atacama Desert ( Martian regolith analog) were collected during a field study in the summer of 2005. The amino acids ( alanine, aspartic acid, glutamic acid, glycine, serine, and valine) chosen for analysis were present in the samples at concentrations of 1 - 70 parts- per- billion. Subcritical water extraction efficiency was examined over the temperature range of 30 - 325 degrees C, at pressures of 17.2 or 20.0 MPa, and for water- sample contact equilibration times of 0 - 30 min. None of the amino acids were extracted in detectable amounts at 30 degrees C ( at 17.2 MPa), suggesting that amino acids are too strongly bound by the soil matrix to be extracted at such a low temperature. Between 150 degrees C and 250 degrees C ( at 17.2 MPa), the extraction efficiencies of glycine, alanine, and valine were observed to increase with increasing water temperature, consistent with higher solubility at higher temperatures, perhaps due to the decreasing dielectric constant of water. Amino acids were not detected in extracts collected at 325 degrees C ( at 20.0 MPa), probably due to amino acid decomposition at this temperature. The optimal subcritical water extraction conditions for these amino acids from Atacama Desert soils were achieved at 200 degrees C, 17.2 MPa, and a water- sample contact equilibration time of 10 min.

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Solvent extraction process for citric acid. 173..., Lubricants, Release Agents and Related Substances § 173.280 Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation...

Fermentation of aqueous plant seed extracts by lactic acid bacteria

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

Schafner, D.W.; Beuchat, R.L.

1986-05-01

The effects of lactic acid bacterial fermentation on chemical and physical changes in aqueous extracts of cowpea (Vigna unguiculata), peanut (Arachis hypogea), soybean (Glycine max), and sorghum (Sorghum vulgare) were studied. The bacteria investigated were Lactobacillus helveticus, L. delbrueckii, L. casei, L. bulgaricus, L. acidophilus, and Streptococcus thermophilus. Organisms were inoculated individually into all of the seed extracts; L. bulgaricus and S. thermophilus were also evaluated together as inocula for fermenting the legume extracts. During fermentation, bacterial population and changes in titratable acidity, pH, viscosity, and color were measured over a 72 h period at 37 degrees C. Maximum bacterialmore » populations, titratable acidity, pH, and viscosity varied depending upon the type of extract and bacterial strain. The maximum population of each organism was influenced by fermentable carbohydrates, which, in turn, influenced acid production and change in pH. Change in viscosity was correlated with the amount of protein and titratable acidity of products. Color was affected by pasteurization treatment and fermentation as well as the source of extract. In the extracts inoculated simultaneously with L. bulgaricus and S. thermophilus, a synergistic effect resulted in increased bacterial populations, titratable acidity, and viscosity, and decreased pH in all the legume extracts when compared to the extracts fermented with either of these organisms individually. Fermented extracts offer potential as substitutes for cultured dairy products. 24 references.« less

Optimization of acidic extraction of astaxanthin from Phaffia rhodozyma *

PubMed Central

Ni, Hui; Chen, Qi-he; He, Guo-qing; Wu, Guang-bin; Yang, Yuan-fan

2008-01-01

Optimization of a process for extracting astaxanthin from Phaffia rhodozyma by acidic method was investigated, regarding several extraction factors such as acids, organic solvents, temperature and time. Fractional factorial design, central composite design and response surface methodology were used to derive a statistically optimal model, which corresponded to the following optimal condition: concentration of lactic acid at 5.55 mol/L, ratio of ethanol to yeast dry weight at 20.25 ml/g, temperature for cell-disruption at 30 °C, and extraction time for 3 min. Under this condition, astaxanthin and the total carotenoids could be extracted in amounts of 1294.7 μg/g and 1516.0 μg/g, respectively. This acidic method has advantages such as high extraction efficiency, low chemical toxicity and no special requirement of instruments. Therefore, it might be a more feasible and practical method for industrial practice. PMID:18196613

Extractive fermentation of acetic acid

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

Busche, R.M.

1991-12-31

In this technoeconomic evaluation of the manufacture of acetic acid by fermentation, the use of the bacterium: Acetobacter suboxydans from the old vinegar process was compared with expected performance of the newer Clostridium thermoaceticum bacterium. Both systems were projected to operate as immobilized cells in a continuous, fluidized bed bioreactor, using solvent extraction to recover the product. Acetobacter metabolizes ethanol aerobically to produce acid at 100 g/L in a low pH medium. This ensures that the product is in the form of a concentrated extractable free acid, rather than as an unextractable salt. Unfortunately, yields from glucose by way ofmore » the ethanol fermentation are poor, but near the biological limits of the organisms involved. Conversely, C. thermoaceticum is a thermophilic anaerobe that operates at high fermentation rates on glucose at neutral pH to produce acetate salts directly in substantially quantitative yields. However, it is severely inhibited by product, which restricts concentration to a dilute 20 g/L. An improved Acetobacter system operating with recycled cells at 50 g/L appears capable of producing acid at $0.38/lb, as compared with a $0.29/lb price for synthetic acid. However, this system has only a limited margin for process improvement. The present Clostridium system cannot compete, since the required selling price would be $0.42/lb. However, if the organism could be adapted to tolerate higher product concentrations at acid pH, selling price could be reduced to $0.22/lb, or about 80% of the price of synthetic acid.« less

Graphene oxide for solid-phase extraction of bioactive phenolic acids.

PubMed

Hou, Xiudan; Wang, Xusheng; Sun, Yingxin; Wang, Licheng; Guo, Yong

2017-05-01

A solid-phase extraction (SPE) method for the efficient analysis of trace phenolic acids (PAs, caffeic acid, ferulic acid, protocatechuic acid, cinnamic acid) in urine was established. In this work, a graphene oxide (GO) coating was grafted onto pure silica to be investigated as SPE material. The prepared GO surface had a layered and wrinkled structure that was rough and well organized, which could provide more open adsorption sites. Owing to its hydrophilicity and polarity, GO showed higher extraction efficiency toward PAs than reduced GO did, in agreement with the theoretical calculation results performed by Gaussian 09 software. The adsorption mechanism of PAs on GO@Sil was also investigated through static state and kinetic state adsorption experiments, which showed a monolayer surface adsorption. Extraction capacity of the as-prepared material was optimized using the response surface methodology. Under the optimized conditions, the as-established method provided wide linearity range (2-50 μg L -1 for protocatechuic acid and 1-50 μg L -1 for caffeic acid, ferulic acid, and cinnamic acid) and low limits of detection (0.25-1 μg L -1 ). Finally, the established method was applied for the analysis of urine from two healthy volunteers. The results indicate that the prepared material is a practical, cost-effective medium for the extraction and determination of phenolic acids in complex matrices. Graphical Abstract A graphene oxide coating was grafted onto pure silica as the SPE material for the extraction of phenolic acids in urines and the extraction mechanism was also mainly investigated.

Extraction of rare earth elements from a contaminated cropland soil using nitric acid, citric acid, and EDTA.

PubMed

Tang, Hailong; Shuai, Weitao; Wang, Xiaojing; Liu, Yangsheng

2017-08-01

Rare earth elements (REEs) contamination to the surrounding soil has increased the concerns of health risk to the local residents. Soil washing was first attempted in our study to remediate REEs-contaminated cropland soil using nitric acid, citric acid, and ethylene diamine tetraacetic acid (EDTA) for soil decontamination and possible recovery of REEs. The extraction time, washing agent concentration, and pH value of the washing solution were optimized. The sequential extraction analysis proposed by Tessier was adopted to study the speciation changes of the REEs before and after soil washing. The extract containing citric acid was dried to obtain solid for the X-ray fluorescence (XRF) analysis. The results revealed that the optimal extraction time was 72 h, and the REEs extraction efficiency increased as the agent concentration increased from 0.01 to 0.1 mol/L. EDTA was efficient to extract REEs over a wide range of pH values, while citric acid was around pH 6.0. Under optimized conditions, the average extraction efficiencies of the major REEs in the contaminated soil were 70.96%, 64.38%, and 62.12% by EDTA, nitric acid, and citric acid, respectively. The sequential extraction analyses revealed that most soil-bounded REEs were mobilized or extracted except for those in the residual fraction. Under a comprehensive consideration of the extraction efficiency and the environmental impact, citric acid was recommended as the most suitable agent for extraction of the REEs from the contaminated cropland soils. The XRF analysis revealed that Mn, Al, Si, Pb, Fe, and REEs were the major elements in the extract indicating a possibile recovery of the REEs.

Fate and abundance of classical and heteroatomic naphthenic acid species after advanced oxidation processes: Insights and indicators of transformation and degradation.

PubMed

Meshref, Mohamed N A; Chelme-Ayala, Pamela; Gamal El-Din, Mohamed

2017-11-15

The toxicological effects from all components in oil sands process-affected water (OSPW) are not known. Alternatively, monitoring the variations and abundance of different classes and compounds after treatments might be a useful approach in OSPW remediation. In this study, the variations in the compositions of classical and heteroatomic naphthenic acids (NAs) after treatment using advanced oxidation processes (AOPs), mainly ozone and peroxone, and two different mass spectrometry methods; ultra-performance liquid chromatography time-of-flight (UPLC-TOFMS) and Fourier transform ion cyclotron resonance (FTICR-MS), were examined. Two markers (O 2 S:O 3 S:O 4 S and O 2 :O 4 ratios) were used to reveal changes and similarities of the treated water characteristics with those in natural waters. Both ratios decreased after all treatments, from 2.7:4.8:2.1 and 3.59 in raw OSPW to 0:1.4:0.5 and 0.7, respectively, in peroxone (1:2), becoming close to the reported ratios in natural waters. Toxicity toward Vibrio fischeri showed residual toxic effects after AOPs, suggesting that part of OSPW toxicity may be caused by specific compounds of NAs (i.e., similar reduction (50%) was achieved in both toxicity and abundance in O 2 species with carbon 15-26) and/or generated by-products (e.g., O 3 S classes at double bond equivalent (DBE) = 4 and C 9 H 12 O 2 at DBE = 4). Although by-products were generated, the best biodegradability enhancement and chemical oxygen demand reduction were achieved in peroxone (1:2) compared to ozone, suggesting the possibility of using combined OSPW remediation approaches (i.e., peroxone coupled with biological process). The recommended indicators can assist in evaluating the treatments' performance and in examining the best removal levels to accomplish significant toxicity reduction. Copyright © 2017 Elsevier Ltd. All rights reserved.

Extraction Behaviors of Heavy Rare Earths with Organophosphoric Extractants: The Contribution of Extractant Dimer Dissociation, Acid Ionization, and Complexation. A Quantum Chemistry Study.

PubMed

Jing, Yu; Chen, Ji; Chen, Li; Su, Wenrou; Liu, Yu; Li, Deqian

2017-03-30

Heavy rare earths (HREs), namely Ho 3+ , Er 3+ , Tm 3+ , Yb 3+ and Lu 3+ , are rarer and more exceptional than light rare earths, due to the stronger extraction capacity for 100 000 extractions. Therefore, their incomplete stripping and high acidity of stripping become problems for HRE separation by organophosphoric extractants. However, the theories of extractant structure-performance relationship and molecular design method of novel HRE extractants are still not perfect. Beyond the coordination chemistry of the HRE-extracted complex, the extractant dimer dissociation, acid ionization, and complexation behaviors can be crucial to HRE extraction and reactivity of ionic species for understanding and further improving the extraction performance. To address the above issues, three primary fundamental processes, including extractant dimer dissociation, acid ionization, and HRE complexation, were identified and investigated systematically. The intrinsic extraction performances of HRE cations with four acidic organophosphoric extractants (P507, P204, P227 and Cyanex 272) were studied by using relativistic energy-consistent 4f core pseudopotentials, combined with density functional theory and a solvation model. Four acidic organophosphoric extractants have been qualified quantitatively from microscopic structures to chemical properties. It has been found that the Gibbs free energy changes of the overall extraction process (sequence: P204 > P227 > P507 > Cyanex 272) and their differences as a function of HREs (sequence: Ho/Er > Er/Tm > Tm/Yb > Yb/Lu) are in good agreement with the experimental maximum extraction capacities and separation factors. These results could provide an important approach to evaluate HRE extractants by the comprehensive consideration of dimer dissociation, acid ionization, and complexation processes. This paper also demonstrates the importance of the P-O bond, the P-C bond, isomer substituent, and solvation effects on the structure

Subcritical water extraction of amino acids from Mars analog soils.

PubMed

Noell, Aaron C; Fisher, Anita M; Fors-Francis, Kisa; Sherrit, Stewart

2018-01-18

For decades, the Martian regolith has stymied robotic mission efforts to catalog the organic molecules present. Perchlorate salts, found widely throughout Mars, are the main culprit as they breakdown and react with organics liberated from the regolith during pyrolysis, the primary extraction technique attempted to date on Mars. This work further develops subcritical water extraction (SCWE) as a technique for extraction of amino acids on future missions. The effect of SCWE temperature (185, 200, and 215°C) and duration of extraction (10-120 min) on the total amount and distribution of amino acids recovered was explored for three Mars analog soils (JSC Mars-1A simulant, an Atacama desert soil, and an Antarctic Dry Valleys soil) and bovine serum albumin (as a control solution of known amino acid content). Total amounts of amino acids extracted increased with both time and temperature; however, the distribution shifted notably due to the destruction of the amino acids with charged or polar side chains at the higher temperatures. The pure bovine serum albumin solution and JSC Mars 1A also showed lower yields than the Atacama and Antarctic extractions suggesting that SCWE may be less effective at hydrolyzing large or aggregated proteins. Changing solvent from water to a dilute (10 mM) HCl solution allowed total extraction efficiencies comparable to the higher temperature/time combinations while using the lowest temperature/time (185°C/20 min). The dilute HCl extractions also did not lead to the shift in amino acid distribution observed at the higher temperatures. Additionally, adding sodium perchlorate salt to the extraction did not interfere with recoveries. Native magnetite in the JSC Mars-1A may have been responsible for destruction of glycine, as evidenced by its uncharacteristic decrease as the temperature/time of extraction increased. This work shows that SCWE can extract high yields of native amino acids out of Mars analog soils with minimal disruption of the

Effect of Extraction Conditions on the Saccharide (Neutral and Acidic) Composition of the Crude Pectic Extract from Various Agro-Industrial Residues.

PubMed

Babbar, Neha; Roy, Sandra Van; Wijnants, Marc; Dejonghe, Winnie; Caligiani, Augusta; Sforza, Stefano; Elst, Kathy

2016-01-13

The influence of different extraction methodologies was assessed on the composition of both neutral (arabinose, rhamnose, galactose) and acidic (galacturonic acid) pectic polysaccharides obtained from four agro-industrial residues, namely, berry pomace (BP), onion hulls (OH), pressed pumpkin (PP), and sugar beet pulp (SBP). For acidic pectic polysaccharides, the extraction efficiency was obtained as BP (nitric acid-assisted extraction, 2 h, 62.9%), PP (enzymatic-assisted extraction, 12 h, 75.0%), SBP (enzymatic-assisted extraction, 48 h, 89.8%; and nitric acid-assisted extraction, 4 h, 76.5%), and OH (sodium hexametaphosphate-assisted extraction, 0.5 h, 100%; and ammonium oxalate-assisted extraction, 0.5 h, 100%). For neutral pectic polysaccharides, the following results were achieved: BP (enzymatic-assisted extraction, 24 h, 85.9%), PP (nitric acid-assisted extraction, 6 h, 82.2%), and SBP (enzymatic assisted extraction, 48 h, 97.5%; and nitric acid-assisted extraction, 4 h, 83.2%). On the basis of the high recovery of pectic sugars, SBP and OH are interesting candidates for the further purification of pectin and production of pectin-derived products.

Copigmentation Of Anthocyanin Extract of Purple Sweet Potatoes (Ipomea Batatas L.) Using Ferulic Acid And Tannic Acid

NASA Astrophysics Data System (ADS)

Susanti, I.; Wijaya, H.; Hasanah, F.; Heryani, S.

2018-02-01

Copigmentation is one of the methods to improve the color stability and intensity of anthocyanin extract. This study aimed to do the copigmentation of the anthocyanin extract of purple sweet potato using ferulic acid and tannic acid. The anthocyanin extraction was conducted with distilled water at pH 7 and pH 2 while the copigmentation was conducted by varying the concentration of ferulic acid and tannic acid. The results showed that best anthocyanin extraction method of the purple sweet potato was using distilled water at pH 2. The yield of freeze dried anthocyanin on the extraction with distilled water at pH 2 was 1710 ppm, while the yield when using distilled water at pH 7 was 888 ppm. Ferulic acid and tannic acid can be used for the copigmentation of anthocyanin extract of purple sweet potato by observing the maximum wavelength shift (bathochromic effect, Δλmax) and increase of color intensity (hyperchromic effect, ΔAmax). The bathochromic effect of ferulic acid began to occur at a concentration of 0.01M, while the hypochromic effect on tannic acid occurred at a concentration of 0.005M and remained up to a concentration of 0.02M. The best copigmentation concentration of ferulic acid was 0.015M, while tannic acid was 0.02M. The use of tannic acid 0.02M is recommended compared to ferulic acid 0.015M because with the same bathocromic effect (Δλmaks = 3,9) results hyperchromic effect (ΔA = 0,258) higher by tannic acid.

Ultrasound-assisted extraction of amino acids from grapes.

PubMed

Carrera, Ceferino; Ruiz-Rodríguez, Ana; Palma, Miguel; Barroso, Carmelo G

2015-01-01

Recent cultivar techniques on vineyards can have a marked influence on the final nitrogen content of grapes, specifically individual amino acid contents. Furthermore, individual amino acid contents in grapes are related to the final aromatic composition of wines. A new ultrasound-assisted method for the extraction of amino acids from grapes has been developed. Several extraction variables, including solvent (water/ethanol mixtures), solvent pH (2-7), temperature (10-70°C), ultrasonic power (20-70%) and ultrasonic frequency (0.2-1.0s(-)(1)), were optimized to guarantee full recovery of the amino acids from grapes. An experimental design was employed to optimize the extraction parameters. The surface response methodology was used to evaluate the effects of the extraction variables. The analytical properties of the new method were established, including limit of detection (average value 1.4mmolkg(-)(1)), limit of quantification (average value 2.6mmolkg(-)(1)), repeatability (average RSD=12.9%) and reproducibility (average RSD=15.7%). Finally, the new method was applied to three cultivars of white grape throughout the ripening period. Copyright © 2014 Elsevier B.V. All rights reserved.

Ultrasound-assisted extraction (UAE) and solvent extraction of papaya seed oil: yield, fatty acid composition and triacylglycerol profile.

PubMed

Samaram, Shadi; Mirhosseini, Hamed; Tan, Chin Ping; Ghazali, Hasanah Mohd

2013-10-10

The main objective of the current work was to evaluate the suitability of ultrasound-assisted extraction (UAE) for the recovery of oil from papaya seed as compared to conventional extraction techniques (i.e., Soxhlet extraction (SXE) and solvent extraction (SE)). In the present study, the recovery yield, fatty acid composition and triacylglycerol profile of papaya seed oil obtained from different extraction methods and conditions were compared. Results indicated that both solvent extraction (SE, 12 h/25 °C) and ultrasound-assisted extraction (UAE) methods recovered relatively high yields (79.1% and 76.1% of total oil content, respectively). Analysis of fatty acid composition revealed that the predominant fatty acids in papaya seed oil were oleic (18:1, 70.5%-74.7%), palmitic (16:0, 14.9%-17.9%), stearic (18:0, 4.50%-5.25%), and linoleic acid (18:2, 3.63%-4.6%). Moreover, the most abundant triacylglycerols of papaya seed oil were triolein (OOO), palmitoyl diolein (POO) and stearoyl oleoyl linolein (SOL). In this study, ultrasound-assisted extraction (UAE) significantly (p < 0.05) influenced the triacylglycerol profile of papaya seed oil, but no significant differences were observed in the fatty acid composition of papaya seed oil extracted by different extraction methods (SXE, SE and UAE) and conditions.

Military Training Lands Historic Context: Large Arms Ranges

DTIC Science & Technology

2010-03-01

materials. The associated materials used with flamethrowers included gasoline and Diesel oil, and coconut fatty acids , oleic acids , and naphthenic acids ...The supply of loaded ammunition clips was replenished. At the command CEASE FIRING, the firer removed his foot from the 40mm anti-aircraft gun firing...to fire. If the misfired round could not be extracted in the normal manner, it was removed under the direct supervision of an officer using a

Understanding the similarities and differences between ozone and peroxone in the degradation of naphthenic acids: Comparative performance for potential treatment.

PubMed

Meshref, Mohamed N A; Klamerth, Nikolaus; Islam, Md Shahinoor; McPhedran, Kerry N; Gamal El-Din, Mohamed

2017-08-01

Ozonation at high doses is a costly treatment for oil sands process-affected water (OSPW) naphthenic acids (NAs) degradation. To decrease costs and limit doses, different peroxone (hydrogen peroxide/ozone; H 2 O 2 :O 3 ) processes using mild-ozone doses of 30 and 50 mg/L were investigated. The degradation efficiency of O x -NAs (classical (O 2 -NAs) + oxidized NAs) improved from 58% at 30 mg/L ozone to 59%, 63% and 76% at peroxone (1:1), 50 mg/L ozone, and peroxone (1:2), respectively. Suppressing the hydroxyl radical (•OH) pathway by adding tert-butyl alcohol did significantly reduce the degradation in all treatments, while molecular ozone contribution was around 50% and 34% for O 2 -NAs and O x -NAs, respectively. Structure reactivity toward degradation was observed with degradation increase for both O 2 -NAs and O x -NAs with increase of both carbon (n) and hydrogen deficiency/or |-Z| numbers in all treatments. However, the combined effect of n and Z showed specific insights and differences between ozone and peroxone treatments. The degradation pathway for |-Z|≥10 isomers in ozone treatments through molecular ozone was significant compared to •OH. Though peroxone (1:2) highly reduced the fluorophore organics and toxicity to Vibrio fischeri, the best oxidant utilization in the degradation of O 2 -NAs (mg/L) per ozone dose (mg/L) was observed in the peroxone (1:1) (0.91) and 30 mg/L ozone treatments (0.92). At n = 9-11, peroxone (1:1) had similar or enhanced effect on the O 2 -NAs degradation compared to 50 mg/L ozone. Enhancing •OH pathway through peroxone versus ozone may be an effective OSPW treatment that will allow its safe release into receiving environments with marginal cost addition. Copyright © 2017 Elsevier Ltd. All rights reserved.

Degradation of recalcitrant naphthenic acids from raw and ozonated oil sands process-affected waters by a semi-passive biofiltration process.

PubMed

Zhang, Lei; Zhang, Yanyan; Gamal El-Din, Mohamed

2018-04-15

In this study, a fixed-bed biofiltration system (biofilter) that utilized indigenous microorganisms was developed for the reclamation of oil sands process-affected water (OSPW). With the assistance of quantitative polymerase chain reaction (qPCR) and confocal laser scanning microscopy (CLSM), indigenous microorganisms from OSPW were able to attach to the surface of sand media and form biofilms. The number of total bacteria on the biofilter media reached a steady state (10 9 /g) after 23 days of operation. Ultra Performance Liquid Chromatography/High Resolution Mass Spectrometry (UPLC/HRMS) analysis showed that 21.8% of the classical naphthenic acids (NAs) removal was achieved through the circulation of raw OSPW on the biofilter for 8 times (equivalent to a hydraulic retention time of 16 h). When ozonation with utilized ozone dose of 30 mg/L was applied as pretreatment, the classical NAs in the ozonated OSPW were removed by 89.3% with an accelerated biodegradation rate of 0.5 mg/L/h. Compared with other biofilm reactors such as moving bed biofilm reactor (MBBR), ozonation pretreatment could benefit the biodegradation of NAs in the biofilter more (classical NA removal: 89.3% vs. 34.4%), especially for those with high carbon number and cyclicity. The combined ozonation-biofiltration process could remove 92.7% of classical NAs from raw OSPW in 16 h. Although both ozonation and biofiltration alone did not show degradation of oxidized NAs from raw OSPW, the combined process led to a 52.9% and 42.6% removal for O 3 -NAs and O 4 -NAs, respectively, which were the dominant oxidized NA species in OSPW. Metagenomic sequencing analysis showed that Rhodococcus was the dominant bacterial genus on the sand media, which may play a crucial role during the NA biodegradation. With the advantage of high NA removal efficiency, the combined ozonation-biofiltration process is a promising approach for NA degradation and shows high potential to be scaled up for in-situ OSPW

Extraction of steroidal glucosiduronic acids from aqueous solutions by anionic liquid ion-exchangers

PubMed Central

Mattox, Vernon R.; Litwiller, Robert D.; Goodrich, June E.

1972-01-01

A pilot study on the extraction of three steroidal glucosiduronic acids from water into organic solutions of liquid ion-exchangers is reported. A single extraction of a 0.5mm aqueous solution of either 11-deoxycorticosterone 21-glucosiduronic acid or cortisone 21-glucosiduronic acid with 0.1m-tetraheptylammonium chloride in chloroform took more than 99% of the conjugate into the organic phase; under the same conditions, the very polar conjugate, β-cortol 3-glucosiduronic acid, was extracted to the extent of 43%. The presence of a small amount of chloride, acetate, or sulphate ion in the aqueous phase inhibited extraction, but making the aqueous phase 4.0m with ammonium sulphate promoted extraction strongly. An increase in the concentration of ion-exchanger in the organic phase also promoted extraction. The amount of cortisone 21-glucosiduronic acid extracted by tetraheptylammonium chloride over the pH range of 3.9 to 10.7 was essentially constant. Chloroform solutions of a tertiary, a secondary, or a primary amine hydrochloride also will extract cortisone 21-glucosiduronic acid from water. The various liquid ion exchangers will extract steroidal glucosiduronic acid methyl esters from water into chloroform, although less completely than the corresponding free acids. The extraction of the glucosiduronic acids from water by tetraheptylammonium chloride occurs by an ion-exchange process; extraction of the esters does not involve ion exchange. PMID:5075264

Evaluation of Military Field-Water Quality. Volume 3. Opportunity Poisons

DTIC Science & Technology

1987-12-01

Acidic chemical cleaners fluoric acid, nitric acid, perchloric Spent acid acid, sulfuric acid Alkalies Miscellaneous caustic products Ammonia, lime...calcium oxide), potassium Alkaline battery fluid hydroxide, sodium hydroxide, sodium Caustic wastewater silicate Cleaning solutions Lye Nonhalogenated...Laboratory chemicals chloride, polychlorinated biphenyls, zinc Paint and varnish removers naphthenate , copper naphthenate , dichloro- Capacitors and

Extraction of valerenic acids from valerian (Valeriana officinalis L.) rhizomes.

PubMed

Boyadzhiev, L; Kancheva, D; Gourdon, C; Metcheva, D

2004-09-01

Extraction of valerenic acids (valerenic, acetoxyvalerenic and hydroxyvalerenic) from dry ground rhizomes of valerian (Valeriana officinalis L.) was studied. The effect of ethanol concentration in the solvent, extraction temperature and drug particle size on extraction kinetics were investigated and the optimum values of these process parameters were determined for the case of intensively stirred two-phase dispersion. It was found that increased processing temperature favors extraction kinetics, but provokes moderate degradation of valerenic acids.

PROCESS FOR PRODUCING ALKYL ORTHOPHOSPHORIC ACID EXTRACTANTS

DOEpatents

Grinstead, R.R.

1962-01-23

A process is given for producing superior alkyl orthophosphoric acid extractants for use in solvent extraction methods to recover and purify various metals such as uranium and vanadium. The process comprises slurrying P/sub 2/O/ sub 5/ in a solvent diluent such as kerosene, benzene, isopropyl ether, and the like. An alipbatic alcohol having from nine to seventeen carbon atoms, and w- hcrein ihc OH group is situated inward of the terminal carbon atoms, is added to the slurry while the reaction temperature is mainiained below 60 deg C. The alcohol is added in the mole ratio of about 2 to l, alcohol to P/sub 2/O/sub 5/. A pyrophosphate reaotion product is formed in the slurry-alcohol mixture. Subsequently, the pyrophosphate reaction product is hydrolyzed with dilute mineral acid to produce the desired alkyl orthophosphoric aeid extractant. The extraetant may then be separated and utilized in metal-recovery, solvent- extraction processes. (AEC)

Polydopamine-coated magnetic molecularly imprinted polymer for the selective solid-phase extraction of cinnamic acid, ferulic acid and caffeic acid from radix scrophulariae sample.

PubMed

Yin, Yuli; Yan, Liang; Zhang, Zhaohui; Wang, Jing; Luo, Ningjing

2016-04-01

We describe novel cinnamic acid polydopamine-coated magnetic imprinted polymers for the simultaneous selective extraction of cinnamic acid, ferulic acid and caffeic acid from radix scrophulariae sample. The novel magnetic imprinted polymers were synthesized by surface imprinting polymerization using magnetic multi-walled carbon nanotubes as the support material, cinnamic acid as the template and dopamine as the functional monomer. The magnetic imprinted polymers were characterized by transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The results revealed that the magnetic imprinted polymers had outstanding magnetic properties, high adsorption capacity, selectivity and fast kinetic binding toward cinnamic acid, ferulic acid and caffeic acid. Coupled with high-performance liquid chromatography, the extraction conditions of the magnetic imprinted polymers as a magnetic solid-phase extraction sorbent were investigated in detail. The proposed imprinted magnetic solid phase extraction procedure has been used for the purification and enrichment of cinnamic acid, ferulic acid and caffeic acid successfully from radix scrophulariae extraction sample with recoveries of 92.4-115.0% for cinnamic acid, 89.4-103.0% for ferulic acid and 86.6-96.0% for caffeic acid. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chlorogenic acid stability in pressurized liquid extraction conditions.

PubMed

Wianowska, Dorota; Typek, Rafał; Dawidowicz, Andrzej L

2015-01-01

Chlorogenic acids (CQAs) are phenolic compounds naturally occurring in all higher plants. They are potentially useful in pharmaceuticals, foodstuffs, food additives, and cosmetics due to their recently suggested biomedical activity. Hence, research interest in CQA properties, their isomers, and natural occurrence has been growing. Pressurized liquid extraction (PLE) is regarded as an effective and quick sample preparation method in plant analysis. The short time of PLE decreases the risk of chemical degradation of extracted compounds, thus increasing the attractiveness of its application. However, PLE applied for plant sample preparation is not free from limitations. We found that trans-5-O-caffeoylquinic acid (trans-5-CQA), the main CQA isomer, isomerizes to 3- and 4-O-caffeoylquinic acids and undergoes transesterification, hydrolysis, and reaction with water even in rapid PLE. Moreover, the number and concentration of trans-5-CQA derivatives formed in PLE strongly depends on extractant composition, its pH, and extraction time and temperature. It was not possible to find the PLE conditions in which the transformation process of trans-5-CQA would be eliminated.

A novel extractive fermentation process for propionic acid production from whey lactose

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

Lewis, V.P.; Yang, Shangtian

An extractive fermentation process was developed to produce propionate from lactose. The bacterium Propionibacterium acidipropionici was immobilized in a spiral wound, fibrous matrix packed in the reactor. Propionic acid is the major product from lactose fermentation, with acetic acid and carbon dioxide as byproducts. Propionic acid is a strong inhibitor to this fermentation. A tertiary amine was used to selectively extract propionic acid from the bioreactor, hence enhancing reactor productivity by over 100%. The authors also speculate that by selectively extracting propionic acid, lactose metabolism can be directed to yield more propionate and less byproducts. Other advantages of extractive fermentationmore » include better pH control and a purer product. The propionic acid present in the extractant can be easily stripped with small amounts of an alkaline solution, resulting in a concentrated propionate salt. The extractant was also regenerated in this stripping step. Thus, the process is energy-efficient and economically attractive.« less

Extraction equilibrium of indium(III) from nitric acid solutions by di(2-ethylhexyl)phosphoric acid dissolved in kerosene.

PubMed

Tsai, Hung-Sheng; Tsai, Teh-Hua

2012-01-04

The extraction equilibrium of indium(III) from a nitric acid solution using di(2-ethylhexyl) phosphoric acid (D2EHPA) as an acidic extractant of organophosphorus compounds dissolved in kerosene was studied. By graphical and numerical analysis, the compositions of indium-D2EHPA complexes in organic phase and stoichiometry of the extraction reaction were examined. Nitric acid solutions with various indium concentrations at 25 °C were used to obtain the equilibrium constant of InR₃ in the organic phase. The experimental results showed that the extraction distribution ratios of indium(III) between the organic phase and the aqueous solution increased when either the pH value of the aqueous solution and/or the concentration of the organic phase extractant increased. Finally, the recovery efficiency of indium(III) in nitric acid was measured.

Quantifying hydrogen-deuterium exchange of meteoritic dicarboxylic acids during aqueous extraction

NASA Astrophysics Data System (ADS)

Fuller, M.; Huang, Y.

2003-03-01

Hydrogen isotope ratios of organic compounds in carbonaceous chondrites provide critical information about their origins and evolutionary history. However, because many of these compounds are obtained by aqueous extraction, the degree of hydrogen-deuterium (H/D) exchange that occurs during the process needs to be quantitatively evaluated. This study uses compound- specific hydrogen isotopic analysis to quantify the H/D exchange during aqueous extraction. Three common meteoritic dicarboxylic acids (succinic, glutaric, and 2-methyl glutaric acids) were refluxed under conditions simulating the extraction process. Changes in D values of the dicarboxylic acids were measured following the reflux experiments. A pseudo-first order rate law was used to model the H/D exchange rates which were then used to calculate the isotope exchange resulting from aqueous extraction. The degree of H/D exchange varies as a result of differences in molecular structure, the alkalinity of the extraction solution and presence/absence of meteorite powder. However, our model indicates that succinic, glutaric, and 2-methyl glutaric acids with a D of 1800 would experience isotope changes of 38, 10, and 6, respectively during the extraction process. Therefore, the overall change in D values of the dicarboxylic acids during the aqueous extraction process is negligible. We also demonstrate that H/D exchange occurs on the chiral -carbon in 2-methyl glutaric acid. The results suggest that the racemic mixture of 2-methyl glutaric acid in the Tagish Lake meteorite could result from post-synthesis aqueous alteration. The approach employed in this study can also be used to quantify H/D exchange for other important meteoritic compounds such as amino acids.

Electromembrane extraction of zwitterionic compounds as acid or base: comparison of extraction behavior at acidic and basic pHs.

PubMed

Nojavan, Saeed; Pourahadi, Ahmad; Hosseiny Davarani, Saied Saeed; Morteza-Najarian, Amin; Beigzadeh Abbassi, Mojtaba

2012-10-01

This study has performed on electromembrane extraction (EME) of some zwitterionic compounds based on their acidic and basic properties. High performance liquid chromatography (HPLC) equipped with UV detection was used for determination of model compounds. Cetirizine (CTZ) and mesalazine (MS) were chosen as model compounds, and each of them was extracted from acidic (as a cation) and basic (as an anion) sample solutions, separately. 1-Octanol and 2-nitrophenyl octylether (NPOE) were used as the common supported liquid membrane (SLM) solvents. EME parameters, such as extraction time, extraction voltage and pH of donor and acceptor solutions were studied in details for cationic and anionic forms of each model compound and obtained results for two ionic forms (cationic and anionic) of each compound were compared together. Results showed that zwitterionic compounds could be extracted in both cationic and anionic forms. Moreover, it was found that the extraction of anionic form of each model compound could be done in low voltages when 1-octanol was used as the SLM solvent. Results showed that charge type was not highly effective on the extraction efficiency of model compounds whereas the position of charge within the molecule was the key parameter. In optimized conditions, enrichment factors (EF) of 27-60 that corresponded to recoveries ranging from 39 to 86% were achieved. Copyright © 2012 Elsevier B.V. All rights reserved.

Electromembrane extraction using two separate cells: A new design for simultaneous extraction of acidic and basic compounds.

PubMed

Nojavan, Saeed; Asadi, Sakine

2016-02-01

Simultaneous extraction of acidic and basic analytes from a sample is seen to be a challenging task. In this work, a novel and efficient electromembrane extraction (EME) method based on two separate cells was applied to simultaneously extract and preconcentrate two acidic drugs (naproxen and ibuprofen) along with a basic drug (ketamine). Once both cells were filled with the sample solution, basic drug was extracted from one cell with the other cell used to extract acidic drugs. The employed supported liquid membranes for the extraction of acidic and basic drugs were 2-ethyl hexanol and 1-octanol, respectively. Under an applied potential of 250 V in the course of the extraction process, acidic, and basic drugs were extracted from a 3.0 mL aqueous sample solution into 25 μL acceptor solutions. The pH values of the donor and acceptor solutions in the cathodic cell were 5.0 and 1.5, respectively, the corresponding values in the anodic cell were, however, 8.0 and 12.5, respectively. The rates of recovery obtained within 20 min of extraction time at a stirring rate of 750 rpm ranged from 45 to 54%. With correlation coefficients ranging from 0.990 to 0.996, the proposed EME technique provided good linearity over a concentration range of 20-1000 ng/mL. The LOD for all drugs was found to be 6.7 ng/mL, while reproducibility ranged from 7 to 12% (n = 5). Finally, applying the proposed method to determine and quantify the drugs in urine and wastewater samples, satisfactory results were achieved. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of citrus pectin samples extracted under different conditions: influence of acid type and pH of extraction

PubMed Central

Kaya, Merve; Sousa, António G.; Crépeau, Marie-Jeanne; Sørensen, Susanne O.; Ralet, Marie-Christine

2014-01-01

Background and Aims Pectin is a complex macromolecule, the fine structure of which is influenced by many factors. It is used as a gelling, thickening and emulsifying agent in a wide range of applications, from food to pharmaceutical products. Current industrial pectin extraction processes are based on fruit peel, a waste product from the juicing industry, in which thousands of tons of citrus are processed worldwide every year. This study examines how pectin components vary in relation to the plant source (orange, lemon, lime, grapefruit) and considers the influence of extraction conditions on the chemical and macromolecular characteristics of pectin samples. Methods Citrus peel (orange, lemon, lime and grapefruit) from a commercial supplier was used as raw material. Pectin samples were obtained on a bulk plant scale (kilograms; harsh nitric acid, mild nitric acid and harsh oxalic acid extraction) and on a laboratory scale (grams; mild oxalic acid extraction). Pectin composition (acidic and neutral sugars) and physicochemical properties (molar mass and intrinsic viscosity) were determined. Key Results Oxalic acid extraction allowed the recovery of pectin samples of high molecular weight. Mild oxalic acid-extracted pectins were rich in long homogalacturonan stretches and contained rhamnogalacturonan I stretches with conserved side chains. Nitric acid-extracted pectins exhibited lower molecular weights and contained rhamnogalacturonan I stretches encompassing few and/or short side chains. Grapefruit pectin was found to have short side chains compared with orange, lime and lemon. Orange and grapefruit pectin samples were both particularly rich in rhamnogalacturonan I backbones. Conclusions Structural, and hence macromolecular, variations within the different citrus pectin samples were mainly related to their rhamnogalacturonan I contents and integrity, and, to a lesser extent, to the length of their homogalacturonan domains. PMID:25081519

Analysis of Free Amino Acids in Different Extracts of Orthosiphon stamineus Leaves by High-Performance Liquid Chromatography Combined with Solid-Phase Extraction

PubMed Central

Shafaei, Armaghan; Halim, Nor Hidayah Ab; Zakaria, Norhidayah; Ismail, Zhari

2017-01-01

Background: Orthosiphon stamineus (OS) Benth is a medicinal plant and native in Southeast Asia. Previous studies have shown that OS leaves possess antioxidant, cytotoxic, diuretic, antihypertensive, and uricosuric effects. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids, and flavonoids. Objective: To develop and validate an high-performance liquid chromatography (HPLC)-diode array detector (DAD) method combined with solid-phase extraction that involves precolumn derivatization with O-phthaladehyde for simultaneous analysis of free amino acids in OS leaves extracts. Materials and Methods: OS leaves were extracted with water (OS-W), ethanol (OS-E), methanol (OS-M), 50% ethanol (OS-EW), and 50% methanol (OS-MW). The extracts were treated by C18 cartridge before derivatization, resulting in great improvement of separation by Zorbox Eclipse XDB-C18 column. Results: The HPLC–DAD method was successfully developed and validated for analyzing the contents of free amino acids in OS extracts. The results showed that l-aspartic acid with 0.93 ± 0.01 nmol/mg was the major free amino acid in OS-W extract. However, in OS-E, OS-M, OS-EW, and OS-MW, l-glutamic acid with 3.53 ± 0.16, 2.17 ± 0.10, 4.01 ± 0.12, and 2.49 ± 0.12 nmol/mg, respectively, was the major free amino acid. Subsequently, l-serine, which was detected in OS-W, OS-E, and OS-M, was the minor free amino acid with 0.33 ± 0.02, 0.12 ± 0.01, and 0.06 ± 0.01 nmol/mg, respectively. However, l-threonine with 0.26 ± 0.02 and 0.19 ± 0.08 nmol/mL in OS-EW and OS-MW, respectively, had the lowest concentration compared with other amino acid components. Conclusion: All validation parameters of the developed method indicate that the method is reliable and efficient to simultaneously determine the free amino acids content for routine analysis of OS extracts. SUMMARY The HPLC-DAD method combined with solid phase extraction was

Analysis of Free Amino Acids in Different Extracts of Orthosiphon stamineus Leaves by High-Performance Liquid Chromatography Combined with Solid-Phase Extraction.

PubMed

Shafaei, Armaghan; Halim, Nor Hidayah Ab; Zakaria, Norhidayah; Ismail, Zhari

2017-10-01

Orthosiphon stamineus (OS) Benth is a medicinal plant and native in Southeast Asia. Previous studies have shown that OS leaves possess antioxidant, cytotoxic, diuretic, antihypertensive, and uricosuric effects. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids, and flavonoids. To develop and validate an high-performance liquid chromatography (HPLC)-diode array detector (DAD) method combined with solid-phase extraction that involves precolumn derivatization with O -phthaladehyde for simultaneous analysis of free amino acids in OS leaves extracts. OS leaves were extracted with water (OS-W), ethanol (OS-E), methanol (OS-M), 50% ethanol (OS-EW), and 50% methanol (OS-MW). The extracts were treated by C18 cartridge before derivatization, resulting in great improvement of separation by Zorbox Eclipse XDB-C 18 column. The HPLC-DAD method was successfully developed and validated for analyzing the contents of free amino acids in OS extracts. The results showed that l-aspartic acid with 0.93 ± 0.01 nmol/mg was the major free amino acid in OS-W extract. However, in OS-E, OS-M, OS-EW, and OS-MW, l-glutamic acid with 3.53 ± 0.16, 2.17 ± 0.10, 4.01 ± 0.12, and 2.49 ± 0.12 nmol/mg, respectively, was the major free amino acid. Subsequently, l-serine, which was detected in OS-W, OS-E, and OS-M, was the minor free amino acid with 0.33 ± 0.02, 0.12 ± 0.01, and 0.06 ± 0.01 nmol/mg, respectively. However, l-threonine with 0.26 ± 0.02 and 0.19 ± 0.08 nmol/mL in OS-EW and OS-MW, respectively, had the lowest concentration compared with other amino acid components. All validation parameters of the developed method indicate that the method is reliable and efficient to simultaneously determine the free amino acids content for routine analysis of OS extracts. The HPLC-DAD method combined with solid phase extraction was successfully developed and validated for simultaneous determination and

Ellagic acid, phenolic acids, and flavonoids in Malaysian honey extracts demonstrate in vitro anti-inflammatory activity.

PubMed

Kassim, Mustafa; Achoui, Mouna; Mustafa, Mohd Rais; Mohd, Mustafa Ali; Yusoff, Kamaruddin Mohd

2010-09-01

Natural honey has been used in traditional medicine of different cultures throughout the world. This study looked into the extraction of Malaysian honey and the evaluation of the anti-inflammatory activity of these extracts. It was hypothesized that honey extracts contain varying amounts of phenolic compounds and that they possess different in vitro anti-inflammatory activities. Honey extracts were analyzed using liquid chromatography-mass spectrometry to identify and compare phenolic compounds, whereas high-performance liquid chromatography was used for their quantification. Subsequently, honey methanol extract (HME) and honey ethyl acetate extract (HEAE) were tested in vitro for their effect on nitric oxide production in stimulated macrophages. The extracts were also tested for their effects on tumor necrosis factor-α (TNF) cytotoxicity in L929 cells. The major phenolics in the extracts were ellagic, gallic, and ferulic acids; myricetin; chlorogenic acid; and caffeic acid. Other compounds found in lower concentrations were hesperetin, p-coumaric acid, chrysin, quercetin, luteolin, and kaempferol. Ellagic acid was the most abundant of the phenolic compounds recorded, with mean concentrations of 3295.83 and 626.74 μg/100 g of honey in HME and HEAE, respectively. The median maximal effective concentrations for in vitro nitric oxide inhibition by HEAE and HME were calculated to be 37.5 and 271.7 μg/mL, respectively. The median maximal effective concentrations for protection from TNF cytotoxicity by HEAE and HME were 168.1 and 235.4 μg/mL, respectively. In conclusion, HEAE exhibited greater activity in vitro, whereas HME contained a higher concentration of phenolic compounds per 100 g of honey. Copyright © 2010 Elsevier Inc. All rights reserved.

21 CFR 573.500 - Condensed, extracted glutamic acid fermentation product.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Condensed, extracted glutamic acid fermentation product. 573.500 Section 573.500 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND... fermentation product. Condensed, extracted glutamic acid fermentation product may be safely used in animal feed...

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.

Investigation of Pu(IV)-acetohydroxamic acid complex by solvent extraction with di(2-ethylhexyl) phosphoric acid

NASA Astrophysics Data System (ADS)

Brown, M. Alex; Paulenova, Alena; Tkac, Peter

2010-03-01

The stability constant of the Pu(IV)-acetohydroxamic acid complex Pu(AHA)3+ at 1 M ionic strength (pH = 0) has been investigated by method of solvent extraction. Di(2-ethylhexyl) phosphoric acid (HDEHP) was used to extract Pu(IV) from perchloric and nitric acid media at various AHA concentrations. Distribution ratios over a range of ligand concentrations were used in conjunction with graphical methods to obtain logβ1 = 14.3 ± 0.03 in perchloric acid. The stability constant determined from solutions in nitric acid was excluded because of the uncertainty in plutonium speciation.

Pharmacological activities of the organic extracts and fatty acid composition of the petroleum ether extract from Haplophyllum tuberculatum leaves.

PubMed

Hamdi, Assia; Majouli, Kaouther; Abdelhamid, Amal; Marzouk, Belsem; Belghith, Hèla; Chraief, Imed; Bouraoui, Abderrahman; Marzouk, Zohra; Heyden, Yvan Vander

2018-04-24

Haplophyllum tuberculatum is used in traditional medicine to treat many disorders including inflammation and pain. The aim of this study is to investigate the organic extracts from H. tuberculatum leaves against inflammation, gastric ulcer and pain. Acute toxicity was studied in vivo to determine the toxic doses of the organic extracts. Anti-inflammatory activity was also evaluated in vivo using carrageenan-induced paw edema in Wistar rats. Gastroprotective activity was tested using the HCl/ethanol-induced gastric ulcer test in rats. Peripheral and central analgesic activities were assessed using the acetic acid-induced writhing test and the hot-plate method, respectively. The chemical composition of the fatty acids in the petroleum ether (PE) extract was determined with GC-MS. At 25, 50 and 100mg/kg PE extract was the most active against inflammation. Percentages inhibition 5h after carrageenan-injection were 51.12; 86.71% and 96.92%, respectively. The same extract at 100mg/kg showed good analgesic activities using the acetic acid-induced writhing test and the hot-plate method. The chloroform, ethyl acetate (EtOAc) and butanolic (n-BuOH) extracts exhibited strong anti-inflammatory, gastroprotective and analgesic activities at 100mg/kg. The GC-FID analysis revealed that the PE extract was rich in γ-linolenic acid (45.50%) followed by palmitic acid (18.48%), linoleic acid (10.73%), erucic acid (4.72), stearic acid (3.96%) and oleic acid (2.57%). The results of the present study support the traditional use of the leaves of H. tuberculatum and may possibly serve as prospective material for further development of safe new phytochemical anti-inflammatory, gastroprotective and/or analgesic agents. Copyright © 2018 Elsevier B.V. All rights reserved.

Production of High Density Aviation Fuels via Novel Zeolite Catalyst Routes

DTIC Science & Technology

1989-10-23

range fraction of a naphthenic crude; saturation of an aromatic FCC cycle stock I the appropriate boiling range: saturation of an appropriate boiling...aromatic hydrocarbons and selected aromatic feedstocks to the corresponding mono- and dicyclic naphthenes in the aviation turbine fuel boiling range; and...Paraffins from Naphthenic Refinery Feed Streams .......... 8 Solvent Extraction ........................................... 8 Shape Selective Catalytic

Hydrothermal-acid treatment for effectual extraction of eicosapentaenoic acid (EPA)-abundant lipids from Nannochloropsis salina.

PubMed

Lee, Ilgyu; Han, Jong-In

2015-09-01

Hydrothermal acid treatment, was adopted to extract eicosapentaenoic acid (EPA) from wet biomass of Nannochloropsis salina. It was found that sulfuric acid-based treatment increased EPA yield from 11.8 to 58.1 mg/g cell in a way that was nearly proportional to its concentration. Nitric acid exhibited the same pattern at low concentrations, but unlike sulfuric acid its effectiveness unexpectedly dropped from 0.5% to 2.0%. The optimal and minimal conditions for hydrothermal acid pretreatment were determined using a statistical approach; its maximum EPA yield (predicted: 43.69 mg/g cell; experimental: 43.93 mg/g cell) was established at a condition of 1.27% of sulfuric acid, 113.34 °C of temperature, and 36.71 min of reaction time. Our work demonstrated that the acid-catalyzed cell disruption, accompanied by heat, can be one potentially promising option for ω-3 fatty acids extraction. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

Alkaline earth cation extraction from acid solution

DOEpatents

Dietz, Mark; Horwitz, E. Philip

2003-01-01

An extractant medium for extracting alkaline earth cations from an aqueous acidic sample solution is described as are a method and apparatus for using the same. The separation medium is free of diluent, free-flowing and particulate, and comprises a Crown ether that is a 4,4'(5')[C.sub.4 -C.sub.8 -alkylcyclohexano]18-Crown-6 dispersed on an inert substrate material.

Membrane-mediated extractive fermentation for lactic acid production from cellulosic biomass

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

Chen, Rongfu; Lee, Y.Y.

1997-12-31

Lactic acid production from cellulosic biomass by cellulose and Lactobacillus delbrueckii was studied in a fermenter-extractor employing a microporous hollow fiber membrane (NIHF). This bioreactor system was operated under a fed-batch mode with continuous removal of lactic acid by an in 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%more » 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. 20 refs., 10 figs., 1 tab.« less

Production of lactic acid from hemicellulose extracts by Bacillus coagulans MXL-9.

PubMed

Walton, Sara L; Bischoff, Kenneth M; van Heiningen, Adriaan R P; van Walsum, G Peter

2010-08-01

Bacillus coagulans MXL-9 was found capable of growing on pre-pulping hemicellulose extracts, utilizing all of the principle monosugars found in woody biomass. This organism is a moderate thermophile isolated from compost for its pentose-utilizing capabilities. It was found to have high tolerance for inhibitors such as acetic acid and sodium, which are present in pre-pulping hemicellulose extracts. Fermentation of 20 g/l xylose in the presence of 30 g/l acetic acid required a longer lag phase but overall lactic acid yield was not diminished. Similarly, fermentation of xylose in the presence of 20 g/l sodium increased the lag time but did not affect overall product yield, though 30 g/l sodium proved completely inhibitory. Fermentation of hot water-extracted Siberian larch containing 45 g/l total monosaccharides, mainly galactose and arabinose, produced 33 g/l lactic acid in 60 h and completely consumed all sugars. Small amounts of co-products were formed, including acetic acid, formic acid, and ethanol. Hemicellulose extract formed during autohydrolysis of mixed hardwoods contained mainly xylose and was converted into lactic acid with a 94% yield. Green liquor-extracted hardwood hemicellulose containing 10 g/l acetic acid and 6 g/l sodium was also completely converted into lactic acid at a 72% yield. The Bacillus coagulans MXL-9 strain was found to be well suited to production of lactic acid from lignocellulosic biomass due to its compatibility with conditions favorable to industrial enzymes and its ability to withstand inhibitors while rapidly consuming all pentose and hexose sugars of interest at high product yields.

Extraction of Oleic Acid from Moroccan Olive Mill Wastewater

PubMed Central

Elkacmi, Reda; Kamil, Noureddine; Bennajah, Mounir; Kitane, Said

2016-01-01

The production of olive oil in Morocco has recently grown considerably for its economic and nutritional importance favored by the country's climate. After the extraction of olive oil by pressing or centrifuging, the obtained liquid contains oil and vegetation water which is subsequently separated by decanting or centrifugation. Despite its treatment throughout the extraction process, this olive mill wastewater, OMW, still contains a very important oily residue, always regarded as a rejection. The separated oil from OMW can not be intended for food because of its high acidity of 3.397% which exceeds the international standard for human consumption defined by the standard of the Codex Alimentarius, proving its poor quality. This work gives value addition to what would normally be regarded as waste by the extraction of oleic acid as a high value product, using the technique of inclusion with urea for the elimination of saturated and unsaturated fatty acids through four successive crystallizations at 4°C and 20°C to have a final phase with oleic acid purity of 95.49%, as a biodegradable soap and a high quality glycerin will be produced by the reaction of saponification and transesterification. PMID:26933663

Extraction of Oleic Acid from Moroccan Olive Mill Wastewater.

PubMed

Elkacmi, Reda; Kamil, Noureddine; Bennajah, Mounir; Kitane, Said

2016-01-01

The production of olive oil in Morocco has recently grown considerably for its economic and nutritional importance favored by the country's climate. After the extraction of olive oil by pressing or centrifuging, the obtained liquid contains oil and vegetation water which is subsequently separated by decanting or centrifugation. Despite its treatment throughout the extraction process, this olive mill wastewater, OMW, still contains a very important oily residue, always regarded as a rejection. The separated oil from OMW can not be intended for food because of its high acidity of 3.397% which exceeds the international standard for human consumption defined by the standard of the Codex Alimentarius, proving its poor quality. This work gives value addition to what would normally be regarded as waste by the extraction of oleic acid as a high value product, using the technique of inclusion with urea for the elimination of saturated and unsaturated fatty acids through four successive crystallizations at 4°C and 20°C to have a final phase with oleic acid purity of 95.49%, as a biodegradable soap and a high quality glycerin will be produced by the reaction of saponification and transesterification.

Varying Conditions for Hexanoic Acid Degradation with BioTiger™

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

Foreman, Koji; Milliken, Charles; Brigmon, Robin

BioTiger™ (BT) is a consortium of 12 bacteria designed for petroleum waste biodegradation. BT is currently being studied and could be considered for bioremediation of the Athabasca oil sands refineries in Canada and elsewhere. The run-off ponds from the petroleum extraction processes, called tailings ponds, are a mixture of polycyclic aromatic hydrocarbons, naphthenic acids, hydrocarbons, toxic chemicals like heavy metals, water, and sand. Due to environmental regulations the oil industry would like to separate and degrade the hazardous chemical species from the tailings ponds while recycling the water. It has been shown that BT at 30 C° is able tomore » completely degrade 10 mM hexanoic acid (HA) co-metabolically with 0.2% yeast extract (w/v) in 48 hours when starting at 0.4 OD 600nm. After establishing this stable degradation capability, variations were tested to explore the wider parameters of BT activity in temperature, pH, intermediate degradation, co-metabolic dependence, and transfer stability. Due to the vast differences in temperature at various points in the refineries, a wide range of temperatures were assessed. The results indicate that BT retains the ability to degrade HA, a model surrogate for tailings pond contaminants, at temperatures ranging from 15°C to 35°C. Hexanamide (HAM) was shown to be an intermediate generated during the degradation of HA in an earlier work and HAM is completely degraded after 48 hours, indicating that HAM is not the final product of HA degradation. Various replacements for yeast extract were attempted. Glucose, a carbon source; casein amino acids, a protein source; additional ammonia, mimicking known media; and additional phosphate with Wolffe’s vitamins and minerals all showed no significant degradation of HA compared to control. Decreasing the yeast extract concentration (0.05%) demonstrated limited but significant degradation. Finally, serial inoculations of BT were performed to determine the stability of

Extractive Fermentation of Lactic Acid in Lactic Acid Bacteria Cultivation: A Review.

PubMed

Othman, Majdiah; Ariff, Arbakariya B; Rios-Solis, Leonardo; Halim, Murni

2017-01-01

Lactic acid bacteria are industrially important microorganisms recognized for their fermentative ability mostly in their probiotic benefits as well as lactic acid production for various applications. Nevertheless, lactic acid fermentation often suffers end-product inhibition which decreases the cell growth rate. The inhibition of lactic acid is due to the solubility of the undissociated lactic acid within the cytoplasmic membrane and insolubility of dissociated lactate, which causes acidification of cytoplasm and failure of proton motive forces. This phenomenon influences the transmembrane pH gradient and decreases the amount of energy available for cell growth. In general, the restriction imposed by lactic acid on its fermentation can be avoided by extractive fermentation techniques, which can also be exploited for product recovery.

Extractive Fermentation of Lactic Acid in Lactic Acid Bacteria Cultivation: A Review

PubMed Central

Othman, Majdiah; Ariff, Arbakariya B.; Rios-Solis, Leonardo; Halim, Murni

2017-01-01

Lactic acid bacteria are industrially important microorganisms recognized for their fermentative ability mostly in their probiotic benefits as well as lactic acid production for various applications. Nevertheless, lactic acid fermentation often suffers end-product inhibition which decreases the cell growth rate. The inhibition of lactic acid is due to the solubility of the undissociated lactic acid within the cytoplasmic membrane and insolubility of dissociated lactate, which causes acidification of cytoplasm and failure of proton motive forces. This phenomenon influences the transmembrane pH gradient and decreases the amount of energy available for cell growth. In general, the restriction imposed by lactic acid on its fermentation can be avoided by extractive fermentation techniques, which can also be exploited for product recovery. PMID:29209295

Study on the extraction, purification and quantification of jasmonic acid, abscisic acid and indole-3-acetic acid in plants.

PubMed

Zhang, Feng Juan; Jin, You Ju; Xu, Xing You; Lu, Rong Chun; Chen, Hua Jun

2008-01-01

Jasmonic acid (JA), abscisic acid (ABA) and indole-3-acetic acid (IAA) are important plant hormones. Plant hormones are difficult to analyse because they occur in small concentrations and other substances in the plant interfere with their detection. To develop a new, inexpensive procedure for the rapid extraction and purification of IAA, ABA and JA from various plant species. Samples were prepared by extraction of plant tissues with methanol and ethyl acetate. Then the extracts were further purified and enriched with C(18) cartridges. The final extracts were derivatised with diazomethane and then measured by GC-MS. The results of the new methodology were compared with those of the Creelman and Mullet procedure. Sequential elution of the assimilates from the C(18 )cartridges revealed that IAA and ABA eluted in 40% methanol, while JA subsequently eluted in 60% methanol. The new plant hormone extraction and purification procedure produced results that were comparable to those obtained with the Creelman and Mullet's procedure. This new procedure requires only 0.5 g leaf samples to quantify these compounds with high reliability and can simultaneously determine the concentrations of the three plant hormones. A simple, inexpensive method was developed for determining endogenous IAA, ABA and JA concentrations in plant tissue.

Extraction and the Fatty Acid Profile of Rosa acicularis Seed Oil.

PubMed

Du, Huanan; Zhang, Xu; Zhang, Ruchun; Zhang, Lu; Yu, Dianyu; Jiang, Lianzhou

2017-12-01

Rosa acicularis seed oil was extracted from Rosa acicularis seeds by the ultrasonic-assisted aqueous enzymatic method using cellulase and protease. Based on a single experiment, Plackett-Burman design was applied to ultrasonic-assisted aqueous enzymatic extraction of wild rose seed oil. The effects of enzyme amount, hydrolysis temperature and initial pH on total extraction rate of wild rose seed oil was studied by using Box-Behnken optimize methodology. Chemical characteristics of a sample of Rosa acicularis seeds and Rosa acicularis seed oil were characterized in this work. The tocopherol content was 200.6±0.3 mg/100 g oil. The Rosa acicularis seed oil was rich in linoleic acid (56.5%) and oleic acid (34.2%). The saturated fatty acids included palmitic acid (4%) and stearic acid (2.9%). The major fatty acids in the sn-2 position of triacylglycerol in Rosa acicularis oil were linoleic acid (60.6%), oleic acid (33.6%) and linolenic acid (3.2%). According to the 1,3-random-2-random hypothesis, the dominant triacylglycerols were LLL (18%), LLnL (1%), LLP (2%), LOL (10%), LLSt (1.2%), PLP (0.2%), LLnP (0.1%), LLnO (0.6%) and LOP (1.1%). This work could be useful for developing applications for Rosa acicularis seed oil.

Microwave-assisted organic acids extraction of chromate copper arsenate (CCA)-treated southern pine

Treesearch

Bin Yu; Chung Y. Hse; Todd F. Shupe

2010-01-01

The extraction effects of acid concentration, reaction time and temperature in a microwave reactor on recovery of CCA-treated wood were evaluated. Extraction of copper, chromium, and arsenic metals from chromated copper arsenate (CCA)-treated southern pine wood samples with two different organic acids (i.e., acetic acid and oxalic acid) was investigated using a...

Validated Method for the Characterization and Quantification of Extractable and Nonextractable Ellagitannins after Acid Hydrolysis in Pomegranate Fruits, Juices, and Extracts.

PubMed

García-Villalba, Rocío; Espín, Juan Carlos; Aaby, Kjersti; Alasalvar, Cesarettin; Heinonen, Marina; Jacobs, Griet; Voorspoels, Stefan; Koivumäki, Tuuli; Kroon, Paul A; Pelvan, Ebru; Saha, Shikha; Tomás-Barberán, Francisco A

2015-07-29

Pomegranates are one of the main highly valuable sources of ellagitannins. Despite the potential health benefits of these compounds, reliable data on their content in pomegranates and derived extracts and food products is lacking, as it is usually underestimated due to their complexity, diversity, and lack of commercially available standards. This study describes a new method for the analysis of the extractable and nonextractable ellagitannins based on the quantification of the acid hydrolysis products that include ellagic acid, gallic acid, sanguisorbic acid dilactone, valoneic acid dilactone, and gallagic acid dilactone in pomegranate samples. The study also shows the occurrence of ellagitannin C-glycosides in pomegranates. The method was optimized using a pomegranate peel extract. To quantify nonextractable ellagitannins, freeze-dried pomegranate fruit samples were directly hydrolyzed with 4 M HCl in water at 90 °C for 24 h followed by extraction of the pellet with dimethyl sulfoxide/methanol (50:50, v/v). The method was validated and reproducibility was assessed by means of an interlaboratory trial, showing high reproducibility across six laboratories with relative standard deviations below 15%. Their applicability was demonstrated in several pomegranate extracts, different parts of pomegranate fruit (husk, peels, and mesocarp), and commercial juices. A large variability has been found in the ellagitannin content (150-750 mg of hydrolysis products/g) and type (gallagic acid/ellagic acid ratios between 4 and 0.15) of the 11 pomegranate extracts studied.

Study on Process Parameters of Extraction of γ-aminobutyric Acid Instant Moringa oleifera Powder

NASA Astrophysics Data System (ADS)

Tiaokun, Fu; Suhui, Zhang; Neng, Liu; Jihua, Li; Shaodan, Peng; Changqing, Guo; Wei, Zhou

2017-12-01

To preliminary optimize the extraction of γ-aminobutyric acid instant tea powder from Moringa oleifera leaves,taking γ-aminobutyric acid Moringa oleifera leaves as raw material and pure water as extraction solvent and GABA content as the main evaluation index,the effects of extraction temperature, ratio of liquid to material and extraction time on biochemical components and sensory qualities of Moringa oleifera leaves extractor was studied by using one-factor-at-a-time experiment.The results showed shat the optimal extraction conditions for γ-aminobutyric acid instant tea powder were extraction temperature of 60 °C, material-to-water ration of 1:10 and extraction time of 40 min.

Modulation of GABAA receptors by valerian extracts is related to the content of valerenic acid.

PubMed

Trauner, Gabriele; Khom, Sophia; Baburin, Igor; Benedek, Birgit; Hering, Steffen; Kopp, Brigitte

2008-01-01

Valeriana Officinalis L . is a traditionally used sleep remedy, however, the mechanism of action and the substances responsible for its sedative and sleep-enhancing properties are not fully understood. As we previously identified valerenic acid as a subunit-specific allosteric modulator of GABAA receptors, we now investigated the relation between modulation of GABAA receptors by Valerian extracts of different polarity and the content of sesquiterpenic acids (valerenic acid, acetoxyvalerenic acid). All extracts were analysed by HPLC concerning the content of sesquiterpenic acids. GABAA receptors composed of alpha 1, beta 2 and gamma 2S subunits were expressed in Xenopus laevis oocytes and the modulation of chloride currents through GABAA receptors (IGABA) by Valerian extracts was investigated using the two-microelectrode voltage clamp technique. Apolar extracts induced a significant enhancement of IGABA, whereas polar extracts showed no effect. These results were confirmed by fractionating a highly active ethyl acetate extract: again fractions with high contents of valerenic acid exhibited strong receptor activation. In addition, removal of sesquiterpenic acids from the ethyl acetate extract led to a loss of I (GABA) enhancement. In conclusion, our data show that the extent of GABAA receptor modulation by Valerian extracts is related to the content of valerenic acid.

The behavior and importance of lactic acid complexation in Talspeak extraction systems

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

Grimes, Travis S.; Nilsson, Mikael; Nash, Kenneth L.

2008-07-01

Advanced partitioning of spent nuclear fuel in the UREX +la process relies on the TALSPEAK process for separation of fission-product lanthanides from trivalent actinides. The classic TALSPEAK utilizes an aqueous medium of both lactic acid and diethylenetriaminepentaacetic acid and the extraction reagent di(2-ethylhexyl)phosphoric acid in an aromatic diluent. In this study, the specific role of lactic acid and the complexes involved in the extraction of the trivalent actinides and lanthanides have been investigated using {sup 14}C-labeled lactic acid. Our results show that lactic acid partitions between the phases in a complex fashion. (authors)

Nitric Acid and Water Extraction by T2EHDGA in n -Dodecane

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

Campbell, Emily L.; Holfeltz, Vanessa E.; Hall, Gabriel B.

Liquid-liquid distribution behavior of nitric acid (HNO3) and water by a diglycolamide ligand, N,N,N',N'-tetra-2-ethylhexyldiglycolamide (T2EHDGA) into n-dodecane diluent was investigated. Spectroscopic FTIR and NMR characterization of the organic extraction solutions indicate T2EHDGA carbonyl coordinates HNO3 and progressively aggregates at high acid conditions. Water extraction increases in the presence of HNO3. The experimentally observed distribution of HNO3 was modeled using the computer program, SXLSQI. The results indicated that the formation of two organic phase species—HNO3·T2EHDGA and (HNO3)2·T2EHDGA—satisfactory describes the acid transport behavior. Temperature dependent solvent extraction studies allowed for determination of thermodynamic extraction constants and ΔH and ΔS parameters for themore » corresponding extractive processes.« less

Rare Earth Extraction from NdFeB Magnet Using a Closed-Loop Acid Process.

PubMed

Kitagawa, Jiro; Uemura, Ryohei

2017-08-14

There is considerable interest in extraction of rare earth elements from NdFeB magnets to enable recycling of these elements. In practical extraction methods using wet processes, the acid waste solution discharge is a problem that must be resolved to reduce the environmental impact of the process. Here, we present an encouraging demonstration of rare earth element extraction from a NdFeB magnet using a closed-loop hydrochloric acid (HCl)-based process. The extraction method is based on corrosion of the magnet in a pretreatment stage and a subsequent ionic liquid technique for Fe extraction from the HCl solution. The rare earth elements are then precipitated using oxalic acid. Triple extraction has been conducted and the recovery ratio of the rare earth elements from the solution is approximately 50% for each extraction process, as compared to almost 100% recovery when using a one-shot extraction process without the ionic liquid but with sufficient oxalic acid. Despite its reduced extraction efficiency, the proposed method with its small number of procedures at almost room temperature is still highly advantageous in terms of both cost and environmental friendliness. This study represents an initial step towards realization of a closed-loop acid process for recycling of rare earth elements.

Antibacterial effects of roselle calyx extracts and protocatechuic acid in ground beef and apple juice.

PubMed

Chao, Che-Yi; Yin, Mei-Chin

2009-03-01

The antibacterial effects of roselle calyx aqueous and ethanol extracts and protocatechuic acid against food spoilage bacteria Salmonella typhimurium DT104, Escherichia coli O157:H7, Listeria monocytogenes, Staphylococcus aureus, and Bacillus cereus were examined. Minimal inhibitory concentrations of roselle calyx aqueous and ethanol extracts and protocatechuic acid against these bacteria were in the range of 112-144, 72-96, and 24-44 microg/mL, respectively. Protocatechuic acid content in roselle calyx aqueous and ethanol extracts was 2.8 +/- 0.7 and 11.9 +/- 1.2 mg/g, respectively. Antibacterial activity of roselle calyx ethanol extract and protocatechuic acid was not affected by heat treatments from 25 degrees to 75 degrees C and 25 degrees to 100 degrees C, respectively. After 3 days storage at 25 degrees C, the addition of roselle calyx extracts and protocatechuic acid exhibited dose-dependent inhibitory effects against test bacteria in ground beef and apple juice, in which the roselle calyx ethanol extract showed greater antibacterial effects than the aqueous extract. These data suggest that roselle calyx ethanol extract and protocatechuic acid might be potent agents as food additives to prevent contamination from these bacteria.

Effects of ultrahigh pressure extraction on yield and antioxidant activity of chlorogenic acid and cynaroside extracted from flower buds of Lonicera japonica.

PubMed

Hu, Wen; Guo, Ting; Jiang, Wen-Jun; Dong, Guang-Li; Chen, Da-Wei; Yang, Shi-Lin; Li, He-Ran

2015-06-01

The present study was designed to establish and optimize a new method for extracting chlorogenic acid and cynaroside from Lonicera japonica Thunb. through orthogonal experimental designl. A new ultrahigh pressure extraction (UPE) technology was applied to extract chlorogenic acid and cynaroside from L. japonica. The influential factors, including solvent type, ethanol concentration, extraction pressure, time, and temperature, and the solid/liquid ratio, have been studied to optimize the extraction process. The optimal conditions for the UPE were developed by quantitative analysis of the extraction products by HPLC-DAD in comparison with standard samples. In addition, the microstructures of the medicinal materials before and after extraction were studied by scanning electron microscopy (SEM). Furthermore, the extraction efficiency of different extraction methods and the 2, 2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activities of the extracts were investigated. The optimal conditions for extracting chlorogenic acid and cynaroside were as follows: ethanol concentration, 60%; extraction pressure, 400 MPa; extraction time, 2 min; extraction temperature, 30 °C; and the solid/liquid ratio, 1 : 50. Under these conditions, the yields of chlorogenic acid and cynaroside were raised to 4.863% and 0.080%, respectively. Compared with other extraction methods, such as heat reflux extraction (HRE), ultrasonic extraction (UE), and Sohxlet extraction (SE), the UPE method showed several advantages, including higher extraction yield, shorter extraction time, lower energy consumption, and higher purity of the extracts. This study could help better utilize L. japonica flower buds as a readily accessible source of natural antioxidants in food and pharmaceutical industries. Copyright © 2015 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

Role of modifier in microwave assisted extraction of oleanolic acid from Gymnema sylvestre: application of green extraction technology for botanicals.

PubMed

Mandal, Vivekananda; Dewanjee, Saikat; Mandal, Subhash C

2009-08-01

This work highlights the development of a green extraction technology for botanicals with the use of microwave energy. Taking into consideration the extensive time involved in conventional extraction methods, coupled with usage of large volumes of organic solvent and energy resources, an ecofriendly green method that can overcome the above problems has been developed. The work compares the effect of sample pretreatment with untreated sample for improved yield of oleanolic acid from Gymnema sylvestre leaves. The pretreated sample with water produced 0.71% w/w oleanolic acid in one extraction cycle with 500 W microwave power, 25 mL methanol and only an 8 min extraction time. On the other hand, a conventional heat reflux extraction for 6 hours could produce only 0.62% w/w oleanolic acid. The detailed mechanism of extraction has been studied through scanning electron micrographs. The environmental impact of the proposed green method has also been evaluated.

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

NASA Astrophysics Data System (ADS)

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

2016-02-01

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

Choice of solvent extraction technique affects fatty acid composition of pistachio (Pistacia vera L.) oil.

PubMed

Abdolshahi, Anna; Majd, Mojtaba Heydari; Rad, Javad Sharifi; Taheri, Mehrdad; Shabani, Aliakbar; Teixeira da Silva, Jaime A

2015-04-01

Pistachio (Pistacia vera L.) oil has important nutritional and therapeutic properties because of its high concentration of essential fatty acids. The extraction method used to obtain natural compounds from raw material is critical for product quality, in particular to protect nutritional value. This study compared the fatty acid composition of pistachio oil extracted by two conventional procedures, Soxhlet extraction and maceration, analyzed by a gas chromatography-flame ionization detector (GC-FID). Four solvents with different polarities were tested: n-hexane (Hx), dichloromethane (DCM), ethyl acetate (EtAc) and ethanol (EtOH). The highest unsaturated fatty acid content (88.493 %) was obtained by Soxhlet extraction with EtAc. The Soxhlet method extracted the most oleic and linolenic acids (51.99 % and 0.385 %, respectively) although a higher concentration (36.32 %) of linoleic acid was extracted by maceration.

Acid Extraction - Ion Exchange Recovery of Cinchona Alkaloids Process and Plant Development

DTIC Science & Technology

1945-06-08

of commercial vinegar for a period of three days. The maceration was followed by successive percola- tions with the same material. A yield of...16.2 grams out of a possible 25 was effected for an efficiency of 72 percent. The extraction with commflrcial vinegar was conducted at the request...Program by Lt. Ronsone 75 The Sulfur ic Acid Extraction of Remijia Bark, by Dr. Arthur W. Walde 85 Preliminary Vinegar and Acetic Acid Extraction

[Comparison of two nucleic acid extraction methods for norovirus in oysters].

PubMed

Yuan, Qiao; Li, Hui; Deng, Xiaoling; Mo, Yanling; Fang, Ling; Ke, Changwen

2013-04-01

To explore a convenient and effective method for norovirus nucleic acid extraction from oysters suitable for long-term viral surveillance. Two methods, namely method A (glycine washing and polyethylene glycol precipitation of the virus followed by silica gel centrifugal column) and method B (protease K digestion followed by application of paramagnetic silicon) were compared for their performance in norovirus nucleic acid extraction from oysters. Real-time RT-PCR was used to detect norovirus in naturally infected oysters and in oysters with induced infection. The two methods yielded comparable positive detection rates for the samples, but the recovery rate of the virus was higher with method B than with method A. Method B is a more convenient and rapid method for norovirus nucleic acid extraction from oysters and suitable for long-term surveillance of norovirus.

Comparative evaluation of three commercial systems for nucleic acid extraction from urine specimens.

PubMed

Tang, Yi-Wei; Sefers, Susan E; Li, Haijing; Kohn, Debra J; Procop, Gary W

2005-09-01

A nucleic acid extraction system that can handle small numbers of specimens with a short test turnaround time and short hands-on time is desirable for emergent testing. We performed a comparative validation on three systems: the MagNA Pure compact system (Compact), the NucliSens miniMAG extraction instrument (miniMAG), and the BioRobot EZ1 system (EZ1). A total of 75 urine specimens submitted for polyomavirus BK virus detection were used. The human beta-actin gene was detected on 75 (100%), 75 (100%), and 72 (96%) nucleic acid extracts prepared by the miniMAG, EZ1, and Compact, respectively. The miniMAG produced the highest quantity of nucleic acids and the best precision among the three systems. The agreement rate was 100% for BKV detection on nucleic acid extracts prepared by the three extraction systems. When a full panel of specimens was run, the hands-on time and test turnaround time were 105.7 and 121.1 min for miniMAG, 6.1 and 22.6 min for EZ1, and 7.4 and 33.7 min for Compact, respectively. The EZ1 and Compact systems processed automatic nucleic acid extraction properly, providing a good solution to the need for sporadic but emergent specimen detection. The miniMAG yielded the highest quantity of nucleic acids, suggesting that this system would be the best for specimens containing a low number of microorganisms of interest.

Carboxylic and Dicarboxylic Acids Extracted from Crushed Magnesium Oxide Single Crystals

NASA Technical Reports Server (NTRS)

Freund, Friedemann; Gupta, Alka D.; Kumar, Devendra; DeVincenzi, Donald (Technical Monitor)

1998-01-01

Carboxylic and dicarboxylic acids (glycolic, oxalic, malonic and succinic) have been extracted with tetrahydrofuran (THE) and H2O from large synthetic MgO crystals, crushed to a medium fine powder. The extracts were characterized by infrared spectroscopy and (sup 1)H-NMR (Nuclear Magnetic Resonance). The THF extracts were derivatized with tert-butyldimethylsilyl (t-BDMS) for GC-MS (Gas Chromatography - Mass Spectroscopy) analysis. A single crystal separated from the extract was used for an x-ray structure analysis, giving the monoclinic unit cell, space group P2(sub 1)/c with a(sub o) = 5.543 A, b(sub o) = 8.845 A, c(sub o) = 5.086 A, and beta = 91.9 degrees, consistent with beta-succinic acid, HOOC(CH2)COOH. The amount of extracted acids is estimated to be of the order of 0.1 to 0.5 mg/g MgO. The MgO crystals from which these organic acids were extracted grew from the 2360 C hot melt, saturated with CO/CO2 and H2O, thereby incorporating small amounts of the gaseous components to form a solid solution (ss) with MgO. Upon cooling, the ss becomes supersaturated, causing solute carbon and other solute species to segregate not only to the surface but also internally, to dislocations and subgrain boundaries. The organic acids extracted from the MgO crystals after crushing appear to derive from these segregated solutes that formed C-C, C-H, and C-O bonds along dislocations and other defects in the MgO structure, leading to entities that can generically be described as (HxCyOz)(sup n-). The processes underlying the formation of these precursors are fundamental in nature and expected to be operational in any minerals, preferentially those with dense structures, that crystallized in H2O-CO2-laden environments. This opens the possibility that common magmatic and metamorphic rocks when weathering at the surface of a tectonically active planet like Earth may be an important source of abiogenically formed complex organic compounds.

Carboxylic and dicarboxylic acids extracted from crushed magnesium oxide single crystals

NASA Technical Reports Server (NTRS)

Freund, F.; Gupta, A. D.; Kumar, D.

1999-01-01

Carboxylic and dicarboxylic acids (glycolic, oxalic, malonic and succinic) have been extracted with tetrahydrofuran (THF) and H2O from large synthetic MgO crystals, crushed to a medium fine powder. The extracts were characterized by infrared spectroscopy and 1H-NMR. The THF extracts were derivatized with tert-butyldimethylsilyl (t-BDMS) for GC-MS analysis. A single crystal separated from the extract was used for an x-ray structure analysis, giving the monoclinic unit cell, space group P21/c with ao = 5.543 A, bo = 8.845 A, co = 5.086 A, and beta = 91.9 degrees, consistent with beta-succinic acid, HOOC(CH2)COOH. The amount of extracted acids is estimated to be of the order of 0.1 to 0.5 mg g-1 MgO. The MgO crystals from which these organic acids were extracted grew from the 2860 degrees C hot melt, saturated with CO/CO2 and H2O, thereby incorporating small amounts of the gaseous components to form a solid solution (ss) with MgO. Upon cooling, the ss becomes supersaturated, causing solute carbon and other solute species to segregate not only to the surface but also internally, to dislocations and subgrain boundaries. The organic acids extracted from the MgO crystals after crushing appear to derive from these segregated solutes that formed C-C, C-H and C-O bonds along dislocations and other defects in the MgO structure, leading to entities that can generically be described as (HxCyOz)n-. The processes underlying the formation of these precursors are fundamental in nature and expected to be operational in any minerals, preferentially those with dense structures, that crystallized in H2O-CO2-laden environments. This opens the possibility that common magmatic and metamorphic rocks when weathering at the surface of a tectonically active planet like Earth may be an important source of abiogenically formed complex organic compounds.

FT-IR Spectroscopic Evidence Of Phase Transition For NaA-ROH-Kerosine-H2O Microemulsion System Containing Nd3+ Ions

NASA Astrophysics Data System (ADS)

Liao, Hua; Xu, Zhen-Hua; Shi, Nai; Wu, Jin-Guang; Xu, Guang-Xian

1989-12-01

In the previous investigation, the saponification of naphthenic acid extractant system has been proved to be a process of the formation of a microemulsion of 14/0 type, and its full extraction of rare earths is a process of destruction of the W/O microemulsion[1]. When NdCl3 is partially extracted with NaA (sodium naphthenate) secoctylalcohol-- kerosine-- water microemulsion system (ME), both the NdA3 and the NaA co-exist in the same organic phase. However,the formation mechanism of microemulsion containing neodymium has not been much studied. In this paper, 10 aliquots of fully saponificated extractants were equilibrated with various amounts of NdC13 solutions respectively, then ten organic phases with different extraction efficiencies of neodymium from 094 to 9094 were obtained. After extraction,the volume of neodymium containing organic phase increased by 5 to 4594, because of the transfer of water molecules. The appearance of these organic phase still remained clear and transparent. The average hydrodynamic radius of the drops were found to be 100-300 Angstrom by using light scattering techniques. The results give a direct evidence of the microemulsion formation in the organic phase. Their FT-IR spectra were measured with CaFa liquid cells utilizing a Nicolet 7199B FT-IR spectrometer. The presence of various amounts of water in the organic phases was clearly detected from the relative intensity changes of 1644 cm-I, which is assigned to the bending mode of 1110 molecules. Fig.1 shows the change of water contents to the percent extraction of neodymium. Comparsion with the FT-IR spectra, it is seen that the 1560 cm-1 peak of the full saponificated extractant is attributed to the asym. stretching vibration of COO''' group, it shifted to 1536 for 100% extration of Nd ions, indicating the formation of neodymium naphthenate (NdA ) from ionic sodium naphthenate. The sym. strethching vibration of COO''' located at 1406 cm-1, it shifted to 1408 cm in 45% Nd extration

Improved Butanol-Methanol (BUME) Method by Replacing Acetic Acid for Lipid Extraction of Biological Samples.

PubMed

Cruz, Mutya; Wang, Miao; Frisch-Daiello, Jessica; Han, Xianlin

2016-07-01

Extraction of lipids from biological samples is a critical step in lipidomics, especially for shotgun lipidomics where lipid extracts are directly infused into a mass spectrometer. The butanol-methanol (BUME) extraction method was originally developed to extract lipids from plasma samples with 1 % acetic acid. Considering some lipids are sensitive to acidic environments, we modified this protocol by replacing acetic acid with lithium chloride solution and extended the modified extraction to tissue samples. Although no significant reduction of plasmalogen levels in the acidic BUME extracts of rat heart samples was found, the modified method was established to extract various tissue samples, including rat liver, heart, and plasma. Essentially identical profiles of the majority of lipid classes were obtained from the extracts of the modified BUME and traditional Bligh-Dyer methods. However, it was found that neither the original, nor the modified BUME method was suitable for 4-hydroxyalkenal species measurement in biological samples.

Improved Butanol-Methanol (BUME) Method by Replacing Acetic Acid for Lipid Extraction of Biological Samples

PubMed Central

Cruz, Mutya; Wang, Miao; Frisch-Daiello, Jessica; Han, Xianlin

2016-01-01

Extraction of lipids from biological samples is a critical step in lipidomics, especially for shotgun lipidomics where lipid extracts are directly infused into a mass spectrometer. The butanol-methanol (BUME) extraction method was originally developed to extract lipids from plasma samples with 1% acetic acid. Considering some lipids are sensitive to acidic environments, we modified this protocol by replacing acetic acid with lithium chloride solution and extended the modified extraction to tissue samples. Although no significant reduction of plasmalogen levels in the acidic BUME extracts of rat heart samples was found, the modified method was established to extract various tissue samples, including rat liver, heart, and plasma. Essentially identical profiles of the majority of lipid classes were obtained from the extracts of the modified BUME and traditional Bligh-Dyer methods. However, it was found that neither the original, nor the modified BUME method was suitable for 4-hydroxyalkenal species measurement in biological samples. PMID:27245345

Performances of different protocols for exocellular polysaccharides extraction from milk acid gels: Application to yogurt.

PubMed

Nguyen, An Thi-Binh; Nigen, Michaël; Jimenez, Luciana; Ait-Abderrahim, Hassina; Marchesseau, Sylvie; Picart-Palmade, Laetitia

2018-01-15

Dextran or xanthan were used as model exocellular polysaccharides (EPS) to compare the extraction efficiency of EPS from skim milk acid gels using three different protocols. Extraction yields, residual protein concentrations and the macromolecular properties of extracted EPS were determined. For both model EPS, the highest extraction yield (∼80%) was obtained when samples were heated in acidic conditions at the first step of extraction (Protocol 1). Protocols that contained steps of acid/ethanol precipitation without heating (Protocols 2 and 3) show lower extraction yields (∼55%) but allow a better preservation of the EPS macromolecular properties. Changing the pH of acid gels up to 7 before extraction (Protocol 3) improved the extraction yield of anionic EPS without effect on the macromolecular properties of EPS. Protocol 1 was then applied for the quantification of EPS produced during the yogurt fermentation, while Protocol 3 was dedicated to their macromolecular characterization. Copyright © 2017 Elsevier Ltd. All rights reserved.

Extraction of domoic acid from seawater and urine using a resin based on 2-(trifluoromethyl)acrylic acid.

PubMed

Piletska, Elena V; Villoslada, Fernando Navarro; Chianella, Iva; Bossi, Alessandra; Karim, Kal; Whitcombe, Michael J; Piletsky, Sergey A; Doucette, Gregory J; Ramsdell, John S

2008-03-03

A new solid-phase extraction (SPE) matrix with high affinity for the neurotoxin domoic acid (DA) was designed and tested. A computational modelling study led to the selection of 2-(trifluoromethyl)acrylic acid (TFMAA) as a functional monomer capable of imparting affinity towards domoic acid. Polymeric adsorbents containing TFMAA were synthesised and tested in high ionic strength solutions such as urine and seawater. The TFMAA-based polymers demonstrated excellent performance in solid-phase extraction of domoic acid, retaining the toxin while salts and other interfering compounds such as aspartic and glutamic acids were removed by washing and selective elution. It was shown that the TFMAA-based polymer provided the level of purification of domoic acid from urine and seawater acceptable for its quantification by high performance liquid chromatography-mass spectrometry (HPLC-MS) and enzyme-linked immunosorbent assay (ELISA) without any additional pre-concentration and purification steps.

Nucleic Acid Extraction from Synthetic Mars Analog Soils for in situ Life Detection

NASA Astrophysics Data System (ADS)

Mojarro, Angel; Ruvkun, Gary; Zuber, Maria T.; Carr, Christopher E.

2017-08-01

Biological informational polymers such as nucleic acids have the potential to provide unambiguous evidence of life beyond Earth. To this end, we are developing an automated in situ life-detection instrument that integrates nucleic acid extraction and nanopore sequencing: the Search for Extra-Terrestrial Genomes (SETG) instrument. Our goal is to isolate and determine the sequence of nucleic acids from extant or preserved life on Mars, if, for example, there is common ancestry to life on Mars and Earth. As is true of metagenomic analysis of terrestrial environmental samples, the SETG instrument must isolate nucleic acids from crude samples and then determine the DNA sequence of the unknown nucleic acids. Our initial DNA extraction experiments resulted in low to undetectable amounts of DNA due to soil chemistry-dependent soil-DNA interactions, namely adsorption to mineral surfaces, binding to divalent/trivalent cations, destruction by iron redox cycling, and acidic conditions. Subsequently, we developed soil-specific extraction protocols that increase DNA yields through a combination of desalting, utilization of competitive binders, and promotion of anaerobic conditions. Our results suggest that a combination of desalting and utilizing competitive binders may establish a "universal" nucleic acid extraction protocol suitable for analyzing samples from diverse soils on Mars.

Direct lactic acid fermentation of Jerusalem artichoke tuber extract using Lactobacillus paracasei without acidic or enzymatic inulin hydrolysis.

PubMed

Choi, Hwa-Young; Ryu, Hee-Kyoung; Park, Kyung-Min; Lee, Eun Gyo; Lee, Hongweon; Kim, Seon-Won; Choi, Eui-Sung

2012-06-01

Lactic acid fermentation of Jerusalem artichoke tuber was performed with strains of Lactobacillus paracasei without acidic or enzymatic inulin hydrolysis prior to fermentation. Some strains of L. paracasei, notably KCTC13090 and KCTC13169, could ferment hot-water extract of Jerusalem artichoke tuber more efficiently compared with other Lactobacillus spp. such as L. casei type strain KCTC3109. The L. paracasei strains could utilize almost completely the fructo-oligosaccharides present in Jerusalem artichoke. Inulin-fermenting L. paracasei strains produced c.a. six times more lactic acid compared with L. casei KCTC3109. Direct lactic fermentation of Jerusalem artichoke tuber extract at 111.6g/L of sugar content with a supplement of 5 g/L of yeast extract by L. paracasei KCTC13169 in a 5L jar fermentor produced 92.5 ce:hsp sp="0.25"/>g/L of lactic acid with 16.8 g/L fructose equivalent remained unutilized in 72 h. The conversion efficiency of inulin-type sugars to lactic acid was 98% of the theoretical yield. Copyright © 2012 Elsevier Ltd. All rights reserved.

Nucleic Acid Extraction from Synthetic Mars Analog Soils for in situ Life Detection.

PubMed

Mojarro, Angel; Ruvkun, Gary; Zuber, Maria T; Carr, Christopher E

2017-08-01

Biological informational polymers such as nucleic acids have the potential to provide unambiguous evidence of life beyond Earth. To this end, we are developing an automated in situ life-detection instrument that integrates nucleic acid extraction and nanopore sequencing: the Search for Extra-Terrestrial Genomes (SETG) instrument. Our goal is to isolate and determine the sequence of nucleic acids from extant or preserved life on Mars, if, for example, there is common ancestry to life on Mars and Earth. As is true of metagenomic analysis of terrestrial environmental samples, the SETG instrument must isolate nucleic acids from crude samples and then determine the DNA sequence of the unknown nucleic acids. Our initial DNA extraction experiments resulted in low to undetectable amounts of DNA due to soil chemistry-dependent soil-DNA interactions, namely adsorption to mineral surfaces, binding to divalent/trivalent cations, destruction by iron redox cycling, and acidic conditions. Subsequently, we developed soil-specific extraction protocols that increase DNA yields through a combination of desalting, utilization of competitive binders, and promotion of anaerobic conditions. Our results suggest that a combination of desalting and utilizing competitive binders may establish a "universal" nucleic acid extraction protocol suitable for analyzing samples from diverse soils on Mars. Key Words: Life-detection instruments-Nucleic acids-Mars-Panspermia. Astrobiology 17, 747-760.

Nucleic acid extraction techniques and application to the microchip.

PubMed

Price, Carol W; Leslie, Daniel C; Landers, James P

2009-09-07

As recently as the early 1990s, DNA purification was time-consuming, requiring the use of toxic, hazardous reagents. The advent of solid phase extraction techniques and the availability of commercial kits for quick and reliable DNA extraction has relegated those early techniques largely to the history books. High quality DNA can now be extracted from whole blood, serum, saliva, urine, stool, cerebral spinal fluid, tissues, and cells in less time without sacrificing recovery. Having achieved such a radical change in the methodology of DNA extraction, focus has shifted to adapting these methods to a miniaturized system, or "lab-on-a-chip" (A. Manz, N. Graber and H. M. Widmer, Sens. Actuators, B, 1990, 1, 244-248). Manz et al.'s concept of a "miniaturized total chemical analysis system" (microTAS) involved a silicon chip that incorporated sample pretreatment, separation and detection. This review will focus on the first of these steps, sample pretreatment in the form of DNA purification. The intention of this review is to provide an overview of the fundamentals of nucleic acid purification and solid phase extraction (SPE) and to discuss specific microchip DNA extraction successes and challenges. In order to fully appreciate the advances in DNA purification, a brief review of the history of DNA extraction is provided so that the reader has an understanding of the impact that the development of SPE techniques have had. This review will highlight the different methods of nucleic acid extraction (Table 1), including relevant citations, but without an exhaustive summary of the literature. A recent review by Wen et al. (J. Wen, L. A. Legendre, J. M. Bienvenue and J. P. Landers, Anal. Chem., 2008, 80, 6472-6479) covers solid phase extraction methods with a greater focus on their incorporation into integrated microfluidic systems.

Nucleic Acid Extraction from Synthetic Mars Analog Soils for in situ Life Detection

PubMed Central

Mojarro, Angel; Ruvkun, Gary; Zuber, Maria T.

2017-01-01

Abstract Biological informational polymers such as nucleic acids have the potential to provide unambiguous evidence of life beyond Earth. To this end, we are developing an automated in situ life-detection instrument that integrates nucleic acid extraction and nanopore sequencing: the Search for Extra-Terrestrial Genomes (SETG) instrument. Our goal is to isolate and determine the sequence of nucleic acids from extant or preserved life on Mars, if, for example, there is common ancestry to life on Mars and Earth. As is true of metagenomic analysis of terrestrial environmental samples, the SETG instrument must isolate nucleic acids from crude samples and then determine the DNA sequence of the unknown nucleic acids. Our initial DNA extraction experiments resulted in low to undetectable amounts of DNA due to soil chemistry–dependent soil-DNA interactions, namely adsorption to mineral surfaces, binding to divalent/trivalent cations, destruction by iron redox cycling, and acidic conditions. Subsequently, we developed soil-specific extraction protocols that increase DNA yields through a combination of desalting, utilization of competitive binders, and promotion of anaerobic conditions. Our results suggest that a combination of desalting and utilizing competitive binders may establish a “universal” nucleic acid extraction protocol suitable for analyzing samples from diverse soils on Mars. Key Words: Life-detection instruments—Nucleic acids—Mars—Panspermia. Astrobiology 17, 747–760. PMID:28704064

Validation of a One-Step Method for Extracting Fatty Acids from Salmon, Chicken and Beef Samples.

PubMed

Zhang, Zhichao; Richardson, Christine E; Hennebelle, Marie; Taha, Ameer Y

2017-10-01

Fatty acid extraction methods are time-consuming and expensive because they involve multiple steps and copious amounts of extraction solvents. In an effort to streamline the fatty acid extraction process, this study compared the standard Folch lipid extraction method to a one-step method involving a column that selectively elutes the lipid phase. The methods were tested on raw beef, salmon, and chicken. Compared to the standard Folch method, the one-step extraction process generally yielded statistically insignificant differences in chicken and salmon fatty acid concentrations, percent composition and weight percent. Initial testing showed that beef stearic, oleic and total fatty acid concentrations were significantly lower by 9-11% with the one-step method as compared to the Folch method, but retesting on a different batch of samples showed a significant 4-8% increase in several omega-3 and omega-6 fatty acid concentrations with the one-step method relative to the Folch. Overall, the findings reflect the utility of a one-step extraction method for routine and rapid monitoring of fatty acids in chicken and salmon. Inconsistencies in beef concentrations, although minor (within 11%), may be due to matrix effects. A one-step fatty acid extraction method has broad applications for rapidly and routinely monitoring fatty acids in the food supply and formulating controlled dietary interventions. © 2017 Institute of Food Technologists®.

Facile Separation of 5-O-Galloylquinic Acid from Chinese Green Tea Extract using Mesoporous Zirconium Phosphate.

PubMed

Ma, Yilong; Shang, Yafang; Zhu, Danye; Wang, Caihong; Zhong, Zhifeng; Xu, Ziyang

2016-05-01

5-O-Galloylquinic acid from green tea and other plants is attracting increasing attention for its antioxidant and antileishmanial bioactivities. It is always isolated using a silica column, a Sephadex column and high-performance liquid chromatography (HPLC) methods, which are either laborious or instrument dependent. To develop a new method to easily separate 5-O-galloylquinic acid. Mesoporous zirconium phosphate (m-ZrP) was prepared to conveniently separate 5-O-galloylquinic acid from Chinese green tea extract, and the target compound was easily obtained by simple steps of adsorption, washing and desorption. The effects of the green tea extraction conditions, extract concentrations, and m-ZrP adsorption/desorption dynamics on the 5-O-galloylquinic acid separation were evaluated. 5-O-Galloylquinic acid that was separated from a 70% ethanol extract of green tea was of moderate HPLC purity (92%) and recovery (88%), and an increased non-specific binding of epigallocatechin gallate (EGCG) on m-ZrP was observed in the diluted tea extract. The times for maximal adsorption of 5-O-galloylquinic acid in 70% ethanol extract and maximal desorption of 5-O-galloylquinic acid in 0.4% phosphoric acid solution were confirmed as 7 h and 5 h, respectively. A facile method to separate 5-O-galloylquinic acid from Chinese green tea extract using m-ZrP was established. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Method for extracting lanthanides and actinides from acid solutions by modification of Purex solvent

DOEpatents

Horwitz, E.P.; Kalina, D.G.

1984-05-21

A process has been developed for the extraction of multivalent lanthanide and actinide values from acidic waste solutions, and for the separation of these values from fission product and other values, which utilizes a new series of neutral bi-functional extractants, the alkyl(phenyl)-N, N-dialkylcarbamoylmethylphosphine oxides, in combination with a phase modifier to form an extraction solution. The addition of the extractant to the Purex process extractant, tri-n-butylphosphate in normal paraffin hydrocarbon diluent, will permit the extraction of multivalent lanthanide and actinide values from 0.1 to 12.0 molar acid solutions.

Two-step voltage dual electromembrane extraction: A new approach to simultaneous extraction of acidic and basic drugs.

PubMed

Asadi, Sakine; Nojavan, Saeed

2016-06-07

In the present work, acidic and basic drugs were simultaneously extracted by a novel method of high efficiency herein referred to as two-step voltage dual electromembrane extraction (TSV-DEME). Optimizing effective parameters such as composition of organic liquid membrane, pH values of donor and acceptor solutions, voltage and duration of each step, the method had its figures of merit investigated in pure water, human plasma, wastewater, and breast milk samples. Simultaneous extraction of acidic and basic drugs was done by applying potentials of 150 V and 400 V for 6 min and 19 min as the first and second steps, respectively. The model compounds were extracted from 4 mL of sample solution (pH = 6) into 20 μL of each acceptor solution (32 mM NaOH for acidic drugs and 32 mM HCL for basic drugs). 1-Octanol was immobilized within the pores of a porous hollow fiber of polypropylene, as the supported liquid membrane (SLM) for acidic drugs, and 2-ethyle hexanol, as the SLM for basic drugs. The proposed TSV-DEME technique provided good linearity with the resulting correlation coefficients ranging from 0.993 to 0.998 over a concentration range of 1-1000 ng mL(-1). The limit of detections of the drugs were found to range within 0.3-1.5 ng mL(-1), while the corresponding repeatability ranged from 7.7 to 15.5% (n = 4). The proposed method was further compared to simple dual electromembrane extraction (DEME), indicating significantly higher recoveries for TSV-DEME procedure (38.1-68%), as compared to those of simple DEME procedure (17.7-46%). Finally, the optimized TSV-DEME was applied to extract and quantify model compounds in breast milk, wastewater, and plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Citric acid production from extract of Jerusalem artichoke tubers by the genetically engineered yeast Yarrowia lipolytica strain 30 and purification of citric acid.

PubMed

Wang, Ling-Fei; Wang, Zhi-Peng; Liu, Xiao-Yan; Chi, Zhen-Ming

2013-11-01

In this study, citric acid production from extract of Jerusalem artichoke tubers by the genetically engineered yeast Yarrowia lipolytica strain 30 was investigated. After the compositions of the extract of Jerusalem artichoke tubers for citric acid production were optimized, the results showed that natural components of extract of Jerusalem artichoke tubers without addition of any other components were suitable for citric acid production by the yeast strain. During 10 L fermentation using the extract containing 84.3 g L(-1) total sugars, 68.3 g L(-1) citric acid was produced and the yield of citric acid was 0.91 g g(-1) within 336 h. At the end of the fermentation, 9.2 g L(-1) of residual total sugar and 2.1 g L(-1) of reducing sugar were left in the fermented medium. At the same time, citric acid in the supernatant of the culture was purified. It was found that 67.2 % of the citric acid in the supernatant of the culture was recovered and purity of citric acid in the crystal was 96 %.

Pro-static Agents in Jet Fuels

DTIC Science & Technology

1976-08-16

1000 10,000 CHARGE DENSITY (juC/ms) Fig. 5- Effect otpolar compounds on charging tendency of silica-gel-treated n-heptane Naphthenic acid is neither a...Eastmant Naphthenic acids Practical Eastman t 30 NRL REPORT 8021 Compound Purity Supplier Pararosandine hydrochloride Not available Eastmant...silica gel to remove moisture and polar contaminants that might interfere with the compound or additive being screened. This treatment Manuscript

Microwave-assisted organic acid extraction of lignin from bamboo: structure and antioxidant activity investigation.

PubMed

Li, Ming-Fei; Sun, Shao-Ni; Xu, Feng; Sun, Run-Cang

2012-10-01

Microwave-assisted extraction in organic acid aqueous solution (formic acid/acetic acid/water, 3/5/2, v/v/v) was applied to isolate lignin from bamboo. Additionally, the structural features of the extracted lignins were thoroughly investigated in terms of C₉ formula, molecular weight distribution, FT-IR, (1)H NMR and HSQC spectroscopy. It was found that with an increase in the severity of microwave-assisted extraction, there was an increase of phenolic hydroxyl content in the lignin. In addition, an increase of the severity resulted in a decrease of the bound carbohydrate content as well as molecular weight of the lignin. Antioxidant activity investigation indicated that the radical scavenging index of the extracted lignins (0.35-1.15) was higher than that of BHT (0.29) but lower than that of BHA (3.85). The results suggested that microwave-assisted organic acid extraction provides a promising way to prepare lignin from bamboo with good antioxidant activity for potential application in the food industry. Copyright © 2012 Elsevier Ltd. All rights reserved.

Microwave-assisted extraction with water for fast extraction and simultaneous RP-HPLC determination of phenolic acids in radix Salviae Miltiorrhizae.

PubMed

Fang, Xinsheng; Wang, Jianhua; Zhou, Hongying; Jiang, Xingkai; Zhu, Lixiang; Gao, Xin

2009-07-01

An optimized microwave-assisted extraction method using water (MAE-W) as the extractant and an efficient HPLC analysis method were first developed for the fast extraction and simultaneous determination of D(+)-(3,4-dihydroxyphenyl) lactic acid (Dla), salvianolic acid B (SaB), and lithospermic acid (La) in radix Salviae Miltiorrhizae. The key parameters of MAE-W were optimized. It was found that the degradation of SaB was inhibited when using the optimized MAE-W and the stable content of Dla, La, and SaB in danshen was obtained. Furthermore, compared to the conventional extraction methods, the proposed MAE-W is a more rapid method with higher yield and lower solvent consumption with a reproducibility (RSD <6%). In addition, using water as extractant is safe and helpful for environment protection, which could be referred to as green extraction. The separation and quantitative determination of the three compounds was carried out by a developed reverse-phase high-performance liquid chromatographic (RP-HPLC) method with UV detection. Highly efficient separation was obtained using gradient solvent system. The optimized HPLC analysis method was validated to have specificity, linearity, precision, and accuracy. The results indicated that MAE-W followed by HPLC-UV determination is an appropriate alternative to previously proposed method for quality control of radix Salviae Miltiorrhizae.

Acidic solvent extraction of gossypol from cottonseed meal

USDA-ARS?s Scientific Manuscript database

In order to expand the use of cottonseed meal in animal feeding, extraction of the meal gossypol was studied with acetic acetone- and ethanol-based solutions. Phosphoric acid was added to hydrolyze and release gossypol bound within the meal. Both solvent systems were effective at reducing gossypo...

Permeability of rosmarinic acid in Prunella vulgaris and ursolic acid in Salvia officinalis extracts across Caco-2 cell monolayers.

PubMed

Qiang, Zhiyi; Ye, Zhong; Hauck, Cathy; Murphy, Patricia A; McCoy, Joe-Ann; Widrlechner, Mark P; Reddy, Manju B; Hendrich, Suzanne

2011-10-11

Rosmarinic acid (RA), a caffeic acid-related compound found in high concentrations in Prunella vulgaris (self-heal), and ursolic acid (UA), a pentacyclic triterpene acid concentrated in Salvia officinalis (sage), have been traditionally used to treat inflammation in the mouth, and may also be beneficial for gastrointestinal health in general. To investigate the permeabilities of RA and UA as pure compounds and in Prunella vulgaris and Salvia officinalis ethanol extracts across human intestinal epithelial Caco-2 cell monolayers. The permeabilities and phase II biotransformation of RA and UA as pure compounds and in herbal extracts were compared using Caco-2 cells with HPLC detection. The apparent permeability coefficient (P(app)) for RA and RA in Prunella vulgaris extracts was 0.2 ± 0.05 × 10(-6)cm/s, significantly increased to 0.9 ± 0.2 × 10(-6)cm/s after β-glucuronidase/sulfatase treatment. P(app) for UA and UA in Salvia officinalis extract was 2.7 ± 0.3 × 10(-6)cm/s and 2.3 ± 0.5 × 10(-6)cm/s before and after β-glucuronidase/sulfatase treatment, respectively. Neither compound was affected in permeability by the herbal extract matrix. RA and UA in herbal extracts had similar uptake as that found using the pure compounds, which may simplify the prediction of compound efficacy, but the apparent lack of intestinal glucuronidation/sulfation of UA is likely to further enhance the bioavailability of that compound compared with RA. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

Permeability of Rosmarinic acid in Prunella vulgaris and Ursolic acid in Salvia officinalis Extracts across Caco-2 Cell Monolayers

PubMed Central

Qiang, Zhiyi; Ye, Zhong; Hauck, Cathy; Murphy, Patricia A.; McCoy, Joe-Ann; Widrlechner, Mark P.; Reddy, Manju B.; Hendrich, Suzanne

2011-01-01

Ethnopharmacological relevance Rosmarinic acid (RA), a caffeic acid-related compound found in high concentrations in Prunella vulgaris (self-heal), and ursolic acid (UA), a pentacyclic triterpene acid concentrated in Salvia officinalis (sage), have been traditionally used to treat inflammation in the mouth, and may also be beneficial for gastrointestinal health in general. Aim of the study To investigate the permeabilities of RA and UA as pure compounds and in P. vulgaris and S. officinalis ethanol extracts across human intestinal epithelial Caco-2 cell monolayers. Materials and methods The permeabilities and Phase II biotransformation of RA and UA as pure compounds and in herbal extracts were compared using Caco-2 cells with HPLC detection. Results The apparent permeability coefficient (Papp) for RA and RA in P. vulgaris extracts was 0.2 ± 0.05 × 10−6 cm/s, significantly increased to 0.9 ± 0.2 × 10−6 cm/s after β-glucuronidase/sulfatase treatment. Papp for UA and UA in S. officinalis extract was 2.7 ± 0.3 × 10−6 cm/s and 2.3 ± 0.5 × 10−6 cm/s before and after β-glucuronidase/sulfatase treatment, respectively. Neither compound was affected in permeability by the herbal extract matrix. Conclusion RA and UA in herbal extracts had similar uptake as that found using the pure compounds, which may simplify the prediction of compound efficacy, but the apparent lack of intestinal glucuronidation/sulfation of UA is likely to further enhance the bioavailability of that compound compared with RA. PMID:21798330

Efficient production of succinic acid from herbal extraction residue hydrolysate.

PubMed

Wang, Caixia; Su, Xinyao; Sun, Wei; Zhou, Sijing; Zheng, Junyu; Zhang, Mengting; Sun, Mengchu; Xue, Jianping; Liu, Xia; Xing, Jianmin; Chen, Shilin

2018-06-15

In this study, six different herbal-extraction residues were evaluated for succinic acid production in terms of chemical composition before and after dilute acid pretreatment (DAP) and sugar release performance. Chemical composition showed that pretreated residues of Glycyrrhiza uralensis Fisch (GUR) and Morus alba L. (MAR) had the highest cellulose content, 50% and 52%, respectively. Higher concentrations of free sugars (71.6 g/L total sugar) and higher hydrolysis yield (92%) were both obtained under 40 FPU/g DM at 10% solid loading for GUR. Using scanning electron microscopy (SEM), GUR was found to show a less compact structure due to process of extraction. Specifically, the fibers in pretreated GUR were coarse and disordered compared with that of GUR indicated by SEM. Finally, 65 g/L succinic acid was produced with a higher yield of 0.89 g/g total sugar or 0.49 g/g GUR. Our results illustrate the potential of GUR for succinic acid production. Copyright © 2018 Elsevier Ltd. All rights reserved.

Extreme Pressure Synergistic Mechanism of Bismuth Naphthenate and Sulfurized Isobutene Additives

NASA Astrophysics Data System (ADS)

Xu, Xin; Hu, Jianqiang; Yang, Shizhao; Xie, Feng; Guo, Li

A four-ball tester was used to evaluate the tribological performances of bismuth naphthenate (BiNap), sulfurized isobutene (VSB), and their combinations. The results show that the antiwear properties of BiNap and VSB are not very visible, but they possess good extreme pressure (EP) properties, particularly sulfur containing bismuth additives. Synergistic EP properties of BiNap with various sulfur-containing additives were investigated. The results indicate that BiNap exhibits good EP synergism with sulfur-containing additives. The surface analytical tools, such as X-ray photoelectron spectrometer (XPS) scanning electron microscope (SEM) and energy dispersive X-ray (EDX), were used to investigate the topography, composition contents, and depth profile of some typical elements on the rubbing surface. Smooth topography of wear scar further confirms that the additive showed good EP capacities, and XPS and EDX analyzes indicate that tribochemical mixed protective films composed of bismuth, bismuth oxides, sulfides, and sulfates are formed on the rubbing surface, which improves the tribological properties of lubricants. In particular, a large number of bismuth atoms and bismuth sulfides play an important role in improving the EP properties of oils.

Extraction of uranium from tailings by sulfuric acid leaching with oxidants

NASA Astrophysics Data System (ADS)

Huang, Jing; Li, Mi; Zhang, Xiaowen; Huang, Chunmei; Wu, Xiaoyan

2017-06-01

Recovery of uranium have been performed by leaching uranium-containing tailings in sulfuric acid system with the assistance of HF, HClO4, H2O2 and MnO2. The effect of reagent dosage, sulfuric acid concentration, Liquid/solid ratio, reaction temperature and particle size on the leaching of uranium were investigated. The results show that addiction of HF, HClO4, H2O2 and MnO2 significantly increased the extraction of uranium under 1M sulphuric acid condition and under the optimum reaction conditions a dissolution fraction of 85% by HClO4, 90% by HF, 95% by H2O2 can be reached respectively. The variation of technological mineralogy properites of tailings during leaching process show that the assistants can break gangue effectively. These observations suggest that optimum oxidants could potentially influence the extraction of uranium from tailings even under dilute acid condition.

Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

PubMed

Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

2018-01-26

The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comprehensive analysis of oil sands processed water by direct-infusion Fourier-transform ion cyclotron resonance mass spectrometry with and without offline UHPLC sample prefractionation.

PubMed

Nyakas, Adrien; Han, Jun; Peru, Kerry M; Headley, John V; Borchers, Christoph H

2013-05-07

Oil sands processed water (OSPW) is the main byproduct of the large-scale bitumen extraction activity in the Athabasca oil sands region (Alberta, Canada). We have investigated the acid-extractable fraction (AEF) of OSPW by extraction-only (EO) direct infusion (DI) negative-ion mode electrospray ionization (ESI) on a 12T-Fourier transform ion cyclotron resonance mass spectrometer (FTICR-MS), as well as by offline ultrahigh performance liquid chromatography (UHPLC) followed by DI-FTICR-MS. A preliminary offline UHPLC separation into 8 fractions using a reversed-phase C4 column led to approximately twice as many detected peaks and identified compounds (973 peaks versus 2231 peaks, of which 856 and 1734 peaks, respectively, could be assigned to chemical formulas based on accurate mass measurements). Conversion of these masses to the Kendrick mass scale allowed the straightforward recognition of homologues. Naphthenic (CnH2n+zO2) and oxy-naphthenic (CnH2n+zOx) acids represented the largest group of molecules with assigned formulas (64%), followed by sulfur-containing compounds (23%) and nitrogen-containing compounds (8%). Pooling of corresponding fractions from two consecutive offline UHPLC runs prior to MS analysis resulted in ~50% more assignments than a single injection, resulting in 3-fold increase of identifications compared to EO-DI-FTICR-MS using the same volume of starting material. Liquid-liquid extraction followed by offline UHPLC fractionation thus holds enormous potential for a more comprehensive profiling of OSPW, which may provide a deeper understanding of its chemical nature and environmental impact.

Simultaneous determination of docosahexaenoic acid and eicosapentaenoic acid in common seafood using ultrasonic cell crusher extraction combined with gas chromatography.

PubMed

Zhao, Juanjuan; Ren, Yan; Yu, Chen; Chen, Xiangming; Shi, Yanan

2017-02-01

An effective method for the simultaneous determination of docosahexaenoic acid and eicosapentaenoic acid in common seafood by gas chromatography was developed and validated. Total docosahexaenoic acid and eicosapentaenoic acid were extracted from seafood by ultrasonic cell crusher assisted extraction and methyl esterified for gas chromatography analysis in the presence of the internal standard. The linearity was good (r > 0.999) in 9.59 ∼ 479.5 μg/mL for docosahexaenoic acid and 9.56 ∼ 477.8 μg/mL for eicosapentaenoic acid. The intrarun and interrun precisions were both within 4.8 and 6.1% for the two analytes, while the accuracy was less than 5.8%. The developed method was applied for determination of docosahexaenoic acid and eicosapentaenoic acid in six kinds of seafood. The result showed the content of docosahexaenoic acid and eicosapentaenoic acid was all higher than 1 mg/g in yellow croaker, hairtail, venerupis philippinarum, mussel, and oyster. Our work may be helpful for dietary optimization and production of docosahexaenoic acid and eicosapentaenoic acid. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fuel Lubricity--Survey of the Literature

DTIC Science & Technology

1981-01-01

composition of sulfur com- pounds in the fuel, and the presence of naphthenic acids and finely dispersed free water. 16 Contrary to the results when using...compounds in the fuel, and the presence of naphthenic acids and finely dispersed free water was determined. The experiments employed a friction tester which...served to reduce/ remove the polar, surface-active constituents of the fuel which are believed to provide improved lubricating characterstics. The

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...

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.

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...

Downstream extraction process development for recovery of organic acids from a fermentation broth.

PubMed

Bekatorou, Argyro; Dima, Agapi; Tsafrakidou, Panagiotia; Boura, Konstantina; Lappa, Katerina; Kandylis, Panagiotis; Pissaridi, Katerina; Kanellaki, Maria; Koutinas, Athanasios A

2016-11-01

The present study focused on organic acids (OAs) recovery from an acidogenic fermentation broth, which is the main problem regarding the use of OAs for production of ester-based new generation biofuels or other applications. Specifically, 10 solvents were evaluated for OAs recovery from aqueous media and fermentation broths. The effects of pH, solvent/OAs solution ratios and application of successive extractions were studied. The 1:1 solvent/OAs ratio showed the best recovery rates in most cases. Butyric and isobutyric acids showed the highest recovery rates (80-90%), while lactic, succinic, and acetic acids were poorly recovered (up to 45%). The OAs recovery was significantly improved by successive 10-min extractions. Alcohols presented the best extraction performance. The process using repeated extractions with 3-methyl-1-butanol led to the highest OAs recovery. However, 1-butanol can be considered as the most cost-effective option taking into account its price and availability. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of fatty acid composition and quality characteristics of oils from palm fruits using solvent extraction

NASA Astrophysics Data System (ADS)

Kasmin, Hasimah; Lazim, Azwan Mat; Awang, Roila

2015-09-01

Palm oil contains about 45% of saturated palmitic acid and 39% of mono-unsaturated oleic acid. Investigations made in the past to trace the fatty acid composition in palm revealed that ripeness of fresh fruit bunch (FFB) affect oil composition. However, there is no evidence that processing operations affect oil composition, although different stage of processing does affect the quality of oil extracted. An improved method for sterilizing the oil palm fruits by dry heating, followed by oil extraction has been studied. This method eliminates the use of water, thus, increasing the extraction of lipid soluble. The objective of this study is to determine the possibility production of palm oil with different fatty acid composition (FAC) as well as the changes in quality from conventional milling. The unripe and ripe FFB were collected, sterilized and extracted using different method of solvent extraction. Preliminary data have shown that variation in FAC will also alter the physical and chemical properties of the oil extracted.

Comparison of Nitrilotriacetic Acid and [S,S]-Ethylenediamine-N,N'-disuccinic Acid in UV-Fenton for the Treatment of Oil Sands Process-Affected Water at Natural pH.

PubMed

Zhang, Ying; Klamerth, Nikolaus; Chelme-Ayala, Pamela; Gamal El-Din, Mohamed

2016-10-04

The application of UV-Fenton processes with two chelating agents, nitrilotriacetic acid (NTA) and [S,S]-ethylenediamine-N,N'-disuccinic acid ([S,S]-EDDS), for the treatment of oil sands process-affected water (OSPW) at natural pH was investigated. The half-wave potentials of Fe(III/II)NTA and Fe(III/II)EDDS and the UV photolysis of the complexes in Milli-Q water and OSPW were compared. Under optimum conditions, UV-NTA-Fenton exhibited higher efficiency than UV-EDDS-Fenton in the removal of acid extractable organic fraction (66.8% for the former and 50.0% for the latter) and aromatics (93.5% for the former and 74.2% for the latter). Naphthenic acids (NAs) removals in the UV-NTA-Fenton process (98.4%, 86.0%, and 81.0% for classical NAs, NAs + O (oxidized NAs with one additional oxygen atom), and NAs + 2O (oxidized NAs with two additional oxygen atoms), respectively) under the experimental conditions were much higher than those in the UV-H 2 O 2 (88.9%, 48.7%, and 54.6%, correspondingly) and NTA-Fenton (69.6%, 35.3%, and 44.2%, correspondingly) processes. Both UV-NTA-Fenton and UV-EDDS-Fenton processes presented promoting effect on the acute toxicity of OSPW toward Vibrio fischeri. No significant change of the NTA toxicity occurred during the photolysis of Fe(III)NTA; however, the acute toxicity of EDDS increased as the photolysis of Fe(III)EDDS proceeded. NTA is a much better agent than EDDS for the application of UV-Fenton process in the treatment of OSPW.

Vanadium Extraction from Shale via Sulfuric Acid Baking and Leaching

NASA Astrophysics Data System (ADS)

Shi, Qihua; Zhang, Yimin; Liu, Tao; Huang, Jing

2018-01-01

Fluorides are widely used to improve vanadium extraction from shale in China. Sulfuric acid baking-leaching (SABL) was investigated as a means of recovering vanadium which does not require the use of fluorides and avoids the productions of harmful fluoride-containing wastewater. Various effective factors were systematically studied and the experimental results showed that 90.1% vanadium could be leached from the shale. On the basis of phase transformations and structural changes after baking the shale, a mechanism of vanadium extraction from shale via SABL was proposed. The mechanism can be described as: (1) sulfuric acid diffusion into particles; (2) the formation of concentrated sulfuric acid media in the particles after water evaporation; (3) hydroxyl groups in the muscovite were removed and transient state [SO4 2-] was generated; and (4) the metals in the muscovite were sulfated by active [SO4 2-] and the vanadium was released. Thermodynamics modeling confirmed this mechanism.

Effect of Psidium cattleianum leaf extract on Streptococcus mutans viability, protein expression and acid production.

PubMed

Brighenti, F L; Luppens, S B I; Delbem, A C B; Deng, D M; Hoogenkamp, M A; Gaetti-Jardim, E; Dekker, H L; Crielaard, W; ten Cate, J M

2008-01-01

Plants naturally produce secondary metabolites that can be used as antimicrobials. The aim of this study was to assess the effects of Psidium cattleianum leaf extract on Streptococcus mutans. The extract (100%) was obtained by decoction of 100 g of leaves in 600 ml of deionized water. To assess killing, S. mutans biofilms were treated with water (negative control) or various extract dilutions [100, 50, 25% (v/v) in water] for 5 or 60 min. To evaluate the effect on protein expression, biofilms were exposed to water or 1.6% (v/v) extract for 120 min, proteins were extracted and submitted to 2-dimensional difference gel electrophoresis. Differentially expressed proteins were identified by mass spectrometry. The effect of 1.6% (v/v) extract on acid production was determined by pH measurements and compared to a water control. Viability was similar after 5 min of treatment with the 100% extract or 60 min with the 50% extract (about 0.03% survival). There were no differences in viability between the biofilms exposed to the 25 or 50% extract after 60 min of treatment (about 0.02% survival). Treatment with the 1.6% extract significantly changed protein expression. The abundance of 24 spots was decreased compared to water (p < 0.05). The extract significantly inhibited acid production (p < 0.05). It is concluded that P. cattleianum leaf extract kills S. mutans grown in biofilms when applied at high concentrations. At low concentrations it inhibits S. mutans acid production and reduces the expression of proteins involved in general metabolism, glycolysis and lactic acid production. (c) 2008 S. Karger AG, Basel

Liquefaction process wherein solvents derived from the material liquefied and containing increased concentrations of donor species are employed

DOEpatents

Fant, B. T.; Miller, John D.; Ryan, D. F.

1982-01-01

An improved process for the liquefaction of solid carbonaceous materials wherein a solvent or diluent derived from the solid carbonaceous material being liquefied is used to form a slurry of the solid carbonaceous material and wherein the solvent or diluent comprises from about 65 to about 85 wt. % hydroaromatic components. The solvent is prepared by first separating a solvent or diluent distillate fraction from the liquefaction product, subjecting this distillate fraction to hydrogenation and then extracting the naphthenic components from the hydrogenated product. The extracted naphthenic components are then dehydrogenated and hydrotreated to produce additional hydroaromatic components. These components are combined with the solvent or diluent distillate fraction. The solvent may also contain hydroaromatic constituents prepared by extracting naphthenic components from a heavy naphtha, dehydrogenating the same and then hydrotreating the dehydrogenated product. When the amount of solvent produced in this manner exceeds that required for steady state operation of the liquefaction process a portion of the solvent or diluent distillated fraction will be withdrawn as product.

Combination of graphene oxide-based solid phase extraction and electro membrane extraction for the preconcentration of chlorophenoxy acid herbicides in environmental samples.

PubMed

Tabani, Hadi; Fakhari, Ali Reza; Shahsavani, Abolfath; Behbahani, Mohammad; Salarian, Mani; Bagheri, Akbar; Nojavan, Saeed

2013-07-26

Combination of different extraction methods is an interesting and debatable work in the field of sample preparation. In the current study, for the first time, solid phase extraction combined with electro membrane extraction (SPE-EME) was developed for ultra-preconcentration and determination of chlorophenoxy acid herbicides in environmental samples using capillary electrophoresis (CE). In the mentioned method, first, a 100mL of chlorophenoxy acid herbicides (2-methyl-4-chlorophenoxyacetic acid (MCPA), 2-(2,4-dichlorophenoxy) propanoic acid (2,4-DP) and 2-(4-chloro-2-methylphenoxy) propanoic acid (MCPP)) was passed through a column of graphene oxide as a solid phase, and then the adsorbed herbicides were eluted by 4.0mL of 8% acetic acid (HOAC) in methanol. Then, the elution solvent was evaporated and the herbicides residue was dissolved in 4.0mL of double distilled water (pH 9.0). Afterwards, the herbicides in 4.0mL of the aqueous solution were transferred to an EME glass vial. In the EME step, the herbicides were extracted from the sample solution into the basic acceptor solution (pH 13.0) under electrical potential, which was held inside the lumen of the fiber with 1-octanol as the supported liquid membrane (SLM). Under the optimized conditions, high enrichment factors were obtained in the range of 1950-2000. The limits of quantification (LOQs) and method detection limits (MDLs) were obtained in the range of 1.0-1.5 and 0.3-0.5ngmL(-1), respectively. Finally, the performance of the present method was evaluated for extraction and determination of chlorophenoxy acid herbicides in environmental samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Selection of optimum ionic liquid solvents for flavonoid and phenolic acids extraction

NASA Astrophysics Data System (ADS)

Rahman, N. R. A.; Yunus, N. A.; Mustaffa, A. A.

2017-06-01

Phytochemicals are important in improving human health with their functions as antioxidants, antimicrobials and anticancer agents. However, the quality of phytochemicals extract relies on the efficiency of extraction process. Ionic liquids (ILs) have become a research phenomenal as extraction solvent due to their unique properties such as unlimited range of ILs, non-volatile, strongly solvating and may become either polarity. In phytochemical extraction, the determination of the best solvent that can extract highest yield of solute (phytochemical) is very important. Therefore, this study is conducted to determine the best IL solvent to extract flavonoids and phenolic acids through a property prediction modeling approach. ILs were selected from the imidazolium-based anion for alkyl chains ranging from ethyl > octyl and cations consisting of Br, Cl, [PF6], BF4], [H2PO4], [SO4], [CF3SO3], [TF2N] and [HSO4]. This work are divided into several stages. In Stage 1, a Microsoft Excel-based database containing available solubility parameter values of phytochemicals and ILs including its prediction models and their parameters has been established. The database also includes available solubility data of phytochemicals in IL, and activity coefficient models, for solid-liquid phase equilibrium (SLE) calculations. In Stage 2, the solubility parameter values of the flavonoids (e.g. kaempferol, quercetin and myricetin) and phenolic acids (e.g. gallic acid and caffeic acid) are determined either directly from database or predicted using Stefanis and Marrero-Gani group contribution model for the phytochemicals. A cation-anion contribution model is used for IL. In Stage 3, the amount of phytochemicals extracted can be determined by using SLE relationship involving UNIFAC-IL model. For missing parameters (UNIFAC-IL), they are regressed using available solubility data. Finally, in Stage 4, the solvent candidates are ranked and five ILs, ([OMIM] [TF2N], [HeMIM] [TF2N], [HMIM] [TF2N

Integrated printed circuit board device for cell lysis and nucleic acid extraction.

PubMed

Marshall, Lewis A; Wu, Liang Li; Babikian, Sarkis; Bachman, Mark; Santiago, Juan G

2012-11-06

Preparation of raw, untreated biological samples remains a major challenge in microfluidics. We present a novel microfluidic device based on the integration of printed circuit boards and an isotachophoresis assay for sample preparation of nucleic acids from biological samples. The device has integrated resistive heaters and temperature sensors as well as a 70 μm × 300 μm × 3.7 cm microfluidic channel connecting two 15 μL reservoirs. We demonstrated this device by extracting pathogenic nucleic acids from 1 μL dispensed volume of whole blood spiked with Plasmodium falciparum. We dispensed whole blood directly onto an on-chip reservoir, and the system's integrated heaters simultaneously lysed and mixed the sample. We used isotachophoresis to extract the nucleic acids into a secondary buffer via isotachophoresis. We analyzed the convective mixing action with micro particle image velocimetry (micro-PIV) and verified the purity and amount of extracted nucleic acids using off-chip quantitative polymerase chain reaction (PCR). We achieved a clinically relevant limit of detection of 500 parasites per microliter. The system has no moving parts, and the process is potentially compatible with a wide range of on-chip hybridization or amplification assays.

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

USDA-ARS?s Scientific Manuscript database

An extract of S. officinalis (garden sage) was prepared using supercritical carbon dioxide (SC-CO2) extraction, followed by a Soxhlet hot water extraction. The resulting extract was enriched in polyphenols, including rosmarinic acid (RA), which has shown promising health benefits in animals. The ext...

Rapid Nucleic Acid Extraction and Purification Using a Miniature Ultrasonic Technique

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

Branch, Darren W.; Vreeland, Erika C.; McClain, Jamie L.

Miniature ultrasonic lysis for biological sample preparation is a promising technique for efficient and rapid extraction of nucleic acids and proteins from a wide variety of biological sources. Acoustic methods achieve rapid, unbiased, and efficacious disruption of cellular membranes while avoiding the use of harsh chemicals and enzymes, which interfere with detection assays. In this work, a miniature acoustic nucleic acid extraction system is presented. Using a miniature bulk acoustic wave (BAW) transducer array based on 36° Y-cut lithium niobate, acoustic waves were coupled into disposable laminate-based microfluidic cartridges. To verify the lysing effectiveness, the amount of liberated ATP andmore » the cell viability were measured and compared to untreated samples. The relationship between input power, energy dose, flow-rate, and lysing efficiency were determined. DNA was purified on-chip using three approaches implemented in the cartridges: a silica-based sol-gel silica-bead filled microchannel, nucleic acid binding magnetic beads, and Nafion-coated electrodes. Using E. coli, the lysing dose defined as ATP released per joule was 2.2× greater, releasing 6.1× more ATP for the miniature BAW array compared to a bench-top acoustic lysis system. An electric field-based nucleic acid purification approach using Nafion films yielded an extraction efficiency of 69.2% in 10 min for 50 µL samples.« less

Rapid Nucleic Acid Extraction and Purification Using a Miniature Ultrasonic Technique

DOE PAGES

Branch, Darren W.; Vreeland, Erika C.; McClain, Jamie L.; ...

2017-07-21

Miniature ultrasonic lysis for biological sample preparation is a promising technique for efficient and rapid extraction of nucleic acids and proteins from a wide variety of biological sources. Acoustic methods achieve rapid, unbiased, and efficacious disruption of cellular membranes while avoiding the use of harsh chemicals and enzymes, which interfere with detection assays. In this work, a miniature acoustic nucleic acid extraction system is presented. Using a miniature bulk acoustic wave (BAW) transducer array based on 36° Y-cut lithium niobate, acoustic waves were coupled into disposable laminate-based microfluidic cartridges. To verify the lysing effectiveness, the amount of liberated ATP andmore » the cell viability were measured and compared to untreated samples. The relationship between input power, energy dose, flow-rate, and lysing efficiency were determined. DNA was purified on-chip using three approaches implemented in the cartridges: a silica-based sol-gel silica-bead filled microchannel, nucleic acid binding magnetic beads, and Nafion-coated electrodes. Using E. coli, the lysing dose defined as ATP released per joule was 2.2× greater, releasing 6.1× more ATP for the miniature BAW array compared to a bench-top acoustic lysis system. An electric field-based nucleic acid purification approach using Nafion films yielded an extraction efficiency of 69.2% in 10 min for 50 µL samples.« less

Sequential ultrasound-microwave assisted acid extraction (UMAE) of pectin from pomelo peels.

PubMed

Liew, Shan Qin; Ngoh, Gek Cheng; Yusoff, Rozita; Teoh, Wen Hui

2016-12-01

This study aims to optimize sequential ultrasound-microwave assisted extraction (UMAE) on pomelo peel using citric acid. The effects of pH, sonication time, microwave power and irradiation time on the yield and the degree of esterification (DE) of pectin were investigated. Under optimized conditions of pH 1.80, 27.52min sonication followed by 6.40min microwave irradiation at 643.44W, the yield and the DE value of pectin obtained was respectively at 38.00% and 56.88%. Based upon optimized UMAE condition, the pectin from microwave-ultrasound assisted extraction (MUAE), ultrasound assisted extraction (UAE) and microwave assisted extraction (MAE) were studied. The yield of pectin adopting the UMAE was higher than all other techniques in the order of UMAE>MUAE>MAE>UAE. The pectin's galacturonic acid content obtained from combined extraction technique is higher than that obtained from sole extraction technique and the pectin gel produced from various techniques exhibited a pseudoplastic behaviour. The morphological structures of pectin extracted from MUAE and MAE closely resemble each other. The extracted pectin from UMAE with smaller and more regular surface differs greatly from that of UAE. This has substantiated the highest pectin yield of 36.33% from UMAE and further signified their compatibility and potentiality in pectin extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

Evaluation of the antibacterial activity of the methylene chloride extract of Miconia ligustroides, isolated triterpene acids, and ursolic acid derivatives.

PubMed

Cunha, Wilson R; de Matos, Geilton X; Souza, Maria Goreti M; Tozatti, Marcos G; Andrade e Silva, Márcio L; Martins, Carlos H G; da Silva, Rosangela; Da Silva Filho, Ademar A

2010-02-01

The methylene chloride extract of Miconia ligustroides (DC.) Naudin (Melastomataceae), the isolated compounds ursolic and oleanolic acids and a mixture of these acids, and ursolic acid derivatives were evaluated against the following microorganisms: Bacillus cereus (ATCC 14579), Vibrio cholerae (ATCC 9458), Salmonella choleraesuis (ATCC 10708), Klebsiella pneumoniae (ATCC 10031), and Streptococcus pneumoniae (ATCC 6305). The microdilution method was used for determination of the minimum inhibitory concentration (MIC) during evaluation of the antibacterial activity. The methylene chloride extract showed no activity against the selected microorganisms. Ursolic acid was active against B. cereus, showing a MIC value of 20 microg/mL. Oleanolic acid was effective against B. cereus and S. pneumoniae with a MIC of 80 microg/mL in both cases. The mixture of triterpenes, ursolic and oleanolic acids, did not enhance the antimicrobial activity. However, the acetyl and methyl ester derivatives, prepared from ursolic acid, increased the inhibitory activity for S. pneumoniae.

Ulcer healing activity of Mumijo aqueous extract against acetic acid induced gastric ulcer in rats

PubMed Central

Shahrokhi, Nader; Keshavarzi, Zakieh; Khaksari, Mohammad

2015-01-01

Objective: Gastric ulcer is an important clinical problem, chiefly due to extensive use of some drugs. The aim was to assess the activity of Mumijo extract (which is used in traditional medicine) against acetic acid induced gastric ulcer in rats. Materials and Methods: The aqueous extract of Mumijo was prepared. Animals were randomly (n = 10) divided into four groups: Control, sham-operated group (received 0.2 ml of acetic acid to induce gastric ulcer), Mumijo (100 mg/kg/daily) were given for 4 days postacetic acid administration, and ranitidine group (20 mg/kg). The assessed parameters were pH and pepsin levels (by Anson method) of gastric contents and gastric histopathology. Ranitidine was used as reference anti-ulcer drug. Results: The extract (100 mg/kg/daily, p.o.) inhibited acid acetic-induced gastric ulceration by elevating its pH versus sham group (P < 0.01) and decreasing the pepsin levels compared to standard drug, ranitidine (P < 0.05). The histopathology data showed that the treatment with Mumijo extract had a significant protection against all mucosal damages. Conclusion: Mumijo extract has potent antiulcer activity. Its anti-ulcer property probably acts via a reduction in gastric acid secretion and pepsin levels. The obtained results support the use of this herbal material in folk medicine. PMID:25709338

Ginger extract as green corrosion inhibitor of mild steel in hydrochloric acid solution

NASA Astrophysics Data System (ADS)

Fidrusli, A.; Suryanto; Mahmood, M.

2018-01-01

Ginger extract as corrosion inhibitor from natural resources was studied to prevent corrosion of mild steel in acid media. Ginger rhizome was extracted to produce green corrosion inhibitor (G-1) while ginger powder bought at supermarket was also extract to form green corrosion inhibitor (G-2). Effectiveness of inhibitor in preventing corrosion process of mild steel was studied in 1.0 M of hydrochloric acid. The experiment of weight loss method and polarization technique were conducted to measure corrosion rate and inhibition efficiency of mild steel in solution containing 1.0 M of hydrochloric acid with various concentration of inhibitor at room temperature. The results showed that, the rate of corrosion dropped from 8.09 mmpy in solution containing no inhibitor to 0.72 mmpy in solution containing 150g/l inhibitor while inhibition efficiency up to 91% was obtained. The polarization curve in polarization experiments shows that the inhibition efficiency is 86% with high concentration of inhibitor. The adsorption of ginger extract on the surface of mild steel was observed by using optical microscope and the characterization analysis was done by using pH measurement method. When high concentration of green inhibitor in the acid solution is used, the pH at the surface of steel is increasing.

Aqueous extracts of Mozambican plants as alternative and environmentally safe acid-base indicators.

PubMed

Macuvele, Domingos Lusitaneo Pier; Sithole, Gerre Zebedias Samo; Cesca, Karina; Macuvele, Suzana Lília Pinare; Matsinhe, Jonas Valente

2016-06-01

Indicators are substances that change color as the pH of the medium. Many of these substances are dyes of synthetic origin. The mulala plant (Euclea natalensis), which roots are commonly used by rural communities for their oral hygiene, and roseira (Hibiscus rosa-sinensis), an ornamental plant, are abundant in Mozambique. Currently, synthetic acid-base indicators are most commonly used but have environmental implications and, on the other hand, are expensive products, so the demand for natural indicators started. This study investigated the applicability of aqueous extracts of H. rosa-sinensis and E. natalensis as acid-base indicators. Ground on this work, the extracts can be used as acid-base indicators. On the basis of the absorption spectroscopy in both the UV-Vis region and previous studies, it was possible to preliminarily pinpoint anthocyanins and naphthoquinones as responsible for the shifting of colors depending on the pH range of aqueous extracts of H. rosa-sinensis and E. natalensis. These natural indicators are easily accessible, inexpensive, easy to extract, environmentally safe, and locally available.

Improving the two-step remediation process for CCA-treated wood. Part I, Evaluating oxalic acid extraction

Treesearch

Carol Clausen

2004-01-01

In this study, three possible improvements to a remediation process for chromated-copper-arsenate (CCA) treated wood were evaluated. The process involves two steps: oxalic acid extraction of wood fiber followed by bacterial culture with Bacillus licheniformis CC01. The three potential improvements to the oxalic acid extraction step were (1) reusing oxalic acid for...

Effect of steam explosion-assisted extraction on phenolic acid profiles and antioxidant properties of wheat bran.

PubMed

Liu, Liya; Zhao, Mengli; Liu, Xingxun; Zhong, Kui; Tong, Litao; Zhou, Xianrong; Zhou, Sumei

2016-08-01

The majority of phenolic acids in wheat bran are bound to the cell walls. Hence, a high proportion of phenolic acids cannot be extracted with conventional extraction methods. This study aimed to investigate the efficiency of steam explosion pre-treatment in increasing the extractability of phenolic compounds from wheat bran. Bound phenolic acids (BPA) can be released by steam explosion-assisted extraction. Within the experimental range, soluble free phenolic acids (FPA) and soluble conjugated phenolic acids (CPA) increased gradually with residence time and temperature. After steam explosion at 215 °C for 120 s, the total FPA and CPA reached 6671.8 and 2578.6 µg GAE g(-1) bran, respectively, which was about 39-fold and seven-fold higher than that of the untreated sample. Ferulic acid, the major individual phenolic acids in bran, increased from 55.7 to 586.3 µg g(-1) for FPA, and from 44.9 to 1108.4 µg g(-1) for CPA. The antioxidant properties of FPA and CPA extracts were significantly improved after treated. Correlation analysis indicated that the antioxidant capacity was in close relationship with phenolic content in FPA and CPA. Steam explosion pre-treatment could be effectively used to release of BPA and enhance the antioxidant capacity of wheat bran. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

Extraction of Total Nucleic Acids From Ticks for the Detection of Bacterial and Viral Pathogens

PubMed Central

Crowder, Chris D.; Rounds, Megan A.; Phillipson, Curtis A.; Picuri, John M.; Matthews, Heather E.; Halverson, Justina; Schutzer, Steven E.; Ecker, David J.; Eshoo, Mark W.

2010-01-01

Ticks harbor numerous bacterial, protozoal, and viral pathogens that can cause serious infections in humans and domestic animals. Active surveillance of the tick vector can provide insight into the frequency and distribution of important pathogens in the environment. Nucleic-acid based detection of tick-borne bacterial, protozoan, and viral pathogens requires the extraction of both DNA and RNA (total nucleic acids) from ticks. Traditional methods for nucleic acid extraction are limited to extraction of either DNA or the RNA from a sample. Here we present a simple bead-beating based protocol for extraction of DNA and RNA from a single tick and show detection of Borrelia burgdorferi and Powassan virus from individual, infected Ixodes scapularis ticks. We determined expected yields for total nucleic acids by this protocol for a variety of adult tick species. The method is applicable to a variety of arthropod vectors, including fleas and mosquitoes, and was partially automated on a liquid handling robot. PMID:20180313

A hollow-fiber membrane extraction process for recovery and separation of lactic acid from aqueous solution.

PubMed

Huang, Hanjing; Yang, Shang-Tian; Ramey, David E

2004-01-01

An energy-efficient hollow-fiber membrane extraction process was successfully developed to separate and recover lactic acid produced in fermentation. Although many fermentation processes have been developed for lactic acid production, an economical method for lactic acid recovery from the fermentation broth is still needed. Continuous extraction of lactic acid from a simulated aqueous stream was achieved by using Alamine 336 in 2-octanol contained in a hollow-fiber membrane extractor. In this process, the extractant was simultaneously regenerated by stripping with NaOH in a second membrane extractor, and the final product is a concentrated lactate salt solution. The extraction rate increased linearly with an increase in the Alamine 336 content in the solvent (from 5 to 40%). Increasing the concentration of the undissociated lactic acid in the feed solution by either increasing the lactate concentration (from 5 to 40 g/L) or decreasing the solution pH (from 5.0 to 4.0) also increased the extraction rate. Based on these observations, a reactive extraction model with a first-order reaction mechanism for both lactic acid and amine concentrations was proposed. The extraction rate also increased with an increase in the feed flow rate, but not the flow rates of solvent and the stripping solution, suggesting that the process was not limited by diffusion in the liquid films or membrane pores. A mathematical model considering both diffusion and chemical reaction in the extractor and back extractor was developed to simulate the process. The model fits the experimental data well and can be used in scale up design of the process.

Lactic acid bacterial extract as a biogenic mineral growth modifier

NASA Astrophysics Data System (ADS)

Borah, Ballav M.; Singh, Atul K.; Ramesh, Aiyagari; Das, Gopal

2009-04-01

The formation of minerals and mechanisms by which bacteria could control their formation in natural habitats is now of current interest for material scientists to have an insight of the mechanism of in vivo mineralization, as well as to seek industrial and technological applications. Crystalline uniform structures of calcium and barium minerals formed micron-sized building blocks when synthesized in the presence of an organic matrix consisting of secreted protein extracts from three different lactic acid bacteria (LAB) viz.: Lactobacillus plantarum MTCC 1325, Lactobacillus acidophilus NRRL B4495 and Pediococcus acidilactici CFR K7. LABs are not known to form organic matrix in biological materialization processes. The influence of these bacterial extracts on the crystallization behavior was investigated in details to test the basic coordination behavior of the acidic protein. In this report, varied architecture of the mineral crystals obtained in presence of high molecular weight protein extracts of three different LAB strains has been discussed. The role of native form of high molecular weight bacterial protein extracts in the generation of nucleation centers for crystal growth was clearly established. A model for the formation of organic matrix-cation complex and the subsequent events leading to crystal growth is proposed.

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

Identification of Bioactivity, Volatile and Fatty Acid Profile in Supercritical Fluid Extracts of Mexican arnica.

PubMed

García-Pérez, J Saúl; Cuéllar-Bermúdez, Sara P; Arévalo-Gallegos, Alejandra; Rodríguez-Rodríguez, José; Iqbal, Hafiz M N; Parra-Saldivar, Roberto

2016-09-12

Supercritical fluid extraction (SFE) is a sustainable technique used for the extraction of lipophilic metabolites such as pigments and fatty acids. Arnica plant is considered a potential candidate material with high antioxidant and antimicrobial activities. Therefore, in this study, a locally available Heterotheca inuloides, also known as Mexican arnica, was analyzed for the extraction of high-value compounds. Based on different pressure (P), temperature (T), and co-solvent (CoS), four treatments (T) were prepared. A maximum 7.13% yield was recovered from T2 (T = 60 °C, P = 10 MPa, CoS = 8 g/min), followed by 6.69% from T4 (T = 60 °C, P = 30 MPa, CoS = 4 g/min). Some bioactive sesquiterpenoids such as 7-hydroxycadalene, caryophyllene and δ-cadinene were identified in the extracts by GC/MS. The fatty acid profile revealed that the main components were palmitic acid (C16:0), followed by linoleic acid (C18:2ω6c), α-linolenic acid (C18:3ω3) and stearic acid (C18:0) differing in percent yield per treatment. Antibacterial activities were determined by the agar diffusion method, indicating that all the treatments exerted strong antibacterial activity against S. aureus, C. albicans, and E. coli strains. The antioxidant capacity of the extracts was also measured by three in vitro assays, DPPH, TEAC and FRAP, using Trolox as a standard. Results showed high antioxidant capacity enabling pharmaceutical applications of Mexican arnica.

Identification of Bioactivity, Volatile and Fatty Acid Profile in Supercritical Fluid Extracts of Mexican arnica

PubMed Central

García-Pérez, J. Saúl; Cuéllar-Bermúdez, Sara P.; Arévalo-Gallegos, Alejandra; Rodríguez-Rodríguez, José; Iqbal, Hafiz M. N.; Parra-Saldivar, Roberto

2016-01-01

Supercritical fluid extraction (SFE) is a sustainable technique used for the extraction of lipophilic metabolites such as pigments and fatty acids. Arnica plant is considered a potential candidate material with high antioxidant and antimicrobial activities. Therefore, in this study, a locally available Heterotheca inuloides, also known as Mexican arnica, was analyzed for the extraction of high-value compounds. Based on different pressure (P), temperature (T), and co-solvent (CoS), four treatments (T) were prepared. A maximum 7.13% yield was recovered from T2 (T = 60 °C, P = 10 MPa, CoS = 8 g/min), followed by 6.69% from T4 (T = 60 °C, P = 30 MPa, CoS = 4 g/min). Some bioactive sesquiterpenoids such as 7-hydroxycadalene, caryophyllene and δ-cadinene were identified in the extracts by GC/MS. The fatty acid profile revealed that the main components were palmitic acid (C16:0), followed by linoleic acid (C18:2ω6c), α-linolenic acid (C18:3ω3) and stearic acid (C18:0) differing in percent yield per treatment. Antibacterial activities were determined by the agar diffusion method, indicating that all the treatments exerted strong antibacterial activity against S. aureus, C. albicans, and E. coli strains. The antioxidant capacity of the extracts was also measured by three in vitro assays, DPPH, TEAC and FRAP, using Trolox as a standard. Results showed high antioxidant capacity enabling pharmaceutical applications of Mexican arnica. PMID:27626416

Separation of phenolic acids from sugarcane rind by online solid-phase extraction with high-speed counter-current chromatography.

PubMed

Geng, Ping; Fang, Yingtong; Xie, Ronglong; Hu, Weilun; Xi, Xingjun; Chu, Qiao; Dong, Genlai; Shaheen, Nusrat; Wei, Yun

2017-02-01

Sugarcane rind contains some functional phenolic acids. The separation of these compounds from sugarcane rind is able to realize the integrated utilization of the crop and reduce environment pollution. In this paper, a novel protocol based on interfacing online solid-phase extraction with high-speed counter-current chromatography (HSCCC) was established, aiming at improving and simplifying the process of phenolic acids separation from sugarcane rind. The conditions of online solid-phase extraction with HSCCC involving solvent system, flow rate of mobile phase as well as saturated extent of absorption of solid-phase extraction were optimized to improve extraction efficiency and reduce separation time. The separation of phenolic acids was performed with a two-phase solvent system composed of butanol/acetic acid/water at a volume ratio of 4:1:5, and the developed online solid-phase extraction with HSCCC method was validated and successfully applied for sugarcane rind, and three phenolic acids including 6.73 mg of gallic acid, 10.85 mg of p-coumaric acid, and 2.78 mg of ferulic acid with purities of 60.2, 95.4, and 84%, respectively, were obtained from 150 mg sugarcane rind crude extracts. In addition, the three different elution methods of phenolic acids purification including HSCCC, elution-extrusion counter-current chromatography and back-extrusion counter-current chromatography were compared. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

SOLVENT EXTRACTION PROCESS FOR THE RECOVERY OF METALS FROM PHOSPHORIC ACID

DOEpatents

Bailes, R.H.; Long, R.S.

1958-11-01

> A solvent extraction process is presented for recovering metal values including uranium, thorium, and other lanthanide and actinide elements from crude industrial phosphoric acid solutions. The process conslsts of contacting said solution with an immisclble organic solvent extractant containing a diluent and a material selected from the group consisting of mono and di alkyl phosphates, alkyl phosphonates and alkyl phosphites. The uranlum enters the extractant phase and is subsequently recovered by any of the methods known to the art. Recovery is improved if the phosphate solution is treated with a reducing agent such as iron or aluminum powder prior to the extraction step.

Microbial process for the preparation of acetic acid, as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2007-03-27

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. Solvent mixtures formed of such a modified solvent with a desired co-solvent, preferably a low boiling hydrocarbon, are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Microbial process for the preparation of acetic acid, as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2004-06-22

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. Solvent mixtures formed of such a modified solvent with a desired co-solvent, preferably a low boiling hydrocarbon, are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

Selective extraction of derivates of p-hydroxy-benzoic acid from plant material by using a molecularly imprinted polymer.

PubMed

Karasová, Gabriela; Lehotay, Jozef; Sádecká, Jana; Skacáni, Ivan; Lachová, Miroslava

2005-12-01

Selective SPE of derivates of p-hydroxybenzoic acid (pHBA) from plant extract of Melissa officinalis is presented using a molecularly imprinted polymer (MIP) made with protocatechuic acid (PA) as template molecule. MIP was prepared with acrylamide as functional monomer, ethylene glycol dimethacrylate as crosslinking monomer and ACN as porogen. MIP was evaluated towards six phenolic acids: PA, gallic acid, pHBA, vanillic acid (VA), gentisic acid (GeA) and syringic acid (SyrA), and then steps of molecularly imprinted SPE (MISPE) procedure were optimized. The best specific binding capacity of MIP was obtained for PA in ACN (34.7 microg/g of MIP). Other tested acids were also bound on MIP if they were dissolved in this solvent. ACN was chosen as solvent for sample application. M. officinalis was extracted into methanol/water (4:1, v/v), the extract was then evaporated to dryness and dissolved in ACN before application on MIP. Water and ACN were used as washing solvents and elution of benzoic acids was performed by means of a mixture methanol/acetic acid (9:1, v/v). pHBA, GA, PA and VA were extracted with recoveries of 56.3-82.1% using this MISPE method. GeA was not determined in plant extract.

Kinetic study on ferulic acid production from banana stem waste via mechanical extraction

NASA Astrophysics Data System (ADS)

Zainol, Norazwina; Masngut, Nasratun; Khairi Jusup, Muhamad

2018-04-01

Banana is the tropical plants associated with lots of medicinal properties. It has been reported to be a potential source of phenolic compounds such as ferulic acid (FA). FA has excellent antioxidant properties higher than vitamin C and E. FA also have a wide range of biological activities, such as antioxidant activities and anti-microbial activities. This paper presents an experimental and kinetic study on ferulic acid (FA) production from banana stem waste (BSW) via mechanical extraction. The objective of this research is to determine the kinetic parameters in the ferulic acid production. The banana stem waste was randomly collected from the local banana plantation in Felda Lepar Hilir, Pahang. The banana stem juice was mechanically extracted by using sugarcane press machine (KR3176) and further analyzed in high performance liquid chromatography. The differential and integral method was applied to determine the kinetic parameter of the extraction process and the data obtained were fitted into the 0th, 1st and 2nd order of extraction process. Based on the results, the kinetic parameter and R2 value from were 0.05 and 0.93, respectively. It was determined that the 0th kinetic order fitted the reaction processes to best represent the mechanical extraction.

Freeze-out extraction of monocarboxylic acids from water into acetonitrile under the action of centrifugal forces

NASA Astrophysics Data System (ADS)

Bekhterev, V. N.

2016-10-01

It is established that the efficiency of the freezing-out extraction of monocarboxylic acids C3-C;8 and sorbic acid from water into acetonitrile increases under the action of centrifugal forces. The linear growth of the partition coefficient in the homologous series of C2-C8 acids with an increase in molecule length, and the difference between the efficiency of extracting sorbic and hexanoic acid, are discussed using a theoretical model proposed earlier and based on the adsorption-desorption equilibrium of the partition of dissolved organic compounds between the resulting surface of ice and the liquid phase of the extract. The advantages of the proposed technique with respect to the degree of concentration over the method of low-temperature liquid-liquid extraction are explained in light of the phase diagram for the water-acetonitrile mixture.

Composition and structure of asphaltenes in oils of various chemical nature

NASA Astrophysics Data System (ADS)

Sergun, Valeriy P.; Cheshkova, Tatiana V.; Kovalenko, Elena Yu.; Min, Raisa S.; Sagachenko, Tatiana A.

2017-12-01

The asphaltene substances of methane-naphthenic and naphthenic-aromatic oils are characterized via methods of extraction, adsorption chromatography, IR and NMR spectroscopy, and chromatography-mass spectrometry. The data on the composition of their high-molecular components and compounds adsorbed/occluded by molecules of asphaltenes are represented. The role of nitrogenous compounds in the course of structuring of asphaltene components is shown.

Optimization of pectin extraction from banana peels with citric acid by using response surface methodology.

PubMed

Oliveira, Túlio Ítalo S; Rosa, Morsyleide F; Cavalcante, Fabio Lima; Pereira, Paulo Henrique F; Moates, Graham K; Wellner, Nikolaus; Mazzetto, Selma E; Waldron, Keith W; Azeredo, Henriette M C

2016-05-01

A central composite design was used to determine effects of pH (2.0-4.5), extraction temperature (70-90 °C) and time (120-240 min) on the yield, degree of methoxylation (DM) and galacturonic acid content (GA) of pectins extracted from banana peels with citric acid. Changes in composition during the main steps of pectin extraction were followed by Fourier transform infrared (FTIR) spectroscopy. FTIR was also used to determine DM and GA of pectins. Harsh temperature and pH conditions enhanced the extraction yield, but decreased DM. GA presented a maximum value at 83 °C, 190 min, and pH 2.7. The yield of galacturonic acid (YGA), which took into account both the extraction yield and the pectin purity, was improved by higher temperature and lower pH values. The optimum extraction conditions, defined as those resulting in a maximum YGA while keeping DM at a minimum of 51%, were: 87 °C, 160 min, pH 2.0. Copyright © 2015 Elsevier Ltd. All rights reserved.

Use of Dimethyl Pimelimidate with Microfluidic System for Nucleic Acids Extraction without Electricity.

PubMed

Jin, Choong Eun; Lee, Tae Yoon; Koo, Bonhan; Choi, Kyung-Chul; Chang, Suhwan; Park, Se Yoon; Kim, Ji Yeun; Kim, Sung-Han; Shin, Yong

2017-07-18

The isolation of nucleic acids in the lab on a chip is crucial to achieve the maximal effectiveness of point-of-care testing for detection in clinical applications. Here, we report on the use of a simple and versatile single-channel microfluidic platform that combines dimethyl pimelimidate (DMP) for nucleic acids (both RNA and DNA) extraction without electricity using a thin-film system. The system is based on the adaption of DMP into nonchaotropic-based nucleic acids and the capture of reagents into a low-cost thin-film platform for use as a microfluidic total analysis system, which can be utilized for sample processing in clinical diagnostics. Moreover, we assessed the use of the DMP system for the extraction of nucleic acids from various samples, including mammalian cells, bacterial cells, and viruses from human disease, and we also confirmed that the quality and quantity of the nucleic acids extracted were sufficient to allow for the robust detection of biomarkers and/or pathogens in downstream analysis. Furthermore, this DMP system does not require any instruments and electricity, and has improved time efficiency, portability, and affordability. Thus, we believe that the DMP system may change the paradigm of sample processing in clinical diagnostics.

Experimental design for extraction and quantification of phenolic compounds and organic acids in white "Vinho Verde" grapes.

PubMed

Dopico-García, M S; Valentão, P; Guerra, L; Andrade, P B; Seabra, R M

2007-01-30

An experimental design was applied for the optimization of extraction and clean-up processes of phenolic compounds and organic acids from white "Vinho Verde" grapes. The developed analytical method consisted in two steps: first a solid-liquid extraction of both phenolic compounds and organic acids and then a clean-up step using solid-phase extraction (SPE). Afterwards, phenolic compounds and organic acids were determined by high-performance liquid chromatography (HPLC) coupled to a diode array detector (DAD) and HPLC-UV, respectively. Plackett-Burman design was carried out to select the significant experimental parameters affecting both the extraction and the clean-up steps. The identified and quantified phenolic compounds were: quercetin-3-O-glucoside, quercetin-3-O-rutinoside, kaempferol-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin, kaempferol and epicatechin. The determined organic acids were oxalic, citric, tartaric, malic, shikimic and fumaric acids. The obtained results showed that the most important variables were the temperature (40 degrees C) and the solvent (acid water at pH 2 with 5% methanol) for the extraction step and the type of sorbent (C18 non end-capped) for the clean-up step.

Extraction of ethanol with higher carboxylic acid solvents and their toxicity to yeast

USDA-ARS?s Scientific Manuscript database

In a screening exercise for ethanol-selective extraction solvents, partitioning of ethanol and water from a 5 wt% aqueous solution into several C8 – C18 carboxylic acids was studied. Results for the acids are compared with those from alcohols of similar structure. In all cases studied, the acids exh...

Influence of gelatinization on the extraction of phenolic acids from wheat fractions

USDA-ARS?s Scientific Manuscript database

The effect of gelatinization on the analysis of phenolic acids from wheat bran, whole-wheat, and refined flour samples was investigated using two extraction procedures, namely, ultrasonic (UAE) and microwave (MAE). The total phenolic acid (TPA) concentration quantity in wheat bran (2711-2913 µg/g) w...

Production of citric acid using its extraction wastewater treated by anaerobic digestion and ion exchange in an integrated citric acid-methane fermentation process.

PubMed

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

2014-08-01

In order to solve the problem of extraction wastewater pollution in citric acid industry, an integrated citric acid-methane fermentation process is proposed in this study. Extraction wastewater was treated by mesophilic anaerobic digestion and then used to make mash for the next batch of citric acid fermentation. The recycling process was done for seven batches. Citric acid production (82.4 g/L on average) decreased by 34.1 % in the recycling batches (2nd-7th) compared with the first batch. And the residual reducing sugar exceeded 40 g/L on average in the recycling batches. Pigment substances, acetic acid, ammonium, and metal ions in anaerobic digestion effluent (ADE) were considered to be the inhibitors, and their effects on the fermentation were studied. Results indicated that ammonium, Na(+) and K(+) in the ADE significantly inhibited citric acid fermentation. Therefore, the ADE was treated by acidic cation exchange resin prior to reuse to make mash for citric acid fermentation. The recycling process was performed for ten batches, and citric acid productions in the recycling batches were 126.6 g/L on average, increasing by 1.7 % compared with the first batch. This process could eliminate extraction wastewater discharge and reduce water resource consumption.

Valerenic acid and Valeriana officinalis extracts delay onset of Pentylenetetrazole (PTZ)-Induced seizures in adult Danio rerio (Zebrafish).

PubMed

Torres-Hernández, Bianca A; Del Valle-Mojica, Lisa M; Ortíz, José G

2015-07-14

Anticonvulsant properties have been attributed to extracts of the herbal medicine Valeriana officinalis. Our aims were to examine the anticonvulsant properties of valerenic acid and valerian extracts and to determine whether valerian preparations interact with the activity of other anti-epileptic drugs (phenytoin or clonazepam). To achieve these goals, we validated the adult zebrafish, Danio rerio, as an animal model for studying anticonvulsant drugs. All drug treatments were administered by immersion in water containing the drug. For assays of anticonvulsant activity, zebrafish were pretreated with: anti-epileptic drugs, valerenic acid, aqueous or ethanolic valerian extracts, or mixtures (phenytoin or clonazepam with valerenic acid or valerian extracts). Seizures were then induced with pentylenetetrazole (PTZ). A behavioral scale was developed for scoring PTZ-induced seizures in adult zebrafish. The seizure latency was evaluated for all pretreatments and control, untreated fish. Valerenic acid and both aqueous and ethanolic extracts of valerian root were also evaluated for their ability to improve survival after pentylenetetrazole-challenge. The assay was validated by comparison with well-studied anticonvulsant drugs (phenytoin, clonazepam, gabapentin and valproate). One-way ANOVA followed by Tukey post-hoc test was performed, using a p < 0.05 level of significance. All treatments were compared with the untreated animals and with the other pretreatments. After exposure to pentylenetetrazole, zebrafish exhibited a series of stereotypical behaviors prior to the appearance of clonic-like movements--convulsions. Both valerenic acid and valerian extracts (aqueous and ethanolic) significantly extended the latency period to the onset of seizure (convulsion) in adult zebrafish. The ethanolic valerian extract was a more potent anticonvulsant than the aqueous extract. Valerenic acid and both valerian extracts interacted synergistically with clonazepam to extended the

Rosmarinic acid content in antidiabetic aqueous extract of Ocimum canum sims grown in Ghana.

PubMed

Berhow, Mark A; Affum, Andrews Obeng; Gyan, Ben A

2012-07-01

Rosmarinic acid (RA) is an important antioxidant polyphenol that is found in a variety of spices and herbs, including Ocimum canum Sims (locally called eme or akokobesa in Ghana). Aqueous extracts from the leaves of O. canum are used as an antidiabetic herbal medicine in Ghana. Analytical thin-layer chromatography was used to examine the composition of the polyphenols in leaf extracts. The polyphenol content in the aqueous and methanol extracts from the leaf, as determined by the Folin-Ciocalteu method, were 314 and 315 mg gallic acid equivalent/g leaf sample, respectively. The total flavonoid concentration as determined by the aluminum(III) chloride method was 135 mg catechin equivalent/g leaf sample. High-performance liquid chromatography coupled to an electrospray Quadrupole time-of-flight mass spectrometer was also used to determine the polyphenol fingerprint profile in the leaf extracts of O. canum. Although the average RA concentration in the O. canum leaf extracts from Ghana was 1.69 mg/g dry weight (reported values range from 0.01 to 99.62 mg/g dry weight), this polyphenol was still a prominent peak in addition to caffeic acid derivatives.

Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2006-07-11

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2002-01-01

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Methanol extract of grain dust shows complement fixing activity and other characteristics similar to tannic acid.

PubMed Central

Skea, D; Broder, I

1986-01-01

We have found several similarities between tannic acid and grain dust extract prepared with methanol. Both formed a precipitate with IgG, and these interactions were inhibited by albumin. In addition, both preparations fixed complement; this activity was heat stable and was removed by prior adsorption of the preparations with hide powder. Adsorption with polyvinyl polypyrrolidone reduced the complement-fixing activity of tannic acid but not that of the methanol grain dust extract. The similarities between tannic acid and the methanol grain dust extract are consistent with the presence of a tannin or tanninlike material in grain dust. Images FIGURE 1. PMID:3709479

Sodium sulphite inhibition of potato and cherry polyphenolics in nucleic acid extraction for virus detection by RT-PCR.

PubMed

Singh, R P; Nie, X; Singh, M; Coffin, R; Duplessis, P

2002-01-01

Phenolic compounds from plant tissues inhibit reverse transcription-polymerase chain reaction (RT-PCR). Multiple-step protocols using several additives to inhibit polyphenolic compounds during nucleic acid extraction are common, but time consuming and laborious. The current research highlights that the inclusion of 0.65 to 0.70% of sodium sulphite in the extraction buffer minimizes the pigmentation of nucleic acid extracts and improves the RT-PCR detection of Potato virus Y (PVY) and Potato leafroll virus (PLRV) in potato (Solanum tuberosum) tubers and Prune dwarf virus (PDV) and Prunus necrotic ringspot virus (PNRSV) in leaves and bark in the sweet cherry (Prunus avium) tree. Substituting sodium sulphite in the nucleic acid extraction buffer eliminated the use of proteinase K during extraction. Reagents phosphate buffered saline (PBS)-Tween 20 and polyvinylpyrrolidone (PVP) were also no longer required during RT or PCR phase. The resultant nucleic acid extracts were suitable for both duplex and multiplex RT-PCR. This simple and less expensive nucleic acid extraction protocol has proved very effective for potato cv. Russet Norkotah, which contains a high amount of polyphenolics. Comparing commercially available RNA extraction kits (Catrimox and RNeasy), the sodium sulphite based extraction protocol yielded two to three times higher amounts of RNA, while maintaining comparable virus detection by RT-PCR. The sodium sulphite based extraction protocol was equally effective in potato tubers, and in leaves and bark from the cherry tree.

Effects of microwave power and irradiation time on pectin extraction from watermelon rinds (Citrullus lanatus) with acetic acid using microwave assisted extraction method

NASA Astrophysics Data System (ADS)

Sari, A. M.; Ishartani, D.; Dewanty, P. S.

2018-01-01

The aims of this research are to study the effect of microwave power (119.7 W, 199.5 W and 279.3 W) and irradiation time (6, 9 and 12 min) on pectin extraction by using Microwave Assisted Extraction (MAE) with acetic acid and to do a preliminary characterization of pectin from watermelon rinds. A randomized factorial design with two factors was used to determine the effect of microwave power and processing time on the yield, equivalent weight, degree of methoxylation (DM), galacturonic acid content (GA) and the degree of esterification (DE) of extracted pectin. The results showed that extracted pectin from watermelon rinds using MAE method have yield ranged from 3.925% to 5.766%, with equivalent weight ranged from 1249.702 to 2007.756. Extracted pectin have a DM value ranged from 3.89% to 10.81%. Galacturonic acid content that meets with IPPA standard resulted from extraction condition of 279.3-watt microwave power for 9 min and 12 min. The degree of esterification (DE) value ranged from 56.86% to 85.76%, and this value exhibited a relatively high methoxyl pectin (>50%). The best pectin properties was obtained at a microwave power of 279.3 watts for 12 min.

Simultaneous Determination of Oleanolic Acid and Ursolic Acid by in Vivo Microdialysis via UHPLC-MS/MS Using Magnetic Dispersive Solid Phase Extraction Coupling with Microwave-Assisted Derivatization and Its Application to a Pharmacokinetic Study of Arctiumlappa L. Root Extract in Rats.

PubMed

Zheng, Zhenjia; Zhao, Xian-En; Zhu, Shuyun; Dang, Jun; Qiao, Xuguang; Qiu, Zhichang; Tao, Yanduo

2018-04-18

Simultaneous detection of oleanolic acid and ursolic acid in rat blood by in vivo microdialysis can provide important pharmacokinetics information. Microwave-assisted derivatization coupled with magnetic dispersive solid phase extraction was established for the determination of oleanolic acid and ursolic acid by liquid chromatography tandem mass spectrometry. 2'-Carbonyl-piperazine rhodamine B was first designed and synthesized as the derivatization reagent, which was easily adsorbed onto the surface of Fe 3 O 4 /graphene oxide. Simultaneous derivatization and extraction of oleanolic acid and ursolic acid were performed on Fe 3 O 4 /graphene oxide. The permanent positive charge of the derivatization reagent significantly improved the ionization efficiencies. The limits of detection were 0.025 and 0.020 ng/mL for oleanolic acid and ursolic acid, respectively. The validated method was shown to be promising for sensitive, accurate, and simultaneous determination of oleanolic acid and ursolic acid. It was used for their pharmacokinetics study in rat blood after oral administration of Arctiumlappa L. root extract.

Development of an improved sample preparation platform for acidic endogenous hormones in plant tissues using electromembrane extraction.

PubMed

Suh, Joon Hyuk; Han, Sang Beom; Wang, Yu

2018-02-02

Despite their importance in pivotal signaling pathways due to trace quantities and complex matrices, the analysis of plant hormones is a challenge. Here, to improve this issue, we present an electromembrane extraction technology combined with liquid chromatography-tandem mass spectrometry for determination of acidic plant hormones including jasmonic acid, abscisic acid, salicylic acid, benzoic acid, gibberellic acid and gibberellin A 4 in plant tissues. Factors influencing extraction efficiency, such as voltage, extraction time and stirring rate were optimized using a design of experiments. Analytical performance was evaluated in terms of specificity, linearity, limit of quantification, precision, accuracy, recovery and repeatability. The results showed good linearity (r 2  > 0.995), precision and acceptable accuracy. The limit of quantification ranged from 0.1 to 10 ng mL -1 , and the recoveries were 34.6-50.3%. The developed method was applied in citrus leaf samples, showing better clean-up efficiency, as well as higher sensitivity compared to a previous method using liquid-liquid extraction. Organic solvent consumption was minimized during the process, making it an appealing method. More noteworthy, electromembrane extraction has been scarcely applied to plant tissues, and this is the first time that major plant hormones were extracted using this technology, with high sensitivity and selectivity. Taken together, this work gives not only a novel sample preparation platform using an electric field for plant hormones, but also a good example of extracting complex plant tissues in a simple and effective way. Copyright © 2017 Elsevier B.V. All rights reserved.

Isolation and pharmacological characterization of fatty acids from saw palmetto extract.

PubMed

Abe, Masayuki; Ito, Yoshihiko; Suzuki, Asahi; Onoue, Satomi; Noguchi, Hiroshi; Yamada, Shizuo

2009-04-01

Saw palmetto extract (SPE) has been widely used for the treatment of lower urinary-tract symptoms secondary to benign prostatic hyperplasia. The mechanisms of pharmacological effects of SPE include the inhibition of 5alpha-reductase, anti-androgenic effects, anti-proliferative effects, and anti-inflammatory effects. Previously, we showed that SPE bound actively to alpha(1)-adrenergic, muscarinic and 1,4-dihydropyridine calcium channel (1,4-DHP) receptors in the prostate and bladder of rats, whereas its active constituents have not been fully clarified. The present investigation is aimed to identify the main active components contained in hexane and diethyl ether extracts of SPE with the use of column chromatography and preparative HPLC. Based on the binding activity with alpha(1)-adrenergic, muscarinic, and 1,4-DHP receptors, both isolated oleic and lauric acids were deduced to be active components. Authentic samples of oleic and lauric acids also exhibited similar binding activities to these receptors as the fatty acids isolated from SPE, consistent with our findings. In addition, oleic and lauric acids inhibited 5alpha-reductase, possibly leading to therapeutic effects against benign prostatic hyperplasia and related lower urinary-tract symptoms.

[Colorectal cancer preventive effect of combined administration of phenolic acids and supercritical extracts from Angelica sinensis].

PubMed

Peng, Yu; Zhao, Bo-Chen; Kang, Qian; Liu, Jia; Chen, Cheng; Li, Bing-Shao; Xie, Yuan-Ping; Wu, Qing

2018-03-01

This study aimed to investigate the colorectal cancer preventive effect of the combined administration of phenolic acids and supercritical extracts from Angelica sinensis. The AOM/DSS model in mice was adopted. Phenolic acids were administrated orally in the initial stage of the model at a dose of 1 g·kg⁻¹ BW, which was combined withtherectal administration with three doses of supercritical extracts (15, 30, 60 g·kg⁻¹ BW). PCNA, 8-oxoguaine, γ-H2AX, iNOS and COX-2 were tested by immunohistochemistry and Western blot assays. The results showed that the combined administration of phenolic acids and supercritical extracts from A. sinensis suppressed the tumor growth and cell proliferation, and DNA damages and inflammatory responses were reduced in a dose-dependent manner. These results indicate that the combined administration of phenolic acids and supercritical extracts from A. sinensis have a certain effect in preventing carcinogenesis. Copyright© by the Chinese Pharmaceutical Association.

Some Antifungal Properties of Sorbic Acid Extracted from Berries of Rowan (Sorbus Aucuparia).

ERIC Educational Resources Information Center

Brunner, Ulrich

1985-01-01

The food preservative sorbic acid can be extracted from Eurasian mountain ash berries (commercially available) and used to show antifungal properties in microbiological investigations. Techniques for extraction, purification, ultraviolet analysis, and experiments displaying antifungal activity are described. A systematic search for similar…

Anti-Inflammatory Activity of Citric Acid-Treated Wheat Germ Extract in Lipopolysaccharide-Stimulated Macrophages.

PubMed

Jeong, Hee-Yeong; Choi, Yong-Seok; Lee, Jae-Kang; Lee, Beom-Joon; Kim, Woo-Ki; Kang, Hee

2017-07-10

Until recently, fermentation was the only processing used to improve the functionality of wheat germ. The release of 2,6-dimethoxy-1,4-benzoquinone (DMBQ) from hydroquinone glycosides during the fermentation process is considered a marker of quality control. Here, we treated wheat germ extract with citric acid (CWG) to release DMBQ and examined the anti-inflammatory activity of this extract using a lipopolysaccharide-activated macrophage model. Treatment of wheat germ with citric acid resulted in detectable release of DMBQ but reduced total phenolic and total flavonoid contents compared with untreated wheat germ extract (UWG). CWG inhibited secretion of the pro-inflammatory cytokines tumor necrosis factor-α, interleukin (IL)-6, and IL-12 and the synthesis of cyclooxygenase-2, while UWG only decreased IL-12 production. CWG and UWG induced high levels of anti-inflammatory IL-10 and heme oxygenase-1. CWG specifically inhibited phosphorylation of NF-κB p65 and p38 kinase at 15 min after LPS stimulation. Our study showed that citric acid treatment enhanced the anti-inflammatory activity of wheat germ extract.

Evaluation of in-situ fatty acid extraction protocols for the analysis of staphylococcal cell membrane associated fatty acids by gas chromatography.

PubMed

Crompton, Marcus J; Dunstan, R Hugh

2018-05-01

The composition and integrity of the bacterial cytoplasmic membrane is critical to the survival of staphylococci in dynamic environments and it is important to investigate how the cell membrane responds to changes in the environmental conditions. The staphylococcal membrane differs from eukaryotic and many other bacterial cell membranes by having a high abundance of branch fatty acids and relatively few unsaturated fatty acids. The range of available methods for extraction and efficient analyses of staphylococcal fatty acids was initially appraised to identify the best potential procedures for appraisal. Staphylococcus aureus subsp. aureus Rosenbach (ATCC® 29213) was grown under optimal conditions to generate a cell biomass to compare the efficiencies of three approaches to extract and prepare methyl esters of the membrane fatty acids: (1) acidic direct transesterification of lipids, (2) modified basic direct transesterification of membrane lipids with adjusted reaction times and temperatures, and (3) base catalysed hydrolysis followed by acid catalysed esterification in two separate chemical reactions (MIDI process). All methods were able to extract fatty acids from the cell mass effectively where these lipids represented approximately 5% of the cellular dry mass. The acidic transesterification method had the least number of steps, the lowest coefficient of variation at 6.7% and good resistance to tolerating water. Basic transesterification was the least accurate method showing the highest coefficient of variation (26%). The MIDI method showed good recoveries, but had twice the number of steps and a coefficient of variation of 16%. It was also found that there was no need to use an anti-oxidant such as BHT for the protection of polyunsaturated fatty acids when the GC-MS injection liner was clean. It was concluded that the acidic transesterification procedures formed the most efficient and reproducible method for the analyses of staphylococcal membrane fatty acids

Comparison of supercritical fluid extraction and ultrasound-assisted extraction of fatty acids from quince (Cydonia oblonga Miller) seed using response surface methodology and central composite design.

PubMed

Daneshvand, Behnaz; Ara, Katayoun Mahdavi; Raofie, Farhad

2012-08-24

Fatty acids of Cydonia oblonga Miller cultivated in Iran were obtained by supercritical (carbon dioxide) extraction and ultrasound-assisted extraction methods. The oils were analyzed by capillary gas chromatography using mass spectrometric detections. The compounds were identified according to their retention indices and mass spectra (EI, 70eV). The experimental parameters of SFE such as pressure, temperature, modifier volume, static and dynamic extraction time were optimized using a Central Composite Design (CCD) after a 2(5) factorial design. Pressure and dynamic extraction time had significant effect on the extraction yield, while the other factors (temperature, static extraction time and modifier volume) were not identified as significant factors under the selected conditions. The results of chemometrics analysis showed the highest yield for SFE (24.32%), which was obtained at a pressure of 353bar, temperature of 35°C, modifier (methanol) volume of 150μL, and static and dynamic extraction times of 10 and 60min, respectively. Ultrasound-assisted extraction (UAE) of Fatty acids from C. oblonga Miller was optimized, using a rotatable central composite design. The optimum conditions were as follows: solvent (n-hexane) volume, 22mL; extraction time, 30min; and extraction temperature, 55°C. This resulted in a maximum oil recovery of 19.5%. The extracts with higher yield from both methods were subjected to transesterification and GC-MS analysis. The results show that the oil obtained by SFE with the optimal operating conditions allowed a fatty acid composition similar to the oil obtained by UAE in optimum condition and no significant differences were found. The major components of oil extract were Linoleic, Palmitic, Oleic, Stearic and Eicosanoic acids. Copyright © 2012 Elsevier B.V. All rights reserved.

Simultaneous extraction and HPLC determination of 3-indole butyric acid and 3-indole acetic acid in pea plant by using ionic liquid-modified silica as sorbent.

PubMed

Sheikhian, Leila; Bina, Sedigheh

2016-01-15

In this study, ionic liquid-modified silica was used as sorbent for simultaneous extraction and preconcentration of 3-indole butyric acid and 3-indole acetic acid in pea plants. The effect of some parameters such as pH and ionic strength of sample solution, amount of sorbent, flow rate of aqueous sample solution and eluent solution, concentration of eluent solution, and temperature were studied for each hormone solution. Percent extraction of 3-indole butyric acid and 3-indole acetic acid was strongly affected by pH of aqueous sample solution. Ionic strength of aqueous phase and temperature showed no serious effects on extraction efficiency of studied plant hormones. Obtained breakthrough volume was 200mL for each of studied hormones. Preconcentration factor for spectroscopic and chromatographic determination of studied hormones was 100 and 4.0×10(3) respectively. Each solid sorbent phase was reusable for almost 10 times of extraction/stripping procedure. Relative standard deviations of extraction/stripping processes of 3-indole butyric acid and 3-indole acetic acid were 2.79% and 3.66% respectively. The calculated limit of detections for IBA and IAA were 9.1×10(-2)mgL(-1) and 1.6×10(-1)mgL(-1) respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Antiulcerogenic activity of crude extract, fractions and populnoic acid isolated from Austroplenckia populnea (Celastraceae).

PubMed

Andrade, Sérgio F; Antoniolli, Daiane; Comunello, Eros; Cardoso, Luis G V; Carvalho, José C T; Bastos, Jairo K

2006-01-01

Many plant crude extracts and their isolated compounds are the most attractive sources of new drugs and show promising results for the treatment of gastric ulcers. Austroplenckia populnea is commonly known as "marmelinho-do campo, mangabeira-brava, mangabarana and vime" and it has been used in folk medicine as anti-dysenteric and anti-rheumatic. Powdered bark wood (3.25 kg) was macerated with aqueous ethanol (96%) and the extract was concentrated under reduced pressure to yield 406 g of crude hydralcoholic extract. The hydralcoholic extract was suspended in aqueous methanol and partitioned with hexane, chloroform and ethyl acetate (EtOAc) in sequence, yielding 8.0 g, 9.5 g and 98.17 g of crude extracts, respectively. Chromatography of the hexane extract over a silica gel column led to the isolation of the triterpene populnoic acid. The oral administration of hydralcoholic, hexane, chloroform and EtOAc extracts (200 mg/kg) decreased the ulcer lesion index (ULI) by 83.15%, 46.87%, 32.2%, 68.12%, respectively. Oral administration of populnoic acid (100 mg/kg) diminished the ULI by 55.29%. All the obtained results were significant in comparison with the negative control, with exception of the chloroform extract.

Fatty acid profile and elemental content of avocado (Persea americana Mill.) oil--effect of extraction methods.

PubMed

Reddy, Mageshni; Moodley, Roshila; Jonnalagadda, Sreekanth B

2012-01-01

Interest in vegetable oil extracted from idioblast cells of avocado fruit is growing. In this study, five extraction methods to produce avocado oil have been compared: traditional solvent extraction using a Soxhlet or ultrasound, Soxhlet extraction combined with microwave or ultra-turrax treatment and supercritical fluid extraction (SFE). Traditional Soxhlet extraction produced the most reproducible results, 64.76 ± 0.24 g oil/100 g dry weight (DW) and 63.67 ± 0.20 g oil/100 g DW for Hass and Fuerte varieties, respectively. Microwave extraction gave the highest yield of oil (69.94%) from the Hass variety. Oils from microwave extraction had the highest fatty acid content; oils from SFE had wider range of fatty acids. Oils from Fuerte variety had a higher monounsaturated: saturated FA ratio (3.45-3.70). SFE and microwave extraction produced the best quality oil, better than traditional Soxhlet extraction, with the least amount of oxidizing metals present. Copyright © Taylor & Francis Group, LLC

Ultrasound-assisted extraction of pectins from grape pomace using citric acid: a response surface methodology approach.

PubMed

Minjares-Fuentes, R; Femenia, A; Garau, M C; Meza-Velázquez, J A; Simal, S; Rosselló, C

2014-06-15

An ultrasound-assisted procedure for the extraction of pectins from grape pomace with citric acid as the extracting agent was established. A Box-Behnken design (BBD) was employed to optimize the extraction temperature (X1: 35-75°C), extraction time (X2: 20-60 min) and pH (X3: 1.0-2.0) to obtain a high yield of pectins with high average molecular weight (MW) and degree of esterification (DE) from grape pomace. Analysis of variance showed that the contribution of a quadratic model was significant for the pectin extraction yield and for pectin MW whereas the DE of pectins was more influenced by a linear model. An optimization study using response surface methodology was performed and 3D response surfaces were plotted from the mathematical model. According to the RSM model, the highest pectin yield (∼32.3%) can be achieved when the UAE process is carried out at 75°C for 60 min using a citric acid solution of pH 2.0. These pectic polysaccharides, composed mainly by galacturonic acid units (<97% of total sugars), have an average MW of 163.9 kDa and a DE of 55.2%. Close agreement between experimental and predicted values was found. These results suggest that ultrasound-assisted extraction could be a good option for the extraction of functional pectins with citric acid from grape pomace at industrial level. Copyright © 2014 Elsevier Ltd. All rights reserved.

Optimization of squalene extraction from Palm Fatty Acid Distillate (PFAD) in multistage process

NASA Astrophysics Data System (ADS)

Sibuyo, Leah; Widiputri, Diah; Legowo, Evita

2017-01-01

Squalene is a compound widely known as one of the natural antioxidants used in the cosmetic and pharmaceutical industries. As the main source of squalene, which is shark liver oil, is becoming more limited in its availability, attempts have been made to extract squalene from other sources, e.g. from vegetable oils. Research has found that one of the wastes produced by palm oil industry, namely the palm fatty acid distillate (PFAD), contains squalene among other useful compounds. Since Indonesia is one of the largest producers of palm oil, the abundant amount of PFAD becomes very interesting to be a solution in coping with today demand of natural squalene. In this research, the extraction of squalene from PFAD is optimized through a multiple-stage extraction process, where results show a significant increase of squalene yield. Furthermore, the liquid-liquid phase equilibrium data for an extraction using dichloromethane (DCM) were plotted to develop a ternary-phase-diagram between squalene, DCM and free-fatty acids.

Enhanced extraction of butyric acid under high-pressure CO2 conditions to integrate chemical catalysis for value-added chemicals and biofuels.

PubMed

Chun, Jaesung; Choi, Okkyoung; Sang, Byoung-In

2018-01-01

Extractive fermentation with the removal of carboxylic acid requires low pH conditions because acids are better partitioned into the solvent phase at low pH values. However, this requirement conflicts with the optimal near-neutral pH conditions for microbial growth. CO 2 pressurization was used, instead of the addition of chemicals, to decrease pH for the extraction of butyric acid, a fermentation product of Clostridium tyrobutyricum , and butyl butyrate was selected as an extractant. CO 2 pressurization (50 bar) improved the extraction efficiency of butyric acid from a solution at pH 6, yielding a distribution coefficient ( D ) 0.42. In situ removal of butyric acid during fermentation increased the production of butyric acid by up to 4.10 g/L h, an almost twofold increase over control without the use of an extraction process. In situ extraction of butyric acid using temporal CO 2 pressurization may be applied to an integrated downstream catalytic process for upgrading butyric acid to value-added chemicals in an organic solvent.

Recovery of Uranium from Wet Phosphoric Acid by Solvent Extraction Processes

DOE PAGES

Beltrami, Denis; Cote, Gérard; Mokhtari, Hamid; ...

2014-11-17

Between 1951 and 1991, we developed about 17 processes to recover uranium from wet phosphoric acid (WPA), but the viability of these processes was subject to the variation of the uranium price market. Nowadays, uranium from WPA appears to be attractive due to the increase of the global uranium demand resulting from the emergence of developing countries. Moreover, the increasing demand provides impetus for a new look at the applicable technology with a view to improvements as well as altogether new approaches. This paper gives an overview on extraction processes developed in the past to recover uranium from wet phosphoricmore » acid (WPA) as well as the physicochemistry involved in these processes. Recent advances concerning the development of new extraction systems are also reported and discussed.« less

Supercritical carbon dioxide extraction of seed oil from winter melon (Benincasa hispida) and its antioxidant activity and fatty acid composition.

PubMed

Bimakr, Mandana; Rahman, Russly Abdul; Taip, Farah Saleena; Adzahan, Noranizan Mohd; Sarker, Md Zaidul Islam; Ganjloo, Ali

2013-01-15

In the present study, supercritical carbon dioxide (SC-CO(2)) extraction of seed oil from winter melon (Benincasa hispida) was investigated. The effects of process variables namely pressure (150-300 bar), temperature (40-50 °C) and dynamic extraction time (60-120 min) on crude extraction yield (CEY) were studied through response surface methodology (RSM). The SC-CO(2) extraction process was modified using ethanol (99.9%) as co-solvent. Perturbation plot revealed the significant effect of all process variables on the CEY. A central composite design (CCD) was used to optimize the process conditions to achieve maximum CEY. The optimum conditions were 244 bar pressure, 46 °C temperature and 97 min dynamic extraction time. Under these optimal conditions, the CEY was predicted to be 176.30 mg-extract/g-dried sample. The validation experiment results agreed with the predicted value. The antioxidant activity and fatty acid composition of crude oil obtained under optimized conditions were determined and compared with published results using Soxhlet extraction (SE) and ultrasound assisted extraction (UAE). It was found that the antioxidant activity of the extract obtained by SC-CO(2) extraction was strongly higher than those obtained by SE and UAE. Identification of fatty acid composition using gas chromatography (GC) showed that all the extracts were rich in unsaturated fatty acids with the most being linoleic acid. In contrast, the amount of saturated fatty acids extracted by SE was higher than that extracted under optimized SC-CO(2) extraction conditions.

Application of ionic liquids based microwave-assisted simultaneous extraction of carnosic acid, rosmarinic acid and essential oil from Rosmarinus officinalis.

PubMed

Liu, Tingting; Sui, Xiaoyu; Zhang, Rongrui; Yang, Lei; Zu, Yuangang; Zhang, Lin; Zhang, Ying; Zhang, Zhonghua

2011-11-25

An ionic liquid based microwave-assisted simultaneous extraction and distillation (ILMSED) method has been developed for the effective extraction of carnosic acid (CA), rosmarinic acid (RA) and essential oil (EO) from Rosmarinus officinalis. A series of 1-alkyl-3-methylimidazolium ionic liquids differing in composition of anion and cation were evaluated for extraction yield in this work. The results obtained indicated that the anions and cations of ionic liquids had influences on the extraction of CA and RA, 1.0M 1-octyl-3-methylimidazolium bromide ([C8mim]Br) solution was selected as solvent. In addition, the ILMSED procedures for the three target ingredients were optimized and compared with other conventional extraction techniques. ILMSED gave the best result due to the highest extraction yield within the shortest extraction time for CA and RA. The novel process developed offered advantages in term of yield and selectivity of EO and shorter isolation time (20 min in comparison of 4h of hydrodistillation), and provides a more valuable EO (with high amount of oxygenated compounds). The microstructures and chemical structures of rosemary samples before and after extraction were also investigated. Moreover, the proposed method was validated by the stability, repeatability and recovery experiments. The results indicated that the developed ILMSED method provided a good alternative for the both extraction of non-volatile compounds (CA and RA) and EO from rosemary as well as other herbs. Copyright © 2011 Elsevier B.V. All rights reserved.

Extraction of long-chain fatty acids in isolated rat heart during acute low-flow ischemia.

PubMed

Richter, W S; Fischer, S; Ernst, N; Munz, D L

2001-07-01

Although beta-oxidation of fatty acids is suppressed rapidly during ischemia, the behavior of fatty acid extraction at different flow rates is incompletely understood. This study assessed the relationship between flow and extraction of (123)I-iodophenylpentadecanoic acid (IPPA) in the isolated heart model, especially at low flow. Isolated hearts from male Wistar rats (n = 15) were subjected to retrograde perfusion with constant flow (Krebs Henseleit solution containing 10 mmol/L glucose). A latex balloon in the left ventricle allowed isovolumetric contractions and ventricular pressure measurements. The extraction of (123)I-IPPA was assessed with the indicator dilution technique and (99m)Tc-albumin as the intravascular reference. The flow was either increased from the control flow (8 mL/min) until 300% or reduced until 10%. (123)I-IPPA extraction was measured three times before and 10 min after flow alteration. The tracer uptake was estimated from the product of net extraction and flow. The mean (123)I-IPPA extraction at the control flow (third measurement) was 51.6% +/- 2.8%. Between flow rates of approximately 25% and 300%, (123)I-IPPA extraction increased exponentially at decreasing flow rates. At flow rates < or =25% of the control flow, (123)I-IPPA extraction was exponentially higher than predicted. (123)I-IPPA uptake and flow changed largely in parallel. During low flow, the rate-pressure product showed the expected decline (perfusion-contraction matching). The extraction of (123)I-IPPA is preserved and slightly increased (relative to flow) during acute low-flow ischemia.

Towards an efficient protocol for the determination of triterpenic acids in olive fruit: a comparative study of drying and extraction methods.

PubMed

Goulas, Vlasios; Manganaris, George A

2012-01-01

Triterpenic acids, such as maslinic acid and oleanolic acid, are commonly found in olive fruits and have been associated with many health benefits. The drying and extraction methods, as well as the solvents used, are critical factors in the determination of their concentration in plant tissues. Thus, there is an emerging need for standardisation of an efficient extraction protocol that determines triterpenic acid content in olive fruits. To evaluate common extraction methods of triterpenic acids from olive fruits and to determine the effect of the drying method on their content in order to propose an optimum protocol for their quantification. The efficacy of different drying and extraction methods was evaluated through the quantification of maslinic acid and oleanolic acid contents using the reversed-phase HPLC technique. Data showed that ultrasonic assisted extraction with ethanol or a mixture of ethanol:methanol (1:1, v/v) resulted in the recovery of significantly higher amounts of triterpenic acids than other methods used. The drying method also affected the estimated triterpenic acid content; frozen or lyophilised olive fruit material gave higher yields of triterpenic acids compared with air-dried material at both 35°C and 105°C. This study provides a rapid and low-cost extraction method, i.e. ultrasonic assisted extraction with an eco-friendly solvent such as ethanol, from frozen or lyophilised olive fruit for the accurate determination of the triterpenic acid content in olive fruit. Copyright © 2011 John Wiley & Sons, Ltd.

Ultrasonic-Assisted Extraction of Raspberry Seed Oil and Evaluation of Its Physicochemical Properties, Fatty Acid Compositions and Antioxidant Activities

PubMed Central

Huang, Qun; Wang, Jinli; Lin, Qiyang; Liu, Mingxin; Lee, Won Young; Song, Hongbo

2016-01-01

Ultrasonic-assisted extraction was employed for highly efficient separation of aroma oil from raspberry seeds. A central composite design with two variables and five levels was employed and effects of process variables of sonication time and extraction temperature on oil recovery and quality were investigated. Optimal conditions predicted by response surface methodology were sonication time of 37 min and extraction temperature of 54°C. Specifically, ultrasonic-assisted extraction (UAE) was able to provide a higher content of beneficial unsaturated fatty acids, whereas conventional Soxhlet extraction (SE) resulted in a higher amount of saturated fatty acids. Moreover, raspberry seed oil contained abundant amounts of edible linoleic acid and linolenic acid, which suggest raspberry seeds could be valuable edible sources of natural γ-linolenic acid products. In comparison with SE, UAE exerted higher free radical scavenging capacities. In addition, UAE significantly blocked H2O2-induced intracellular reactive oxygen species (ROS) generation. PMID:27120053

Antioxidant activity and sensory analysis of a rosmarinic acid-enriched extract of garden sage (Salvia officinalis)

USDA-ARS?s Scientific Manuscript database

A novel extract of S. officinalis (garden sage) was prepared using supercritical carbon dioxide (SC-CO2) extraction, followed by a Soxhlet hot water extraction. The resulting extract was enriched in polyphenols, including rosmarinic acid (RA), which has shown promising health benefits in animals. Th...

The fluorimetric microdetermination of glyoxylic acid in blood, urine and bacterial extracts

PubMed Central

Zarembski, P. M.; Hodgkinson, A.

1965-01-01

1. A spectrophotofluorimetric method for the determination of glyoxylic acid in biological materials is described. 2. The method is based on the reaction between glyoxylic acid and resorcinol in acid solution, a fluorescent complex being obtained on the subsequent addition of alkali. 3. The reaction was found to be sensitive and highly specific, the minimum detectable amount of glyoxylic acid being 1·35×10−8 mole. 4. The urinary excretion of glyoxylic acid by ten normal adults ranged from 1·4 to 4·7mg./24hr. Small but measurable amounts of glyoxylic acid were found in cell-free extracts of Pseudomonas oxalaticus OX1 grown on oxalic acid as a source of carbon. No glyoxylic acid was detected in human serum. PMID:14343135

RAPESEED PHOSPHATIDYLCHOLINE HYDROLYSIS TO PHOSPHATIDIC ACID USING PLANT EXTRACTS WITH PHOPSPHOLIPASE D.

PubMed

Pasker, Beata; Sosada, Marian; Fraś, Paweł; Boryczka, Monika; Górecki, Michał; Zych, Maria

2015-01-01

Phosphatidic acid (PA) has a crucial role in cell membrane structure and function. For that reason it has a possible application in the treatment of some health disorders in humans, can be used as a natural and non toxic emulsifier and the component of drug carriers in pharmaceuticals and cosmetics as well as a component for synthesis of some new phospholipids. PA is short-lived in the cell and is difficult to extract directly from the biological material. PA may be easily prepared by hydrolysis of phospholipids, especially phosphatidylcholine (PC), using cabbage phospholipase D (PLD). Hydrolytic activity of purified by us PLD extracts from cabbage towards rapeseed phosphatidylcholine (RPC) was investigated. Hydrolysis was carried out in the biphasic system (water/diethyl ether) at pH 6,5 and temp 30°C. Influence of enzymatic extracts from three cabbage varieties, reaction time, Ca2+ concentration and enzyme extracts/PC ratio, on activity towards RPC resulting in rapeseed phosphatidic acid (RPA) formation were examined. Our study shows that the PLD extracts from savoy cabbage (PLDsc), white cabbage (PLDwc) and brussels sprouts (PLDbs) used in experiments exhibit hydrolytic activity towards RPC resulting in rapeseed RPA with different yield. The highest activity towards RPC shows PLD extract from PLDsc with the RPC conversion degree to RPA (90%) was observed at 120 mM Ca2+ concentration, reaction time 60 min and ratio of PLD extract to RPC 6 : 1 (w/w). Our study shows that purified by us PLDsc extracts exhibit hydrolytic activity towards RPC giving new RPA with satisfying conversion degree for use in pharmacy, cosmetics and as a standard in analytical chemistry.

Population impacts in white sucker (Catostomus commersonii) exposed to oil sands-derived contaminants in the Athabasca River.

PubMed

Arens, Collin J; Arens, Jennifer C; Hogan, Natacha S; Kavanagh, Richard J; Berrue, Fabrice; Van Der Kraak, Glen J; van den Heuvel, Michael R

2017-08-01

Biological and chemical endpoints were measured in white sucker collected downstream of Athabasca oil sands developments (AB, Canada) and compared with those at Calling Lake (AB, Canada), a reference location upstream of the Athabasca oil sands deposit. Naphthenic acid concentrations were also measured at 14 sites in the Athabasca River watershed. Concentrations of naphthenic acids were elevated in tributaries adjacent to oil sands mining developments. Tributary naphthenic acid profiles were more similar to aged oil sands process water than samples from the Athabasca River, suggesting an influence of tailings in the tributaries. White sucker showed higher energy storage in the Athabasca River as indicated by significantly higher condition and liver size. White sucker were not investing that energy into reproductive effort as measured by gonad size and fecundity, which were significantly reduced relative to the reference location. White sucker showed increased exposure to polycyclic aromatic hydrocarbons as indicated by hepatic cytochrome P4501A (CYP1A) activity and fluorescent bile metabolites, as well as higher concentrations of naphthenic acids in bile. Cadmium, copper, nickel, and selenium were also elevated in white sucker liver tissue compared with the reference location. Based on the exposure profile and response pattern observed, effects on energy storage and utilization in white sucker from the Athabasca River most likely resulted from exposure to polycyclic aromatic hydrocarbons derived from petrogenic and pyrolytic sources. Environ Toxicol Chem 2017;36:2058-2067. © 2017 SETAC. © 2017 SETAC.

Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

PubMed

Washington, John W; Henderson, W Matthew; Ellington, J Jackson; Jenkins, Thomas M; Evans, John J

2008-02-15

With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorooctanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary phases, two different liquid chromatography-tandem mass spectrometry (LC/MS/MS) systems, and eight combinations of sample-extract pretreatments, extractions and cleanups on three test soils. For the columns and systems we tested, we achieved the greatest analytical sensitivity for PFCAs using a column with a C(18) stationary phase in a Waters LC/MS/MS. In this system we achieved an instrument detection limit for PFOA of 270 ag/microL, equating to about 14 fg of PFOA on-column. While an elementary acetonitrile/water extraction of soils recovers PFCAs effectively, natural soil organic matter also dissolved in the extracts commonly imparts significant noise that appears as broad, multi-nodal, asymmetric peaks that coelute with several PFCAs. The intensity and elution profile of this noise is highly variable among soils and it challenges detection of low concentrations of PFCAs by decreasing the signal-to-noise contrast. In an effort to decrease this background noise, we investigated several methods of pretreatment, extraction and cleanup, in a variety of combinations, that used alkaline and unbuffered water, acetonitrile, tetrabutylammonium hydrogen sulfate, methyl-tert-butyl ether, dispersed activated carbon and solid-phase extraction. For the combined objectives of complete recovery and minimization of background noise, we have chosen: (1) alkaline pretreatment; (2) extraction with acetonitrile/water; (3) evaporation to dryness; (4) reconstitution with tetrabutylammonium-hydrogen-sulfate ion-pairing solution; (5) ion-pair extraction to methyl-tert-butyl ether; (6) evaporation to dryness; (7) reconstitution with 60/40 acetonitrile/water (v/v); and (8) analysis by LC/MS/MS. Using this method, we

Application of a continuous distribution model for proton binding by humic acids extracted from acidic lake sediments

NASA Astrophysics Data System (ADS)

Rhea, James R.; Young, Thomas C.

1987-10-01

The proton binding characteristics of humic acids extracted from the sediments of Cranberry Pond, an acidic water body located in the Adirondack Mountain region of New York State, were explored by the application of a multiligand distribution model. The model characterizes a class of proton binding sites by mean log K values and the standard deviations of log K values about the mean. Mean log K values and their relative abundances were determined directly from experimental titration data. The model accurately predicts the binding of protons by the humic acids for pH values in the range 3.5 to 10.0.

Application of a continuous distribution model for proton binding by humic acids extracted from acidic lake sediments

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

Rhea, J.R.; Young, T.C.

1987-01-01

The proton binding characteristics of humic acids extracted from the sediments of Cranberry Pond, an acidic water body located in the Adirondack Mountain region of New York State, were explored by the application of a nultiligand distribution model. The model characterizes a class of proton binding sites by mean log K values and the standard deviations of log K values and the mean. Mean log K values and their relative abundances were determined directly from experimental titration data. The model accurately predicts the binding of protons by the humic acids for pH values in the range 3.5 to 10.0.

Optimization of Extraction Conditions for Phenolic Acids from the Leaves of Melissa officinalis L. Using Response Surface Methodology

PubMed Central

Yoo, Guijae; Lee, Il Kyun; Park, Seonju; Kim, Nanyoung; Park, Jun Hyung; Kim, Seung Hyun

2018-01-01

Background: Melissa officinalis L. is a well-known medicinal plant from the family Lamiaceae, which is distributed throughout Eastern Mediterranean region and Western Asia. Objective: In this study, response surface methodology (RSM) was utilized to optimize the extraction conditions for bioactive compounds from the leaves of M. officinalis L. Materials and Methods: A Box–Behnken design (BBD) was utilized to evaluate the effects of three independent variables, namely extraction temperature (°C), methanol concentration (%), and solvent-to-material ratio (mL/g) on the responses of the contents of caffeic acid and rosmarinic acid. Results: Regression analysis showed a good fit of the experimental data. The optimal condition was obtained at extraction temperature 80.53°C, methanol concentration 29.89%, and solvent-to-material ratio 30 mL/g. Conclusion: These results indicate the suitability of the model employed and the successful application of RSM in optimizing the extraction conditions. This study may be useful for standardizing production quality, including improving the efficiency of large-scale extraction systems. SUMMARY The optimum conditions for the extraction of major phenolic acids from the leaves of Melissa officinalis L. were determined using response surface methodologyBox–Behnken design was utilized to evaluate the effects of three independent variablesQuadratic polynomial model provided a satisfactory description of the experimental dataThe optimized condition for simultaneous maximum contents of caffeic acid and rosmarinic acid was determined. Abbreviations used: RSM: Response surface methodology, BBD: Box–Behnken design, CA: Caffeic acid, RA: Rosmarinic acid, HPLC: High-performance liquid chromatography. PMID:29720824

Sorption of Cu(2+) on humic acids sequentially extracted from a sediment.

PubMed

Yang, Kun; Miao, Gangfen; Wu, Wenhao; Lin, Daohui; Pan, Bo; Wu, Fengchang; Xing, Baoshan

2015-11-01

In addition to the diverse properties of humic acids (HAs) extracted from different soils or sediments, chemical compositions, functional groups and structures of HAs extracted from a single soil or sediment could also be diverse and thus significantly affect sorption of heavy metals, which is a key process controlling the transfer, transformation and fate of heavy metals in the environment. In this study, we sequentially extracted four HA fractions from a single sediment and conducted the sorption experiments of Cu(2+) on these HA fractions. Our results showed that aromaticity and acidic group content of HA fraction decreased with increasing extraction. Earlier extracted HA fraction had higher sorption capacity and affinity for Cu(2+). There were two fractions of adsorbed Cu(2+) on HAs, i.e., ion exchanged fraction and surface bonded fraction, which can be captured mechanically by the bi-Langmuir model with good isotherm fitting. The ion exchanged fraction had larger sorption capacity but lower sorption affinity, compared with the surface bonded fraction. The dissociated carboxyl groups of HAs were responsible for both fractions of Cu(2+) sorption, due to the more Cu(2+) sorption on the earlier extracted HA fraction with more carboxyl groups and at higher pH. The intensive competition between H(+) and the exchangeable Cu(2+) could result in the decrease of ion exchanged capacity and affinity for Cu(2+) on HAs. Copyright © 2015 Elsevier Ltd. All rights reserved.

Deproteinization of water-soluble ß-glucan during acid extraction from fruiting bodies of Pleurotus ostreatus mushrooms.

PubMed

Szwengiel, Artur; Stachowiak, Barbara

2016-08-01

Some ß-glucans can be easily extracted from Basidiomycete mushrooms but commonly used extraction procedures are not satisfactory. A simultaneous method for acid extraction and deproteinization in the case of Pleurotus ostreatus was developed using response surface methodology. The optimized extraction conditions proposed here (30°C, 3.8% HCl, 300min, stirring) allow for the simultaneous extraction and deproteinization of polysaccharides. Additionally, the acid extraction yield was 7 times greater than that of hot water extraction. The combined enzymatic digestion with lyticase, ß-glucanase, exo-1,3-ß-d-glucanase, and ß-glucosidase results elucidated that an extract containing ß-1,3-ß-1,6-ß-1,4-glucan. The gel permeation chromatography (GPC) results showed that the two glucan fractions obtained do not contain linked proteins. The weight average molecular weight of the first fraction (Mw=1137kDa) was 60 times higher than that of the second fraction (Mw=19kDa). Copyright © 2016 Elsevier Ltd. All rights reserved.

Bacillus subtilis Lipid Extract, A Branched-Chain Fatty Acid Model Membrane

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

Nickels, Jonathan D.; Chatterjee, Sneha; Mostofian, Barmak

Lipid extracts are an excellent choice of model biomembrane; however at present, there are no commercially available lipid extracts or computational models that mimic microbial membranes containing the branched-chain fatty acids found in many pathogenic and industrially relevant bacteria. Here, we advance the extract of Bacillus subtilis as a standard model for these diverse systems, providing a detailed experimental description and equilibrated atomistic bilayer model included as Supporting Information to this Letter and at (http://cmb.ornl.gov/members/cheng). The development and validation of this model represents an advance that enables more realistic simulations and experiments on bacterial membranes and reconstituted bacterial membrane proteins.

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.

Biotransformation of caffeoyl quinic acids from green coffee extracts by Lactobacillus johnsonii NCC 533.

PubMed

Bel-Rhlid, Rachid; Thapa, Dinesh; Kraehenbuehl, Karin; Hansen, Carl Erik; Fischer, Lutz

2013-01-01

The potential of Lactobacillus johnsonii NCC 533 to metabolize chlorogenic acids from green coffee extract was investigated. Two enzymes, an esterase and a hydroxycinnamate decarboxylase (HCD), were involved in this biotransformation. The complete hydrolysis of 5-caffeoylquinic acid (5-CQA) into caffeic acid (CA) by L. johnsonii esterase occurred during the first 16 h of reaction time. No dihydrocaffeic acid was identified in the reaction mixture. The decarboxylation of CA into 4-vinylcatechol (4-VC) started only when the maximum concentration of CA was reached (10 μmol/ml). CA was completely transformed into 4-VC after 48 h of incubation. No 4-vinylphenol or other derivatives could be identified in the reaction media. In this study we demonstrate the capability of L. johnsonii to transform chlorogenic acids from green coffee extract into 4-VC in two steps one pot reaction. Thus, the enzymatic potential of certain lactobacilli might be explored to generate flavor compounds from plant polyphenols.

Spiroketalcarminic Acid, a Novel Minor Anthraquinone Pigment in Cochineal Extract Used in Food Additives.

PubMed

Ito, Yusai; Harikai, Naoki; Ishizuki, Kyoko; Shinomiya, Kazufusa; Sugimoto, Naoki; Akiyama, Hiroshi

2017-09-01

Cochineal extract prepared from the scale insect Dactylopus coccus (American cochineal) has been used as a natural red dye for food, cosmetics, and pharmaceuticals. The major pigment in cochineal extract is carminic acid (CA), an anthraquinone glucoside, and several minor pigments have been previously reported. Our investigation aimed at establishing the safety of cochineal dye products using ultra performance liquid chromatography-photo diode array-electrospray ionization-time of flight (UPLC-PDA-ESI-TOF)/MS found an unknown minor pigment, spiroketalcarminic acid (1), in three commercial cochineal extract samples; cochineal extract used in food additives, carmine that is an aluminum salt of cochineal extract used as natural dye, and a research reagent of CA. The purification of 1 from cochineal extract involved sequential chromatographic techniques, including preparative reversed-phase HPLC. Two dimensional (2D)-NMR and mass analyses established the structure of 1 to be a novel anthraquinone with an unusual 6,5-spiroketal system instead of the C-glucosyl moiety of CA. The absolute stereochemistry of the spiroketal moiety in 1 was determined by nuclear Overhauser effect spectroscopy (NOESY) correlations and optical rotation. No data corresponding to 1 had previously been reported for extracts of dried cochineal insects and traditional art products dyed with cochineal extract, indicating that 1 is likely produced during the preparation of commercial cochineal extract.

Total lactic acid bacteria, antioxidant activity, and acceptance of synbiotic yoghurt with red ginger extract (Zingiberofficinale var. rubrum)

NASA Astrophysics Data System (ADS)

Larasati, B. A.; Panunggal, B.; Afifah, D. N.; Anjani, G.; Rustanti, N.

2018-02-01

Antioxidant related to oxidative stress can caused the metabolic disorders. A functional food that high in antioxidant can be use as the alternative prevention. The addition of red ginger extract in yoghurt could form a functional food, that high in antioxidant, synbiotic and fiber. The influence of red ginger extract on yoghurt synbiotic against lactic acid bacteria, antioxidant activity and acceptance were analyzed. This was an experimental research with one factor complete randomized design, specifically the addition of red ginger extract 0%; 0,1%; 0,3% and 0,5% into synbiotic yoghurt. Total plate count method used to analyze the lactic acid bacteria, 1-1-diphenyl-2-picrylhydrazyl (DPPH) method for antioxidant activity, and acceptance analyzed with hedonic test. The higher the dose of extract added to synbiotic yoghurt, the antioxidant activity got significantly increased (ρ=0,0001), while the lactic acid bacteria got insignificantly decreased (ρ=0,085). The addition of 0,5% red ginger extract obtained the antioxidant activity of 71% and 4,86 × 1013 CFU/ml on lactic acid bacteria, which the requirement for probiotic on National Standard of Indonesia is >107 CFU/ml. The addition of extract had a significant effect on acceptance (ρ=0,0001) in flavor, color, and texture, but not aroma (ρ=0,266). The optimal product in this research was the yoghurt synbiotic with addition of 0,1% red ginger extract. To summarize, the addition of red ginger extract in synbiotic yoghurt had significant effect on antioxidant activity, flavor, color, and texture, but no significant effect on lactic acid bacteria and aroma.

Influence of Humic Acids Extracted from Peat by Different Methods on Functional Activity of Macrophages in Vitro.

PubMed

Trofimova, E S; Zykova, M V; Ligacheva, A A; Sherstoboev, E Y; Zhdanov, V V; Belousov, M V; Yusubov, M S; Krivoshchekov, S V; Danilets, M G; Dygai, A M

2017-04-01

We studied activation of macrophages with humic acids extracted from peat of large deposits in the Tomsk region by two extraction methods: by hydroxide or sodium pyrophosphate. Humic acid of lowland peat types containing large amounts of aromatic carbon, phenolic and alcohol groups, carbohydrate residues and ethers, irrespectively of the extraction methods contained LPS admixture that probably determines their activating properties. Humic acid of upland peat types characterized by high content of carbonyl, carboxyl, and ester groups enhance NO production and reduce arginase expression, but these effects were minimized when sodium hydroxide was used as an extraction solvent. Pyrophosphate samples of the upland peat types were characterized by aromaticity and diversity of functional groups and have a significant advantage because of they induce specific endotoxin-independent stimulating action on antigen presenting cells.

Needle trap extraction for GC analysis of formic and acetic acids in aqueous solution.

PubMed

Lee, Xinqing; Huang, Daikuan; Lou, Dawei; Pawliszyn, Janusz

2012-07-01

Formic and acetic acids are ubiquitous in the environment, food, and most of the natural products. Extraction of the acids from aqueous solution is required for their isotope analysis by the gas chromatography-isotope ratio mass spectrometry. To this objective, we have previously developed a purge-and-trap technique using the dynamic solid-phase microextraction technology, the NeedlEX. The extraction efficiency, however, remains unexamined. Here, we address this question using the flame ionization detector and isotope ratio mass spectrometer while comparing it with that of the CAR/PDMS fiber. The results show that the NeedlEX is applicable at a wide range of concentration through coordination of purge volume given the minimum amount 3.7 ng and 1.8 ng of formic and acetic, respectively, is extracted. The efficiency of NeedlEX was 6-7 times lower than the fiber at 1000 μg/mL depending on the analyte. It is, however, superior to the latter at 10 μg/mL or less owing to its lower detection limit. The extraction efficiency of both acids is equivalent in molar amount. This is, however, disguised by the different response of the flame ionization detector. The isotope ratio mass spectrometor overcomes this problem but is compromised by relatively large errors. These results are particularly useful for isotopic analysis of carboxylic acids. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of medium chain fatty acids from organic municipal waste and subsequent production of bio-based fuels.

PubMed

Kannengiesser, Jan; Sakaguchi-Söder, Kaori; Mrukwia, Timo; Jager, Johannes; Schebek, Liselotte

2016-01-01

these three pre-treatments, the percolate is brought to a refinery to extract the non-polar fatty acids using bio-diesel, which was generated from used kitchen oil at the refinery. The extraction tests in the lab have proved that the efficiency of the liquid-liquid-extraction is directly linked with the chain length and polarity of the fatty acids. By using a non-polar bio-diesel mainly the non-polar fatty acids, like pentanoic to octanoic acid, are extracted. After extraction, the bio-diesel enriched with the fatty acids is esterified. As a result bio-diesel with a lower viscosity than usual is produced. The fatty acids remaining in the percolate after the extraction can be used in another fermentation process to generate biogas. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of aluminum, zinc, copper, and lead on the acid-base properties of water extracts from soils

NASA Astrophysics Data System (ADS)

Motuzova, G. V.; Makarychev, I. P.; Petrov, M. I.

2013-01-01

The potentiometric titration of water extracts from the upper horizons of taiga-zone soils by salt solutions of heavy metals (Pb, Cu, and Zn) showed that their addition is an additional source of the extract acidity because of the involvement of the metal ions in complexation with water-soluble organic substances (WSOSs). At the addition of 0.01 M water solutions of Al(NO3)3 to water extracts from soils, Al3+ ions are also involved in complexes with WSOSs, which is accompanied by stronger acidification of the extracts from the upper horizon of soddy soils (with a near-neutral reaction) than from the litter of bog-podzolic soil (with a strongly acid reaction). The effect of the Al3+ hydrolysis on the acidity of the extracts is insignificantly low in both cases. A quantitative relationship was revealed between the release of protons and the ratio of free Cu2+ ions to those complexed with WSOSs at the titration of water extracts from soils by a solution of copper salt.

Studies of the acidic components of the Colorado Green River formation oil shale-Mass spectrometric identification of the methyl esters of extractable acids.

NASA Technical Reports Server (NTRS)

Haug, P.; Schnoes, H. K.; Burlingame, A. L.

1971-01-01

Study of solvent extractable acidic constituents of oil shale from the Colorado Green River Formation. Identification of individual components is based on gas chromatographic and mass spectrometric data obtained for their respective methyl esters. Normal acids, isoprenoidal acids, alpha, omega-dicarboxylic acids, mono-alpha-methyl dicarboxylic acids and methyl ketoacids were identified. In addition, the presence of monocyclic, benzoic, phenylalkanoic and naphthyl-carboxylic acids, as well as cycloaromatic acids, is demonstrated by partial identification.

Identification of optimum fatty acid extraction methods for two different microalgae Phaeodactylum tricornutum and Haematococcus pluvialis for food and biodiesel applications.

PubMed

Otero, Paz; Saha, Sushanta Kumar; Gushin, Joanne Mc; Moane, Siobhan; Barron, John; Murray, Patrick

2017-07-01

Microalgae have the potential to synthesize and accumulate lipids which contain high value fatty acids intended for nutrition and biodiesel applications. Nevertheless, lipid extraction methods for microalgae cells are not well established and there is not a standard analytical methodology to extract fatty acids from lipid-producing microalgae. In this paper, current lipid extraction procedures employing organic solvents (chloroform/methanol, 2:1 and 1:2, v/v), sodium hypochlorite solution (NaClO), acid-catalysed hot-water extraction and the saponification process [2.5 M KOH/methanol (1:4, v/v)] have been evaluated with two species of microalgae with different types of cell walls. One is a marine diatom, Phaeodactylum tricornutum, and the other a freshwater green microalga, Haematococcus pluvialis. Lipids from all types of extracts were estimated gravimetrically and their fatty acids were quantified by a HPLC equipped with Q-TOF mass spectrometer. Results indicated significant differences both in lipids yield and fatty acids composition. The chloroform and methanol mixture was the most effective extraction solvent for the unsaturated fatty acids such as DPA (C22:05), DHA, (C22:06), EPA (C20:05) and ARA (C20:04). While acid treatments improved the saturated fatty acids (SFAs) yield, especially the short chain SFA, lauric acid (C12:0), whose amount was 64% higher in P. tricornutum and 156% higher in H. pluvialis compared to organic solvent extractions. Graphical abstract ᅟ.

Engineering Design Handbook - Military Pyrotechnics Series. Part Four. Design of Ammunition for Pyrotechnic Effects

DTIC Science & Technology

1974-03-15

Type 1) is a mixture of 88.5 percent gasoline and 11.5 percent napalm thickener. Napalm thickener is a granular base aluminum soap of naphthenic ...methacrylate polymer AE (IM) 5.0 5.0 2.0 3.0 3.0 3.0 3.0 Stearic acid 3.0 — — 1.0 4.0 3.0 4.5 Fatty acids - 2.5 3.0 - — — — Naphthenic acid - 2.5...3.0 3.0 — 1.0 0.5 Calcium oxide 2.0 — — 3.1 4.0 3.5 _ Caustic soda (40% solution) — 3.0 4.5 — — — — Ammonium hydroxide (27% solution

Used Oil and Its Regulation in the United States

DTIC Science & Technology

1988-09-30

product containing significant quantities of alkyl, naphthenic , and aromatic hydrocarbons. The oil may also contain additives to improve its...delivered to the re-refiners each year is disposed of primarily in the process residues including spent clay, acid sludge, and wastewater.13 8 13 7 Frank...hydrocarbon structure into three main groups: parafinic, naphthenic , and aromatic. Paraffinic (alkanic) crude oils contain mostly saturated straight and

Acid-switched Eu(III) coordination inside reverse aggregates: Insights into a synergistic liquid-liquid extraction system

DOE PAGES

Ellis, Ross J.

2016-08-09

Determining the structure of complex solutions bearing metal ions is challenging, but crucial for developing important technologies such as liquid-liquid extraction for metal refining and separation purposes. Herein, the structure of an organic Eu(III) solution consisting a binary mixture of lipophilic ligands di-2-ethylhexyl phosphoric acid (HDEHP) and tetraoctyl diglycolamide (TODGA) in dodecane is studied using synchrotron small angle X-ray scattering (SAXS) and X-ray absorption fine structure spectroscopy (EXAFS). This system is of technological importance in f-element separation for nuclear fuel cycle applications, where extraction is controlled by varying nitric acid concentration. Extraction is promoted at low and high concentration, butmore » is retarded at intermediate concentration, leading to a U-shaped function; the structural origins of which we investigate. At the nanoscale, the solution is apparently comprised of reverse micelles with polar cores of approximately 1 nm in size, and these remain virtually unchanged as acid concentration is varied. Inside the polar cores, the coordination environment of Eu(III) switches from a 9-coordinate [Eu(TODGA) 3] 3+ motif at high acid, to a 6-coordinate HDEHP-dominated complex resembling Eu(HDEHP·DEHP) 3 at low acid. The results show that extraction is controlled within the coordination sphere, where it is promoted under conditions that favor coordination of either one of the two organic ligands, but is retarded under conditions that encourage mixed complexes. Lastly, our results link solution structure with ion transport properties in a technologically-important liquid-liquid ion extraction system.« less

Selective Interactions of Valeriana officinalis Extracts and Valerenic Acid with [H]Glutamate Binding to Rat Synaptic Membranes.

PubMed

Del Valle-Mojica, Lisa M; Ayala-Marín, Yoshira M; Ortiz-Sanchez, Carmen M; Torres-Hernández, Bianca A; Abdalla-Mukhaimer, Safa; Ortiz, José G

2011-01-01

Although GABA neurotransmission has been suggested as a mechanism for Valeriana officinalis effects, CNS depression can also be evoked by inhibition of ionotropic (iGluR) and metabotropic glutamate receptors (mGluR). In this study, we examined if aqueous valerian extract interacted with glutamatergic receptors. Freshly prepared aqueous valerian extract was incubated with rat cortical synaptic membranes in presence of 20 nM [(3)H]Glutamate. Aqueous valerian extract increased [(3)H]Glutamate binding from 1 × 10(-7) to 1 × 10(-3) mg/mL. In the presence of (2S,1'S,2'S)-2-(Carboxycyclopropyl)glycine (LCCG-I) and (2S,2'R,3'R)-2-(2',3'-Dicarboxycyclopropyl)glycine (DCG-IV), Group II mGluR agents, valerian extract markedly decreased [(3)H]Glutamate binding, while (2S)-2-amino-3-(3,5-dioxo-1,2,4-oxadiazolidin-2-yl) propanoic acid) (quisqualic acid, QA), Group I mGluR agonist, increased [(3)H]Glutamate binding. At 0.05 mg/mL aqueous valerian extract specifically interacted with kainic acid NMDA and AMPA receptors. Valerenic acid, a marker compound for Valeriana officinalis, increased the [(3)H]Glutamate binding after 1.6 × 10(-2) mg/mL, and at 0.008 mg/mL it interacted only with QA (Group I mGluR). The selective interactions of valerian extract and valerenic acid with Group I and Group II mGluR may represent an alternative explanation for the anxiolytic properties of this plant.

Rapid microwave-assisted acid extraction of metals from chromated copper arsenate (CCA)-treated southern pine wood

Treesearch

Bin Yu; Chung Y. Hse; Todd F. Shupe

2009-01-01

The effects of acid concentration, reaction time, and temperature in a microwave reactor on recovery of CCA-treated wood were evaluated. Extraction of copper, chromium, and arsenic metals from chromated copper arsenate (CCA)-treated southern pine wood samples with three different acids (i.e., acetic acid, oxalic acid, and phosphoric acid) was investigated using in...

Improved method for extracting lanthanides and actinides from acid solutions

DOEpatents

Horwitz, E.P.; Kalina, D.G.; Kaplan, L.; Mason, G.W.

1983-07-26

A process for the recovery of actinide and lanthanide values from aqueous acidic solutions uses a new series of neutral bi-functional extractants, the alkyl(phenyl)-N,N-dialkylcarbamoylmethylphosphine oxides. The process is suitable for the separation of actinide and lanthanide values from fission product values found together in high-level nuclear reprocessing waste solutions.

Ultrasound-assisted Extraction of Ursolic Acid from the Flowers of Ixora coccinia Linn (Rubiaceae) and Antiproliferative Activity of Ursolic Acid and Synthesized Derivatives

PubMed Central

Alves Monteath, Silvana Amadeu Ferreira; Maciel, Maria Aparecida M.; Vega, Raquel Garcia; de Mello, Heloisa; de Araújo Martins, Carollina; Esteves-Souza, Andressa; Gattass, Cerli Rocha; Echevarria, Aurea

2017-01-01

Background: Ixora coccinea Linn (Rubiaceae) is an evergreen shrub with bright scarlet colored flowers found in several tropical and subtropical countries. It is used as an ornamental and medicinal plant. Phytochemical studies revealed that its major special metabolites are triterpene acids, such as ursolic and oleanolic acid. Objective: To evaluate the isolation of ursolic acid (UA) (1) from methanol extracts of I. coccinea flowers through two methodologies, to prepare four derivatives, and to evaluate the cytotoxic effect against six cancer cell lines. Materials and Methods: The UA was isolated from vegetal material by percolation at room temperature and by ultrasound-assisted extraction. The preparation of derivatives was performed according to literature methods, and the cytotoxic effects were evaluated using the MTT (3,4,5-dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide) assay. Results: The most efficient extraction was achieved through ultrasound irradiation with a yield of 35% after KOH-impregnated silica in chromatography column. Furthermore, four derivatives (3, 5, 6, 7) of UA were prepared and evaluated, including 1, against two lung cancer (A549 and H460) and four leukemia (K562, Lucena, HL60, and Jurkat) cell lines. Generally, results showed that 1 and 7 were the most active compounds against the assayed cell lines. Also, the cytotoxic effects observed on terpenes 1 and 7 were higher when compared with cisplatin, used as positive control, with the exception of Jurkat cell line. Conclusion: The efficiency of such an alternative extraction method led to the principal and abundant active component, 1, of I. coccinea, thus representing a considerable contribution for promising triterpenoid in cancer chemotherapy. SUMMARY The ultrasound-assisted extraction of Ixora coccinea flowers improved of the ursolic acid isolationMethanolic extract from flowers of I. coccinea provided, by ultrasound irradiation, after KOH-impregnated silica in chromatography column

Hollow Fiber Supported Liquid Membrane Extraction Combined with HPLC-UV for Simultaneous Preconcentration and Determination of Urinary Hippuric Acid and Mandelic Acid

PubMed Central

Bahrami, Abdulrahman; Ghamari, Farhad; Yamini, Yadollah; Ghorbani Shahna, Farshid; Moghimbeigi, Abbas

2017-01-01

This work describes a new extraction method with hollow-fiber liquid-phase microextraction based on facilitated pH gradient transport for analyzing hippuric acid and mandelic acid in aqueous samples. The factors affecting the metabolites extraction were optimized as follows: the volume of sample solution was 10 mL with pH 2 containing 0.5 mol·L−1 sodium chloride, liquid membrane containing 1-octanol with 20% (w/v) tributyl phosphate as the carrier, the time of extraction was 150 min, and stirring rate was 500 rpm. The organic phase immobilized in the pores of a hollow fiber was back-extracted into 24 µL of a solution containing sodium carbonate with pH 11, which was placed inside the lumen of the fiber. Under optimized conditions, the high enrichment factors of 172 and 195 folds, detection limit of 0.007 and 0.009 µg·mL−1 were obtained. The relative standard deviation (RSD) (%) values for intra- and inter-day precisions were calculated at 2.5%–8.2% and 4.1%–10.7%, respectively. The proposed method was successfully applied to the analysis of these metabolites in real urine samples. The results indicated that hollow-fiber liquid-phase microextraction (HF-LPME) based on facilitated pH gradient transport can be used as a sensitive and effective method for the determination of mandelic acid and hippuric acid in urine specimens. PMID:28208685

A novel automated device for rapid nucleic acid extraction utilizing a zigzag motion of magnetic silica beads.

PubMed

Yamaguchi, Akemi; Matsuda, Kazuyuki; Uehara, Masayuki; Honda, Takayuki; Saito, Yasunori

2016-02-04

We report a novel automated device for nucleic acid extraction, which consists of a mechanical control system and a disposable cassette. The cassette is composed of a bottle, a capillary tube, and a chamber. After sample injection in the bottle, the sample is lysed, and nucleic acids are adsorbed on the surface of magnetic silica beads. These magnetic beads are transported and are vibrated through the washing reagents in the capillary tube under the control of the mechanical control system, and thus, the nucleic acid is purified without centrifugation. The purified nucleic acid is automatically extracted in 3 min for the polymerase chain reaction (PCR). The nucleic acid extraction is dependent on the transport speed and the vibration frequency of the magnetic beads, and optimizing these two parameters provided better PCR efficiency than the conventional manual procedure. There was no difference between the detection limits of our novel device and that of the conventional manual procedure. We have already developed the droplet-PCR machine, which can amplify and detect specific nucleic acids rapidly and automatically. Connecting the droplet-PCR machine to our novel automated extraction device enables PCR analysis within 15 min, and this system can be made available as a point-of-care testing in clinics as well as general hospitals. Copyright © 2015 Elsevier B.V. All rights reserved.

A Magnetic Nanoparticle Based Nucleic Acid Isolation and Purification Instrument for DNA Extraction of Escherichia Coli O157: H7.

PubMed

Chen, Yahui; Lin, Jianhan; Jiang, Qin; Chen, Qi; Zhang, Shengjun; Li, Li

2016-03-01

The objective of this study was to evaluate the performance of a nucleic acid isolation and purification instrument using Escherichia coli O157:H7 as the model. The instrument was developed with magnetic nanoparticles for efficiently capturing nucleic acids and an intelligent mechanical unit for automatically performing the whole nucleic acid extraction process. A commercial DNA extraction kit from Huier Nano Company was used as reference. Nucleic acids in 1 ml of E. coli O157: H7 at a concentration of 5 x 10(8) CFU/mL were extracted by using this instrument and the kit in parallel and then detected by an ultraviolet spectrophotometer to obtain A260 values and A260/A280 values for the determination of the extracted DNA's quantity and purity, respectively. The A260 values for the instrument and the kit were 0.78 and 0.61, respectively, and the A260/A280 values were 1.98 and 1.93. The coefficient of variations of these parallel tests ranged from 10.5% to 16.7%. The results indicated that this nucleic acid isolation and purification instrument could extract a comparable level of nucleic acid within 50 min compared to the commercial DNA extraction kit.

Phenylboronic acid modified solid-phase extraction column: Preparation, characterization, and application to the analysis of amino acids in sepia capsule by removing the maltose.

PubMed

Guo, Mengzhe; Yin, Dengyang; Han, Jie; Zhang, Liyan; Li, Xiao; He, Dandan; Du, Yan; Tang, Daoquan

2016-09-01

Maltose, a common auxiliary material of pharmaceutical preparation, may disturb the analysis of total amino acids in sepia capsule by aldolization. Therefore, it is necessary to remove the maltose through a convenient method. In this work, a phenylboronic acid modified solid-phase extraction column has been synthesized and used to remove the maltose. The materials were synthesized by one step "thiol-ene" reaction and the parameters of the column such as absorption capacity, recovery, and absorption specificity have been investigated. The results showed the column (0.5 cm of length × 0.5 cm of inner diameter) can absorb 4.6 mg maltose with a linear absorption and absorption specificity. Then this technique was applied in the quantification of amino acids in sepia capsule. After the optimization of the method, four kinds of amino acids, which were the most abundant, were quantified by high-performance liquid chromatography with diode array detection. The amounts of the four kinds of amino acids are 1.5∼2 times more than that without the treatment of solid-phase extraction column, which almost overcomes the influence of the maltose. All the results indicate that the phenylboronic acid modified solid-phase extraction column can successfully help to accurately quantify the total amino acids in sepia capsule. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evidence that inhibitory factor extracted from bovine retractor penis is nitrite, whose acid-activated derivative is stabilized nitric oxide.

PubMed Central

Martin, W.; Smith, J. A.; Lewis, M. J.; Henderson, A. H.

1988-01-01

1. Unactivated extracts of bovine retractor penis (BRP) contains 3-7 microM nitrite. Acid-activation of these extracts at pH 2 for 10 min followed by neutralization generates the active form of inhibitory factor (IF; assayed by its vasodilator action on rabbit aorta), and is associated with partial loss of nitrite. 2. Increasing the time of acid-activation at pH 2 from 10 to 60 min with intermittent vortex mixing generates greater vasodilator activity and increases nitrite loss. 3. When acid-activated and neutralized extracts are incubated at 37 degrees C or 30 min or boiled for 5 min, vasodilator activity is lost and nitrite content increased. Reactivation of these samples at pH 2 for 10 min followed by neutralization leads to partial recoveries of vasodilator activity with loss in nitrite content. 4. Addition of sodium nitrite to BRP extracts increases acid-activatable vasodilator activity pro rata. 5. Acid-activation of aqueous sodium nitrite solutions results in less loss of nitrite and generation of less vasodilator activity than BRP extracts. Vasodilatation is only transient and is rapidly abolished on neutralization, whereas responses to acid-activated BRP extracts are more prolonged and activity is stable on ice. 6. Bovine aortic endothelial cells yield vasodilator activity that is indistinguishable from that isolated from BRP. It is activated by acid, stable on ice, abolished by boiling or by haemoglobin, and appears to be due to the generation of nitric oxide (NO) from nitrite.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:2897219

Chlorogenic Acid-Enriched Extract of Ilex kudingcha C.J. Tseng Inhibits Angiogenesis in Zebrafish.

PubMed

Zhong, Tao; Piao, Linghua; Kim, Hyun Jung; Liu, Xiande; Jiang, Shengnan; Liu, Guomin

2017-12-01

Kudingcha is a particularly bitter tasting tea that has been widely used in China to eliminate fever and itching eyes, and to clear blood toxins. Kudingcha is considered of value for its potential anticancer effects that are attributed to the presence of characteristic bioactive ingredients. The chlorogenic acid (CGA) derivatives 3-0-caffeoylquinic acid, 5-0-caffeoylquinic acid, 3,5-0-dicaffeoylquinic acid, and 4,5-0-dicaffeoylquinic acid were separated from Ilex kudingcha C.J. Tseng extract by high-performance liquid chromatography (HPLC)-photodiode array detector (PDA) and HPLC-nuclear magnetic resonance (NMR). In Tg(flk1:EGFP) zebrafish embryos at 52 hours postfertilization (hpf), angiogenesis was significantly inhibited by kudingcha extract (KDCE) at concentrations of 400 and 500 μg/mL and CGA also showed significant inhibition in embryos treated with 80, 100, and 130 μg/mL. Endothelial cell apoptosis showed a dose-dependent increase in response to KDCE and CGA. CGA derivatives from KDCE could have potential as anticancer agents against tumor angiogenesis.

Optimization of pulsed ultrasound-assisted technique for extraction of phenolics from pomegranate peel of Malas variety: Punicalagin and hydroxybenzoic acids.

PubMed

Kazemi, Milad; Karim, Roselina; Mirhosseini, Hamed; Abdul Hamid, Azizah

2016-09-01

Pomegranate peel is a rich source of phenolic compounds (such as punicalagin and hydroxybenzoic acids). However, the content of such bioactive compounds in the peel extract can be affected by extraction type and condition. It was hypothesized that the optimization of a pulsed ultrasound-assisted extraction (PUAE) technique could result in the pomegranate peel extract with higher yield and antioxidant activity. The main goal was to optimize PUAE condition resulting in the highest yield and antioxidant activity as well as the highest contents of punicalagin and hydroxybenzoic acids. The operation at the intensity level of 105W/cm(2) and duty cycle of 50% for a short time (10min) had a high efficiency for extraction of phenolics from pomegranate peel. The application of such short extraction can save the energy and cost of the production. Punicalagin and ellagic acid were the most predominant phenolic compounds quantified in the pomegranate peel extract (PPE) from Malas variety. PPE contained a minor content of gallic acid. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Determination of three phenoxyalkanoic acid herbicides in blood using gas chromatography coupled with solid-phase extraction and derivatization].

PubMed

Xin, Guobin; Tan, Jiayi; Yao, Lijuan; Zhu, Yu; Jiang, Zhaolin; Song, Hui

2008-01-01

A method for the determination of three phenoxyalkanoic acid herbicides, 2,4-dichlorophenoxyacetic acid (2,4-D), 2-(2,4-dichlorophenoxy)-propanoic acid (2,4-DP), and 4-chloro-2-methylphenoxy-acetic acid (MCPA), in blood was developed. The blood sample was diluted with 0.1 mol/L hydrochloric acid, and extracted by solid-phase extraction using porous resin GDX401 as adsorbent and ethyl ether as eluent. The extract was esterified with dichloropropanol in the presence of sulfuric acid as catalyst. The derivatives were analysed by gas chromatography with electron-capture detection. The detection limits of 2,4-D, 2,4-DP and MCPA were 20, 8 and 40 ng/mL, respectively. In quantitative analysis, 2,4-dichlorophenylacetic acid was used as an internal standard. The linear relationships and recoveries were satisfactory. The derivatization of the three herbicides with methanol, ethanol, n-propanol, n-butanol, and trifluoroethanol were also studied, and the analytical methods of these derivatization were compared with that of dichloropropanol as esterifying agent. The method is sensitive enough for the examination of the poison samples in actual.

Validation of internal controls for extraction and amplification of nucleic acids from enteric viruses in water samples.

PubMed

Hata, Akihiko; Katayama, Hiroyuki; Kitajima, Masaaki; Visvanathan, Chettiyappan; Nol, Chea; Furumai, Hiroaki

2011-07-01

Inhibitors that reduce viral nucleic acid extraction efficiency and interfere with cDNA synthesis and/or polymerase activity affect the molecular detection of viruses in aquatic environments. To overcome these significant problems, we developed a methodology for assessing nucleic acid yields and DNA amplification efficiencies for environmental water samples. This involved adding particles of adenovirus type 5 and murine norovirus and newly developed primer-sharing controls, which are amplified with the same primer pairs and result in the same amplicon sizes as the targets, to these samples. We found that nucleic acid loss during the extraction process, rather than reverse transcription-PCR (RT-PCR) inhibition, more significantly attributed to underestimation of the presence of viral genomes in the environmental water samples tested in this study. Our success rate for satisfactorily amplifying viral RNAs and DNAs by RT-PCR was higher than that for obtaining adequate nucleic acid preparations. We found that inhibitory properties were greatest when we used larger sample volumes. A magnetic silica bead-based RNA extraction method effectively removed inhibitors that interfere with viral nucleic acid extraction and RT-PCR. To our knowledge, this is the first study to assess the inhibitory properties of environmental water samples by using both control virus particles and primer-sharing controls.

Comparison of the activities of extracts of Escherichia coli and Salmonella typhimurium in amino acid incorporation.

PubMed

Bassel, B A; Curry, M E

1973-11-01

We have compared the amino acid incorporating activities of extracts of Escherichia coli and Salmonella typhimurium in in vitro protein-synthesizing systems directed by bacterial messenger ribonucleic acid (mRNA) of both species and by the genomes of coliphages Qbeta and f2. E. coli and S. typhimurium extracts translate both homologous and heterologous bacterial mRNAs at comparable rates. S. typhimurium extracts translate phage RNAs only 10 to 15% as fast as E. coli extracts do. The presence of glucose in the growth medium increases the activity of S. typhimurium extracts three- to fourfold in the phage RNA-directed systems. Glucose has a much more limited effect on the activities of E. coli extracts. We show that similar amounts of phage RNA-ribosome complexes are formed in both the E. coli and the S. typhimurium systems, indicating that the different activities observed may be attributed to different rates of peptide elongation or to the formation of complexes at different sites on the RNA strand.

Effects of molten-salt/ionic-liquid mixture on extraction of docosahexaenoic acid (DHA)-rich lipids from Aurantiochytrium sp. KRS101.

PubMed

Choi, Sun-A; Jung, Joo-Young; Kim, Kyochan; Kwon, Jong-Hee; Lee, Jin-Suk; Kim, Seung Wook; Park, Ji-Yeon; Yang, Ji-Won

2014-11-01

In this study, lipid extraction from Aurantiochytrium sp. was performed using a molten-salt/ionic-liquid mixture. The total fatty acid content of Aurantiochytrium sp. was 478.8 mg/g cell, from which 145 mg/g cell (30.3% of total fatty acids) of docosahexaenoic acid (DHA) was obtained. FeCl3·6H2O showed a high lipid extraction yield (207.9 mg/g cell), when compared with that of [Emim]OAc, which was only 118.1 mg/g cell; notably however, when FeCl3·6H2O was mixed with [Emim]OAc (5:1, w/w), the yield was increased to 478.6 mg/g cell. When lipid was extracted by the FeCl3·6H2O/[Emim]OAc mixture at a 5:1 (w/w) blending ratio under 90 °C, 30 min reaction conditions, the fatty acid content of the extracted lipid was a high purity 997.7 mg/g lipid, with most of the DHA having been extracted (30.2% of total fatty acids). Overall, lipid extraction from Aurantiochytrium sp. was enhanced by the synergistic effects of the molten-salt/ionic-liquid mixture with different ions.

Anticandidal activity of cell extracts from 13 probiotic Lactobacillus strains and characterisation of lactic acid and a novel fatty acid derivative from one strain.

PubMed

Nyanzi, Richard; Awouafack, Maurice D; Steenkamp, Paul; Jooste, Piet J; Eloff, Jacobus N

2014-12-01

This study investigated the anti-Candida activity of methanol extracts from freeze-dried probiotic cells and the isolation of some constituents in the extracts. The MIC values of the probiotic methanol cell extracts against Candida albicans ranged between 1.25 and 5mg/ml after 48 h of incubation. However, Lactococcus latics subsp. lactis strain X and Lactobacillus casei strain B extracts had an MIC of 10mg/ml after 48 h of incubation. The extracts had fungistatic rather than fungicidal activity. These extracts had a much higher antifungal activity than antifungal compounds isolated from the growth medium by many other authors. This indicates that probiotics may also release antifungal compounds in their cells that could contribute to a therapeutic effect. Lactic acid (1) and 6-O-(α-D-glucopyranosyl)-1,6-di-O-pentadecanoyl-α-D-glucopyranose a novel fatty acid derivative (2) were isolated from methanol probiotic extracts and the structure of these compounds were elucidated using NMR (1 and 2D) and mass spectrometry (MS). Copyright © 2014 Elsevier Ltd. All rights reserved.

Forensic analysis of anthraquinone, azo, and metal complex acid dyes from nylon fibers by micro-extraction and capillary electrophoresis.

PubMed

Stefan, Amy R; Dockery, Christopher R; Nieuwland, Alexander A; Roberson, Samantha N; Baguley, Brittany M; Hendrix, James E; Morgan, Stephen L

2009-08-01

The extraction and separation of dyes present on textile fibers offers the possibility of enhanced discrimination between forensic trace fiber evidence. An automated liquid sample handling workstation was programmed to deliver varying solvent combinations to acid-dyed nylon samples, and the resulting extracts were analyzed by an ultraviolet/visible microplate reader to evaluate extraction efficiencies at different experimental conditions. Combinatorial experiments using three-component mixture designs varied three solvents (water, pyridine, and aqueous ammonia) and were employed at different extraction temperatures for various extraction durations. The extraction efficiency as a function of the three solvents (pyridine/ammonia/water) was modeled and used to define optimum conditions for the extraction of three subclasses of acid dyes (anthraquinone, azo, and metal complex) from nylon fibers. The capillary electrophoresis analysis of acid dye extracts is demonstrated using an electrolyte solution of 15 mM ammonium acetate in acetonitrile/water (40:60, v/v) at pH 9.3. Excellent separations and discriminating diode array spectra are obtained even for dyes of similar color.

Development of a rapid LC-DAD/FLD method for the simultaneous determination of auxins and abscisic acid in plant extracts.

PubMed

Bosco, Renato; Caser, Matteo; Vanara, Francesca; Scariot, Valentina

2013-11-20

Plant hormones play a crucial role in controlling plant growth and development. These groups of naturally occurring substances trigger physiological processes at very low concentrations, which mandate sensitive techniques for their quantitation. This paper describes a method to quantify endogenous (±)-2-cis-4-trans-abscisic acid, indole-3-acetic acid, indole-3-propionic acid, and indole-3-butyric acid. The method combines high-performance liquid chromatography (HPLC) with diode array and fluorescence detection in a single run. Hybrid tea rose 'Monferrato' matrices (leaves, petals, roots, seeds, androecium, gynoecium, and pollen) were used as references. Rose samples were separated and suspended in extracting methanol, after which (±)-2-cis-4-trans-abscisic acid and auxins were extracted by solvent extraction. Sample solutions were added first to cation solid phase extraction (SPE) cartridges and the eluates to anion SPE cartridges. The acidic hormones were bound to the last column and eluted with 5% phosphoric acid in methanol. Experimental results showed that this approach can be successfully applied to real samples and that sample preparation and total time for routine analysis can be greatly reduced.

Supercritical fluid extraction of 13-cis retinoic acid and its photoisomers from selected pharmaceutical dosage forms.

PubMed

Simmons, B R; Chukwumerije, O; Stewart, J T

1997-11-01

13-Cis retinoic acid (Accutane) was extracted from a cream, gel, capsule and beadlet dosage from using supercritical carbon dioxide modified with 5% methanol as the mobile phase. The pump pressure and the extraction chamber and restrictor temperature were experimentally optimized at 325 atm and 45 degrees C, respectively. A 2.5-min static and 5-min dynamic extraction time were used. The supercritical fluid extraction (SFE) eluent was trapped in methanol, injected into the high-performance liquid chromatographic (HPLC) system, and quantitated by ultraviolet detection at 360 nm. Application of the SFE method to spiked placebo dosage forms gave 13-cis retinoic acid recoveries of 98.8, 98.9, 98.8 and 100% for the cream, gel, capsule and beadlet, respectively, with R.S.D.s in the range 0.6-0.9% (n = 4). Inter-day percent error and precision of the extraction were 1.1-2.0 and 0.2-2.4% (n = 3), respectively, and intra-day percent error and precision were 1.0-3.0 and 0.3-2.1% (n = 8), respectively. Percent error and precision data for spiked celite samples in the 0.05-1.0 microgram ml-1 range were 0.59-4.75 and 1.8-2.1% (n = 3), respectively. The extraction method was applied to commercial 13-cis retinoic acid dosage forms and the results compared to unextracted samples. Linear regression analysis of concentration versus peak height gave a correlation coefficient of 0.9991 with a slope of 7.468 and a y-intercept of 0.1923. The percent error and precision data were 1.3-5.3 and 0.2-1.5% (n = 4), respectively. The photoisomers of 13-cis retinoic acid were also extracted with the method and recoveries of 90.4-92.4% with R.S.D.s of 1.5-3.4% were obtained (n = 4).

Acid extraction by supported liquid membranes containing basic carriers

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

Danesi, P.R.; Cianetti, C.; Horwitz, E.P.

1983-01-01

The extraction of HNO/sub 3/ (nitric acid) from aqueous solutions by permeation through a number of supported liquid membranes containing basic carriers dissolved in diethylbenzene has been studied. The results have shown that the best permeations are obtained with long chain aliphatic amines (TLA, Primene JM-T) followed by TOPO (trioctylphosphine oxide) and then by other monofunctional and bifunctional organophosphorous basic carriers. The influence of an aliphatic diluent on the permeability of HNO/sub 3/ through a supported liquid membrane containing TLA as carrier was also investigated. In this case the permeability to HNO/sub 3/ decreases as a result of the lowermore » diffusion coefficient of the acid-carrier complex in the more vicous aliphatic solvent. 4 figures.« less

Effect of artichoke extract (Cynara scolymus L.) on palmitic-1-14C acid oxidation in rats.

PubMed

Juzyszyn, Zygmunt; Czerny, Boguslaw; Pawlik, Andrzej; Drozdzik, Marek

2008-05-01

Studies on the effect of the artichoke extract (AE) on oxidation of palmitic-1-14C acid administered intravenously to rats at a dose 25 and 50 mg/kg bw demonstrated marked enhancement of both 14CO2 expiration rate and 14CO2 recovery in the expired air. The extract suppressed accumulation of palmitic-1-14C acid in serum lipids and epididymal fat pad tissue as well. The effects of the extract on 14CO2 expiration rate, 14CO2 recovery, as well as accumulation of palmitic-1-14C acid were dose dependent. Total14CO2 recovery in expired air during 60 min was elevated by 17.3% (p < 0.05) and 52.1% (p < 0.001) in rats administered the extract at a dose of 25 and 50 mg/kg, respectively. The rats supplemented with the AE at a dose of 25 and 50 mg/kg bw were characterized by 10.0% (not significant) and 19% (p < 0.05) decrease in( 14)C radioactivity of serum lipids as well as reduction of epididymal fat tissue 14C radioactivity by 8.7 and 17.5% (p < 0.05), respectively, in comparison with the control rats. Thus, the results demonstrate that the AE possess stimulatory properties with respect to oxidation of palmitic acid administered to rats, and provide new information on the mechanism of antilipemic activity of the extract associated with activation of lipid oxidation in the organism.

Rosmarinic acid content in antidiabetic aqueous extract of Ocimum canum Sims grown in Ghana

USDA-ARS?s Scientific Manuscript database

Rosmarinic acid (RA) is an important polyphenol that is found in a variety of herbs including Ocimum canum sims (locally called eme or akokobesa in Ghana). Aqueous extracts from the leaves of O.canum are used as an antidiabetic herbal medicine in Ghana. Interestingly, rosmarinic acid content and p...

Calcium extraction from brine water and seawater using oxalic acid

NASA Astrophysics Data System (ADS)

Natasha, Nadia Chrisayu; Lalasari, Latifa Hanum

2017-01-01

Calcium can be extracted not only from rocks but also from natural liquor such as seawater and brine water. In order to extract the calcium from seawater and brine water, oxalic acid was used in this research. Effect of variations of the volume of the oxalic acid at a constant concentration in seawater and brine water to produce calcium was investigated. The concentration of oxalic acid was 100 g/l and the variations of its volume were 2 ml, 4 ml, 6 ml, 8 ml, 10 ml, 20 ml, 30 ml, 40 ml, and 50 ml. The used seawater and brine water were firstly evaporated from 100 ml into 50 ml and then the oxalic acid was added into them with mixing to produce the calcium precipitates. The precipitates were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM) and the filtrates were analyzed by inductively coupled plasma-optical emission spectrometry (ICP-OES). The SEM analysis showed that the precipitates from brine water were consisted of only calcium compound while from seawater sodium one was also found along with calcium compound. The XRD analysis showed that the calcium was present in the form of calcium oxalate for both seawater and brine water. The ICP-OES analysis of the filtrate from seawater precipitation showed that the its calcium content was decreased from 826.20 ppm to 0.04 ppm while from brine water, it decreased from 170.06 ppm to 1.96 ppm. These results showed that both seawater and brine water have the potential to be a raw material for calcium production.

The acid tolerance response and pH adaptation of Enterococcus faecalis in extract of lime Citrus aurantiifolia from Aceh Indonesia.

PubMed

Mubarak, Zaki; Soraya, Cut

2018-01-01

Background:  The objective of the present study was to evaluate the acid tolerance response and pH adaptation when Enterococcus faecalis interacted with extract of lime ( Citrus aurant iifolia ). Methods : We used E. faecalis ATCC 29212 and lime extract from Aceh, Indonesia. The microbe was analyzed for its pH adaptation, acid tolerance response, and adhesion assay using a light microscope with a magnification of x1000. Further, statistical tests were performed to analyze both correlation and significance of the acid tolerance and pH adaptation as well as the interaction activity. Results : E. faecalis was able to adapt to a very acidic environment (pH 2.9), which was characterized by an increase in its pH (reaching 4.2) at all concentrations of the lime extract (p < 0.05). E. faecalis was also able to provide acid tolerance response to lime extract based on spectrophotometric data (595 nm) (p < 0.05). Also, the interaction activity of E. faecalis in different concentrations of lime extract was relatively stable within 6 up to 12 hours (p < 0.05), but it became unstable within 24-72 hours (p > 0.05) based on the mass profiles of its interaction activity. Conclusions : E. faecalis can adapt to acidic environments (pH 2.9-4.2); it is also able to tolerate acid generated by Citrus auranti ifolia extract, revealing a stable interaction in the first 6-12 hours.

Ocimum grastissimum extract inhibits stimulated acid secretion by carbachol and induces gastric mucus secretion.

PubMed

Onasanwo, S A; Omolaso, B O; Ukoha, N

2012-12-01

In this study, the effects of ethanol extract of Ocimum gratissimum (EEOG) on both basal and stimulated gastric acid secretion and gastric mucus secretion were investigated in Albino rats treated with the extract. Four groups of animals were used. Sub-group 1A serves as control. Animals in Group 2A, 3B and 4B were pretreated with 200 mg/kg of (E3EOG) for 1, 7 and 14 days respectively. Basal gastric effluents were collected from all the groups of animals at intervals of 10 mins for 60 mins. Thereafter, Subgroups 1A, 2A, 3A and 4A were administered with 50 micro/kg b.w. of carbachol (i.p.) intraperitonialy and effluents collected. Animals in Sub-group B were used for gastric mucus study. Carbachol stimulates gastric acid secretion in animals pretreated with the extract for 1, 7 and 14 days. 50-400 mg/kg b.w. doses of the extract significantly increase gastric mucus secretion. These results indicate the mechanism of anti-ulcer activity of the extract may be due to stimulation of gastric mucus secretion amongst pathways.

Comparison of commercial systems for extraction of nucleic acids from DNA/RNA respiratory pathogens.

PubMed

Yang, Genyan; Erdman, Dean E; Kodani, Maja; Kools, John; Bowen, Michael D; Fields, Barry S

2011-01-01

This study compared six automated nucleic acid extraction systems and one manual kit for their ability to recover nucleic acids from human nasal wash specimens spiked with five respiratory pathogens, representing Gram-positive bacteria (Streptococcus pyogenes), Gram-negative bacteria (Legionella pneumophila), DNA viruses (adenovirus), segmented RNA viruses (human influenza virus A), and non-segmented RNA viruses (respiratory syncytial virus). The robots and kit evaluated represent major commercially available methods that are capable of simultaneous extraction of DNA and RNA from respiratory specimens, and included platforms based on magnetic-bead technology (KingFisher mL, Biorobot EZ1, easyMAG, KingFisher Flex, and MagNA Pure Compact) or glass fiber filter technology (Biorobot MDX and the manual kit Allprep). All methods yielded extracts free of cross-contamination and RT-PCR inhibition. All automated systems recovered L. pneumophila and adenovirus DNA equivalently. However, the MagNA Pure protocol demonstrated more than 4-fold higher DNA recovery from the S. pyogenes than other methods. The KingFisher mL and easyMAG protocols provided 1- to 3-log wider linearity and extracted 3- to 4-fold more RNA from the human influenza virus and respiratory syncytial virus. These findings suggest that systems differed in nucleic acid recovery, reproducibility, and linearity in a pathogen specific manner. Published by Elsevier B.V.

[AAPH scavenging activities of 22 flavonoids and phenolic acids and 9 extracts of Chinese materia medica].

PubMed

Dai, Huiqing; Chen, Chengyu; Yang, Bin

2010-09-01

To investigate the AAPH scavenging activities of 22 flavonoids and phenolic acids and 9 extracts of Chinese materia medica. The antioxidant activities of the samples were evaluated by an oxygen radical absorbance capacity method (ORAC), at the same time, the total contents of flavonoids and phenolic the 9 herb extracts were analyzed by Folin-Ciocalteu method, and the active components were qualitatively and quantitatively analyzed by an HPLC method. It was found that the tea extract showed the strongest AAPH activity with the ORAC value of 4786.40 micromol x g(-1) whereas safflower demonstrated the weakest activity with the ORAC value of 784.04 micromol x g(-1). As for compounds, quercetin had the strongest AAPH activity with the ORAC value of 12.90 while ( - )-EGC had the weakest activity with the ORAC value of 2.47. A quantitative relationship was obtained to describe the AAPH scavenging activity of the herb extracts: Y = 1844.8 lnX-3577.5, r = 0.8675, where Y stands for the ORAC vaule, and X stands for the concentration of total phenolic acids. Flavonoids and phenolic acids are the AAPH scavenging active ingredients in the Chinese herb extracts. It's a good way to study the antioxidant activity of Chinese herb extract and its chemical composition by combing ORAC method and HPLC method.

Linking Laboratory Experiences to the Real World: The Extraction of Octylphenoxyacetic Acid from Water

ERIC Educational Resources Information Center

Loyo-Rosales, Jorge E.; Torrents, Alba; Rosales-Rivera, Georgina C.; Rice, Clifford C.

2006-01-01

Several chemical concepts to the extraction of a water pollutant OPC (octylphenoxyacetic acid) is presented. As an introduction to the laboratory experiment, a discussion on endocrine disrupters is conducted to familiarize the student with the background of the experiment and to explain the need for the extraction and quantitation of the OPC which…

The enrichment of chlorogenic acid from Eucommia ulmoides leaves extract by mesoporous carbons.

PubMed

Qin, Guotong; Ma, Jing; Wei, Wei; Li, Jaja; Yue, Fangqing

2018-06-15

Herein, we report an efficient separation and enrichment method for chlorogenic acid from crude extracts of Eucommia ulmoides leaves using carbon adsorbents. The effects of the pore structure of the carbon adsorbents on the adsorption capacity were studied. Of the four adsorbents investigated, mesoporous carbon (MC3) showed the highest adsorption capacity (294 mg/g of carbon) for chlorogenic acid due to its high mesopore volume. The static adsorption of CGA on carbon can be accurately described using the Freundlich equation. The kinetics of adsorption follow a pseudo-second-order process. External mass transfer was the controlling step of the adsorption process. Dynamic adsorption on MC3 demonstrated that chlorogenic acid began to break through after 28 bed volumes of extract was loaded. This mesoporous carbon-treatment procedure is safe, economic and has the potential to be scaled up for commercial application. Copyright © 2018 Elsevier B.V. All rights reserved.

Cleaner production of citric acid by recycling its extraction wastewater treated with anaerobic digestion and electrodialysis in an integrated citric acid-methane production process.

PubMed

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

2015-01-01

To solve the pollution problem of extraction wastewater in citric acid production, an integrated citric acid-methane production process was proposed. Extraction wastewater was treated through anaerobic digestion and the anaerobic digestion effluent (ADE) was recycled for the next batch of citric acid fermentation, thus eliminating wastewater discharge and reducing water consumption. Excessive Na(+) contained in ADE could significantly inhibit citric acid fermentation in recycling and was removed by electrodialysis in this paper. Electrodialysis performance was improved after pretreatment of ADE with air stripping and activated carbon adsorption to remove precipitable metal ions and pigments. Moreover, the concentrate water was recycled and mixed with feed to improve the water recovery rate above 95% in electrodialysis treatment, while the dilute water was collected for citric acid fermentation. The removal rate of Na(+) in ADE was above 95% and the citric acid production was even higher than that with tap water. Copyright © 2015 Elsevier Ltd. All rights reserved.

Characterization and purification of a bacterial chlorogenic acid esterase detected during the extraction of chlorogenic acid from arbuscular mycorrhizal tomato roots.

PubMed

Negrel, Jonathan; Javelle, Francine; Morandi, Dominique; Lucchi, Géraldine

2016-12-01

A Gram-negative bacterium able to grow using chlorogenic acid (5-caffeoylquinic acid) as sole carbon source has been isolated from the roots of tomato plants inoculated with the arbuscular mycorrhizal fungus Rhizophagus irregularis. An intracellular esterase exhibiting very high affinity (K m  = 2 μM) for chlorogenic acid has been extracted and purified by FPLC from the chlorogenate-grown cultures of this bacterium. The molecular mass of the purified esterase determined by SDS-PAGE was 61 kDa and its isoelectric point determined by chromatofocusing was 7.75. The esterase hydrolysed chlorogenic acid analogues (caffeoylshikimate, and the 4- and 3-caffeoylquinic acid isomers), feruloyl esterases substrates (methyl caffeate and methyl ferulate), and even caffeoyl-CoA in vitro but all of them were less active than chlorogenic acid, demonstrating that the esterase is a genuine chlorogenic acid esterase. It was also induced when the bacterial strain was cultured in the presence of hydroxycinnamic acids (caffeic, p-coumaric or ferulic acid) as sole carbon source, but not in the presence of simple phenolics such as catechol or protocatechuic acid, nor in the presence of organic acids such as succinic or quinic acids. The purified esterase was remarkably stable in the presence of methanol, rapid formation of methyl caffeate occurring when its activity was measured in aqueous solutions containing 10-60% methanol. Our results therefore show that this bacterial chlorogenase can catalyse the transesterification reaction previously detected during the methanolic extraction of chlorogenic acid from arbuscular mycorrhizal tomato roots. Data are presented suggesting that colonisation by Rhizophagus irregularis could increase chlorogenic acid exudation from tomato roots, especially in nutrient-deprived plants, and thus favour the growth of chlorogenate-metabolizing bacteria on the root surface or in the mycorhizosphere. Copyright © 2016 Elsevier Masson SAS. All rights

Design of experiments for amino acid extraction from tobacco leaves and their subsequent determination by capillary zone electrophoresis.

PubMed

Hodek, Ondřej; Křížek, Tomáš; Coufal, Pavel; Ryšlavá, Helena

2017-03-01

In this study, we optimized a method for the determination of free amino acids in Nicotiana tabacum leaves. Capillary electrophoresis with contactless conductivity detector was used for the separation of 20 proteinogenic amino acids in acidic background electrolyte. Subsequently, the conditions of extraction with HCl were optimized for the highest extraction yield of the amino acids because sample treatment of plant materials brings some specific challenges. Central composite face-centered design with fractional factorial design was used in order to evaluate the significance of selected factors (HCl volume, HCl concentration, sonication, shaking) on the extraction process. In addition, the composite design helped us to find the optimal values for each factor using the response surface method. The limits of detection and limits of quantification for the 20 proteinogenic amino acids were found to be in the order of 10 -5 and 10 -4  mol l -1 , respectively. Addition of acetonitrile to the sample was tested as a method commonly used to decrease limits of detection. Ambiguous results of this experiment pointed out some features of plant extract samples, which often required specific approaches. Suitability of the method for metabolomic studies was tested by analysis of a real sample, in which all amino acids, except for L-methionine and L-cysteine, were successfully detected. The optimized extraction process together with the capillary electrophoresis method can be used for the determination of proteinogenic amino acids in plant materials. The resulting inexpensive, simple, and robust method is well suited for various metabolomic studies in plants. As such, the method represents a valuable tool for research and practical application in the fields of biology, biochemistry, and agriculture.

Third phase formation in the extraction of phosphotungstic acid by TBP in n-octane.

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

Antonio, M. R.; Chiarizia, R.; Jaffrennou, F.

2010-08-30

The solvent extraction of 12-phosphotungstic acid, also known as 12-tungstophosphoric acid-H{sub 3}PW{sub 12}O{sub 40}, the so-called Keggin heteropolyacid - by 0.73 M (20%v/v) tri-n-butyl phosphate (TBP) in n-octane under conditions comparable to those used previously for the extraction of conventional inorganic mineral acids is described. A simplified phase diagram for the pentanary system comprised of H{sub 3}PW{sub 12}O{sub 40}, HNO{sub 3}, H{sub 2}O, TBP, and n-octane reveals an extremely low initial concentration of H{sub 3}PW{sub 12}O{sub 40} (1.1 mM) at the LOC (limiting organic concentration) condition, far lower than the most effective third-phase-forming inorganic acid, namely HClO{sub 4}. The resultsmore » from small-angle neutron scattering (SANS) indicate that the interparticle attraction energy - U(r) calculated through application of the Baxter sticky sphere model to the SANS data at the LOC condition - does not approach the -2 k{sub B} T value associated with phase splitting in previous studies of TBP third-phase formation. The third-phase formation model based on attractive interactions between polar cores of reverse micelles, successfully developed for TBP and other extraction systems does not apply to the extraction of H{sub 3}PW{sub 12}O{sub 40}. Rather, the separation of a third-phase from the TBP organic phase stems from the limited solubility of the heavy and highly polar H{sub 3}PW{sub 12}O{sub 40}-TBP species in the alkane diluent.« less

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

PubMed

Cho, GyeYoon; Han, KyuChul; Yoon, JinYoung

2015-03-01

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

Method for extracting lanthanides and actinides from acid solutions by modification of purex solvent

DOEpatents

Horwitz, E. Philip; Kalina, Dale G.

1986-01-01

A process for the recovery of actinide and lanthanide values from aqueous solutions with an extraction solution containing an organic extractant having the formula: ##STR1## where .phi. is phenyl, R.sup.1 is a straight or branched alkyl or alkoxyalkyl containing from 6 to 12 carbon atoms and R.sup.2 is an alkyl containing from 3 to 6 carbon atoms and phase modifiers in a water-immiscible hydrocarbon diluent. The addition of the extractant to the Purex process extractant, tri-n-butylphosphate in normal paraffin hydrocarbon diluent, will permit the extraction of multivalent lanthanide and actinide values from 0.1 to 12.0 molar acid solutions.

Degradation study of carnosic acid, carnosol, rosmarinic acid, and rosemary extract (Rosmarinus officinalis L.) assessed using HPLC.

PubMed

Zhang, Ying; Smuts, Jonathan P; Dodbiba, Edra; Rangarajan, Rekha; Lang, John C; Armstrong, Daniel W

2012-09-12

Rosemary, whose major caffeoyl-derived and diterpenoid ingredients are rosmarinic acid, carnosol, and carnosic acid, is an important source of natural antioxidants and is being recognized increasingly as a useful preservative, protectant, and even as a potential medicinal agent. Understanding the stability of these components and their mode of interaction in mixtures is important if they are to be utilized to greatest effect. A study of the degradation of rosmarinic acid, carnosol, carnosic acid, and a mixture of the three was conducted in ethanolic solutions at different temperatures and light exposure. As expected, degradation increased with temperature. Some unique degradation products were formed with exposure to light. Several degradation products were reported for the first time. The degradation products were identified by HPLC/MS/MS, UV, and NMR. The degradation of rosemary extract in fish oil also was investigated, and much slower rates of degradation were observed for carnosic acid. In the mixture of the three antioxidants, carnosic acid serves to maintain levels of carnosol, though it does so at least in part at the cost of its own degradation.

Anticarcinogenic efficacy of phytic acid extracted from rice bran on azoxymethane-induced colon carcinogenesis in rats.

PubMed

Norazalina, S; Norhaizan, M E; Hairuszah, I; Norashareena, M S

2010-05-01

This study is carried out to determine the potential of phytic acid extracted from rice bran in the suppression of colon carcinogenesis induced by azoxymethane (AOM) in rats. Seventy-two male Sprague-Dawley rats were divided into 6 groups with 12 rats in each group. The intended rats for cancer treatment received two intraperitoneal injections of AOM in saline (15mg/kg bodyweight) over a 2-week period. The treatments of phytic acid were given in two concentrations: 0.2% (w/v) and 0.5% (w/v) during the post-initiation phase of carcinogenesis phase via drinking water. The colons of the animals were analyzed for detection and quantification of aberrant crypt foci (ACF) after 8 weeks of treatment. The finding showed treatment with 0.2% (w/v) extract phytic acid (EPA) gave the greatest reduction in the formation of ACF. In addition, phytic acid significantly suppressed the number of ACF in the distal, middle and proximal colon as compared to AOM alone (p<0.05). For the histological classification of ACF, treatment with 0.5% (w/v) commercial phytic acid (CPA) had the highest percentage (71%) of non-dysplastic ACF followed by treatment with 0.2% (w/v) EPA (61%). Administration of phytic acid also reduced the incidence and multiplicity of total tumors even though there were no significant differences between groups. In conclusion, this study found the potential value of phytic acid extracted from rice bran in reducing colon cancer risk in rats.

Development of a rapid method for the sequential extraction and subsequent quantification of fatty acids and sugars from avocado mesocarp tissue.

PubMed

Meyer, Marjolaine D; Terry, Leon A

2008-08-27

Methods devised for oil extraction from avocado (Persea americana Mill.) mesocarp (e.g., Soxhlet) are usually lengthy and require operation at high temperature. Moreover, methods for extracting sugars from avocado tissue (e.g., 80% ethanol, v/v) do not allow for lipids to be easily measured from the same sample. This study describes a new simple method that enabled sequential extraction and subsequent quantification of both fatty acids and sugars from the same avocado mesocarp tissue sample. Freeze-dried mesocarp samples of avocado cv. Hass fruit of different ripening stages were extracted by homogenization with hexane and the oil extracts quantified for fatty acid composition by GC. The resulting filter residues were readily usable for sugar extraction with methanol (62.5%, v/v). For comparison, oil was also extracted using the standard Soxhlet technique and the resulting thimble residue extracted for sugars as before. An additional experiment was carried out whereby filter residues were also extracted using ethanol. Average oil yield using the Soxhlet technique was significantly (P < 0.05) higher than that obtained by homogenization with hexane, although the difference remained very slight, and fatty acid profiles of the oil extracts following both methods were very similar. Oil recovery improved with increasing ripeness of the fruit with minor differences observed in the fatty acid composition during postharvest ripening. After lipid removal, methanolic extraction was superior in recovering sucrose and perseitol as compared to 80% ethanol (v/v), whereas mannoheptulose recovery was not affected by solvent used. The method presented has the benefits of shorter extraction time, lower extraction temperature, and reduced amount of solvent and can be used for sequential extraction of fatty acids and sugars from the same sample.

Separation of Molybdenum from Acidic High-Phosphorus Tungsten Solution by Solvent Extraction

NASA Astrophysics Data System (ADS)

Li, Yongli; Zhao, Zhongwei

2017-10-01

A solvent-extraction process for deep separation of molybdenum from an acidic high-phosphate tungsten solution was developed using tributyl phosphate (TBP) as the extractant and hydrogen peroxide (H2O2) as a complexing agent. The common aqueous complexes of tungsten and molybdenum (PMoxW12-xO40 3-, x = 0-12) are depolymerized to {PO4[Mo(O)2(O-O)]4}3- and {PO4[W(O)2(O-O)]4}3- by H2O2. The former can be preferentially extracted by TBP. The extractant concentration, phase contact time, H2O2 dosage, and H2SO4 concentration were optimized. By employing 80% by volume TBP, O:A = 1:1, 1.0 mol/L H2SO4, 1.0 mol/L H3PO4, a contact time of 2 min, and a molar ratio of H2O2/(W + Mo) equal to 1.5, 60.2% molybdenum was extracted in a single stage, while limiting tungsten co-extraction to 3.2%. An extraction isotherm indicated that the raffinate could be reduced to <0.1 g/L Mo in six stages of continuous counter-current extraction.

Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

PubMed

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2018-01-01

The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

Chlorella sp : Extraction of fatty acid by using avocado oil as solvent and its application as an anti-aging cream

NASA Astrophysics Data System (ADS)

Putri, T. W.; Raya, I.; Natsir, H.; Mayasari, E.

2018-03-01

The study aimed to analyze the fatty acid content of Chlorella sp crude extract by using avocado oil solvent and determining the effectiveness of fatty acids Chlorella sp as the anti-aging cream The extraction of fatty acids from Chlorella sp using avocado oil as a solvent with three ratios were 1:10, 1:20 and 1:25 w/V. The highest lipid content was obtained at 1:20 w/V (gram microalgae: mL avocado oil) yielding 52.73%. Crude extracted were analysis by GC-MS and FTIR, and skin condition was determined by skin analyzer. The effectiveness test of Chlorella sp cream was applicated on the face of the panelists aged 20-60 years. From 10 panelists, the applied of Chlorella sp cream was 90% increased on the facial skin yielded moisture and oil content, 70% repair the skin structure. The composition of fatty acids Chlorella sp extract was palmitic acid, linoleic, oleic and stearate. Fatty acids crude extract of Chlorella sp can improve the effectiveness of anti-aging cream. The cream from Chlorella sp was more effective than the cream without containing microalgae. This is very promising because it is alternative to organic solvents i.e. green chemistry.

Analysis of non-esterified fatty acids in human samples by solid-phase-extraction and gas chromatography/mass spectrometry.

PubMed

Kopf, Thomas; Schmitz, Gerd

2013-11-01

The determination of the fatty acid (FA) profile of lipid classes is essential for lipidomic analysis. We recently developed a GC/MS-method for the analysis of the FA profile of total FAs, i.e. the totality of bound and unbound FAs, in any given biological sample (TOFAs). Here, we present a method for the analysis of non-esterified fatty acids (NEFAs) in biological samples, i.e. the fraction that is present as extractable free fatty acids. Lipid extraction is performed according to Dole using 80/20 2-propanol/n-hexane (v/v), with 0.1% H2SO4. The fatty acid-species composition of this NEFA-fraction is determined as FAME after derivatization with our GC/MS-method on a BPX column (Shimadzu). Validation of the NEFA-method presented was performed in human plasma samples. The validated method has been used with human plasma, cells and tissues, as well as mammalian body fluids and tissue samples. The newly developed solid-phase-extraction (SPE)-GC-MS method allows the rapid separation of the NEFA-fraction from a neutral lipid extract of plasma samples. As a major advantage compared to G-FID-methods, GC-MS allows the use of stable isotope labeled fatty acid precursors to monitor fatty acid metabolism. Copyright © 2013 Elsevier B.V. All rights reserved.

Ultrasound-assisted extraction of gymnemic acids from Gymnema sylvestre leaves and its effect on insulin-producing RINm-5 F β cell lines.

PubMed

Sheoran, Sunita; Panda, Bibhu Prasad; Admane, Prasad S; Panda, Amulya Kumar; Wajid, Saima

2015-01-01

Gymnema sylvestre is an important anti-diabetic medicinal plant, hence it is necessary to study the effective extraction of its active medicinal components. To develop an efficient ultrasound-assisted extraction method for anti-diabetic gymnemic acids from Gymnema sylvestre leaves and measure their effect on insulin-producing RINm-5 F β cells. Box-Behnken's design and response surface methodology was applied to the ultrasound-assisted extraction of gymnemic acids from Gymnema sylvestre leaves. Analysis of gymnemic acids was carried out by high-performance thin-layer chromatography by converting total gymnemic acids into gymnemagenin by alkali hydrolysis. Effects of extracts on insulin production were tested on cultured, insulin-producing RINm-5 F β cell lines. The point prediction tool of the design expert software predicted 397.9 mg gymnemic acids per gram of the defatted G. sylvestre leaves using ultrasound-assisted extraction, with ethanol at 60 °C for 30 min. The predicted condition shows 93.34% validity under experimental conditions. The ultrasound-assisted extract caused up to about four times more insulin production from RINm-5 F β cells than extracts obtained from Soxhlet extraction. Response surface methodology was successfully used to improve the extraction of gymnemic acids from G. sylvestre leaves. The ultrasound-assisted extraction process may be a better alternative to prepare such herbal extracts because it saves time and may prevent excess degradation of the target analytes. Copyright © 2014 John Wiley & Sons, Ltd.

Evaluation of Method-Specific Extraction Variability for the Measurement of Fatty Acids in a Candidate Infant/Adult Nutritional Formula Reference Material.

PubMed

Place, Benjamin J

2017-05-01

To address community needs, the National Institute of Standards and Technology has developed a candidate Standard Reference Material (SRM) for infant/adult nutritional formula based on milk and whey protein concentrates with isolated soy protein called SRM 1869 Infant/Adult Nutritional Formula. One major component of this candidate SRM is the fatty acid content. In this study, multiple extraction techniques were evaluated to quantify the fatty acids in this new material. Extraction methods that were based on lipid extraction followed by transesterification resulted in lower mass fraction values for all fatty acids than the values measured by methods utilizing in situ transesterification followed by fatty acid methyl ester extraction (ISTE). An ISTE method, based on the identified optimal parameters, was used to determine the fatty acid content of the new infant/adult nutritional formula reference material.

Phytochemistry of cimicifugic acids and associated bases in Cimicifuga racemosa root extracts.

PubMed

Gödecke, Tanja; Nikolic, Dejan; Lankin, David C; Chen, Shao-Nong; Powell, Sharla L; Dietz, Birgit; Bolton, Judy L; van Breemen, Richard B; Farnsworth, Norman R; Pauli, Guido F

2009-01-01

Earlier studies reported serotonergic activity for cimicifugic acids (CA) isolated from Cimicifuga racemosa. The discovery of strongly basic alkaloids, cimipronidines, from the active extract partition and evaluation of previously employed work-up procedures has led to the hypothesis of strong acid/base association in the extract. Re-isolation of the CAs was desired to permit further detailed studies. Based on the acid/base association hypothesis, a new separation scheme of the active partition was required, which separates acids from associated bases. A new 5-HT(7) bioassay guided work-up procedure was developed that concentrates activity into one partition. The latter was subjected to a new two-step centrifugal partitioning chromatography (CPC) method, which applies pH zone refinement gradient (pHZR CPC) to dissociate the acid/base complexes. The resulting CA fraction was subjected to a second CPC step. Fractions and compounds were monitored by (1)H NMR using a structure-based spin-pattern analysis facilitating dereplication of the known acids. Bioassay results were obtained for the pHZR CPC fractions and for purified CAs. A new CA was characterised. While none of the pure CAs was active, the serotonergic activity was concentrated in a single pHZR CPC fraction, which was subsequently shown to contain low levels of the potent 5-HT(7) ligand, N(omega)-methylserotonin. This study shows that CAs are not responsible for serotonergic activity in black cohosh. New phytochemical methodology (pHZR CPC) and a sensitive dereplication method (LC-MS) led to the identification of N(omega)-methylserotonin as serotonergic active principle. Copyright (c) 2009 John Wiley & Sons, Ltd.

Phytochemistry of Cimicifugic Acids and Associated Bases in Cimicifuga racemosa Root Extracts

PubMed Central

GÖdecke, Tanja; Nikolic, Dejan; Lankin, David C.; Chen, Shao-Nong; Powell, Sharla L.; Dietz, Birgit; Bolton, Judy L.; Van Breemen, Richard B.; Farnsworth, Norman R.; Pauli, Guido F.

2009-01-01

Introduction Earlier studies reported serotonergic activity for cimicifugic acids (CA) isolated from Cimicifuga racemosa. The discovery of strongly basic alkaloids, cimipronidines, from the active extract partition and evaluation of previously employed work-up procedures has led to the hypothesis of strong acid/base association in the extract. Objective Re-isolation of the CAs was desired to permit further detailed studies. Based on the acid/base association hypothesis, a new separation scheme of the active partition was required, which separates acids from associated bases. Methodology A new 5-HT7 bioassay guided work-up procedure was developed that concentrates activity into one partition. The latter was subjected to a new 2-step centrifugal partitioning chromatography (CPC) method, which applies pH zone refinement gradient (pHZR CPC) to dissociate the acid/base complexes. The resulting CA fraction was subjected to a second CPC step. Fractions and compounds were monitored by 1H NMR using a structure based spin-pattern analysis facilitating dereplication of the known acids. Bioassay results were obtained for the pHZR CPC fractions and for purified CAs. Results A new CA was characterized. While none of the pure CAs was active, the serotonergic activity was concentrated in a single pHZR CPC fraction, which was subsequently shown to contain low levels of the potent 5-HT7 ligand, Nω–methylserotonin. Conclusion This study shows that CAs are not responsible for serotonergic activity in black cohosh. New phytochemical methodology (pHZR CPC) and a sensitive dereplication method (LC-MS) led to the identification of Nω–methylserotonin as serotonergic active principle. PMID:19140115

Binary Solvent Extraction of Tocols, γ-Oryzanol, and Ferulic Acid from Rice Bran Using Alkaline Treatment Combined with Ultrasonication.

PubMed

Truong, Hoa Thi; Luu, Phuong Duc; Imamura, Kiyoshi; Matsubara, Takeo; Takahashi, Hideki; Takenaka, Norimichi; Boi, Luu Van; Maeda, Yasuaki

2017-06-21

Alkaline treatment (Alk) combined with ultrasound-assisted extraction (UAE) (Alk+UAE) was examined as a means of extracting tocols and γ-oryzanol from rice bran into an organic phase while simultaneously recovering ferulic acid into an aqueous phase. The tocols and γ-oryzanol/ferulic acid yields were determined using high-performance liquid chromatography with fluorescence and UV detection. The effects of extraction conditions were evaluated by varying the Alk treatment temperature and extraction duration. The maximum yields of tocols and γ-oryzanol were obtained at 25 °C over a time span of 30 min. When the temperature was increased to 80 °C, the yield of ferulic acid increased dramatically, whereas the recovery of γ-oryzanol slightly decreased. Employing the Alk+UAE procedure, the recovered concentrations of tocols, γ-oryzanol, and ferulic acid were in the ranges of 146-518, 1591-3629, and 352-970 μg/g, respectively. These results are in good agreement with those reported for rice bran samples from Thailand.

Effects of hyaluronic acid on bleeding following third molar extraction.

PubMed

Gocmen, Gokhan; Aktop, Sertac; Tüzüner, Burcin; Goker, Bahar; Yarat, Aysen

2017-01-01

To explore the effects of hyaluronic acid (HA) on bleeding and associated outcomes after third molar extraction. Forty patients who had undergone molar extraction were randomly divided into two groups; 0.8% (w/v) HA was applied to the HA group (n=20) whereas a control group (n=20) was not treated. Salivary and gingival tissue factor (TF) levels, bleeding time, maximum interincisal opening (MIO), pain scored on a visual analog scale (VAS), and the swelling extent were compared between the two groups. HA did not significantly affect gingival TF levels. Salivary TF levels increased significantly 1 week after HA application but not in the control group. Neither the VAS pain level nor MIO differed significantly between the two groups. The swelling extent on day 3 and the bleeding time were greater in the HA group than in the control group. Local injection of HA at 0.8% prolonged the bleeding time, and increased hemorrhage and swelling in the early postoperative period after third molar extractions.

Effects of different biomass drying and lipid extraction methods on algal lipid yield, fatty acid profile, and biodiesel quality.

PubMed

Hussain, Javid; Liu, Yan; Lopes, Wilson A; Druzian, Janice I; Souza, Carolina O; Carvalho, Gilson C; Nascimento, Iracema A; Liao, Wei

2015-03-01

Three lipid extraction methods of hexane Soxhlet (Sox-Hex), Halim (HIP), and Bligh and Dyer (BD) were applied on freeze-dried (FD) and oven-dried (OD) Chlorella vulgaris biomass to evaluate their effects on lipid yield, fatty acid profile, and algal biodiesel quality. Among these three methods, HIP was the preferred one for C. vulgaris lipid recovery considering both extraction efficiency and solvent toxicity. It had the highest lipid yields of 20.0 and 22.0% on FD and OD biomass, respectively, with corresponding neutral lipid yields of 14.8 and 12.7%. The lipid profiling analysis showed that palmitic, oleic, linoleic, and α-linolenic acids were the major fatty acids in the algal lipids, and there were no significant differences on the amount of these acids between different drying and extraction methods. Correlative models applied to the fatty acid profiles concluded that high contents of palmitic and oleic acids in algal lipids contributed to balancing the ratio of saturated and unsaturated fatty acids and led to a high-quality algal biodiesel.

Estimates of Soil Bacterial Ribosome Content and Diversity Are Significantly Affected by the Nucleic Acid Extraction Method Employed

PubMed Central

Wüst, Pia K.; Nacke, Heiko; Kaiser, Kristin; Marhan, Sven; Sikorski, Johannes; Kandeler, Ellen; Daniel, Rolf

2016-01-01

Modern sequencing technologies allow high-resolution analyses of total and potentially active soil microbial communities based on their DNA and RNA, respectively. In the present study, quantitative PCR and 454 pyrosequencing were used to evaluate the effects of different extraction methods on the abundance and diversity of 16S rRNA genes and transcripts recovered from three different types of soils (leptosol, stagnosol, and gleysol). The quality and yield of nucleic acids varied considerably with respect to both the applied extraction method and the analyzed type of soil. The bacterial ribosome content (calculated as the ratio of 16S rRNA transcripts to 16S rRNA genes) can serve as an indicator of the potential activity of bacterial cells and differed by 2 orders of magnitude between nucleic acid extracts obtained by the various extraction methods. Depending on the extraction method, the relative abundances of dominant soil taxa, in particular Actinobacteria and Proteobacteria, varied by a factor of up to 10. Through this systematic approach, the present study allows guidelines to be deduced for the selection of the appropriate extraction protocol according to the specific soil properties, the nucleic acid of interest, and the target organisms. PMID:26896137

Compositional similarities of non-solvent extractable fatty acids from recent marine sediments deposited in differing environments

NASA Astrophysics Data System (ADS)

Nishimura, Mitsugu; Baker, Earl W.

1987-06-01

Five recent sediment samples from a variety of North American continental shelves were analyzed for fatty acids (FAs) in the solvent-extractable (SOLEX) lipids as well as four types of non-solvent extractable (NONEX) lipids. The NONEX lipids were operationally defined by the succession of extraction procedure required to recover them. The complete procedure included (i) very mild acid treatment, (ii) HF digestion and (iii) saponification of the sediment residue following exhaustive solvent extraction. The distribution pattern and various compositional parameters of SOLEX FAs in the five sediments were divided into three different groups, indicating the difference of biological sources and also diagenetic factors and processes among the three groups of samples. Nevertheless, the compositions of the corresponding NONEX FAs after acid treatment were surprisingly very similar. This was also true for the remaining NONEX FA groups in the five sediment samples. The findings implied that most of the NONEX FAs reported here are derived directly from living organisms. It is also concluded that a large part of NONEX FAs are much more resistant to biodegradation than we have thought, so that they can form the large percentage of total lipids with increasing depth of water and sediments.

Selective Interactions of Valeriana officinalis Extracts and Valerenic Acid with [3H]Glutamate Binding to Rat Synaptic Membranes

PubMed Central

Del Valle-Mojica, Lisa M.; Ayala-Marín, Yoshira M.; Ortiz-Sanchez, Carmen M.; Torres-Hernández, Bianca A.; Abdalla-Mukhaimer, Safa; Ortiz, José G.

2011-01-01

Although GABA neurotransmission has been suggested as a mechanism for Valeriana officinalis effects, CNS depression can also be evoked by inhibition of ionotropic (iGluR) and metabotropic glutamate receptors (mGluR). In this study, we examined if aqueous valerian extract interacted with glutamatergic receptors. Freshly prepared aqueous valerian extract was incubated with rat cortical synaptic membranes in presence of 20 nM [3H]Glutamate. Aqueous valerian extract increased [3H]Glutamate binding from 1 × 10−7 to 1 × 10−3 mg/mL. In the presence of (2S,1′S,2′S)-2-(Carboxycyclopropyl)glycine (LCCG-I) and (2S,2′R,3′R)-2-(2′,3′-Dicarboxycyclopropyl)glycine (DCG-IV), Group II mGluR agents, valerian extract markedly decreased [3H]Glutamate binding, while (2S)-2-amino-3-(3,5-dioxo-1,2,4-oxadiazolidin-2-yl) propanoic acid) (quisqualic acid, QA), Group I mGluR agonist, increased [3H]Glutamate binding. At 0.05 mg/mL aqueous valerian extract specifically interacted with kainic acid NMDA and AMPA receptors. Valerenic acid, a marker compound for Valeriana officinalis, increased the [3H]Glutamate binding after 1.6 × 10−2 mg/mL, and at 0.008 mg/mL it interacted only with QA (Group I mGluR). The selective interactions of valerian extract and valerenic acid with Group I and Group II mGluR may represent an alternative explanation for the anxiolytic properties of this plant. PMID:21584239

Method for extracting lanthanides and actinides from acid solutions by modification of Purex solvent

DOEpatents

Horwitz, E.P.; Kalina, D.G.

1986-03-04

A process is described for the recovery of actinide and lanthanide values from aqueous solutions with an extraction solution containing an organic extractant having the formula as shown in a diagram where [phi] is phenyl, R[sup 1] is a straight or branched alkyl or alkoxyalkyl containing from 6 to 12 carbon atoms and R[sup 2] is an alkyl containing from 3 to 6 carbon atoms and phase modifiers in a water-immiscible hydrocarbon diluent. The addition of the extractant to the Purex process extractant, tri-n-butylphosphate in normal paraffin hydrocarbon diluent, will permit the extraction of multivalent lanthanide and actinide values from 0.1 to 12.0 molar acid solutions. 6 figs.

Extraction of acidic degradation products of organophosphorus chemical warfare agents. Comparison between silica and mixed-mode strong anion-exchange cartridges.

PubMed

Kanaujia, Pankaj K; Pardasani, Deepak; Gupta, A K; Kumar, Rajesh; Srivastava, R K; Dubey, D K

2007-08-17

The analysis of alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs), the hydrolyzed products of nerve agents, constitutes an important aspect for verifying the compliance to the Chemical weapons convention (CWC). This work devotes on the development of solid-phase extraction method using polymeric mixed-mode strong anion-exchange (Oasis MAX) cartridges for extraction of AAPAs and APAs from water. The extracted analytes were analyzed by GC-MS under full scan and selected ion monitoring mode. The extraction efficiencies of MAX and silica-based anion-exchange cartridges were compared, and results revealed that MAX sorbents yielded better recoveries. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 1 mL of acidic methanol (0.1 M), and limits of detection could be achieved up to 5 x 10(-4) microg mL(-1) (in SIM) and 0.05 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of alkylphosphonic acids present in soil sample sent by the Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests.

The ability of walnut extract and fatty acids to protect against the deleterious effects of oxidative stress and inflammation in hippocampal cells.

PubMed

Carey, Amanda N; Fisher, Derek R; Joseph, James A; Shukitt-Hale, Barbara

2013-01-01

Previous research from our lab has demonstrated that dietary walnut supplementation protects against age-related cognitive declines in rats; however, the cellular mechanisms by which walnuts and polyunsaturated fatty acids (PUFAs) may affect neuronal health and functioning in aging are undetermined. We assessed if pretreatment of primary hippocampal neurons with walnut extract or PUFAs would protect cells against dopamine- and lipopolysaccharide-mediated cell death and calcium dysregulation. Rat primary hippocampal neurons were pretreated with varying concentrations of walnut extract, linoleic acid, alpha-linolenic acid, eicosapentaenoic acid, or docosahexaenoic acid prior to exposure to either dopamine or lipopolysaccharide. Viability was assessed using the Live/Dead Cellular Viability/Cytotoxicity Kit. Also, the ability of the cells to return to baseline calcium levels after depolarization was measured with fluorescent imaging. Results indicated that walnut extract, alpha-linolenic acid, and docosahexaenoic acid provided significant protection against cell death and calcium dysregulation; the effects were pretreatment concentration dependent and stressor dependent. Linoleic acid and eicosapentaenoic acid were not as effective at protecting hippocampal cells from these insults. Walnut extract and omega-3 fatty acids may protect against age-related cellular dysfunction, but not all PUFAs are equivalent in their beneficial effects.

Comparison of four extraction/methylation analytical methods to measure fatty acid composition by gas chromatography in meat.

PubMed

Juárez, M; Polvillo, O; Contò, M; Ficco, A; Ballico, S; Failla, S

2008-05-09

Four different extraction-derivatization methods commonly used for fatty acid analysis in meat (in situ or one-step method, saponification method, classic method and a combination of classic extraction and saponification derivatization) were tested. The in situ method had low recovery and variation. The saponification method showed the best balance between recovery, precision, repeatability and reproducibility. The classic method had high recovery and acceptable variation values, except for the polyunsaturated fatty acids, showing higher variation than the former methods. The combination of extraction and methylation steps had great recovery values, but the precision, repeatability and reproducibility were not acceptable. Therefore the saponification method would be more convenient for polyunsaturated fatty acid analysis, whereas the in situ method would be an alternative for fast analysis. However the classic method would be the method of choice for the determination of the different lipid classes.

SIMPLE METHOD FOR THE EXTRACTION OF PHOTOPIGMENTS AND MYCOSPORINE-LIKE AMINO ACIDS (MAAS) FROM SYMBIODINIUM SPP.

EPA Science Inventory

Numerous extraction methods have been developed and used in the quantitation of both photopigments and mycosporine amino acids (MAAs) found in Symbiodinium sp. and zooanthellate metazoans. We have development of a simple, mild extraction procedure using methanol, which when coupl...

Vine-shoot waste aqueous extract applied as foliar fertilizer to grapevines: Effect on amino acids and fermentative volatile content.

PubMed

Sánchez-Gómez, R; Garde-Cerdán, T; Zalacain, A; Garcia, R; Cabrita, M J; Salinas, M R

2016-04-15

The aim of this work was to study the influence of foliar applications of different wood aqueous extracts on the amino acid content of musts and wines from Airén variety; and to study their relationship with the volatile compounds formed during alcoholic fermentation. For this purpose, the foliar treatments proposed were a vine-shoot aqueous extract applied in one and two times, and an oak extract which was only applied once. Results obtained show the potential of Airén vine-shoot waste aqueous extracts to be used as foliar fertilizer, enhancing the wine amino acid content especially when they were applied once. Similar results were observed with the aqueous oak extract. Regarding wine fermentative volatile compounds, there is a close relationship between musts and their wines amino acid content allowing us to discuss about the role of proline during the alcoholic fermentation and the generation of certain volatiles. Copyright © 2015 Elsevier Ltd. All rights reserved.

Indigenous microbes survive in situ ozonation improving biodegradation of dissolved organic matter in aged oil sands process-affected waters.

PubMed

Brown, Lisa D; Pérez-Estrada, Leonidas; Wang, Nan; El-Din, Mohamed Gamal; Martin, Jonathan W; Fedorak, Phillip M; Ulrich, Ania C

2013-11-01

The oil sands industry faces significant challenges in developing effective remediation technologies for process-affected water stored in tailings ponds. Naphthenic acids, a complex mixture of cycloaliphatic carboxylic acids, have been of particular concern because they concentrate in tailings ponds and are a component of the acutely toxic fraction of process water. Ozone treatment has been demonstrated as an effective means of rapidly degrading naphthenic acids, reducing process water toxicity, and increasing its biodegradability following seeding with the endogenous process water bacteria. This study is the first to examine subsequent in situ biodegradation following ozone pretreatment. Two aged oil sands process-affected waters from experimental reclamation tailings ponds were ozonated to reduce the dissolved organic carbon, to which naphthenic acids contributed minimally (<1mgL(-1)). Treatment with an ozone dose of 50mgL(-1) improved the 84d biodegradability of remaining dissolved organic carbon during subsequent aerobic incubation (11-13mgL(-1) removed from aged process-affected waters versus 5mgL(-1) when not pretreated with ozone). The ozone-treated indigenous microbial communities were as capable of degrading organic matter as the same community not exposed to ozone. This supports ozonation coupled with biodegradation as an effective and feasible treatment option. Copyright © 2013 Elsevier Ltd. All rights reserved.

Novel assay system for acidic Peptide:N-glycanase (aPNGase) activity in crude plant extract.

PubMed

Uemura, Ryota; Ogura, Mikako; Matsumaru, Chihiro; Akiyama, Tsuyoshi; Maeda, Megumi; Kimura, Yoshinobu

2018-04-15

Acidic peptide:N-glycanase (aPNGase) plays a pivotal role in plant glycoprotein turnover. For the construction of aPNGase-knockout or -overexpressing plants, a new method to detect the activity in crude plant extracts is required because endogenous peptidases present in the extract hamper enzyme assays using fluorescence-labeled N-glycopeptides as a substrate. In this study, we developed a new method for measuring aPNGase activity in crude extracts from plant materials.

A fully disposable and integrated paper-based device for nucleic acid extraction, amplification and detection.

PubMed

Tang, Ruihua; Yang, Hui; Gong, Yan; You, MinLi; Liu, Zhi; Choi, Jane Ru; Wen, Ting; Qu, Zhiguo; Mei, Qibing; Xu, Feng

2017-03-29

Nucleic acid testing (NAT) has been widely used for disease diagnosis, food safety control and environmental monitoring. At present, NAT mainly involves nucleic acid extraction, amplification and detection steps that heavily rely on large equipment and skilled workers, making the test expensive, time-consuming, and thus less suitable for point-of-care (POC) applications. With advances in paper-based microfluidic technologies, various integrated paper-based devices have recently been developed for NAT, which however require off-chip reagent storage, complex operation steps and equipment-dependent nucleic acid amplification, restricting their use for POC testing. To overcome these challenges, we demonstrate a fully disposable and integrated paper-based sample-in-answer-out device for NAT by integrating nucleic acid extraction, helicase-dependent isothermal amplification and lateral flow assay detection into one paper device. This simple device allows on-chip dried reagent storage and equipment-free nucleic acid amplification with simple operation steps, which could be performed by untrained users in remote settings. The proposed device consists of a sponge-based reservoir and a paper-based valve for nucleic acid extraction, an integrated battery, a PTC ultrathin heater, temperature control switch and on-chip dried enzyme mix storage for isothermal amplification, and a lateral flow test strip for naked-eye detection. It can sensitively detect Salmonella typhimurium, as a model target, with a detection limit of as low as 10 2 CFU ml -1 in wastewater and egg, and 10 3 CFU ml -1 in milk and juice in about an hour. This fully disposable and integrated paper-based device has great potential for future POC applications in resource-limited settings.

Selective Extraction and Purification of Azaspiracids from Blue Mussels ( Mytilus edulis) Using Boric Acid Gel.

PubMed

Miles, Christopher O; Kilcoyne, Jane; McCarron, Pearse; Giddings, Sabrina D; Waaler, Thor; Rundberget, Thomas; Samdal, Ingunn A; Løvberg, Kjersti E

2018-03-21

Azaspiracids belong to a family of more than 50 polyether toxins originating from marine dinoflagellates such as Azadinium spinosum. All of the azaspiracids reported thus far contain a 21,22-dihydroxy group. Boric acid gel can bind selectively to compounds containing vic-diols or α-hydroxycarboxylic acids via formation of reversible boronate complexes. Here we report use of the gel to selectively capture and release azaspiracids from extracts of blue mussels. Analysis of the extracts and fractions by liquid chromatography-tandem mass spectrometry (LC-MS) showed that this procedure resulted in an excellent cleanup of the azaspiracids in the extract. Analysis by enzyme-linked immunoasorbent assay (ELISA) and LC-MS indicated that most azaspiracid analogues were recovered in good yield by this procedure. The capacity of boric acid gel for azaspiracids was at least 50 μg/g, making this procedure suitable for use in the early stages of preparative purification of azaspiracids. In addition to its potential for concentration of dilute samples, the extensive cleanup provided by boric acid gel fractionation of azaspiracids in mussel samples almost eliminated matrix effects during subsequent LC-MS and could be expected to reduce matrix effects during ELISA analysis. The method may therefore prove useful for quantitative analysis of azaspiracids as part of monitoring programs. Although LC-MS data showed that okadaic acid analogues also bound to the gel, this was much less efficient than for azaspiracids under the conditions used. The boric acid gel methodology is potentially applicable to other important groups of natural toxins containing diols including ciguatoxins, palytoxins, pectenotoxins, tetrodotoxin, trichothecenes, and toxin glycosides.

Solvent Extraction and GC-MS Analysis of Sesame Seeds for Determination of Bioactive Antioxidant Fatty Acid/Fatty Oil Components.

PubMed

Qadir, Abdul; Ali, Athar; Arif, Muhammad; Al-Rohaimi, Abdulmohsen H; Singh, Satya Prakash; Ahmad, Usama; Khalid, Mohd; Kumar, Arun

2018-06-01

The seed kernels of Sesamum indicum L. (family: Pedaliaceae) were extracted with ethanol and yield of components determined by Gas Chromatography/Mass Spectrometry (GC/MS). The free radical scavenging activities of ethanolic extract against1, 1-Diphenyl-2-picrylhydrazyl (DPPH) were determined by UV spectrophotometer at 517 nm. Phytochemical screening revealed the presence of numerous bioactive compounds including steroids, phenolic, terpenoids, fatty acids and different types of ester compounds. The ethanolic extract was purified and analyzed by GC MS.The prevailing compounds found in ethanolic extract were Carvacrol (0.04%),Sesamol (0.11%), 4-Allyl-2-methoxy-phenol(0.04%),Palmitic acid (1.08%), cis-9-Hexadecenal (85.40%), Lineoleoyl chloride (0.52%), Palmitic acid β-monoglyceride (0.40%), Dihydro-aplotaxene (0.61%), Oleoyl chloride (1.11%), (+)-Sesamin (4.73%), 1,3-Benzodioxole, 5-[4-(1,3-benzodioxol-5-yloxy)tetrahydro-1 H,3 H-furo [3,4-c]furan-1-yl], [1 S-(1,3,4,6α.), (2.01%)], 6-Nitrocholest-5-en-3-yl acetate (0.22%), Ergost-5-en-3β-ol (2.35%) and 24-Propylidenecholesterol (0.16%). The presence ofsaturated and unsaturated fatty acids in ethanolicextract justifies the use of this plant to treat many ailments in folk and traditional medicine. Ethanolic extract have shown significant antioxidant activity(IC 50 120.38±2.8 µg/ml). The presence of phenolic (Sesamol), lignin (Sesamin) compounds and unsaturated fatty acids are reported as possible contributor for antioxidantactivity of seed extract. © Georg Thieme Verlag KG Stuttgart · New York.

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

PubMed Central

Cho, GyeYoon; Han, KyuChul; Yoon, JinYoung

2015-01-01

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

Structural and technological characterisation of pectin extracted with sodium citrate and nitric acid from sunflower heads.

PubMed

Muñoz-Almagro, Nerea; Rico-Rodriguez, Fabián; Wilde, Peter J; Montilla, Antonia; Villamiel, Mar

2018-05-18

An optimisation of temperature, time and extracting agent concentration of pectin extraction from sunflower heads using sodium citrate and nitric acid (SP-SC and SP-NA) was carried out. At optimal conditions, the yield of extraction with nitric acid (SPO-NA) was 2-fold greater than the corresponding with sodium citrate (SPO-SC) (14.3 vs 7.7%, respectively). Regarding pectin structure, the galacturonic acid (GalA) content in both, SPO-SC and SPO-NA, was similar (∼85%). However, SPO-NA showed lower molecular weight (Mw) (88.9 kDa) and neutral sugar content (4%) than SPO-SC (464 kDa, 9%), indicating that nitric acid deeply degraded pectin structure. These differences derived into dissimilar behaviour in their technological functionality. SPO-SC showed higher viscosity and better emulsifying capacity than SPO-NA, although any of them were able to stabilise the oil/water emulsion. Both sunflower pectins formed gels with Ca 2+ (75 mg/g of pectin) at pH 3.0. However, when sucrose was added, the gels formed by SP-SC and 20% sucrose presented the same hardness as those of SP-NA with 40% sucrose. These results suggest that the pectin extracted with sodium citrate, an eco-friendly agent, could be a promising ingredient, with good thickening and gelling properties. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Method for extracting lanthanides and actinides from acid solutions

DOEpatents

Horwitz, E. Philip; Kalina, Dale G.; Kaplan, Louis; Mason, George W.

1985-01-01

A process for the recovery of actinide and lanthanide values from aqueous acidic solutions with an organic extractant having the formula: ##STR1## where .phi. is phenyl, R.sup.1 is a straight or branched alkyl or alkoxyalkyl containing from 6 to 12 carbon atoms and R.sup.2 is an alkyl containing from 3 to 6 carbon atoms. The process is suitable for the separation of actinide and lanthanide values from fission product values found together in high level nuclear reprocessing waste solutions.

Tranexamic Acid in Control of Haemorrhage after Dental Extraction in Haemophilia and Christmas Disease

PubMed Central

Forbes, C. D.; Barr, R. D.; Reid, G.; Thomson, C.; Prentice, C. R. M.; Nicol, G. P. Mc; Douglas, A. S.

1972-01-01

In a double-blind trial tranexamic acid (AMCA, Cyclokapron), 1 g three times a day for five days, significantly reduced blood loss and transfusion requirements after dental extraction in patients with haemophilia and Christmas disease. No side effects were seen in either group of patients. Screening tests showed no toxic action of tranexamic acid on the liver, kidney, or heart. PMID:4553818