Sequential extractions of selenium soils from Stewart Lake: total selenium and speciation measurements with ICP-MS detection.

PubMed

Ponce de León, Claudia A; DeNicola, Katie; Montes Bayón, Maria; Caruso, Joseph A

2003-06-01

Different techniques have been employed in order to evaluate the most efficient procedure for the extraction of selenium from soil as required for speciation. Selenium contaminated sediments from Stewart Lake Wetland, California were used. A strong acid mineralization of the samples gives quantitative total selenium, which is then used to estimate recoveries for the milder extraction methods. The different extraction methodologies involve the sequential use of water, buffer (phosphate, pH 7) and either acid solution (e.g. HNO3 or HCl) or basic solutions (e.g. ammonium acetate, NaOH or TMAH). Pyrophosphate extraction was also evaluated and showed that selenium was not associated with humic acids. The extractants were subsequently analyzed by size exclusion chromatography (SEC) with UV (254 and 400 nm) and on-line ICP-MS detection; anion exchange chromatography, and ion-pair reversed phase chromatography with ICP-MS detection. For sequential extractions the extraction efficiencies showed that the basic extractions were more efficient than the acidic. The difference between the acidic and the basic extraction efficiency is carried to the sulfite extraction, suggesting that whatever is not extracted by the acid is subsequently extracted by the sulfite. The species identified with the different chromatographies were selenate, selenite, elemental selenium and some organic selenium.

Development of new efficient method for isolation of phenolics from sea algae prior to their rapid resolution liquid chromatographic-tandem mass spectrometric determination.

PubMed

Klejdus, Bořivoj; Plaza, Merichel; Šnóblová, Marie; Lojková, Lea

2017-02-20

The extraction of phenolic compounds from 4 different sea algae samples, three brown algae (Cystoseira abies-marina, C. abies-marina grinded under cryogenic conditions with liquid nitrogen, Undaria pinnatifida and Sargassum muticum) and one red algae (Chondrus crispus) via solid phase extraction using micro-elution solid-phase extraction (μ-SPE) plate method was studied. Prior to μ-SPE, 50mg of algae with 80% methanol mixture was extracted in hyphenated series by various extraction techniques, such as pressurized liquid extraction and Ika Ultra-Turrax ® Tube Drive, in combination with ultrasound assisted extraction. The μ-SPE plate technique reduced the time of sample pre-treatment thanks to higher sensitivity and pre-concentration effect. Selected groups of benzoic acid derivatives (p-hydroxybenzoic, protocatechuic, gallic, vanillic, and syringic acids), hydroxybenzaldehydes (4-hydroxybenzaldehyde, and 3,4-dihydroxybenzaldehyde), and cinnamic acid derivatives (p-coumaric, caffeic, ferulic, sinapic, and chlorogenic acids) were determined using rapid resolution liquid chromatography coupled to mass spectrometry detection with negative ion electrospray ionization (RRLC-ESI-MS) using multiple reactions monitoring. LOQs of measured samples varied in the range 0.23-1.68ng/mL and LODs in the range 0.07-0.52ng/mL. The applied method allowed a simultaneous determination of phenolics (i.e. free, esters soluble in methanol, glycosides, and esters insoluble in methanol) in less than 5min (including alkaline or acidic hydrolysis of raw extracts) from sea algae extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

Isolation of Shikimic Acid from Star Aniseed

ERIC Educational Resources Information Center

Payne, Richard; Edmonds, Michael

2005-01-01

A new undergraduate laboratory experiment suitable for demonstrating some key techniques used in natural products chemistry is described. A laboratory experiment is developed which in the process of extracting shikimic acid from star aniseed exposes students to a number of important experimental techniques.

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.

Amino acid distribution in meteorites: diagenesis, extraction methods, and standard metrics in the search for extraterrestrial biosignatures.

PubMed

McDonald, Gene D; Storrie-Lombardi, Michael C

2006-02-01

The relative abundance of the protein amino acids has been previously investigated as a potential marker for biogenicity in meteoritic samples. However, these investigations were executed without a quantitative metric to evaluate distribution variations, and they did not account for the possibility of interdisciplinary systematic error arising from inter-laboratory differences in extraction and detection techniques. Principal component analysis (PCA), hierarchical cluster analysis (HCA), and stochastic probabilistic artificial neural networks (ANNs) were used to compare the distributions for nine protein amino acids previously reported for the Murchison carbonaceous chondrite, Mars meteorites (ALH84001, Nakhla, and EETA79001), prebiotic synthesis experiments, and terrestrial biota and sediments. These techniques allowed us (1) to identify a shift in terrestrial amino acid distributions secondary to diagenesis; (2) to detect differences in terrestrial distributions that may be systematic differences between extraction and analysis techniques in biological and geological laboratories; and (3) to determine that distributions in meteoritic samples appear more similar to prebiotic chemistry samples than they do to the terrestrial unaltered or diagenetic samples. Both diagenesis and putative interdisciplinary differences in analysis complicate interpretation of meteoritic amino acid distributions. We propose that the analysis of future samples from such diverse sources as meteoritic influx, sample return missions, and in situ exploration of Mars would be less ambiguous with adoption of standardized assay techniques, systematic inclusion of assay standards, and the use of a quantitative, probabilistic metric. We present here one such metric determined by sequential feature extraction and normalization (PCA), information-driven automated exploration of classification possibilities (HCA), and prediction of classification accuracy (ANNs).

Supercritical Fluid Extraction and Separation of Uranium from Other Actinides

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

Donna L. Quach; Bruce J. Mincher; Chien M. Wai

2014-06-01

This paper investigates the feasibility of separating uranium from other actinides by using supercritical fluid carbon dioxide (sc-CO2) as a solvent modified with tri-n-butylphosphate (TBP) for the development of an extraction and counter current stripping technique, which would be a more efficient and environmentally benign technology for used nuclear fuel reprocessing compared to traditional solvent extraction. Several actinides (U(VI), Np(VI), Pu(IV), and Am(III)) were extracted in sc-CO2 modified with TBP over a range of nitric acid concentrations and then the actinides were exposed to reducing and complexing agents to suppress their extractability. According to this study, the separation of uraniummore » from plutonium in sc-CO2 modified with TBP was successful at nitric acid concentrations of less than 3 M in the presence of acetohydroxamic acid or oxalic acid, and the separation of uranium from neptunium was successful at nitric acid concentrations of less than 1 M in the presence of acetohydroxamic acid, oxalic acid, or sodium nitrite.« less

Characterization of Linum usitatissimum L. oil obtained from different extraction technique and in vitro antioxidant potential of supercritical fluid extract

PubMed Central

Chauhan, Rishika; Chester, Karishma; Khan, Yasmeen; Tamboli, Ennus Tajuddin; Ahmad, Sayeed

2015-01-01

Aim: Present investigation was aimed to characterize the fixed oil of Linum usitatissimum L. using five different extraction methods: Supercritical fluid extraction (SFE), ultrasound-assistance, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO2) were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high performance thin layer chromatography (HPTLC), gas chromatography-mass spectrometry (GC-MS), and Fourier-transformed infrared spectroscopy (FT-IR) fingerprinting. Antioxidant activity was also determined using 1,1-diphenyl-2-picrylhydrazyl and superoxide scavenging method. Result: The main fatty acids were α-linolenic acid, linoleic acid, palmitic acid, and stearic acid as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks, as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods, were superimposable. Conclusion: Analysis reported that the fixed oil of L. usitatissimum L. is a good source of n-3 fatty acid with the significant antioxidant activity of oil obtained from SFE extraction method. PMID:26681884

Extraction techniques for arsenic species in rice flour and their speciation by HPLC-ICP-MS.

PubMed

Narukawa, Tomohiro; Suzuki, Toshihiro; Inagaki, Kazumi; Hioki, Akiharu

2014-12-01

The extraction of arsenic (As) species present in rice flour samples was investigated using different extracting solvents, and the concentration of each species was determined by HPLC-ICP-MS after heat-assisted extraction. The extraction efficiencies for total arsenic species and especially for arsenite [As(III)] and arsenate [As(V)] were investigated. As(III), As(V) and dimethylarsinic acid (DMAA) were found in the samples, and the concentration of DMAA did not vary with treatment conditions. However, the concentrations of extracted total arsenic and those of As(III) and As(V) depended on the extracting solvents. When an extracting solvent was highly acidic, the concentrations of extracted total arsenic were in good agreement with the total arsenic concentration determined by ICP-MS after microwave-assisted digestion, though a part of the As(V) was reduced to As(III) during the highly acidic extraction process. Extraction under neutral conditions increased the extracted As(V), but extracted total arsenic was decreased because a part of the As(III) could not be extracted. Optimum conditions for the extraction of As(III) and As(V) from rice flour samples are discussed to allow the accurate determinations of As(III), As(V) and DMAA in the rice flour samples. Heat block extraction techniques using 0.05 mol L(-1) HClO4 and silver-containing 0.15 mol L(-1) HNO3 were also developed. Copyright © 2014 Elsevier B.V. All rights reserved.

Green Extraction of Natural Antioxidants from the Sterculia nobilis Fruit Waste and Analysis of Phenolic Profile.

PubMed

Zhang, Jiao-Jiao; Li, Ya; Lin, Sheng-Jun; Li, Hua-Bin

2018-05-02

The waste of Sterculia nobilis fruit was massively produced during food processing, which contains lots of natural antioxidants. In this study, antioxidants in the Sterculia nobilis fruit waste were extracted using the green microwave-assisted extraction (MAE) technique. The effects of five independent variables (ethanol concentration, solvent/material ratio, extraction time, temperature, and microwave power) on extraction efficiency were explored, and three major factors (ethanol concentration, extraction time, and temperature) showing great influences were chosen to study their interactions by response surface methodology. The optimal conditions were as follows: 40.96% ethanol concentration, 30 mL/g solvent/material ratio, 37.37 min extraction time at 66.76 °C, and 700 W microwave power. The Trolox equivalent antioxidant capacity value obtained in optimal conditions was in agreement with the predicted value. Besides, MAE improved the extraction efficiency compared with maceration and Soxhlet extraction methods. Additionally, the phenolic profile in the extract was analyzed by UPLC-MS/MS, and eight kinds of phenolic compounds were identified and quantified, including epicatechin, protocatechuic acid, ferulic acid, gallic acid, p -coumaric acid, caffeic acid, quercetin, and p -hydroxycinnamic acid. This study could contribute to the value-added utilization of the waste from Sterculia nobilis fruit, and the extract could be developed as food additive or functional food.

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.

Metabonomics study on Polygonum multiflorum induced liver toxicity in rats by GC-MS

PubMed Central

Zhang, Yuan; Wang, Nannan; Zhang, Meiling; Diao, Tingting; Tang, Jingyue; Dai, Mingzhu; Chen, Suhong; Lin, Guanyang

2015-01-01

Polygonum multiflorum, a traditional Chinese medicinal herb, is widely used in liver and liver nourishing. Recent years, drug regulatory departments reported that Polygonum multiflorum caused serious adverse reaction in clinic, especially liver injury. In this study, we detected the changes in rat serum and liver tissue metabolites through gas chromatography-mass spectrometry (GC-MS). Mass spectrometry, partial least squares-discriminate analysis (PLS-DA) and other diversified techniques were used to analyze the differences among their metabolites. Compared to the control group, the serum concentrations of L-threonine and serine in water extraction groups increased. The serum concentrations of 9,12-octadecadienoic acid, hexadecanoic acid, oleic acid, D-glucose and octadecanoic acid in alcohol extraction groups increased, while lactic acid decreased to a great extent. For liver tissue, compared to the control group, the concentrations of myo-inositol, oleic acid and cholesterol in water extraction groups increased, while those of hexadecanoic acid, octadecanoic acid, ribitol and butanedioic acid decreased to a great extent. The concentrations of myo-inositol, phosphoric acid, uridine, oleic acid, cholesterol and butanoic acid in alcohol extraction groups increased to a great extent, while those of hexadecanoic acid, octadecanoic acid, ribitol and butanedioic acid decreased. The results indicate that Polygonum multiflorum induces the metabolic disorders of energy metabolism, amino acid and lipid metabolism. What’s more, liver injury of alcohol extraction group was more serious than group of water extraction. PMID:26379894

Metal separation from mixed types of batteries using selective precipitation and liquid-liquid extraction techniques.

PubMed

Provazi, Kellie; Campos, Beatriz Amaral; Espinosa, Denise Crocce Romano; Tenório, Jorge Alberto Soares

2011-01-01

The purpose of this paper is to study metal separation from a sample composed of a mixture of the main types of spent household batteries, using a hydrometallurgical route, comparing selective precipitation and liquid-liquid extraction separation techniques. The preparation of the solution consisted of: grinding the waste of mixed batteries, reduction and volatile metals elimination using electric furnace and acid leaching. From this solution two different routes were studied: selective precipitation with sodium hydroxide and liquid-liquid extraction using Cyanex 272 [bis(2,4,4-trimethylpentyl) phosphoric acid] as extracting agent. The best results were obtained from liquid-liquid extraction in which Zn had a 99% extraction rate at pH 2.5. More than 95% Fe was extracted at pH 7.0, the same pH at which more than 90% Ce was extracted. About 88% Mn, Cr and Co was extracted at this pH. At pH 3.0, more than 85% Ni was extracted, and at pH 3.5 more than 80% of Cd and La was extracted. Copyright © 2010 Elsevier Ltd. All rights reserved.

Analysis of Phenolic Compounds and Antioxidant Activity in Wild Blackberry Fruits

PubMed Central

Oszmiański, Jan; Nowicka, Paulina; Teleszko, Mirosława; Wojdyło, Aneta; Cebulak, Tomasz; Oklejewicz, Krzysztof

2015-01-01

Twenty three different wild blackberry fruit samples were assessed regarding their phenolic profiles and contents (by LC/MS quadrupole time-of-flight (QTOF) and antioxidant activity (ferric reducing ability of plasma (FRAP) and 2,2-azinobis (3-ethyl-benzothiazoline-6-sulfonic acid) (ABTS)) by two different extraction methods. Thirty four phenolic compounds were detected (8 anthocyanins, 15 flavonols, 3 hydroxycinnamic acids, 6 ellagic acid derivatives and 2 flavones). In samples, where pressurized liquid extraction (PLE) was used for extraction, a greater increase in yields of phenolic compounds was observed, especially in ellagic acid derivatives (max. 59%), flavonols (max. 44%) and anthocyanins (max. 29%), than after extraction by the ultrasonic technique extraction (UAE) method. The content of phenolic compounds was significantly correlated with the antioxidant activity of the analyzed samples. Principal component analysis (PCA) revealed that the PLE method was more suitable for the quantitative extraction of flavonols, while the UAE method was for hydroxycinnamic acids. PMID:26132562

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.

Comparison of two extraction techniques, solid-phase microextraction versus continuous liquid-liquid extraction/solvent-assisted flavor evaporation, for the analysis of flavor compounds in gueuze lambic beer.

PubMed

Thompson-Witrick, Katherine A; Rouseff, Russell L; Cadawallader, Keith R; Duncan, Susan E; Eigel, William N; Tanko, James M; O'Keefe, Sean F

2015-03-01

Lambic is a beer style that undergoes spontaneous fermentation and is traditionally produced in the Payottenland region of Belgium, a valley on the Senne River west of Brussels. This region appears to have the perfect combination of airborne microorganisms required for lambic's spontaneous fermentation. Gueuze lambic is a substyle of lambic that is made by mixing young (approximately 1 year) and old (approximately 2 to 3 years) lambics with subsequent bottle conditioning. We compared 2 extraction techniques, solid-phase microextraction (SPME) and continuous liquid-liquid extraction/solvent-assisted flavor evaporation (CCLE/SAFE), for the isolation of volatile compounds in commercially produced gueuze lambic beer. Fifty-four volatile compounds were identified and could be divided into acids (14), alcohols (12), aldehydes (3), esters (20), phenols (3), and miscellaneous (2). SPME extracted a total of 40 volatile compounds, whereas CLLE/SAFE extracted 36 volatile compounds. CLLE/SAFE extracted a greater number of acids than SPME, whereas SPME was able to isolate a greater number of esters. Neither extraction technique proved to be clearly superior and both extraction methods can be utilized for the isolation of volatile compounds found in gueuze lambic beer. © 2015 Institute of Food Technologists®

Development of Novel Method for Rapid Extract of Radionuclides from Solution Using Polymer Ligand Film

NASA Astrophysics Data System (ADS)

Rim, Jung H.

Accurate and fast determination of the activity of radionuclides in a sample is critical for nuclear forensics and emergency response. Radioanalytical techniques are well established for radionuclides measurement, however, they are slow and labor intensive, requiring extensive radiochemical separations and purification prior to analysis. With these limitations of current methods, there is great interest for a new technique to rapidly process samples. This dissertation describes a new analyte extraction medium called Polymer Ligand Film (PLF) developed to rapidly extract radionuclides. Polymer Ligand Film is a polymer medium with ligands incorporated in its matrix that selectively and rapidly extract analytes from a solution. The main focus of the new technique is to shorten and simplify the procedure necessary to chemically isolate radionuclides for determination by alpha spectrometry or beta counting. Five different ligands were tested for plutonium extraction: bis(2-ethylhexyl) methanediphosphonic acid (H2DEH[MDP]), di(2-ethyl hexyl) phosphoric acid (HDEHP), trialkyl methylammonium chloride (Aliquat-336), 4,4'(5')-di-t-butylcyclohexano 18-crown-6 (DtBuCH18C6), and 2-ethylhexyl 2-ethylhexylphosphonic acid (HEH[EHP]). The ligands that were effective for plutonium extraction further studied for uranium extraction. The plutonium recovery by PLFs has shown dependency on nitric acid concentration and ligand to total mass ratio. H2DEH[MDP] PLFs performed best with 1:10 and 1:20 ratio PLFs. 50.44% and 47.61% of plutonium were extracted on the surface of PLFs with 1M nitric acid for 1:10 and 1:20 PLF, respectively. HDEHP PLF provided the best combination of alpha spectroscopy resolution and plutonium recovery with 1:5 PLF when used with 0.1M nitric acid. The overall analyte recovery was lower than electrodeposited samples, which typically has recovery above 80%. However, PLF is designed to be a rapid field deployable screening technique and consistency is more important than recovery. PLFs were also tested using blind quality control samples and the activities were accurately measured. It is important to point out that PLFs were consistently susceptible to analytes penetrating and depositing below the surface. The internal radiation within the body of PLF is mostly contained and did not cause excessive self-attenuation and peak broadening in alpha spectroscopy. The analyte penetration issue was beneficial in the destructive analysis. H2DEH[MDP] PLF was tested with environmental samples to fully understand the capabilities and limitations of the PLF in relevant environments. The extraction system was very effective in extracting plutonium from environmental water collected from Mortandad Canyon at Los Alamos National Laboratory with minimal sample processing. Soil samples were tougher to process than the water samples. Analytes were first leached from the soil matrixes using nitric acid before processing with PLF. This approach had a limitation in extracting plutonium using PLF. The soil samples from Mortandad Canyon, which are about 1% iron by weight, were effectively processed with the PLF system. Even with certain limitations of the PLF extraction system, this technique was able to considerably decrease the sample analysis time. The entire environmental sample was analyzed within one to two days. The decrease in time can be attributed to the fact that PLF is replacing column chromatography and electrodeposition with a single step for preparing alpha spectrometry samples. The two-step process of column chromatography and electrodeposition takes a couple days to a week to complete depending on the sample. The decrease in time and the simplified procedure make this technique a unique solution for application to nuclear forensics and emergency response. A large number of samples can be quickly analyzed and selective samples can be further analyzed with more sensitive techniques based on the initial data. The deployment of a PLF system as a screening method will greatly reduce a total analysis time required to gain meaningful isotopic data for the nuclear forensics application. (Abstract shortened by UMI.)

Evaluation of current techniques for isolation of chars as natural adsorbents

USGS Publications Warehouse

Chun, Y.; Sheng, G.; Chiou, C.T.

2004-01-01

Chars in soils or sediments may potentially influence the soil/sediment sorption behavior. Current techniques for the isolation of black carbon including chars rely often on acid demineralization, base extraction, and chemical oxidation to remove salts and minerals, humic acid, and refractory kerogen, respectively. Little is known about the potential effects of these chemical processes on the char surface and adsorptive properties. This study examined the effects of acid demineralization, base extraction, and acidic Cr2O72- oxidation on the surface areas, surface acidity, and benzene adsorption characteristics of laboratory-produced pinewood and wheat-residue chars, pure or mixed with soils, and a commercial activated carbon. Demineralization resulted in a small reduction in the char surface area, whereas base extraction showed no obvious effect. Neither demineralization nor base extraction caused an appreciable variation in benzene adsorption and presumably the char surface properties. By contrast, the Cr2O 72- oxidation caused a >31% reduction in char surface area. The Boehm titration, supplemented by FTIR spectra, indicated that the surface acidity of oxidized chars increased by a factor between 2.3 and 12 compared to nonoxidized chars. Benzene adsorption with the oxidized chars was lower than that with the non-oxidized chars by a factor of >8.9; both the decrease in char surface area and the increase in char surface acidity contributed to the reduction in char adsorptive power. Although the Cr 2O72- oxidation effectively removes resistant kerogen, it is not well suited for the isolation of chars as contaminant adsorbents because of its destructive nature. Alternative nondestructive techniques that preserve the char surface properties and effectively remove kerogen must be sought.

[The isolation of organic compounds from hydrosulfuric mineral waters with the use of the extractive freezing-out technique with centrifugation].

PubMed

Bekhterev, V N; Kabina, E A

The mineral waters, enriched with organic substances find extensive application in balneotherapy. The fast and efficient methods for the identification and quantitative measurement of organic compounds (in the first place, organic acids) in such waters need to be developed for the estimation of their quality and biological activity. The objective of the present study was to elaborate a gas chromatographic method for the determination of monobasic carbonic acids in sulfide-containing mineral waters by means of extractive freezing-out in combination with the application of the centrifugal forces for the elucidation of the metrological characteristics of the compounds of interest. The secondary objective was to estimate the prospects for the application of the method of interest for determining the dissolved organic compounds in mineral waters. The following carbonic acids were used for the purposes of the study: acetic acid (analytical grade), Russia; propionic grade (extra pure), Ferak, Germany; butyric acid (pure), Russia; valeric acid (pure), Russia; caproic acid (pure), Russia; oenanthic acid (pure), Russia; and caprylic acid (pure), Russia). Acetonitrile («O» grade), Russia, was used as the extracting agent. The LV-210 analytical balance (Russia) was used to prepare the model and standard solutions of the organic compounds and to determine their mass. The extracts and standard mixture were investigated by the gas chromatographic technique with the use of the Kristallyuks apparatus («Meta-Khrom», Russia) equipped with the flame ionization detector and the capillary column. Extractive freezing-out in the combination with centrifugation was performed with the laboratory installation for this purpose. Under the model conditions, a single extractive freezing-out procedure with the centrifugation of the sample made it possible to reach the 22-37-fold concentration of C2-C8 monobasic carbonic acids during their transfer from water into acetonitrile. The metrological parameters of the proposed procedure for gas-chromatographic determination of the aforementioned acids in hydrosulfuric mineral waters were estimated. The limit of detection of acetic and propionic acids has been 0,2 mg/l, that for butyric acid 0,1 mg/l, for valeric, caproic, oenanthic and caprylic acids 0,05 mg/l. We failed to identify C2-C8 carbonic acids in hydrosulfuric water from the 6T well of the field Matsesta fields. The investigation of the extracts obtained by the proposed extraction procedure with the use of the newly developed variant of high performance liquid chromatography (HPLC) with diode-matrix detection revealed the presence of various amounts of unknown organic substances. The UV-spectrum of one of those components was obtained which made it possible to conjecture its molecular structure. The procedure for the sample preparation and the following determination of organic acids in water is simple, carried out in a single stage, and does not impose special requirements to the qualification of the researcher. It allows to describe the newly developed technique as a rapid test method. Along with it, realization of extraction in the negative temperature mode reduces the risk of decomposition of the thermally unstable chemical compounds being extracted and reduces volatility of the organic solvents being used. The technology of the method does not demand a special laboratory glassware and expendables.

[Study on extraction of the total saponins of Chinese yam].

PubMed

Zhang, Min; Du, Lin; Huang, Gui-dong; Zhong, Xian-feng

2007-07-01

A method for the determination of total saponins of Chinese yam was established. The dioscin was used as a standard compound, the vanillin-perchloric acid as chromogenic agent and glacial acetic acid as solvent. The extraction technique of asponins from Chinese yam was studied by spectrometric method. Extracting temperature, extracting time, ethanol concentration and the ratio of raw material and water were selected as four factors to design the orthogonal test, and the optical condition of extraction was obtained. The results showed that the optical condition of extraction was as following: extracting temperature 60 degrees C, extracting time 6 h, ethanol concetration 80%, and the ratio of raw material and water 1:8.

Measurement of technetium-99 in Marshall Islands soil samples by ICP-MS

PubMed

Tagami; Uchida; Hamilton; Robison

2000-07-01

Extraction techniques for recovery of technetium-99 (99Tc) for Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (MI) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for 99Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the 99Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The 99Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq g(-1) dry weight (dw). The limit of detection for 99Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq g(-1) dw under standard operating conditions.

Phospholipid Fatty Acid Analysis: Past, Present and Future

NASA Astrophysics Data System (ADS)

Findlay, R. H.

2008-12-01

With their 1980 publication, Bobbie and White initiated the use of phospholipid fatty acids for the study of microbial communities. This method, integrated with a previously published biomass assay based on the colorimetric detection of orthophosphate liberated from phospholipids, provided the first quantitative method for determining microbial community structure. The method is based on a quantitative extraction of lipids from the sample matrix, isolation of the phospholipids, conversion of the phospholipid fatty acids to their corresponding fatty acid methyl esters (known by the acronym FAME) and the separation, identification and quantification of the FAME by gas chromatography. Early laboratory and field samples focused on correlating individual fatty acids to particular groups of microorganisms. Subsequent improvements to the methodology include reduced solvent volumes for extractions, improved sensitivity in the detection of orthophosphate and the use of solid phase extraction technology. Improvements in the field of gas chromatography also increased accessibility of the technique and it has been widely applied to water, sediment, soil and aerosol samples. Whole cell fatty acid analysis, a related but not equal technique, is currently used for phenotypic characterization in bacterial species descriptions and is the basis for a commercial, rapid bacterial identification system. In the early 1990ês application of multivariate statistical analysis, first cluster analysis and then principal component analysis, further improved the usefulness of the technique and allowed the development of a functional group approach to interpretation of phospholipid fatty acid profiles. Statistical techniques currently applied to the analysis of phospholipid fatty acid profiles include constrained ordinations and neutral networks. Using redundancy analysis, a form of constrained ordination, we have recently shown that both cation concentration and dissolved organic matter (DOM) quality are determinates of microbial community structure in forested headwater streams. One of the most exciting recent developments in phospholipid fatty acid analysis is the application of compound specific stable isotope analysis. We are currently applying this technique to stream sediments to help determine which microorganisms are involved in the initial processing of DOM and the technique promises to be a useful tool for assigning ecological function to microbial populations.

Lipids and Fatty Acids in Algae: Extraction, Fractionation into Lipid Classes, and Analysis by Gas Chromatography Coupled with Flame Ionization Detector (GC-FID).

PubMed

Guihéneuf, Freddy; Schmid, Matthias; Stengel, Dagmar B

2015-01-01

Despite the number of biochemical studies exploring algal lipids and fatty acid biosynthesis pathways and profiles, analytical methods used by phycologists for this purpose are often diverse and incompletely described. Potential confusion and potential variability of the results between studies can therefore occur due to change of protocols for lipid extraction and fractionation, as well as fatty acid methyl esters (FAME) preparation before gas chromatography (GC) analyses. Here, we describe a step-by-step procedure for the profiling of neutral and polar lipids using techniques such as solid-liquid extraction (SLE), thin-layer chromatography (TLC), and gas chromatography coupled with flame ionization detector (GC-FID). As an example, in this protocol chapter, analyses of neutral and polar lipids from the marine microalga Pavlova lutheri (an EPA/DHA-rich haptophyte) will be outlined to describe the distribution of fatty acid residues within its major lipid classes. This method has been proven to be a reliable technique to assess changes in lipid and fatty acid profiles in several other microalgal species and seaweeds.

Αntioxidant activity of Cynara scolymus L. and Cynara cardunculus L. extracts obtained by different extraction techniques.

PubMed

Kollia, Eleni; Markaki, Panagiota; Zoumpoulakis, Panagiotis; Proestos, Charalampos

2017-05-01

Extracts of different parts (heads, bracts and stems) of Cynara cardunculus L. (cardoon) and Cynara scolymus L. (globe artichoke), obtained by two different extraction techniques (Ultrasound-Assisted Extraction (UAE) and classical extraction (CE)) were examined and compared for their total phenolic content (TPC) and their antioxidant activity. Moreover, infusions of the plant's parts were also analysed and compared to aforementioned samples. Results showed that cardoon's heads extract (obtained by Ultrasound-Assisted Extraction) displayed the highest TPC values (1.57 mg Gallic Acid Equivalents (GAE) g -1 fresh weight (fw)), the highest DPPH • scavenging activity (IC50; 0.91 mg ml -1 ) and the highest ABTS •+ radical scavenging capacity (2.08 mg Trolox Equivalents (TE) g -1 fw) compared to infusions and other extracts studied. Moreover, Ultrasound-Assisted Extraction technique proved to be more appropriate and effective for the extraction of antiradical and phenolic compounds.

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.

An efficient chemical analysis of phenolic acids and flavonoids in raw propolis by microwave-assisted extraction combined with high-performance liquid chromatography using the fused-core technology.

PubMed

Pellati, Federica; Prencipe, Francesco Pio; Bertelli, Davide; Benvenuti, Stefania

2013-01-01

A closed-vessel microwave-assisted extraction (MAE) technique was optimized for the first time for the extraction of polyphenols from raw propolis. The results obtained by means of response surface experimental design methodology showed that the best global response was reached when the extraction temperature was set at 106 °C, the solvent composition close to EtOH-H2O 80:20 (v/v), with an extraction time of 15 min. In comparison with other techniques, such as maceration, heat reflux extraction (HRE) and ultrasound-assisted extraction (UAE), the extraction with MAE was improved by shorter extraction time and lower volume of solvent needed. The HPLC analyses of propolis extracts were carried out on a fused-core Ascentis Express C18 column (150 mm × 3.0 mm I.D., 2.7 μm), with a gradient mobile phase composed by 0.1% formic acid in water and acetonitrile. Detection was performed by DAD and MS. The method validation indicated that the correlation coefficients were >0.999; the limit of detection was in the range 0.5-0.8 μg/ml for phenolic acids and 1.2-3.0 μg/ml for flavonoids; the recovery range was 95.3-98.1% for phenolic acids and 94.1-101.3% for flavonoids; the intra- and inter-day %RSD values for retention times and peak areas were ≤ 0.3 and 2.2%, respectively. The quali- and quantitative analysis of polyphenols in Italian samples of raw propolis was performed with the validated method. Total phenolic acids ranged from 5.0 to 120.8 mg/g and total flavonoids from 2.5 to 168.0mg/g. The proposed MAE procedure and HPLC method can be considered reliable and useful tools for the comprehensive multi-component analysis of polyphenols in propolis extracts to be used in apitherapy. Copyright © 2013 Elsevier B.V. All rights reserved.

Recovery of Fuel-Precursor Lipids from Oleaginous Yeast

DOE PAGES

Kruger, Jacob S.; Cleveland, Nicholas S.; Yeap, Rou Yi; ...

2018-01-24

Bio-derived lipids offer a potentially promising intermediate to displace petroleum-derived diesel. One of the key challenges for the production of lipids via microbial cell mass is that these products are stored intracellularly and must be extracted and recovered efficiently and economically. Thus, improved methods of cell lysis and lipid extraction are needed. In this study, we examine lipid extraction from wet oleaginous yeast in combination with seven different cell lysis approaches encompassing both physical and chemical techniques (high-pressure homogenization, microwave and conventional thermal treatments, bead beating, acid, base, and enzymatic treatments) to facilitate lipid extraction from a model oleaginous yeastmore » strain, Lipomyces starkeyi. Of the seven techniques investigated, acid treatment led to the highest lipid recovery yields. Further exploration of acid treatment and integration with an economic model revealed that treatment at 170 degrees C for 60 min at 1 wt% H 2SO 4 and 8 wt% yeast solids represents a viable option for both lipid recovery yield and process economics, enabling experimental lipid recovery yields of 88.5-93.0% to be achieved at a corresponding estimated minimum fuel selling price (MFSP) of $5.13-$5.61/gallon of gasoline equivalent (GGE). The same acid treatment conditions applied to two other strains of oleaginous yeast (Cutaneotrichosporon curvatus and Rhodotorula toruloides) resulted in similar lipid recovery yields. In pretreatment experiments scaled up to 300 mL, slightly lower temperatures or shorter pretreatment times, along with higher yeast solids loading, resulted in higher lipid yields than the conditions identified from the small-scale runs. Two replicate runs carried out at 170 degrees C for 30 min using 1 wt% H2SO4 and 19 wt% yeast solids achieved an average lipid recovery of 96.1% at a corresponding estimated MFSP of $4.89/GGE. In all cases, the lipids are primarily triglycerides and free fatty acids comprised mainly of palmitic, stearic, and oleic acids, with smaller fractions of polar lipids. The fatty acid composition of the lipids extracted from the wet treated cell mass is the same as that in freeze-dried whole oleaginous yeast cell mass, suggesting the acid treatment renders all lipids extractable. This work demonstrates that acid treatment is a robust and effective cell lysis technique in a microbial lipid-based biofuel scenario and provides a baseline for further scale-up and process integration.« less

Recovery of Fuel-Precursor Lipids from Oleaginous Yeast

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

Kruger, Jacob S.; Cleveland, Nicholas S.; Yeap, Rou Yi

Bio-derived lipids offer a potentially promising intermediate to displace petroleum-derived diesel. One of the key challenges for the production of lipids via microbial cell mass is that these products are stored intracellularly and must be extracted and recovered efficiently and economically. Thus, improved methods of cell lysis and lipid extraction are needed. In this study, we examine lipid extraction from wet oleaginous yeast in combination with seven different cell lysis approaches encompassing both physical and chemical techniques (high-pressure homogenization, microwave and conventional thermal treatments, bead beating, acid, base, and enzymatic treatments) to facilitate lipid extraction from a model oleaginous yeastmore » strain, Lipomyces starkeyi. Of the seven techniques investigated, acid treatment led to the highest lipid recovery yields. Further exploration of acid treatment and integration with an economic model revealed that treatment at 170 degrees C for 60 min at 1 wt% H 2SO 4 and 8 wt% yeast solids represents a viable option for both lipid recovery yield and process economics, enabling experimental lipid recovery yields of 88.5-93.0% to be achieved at a corresponding estimated minimum fuel selling price (MFSP) of $5.13-$5.61/gallon of gasoline equivalent (GGE). The same acid treatment conditions applied to two other strains of oleaginous yeast (Cutaneotrichosporon curvatus and Rhodotorula toruloides) resulted in similar lipid recovery yields. In pretreatment experiments scaled up to 300 mL, slightly lower temperatures or shorter pretreatment times, along with higher yeast solids loading, resulted in higher lipid yields than the conditions identified from the small-scale runs. Two replicate runs carried out at 170 degrees C for 30 min using 1 wt% H2SO4 and 19 wt% yeast solids achieved an average lipid recovery of 96.1% at a corresponding estimated MFSP of $4.89/GGE. In all cases, the lipids are primarily triglycerides and free fatty acids comprised mainly of palmitic, stearic, and oleic acids, with smaller fractions of polar lipids. The fatty acid composition of the lipids extracted from the wet treated cell mass is the same as that in freeze-dried whole oleaginous yeast cell mass, suggesting the acid treatment renders all lipids extractable. This work demonstrates that acid treatment is a robust and effective cell lysis technique in a microbial lipid-based biofuel scenario and provides a baseline for further scale-up and process integration.« less

Uranium extraction by complexation with siderophores

NASA Astrophysics Data System (ADS)

Bahamonde Castro, Cristina

One of the major concerns of energy production is the environmental impact associated with the extraction of natural resources. Nuclear energy fuel is obtained from uranium, an abundant and naturally occurring element in the environment, but the currently used techniques for uranium extraction leave either a significant fingerprint (open pit mines) or a chemical residue that alters the pH of the environment (acid or alkali leaching). It is therefore clear that a new and greener approach to uranium extraction is needed. Bioleaching is one potential alternative. In bioleaching, complexants naturally produced from fungi or bacteria may be used to extract the uranium. In the following research, the siderophore enterobactin, which is naturally produced by bacteria to extract and solubilize iron from the environment, is evaluated to determine its potential for complexing with uranium. To determine whether enterobactin could be used for uranium extraction, its acid dissociation and its binding strength with the metal of interest must be determined. Due to the complexity of working with radioactive materials, lanthanides were used as analogs for uranium. In addition, polyprotic acids were used as structural and chemical analogs for the siderophore during method development. To evaluate the acid dissociation of enterobactin and the subsequent binding constants with lanthanides, three different analytical techniques were studied including: potentiometric titration, UltraViolet Visible (UV-Vis) spectrophotometry and Isothermal Titration Calorimetry (ITC). After evaluation of three techniques, a combination of ITC and potentiometric titrations was deemed to be the most viable way for studying the siderophore of interest. The results obtained from these studies corroborate the ideal pH range for enterobactin complexation to the lanthanide of interest and pave the way for determining the strength of complexation relative to other naturally occurring metals. Ultimately, this fundamental research enhances our current understanding of heavy metal complexation to naturally occurring complexants, which may enhance the metals mobility in the environment or potentially be used as a greener alternative in uranium extraction or remediation.

Extraction of Pentachlorophenol from Soils using Environmentally Benign Lactic Acid Solutions

EPA Science Inventory

Soil contamination with pentachlorophenol (PCP) is widespread across the globe. Soil washing/extraction is a common technique to remove this compound. Several soil washing/extraction solutions have been used but a majority of them have the problem of persistence in the environmen...

A review on methods of regeneration of spent pickling solutions from steel processing.

PubMed

Regel-Rosocka, Magdalena

2010-05-15

The review presents various techniques of regeneration of spent pickling solutions, including the methods with acid recovery, such as diffusion dialysis, electrodialysis, membrane electrolysis and membrane distillation, evaporation, precipitation and spray roasting as well as those with acid and metal recovery: ion exchange, retardation, crystallization solvent and membrane extraction. Advantages and disadvantages of the techniques are presented, discussed and confronted with the best available techniques requirements. Most of the methods presented meet the BAT requirements. The best available techniques are electrodialysis, diffusion dialysis and crystallization; however, in practice spray roasting and retardation/ion-exchange are applied most frequently for spent pickling solution regeneration. As "waiting for their chance" solvent extraction, non-dispersive solvent extraction and membrane distillation should be indicated because they are well investigated and developed. Environmental and economic benefits of the methods presented in the review depend on the cost of chemicals and wastewater treatment, legislative regulations and cost of modernization of existing technologies or implementation of new ones. Copyright (c) 2009 Elsevier B.V. All rights reserved.

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.

Antioxidant activities and phenolics profiling of different parts of Carica papaya by LCMS-MS.

PubMed

Zunjar, V; Mammen, D; Trivedi, B M

2015-01-01

This article deals with the comparison of the antioxidant activity of aqueous extracts of various parts of Carica papaya L. The evaluation of total phenolic content and total flavonoid content revealed high antioxidant potential of the seeds and fruits. The free radical-scavenging potential of the aqueous extracts indicated the seeds to have better DPPH-scavenging activity than fruits. The results were augmented by the FRAP activity as well. The phenolics present in the extracts were separated and identified as 5-hydroxy feruloyl quinic acid, acetyl p-coumaryl quinic acid, quercetin-3-O-rhamnoside, syringic acid hexoside, 5-hydroxy caffeic quinic acid, peonidin-3-O-glucoside, sinapic acid-O-hexoside, cyaniding-3-O-glucose and methyl feruloyl glycoside by LCMS-MS technique.

[Relation between distribution of phosphorus form in the sediment of typical urban shallow lakes and eutrophication].

PubMed

Wang, Chao; Zou, Li-Min; Wang, Pei-Fang; Lin, Zhi-Ping

2008-05-01

The forms of phosphorus in the surface sediments were extracted and determined sequentially with ethylene dinitrilo tetracetic acid (EDTA) technique in three urban shallow lakes: Lake Xuanwu, Lake Mochou and Lake Daming. The results showed that the iron and calcium-bound phosphate, about accounting for 80%, were the main forms of total phosphorus. The contents of iron bound phosphate in Lake Xuanwu and Lake Mochou were higher than that of Lake Daming, reaching 30%-40%. The organic phosphorus existed mainly in the form of alkali extractable phosphorus, while the contents of acid extractable organic phosphorus were low. However, the proportion of acid extractable organic phosphorus to the total phosphorus can indicate the degree of lake eutrophication.

Bioassay-guided supercritical fluid extraction of cyclooxygenase-2 inhibiting substances in Plantago major L.

PubMed

Stenholm, A; Göransson, U; Bohlin, L

2013-02-01

Selective extraction of plant materials is advantageous for obtaining extracts enriched with desired constituents, thereby reducing the need for subsequent chromatography purification. Such compounds include three cyclooxygenase-2 (COX-2) inhibitory substances in Plantago major L. targeted in this investigation: α-linolenic acid (α-LNA) (18:3 ω-3) and the triterpenic acids ursolic acid and oleanolic acid. To investigate the scope for tuning the selectivity of supercritical fluid extraction (SFE) using bioassay guidance, and Soxhlet extraction with dichloromethane as solvent as a reference technique, to optimise yields of these substances. Extraction parameters were varied to optimise extracts' COX-2/COX-1 inhibitory effect ratios. The crude extracts were purified initially using a solid phase extraction (SPE) clean-up procedure and the target compounds were identified with GC-MS, LC-ESI-MS and LC-ESI-MS² using GC-FID for quantification. α-LNA was preferentially extracted in dynamic mode using unmodified carbon dioxide at 40°C and 172 bar, at a 0.04% (w/w) yield with a COX-2/COX-1 inhibitory effect ratio of 1.5. Ursolic and oleanolic acids were dynamically extracted at 0.25% and 0.06% yields, respectively, with no traces of (α-LNA) and a COX-2/COX-1-inhibitory effect ratio of 1.1 using 10% (v/v) ethanol as polar modifier at 75°C and 483 bar. The Soxhlet extracts had ursolic acid, oleanolic acid and αLNA yields up to 1.36%, 0.34% and 0.15%, respectively, with a COX-2/COX-1 inhibitory effect ratio of 1.2. The target substances can be extracted selectively by bioassay guided optimisation of SFE conditions. Copyright © 2012 John Wiley & Sons, Ltd.

Mathematical modelling for extraction of oil from Dracocephalum kotschyi seeds in supercritical carbon dioxide.

PubMed

Sodeifian, Gholamhossein; Sajadian, Seyed Ali; Honarvar, Bizhan

2018-04-01

Extraction of oil from Dracocephalum kotschyi Boiss seeds using supercritical carbon dioxide was designed using central composite design to evaluate the effect of various operating parameters including pressure, temperature, particle size and extraction time on the oil yield. Maximum extraction yield predicted from response surface method was 71.53% under the process conditions with pressure of 220 bar, temperature of 35 °C, particle diameter of 0.61 mm and extraction time of 130 min. Furthermore, broken and intact cells model was utilised to consider mass transfer kinetics of extracted natural materials. The results revealed that the model had a good agreement with the experimental data. The oil samples obtained via supercritical and solvent extraction methods were analysed by gas chromatography. The most abundant acid was linolenic acid. The results analysis showed that there was no significant difference between the fatty acid contents of the oils obtained by the supercritical and solvent extraction techniques.

Lipophilic ternary complexes in liquid-liquid extraction of trivalent lanthanides

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

Lumetta, Gregg J.; Levitskaia, Tatiana G.; Latesky, Stanley

2012-03-01

The formation of ternary complexes between lanthanide ions [Nd(III) or Eu(III)], octyl(phenyl)-N,N-diisobutyl-carbamoylmethylphosphine oxide (CMPO), and bis-(2-ethylhexyl)phosphoric acid (HDEHP) was probed by liquid-liquid extraction and spectroscopic techniques. Equilibrium modeling of data for the extraction of Nd(III) or Eu(III) from lactic acid media into n-dodecane solutions of CMPO and HDEHP indicates the predominant extracted species are of the type [Ln(AHA){sub 2}(A)] and [Ln(CMPO)(AHA){sub 2}(A)], where Ln = Nd or Eu and A represents the DEHP{sup -} anion. FTIR (for both Eu and Nd) and visible spectrophotometry (in the case of Nd) indicate the formation of the [Ln(CMPO)(A){sup 3}] complexes when CMPO ismore » added to n-dodecane solutions of the LnA{sub 3} compounds. Both techniques indicate a stronger propensity of CMPO to complex Nd(III) versus Eu(III).« less

Comparison of hot hydroxylamine hydrochloride and oxalic acid leaching of stream sediment and coated rock samples as anomaly enhancement techniques

USGS Publications Warehouse

Filipek, L.H.; Chao, T.T.; Theobald, P.K.

1982-01-01

A hot hydroxylamine hydrochloride (H-Hxl) extraction in 25% acetic acid is compared with the commonly used oxalic acid extraction as a method of anomaly enhancement for Cu and Zn in samples from two very different metal deposits and climatic environments. Results obtained on minus-80-mesh stream sediments from an area near the Magruder massive sulfide deposit in Lincoln County, Georgia, where the climate is humid subtropical, indicate that H-Hxl enhances the anomaly for Cu by a factor of 2 and for Zn by a factor of 1.5, compared to the oxalic method. Analyses of Fe oxide-coated rock samples from outcrops overlying the North Silver Bell porphyry copper deposit near Tucson, Arizona, where the climate is semi-arid to arid, indicate that both techniques effectively outline the zones of hydrothermal alteration. The H-Hxl extraction can also perform well in high-carbonate or high-clay environments, where other workers have suggested that oxalic acid is not very effective. Therefore, the H-Hxl method is recommended for general exploration use. ?? 1982.

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

Selective extraction and determination of chlorogenic acids as combined quality markers in herbal medicines using molecularly imprinted polymers based on a mimic template.

PubMed

Ji, Wenhua; Zhang, Mingming; Yan, Huijiao; Zhao, Hengqiang; Mu, Yan; Guo, Lanping; Wang, Xiao

2017-12-01

We describe a solid-phase extraction adsorbent based on molecularly imprinted polymers (MIPs), prepared with use of a mimic template. The MIPs were used for the selective extraction and determination of three chlorogenic acids as combined quality markers for Lonicera japonica and Lianhua qingwen granules. The morphologies and surface groups of the MIPs were assessed by scanning electron microscopy, Brunauer-Emmett-Teller surface area analysis, and Fourier transform infrared spectroscopy. The adsorption isotherms, kinetics, and selectivity of the MIPs were systematically compared with those of non-molecularly imprinted polymers. The MIPs showed high selectivity toward three structurally similar chlorogenic acids (chlorogenic acid, cryptochlorogenic acid, and neochlorogenic acid). A procedure using molecularly imprinted solid-phase extraction coupled with high-performance liquid chromatography was established for the determination of three chlorogenic acids from Lonicera japonica and Lianhua qingwen granules. The recoveries of the chlorogenic acids ranged from 93.1% to 101.4%. The limits of detection and limits of quantification for the three chlorogenic acids were 0.003 mg g -1 and 0.01 mg g -1 , respectively. The newly developed method is thus a promising technique for the enrichment and determination of chlorogenic acids from herbal medicines. Graphical Abstract Mimic molecularly imprinted polymers for the selective extraction of chlorogenic acids.

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

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.

A Teaching Laboratory for Comprehensive Lipid Characterization from Food Samples

ERIC Educational Resources Information Center

Bendinskas, Kestutis; Weber, Benjamin; Nsouli, Tamara; Nguyen, Hoangvy V.; Joyce, Carolyn; Niri, Vadoud; Jaskolla, Thorsten W.

2014-01-01

Traditional and state-of-the-art techniques were combined to probe for various lipid classes from egg yolk and avocado qualitatively and quantitatively. A total lipid extract was isolated using liquid-liquid extraction. An aliquot of the total lipid extract was subjected to transesterification to form volatile fatty acid methyl esters suitable for…

Valuable natural products from marine and freshwater macroalgae obtained from supercritical fluid extracts.

PubMed

Messyasz, Beata; Michalak, Izabela; Łęska, Bogusława; Schroeder, Grzegorz; Górka, Bogusława; Korzeniowska, Karolina; Lipok, Jacek; Wieczorek, Piotr; Rój, Edward; Wilk, Radosław; Dobrzyńska-Inger, Agnieszka; Górecki, Henryk; Chojnacka, Katarzyna

2018-01-01

The biologically active compounds (fatty acids, pigments, phenolics, and flavonoid content) were studied in supercritical fluid extracts from the biomass of marine ( Ulva clathrata , Cladophora glomerata , Polysiphonia fucoides , and their multi-species mixture) and freshwater ( C. glomerata ) macroalgae. Different extraction techniques were used in order to compare differences in the biologically active compound composition of the macroalgal extracts. The results indicated that the saturated and unsaturated fatty acids ranged from C9:0 to C22:0. The analysis of differences in the composition of unsaturated to saturated fatty acids in extracts showed that palmitic acid (C16:0) and oleic acid (C18:1, n-9) reached the highest value not only in marine monospecies and multi-species biomass but also in the freshwater macroalga C. glomerata . When comparing the similarity between the concentration of fatty acids and the ratio of the concentration of unsaturated fatty acids to saturated in macroalgal extracts, we found small but not statistically significant variations in values between years (up to 10%). This is acceptable for applications as a stable raw material for industrial purposes. Significantly higher values of fatty acids, carotenoids, and chlorophylls were obtained in the case of SC-CO 2 extraction. The active ingredients of polyphenols, possessing antioxidant activity ranged from approximately 2-4%. Moreover, flavonoids represented less than 10% of the total content of polyphenolic compounds. The extraction efficiency of polyphenols was higher from a mixture of marine algae for the ultrasound-assisted extraction compared to freshwater. All these findings show that marine and freshwater macroalgae, as a raw material, have the optimal biologically active compounds composition for cosmetics.

Various extraction and analytical techniques for isolation and identification of secondary metabolites from Nigella sativa seeds.

PubMed

Liu, X; Abd El-Aty, A M; Shim, J-H

2011-10-01

Nigella sativa L. (black cumin), commonly known as black seed, is a member of the Ranunculaceae family. This seed is used as a natural remedy in many Middle Eastern and Far Eastern countries. Extracts prepared from N. sativa have, for centuries, been used for medical purposes. Thus far, the organic compounds in N. sativa, including alkaloids, steroids, carbohydrates, flavonoids, fatty acids, etc. have been fairly well characterized. Herein, we summarize some new extraction techniques, including microwave assisted extraction (MAE) and supercritical extraction techniques (SFE), in addition to the classical method of hydrodistillation (HD), which have been employed for isolation and various analytical techniques used for the identification of secondary metabolites in black seed. We believe that some compounds contained in N. sativa remain to be identified, and that high-throughput screening could help to identify new compounds. A study addressing environmentally-friendly techniques that have minimal or no environmental effects is currently underway in our laboratory.

Carbon footprint assessment of recycling technologies for rare earth elements: A case study of recycling yttrium and europium from phosphor.

PubMed

Hu, Allen H; Kuo, Chien-Hung; Huang, Lance H; Su, Chao-Chin

2017-02-01

Rare earth elements are key raw materials in high-technology industries. Mining activities and manufacturing processes of such industries have caused considerable environmental impacts, such as soil erosion, vegetation destruction, and various forms of pollution. Sustaining the long-term supply of rare earth elements is difficult because of the global shortage of rare earth resources. The diminishing supply of rare earth elements has attracted considerable concern because many industrialized countries regarded such elements as important strategic resources for economic growth. This study aims to explore the carbon footprints of yttrium and europium recovery techniques from phosphor. Two extraction recovery methods, namely, acid extraction and solvent extraction, were selected for the analysis and comparison of carbon footprints. The two following functional units were used: (1) the same phosphor amounts for specific Y and Eu recovery concentrations, and (2) the same phosphor amounts for extraction. For acid extraction method, two acidic solutions (H 2 SO 4 and HCl) were used at two different temperatures (60 and 90°C). For solvent extraction method, acid leaching was performed followed by ionic liquid extraction. Carbon footprints from acid and solvent extraction methods were estimated to be 10.1 and 10.6kgCO 2 eq, respectively. Comparison of the carbon emissions of the two extraction methods shows that the solvent extraction method has significantly higher extraction efficiency, even though acid extraction method has a lower carbon footprint. These results may be used to develop strategies for life cycle management of rare earth resources to realize sustainable usage. Copyright © 2016 Elsevier Ltd. All rights reserved.

Sequential cloud-point extraction for toxicological screening analysis of medicaments in human plasma by high pressure liquid chromatography with diode array detector.

PubMed

Madej, Katarzyna; Persona, Karolina; Wandas, Monika; Gomółka, Ewa

2013-10-18

A complex extraction system with the use of cloud-point extraction technique (CPE) was developed for sequential isolation of basic and acidic/neutral medicaments from human plasma/serum, screened by HPLC/DAD method. Eight model drugs (paracetamol, promazine, chlorpromazine, amitriptyline, salicyclic acid, opipramol, alprazolam and carbamazepine) were chosen for the study of optimal CPE conditions. The CPE technique consists in partition of an aqueous sample with addition of a surfactant into two phases: micelle-rich phase with the isolated compounds and water phase containing a surfactant below the critical micellar concentration, mainly under influence of temperature change. The proposed extraction system consists of two chief steps: isolation of basic compounds (from pH 12) and then isolation of acidic/neutral compounds (from pH 6) using surfactant Triton X-114 as the extraction medium. Extraction recovery varied from 25.2 to 107.9% with intra-day and inter-day precision (RSD %) ranged 0.88-1087 and 5.32-17.96, respectively. The limits of detection for the studied medicaments at λ 254nm corresponded to therapeutic or low toxic plasma concentration levels. Usefulness of the proposed CPE-HPLC/DAD method for toxicological drug screening was tested via its application to analysis of two serum samples taken from patients suspected of drug overdosing. Published by Elsevier B.V.

Supercritical fluid extraction of phenolic compounds and antioxidants from grape (Vitis labrusca B.) seeds.

PubMed

Ghafoor, Kashif; Al-Juhaimi, Fahad Y; Choi, Yong Hee

2012-12-01

Supercritical fluid extraction (SFE) technique was applied and optimized for temperature, CO₂ pressure and ethanol (modifier) concentration using orthogonal array design and response surface methodology for the extract yield, total phenols and antioxidants from grape (Vitis labrusca B.) seeds. Effects of extraction temperature and pressure were found to be significant for all these response variables in SFE process. Optimum SFE conditions (44 ~ 46 °C temperature and 153 ~ 161 bar CO₂ pressure) along with ethanol (<7 %) as modifier, for the maximum predicted values of extract yield (12.09 %), total phenols (2.41 mg GAE/ml) and antioxidants (7.08 mg AAE/ml), were used to obtain extracts from grape seeds. The predicted values matched well with the experimental values (12.32 % extract yield, 2.45 mg GAE/ml total phenols and 7.08 mg AAE/ml antioxidants) obtained at optimum SFE conditions. The antiradical assay showed that SFE extracts of grape seeds can scavenge more than 85 % of 1, 1-diphenyl-2-picrylhydrazyl (DPPH) radicals. The grape seeds extracts were also analyzed for hydroxybenzoic acids which included gallic acid (1.21 ~ 3.84 μg/ml), protocatechuic acid (3.57 ~ 11.78 μg/ml) and p-hydroxybenzoic acid (206.72 ~ 688.18 μg/ml).

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.

Preparation of a Ammonia-Treated Lac Dye and Structure Elucidation of Its Main Component.

PubMed

Nishizaki, Yuzo; Ishizuki, Kyoko; Akiyama, Hiroshi; Tada, Atsuko; Sugimoto, Naoki; Sato, Kyoko

2016-01-01

Lac dye and cochineal extract contain laccaic acids and carminic acid as the main pigments, respectively. Both laccaic acids and carminic acid are anthraquinone derivatives. 4-Aminocarminic acid (acid-stable carmine), an illegal colorant, has been detected in several processed foods. 4-Aminocarminic acid is obtained by heating cochineal extract (carminic acid) in ammonia solution. We attempted to prepare ammonia-treated lac dye and to identify the structures of the main pigment components. Ammonia-treated lac dye showed acid stability similar to that of 4-aminocarminic acid. The structures of the main pigments in ammonia-treated lac dye were analyzed using LC/MS. One of the main pigments was isolated and identified as 4-aminolaccaic acid C using various NMR techniques, including 2D-INADEQUATE. These results indicated that ammonia-treatment of lac dye results in the generation of 4-aminolaccaic acids.

Development of a nucleic Acid extraction procedure for simultaneous recovery of DNA and RNA from diverse microbes in water.

PubMed

Hill, Vincent R; Narayanan, Jothikumar; Gallen, Rachel R; Ferdinand, Karen L; Cromeans, Theresa; Vinjé, Jan

2015-05-26

Drinking and environmental water samples contain a diverse array of constituents that can interfere with molecular testing techniques, especially when large volumes of water are concentrated to the small volumes needed for effective molecular analysis. In this study, a suite of enteric viruses, bacteria, and protozoan parasites were seeded into concentrated source water and finished drinking water samples, in order to investigate the relative performance of nucleic acid extraction techniques for molecular testing. Real-time PCR and reverse transcription-PCR crossing threshold (CT) values were used as the metrics for evaluating relative performance. Experimental results were used to develop a guanidinium isothiocyanate-based lysis buffer (UNEX buffer) that enabled effective simultaneous extraction and recovery of DNA and RNA from the suite of study microbes. Procedures for bead beating, nucleic acid purification, and PCR facilitation were also developed and integrated in the protocol. The final lysis buffer and sample preparation procedure was found to be effective for a panel of drinking water and source water concentrates when compared to commercial nucleic acid extraction kits. The UNEX buffer-based extraction protocol enabled PCR detection of six study microbes, in 100 L finished water samples from four drinking water treatment facilities, within three CT values (i.e., within 90% difference) of the reagent-grade water control. The results from this study indicate that this newly formulated lysis buffer and sample preparation procedure can be useful for standardized molecular testing of drinking and environmental waters.

Development of a Nucleic Acid Extraction Procedure for Simultaneous Recovery of DNA and RNA from Diverse Microbes in Water

PubMed Central

Hill, Vincent R.; Narayanan, Jothikumar; Gallen, Rachel R.; Ferdinand, Karen L.; Cromeans, Theresa; Vinjé, Jan

2015-01-01

Drinking and environmental water samples contain a diverse array of constituents that can interfere with molecular testing techniques, especially when large volumes of water are concentrated to the small volumes needed for effective molecular analysis. In this study, a suite of enteric viruses, bacteria, and protozoan parasites were seeded into concentrated source water and finished drinking water samples, in order to investigate the relative performance of nucleic acid extraction techniques for molecular testing. Real-time PCR and reverse transcription-PCR crossing threshold (CT) values were used as the metrics for evaluating relative performance. Experimental results were used to develop a guanidinium isothiocyanate-based lysis buffer (UNEX buffer) that enabled effective simultaneous extraction and recovery of DNA and RNA from the suite of study microbes. Procedures for bead beating, nucleic acid purification, and PCR facilitation were also developed and integrated in the protocol. The final lysis buffer and sample preparation procedure was found to be effective for a panel of drinking water and source water concentrates when compared to commercial nucleic acid extraction kits. The UNEX buffer-based extraction protocol enabled PCR detection of six study microbes, in 100 L finished water samples from four drinking water treatment facilities, within three CT values (i.e., within 90% difference) of the reagent-grade water control. The results from this study indicate that this newly formulated lysis buffer and sample preparation procedure can be useful for standardized molecular testing of drinking and environmental waters. PMID:26016775

Pulverizing processes affect the chemical quality and thermal property of black, white, and green pepper (Piper nigrum L.).

PubMed

Liu, Hong; Zheng, Jie; Liu, Pengzhan; Zeng, Fankui

2018-06-01

In this study, the effects of different pulverizing methods on the chemical attributes and thermal properties of black, white and green pepper were evaluated. Cryogenic grinding minimally damaged the lipid, moisture, crude protein, starch, non-volatile ether extract, piperine, essential oil and the typical pepper essential oil compounds of the spices. The pulverizing methods and storage significantly affected the compositions of the fatty acid in the peppers, except for palmitic acid and lignoceric acid. The amino acid contents and the thermo-gravimetric analysis curve were hardly influenced by the grinding techniques. The use of cryogenic grinding to prepare pepper ensured the highest quality of pepper products. Regardless of grinding technique, the values of moisture, piperine, unsaturated fatty acids, essential oil, monoterpenes, and the absolute concentrations of typical pepper essential oil constituents (except caryophyllene oxide) decreased, whereas the amino acid, lipid, protein, starch, and non-volatile ether extract content as well as the thermal properties were insignificantly changed after storage at 4 °C for 6 months.

[Application of microwave technology in extraction process of Guizhi Fuling capsule].

PubMed

Wang, Zheng-kuan; Zhou, Mao; Liu, Yuan; Bi, Yu-an; Wang, Zhen-zhong; Xiao, Wei

2015-06-01

In this paper, optimization of the conditions of microwave technique in extraction process of Guizhi Fuling capsule in the condition of a pilot scale was carried out. First of all, through the single factor experiment investigation of various factors, the overall impact tendency and range of each factor were determined. Secondly, L9 (3(4)) orthogonal test optimization was used, and the contents of gallic acid in liquid, paeoniflorin, benzoic acid, cinnamic acid, benzoyl paeoniflorin, amygdalin of the liquid medicine were detected. The extraction rate and comprehensive evaluation were calculated with the extraction effect, as the judgment basis. Theoptimum extraction process of Guizhi Fuling capsule by microwave technology was as follows: the ratio of liquid to solid was 6: 1 added to drinking water, the microwave power was 6 kW, extraction time was 20 min for 3 times. The process of the three batch of amplification through verification, the results are stable, and compared with conventional water extraction has the advantages of energy saving, time saving, high efficiency advantages. The above results show the optimum extracting technology of high efficiency, stable and feasible.

Protocol for Future Amino Acid Analyses of Samples Returned by the Stardust Mission

NASA Technical Reports Server (NTRS)

Glavin, D. P.; Doty, J. H., III; Matrajt, G.; Dworkin, J. P.

2006-01-01

We have demonstrated that LC-ToF-MS coupled with UV fluorescence detection is a powerful tool for the detection of amino acids in meteorite extracts. Using this new analytical technique we were able to identify the extraterrestrial amino acid AIB extracted from fifteen 20 micron sized Murchison meteorite grains. We found that the amino acid contamination levels in Stardust aerogels was much lower than the levels observed in the Murchison meteorite. In addition, the alpha-dialkyl amino acids AIB and isovaline which are the most abundant amino acids in Murchison were not detected in the aerogel above blank levels. We are currently integrating LIF detection capability to our existing nanoflow LC-ToF-MS for enhanced sensitivity required for the analysis of amino acids in Stardust samples.

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.

Determination of caffeoylquinic acids in feed and related products by focused ultrasound solid-liquid extraction and ultra-high performance liquid chromatography-mass spectrometry.

PubMed

Tena, M T; Martínez-Moral, M P; Cardozo, P W

2015-06-26

A method to determine caffeoylquinic acids (CQAs) in three sources (herbal extract, feed additive and finished feed) using for the first time focused ultrasound solid-liquid extraction (FUSLE) followed by ultra-high performance liquid chromatography (UPLC) coupled to quadrupole-time of flight mass spectrometry is presented. Pressurized liquid extraction (PLE) was also tested as extraction technique but it was discarded because cynarin was not stable under temperature values used in PLE. The separation of the CQAs isomers was carried out in only seven minutes. FUSLE variables such as extraction solvent, power and time were optimized by a central composite design. Under optimal conditions, FUSLE extraction was performed with 8mL of an 83:17 methanol-water mixture for 30s at a power of 60%. Only two extraction steps were found necessary to recover analytes quantitatively. Sensitivity, linearity, accuracy and precision were established. Matrix effect was studied for each type of sample. It was not detected for mono-CQAs, whereas the cynarin signal was strongly decreased due to ionization suppression in presence of matrix components; so the quantification by standard addition was mandatory for the determination of di-caffeoylquinic acids. Finally, the method was applied to the analysis of herbal extracts, feed additives and finished feed. In all samples, chlorogenic acid was the predominant CQA, followed by criptochlorogenic acid, neochlorogenic acid and cynarin. The method allows an efficient determination of chlorogenic acid with good recovery rates. Therefore, it may be used for screening of raw material and for process and quality control in feed manufacture. Copyright © 2015 Elsevier B.V. All rights reserved.

A technique for extracting Radiolaria from radiolarian cherts.

NASA Technical Reports Server (NTRS)

Pessagno, E. A., Jr.; Newport, R. L.

1972-01-01

Differential solution of Mesozoic radiolarian cherts with hydrofluoric acid has yielded well-preserved, matrix-free Radiolaria. This technique allows the full utilization of Radiolaria in interpreting the stratigraphy of ophiolite sequences and of other successions where cherts are prevalent.

Comparison of methods for extracting kafirin proteins from sorghum distillers dried grains with solubles.

PubMed

Wang, Ying; Tilley, Michael; Bean, Scott; Sun, X Susan; Wang, Donghai

2009-09-23

Use of coproducts generated during fermentation is important to the overall economics of biofuel production. The main coproduct from grain-based ethanol production is distillers dried grains with solubles (DDGS). High in protein, DDGS is a potential source of protein for many bioindustrial applications such as adhesives and resins. The objective of this research was to characterize the composition as well as chemical and physical properties of kafirin proteins from sorghum DDGS with various extraction methods including use of acetic acid, HCl-ethanol and NaOH-ethanol under reducing conditions. Extraction conditions affected purity and thermal properties of the extracted kafirin proteins. Extraction yields of 44.2, 24.2, and 56.8% were achieved by using acetic acid, HCl-ethanol and NaOH-ethanol, respectively. Acetic acid and NaOH-ethanol produced protein with higher purity than kafirins extracted with the HCl-ethanol protocol. The acetic acid extraction protocol produced protein with the highest purity, 98.9%. Several techniques were used to evaluate structural, molecular and thermal properties of kairin extracts. FTIR showed alpha-helix dominated in all three samples, with only a small portion of beta-sheet present. Electrophoresis results showed alpha(1), alpha(2) band and beta kafirins were present in all three extracts. Glass transition peaks of the extracts were shown by DSC to be approximately 230 degrees C. Kafirin degraded at 270-290 degrees C. Size exclusion chromatography revealed that the acetic acid and HCl-ethanol based extraction methods tended to extract more high molecular weight protein than the NaOH-ethanol based method. Reversed phase high-performance liquid chromatography showed that the gamma kafirins were found only in extracts from the NaOH-ethanol extraction method.

Metabolite profiling of polyphenols in the Tunisian plant Tamarix aphylla (L.) Karst.

PubMed

Mahfoudhi, Adel; Prencipe, Francesco Pio; Mighri, Zine; Pellati, Federica

2014-10-01

In this study, a detailed investigation on the composition of polyphenols of Tamarix aphylla (L.) Karst., consisting of phenolic acids and flavonoids, was carried out. In order to optimize the yield of secondary metabolites, three extraction techniques were compared, including dynamic maceration, ultrasound-assisted extraction and Soxhlet extraction. The latter technique provided the best results in terms of both recovery and selectivity, using ethyl acetate as extraction solvent for 2h. The analysis of T. aphylla polyphenols was performed by means of HPLC-UV/DAD, HPLC-ESI-MS and MS(2), using an ion trap mass analyzer. Phenolic acids and flavonoids were separated on an Ascentis C18 column (250mm×4.6mm I.D., 5μm), with a mobile phase composed of 0.1M formic acid in water and acetonitrile, under gradient elution. The proposed method was fully validated in agreement with ICH guidelines and then applied to the analysis of T. aphylla leaves and stems. A total of 14 phenolic compounds were characterized for the first time in this plant extracts by using UV, MS and MS(2) data. The amount of total phenolics was found to be 993.1±22.5μg/g in the leaves and 113.1±25.8μg/g in the stems, respectively. The most abundant constituents found in the leaves include ellagic acid (211.4±10.8μg/g), quercetin (125.7±4.7μg/g) and gallic acid (120.6±1.2μg/g), whereas those in the stems were ellagic acid (44.4±3.9μg/g), gallic acid (24.3±3.3μg/g) and kaempferol (16.3±1.6μg/g). The developed method can be considered a useful tool for the metabolite profiling of T. aphylla, which represents a potential source of bioactive compounds to be used in phytotherapy. Copyright © 2014 Elsevier B.V. All rights reserved.

Antisecretory Action of the Extract of the Aerial Parts of Eremomastax speciosa (Acanthaceae) Occurs through Antihistaminic and Anticholinergic Pathways.

PubMed

André Perfusion, Amang; Tan, Paul V; Ernestine, Nkwengoua; Barthélemy, Nyasse

2014-01-01

Objective. The objective of this study was to find out the possible antiulcer mechanism of action of Eremomastax speciosa. Method. Carbachol- and histamine-induced hypersecretion, associated with the pylorus ligation technique, were used in rats. Gastric mucosal ulceration, mucus production, pH, gastric volume, and acidity were measured. Results. Histamine and carbachol raised gastric acidity to 86.50 and 84.80 mEq/L, respectively, in the control rats, and the extracts (200 mg/kg) reduced gastric acidity to 34.60 and 39.00 mEq/L, respectively. Intraduodenal aqueous extract (400 mg/kg) in histamine- and carbachol-treated rats produced significant (P < 0.001) decreases in acid secretion to 28.50 and 28.80 mEq/L, respectively, and 100 percent inhibition of gastric ulceration. Augmented histamine-induced gastric acid secretion (90.20 mEq/L) was significantly reduced to 52.60 and 27.50 mEq/L by the 200 and 400 mg/kg doses of the aqueous extract, respectively. The extract significantly reduced (P < 0.001) the volume of gastric secretion and significantly increased mucus production. The ulcer inhibition potential of the extract significantly dropped to 25-44% (oral extract) and to 29-37% (duodenal extract) in carbachol/indomethacin-treated rats. Conclusion. The aqueous extract of E. speciosa has both cytoprotective and antisecretory effects. The antisecretory effect may involve a mechanism common to both cholinergic and histaminergic pathways.

Alternative oil extraction methods from Echium plantagineum L. seeds using advanced techniques and green solvents.

PubMed

Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

2018-04-01

The edible oil processing industry involves large losses of organic solvent into the atmosphere and long extraction times. In this work, fast and environmentally friendly alternatives for the production of echium oil using green solvents are proposed. Advanced extraction techniques such as Pressurized Liquid Extraction (PLE), Microwave Assisted Extraction (MAE) and Ultrasound Assisted Extraction (UAE) were evaluated to efficiently extract omega-3 rich oil from Echium plantagineum seeds. Extractions were performed with ethyl acetate, ethanol, water and ethanol:water to develop a hexane-free processing method. Optimal PLE conditions with ethanol at 150 °C during 10 min produced a very similar oil yield (31.2%) to Soxhlet using hexane for 8 h (31.3%). UAE optimized method with ethanol at mild conditions (55 °C) produced a high oil yield (29.1%). Consequently, advanced extraction techniques showed good lipid yields and furthermore, the produced echium oil had the same omega-3 fatty acid composition than traditionally extracted oil. Copyright © 2017 Elsevier Ltd. All rights reserved.

Pressurized liquid extraction and chemical characterization of safflower oil: A comparison between methods.

PubMed

Conte, Rogério; Gullich, Letícia M D; Bilibio, Denise; Zanella, Odivan; Bender, João P; Carniel, Naira; Priamo, Wagner L

2016-12-15

This work investigates the extraction process of safflower oil using pressurized ethanol, and compares the chemical composition obtained (in terms of fatty acids) with other extraction techniques. Soxhlet and Ultrasound showed maximum global yield of 36.53% and 30.41%, respectively (70°C and 240min). PLE presented maximum global yields of 25.62% (3mLmin(-1)), 19.94% (2mLmin(-1)) and 12.37% (1mLmin(-1)) at 40°C, 100bar and 60min. Palmitic acid showed the lower concentration in all experimental conditions (from 5.70% to 7.17%); Stearic and Linoleic acid presented intermediate concentrations (from 2.93% to 25.09% and 14.09% to 19.06%, respectively); Oleic acid showed higher composition (from 55.12% to 83.26%). Differences between percentages of fatty acids, depending on method were observed. Results may be applied to maximize global yields and select fatty acids, reducing the energetic costs and process time. Copyright © 2016 Elsevier Ltd. All rights reserved.

Chelant extraction of heavy metals from contaminated soils.

PubMed

Peters, R W

1999-04-23

The current state of the art regarding the use of chelating agents to extract heavy metal contaminants has been addressed. Results are presented for treatability studies conducted as worst-case and representative soils from Aberdeen Proving Ground's J-Field for extraction of copper (Cu), lead (Pb), and zinc (Zn). The particle size distribution characteristics of the soils determined from hydrometer tests are approximately 60% sand, 30% silt, and 10% clay. Sequential extractions were performed on the 'as-received' soils (worst case and representative) to determine the speciation of the metal forms. The technique speciates the heavy metal distribution into an easily extractable (exchangeable) form, carbonates, reducible oxides, organically-bound, and residual forms. The results indicated that most of the metals are in forms that are amenable to soil washing (i.e. exchangeable+carbonate+reducible oxides). The metals Cu, Pb, Zn, and Cr have greater than 70% of their distribution in forms amenable to soil washing techniques, while Cd, Mn, and Fe are somewhat less amenable to soil washing using chelant extraction. However, the concentrations of Cd and Mn are low in the contaminated soil. From the batch chelant extraction studies, ethylenediaminetetraacetic acid (EDTA), citric acid, and nitrilotriacetic acid (NTA) were all effective in removing copper, lead, and zinc from the J-Field soils. Due to NTA being a Class II carcinogen, it is not recommended for use in remediating contaminated soils. EDTA and citric acid appear to offer the greatest potential as chelating agents to use in soil washing the Aberdeen Proving Ground soils. The other chelating agents studied (gluconate, oxalate, Citranox, ammonium acetate, and phosphoric acid, along with pH-adjusted water) were generally ineffective in mobilizing the heavy metals from the soils. The chelant solution removes the heavy metals (Cd, Cu, Pb, Zn, Fe, Cr, As, and Hg) simultaneously. Using a multiple-stage batch extraction, the soil was successfully treated passing both the Toxicity Characteristics Leaching Procedure (TCLP) and EPA Total Extractable Metal Limit. The final residual Pb concentration was about 300 mg/kg, with a corresponding TCLP of 1.5 mg/l. Removal of the exchangeable and carbonate fractions for Cu and Zn was achieved during the first extraction stage, whereas it required two extraction stages for the same fractions for Pb. Removal of Pb, Cu, and Zn present as exchangeable, carbonates, and reducible oxides occurred between the fourth- and fifth-stage extractions. The overall removal of copper, lead, and zinc from the multiple-stage washing were 98.9%, 98.9%, and 97.2%, respectively. The concentration and operating conditions for the soil washing extractions were not necessarily optimized. If the conditions had been optimized and using a more representative Pb concentration (approximately 12000 mg/kg), it is likely that the TCLP and residual heavy metal soil concentrations could be achieved within two to three extractions. The results indicate that the J-Field contaminated soils can be successfully treated using a soil washing technique. Copyright 1999 Published by Elsevier Science B.V.

Extraction of High Quality DNA from Seized Moroccan Cannabis Resin (Hashish)

PubMed Central

El Alaoui, Moulay Abdelaziz; Melloul, Marouane; Alaoui Amine, Sanaâ; Stambouli, Hamid; El Bouri, Aziz; Soulaymani, Abdelmajid; El Fahime, Elmostafa

2013-01-01

The extraction and purification of nucleic acids is the first step in most molecular biology analysis techniques. The objective of this work is to obtain highly purified nucleic acids derived from Cannabis sativa resin seizure in order to conduct a DNA typing method for the individualization of cannabis resin samples. To obtain highly purified nucleic acids from cannabis resin (Hashish) free from contaminants that cause inhibition of PCR reaction, we have tested two protocols: the CTAB protocol of Wagner and a CTAB protocol described by Somma (2004) adapted for difficult matrix. We obtained high quality genomic DNA from 8 cannabis resin seizures using the adapted protocol. DNA extracted by the Wagner CTAB protocol failed to give polymerase chain reaction (PCR) amplification of tetrahydrocannabinolic acid (THCA) synthase coding gene. However, the extracted DNA by the second protocol permits amplification of THCA synthase coding gene using different sets of primers as assessed by PCR. We describe here for the first time the possibility of DNA extraction from (Hashish) resin derived from Cannabis sativa. This allows the use of DNA molecular tests under special forensic circumstances. PMID:24124454

Effective protein extraction protocol for proteomics studies of Jerusalem artichoke leaves.

PubMed

Zhang, Meide; Shen, Shihua

2013-07-01

Protein extraction is a crucial step for proteomics studies. To establish an effective protein extraction protocol suitable for two-dimensional electrophoresis (2DE) analysis in Jerusalem artichoke (Helianthus tuberosus L.), three different protein extraction methods-trichloroacetic acid/acetone, Mg/NP-40, and phenol/ammonium acetate-were evaluated using Jerusalem artichoke leaves as source materials. Of the three methods, trichloroacetic acid/acetone yielded the best protein separation pattern and highest number of protein spots in 2DE analysis. Proteins highly abundant in leaves, such as Rubisco, are typically problematic during leaf 2DE analysis, however, and this disadvantage was evident using trichloroacetic acid/acetone. To reduce the influence of abundant proteins on the detection of low-abundance proteins, we optimized the trichloroacetic acid/acetone method by incorporating a PEG fractionation approach. After optimization, 363 additional (36.2%) protein spots were detected on the 2DE gel. Our results suggest that trichloroacetic acid/acetone method is a better protein extraction technique than Mg/NP-40 and phenol/ammonium acetate in Jerusalem artichoke leaf 2DE analysis, and that trichloroacetic acid/acetone method combined with PEG fractionation procedure is the most effective approach for leaf 2DE analysis of Jerusalem artichoke. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of the gram-positive bacterial content of soils and sediments by analysis of teichoic acid components

NASA Technical Reports Server (NTRS)

Gehron, M. J.; Davis, J. D.; Smith, G. A.; White, D. C.

1984-01-01

Many gram-positive bacteria form substituted polymers of glycerol and ribitol phosphate esters known as teichoic acids. Utilizing the relative specificity of cold concentrated hydrofluoric acid in the hydrolysis of polyphosphate esters it proved possible to quantitatively assay the teichoic acid-derived glycerol and ribitol from gram-positive bacteria added to various soils and sediments. The lipids are first removed from the soils or sediments with a one phase chloroform-methanol extraction and the lipid extracted residue is hydrolyzed with cold concentrated hydrofluoric acid. To achieve maximum recovery of the teichoic acid ribitol, a second acid hydrolysis of the aqueous extract is required. The glycerol and ribitol are then acetylated after neutralization and analyzed by capillary gas-liquid chromatography. This technique together with measures of the total phospholipid, the phospholipid fatty acid, the muramic acid and the hydroxy fatty acids of the lipopolysaccharide lipid A of the gram-negative bacteria makes it possible to describe the community structure environmental samples. The proportion of gram-positive bacteria measured as the teichoic acid glycerol and ribitol is higher in soils than in sediments and increases with depth in both.

A novel fatty-acid-based in-tube dispersive liquid-liquid microextraction technique for the rapid determination of nonylphenol and 4-tert-octylphenol in aqueous samples using high-performance liquid chromatography-ultraviolet detection.

PubMed

Shih, Hou-Kuang; Shu, Ting-Yun; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2015-01-07

In this study, a novel fatty-acid-based in-tube dispersive liquid-liquid microextraction (FA-IT-DLLME) technique is proposed for the first time and is developed as a simple, rapid and eco-friendly sample extraction method for the determination of alkylphenols in aqueous samples using high-performance liquid chromatography-ultraviolet detection (HPLC-UV). In this extraction method, medium-chain saturated fatty acids were investigated as a pH-dependent phase because they acted as either anionic surfactants or neutral extraction solvents based on the acid-base reaction caused solely by the adjustment of the pH of the solution. A specially designed home-made glass extraction tube with a built-in scaled capillary tube was utilized as the phase-separation device for the FA-IT-DLLME to collect and measure the separated extractant phase for analysis. Nonylphenol (NP) and 4-tert-octylphenol (4-tOP) were chosen as model analytes. The parameters influencing the FA-IT-DLLME were thoroughly investigated and optimized. Under the optimal conditions, the detector responses of NP and 4-tOP were linear in the concentration ranges of 5-4000 μg L(-1), with correlation coefficients of 0.9990 and 0.9996 for NP and 4-tOP, respectively. The limits of detection based on a signal-to-noise ratio of 3 were 0.7 and 0.5 μg L(-1), and the enrichment factors were 195 and 143 for NP and 4-tOP, respectively. The applicability of the developed method was demonstrated for the analysis of alkylphenols in environmental wastewater samples, and the recoveries ranged from 92.9 to 107.1%. The extraction process required less than 4 min and utilized only acids, alkalis, and fatty acids to achieve the extraction. The results demonstrated that the presented FA-IT-DLLME approach is highly cost-effective, simple, rapid and environmentally friendly in its sample preparation. Copyright © 2014 Elsevier B.V. All rights reserved.

OPTIMIZATION OF THE WASH-OFF METHOD FOR MEASURING AEROSOL CONCENTRATIONS

EPA Science Inventory

Using the fluorescence-washing technique, oleic acid particles tagged with uranine were extracted and analyzed fluorometrically. The possible sources of errors in the technique were evaluated in this study. First, the sensitivity of uranine fluorescence in different solutions ...

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

Extraction of pectin from passion fruit rind (Passiflora edulis var. flavicarpa Degener) for edible coating

NASA Astrophysics Data System (ADS)

Inayati, Puspita, Rifka Intan; Fajrin, Vika Latifiana

2018-02-01

One of fruit preservation method is by applying the edible coating. Rind of passion fruit (Passiflora edulis var. flavicarpa Degener), which is kind of waste, can be utilized as edible coating through pectin extraction process. The purposes of this work were to determine the suitable solvent for the pectin extraction and techniques for applying the produced edible coating on strawberry, to produce edible coating from the pectin, and the test the performance of the edible coating which was applied to strawberries. Pectin from passion fruit rind was collected through conventional extraction method using two types of solvent, i.e. acetic acid solution and hydrochloric acid solution with concentration of 0.01 N, 0.015 N, 0.02 N, 0.025 N, and 0.03 N. The results showed that chloric acid solution was more suitable for the pectin extraction from passion fruit. Maximum yield of 30.78% was obtained at hydrochloric acid concentration of 0.02 N. Obtained pectin from the extraction was then processed into the edible coating by adding plasticizers and calcium chloride dihydrate. Storability of the coated strawberry was observed to measure the performance of the edible coating

Thermal effusivity measurement of conventional and organic coffee oils via photopyroelectric technique.

PubMed

Bedoya, A; Gordillo-Delgado, F; Cruz-Santillana, Y E; Plazas, J; Marin, E

2017-12-01

In this work, oil samples extracted from organic and conventional coffee beans were studied. A fatty acids profile analysis was done using gas chromatography and physicochemical analysis of density and acidity index to verify the oil purity. Additionally, Mid-Infrared Fourier Transform Photoacoustic Spectroscopy (FTIR-PAS) aided by Principal Component Analysis (PCA) was used to identify differences between the intensities of the absorption bands related to functional groups. Thermal effusivity values between 592±3 and 610±4Ws 1/2 m -2 K -1 were measured using the photopyroelectric technique in a front detection configuration. The acidity index was between 1.11 and 1.27% and the density changed between 0.921 and 0.94g/mL. These variables, as well as the extraction yield between 12,6 and 14,4%, showed a similar behavior than that observed for the thermal effusivity, demonstrating that this parameter can be used as a criterion for discrimination between oil samples extracted from organic and conventional coffee beans. Copyright © 2017 Elsevier Ltd. All rights reserved.

Kinetic and Thermodynamics studies for Castor Oil Extraction Using Subcritical Water Technology.

PubMed

Abdelmoez, Wael; Ashour, Eman; Naguib, Shahenaz M; Hilal, Amr; Al Mahdy, Dalia A; Mahrous, Engy A; Abdel-Sattar, Essam

2016-06-01

In this work both kinetic and thermodynamics of castor oil extraction from its seeds using subcritical water technique were studied. It was found that the extraction process followed two consecutive steps. In these steps, the oil was firstly extracted from inside the powder by diffusion mechanism. Then the extracted oil, due to extending the extraction time under high temperature and pressure, was subjected to a decomposition reaction following first order mechanism. The experimental data correlated well with the irreversible consecutive unimolecular-type first order mechanism. The values of both oil extraction rate constants and decomposition rate constants were calculated through non-linear fitting using DataFit software. The extraction rate constants were found to be 0.0019, 0.024, 0.098, 0.1 and 0.117 min(-1), while the decomposition rate constants were 0.057, 0.059, 0.014, 0.019 and 0.17 min(-1) at extraction temperatures of 240, 250, 260, 270 and 280°C, respectively. The thermodynamic properties of the oil extraction process were investigated using Arrhenius equation. The values of the activation energy, Ea, and the frequency factor, A, were 73 kJ mol(-1) and 946, 002 min(-1), respectively. The physicochemical properties of the extracted castor oil including the specific gravity, viscosity, acid value, pH value and calorific value were found to be 0.947, 7.487, 1.094 mg KOH/g, 6.1, and 41.5 MJ/Kg, respectively. Gas chromatography analysis showed that ricinoleic acid (83.6%) appears as the predominant fatty acid in the extracted oil followed by oleic acid (5.5%) and linoleic acid (2.3%).

A two-step electrodialysis method for DNA purification from polluted metallic environmental samples.

PubMed

Rodríguez-Mejía, José Luis; Martínez-Anaya, Claudia; Folch-Mallol, Jorge Luis; Dantán-González, Edgar

2008-08-01

Extracting DNA from samples of polluted environments using standard methods often results in low yields of poor-quality material unsuited to subsequent manipulation and analysis by molecular biological techniques. Here, we report a novel two-step electrodialysis-based method for the extraction of DNA from environmental samples. This technique permits the rapid and efficient isolation of high-quality DNA based on its acidic nature, and without the requirement for phenol-chloroform-isoamyl alcohol cleanup and ethanol precipitation steps. Subsequent PCR, endonuclease restriction, and cloning reactions were successfully performed utilizing DNA obtained by electrodialysis, whereas some or all of these techniques failed using DNA extracted with two alternative methods. We also show that his technique is applicable to purify DNA from a range of polluted and nonpolluted samples.

Pomegranate extract exhibits in vitro activity against Clostridium difficile.

PubMed

Finegold, Sydney M; Summanen, Paula H; Corbett, Karen; Downes, Julia; Henning, Susanne M; Li, Zhaoping

2014-10-01

To determine the possible utility of pomegranate extract in the management or prevention of Clostridium difficile infections or colonization. The activity of pomegranate was tested against 29 clinical C. difficile isolates using the Clinical and Laboratory Standards Institute-approved agar dilution technique. Total phenolics content of the pomegranate extract was determined by Folin-Ciocalteau colorimetric method and final concentrations of 6.25 to 400 μg/mL gallic acid equivalent were achieved in the agar. All strains had MICs at 12.5 to 25 mg/mL gallic acid equivalent range. Our results suggest antimicrobial in vitro activity for pomegranate extract against toxigenic C. difficile. Pomegranate extract may be a useful contributor to the management and prevention of C. difficile disease or colonization. Copyright © 2014 Elsevier Inc. All rights reserved.

Ultrasonic Removal of Mucilage for Pressurized Liquid Extraction of Omega-3 Rich Oil from Chia Seeds (Salvia hispanica L.).

PubMed

Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

2017-03-29

Chia (Salvia hispanica L.) seeds contain an important amount of edible oil rich in omega-3 fatty acids. Fast and alternative extraction techniques based on polar solvents, such as ethanol or water, have become relevant for oil extraction in recent years. However, chia seeds also contain a large amount of soluble fiber or mucilage, which makes difficult an oil extraction process with polar solvents. For that reason, the aim of this study was to develop a gentle extraction method for mucilage in order to extract chia oil with polar solvents using pressurized liquids and compare with organic solvent extraction. The proposed mucilage extraction method, using an ultrasonic probe and only water, was optimized at mild conditions (50 °C and sonication 3 min) to guarantee the omega-3 oil quality. Chia oil extraction was performed using pressurized liquid extraction (PLE) with different solvents and their mixtures at five different extraction temperatures (60, 90, 120, 150, and 200 °C). Optimal PLE conditions were achieved with ethyl acetate or hexane at 90 °C in only 10 min of static extraction time (chia oil yield up to 30.93%). In addition, chia oils extracted with nonpolar and polar solvents by PLE were analyzed by gas chromatography-mass spectrometry (GC-MS) to evaluate fatty acid composition at different extraction conditions. Chia oil contained ∼65% of α-linolenic acid regardless of mucilage extraction method, solvent, or temperature used. Furthermore, tocopherols and tocotrienols were also analyzed by HPLC in the extracted chia oils. The mucilage removal allowed the subsequent extraction of the chia oil with polar or nonpolar solvents by PLE producing chia oil with the same fatty acid and tocopherol composition as traditional extraction.

Extraction of glycogen on mild condition lacks AIG fraction.

PubMed

Ghafouri, Z; Rasouli, M

2016-12-01

Extraction of animal tissues with cold water or perchloric acid yields less glycogen than is obtained with hot-alkaline. Extraction with acid and alkaline gives two fractions, acid soluble (ASG) and insoluble glycogen (AIG). The aim of this work is to examine the hypothesis that not all liver glycogen is extractable by Tris-buffer using current techniques. Rat liver was homogenized with Tris-buffer pH 8.3 and extracted for the glycogen fractions, ASG and AIG. The degree of homogenization was changed to remove all glycogen. The content of glycogen was 47.7 ± 1.2 and 11.6 ± 0.8 mg/g wet liver in the supernatant and pellet of the first extraction respectively. About 24% of total glycogen is lost through the first pellet. Increasing the extent of homogenization from 30 to 180 sec and from 15000 to 20000 rpm followed with 30 sec ultrasonication did not improve the extraction. ASG and AIG constitute about 77% and 23% of the pellet glycogen respectively. Extraction with cold Tris-buffer failed to extract glycogen completely.  Increasing the extent of homogenization followed with ultrasonication also did not improve the extraction. Thus it is necessary to re-examine the previous findings obtained by extraction with cold Tris-buffer.

Integrated Micro-Chip Amino Acid Chirality Detector for MOD

NASA Technical Reports Server (NTRS)

Glavin, D. P.; Bada, J. L.; Botta, O.; Kminek, G.; Grunthaner, F.; Mathies, R.

2001-01-01

Integration of a micro-chip capillary electrophoresis analyzer with a sublimation-based extraction technique, as used in the Mars Organic Detector (MOD), for the in-situ detection of amino acids and their enantiomers on solar system bodies. Additional information is contained in the original extended abstract.

Application of HPLC and ESI-MS techniques in the analysis of phenolic acids and flavonoids from green leafy vegetables (GLVs).

PubMed

Kumar, B Ramesh

2017-12-01

Diets containing high proportions of fruits and vegetables reduce the risk of onset of chronic diseases. The role of herbal medicines in improving human health is gaining popularity over the years, which also increases the need for safety and efficiency of these products. Green leafy vegetables (GLVs) are the richest source of phenolic compounds with excellent antioxidant properties. Increased consumption of diets containing phenolic compounds may give positive and better results to human health and significantly improves the immune system. Highly selective, susceptible and versatile analytical techniques are necessary for extraction, identification, and quantification of phenolic compounds from plant extracts, which helps to utilize their important biological properties. Recent advances in the pre-treatment procedures, separation techniques and spectrometry methods are used for qualitative and quantitative analysis of phenolic compounds. The online coupling of liquid chromatography with mass spectrometry (LC-MS) has become a useful tool in the metabolic profiling of plant samples. In this review, the separation and identification of phenolic acids and flavonoids from GLVs by LC-MS have been discussed along with the general extraction procedures and other sources of mass spectrometer used. The review is devoted to the understanding of the structural configuration, nature and accumulation pattern of phenolic acids and flavonoids in plants and to highlighting the recent developments in the chemical investigation of these compounds by chromatographic and spectroscopic techniques. It concludes with the advantages of the combination of these two methods and prospects.

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.

Nucleic acid purification from plants, animals and microbes in under 30 seconds

PubMed Central

Zou, Yiping; Wang, Yuling; Wee, Eugene; Turni, Conny; Blackall, Patrick J.; Trau, Matt; Botella, Jose Ramon

2017-01-01

Nucleic acid amplification is a powerful molecular biology tool, although its use outside the modern laboratory environment is limited due to the relatively cumbersome methods required to extract nucleic acids from biological samples. To address this issue, we investigated a variety of materials for their suitability for nucleic acid capture and purification. We report here that untreated cellulose-based paper can rapidly capture nucleic acids within seconds and retain them during a single washing step, while contaminants present in complex biological samples are quickly removed. Building on this knowledge, we have successfully created an equipment-free nucleic acid extraction dipstick methodology that can obtain amplification-ready DNA and RNA from plants, animals, and microbes from difficult biological samples such as blood and leaves from adult trees in less than 30 seconds. The simplicity and speed of this method as well as the low cost and availability of suitable materials (e.g., common paper towelling), means that nucleic acid extraction is now more accessible and affordable for researchers and the broader community. Furthermore, when combined with recent advancements in isothermal amplification and naked eye DNA visualization techniques, the dipstick extraction technology makes performing molecular diagnostic assays achievable in limited resource settings including university and high school classrooms, field-based environments, and developing countries. PMID:29161268

Ultra-high performance liquid chromatography coupled to mass spectrometry applied to the identification of valuable phenolic compounds from Eucalyptus wood.

PubMed

Santos, Sónia A O; Vilela, Carla; Freire, Carmen S R; Neto, Carlos Pascoal; Silvestre, Armando J D

2013-11-01

Ultra-high performance liquid chromatography (UHPLC) was applied for the first time in the analysis of wood extracts. The potential of this technique coupled to ion trap mass spectrometry in the rapid and effective detection and identification of bioactive components in complex vegetal samples was demonstrated. Several dozens of compounds were detected in less than 30min of analysis time, corresponding to more than 3-fold reduction in time, when compared to conventional HPLC analysis of similar extracts. The phenolic chemical composition of Eucalyptus grandis, Eucalyptus urograndis (E. grandis×E. urophylla) and Eucalyptus maidenii wood extracts was assessed for the first time, with the identification of 51 phenolic compounds in the three wood extracts. Twenty of these compounds are reported for the first time as Eucalyptus genus components. Ellagic acid and ellagic acid-pentoside are the major components in all extracts, followed by gallic and quinic acids in E. grandis and E. urograndis and ellagic acid-pentoside isomer, isorhamnetin-hexoside and gallic acid in E. maidenii. The antioxidant scavenging activity of the extracts was evaluated, with E. grandis wood extract showing the lowest IC50 value. Moreover, the antioxidant activity of these extracts was higher than that of the commercial antioxidant BHT and of those of the corresponding bark extracts. These results, together with the phenolic content values, open good perspectives for the exploitation of these renewable resources as a source of valuable phenolic compounds. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of plant growth regulators in pears by microwave-assisted extraction and liquid chromatography with electrospray ionization mass spectrometry.

PubMed

Mao, Xuejin; Tang, Lijuan; Tan, Ting; Wan, Yiqun

2014-06-01

A new method for the determination of six plant growth regulators, 3-indolylacetic acid, 3-indolepropionic acid, 2-naphthoxyacetic acid, 2,4-dicholrophenoxyacetic acid, 1-naphthlcetic acid, and methyl naphthalene-1-acetate, in pears was established by liquid chromatography with electrospray ionization mass spectrometry. In this study, a microwave-assisted extraction technique was first applied for the determination of plant growth regulators in fruit and three cleanup techniques were, respectively, investigated for the purification of pear samples. The chromatographic separation was performed on a Diamonsil C18 column by using 0.01 mol/L formic acid/ammonium formate buffer solution (pH 3.5)/methanol (35:65, v/v) as the mobile phase with a flow rate of 0.7 mL/min in 1:1 split mode. The LODs ranged from 0.3 to 1.9 μg/kg. Under optimized conditions, the average recoveries (five replicates) for six plant growth regulators (spiked at 0.01, 0.05, and 0.5 mg/kg) ranged from 78.9 to 118.0%, and the RSDs were 1.4-10.3%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Study on chemical constituents from ethyl acetate extract of Myricaria bracteata].

PubMed

Zhang, Ying; Yuan, Yi; Cui, Baosong; Li, Shuai

2011-04-01

To study the chemical constituents from the ethyl acetate extract of Myricaria bracteata. The chemical constituents were isolated and purified by chromatographic techniques, and their structures were identified by physical characters and spectroscopic analysis. Sixteen compounds were isolated from the ethyl acetate portion of the 95% ethanolic extract of Myricaria bracteata, and identified as myricarin (1), myricarin B (2), 3alpha-hydroxytaraxer-14-en-28-oic acid (3), myricadiol (4), trans-ferulic acid 22-hydroxydocosanoic acid ester (5), docosyl-3, 4-dihydroxy-trans-cinnamate (6), dillenetin (7), 3, 5, 4'-trihydroxy-7-methoxyflavone (8), 3, 5, 4'-trihydroxy-7, 3'-dimethoxyflavone (9), methyl 3, 5-dihydroxy-4-methoxybenzoate (10), 3-hydroxy-4-methoxy cinnamic acid (11), sinapaldehyde (12), vanillin (13), syringaldehyde (14), 3, 3', 4'-trimethoxyellagic acid (15), methyl p-hyroxybenzoate (16). Compounds 5, 6, 12-16 were isolated from the genus Myricaria for the fist time, all of the compounds were isolated from this plant for the fist time, except for 8 and 9.

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.

[Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

PubMed

Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

2012-08-01

A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

Spectroscopic study of the humification process during sewage sludge treatment

NASA Astrophysics Data System (ADS)

Pajączkowska, J.; Sułkowska, A.; Sułkowski, W. W.; Jędrzejczyk, M.

2003-06-01

The aim of this work was to study the free radical transition of organic materials during the sewage treatment process. Investigations of sludge from biologic-mechanical sewage treatment plant in Sosnowiec Zagórze were carried out. The course of the humification processes during sewage treatment was studied by electron paramagnetic resonance (EPR) technique. The concentration of free radicals at each process stage and the value g were determined. Sludge samples and extracted fractions of humic acids were examined. Humic acids were extracted from sludge by means of conventional methods elaborated by Stevenson. For study of humic acids structures, besides EPR, the UV-Vis and IR spectroscopy were used.

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.

Simple and rapid analytical method for detection of amino acids in blood using blood spot on filter paper, fast-GC/MS and isotope dilution technique.

PubMed

Kawana, Shuichi; Nakagawa, Katsuhiro; Hasegawa, Yuki; Yamaguchi, Seiji

2010-11-15

A simple and rapid method for quantitative analysis of amino acids, including valine (Val), leucine (Leu), isoleucine (Ile), methionine (Met) and phenylalanine (Phe), in whole blood has been developed using GC/MS. In this method, whole blood was collected using a filter paper technique, and a 1/8 in. blood spot punch was used for sample preparation. Amino acids were extracted from the sample, and the extracts were purified using cation-exchange resins. The isotope dilution method using ²H₈-Val, ²H₃-Leu, ²H₃-Met and ²H₅-Phe as internal standards was applied. Following propyl chloroformate derivatization, the derivatives were analyzed using fast-GC/MS. The extraction recoveries using these techniques ranged from 69.8% to 87.9%, and analysis time for each sample was approximately 26 min. Calibration curves at concentrations from 0.0 to 1666.7 μmol/l for Val, Leu, Ile and Phe and from 0.0 to 333.3 μmol/l for Met showed good linearity with regression coefficients=1. The method detection limits for Val, Leu, Ile, Met and Phe were 24.2, 16.7, 8.7, 1.5 and 12.9 μmol/l, respectively. This method was applied to blood spot samples obtained from patients with phenylketonuria (PKU), maple syrup urine disease (MSUD), hypermethionine and neonatal intrahepatic cholestasis caused by citrin deficiency (NICCD), and the analysis results showed that the concentrations of amino acids that characterize these diseases were increased. These results indicate that this method provides a simple and rapid procedure for precise determination of amino acids in whole blood. Copyright © 2010 Elsevier B.V. All rights reserved.

High efficiency liquid chromatography techniques coupled to mass spectrometry for the characterization of mate extracts.

PubMed

Dugo, Paola; Cacciola, Francesco; Donato, Paola; Jacques, Rosângela Assis; Caramão, Elina Bastos; Mondello, Luigi

2009-10-23

There is growing interest related to rapid screening and full characterization of the constituents of plants with medicinal properties; among these, "Mate" or Yerba Maté is a tea-like beverage widely consumed in South America, obtained from the dried leaves of Ilex paraguariensis. The high content in polyphenols accounts for in vitro and in vivo antioxidant activity of the extracts obtained from this plant; on the other hand, the high complexity of the samples extracted, depending on the method employed, may preclude complete resolution by conventional HPLC techniques. For this purpose, a comprehensive two-dimensional liquid chromatography (LC x LC) system, comprised of an RP-Amide first dimension and a partially porous octadecylsilica column in the second dimension, has been compared with a one-dimensional system. The latter was operated using a partially porous octadecylsilica column, with diode array (DAD) and electrospray/ion trap-time of flight (ESI/IT-TOF) detection for the most complex extracts. The employment of the hybrid mass spectrometer allowed unequivocal identification of several compounds in the mate extracts. Using LC x LC-MS(3), it was possible to discriminate between congeners of chlorogenic acids, along with monoacyl- and diacylchlorogenic acid esters.

Comparison of different methods for extraction and purification of human Papillomavirus (HPV) DNA from serum samples

NASA Astrophysics Data System (ADS)

Azizah, N.; Hashim, U.; Nadzirah, Sh.; Arshad, M. K. Md; Ruslinda, A. R.; Gopinath, Subash C. B.

2017-03-01

The affectability and unwavering quality of PCR for indicative and research purposes require effective fair systems of extraction and sanitization of nucleic acids. One of the real impediments of PCR-based tests is the hindrance of the enhancement procedure by substances exhibit in clinical examples. This examination considers distinctive techniques for extraction and cleaning of viral DNA from serum tests in view of recuperation productivity as far as yield of DNA and rate recouped immaculateness of removed DNA, and rate of restraint. The best extraction strategies were the phenol/chloroform strategy and the silica gel extraction methodology for serum tests, individually. Considering DNA immaculateness, extraction technique by utilizing the phenol/chloroform strategy delivered the most tasteful results in serum tests contrasted with the silica gel, separately. The nearness of inhibitors was overcome by all DNA extraction strategies in serum tests, as confirm by semiquantitative PCR enhancement.

Evaluation of a new eastern blotting technique for the analysis of ginsenoside Re in American ginseng berry pulp extracts.

PubMed

Morinaga, Osamu; Uto, Takuhiro; Yuan, Chun-Su; Tanaka, Hiroyuki; Shoyama, Yukihiro

2010-06-01

A new eastern blotting technique has been established for ginsenoside Re (G-Re) contained in American ginseng berry pulp extracts. G-Re in American ginseng berry pulp was extracted using 100% methanol, 100% ethanol, 50% aqueous methanol, and 50% aqueous ethanol. The combined crude extracts were applied onto a polyethersulfone membrane and developed using the methanol-water-acetic acid solvent system (45:55:1 v/v). Separated components were immunostained using anti-G-Re monoclonal antibody. G-Re was first specifically detected and then quantitatively analyzed using NIH Imaging software. We also confirmed that the most suitable solvent was 50% aqueous methanol for extracting G-Re from American ginseng berry pulp. (c) 2009 Elsevier B.V. All rights reserved.

Antioxidant activity and total phenols from the methanolic extract of Miconia albicans (Sw.) Triana leaves.

PubMed

Pieroni, Laís Goyos; de Rezende, Fernanda Mendes; Ximenes, Valdecir Farias; Dokkedal, Anne Lígia

2011-11-10

Miconia is one of the largest genus of the Melastomataceae, with approximately 1,000 species. Studies aiming to describe the diverse biological activities of the Miconia species have shown promising results, such as analgesic, antimicrobial and trypanocidal properties. M. albicans leaves were dried, powdered and extracted to afford chloroformic and methanolic extracts. Total phenolic contents in the methanolic extract were determined according to modified Folin-Ciocalteu method. The antioxidant activity was measured using AAPH and DPPH radical assays. Chemical analysis was performed with the n-butanol fraction of the methanolic extract and the chloroformic extract, using different chromatographic techniques (CC, HPLC). The structural elucidation of compounds was performed using 500 MHz NMR and HPLC methods. The methanolic extract showed a high level of total phenolic contents; the results with antioxidant assays showed that the methanolic extract, the n-butanolic fraction and the isolated flavonoids from M. albicans had a significant scavenging capacity against AAPH and DPPH. Quercetin, quercetin-3-O-glucoside, rutin, 3-(E)-p-coumaroyl-α-amyrin was isolated from the n-butanolic fraction and α-amyrin, epi-betulinic acid, ursolic acid, epi-ursolic acid from the chloroformic extract. The results presented in this study demonstrate that M. albicans is a promising species in the search for biologically active compounds.

Study on tea leaves extract as green corrosion inhibitor of mild steel in hydrochloric acid solution

NASA Astrophysics Data System (ADS)

Hamdan, A. B.; Suryanto; Haider, F. I.

2018-01-01

Corrosion inhibitor from extraction of plant has been considered as the most preferable and most chosen technique to prevent corrosion of metal in acidic medium because of the environmental friendly factor. In this study, black tea leaves extraction was tested as corrosion inhibitor for mild steel in 0.1M of hydrochloric acid (HCl) with the absence and presence of corrosion inhibitor. The efficiency and effectiveness of black tea as corrosion inhibitor was tested by using corrosion weight loss measurement experiment was carried out with varies parameters which with different concentration of black tea extract solution. The extraction of black tea solution was done by using aqueous solvent method. The FT-IR result shows that black tea extract containing compounds such as catechin, caffeine and tannins that act as anti-corrosive reagents and responsible to enhance the effectiveness of black tea extract as corrosion inhibitor by forming the hydrophobic thin film through absorption process. As a result of weight loss measurement, it shows that loss in weight of mild steel reduces as the concentration of inhibitor increases. The surface analysis was done on the mild steel samples by using SEM.

Chemical mimicking of bio-assisted aluminium extraction by Aspergillus niger's exometabolites.

PubMed

Boriová, Katarína; Urík, Martin; Bujdoš, Marek; Pifková, Ivana; Matúš, Peter

2016-11-01

Presence of microorganisms in soils strongly affects mobility of metals. This fact is often excluded when mobile metal fraction in soil is studied using extraction procedures. Thus, the first objective of this paper was to evaluate strain Aspergillus niger's exometabolites contribution on aluminium mobilization. Fungal exudates collected in various time intervals during cultivation were analyzed and used for two-step bio-assisted extraction of alumina and gibbsite. Oxalic, citric and gluconic acids were identified in collected culture media with concentrations up to 68.4, 2.0 and 16.5 mmol L -1 , respectively. These exometabolites proved to be the most efficient agents in mobile aluminium fraction extraction with aluminium extraction efficiency reaching almost 2.2%. However, fungal cultivation is time demanding process. Therefore, the second objective was to simplify acquisition of equally efficient extracting agent by chemically mimicking composition of main organic acid components of fungal exudates. This was successfully achieved with organic acids mixture prepared according to medium composition collected on the 12th day of Aspergillus niger cultivation. This mixture extracted similar amounts of aluminium from alumina compared to culture medium. The aluminium extraction efficiency from gibbsite by organic acids mixture was lesser than 0.09% which is most likely because of more rigid mineral structure of gibbsite compared to alumina. The prepared organic acid mixture was then successfully applied for aluminium extraction from soil samples and compared to standard single step extraction techniques. This showed there is at least 2.9 times higher content of mobile aluminium fraction in soils than it was previously considered, if contribution of microbial metabolites is considered in extraction procedures. Thus, our contribution highlights the significance of fungal metabolites in aluminium extraction from environmental samples, but it also simplifies the extraction procedure inspired by bio-assisted extraction of aluminium by common soil fungus A. niger. Copyright © 2016 Elsevier Ltd. All rights reserved.

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.

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

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

Peters, R.W.

1995-05-01

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

Analysis of biologically active oxyprenylated phenylpropanoids in Tea tree oil using selective solid-phase extraction with UHPLC-PDA detection.

PubMed

Scotti, Luca; Genovese, Salvatore; Bucciarelli, Tonino; Martini, Filippo; Epifano, Francesco; Fiorito, Serena; Preziuso, Francesca; Taddeo, Vito Alessandro

2018-05-30

An efficient analytical strategy based on different extraction methods of biologically active naturally occurring oxyprenylated umbelliferone and ferulic acid derivatives 7-isopentenyloxycoumarin, auraptene, umbelliprenin, boropinic acid, and 4'-geranyloxyferulic acid and quantification by UHPLC with spectrophotometric (UV/Vis) detection from Tea tree oil is reported. Absorption of the pure oil on Al 2 O 3 (Brockmann activity II) prior washing the resulting solid with MeOH and treatment of this latter with CH 2 Cl 2 resulted the best extraction methodology in terms of yields of oxyprenylated secondary metabolites. Among the five O-prenylphenylpropanoids herein under investigation auraptene and umbelliprenin were never detected while 4'-geranyloxyferulic acid was the most abundant compound resulting from all the three extraction methods employed. The UHPLC analytical methodology set up in the present study resulted to be an effective and versatile technique for the simultaneous characterization and quantification of prenyloxyphenylpropanoids in Tea tree oil and applicable to other complex matrices from the plant kingdom. Copyright © 2018 Elsevier B.V. All rights reserved.

Extraction and derivatization of polar herbicides for GC-MS analyses.

PubMed

Ranz, Andreas; Maier, Eveline; Motter, Herbert; Lankmayr, Ernst

2008-09-01

A sample preparation procedure including a simultaneous microwave-assisted (MA) extraction and derivatization for the determination of chlorophenoxy acids in soil samples is presented. For a selective and sensitive measurement, an analytical technique such as GC coupled with MS needs to be adopted. For GC analyses, chlorophenoxy acids have to be converted into more volatile and thermally stable derivatives. Derivatization by means of microwave radiation offers new alternatives in terms of shorter derivatization time and reduces susceptibility for the formation of artefacts. Extraction and derivatization into methyl esters (ME) were performed with sulphuric acid and methanol. Due to the novelty of the simultaneous extraction and derivatization assisted by means of microwave radiation, a careful investigation and optimization of influential reaction parameters was necessary. It could be shown that the combination of sulphuric acid and methanol provides a fast sample preparation including an efficient clean up procedure. The data obtained by the described method are in good agreement with those published for the reference material. Finally, compared to conventional heating and also to the standard procedure of the EPA, the sample preparation time could be considerably shortened.

Effectiveness of high-throughput miniaturized sorbent- and solid phase microextraction techniques combined with gas chromatography-mass spectrometry analysis for a rapid screening of volatile and semi-volatile composition of wines--a comparative study.

PubMed

Mendes, Berta; Gonçalves, João; Câmara, José S

2012-01-15

In this study the feasibility of different extraction procedures was evaluated in order to test their potential for the extraction of the volatile (VOCs) and semi-volatile constituents (SVOCs) from wines. In this sense, and before they could be analysed by gas chromatography-quadrupole first stage masss spectrometry (GC-qMS), three different high-throughput miniaturized (ad)sorptive extraction techniques, based on solid phase extraction (SPE), microextraction by packed sorbents (MEPS) and solid phase microextraction (SPME), were studied for the first time together, for the extraction step. To achieve the most complete volatile and semi-volatile signature, distinct SPE (LiChrolut EN, Poropak Q, Styrene-Divinylbenzene and Amberlite XAD-2) and MEPS (C(2), C(8), C(18), Silica and M1 (mixed C(8)-SCX)) sorbent materials, and different SPME fibre coatings (PA, PDMS, PEG, DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS), were tested and compared. All the extraction techniques were followed by GC-qMS analysis, which allowed the identification of up to 103 VOCs and SVOCs, distributed by distinct chemical families: higher alcohols, esters, fatty acids, carbonyl compounds and furan compounds. Mass spectra, standard compounds and retention index were used for identification purposes. SPE technique, using LiChrolut EN as sorbent (SPE(LiChrolut EN)), was the most efficient method allowing for the identification of 78 VOCs and SVOCs, 63 and 19 more than MEPS and SPME techniques, respectively. In MEPS technique the best results in terms of number of extractable/identified compounds and total peak areas of volatile and semi-volatile fraction, were obtained by using C(8) resin whereas DVB/CAR/PDMS was revealed the most efficient SPME coating to extract VOCs and SVOCs from Bual wine. Diethyl malate (18.8±3.2%) was the main component found in wine SPE(LiChrolut EN) extracts followed by ethyl succinate (13.5±5.3%), 3-methyl-1-butanol (13.2±1.7%), and 2-phenylethanol (11.2±9.9%), while in SPME(DVB/CAR/PDMS) technique 3-methyl-1-butanol (43.3±0.6%) followed by diethyl succinate (18.9±1.6%), and 2-furfural (10.4±0.4%), are the major compounds. The major VOCs and SVOCs isolated by MEPS(C8) were 3-methyl-1-butanol (26.8±0.6%, from wine total volatile fraction), diethyl succinate (24.9±0.8%), and diethyl malate (16.3±0.9%). Regardless of the extraction technique, the highest extraction efficiency corresponds to esters and higher alcohols and the lowest to fatty acids. Despite some drawbacks associated with the SPE procedure such as the use of organic solvents, the time-consuming and tedious sampling procedure, it was observed that SPE(LiChrolut EN), revealed to be the most effective technique allowing the extraction of a higher number of compounds (78) rather than the other extraction techniques studied. Copyright © 2011 Elsevier B.V. All rights reserved.

Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

PubMed Central

Chen, Fengli; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

2014-01-01

An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. PMID:24782942

Correlating Detergent Fiber Analysis and Dietary Fiber Analysis Data for Corn Stover

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

Wolfrum, E. J.; Lorenz, A. J.; deLeon, N.

There exist large amounts of detergent fiber analysis data [neutral detergent fiber (NDF), acid detergent fiber (ADF), acid detergent lignin (ADL)] for many different potential cellulosic ethanol feedstocks, since these techniques are widely used for the analysis of forages. Researchers working in the area of cellulosic ethanol are interested in the structural carbohydrates in a feedstock (principally glucan and xylan), which are typically determined by acid hydrolysis of the structural fraction after multiple extractions of the biomass. These so-called dietary fiber analysis methods are significantly more involved than detergent fiber analysis methods. The purpose of this study was to determinemore » whether it is feasible to correlate detergent fiber analysis values to glucan and xylan content determined by dietary fiber analysis methods for corn stover. In the detergent fiber analysis literature cellulose is often estimated as the difference between ADF and ADL, while hemicellulose is often estimated as the difference between NDF and ADF. Examination of a corn stover dataset containing both detergent fiber analysis data and dietary fiber analysis data predicted using near infrared spectroscopy shows that correlations between structural glucan measured using dietary fiber techniques and cellulose estimated using detergent techniques, and between structural xylan measured using dietary fiber techniques and hemicellulose estimated using detergent techniques are high, but are driven largely by the underlying correlation between total extractives measured by fiber analysis and NDF/ADF. That is, detergent analysis data is correlated to dietary fiber analysis data for structural carbohydrates, but only indirectly; the main correlation is between detergent analysis data and solvent extraction data produced during the dietary fiber analysis procedure.« less

Significant Enrichment of Polyunsaturated Fatty Acids (PUFAs) in the Lipids Extracted by Supercritical CO2 from the Livers of Australian Rock Lobsters (Jasus edwardsii).

PubMed

Nguyen, Trung T; Zhang, Wei; Barber, Andrew R; Su, Peng; He, Shan

2015-05-13

Australian rock lobster (Jasus edwardsii) liver contains approximately 24.3% (w/w) lipids, which can contain a high amount of polyunsaturated fatty acids (PUFAs). However, this material has been found to be contaminated with arsenic (240 mg/kg) and cadmium (8 mg/kg). The high level of contaminants in the raw material and the large amount of PUFAs in the lipids prove a significant challenge in the extraction of high-quality lipids from this byproduct by conventional methods. Supercritical carbon dioxide (SC-CO2) extraction is a highly promising technology for lipid extraction with advantages including low contamination and low oxidation. The technique was optimized to achieve nearly 94% extraction of lipids relative to conventional Soxhlet extraction in Australian rock lobster liver at conditions of 35 MPa and 50 °C for 4 h. The extracted lipids are significantly enriched in PUFAs at 31.3% of total lipids, 4 times higher than those in the lipids recovered by Soxhlet extraction (7.8%). Specifically, the concentrations of docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA) in SC-CO2 extraction are 7 times higher than those obtained by Soxhlet extraction. Moreover, very small amounts of toxic heavy metals such as lead (Pb), arsenic (As), mercury (Hg), and cadmium (Cd) were detected in the SC-CO2-extracted lipids, 0.5-27 times lower than those in the Soxhlet-extracted lipids, which are 40-200 times lower than the regulatory limit maximum values. The low levels of contaminants and the high proportion of PUFAs (dominated by DHA and EPA) found in the SC-CO2-extracted lipids from Australian rock lobster liver suggest that the material could potentially be used as a valuable source of essential fatty acids for human consumption.

Fatty acids composition of Caenorhabditis elegans using accurate mass GCMS-QTOF

PubMed Central

Henry, Parise; Owopetu, Olufunmilayo; Adisa, Demilade; Nguyen, Thao; Anthony, Kevin; Ijoni-Animadu, David; Jamadar, Sakha; Abdel-Rahman, Fawzia; Saleh, Mahmoud A.

2016-01-01

The free living nematode Caenorhabditis elegans is a proven model organism for lipid metabolism research. Total lipids of C. elegans were extracted using chloroform, methanol 2:1(v/v). Fatty acids composition of the extracted total lipids were converted to their corresponding methyl esters (FAMEs) and analyzed by gas chromatography/accurate mass quadrupole time of flight mass spectrometry (GCMS-QTOF) using both electron ionization (EI) and chemical ionization (CI) techniques. 28 fatty acids consisting of 12 to 22 carbon atoms were identified, 65% of them were unsaturated. Fatty acids containing 12 to 17 carbons were mostly saturated with stearic acid (18:0) as the major constituent. Several branched-chain fatty acids were identified. Methyl-14-methylhexadecanoate (iso-17:0) was the major identified branched fatty acid. This is the first report to detect the intact molecular parent ions of the identified fatty acids using chemical ionization compared to electron ionization which produced fragmentations of the fatty acids methyl esters (FAMEs). PMID:27166662

A comparison of various modes of liquid-liquid based microextraction techniques: determination of picric acid.

PubMed

Burdel, Martin; Šandrejová, Jana; Balogh, Ioseph S; Vishnikin, Andriy; Andruch, Vasil

2013-03-01

Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Assessment of dispersive liquid-liquid microextraction conditions for gas chromatography time-of-flight mass spectrometry identification of organic compounds in honey.

PubMed

Moniruzzaman, M; Rodríguez, I; Rodríguez-Cabo, T; Cela, R; Sulaiman, S A; Gan, S H

2014-11-14

The suitability of the dispersive liquid-liquid microextraction (DLLME) technique for gas chromatography (GC) characterization of minor organic compounds in honey samples is evaluated. Under optimized conditions, samples were pre-treated by liquid-liquid extraction with acetonitrile followed by DLLME using carbon tetrachloride (CCl4, 0.075 mL) as extractant. The yielded settled phase was analyzed by GC using high resolution time-of-flight (TOF) mass spectrometry (MS). The whole sample preparation process is completed in approximately 10 min, with a total consumption of organic solvents below 4 mL, relative standard deviations lower than 12% and with more than 70 organic compounds, displaying linear retention index in the range from 990 to 2900, identified in the obtained extracts. In comparison with HS SPME extraction, higher peak intensities were attained for most volatile and semi-volatile compounds amenable to both extraction techniques. Furthermore, other species such as highly polar and water soluble benzene acids, long chain fatty acids, esters and flavonoids, which are difficult to concentrate by HS SPME, could be identified in DLLME extracts. Some of the compounds identified in DLLME extracts have been proposed as useful for samples classification and/or they are recognized as markers of honeys from certain geographic areas. Copyright © 2014 Elsevier B.V. All rights reserved.

Combined Determination of Poly-β-Hydroxyalkanoic and Cellular Fatty Acids in Starved Marine Bacteria and Sewage Sludge by Gas Chromatography with Flame Ionization or Mass Spectrometry Detection

PubMed Central

Odham, Göran; Tunlid, Anders; Westerdahl, Gunilla; Mårdén, Per

1986-01-01

Extraction of lipids from bacterial cells or sewage sludge samples followed by simple and rapid extraction procedures and room temperature esterification with pentafluorobenzylbromide allowed combined determinations of poly-β-hydroxyalkanoate constituents and fatty acids. Capillary gas chromatography and flame ionization or mass spectrometric detection was used. Flame ionization permitted determination with a coefficient of variation ranging from 10 to 27% at the picomolar level, whereas quantitative chemical ionization mass spectrometry afforded sensitivities for poly-β-hydroxyalkanoate constituuents in the attomolar range. The latter technique suggests the possibility of measuring such components in bacterial assemblies with as few as 102 cells. With the described technique using flame ionization detection, it was possible to study the rapid formation of poly-β-hydroxyalkanoate during feeding of a starved marine bacterium isolate with a complex medium or glucose and correlate the findings to changes in cell volumes. Mass spectrometric detection of short β-hydroxy acids in activated sewage sludge revealed the presence of 3-hydroxybutyric, 3-hydroxyhexanoic, and 3-hydroxyoctanoic acids in the relative proportions of 56, 5 and 39%, respectively. No odd-chain β-hydroxy acids were found. PMID:16347181

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.

Anatomy and cell wall polysaccharides of almond (Prunus dulcis D. A. Webb) seeds.

PubMed

Dourado, Fernando; Barros, António; Mota, Manuel; Coimbra, Manuel A; Gama, Francisco M

2004-03-10

The anatomy of Prunus dulcis was analyzed by applying several differential staining techniques and light microscopy. Prunus dulcis seed has a thin and structurally complex seed coat, with lignified cellulosic tissue. The embryo has two voluminous cotyledons. Cotyledon cells have a high number of protein and lipid bodies, some of which have phytin. The provascular tissue, located in the cotyledons, is oriented in small bundles perpendicular to the transverse embryonic axis. Prunus dulcis cell wall material is very rich in arabinose (45 mol %). Glucose (23%), uronic acids (12%), and xylose (12%) are also major sugar components. The polymers obtained from the imidazole and Na(2)CO(3) extracts contain mainly pectic substances rich in arabinose, but the sugar content of these extracts was very low. The majority of the pectic substances (also rich in arabinose) was recovered with the KOH extracts. These extracts, with high sugar content, yielded also xyloglucans and acidic xylans. The 4 M KOH + H(3)BO(3) extracts yielded polysaccharides rich in uronic acids and xylose and very rich in arabinose, accounting for 27% of the cell wall material.

Microwave-assisted aqueous enzymatic extraction of oil from pumpkin seeds and evaluation of its physicochemical properties, fatty acid compositions and antioxidant activities.

PubMed

Jiao, Jiao; Li, Zhu-Gang; Gai, Qing-Yan; Li, Xiao-Juan; Wei, Fu-Yao; Fu, Yu-Jie; Ma, Wei

2014-03-15

Microwave-assisted aqueous enzymatic extraction (MAAEE) of pumpkin seed oil was performed in this study. An enzyme cocktail comprised of cellulase, pectinase and proteinase (w/w/w) was found to be the most effective in releasing oils. The highest oil recovery of 64.17% was achieved under optimal conditions of enzyme concentration (1.4%, w/w), temperature (44°C), time (66 min) and irradiation power (419W). Moreover, there were no significant variations in physicochemical properties of MAAEE-extracted oil (MAAEEO) and Soxhlet-extracted oil (SEO), but MAAEEO exhibited better oxidation stability. Additionally, MAAEEO had a higher content of linoleic acid (57.33%) than SEO (53.72%), and it showed stronger antioxidant activities with the IC50 values 123.93 and 152.84, mg/mL, according to DPPH radical scavenging assay and β-carotene/linoleic acid bleaching test. SEM results illustrated the destruction of cell walls and membranes by MAAEE. MAAEE is, therefore, a promising and environmental-friendly technique for oil extraction in the food industry. Copyright © 2013 Elsevier Ltd. All rights reserved.

Optimization of Supercritical Carbon Dioxide Extraction of Eucommia ulmoides Seed Oil and Quality Evaluation of the Oil.

PubMed

Zhang, Zhen-Shan; Liu, Yu-Lan; Che, Li-Ming

2018-03-01

Supercritical carbon dioxide extraction (SC-CO 2 ) technology was used to extract oil from Eucommia ulmoides seed. The optimum conditions and significant parameters in SC-CO 2 were obtained using response surface methodology (RSM). The qualities of the extracted oil were evaluated by physicochemical properties, fatty acid composition, vitamin E composition. It was found that the optimum extraction parameters were at pressure of 37 MPa, temperature of 40°C, extraction time of 125 min and CO 2 flow rate of 2.6 SL/min. Pressure, temperature and time were identified as significant parameter effecting on extraction yield. The importance of evaluated parameters decreased in the order of pressure > extraction time > temperature > CO 2 flow rate. GC analysis indicated that E. ulmoides seed oil contained about 61% of linolenic acid and its fatty acid composition was similar with that of flaxseed oil and perilla oil. The content and composition of vitamin E was determined using HPLC. The E. ulmoides seed oil was rich in vitamin E (190.72 mg/100 g), the predominant vitamin E isomers were γ- tocopherol and δ- tocopherol, which accounted for 70.87% and 24.81% of the total vitamin E, respectively. The high yield and good physicochemical properties of extracted oil support the notion that SC-CO 2 technology is an effective technique for extracting oil from E. ulmoides seed.

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.

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

Holser, Ronald A.; King, J. W.; Bost, G.

The genus Hibiscus exhibits great diversity in the production of natural materials with edible and industrial applications. The seeds of twelve varieties of Hibiscus were investigated as a source for triglycerides and phospholipids that could be used in functional foods. Lipid components were extracted from seed samples ground to a nominal particle diameter of 0.1 mm. Extractions were performed with an ISCO model 3560 supercritical fluid extractor using carbon dioxide and a mixture of carbon dioxide modified with ethanol. The neutral lipids were extracted with carbon dioxide at 80 C and 5370 MPa for 45 min. Polar lipids were subsequentlymore » extracted with a mixture of carbon dioxide and 15% ethanol at the same temperature and pressure. High performance liquid chromatography (HPLC) was used to analyze extracts for major neutral and polar lipid classes. A silica column was used with a solvent gradient of hexane/isopropanol/ water and ultraviolet (UV) and evaporative light scattering detectors (ELSD). An aliquot of each triglyceride fraction was trans-methylated with sodium methoxide and analyzed by gas chromatography to obtain the corresponding fatty acid methyl esters. The total lipids extracted ranged from 8.5% for a variety indigenous to Madagascar (H. calyphyllus) to 20% for a hybrid species (Georgia Rose). The average oil yield was 11.4% for the other varieties tested. The fatty acid methyl ester analysis displayed a high degree of unsaturation for all varieties tested, e. g., 75 ' 83%. Oleic, linoleic, and linolenic fatty acids were the predominate unsaturated fatty acids with only minor amounts of C14, C18, and C20 saturated fatty acids measured. Palmitic acid was identified as the predominate saturated fatty acid. The distribution of the major phospholipids, i. e., phosphatidylethanolamine, phosphatidic acid, phosphatidylserine, phosphatidylcholine, and lysophosphatidylcholine, was found to vary significantly among the hibiscus species examined. Phosphatidylcholine and lysophosphatidylcholine were the predominate phospholipids comprising between 50 and 95% of the total phospholipids present. Pressurized extraction techniques provide a rapid method to separate both polar and nonpolar lipids from Hibiscus seeds using carbon dioxide and ethanol mixtures. The seeds require a minimum of processing prior to extraction and the extracts obtained are solvent free and suitable for edible products.« less

Selective and cost-effective protocol to separate bioactive triterpene acids from plant matrices using alkalinized ethanol: Application to leaves of Myrtaceae species

PubMed Central

Lima, Adélia M. Belem; Siani, Antonio Carlos; Nakamura, Marcos Jun; D’Avila, Luiz Antonio

2015-01-01

Background: Triterpenes as betulinic (BA), oleanolic (OA) and ursolic acids (UA) have increasingly gained therapeutic relevance due to their wide scope of pharmacological activities. To fit large-scale demands, exploitable sources of these compounds have to be found and simple, cost-effective methods to extract them developed. Leaf material represents the best plant sustainable raw material. To obtain triterpene acid-rich extracts from leaves of Eugenia, Psidium and Syzygium species (Myrtaceae) by directly treating the dry plant material with alkalinized hydrated ethanol. This procedure was adapted from earlier methods to effect depolymerization of the leaf cutin. Materials and Methods: Extracts were prepared by shaking the milled dry leaves in freshly prepared 2% NaOH in 95% EtOH solution (1:4 w/v) at room temperature for 6 h. Working up the product in acidic aqueous medium led to clear precipitates in which BA, OA and UA were quantified by gas chromatography. Results: Pigment-free and low-polyphenol content extracts (1.2–2.8%) containing 6–50% of total triterpene acids were obtained for the six species assayed. UA (7–20%) predominated in most extracts, but BA preponderated in Eugenia florida (39%). Carried out in parallel, n-hexane defatted leaves led to up to 9% enhancement of total acids in the extracts. The hydroalcoholate treatment of Myrtaceae species dry leaves proved to be a cost-effective and environmentally friendly method to obtain triterpene acids, providing them be resistant to alkaline medium. These combined techniques might be applicable to other plant species and tissues. PMID:26246721

Determination of the asphaltene and carboxylic acid content of a heavy oil using a microfluidic device.

PubMed

Bowden, Stephen A; Wilson, Rab; Parnell, John; Cooper, Jonathan M

2009-03-21

Heavy oil utilisation is set to increase over the coming decades as reserves of conventional oil decline. Heavy oil differs from conventional oil in containing relatively large quantities of asphaltene and carboxylic acids. The proportions of these compounds greatly influence how oil behaves during production and its utilisation as a fuel or feedstock. We report the development of a microfluidic technique, based on a H-cell, that can extract the carboxylic acid components of an oil and assess its asphaltene content. Ultimately this technology could yield a field-deployable device capable of performing measurements that facilitate improved resource management at the point of resource-extraction.

Comparison of metabolic profiles and bioactivities of the leaves of three edible Congolese Hibiscus species.

PubMed

Kapepula, Paulin Mutwale; Kabamba Ngombe, Nadege; Tshisekedi Tshibangu, Pascal; Tsumbu, César; Franck, Thierry; Mouithys-Mickalad, Ange; Mumba, Dieudonné; Tshala-Katumbay, Désiré; Serteyn, Didier; Tits, Monique; Angenot, Luc; Kalenda, Pascal Dibungi T; Frédérich, Michel

2017-12-01

Methanolic and dichloromethane extracts from the leaves of Congolese Hibiscus species were characterised by chromatographic and spectroscopic techniques and their in vitro biochemical activities against ROS production were evaluated in cellular models and on an enzyme, myeloperoxidase (MPO), involved in inflammation. Hibiscus acetosella has a chemical fingerprint different from Hibiscus cannabinus and Hibiscus sabdariffa both having similar fingerprints. Major compounds were polyphenols, represented mainly by caffeoyl-hydroxycitric acid for H. acetosella and neochlorogenic acid for the two other species. All extracts displayed high cellular antioxidant activity with IC 50 values ranging from 0.5 to 3 μg mL -1 using lucigenin on neutrophils. Dichloromethane extracts showed more efficient effects on extracellular ROS production and MPO activity. Antioxidant and anti-inflammatory activities of caffeoyl-hydroxycitric acid were significantly higher than those of neochlorogenic acid. The bioactivities of Hibiscus species were positively correlated with their phytochemical content and could justify their use as local nutraceutical resources and medicines.

Isolation and structural characterization of sugarcane bagasse lignin after dilute phosphoric acid plus steam explosion pretreatment and its effect on cellulose hydrolysis.

PubMed

Zeng, Jijiao; Tong, Zhaohui; Wang, Letian; Zhu, J Y; Ingram, Lonnie

2014-02-01

The structure of lignin after dilute phosphoric acid plus steam explosion pretreatment process of sugarcane bagasse in a pilot scale and the effect of the lignin extracted by ethanol on subsequent cellulose hydrolysis were investigated. The lignin structural changes caused by pretreatment were identified using advanced nondestructive techniques such as gel permeation chromatography (GPC), quantitative (13)C, and 2-D nuclear magnetic resonance (NMR). The structural analysis revealed that ethanol extractable lignin preserved basic lignin structure, but had relatively lower amount of β-O-4 linkages, syringyl/guaiacyl units ratio (S/G), p-coumarate/ferulate ratio, and other ending structures. The results also indicated that approximately 8% of mass weight was extracted by pure ethanol. The bagasse after ethanol extraction had an approximate 22% higher glucose yield after enzyme hydrolysis compared to pretreated bagasse without extraction. Copyright © 2013 Elsevier Ltd. All rights reserved.

Isolation of linoleic acid as an estrogenic compound from the fruits of Vitex agnus-castus L. (chaste-berry).

PubMed

Liu, J; Burdette, J E; Sun, Y; Deng, S; Schlecht, S M; Zheng, W; Nikolic, D; Mahady, G; van Breemen, R B; Fong, H H S; Pezzuto, J M; Bolton, J L; Farnsworth, N R

2004-01-01

A methanol extract of chaste-tree berry (Vitex agnus-castus L.) was tested for its ability to displace radiolabeled estradiol from the binding site of estrogen receptors alpha (ERalpha) and beta (ERbeta). The extract at 46 +/- 3 microg/ml displaced 50% of estradiol from ERalpha and 64 +/- 4 microg/ml from ERbeta. Treatment of the ER+ hormone-dependent T47D:A18 breast cancer cell line with the extract induced up-regulation of ERbeta mRNA. Progesterone receptor (PR) mRNA was upregulated in the Ishikawa endometrial cancer cell line. However, chaste-tree berry extract did not induce estrogen-dependent alkaline phosphatase (AP) activity in Ishikawa cells. Bioassay-guided isolation, utilizing ER binding as a monitor, resulted in the isolation of linoleic acid as one possible estrogenic component of the extract. The use of pulsed ultrafiltration liquid chromatography-mass spectrometry, which is an affinity-based screening technique, also identified linoleic acid as an ER ligand based on its selective affinity, molecular weight, and retention time. Linoleic acid also stimulated mRNA ERbeta expression in T47D:A18 cells, PR expression in Ishikawa cells, but not AP activity in Ishikawa cells. These data suggest that linoleic acid from the fruits of Vitex agnus-castus can bind to estrogen receptors and induce certain estrogen inducible genes.

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.

Protein distribution in lupin protein isolates from Lupinus angustifolius L. prepared by various isolation techniques.

PubMed

Muranyi, Isabel S; Volke, Daniela; Hoffmann, Ralf; Eisner, Peter; Herfellner, Thomas; Brunnbauer, Markus; Koehler, Peter; Schweiggert-Weisz, Ute

2016-09-15

Differences in the protein distribution of various protein isolates from Lupinus angustifolius L. Vitabor were identified as affected by the isolation procedure (alkaline and/or salt-induced extraction followed by isoelectric and/or dilutive precipitation). Protein isolates extracted in alkaline solution showed higher protein yields (26.4-31.7%) compared to salt-induced extraction (19.8-30.0%) or combined alkaline and salt-induced extraction (23.3-25.6%). Chemical variations among the protein isolates especially occurred within the albumins. Protein isolates precipitated isoelectrically showed the highest contents, whereas protein isolates precipitated by dilutive showed the lowest contents of conglutin δ. Furthermore, the alkaline subunits of conglutin α and conglutin γ decreased during alkaline extraction compared to salt-induced extraction. A decrease in protein-bound polar and basic amino acids was shown after protein isolation. In contrast, the amounts of nonpolar, aliphatic, aromatic, hydroxylated and sulfur-rich amino acids were higher in the lupin protein isolates compared to the lupin flakes. However, the functional side chains could not be related to the specific molecular arrangements of the protein isolates, as a similar amino acid composition was found among the protein isolates. Copyright © 2016 Elsevier Ltd. All rights reserved.

The search for and identification of amino acids, nucleobases and nucleosides in samples returned from Mars

NASA Technical Reports Server (NTRS)

Gehrke, Charles W.; Ponnamperuma, Cyril; Kuo, Kenneth C.; Stalling, David L.; Zumwalt, Robert W.

1989-01-01

An investigation of the returned Mars samples for biologically important organic compounds, with emphasis on amino acid, the puring and pyrimidine bases, and nucleosides is proposed. These studies would be conducted on subsurface samples obtained by drilling past the surface oxidizing layer with emphasis on samples containing the larges quantities of organic carbon as determined by the rover gas chromatographic mass spectrometer (GCMS). Extraction of these molecules from the returned samples will be performed using the hydrothermal extraction technique described by Cheng and Ponnamperuma. More rigorous extraction methods will be developed and evaluated. For analysis of the extract for free amino acids or amino acids present in a bound or peptidic form, aliquots will be analyzed by capillary GCMS both before and after hydrolysis with 6N hydrochloric acid. Establishment of the presence of amino acids would then lead to the next logical step which would be the use of chiral stationary gas chromatography phases to determine the enatiomeic composition of the amino acids present, and thus potentially establish their biotic or abiotic origin. Confirmational analyses for amino acids would include ion-exchange and reversed-phase liquid chromatographic analysis. For analyses of the returned Mars samples for nucleobases and nucleosides, affinity and reversed-phase liquid chromatography would be utilized. This technology coupled with scanning UV detection for identification, presents a powerful tool for nucleobase and nucleoside analysis. Mass spectrometric analysis of these compounds would confirm their presence in samples returned form Mars.

A sialic acid assay in isolation and purification of bovine k-casein glycomacropeptide: a review.

PubMed

Nakano, Takuo; Ozimek, Lech

2014-01-01

Sialic acid is a carbohydrate moiety of k-casein glycomacropeptide (GMP), which is a 64 amino acid residue C-terminal sialylated phosphorylated glycopeptide released from k-casein by the action of chymosin during cheese making. GMP lacks aromatic amino acids including phenylalanine, tyrosine, and tryptophan. Because of its unique amino acid composition and various biological activities, GMP is thought to be a potential ingredient for dietetic foods (e.g., a food for PKU patients) and pharmaceuticals. Thus, increased attention has been given to the development of techniques to purify GMP. In this review, techniques of GMP purification described in patents and scientific research papers were introduced. A sialic acid assay is the important method to track GMP isolation and purification processes, for which the thiobarbituric acid reaction with 1-propanol as a chromophore extracting solvent is an inexpensive, practical and specific technique. Sephacryl S-200 gel filtration chromatography, cellulose acetate electrophoresis, and sodium dodecyl sulfate polyacrylamide gel electrophoresis are the major techniques to identify sialic acid specific to GMP. Sephacryl S-200 chromatography and cellulose acetate electrophoresis are also used to detect GMP sialic acid in whey pearmeate and whey added commercial margarine samples. Future research includes development of an economical industrial scale method to produce high purity GMP.

Chemical fractionation-enhanced structural characterization of marine dissolved organic matter

NASA Astrophysics Data System (ADS)

Arakawa, N.; Aluwihare, L.

2016-02-01

Describing the molecular fingerprint of dissolved organic matter (DOM) requires sample processing methods and separation techniques that can adequately minimize its complexity. We have employed acid hydrolysis as a way to make the subcomponents of marine solid phase-extracted (PPL) DOM more accessible to analytical techniques. Using a combination of NMR and chemical derivatization or reduction analyzed by comprehensive (GCxGC) gas chromatography, we observed chemical features strikingly similar to terrestrial DOM. In particular, we observed reduced alicylic hydrocarbons believed to be the backbone of previously identified carboxylic rich alicyclic material (CRAM). Additionally, we found carbohydrates, amino acids and small lipids and acids.

Determination of silver, bismuth, cadmium, copper, lead, and zinc in geologic materials by atomic absorption spectrometry with tricaprylylmethylammonium chloride

USGS Publications Warehouse

Viets, J.G.

1978-01-01

Interferences commonly encountered in the determination of silver, bismuth, cadmium, copper, lead, and zinc at crustal abundance levels are effectively eliminated using a rapid, sensitive, organic extraction technique. A potassium chlorate-hydrochloric acid digestion solubilizes the metals not tightly bound in the silicate lattice of rocks, soils, and stream sediments. The six metals are selectively extracted into a 10% Aliquat 336-MIBK organic phase in the presence of ascorbic acid and potassium iodide. Metals in the organic extract are determined by flame atomic absorption spectrometry to the 0.02-ppm level for silver, cadmium, copper, and zinc and to the 0.2-ppm level for bismuth and lead with a maximum relative standard deviation of 18.8% for known reference samples. An additional hydrofluoric acid digestion may be used to determine metals substituted in the silicate lattice.

Helleborus purpurascens-Amino Acid and Peptide Analysis Linked to the Chemical and Antiproliferative Properties of the Extracted Compounds.

PubMed

Segneanu, Adina-Elena; Grozescu, Ioan; Cziple, Florentina; Berki, Daniel; Damian, Daniel; Niculite, Cristina Mariana; Florea, Alexandru; Leabu, Mircea

2015-12-11

There is a strong drive worldwide to discover and exploit the therapeutic potential of a large variety of plants. In this work, an alcoholic extract of Helleborus purpurascens (family Ranunculaceae) was investigated for the identification of amino acids and peptides with putative antiproliferative effects. In our work, a separation strategy was developed using solvents of different polarity in order to obtain active compounds. Biochemical components were characterized through spectroscopic (mass spectroscopy) and chromatographic techniques (RP-HPLC and GC-MS). The biological activity of the obtained fractions was investigated in terms of their antiproliferative effects on HeLa cells. Through this study, we report an efficient separation of bioactive compounds (amino acids and peptides) from a plant extract dependent on solvent polarity, affording fractions with unaffected antiproliferative activities. Moreover, the two biologically tested fractions exerted a major antiproliferative effect, thereby suggesting potential anticancer therapeutic activity.

A reexamination of amino acids in lunar soil

NASA Technical Reports Server (NTRS)

Brinton, K. L. F.; Bada, J. L.; Arnold, J. R.

1993-01-01

Amino acids in lunar soils provide an important indicator of the level of prebiotic organic compounds on the moon. The results provide insight into the chemistry of amino acid precursors, and furthermore, given the flux of carbonaceous material to the moon, we can evaluate the survival of organics upon impact. The amino acid contents of both hydrolyzed and unhydrolyzed hot-water extracts of Apollo 17 lunar soil were determined using ophthaldialdehyde/N-acetyl cysteine (OPA/NAC) derivatization followed by HPLC analysis. Previous studies of lunar amino acids were inconclusive, as the technique used (derivatization with ninhydrin followed by HPLC analysis) was unable to discriminate between cosmogenic amino acids and terrestrial contaminants. Cosmogenic amino acids are racemic, and many of the amino acids found in carbonaceous meteorites such as Murchison, i.e., alpha-amino-i-butyric acid (aib), are extremely rare on Earth. The ninhydrin method does not distinguish amino acid enantiomers, nor does it detect alpha-alkyl amino acids such as aib, whereas the OPA/NAC technique does both.

Evaluation of Anticancer and Antioxidant Activity of a Commercially Available CO2 Supercritical Extract of Old Man's Beard (Usnea barbata).

PubMed

Zugic, Ana; Jeremic, Ivica; Isakovic, Aleksandra; Arsic, Ivana; Savic, Snezana; Tadic, Vanja

2016-01-01

There is a worldwide ongoing investigation for novel natural constituents with cytotoxic and antioxidant properties. The aim of this study was to investigate chemical profile and stated biological activities of the supercritical CO2 extract (SCE) of old man's beard compared to the extracts obtained using the conventional techniques (Soxhlet extracts and macerate). The most abundant compound identified was usnic acid, which content was inversely proportional to the polarity of the solvent used and was the highest in the SCE, which was the sample revealing the highest cytotoxic activity in tested tumor cell lines (B16 mouse melanoma and C6 rat glioma), with lower IC50 values compared to pure usnic acid. Further investigations suggested both SCE and usnic acid to induce apoptosis and/or autophagy in B16 and C6, indicating higher cytotoxicity of SCE to be related to the higher degree of ROS production. A good correlation of usnic acid content in the extracts and their antioxidant capacity was established, extricating SCE as the most active one. Presented results support further investigations of SCE of old man's beard as a prospective therapeutic agent with potential relevance in the treatment of cancer and/or in oxidative stress-mediated conditions.

Evaluation of Anticancer and Antioxidant Activity of a Commercially Available CO2 Supercritical Extract of Old Man’s Beard (Usnea barbata)

PubMed Central

Isakovic, Aleksandra; Arsic, Ivana; Savic, Snezana; Tadic, Vanja

2016-01-01

There is a worldwide ongoing investigation for novel natural constituents with cytotoxic and antioxidant properties. The aim of this study was to investigate chemical profile and stated biological activities of the supercritical CO2 extract (SCE) of old man’s beard compared to the extracts obtained using the conventional techniques (Soxhlet extracts and macerate). The most abundant compound identified was usnic acid, which content was inversely proportional to the polarity of the solvent used and was the highest in the SCE, which was the sample revealing the highest cytotoxic activity in tested tumor cell lines (B16 mouse melanoma and C6 rat glioma), with lower IC50 values compared to pure usnic acid. Further investigations suggested both SCE and usnic acid to induce apoptosis and/or autophagy in B16 and C6, indicating higher cytotoxicity of SCE to be related to the higher degree of ROS production. A good correlation of usnic acid content in the extracts and their antioxidant capacity was established, extricating SCE as the most active one. Presented results support further investigations of SCE of old man’s beard as a prospective therapeutic agent with potential relevance in the treatment of cancer and/or in oxidative stress-mediated conditions. PMID:26745885

Profiling the Fatty Acids Content of Ornamental Camellia Seeds Cultivated in Galicia by an Optimized Matrix Solid-Phase Dispersion Extraction

PubMed Central

Garcia-Jares, Carmen; Sanchez-Nande, Marta; Lamas, Juan Pablo; Lores, Marta

2017-01-01

Camellia (genus of flowering plants of fam. Theaceae) is one of the main crops in Asia, where tea and oil from leaves and seeds have been utilized for thousands of years. This plant is excellently adapted to the climate and soil of Galicia (northwestern Spain) and northern Portugal where it is grown not only as an ornamental plant, but to be evaluated as a source of bioactive compounds. In this work, the main fatty acids were extracted from Camellia seeds of four varieties of Camellia: sasanqua, reticulata, japonica and sinensis, by means of matrix-solid phase dispersion (MSPD), and analyzed by gas chromatography (GC) with MS detection of the corresponding methyl esters. MSPD constitutes an efficient and greener alternative to conventional extraction techniques, moreover if it is combined with the use of green solvents such as limonene. The optimization of the MSPD extraction procedure has been conducted using a multivariate approach based on strategies of experimental design, which enabled the simultaneous evaluation of the factors influencing the extraction efficiency as well as interactions between factors. The optimized method was applied to characterize the fatty acids profiles of four Camellia varieties seeds, allowing us to compare their fatty acid composition. PMID:29039745

Phenolic compounds from the leaf extract of artichoke (Cynara scolymus L.) and their antimicrobial activities.

PubMed

Zhu, Xianfeng; Zhang, Hongxun; Lo, Raymond

2004-12-01

A preliminary antimicrobial disk assay of chloroform, ethyl acetate, and n-butanol extracts of artichoke (Cynara scolymus L.) leaf extracts showed that the n-butanol fraction exhibited the most significant antimicrobial activities against seven bacteria species, four yeasts, and four molds. Eight phenolic compounds were isolated from the n-butanol soluble fraction of artichoke leaf extracts. On the basis of high-performance liquid chromatography/electrospray ionization mass spectrometry, tandem mass spectrometry, and nuclear magnetic resonance techniques, the structures of the isolated compounds were determined as the four caffeoylquinic acid derivatives, chlorogenic acid (1), cynarin (2), 3,5-di-O-caffeoylquinic acid (3), and 4,5-di-O-caffeoylquinic acid (4), and the four flavonoids, luteolin-7-rutinoside (5), cynaroside (6), apigenin-7-rutinoside (7), and apigenin-7-O-beta-D-glucopyranoside (8), respectively. The isolated compounds were examined for their antimicrobial activities on the above microorganisms, indicating that all eight phenolic compounds showed activity against most of the tested organisms. Among them, chlorogenic acid, cynarin, luteolin-7-rutinoside, and cynaroside exhibited a relatively higher activity than other compounds; in addition, they were more effective against fungi than bacteria. The minimum inhibitory concentrations of these compounds were between 50 and 200 microg/mL.

High-throughput method based on quick, easy, cheap, effective, rugged and safe followed by liquid chromatography-multi-wavelength detection for the quantification of multiclass polyphenols in wines.

PubMed

Fontana, Ariel R; Bottini, Rubén

2014-05-16

In this work, a reliable, simple, fast, inexpensive and robust sample preparation approach for the determination of multiclass polyphenols in wine samples is proposed. The polyphenols selected for this work were gallic acid, (+)-catechin, (-)-epicatechin, caffeic acid, syringic acid, coumaric acid, ferulic acid, trans-resveratrol, quercetin and cinnamic acid. The method is based on QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction technique coupled with dispersive solid-phase extraction (d-SPE) clean-up. Under optimized conditions, the analytes were extracted from 5mL wine samples (previously acidified with 1% formic acid) using 2.5mL acetonitrile. For phase separation, 1.5g NaCl and 4g anhydrous MgSO4 were added. Then, a 1mL aliquot of the partitioned supernatant was cleaned-up using d-SPE with a combination of 150mg CaCl2, 50mg primary-secondary amine (PSA) and 50mgC18 as sorbents. A 250μL aliquot of the obtained cleaned extract was concentrated to dryness and taken up with the initial mobile phase previous to liquid chromatography-multi-wavelength detection (LC-MWD). The proposed method provided limits of detection (LODs) ranging from 0.004 to 0.079μgmL(-1) and an inter-day variability below 12% RSD for all analytes in red and white wine samples. Considering external calibration (red wines) and matrix-matched calibration (white wines) as quantification techniques, the overall recoveries (accuracy) of the method ranged between 75.0% and 119.6% for red and white wine samples, respectively. The developed method was applied for the determination of polyphenols in 10 wines produced in Argentina. Nine phenolic compounds were determined, at concentrations above detectable levels in the method. The maximum concentrations corresponded to (-)-epicatechin in white wines, while gallic acid and (+)-catechin were the most abundant in red wines. Copyright © 2014 Elsevier B.V. All rights reserved.

Supercritical fluid extraction of grape seeds: extract chemical composition, antioxidant activity and inhibition of nitrite production in LPS-stimulated Raw 264.7 cells.

PubMed

Pérez, Concepción; Ruiz del Castillo, María Luisa; Gil, Carmen; Blanch, Gracia Patricia; Flores, Gema

2015-08-01

Grape by-products are a rich source of bioactive compounds having broad medicinal properties, but are usually wasted from juice/wine processing industries. The present study investigates the use of supercritical fluid extraction (SFE) for obtaining an extract rich in bioactive compounds. First, some variables involved in the extraction were applied. SFE conditions were selected based on the oil mass yield, fatty acid profile and total phenolic composition. As a result, 40 °C and 300 bar were selected as operational conditions. The phenolic composition of the grape seed oil was determined using LC-DAD. The antioxidant activity was determined by ABTS and DPPH assays. For the anti-inflammatory activity the inhibition of nitrite production was assessed. The grape seed oil extracted was rich in phenolic compounds and fatty acids with significant antioxidant and anti-inflammatory activities. From these results, added economic value to this agroindustrial residue is proposed using environmentally friendly techniques.

Nutritional and Biochemical Profiling of Leucopaxillus candidus (Bres.) Singer Wild Mushroom.

PubMed

Vieira, Vanessa; Barros, Lillian; Martins, Anabela; Ferreira, Isabel C F R

2016-01-15

The wild mushroom Leucopaxillus candidus (Bres.) Singer was studied for the first time to obtain information about its chemical composition, nutritional value and bioactivity. Free sugars, fatty acids, tocopherols, organic and phenolic acids were analysed by chromatographic techniques coupled to different detectors. L. candidus methanolic extract was tested regarding antioxidant potential (reducing power, radical scavenging activity and lipid peroxidation inhibition). L. candidus was shown to be an interesting species in terms of nutritional value, with high content in proteins and carbohydrates, but low fat levels, with the prevalence of polyunsaturated fatty acids. Mannitol was the most abundant free sugar and β-tocopherol was the main tocopherol isoform. Other compounds detected were oxalic and fumaric acids, p-hydroxybenzoic and cinnamic acids. The methanolic extract revealed antioxidant activity and did not show hepatoxicity in porcine liver primary cells. The present study provides new information about L. candidus.

A green analytical chemistry approach for lipid extraction: computation methods in the selection of green solvents as alternative to hexane.

PubMed

Cascant, Mari Merce; Breil, Cassandra; Garrigues, Salvador; de la Guardia, Miguel; Fabiano-Tixier, Anne Silvie; Chemat, Farid

2017-05-01

There is a great interest in finding alternatives and green solvents in extraction processes to replace petroleum based solvents. In order to investigate these possibilities, computational methods, as Hansen solubility parameters (HSP) and conductor-like screening model for real solvent (COSMO-RS), were used in this work to predict the solvation power of a series of solvents in salmon fish lipids. Additionally, experimental studies were used to evaluate the performance in lipids extraction using 2-methyltetrahydrofurane, cyclopentyl methyl ether, dimethyl carbonate, isopropanol, ethanol, ethyl acetate, p-cymene and d-limonene compared with hexane. Lipid classes of extracts were obtained by using high performance thin-layer chromatography (HPTLC), whereas gas chromatography with a flame ionization detector (GC/FID) technique was employed to obtain fatty acid profiles. Some differences between theoretical and experimental results were observed, especially regarding the behavior of p-cymene and d-limonene, which separate from the predicted capability. Results obtained from HPTLC indicated that p-cymene and d-limonene extract triglycerides (TAGs) and diglycerides (DAGs) at levels of 73 and 19%, respectively, whereas the other studied extracts contain between 75 and 76% of TAGs and between 16 and 17% of DAGs. Fatty acid profiles, obtained by using GC-FID, indicated that saturated fatty acids (SFAs) between 19.5 and 19.9% of extracted oil, monounsaturated fatty acids (MUFAs) in the range between 43.5 and 44.9%, and PUFAs between 31.2 and 34.6% were extracted. p-Cymene and limonene extracts contained lower percentages than the other studied solvents of some PUFAs due probably to the fact that these unsaturated fatty acids are more susceptible to oxidative degradation than MUFAs. Ethyl acetate has been found to be the best alternative solvent to hexane for the extraction of salmon oil lipids. Graphical Abstract ᅟ.

Supercritical fluid extraction of peach (Prunus persica) almond oil: process yield and extract composition.

PubMed

Mezzomo, Natália; Mileo, Bruna R; Friedrich, Maria T; Martínez, Julian; Ferreira, Sandra R S

2010-07-01

Peach kernels are industrial residues from the peach processing, contain oil with important therapeutic properties and attractive nutritional aspects because of the high concentration of oleic and linoleic acids. The extraction method used to obtain natural compounds from raw matter is critical for product quality definition. Thus, the aim of this work was to compare peach almond extraction yields obtained by different procedures: soxhlet extractions (Sox) with different solvents; hydrodistillation (HD); ethanolic maceration (Mac) followed by fractionation with various solvents, and supercritical fluid extraction (SFE) at 30, 40 and 50 degrees C and at 100, 200 and 300bar, performed with pure CO(2) and with a co-solvent. The extracts were evaluated with respect to fatty acid composition (FAC), fractionated chemical profile (FCP) and total phenolic content (TPC). The Sox total yields were generally higher than those obtained by SFE. The crossover pressure for SFE was between 260 and 280bar. The FAC results show oleic and linoleic acids as main components, especially for Sox and SFE extracts. The FCP for samples obtained by Sox and Mac indicated the presence of benzaldehyde and benzyl alcohol, components responsible for almond flavor and with important industrial uses, whereas the SFE extracts present a high content of a possible flavonoid. The higher TPC values were obtained by Sox and Mac with ethanol. In general, the maximum pressure in SFE produced the highest yield, TPC and oleic acid content. The use of ethanol at 5% as co-solvent in SFE did not result in a significant effect on any evaluated parameter. The production of peach almond oil through all techniques is substantially adequate and SFE presented advantages, with respect to the quality of the extracts due to the high oleic acid content, as presented by some Sox samples. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

Application of a simple column-switching ion chromatography technique for removal of matrix interferences and sensitive fluorescence determination of acidic compounds (pharmaceutical drugs) in complex samples.

PubMed

Muhammad, Nadeem; Subhani, Qamar; Wang, Fenglian; Guo, Dandan; Zhao, Qiming; Wu, Shuchao; Zhu, Yan

2017-09-15

This work illustrates the introduction of a simple, rugged and flexible column-switching ion chromatography (IC) technique for an automated on-line QuEChERS extracted samples extracts washing followed by sensitive fluorescence (FLD) determination of five acidic pharmaceutical drugs namely; clofibric acid (CLO), ibuprofen (IBU), aspirin (ASP), naproxen (NAP) and flurobrofen (FLU) in three complex samples (spinach, apple and hospital sewage sludge). An old anion exchange column IonPac ® AS11-HC was utilized as a pre-treatment column for on-line washing of inorganic and organic interferences followed by isocratic separation of five acidic drugs with another anion exchange IonPac ® AS12A analytical column by exploiting the column-switching technique. This novel method exhibited good linearity with correlation coefficients (r 2 ) for all drugs were in the range 0.976-0.996. The limit of detection and quantification of all five acidic drugs were in the range 0.024μg/kg to 8.70μg/kg and 0.082μg/kg to 0.029mg/kg, respectively, and better recoveries in the range 81.17-112.5% with percentage relative standard deviations (RSDs) less than 17.8% were obtained. This on-line sample pre-treatment method showed minimum matrix effect in the range of 0.87-1.25 except for aspirin. This simple rugged and flexible column-switching system required only 28min for maximum elimination of matrices and interferences in three complex samples extracts, isocratic separation of five acidic drugs and for the continuous regeneration of pre-treatment column prior to every subsequent analysis. Finally, this simple automated IC system was appeared so rugged and flexible, which can eliminate and wash out most of interference, impurities and matrices in complex samples, simply by adjusting the NaOH and acetonitrile concentration in washing mobile phase with maximum recoveries of acidic analytes of interest. Copyright © 2017. Published by Elsevier B.V.

Influence of solution acidity and CaCl2 concentration on the removal of heavy metals from metal-contaminated rice soils.

PubMed

Kuo, S; Lai, M S; Lin, C W

2006-12-01

Soil washing is considered a useful technique for remediating metal-contaminated soils. This study examined the release edges of Cd, Zn, Ni, Cr, Cu or Pb in two contaminated rice soils from central Taiwan. The concentrations exceeding the trigger levels established by the regulatory agency of Taiwan were Cu, Zn, Ni and Cr for the Ho-Mei soil and Pb for the Nan-Tou soil. Successive extractions with HCl ranging from 0 to 0.2 M showed increased release of the heavy metals with declining pH, and the threshold pH value below which a sharp increase in the releases of the heavy metals was highest for Cd, Zn, and Ni (pH 4.6 to 4.9), intermediate for Pb and Cu (3.1 to 3.8) and lowest for Fe (2.1), Al (2.2) and Cr (1.7) for the soils. The low response slope of Ni and Cr particularly for the rice soils make soil washing with the acid up to the highest concentration used ineffective to reduce their concentrations to below trigger levels. Although soil washing with 0.1 M HCl was moderately effective in reducing Cu, Pb, Zn and Cd, which brought pH of the soils to 1.1+/-0.1 (S.D.), the concurrent release of large quantities of Fe and Al make this remediation technique undesirable for the rice soils containing high clay. Successive washings with 0.01 M HCl could be considered an alternative as the dissolution of Fe and Al was minimal, and between 46 to 64% of Cd, Zn, and Cu for the Ho-Mei soil and 45% of Pb in the Na-Tou soil were extracted after four successive extractions with this dilute acid solution. The efficacy of Cd extraction improved if CaCl2 was added to the acid solution. The correlation analysis revealed that Cr extracted was highly correlated (P < 0.001) with Fe extracted, whereas the Cu, Ni, Zn, Cd or Pb extracted was better correlated (P < 0.001) with Al than with Fe extracted. It is possible that the past seasonal soil flooding and drainage in the soils for rice production was conducive to incorporating Cr within the structure of Fe oxide, thereby making them extremely insoluble even in 0.2 M HCl solution. The formation of solid solution of Ni with Al oxide was also possible, making it far less extractable than Cd, Zn, Cu, or Pb with the acid concentrations used.

Determination of flavonoids in Triticum aestivum L. treated with ampicillin

NASA Astrophysics Data System (ADS)

Soran, M. L.; Opriş, O.; Copaciu, F.; Varodi, C.

2012-02-01

Pharmaceutical residues in the environment, and their potential toxic effects, have been recognized as one of the emerging research area in the environmental chemistry. Antibiotics can reach plants from treated soil or due to irrigation. The flavonoids extraction from Triticum aestivum L. treated with ampicillin and separation of flavonoids are presented in this study. There were used classical and modern extraction techniques (maceration, microwave assisted solvents, etc). The efficiency of extraction process was spectrophotometricaly evaluated by determining the total flavonoids content and by HPTLC on silica gel plates using the mixture: carbon tetrachloride - acetone - formic acid (35:11:3, v/v) as mobile phase. The developed plates were inspected both in ultraviolet and visible after visualization with NTS reagent (diphenylboryloxyethylamin). The chromatographic plates were compared in respect to determine the changes in extract composition due to the different extraction techniques. Depending on the concentration of ampicillin administered to plants, comparative studies on flavonoids content were performed.

Application of eggshell waste for the immobilization of cadmium and lead in a contaminated soil.

PubMed

Ok, Yong Sik; Lee, Sang Soo; Jeon, Weon-Tai; Oh, Sang-Eun; Usman, Adel R A; Moon, Deok Hyun

2011-01-01

Liming materials have been used to immobilize heavy metals in contaminated soils. However, no studies have evaluated the use of eggshell waste as a source of calcium carbonate (CaCO₃) to immobilize both cadmium (Cd) and lead (Pb) in soils. This study was conducted to evaluate the effectiveness of eggshell waste on the immobilization of Cd and Pb and to determine the metal availability following various single extraction techniques. Incubation experiments were conducted by mixing 0-5% powdered eggshell waste and curing the soil (1,246 mg Pb kg⁻¹ soil and 17 mg Cd kg⁻¹ soil) for 30 days. Five extractants, 0.01 M calcium chloride (CaCl₂), 1 M CaCl₂, 0.1 M hydrochloric acid (HCl), 0.43 M acetic acid (CH₃COOH), and 0.05 M ethylendiaminetetraacetic acid (EDTA), were used to determine the extractability of Cd and Pb following treatments with CaCO₃ and eggshell waste. Generally, the extractability of Cd and Pb in the soils decreased in response to treatments with CaCO₃ and eggshell waste, regardless of extractant. Using CaCl₂ extraction, the lowest Cd concentration was achieved upon both CaCO₃ and eggshell waste treatments, while the lowest Pb concentration was observed using HCl extraction. The highest amount of immobilized Cd and Pb was extracted by CH₃COOH or EDTA in soils treated with CaCO₃ and eggshell waste, indicating that remobilization of Cd and Pb may occur under acidic conditions. Based on the findings obtained, eggshell waste can be used as an alternative to CaCO₃ for the immobilization of heavy metals in soils.

Turkish Scorzonera Species Extracts Attenuate Cytokine Secretion via Inhibition of NF-κB Activation, Showing Anti-Inflammatory Effect in Vitro.

PubMed

Bahadır Acikara, Özlem; Hošek, Jan; Babula, Petr; Cvačka, Josef; Budešínský, Miloš; Dračinský, Martin; Saltan İşcan, Gülçin; Kadlecová, Daniela; Ballová, Ludmila; Šmejkal, Karel

2015-12-30

Scorzonera species are used in different folk medicines to combat many diseases, including the illnesses connected with inflammation. Previous experiments showed anti-inflammatory activity of Scorzonera extracts in vivo. S. latifolia, S. cana var. jacquiniana, S. tomentosa, S. mollis ssp. szowitsii, S. eriophora, S. incisa, S. cinerea, and S. parviflora extracts were, therefore, evaluated for their inhibitory activities of TNF-α and IL-1β production, and NF-κB nuclear translocation in THP-1 macrophages. The HPLC analysis was carried out to elucidate and to compare the composition of these extracts. Major compounds of the tested extracts have been isolated using different chromatographic techniques and further tested for their inhibitory activities on TNF-α and IL-1β production. Several extracts showed promising anti-inflammatory activity in these in vitro tests. Results of HPLC analysis revealed chlorogenic acid as a compound present in all tested extracts. Hyperoside, quercetin-3-O-β-d-glucoside and rutin were also present in varying amount in some Scorzonera species analyzed. Furthermore, eight phenolics which were identified as quercetin-3-O-β-d-glucoside (1), hyperoside (2), hydrangenol-8-O-glucoside (3), swertisin (4), 7-methylisoorientin (5), 4,5-O-dicaffeoyl-quinic acid (6), 3,5-di-O-caffeoyl-quinic acid (7), and chlorogenic acid (8) have been isolated as major phenolic compounds of the tested extracts and, together with eight terpenoids (9-16) previously obtained from different Scorzonera species, have been tested for the inhibition of TNF-α production, unfortunately with no activity comparable with standard.

In-tube extraction and GC-MS analysis of volatile components from wild and cultivated sea buckthorn (Hippophae rhamnoides L. ssp. Carpatica) berry varieties and juice.

PubMed

Socaci, Sonia A; Socaciu, Carmen; Tofană, Maria; Raţi, Ioan V; Pintea, Adela

2013-01-01

The health benefits of sea buckthorn (Hippophae rhamnoides L.) are well documented due to its rich content in bioactive phytochemicals (pigments, phenolics and vitamins) as well as volatiles responsible for specific flavours and bacteriostatic action. The volatile compounds are good biomarkers of berry freshness, quality and authenticity. To develop a fast and efficient GC-MS method including a minimal sample preparation technique (in-tube extraction, ITEX) for the discrimination of sea buckthorn varieties based on their chromatographic volatile fingerprint. Twelve sea buckthorn varieties (wild and cultivated) were collected from forestry departments and experimental fields, respectively. The extraction of volatile compounds was performed using the ITEX technique whereas separation and identification was performed using a GC-MS QP-2010. Principal component analysis (PCA) was applied to discriminate the differences among sample composition. Using GC-MS analysis, from the headspace of sea buckthorn samples, 46 volatile compounds were separated with 43 being identified. The most abundant derivatives were ethyl esters of 2-methylbutanoic acid, 3-methylbutanoic acid, hexanoic acid, octanoic acid and butanoic acid, as well as 3-methylbutyl 3-methylbutanoate, 3-methylbutyl 2-methylbutanoate and benzoic acid ethyl ester (over 80% of all volatile compounds). Principal component analysis showed that the first two components explain 79% of data variance, demonstrating a good discrimination between samples. A reliable, fast and eco-friendly ITEX/GC-MS method was applied to fingerprint the volatile profile and to discriminate between wild and cultivated sea buckthorn berries originating from the Carpathians, with relevance to food science and technology. Copyright © 2013 John Wiley & Sons, Ltd.

Method of simultaneous stir bar sorptive extraction of phenethylamines and THC metabolite from urine.

PubMed

Goto, Yoshiyuki; Takeda, Shiho; Araki, Toshinori; Fuchigami, Takayuki

2011-10-01

Stir bar sorptive extraction is a technique used for extracting target substances from various aqueous matrixes such as environmental water, food, and biological samples. This type of extraction is carried out by rotating a coated stir bar is rotated in the sample solution. In particular, Twister bar is a commercial stir bar that is coated with polydimethylsiloxane (PDMS) and used to perform sorptive extraction. In this study, we developed a method for simultaneous detection of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and a Δ(9)-tetrahydrocannabiniol (THC) metabolite in human urine. For extracting the target analytes, the Twister bar was simply stirred in the sample in the presence of a derivatizing agent. Using this technique, phenethylamines and the acidic THC metabolite can be simultaneously extracted from human urine. This method also enables the extraction of trace amounts of these substances with good reproducibility and high selectivity. The proposed method offers many advantages over other extraction-based approaches and is therefore well suited for screening psychoactive substances in urine specimens.

Removal of arsenic from Janghang smelter site and energy crops-grown soil with soil washing using magnetic iron oxide

NASA Astrophysics Data System (ADS)

Han, Jaemaro; Zhao, Xin; Lee, Jong Keun; Kim, Jae Young

2014-05-01

Arsenic compounds are considered carcinogen and easily enter drinking water supplies with their natural abundance. US Environmental Protection Agency is finalizing a regulation to reduce the public health risks from arsenic in drinking water by revising the current drinking water standard for arsenic from 50 ppb to 10 ppb in 2001 (USEPA, 2001). Therefore, soil remediation is also growing field to prevent contamination of groundwater as well as crop cultivation. Soil washing is adjusted as ex-situ soil remediation technique which reduces volume of the contaminated soil. The technique is composed of physical separation and chemical extraction to extract target metal contamination in the soil. Chemical extraction methods have been developed solubilizing contaminants containing reagents such as acids or chelating agents. And acid extraction is proven as the most commonly used technology to treat heavy metals in soil, sediment, and sludge (FRTR, 2007). Due to the unique physical and chemical properties, magnetic iron oxide have been used in diverse areas including information technology and biomedicine. Magnetic iron oxides also can be used as adsorbent to heavy metal enhancing removal efficiency of arsenic concentration. In this study, magnetite is used as the washing agent with acid extraction condition so that the injected oxide can be separated by magnetic field. Soil samples were collected from three separate areas in the Janghang smelter site and energy crops-grown soil to have synergy effect with phytoremediation. Each sample was air-dried and sieved (2mm). Soil washing condition was adjusted on pH in the range of 0-12 with hydrogen chloride and sodium hydroxide. After performing soil washing procedure, arsenic-extracted samples were analyzed for arsenic concentration by inductively coupled plasma optical emission spectrometer (ICP-OES). All the soils have exceeded worrisome level of soil contamination for region 1 (25mg/kg) so the soil remediation techniques are needed to be applied. The objective of this study is to investigate soil washing efficiency using magnetic iron oxide and derive the availability of the washing technique to the arsenic-contaminated field soils. Acknowledgement This study was supported by Korea Ministry of Environment as 'Knowledge-based environmental service (Waste to Energy) Human Resource Development Project'.

Evaluating bis(2-ethylhexyl) methanediphosphonic acid (H 2DEH[MDP]) based polymer ligand film (PLF) for plutonium and uranium extraction

DOE PAGES

Rim, Jung H.; Armenta, Claudine E.; Gonzales, Edward R.; ...

2015-09-12

This paper describes a new analyte extraction medium called polymer ligand film (PLF) that was developed to rapidly extract radionuclides. PLF is a polymer medium with ligands incorporated in its matrix that selectively and quickly extracts analytes. The main focus of the new technique is to shorten and simplify the procedure for chemically isolating radionuclides for determination through alpha spectroscopy. The PLF system was effective for plutonium and uranium extraction. The PLF was capable of co-extracting or selectively extracting plutonium over uranium depending on the PLF composition. As a result, the PLF and electrodeposited samples had similar alpha spectra resolutions.

Changes in the amino acid profiles and free radical scavenging activities of Tenebrio molitor larvae following enzymatic hydrolysis.

PubMed

Tang, Yujiao; Debnath, Trishna; Choi, Eun-Ju; Kim, Young Wook; Ryu, Jung Pyo; Jang, Sejin; Chung, Sang Uk; Choi, Young-Jin; Kim, Eun-Kyung

2018-01-01

Tenebrio molitor (T. molitor) larvae provide food at low environmental cost and contribute positively to livelihoods. In this research, we compared the amino acids compositions and antioxidant activities of various extracts of T. molitor to enhance their quality as food. For the comparison, distilled water extracts, enzymatic hydrolysates, and condensed enzymatic hydrolysates of T. molitor larvae were prepared. Their amino acids (AAs) profiles and antioxidant activities, including ferric-reducing antioxidant power, oxygen radical absorption capacity, and DPPH, hydroxyl radical, and hydrogen peroxide radical scavenging properties assay were analyzed. DW extracts had the lowest AAs contents and antioxidant activity compared with enzymatic extracts. Condensed hydrolysates with a combination of alcalase and flavourzyme (C-A+F) exhibited the highest levels of total free AAs (11.1759 g/100 g). C-A+F produced higher total hydrolyzed AAs (32.5292 g/100 g) compared with the other groups. The C-A+F possessed the strongest antioxidant activity. Notably, the antioxidant activities of the hydrolysates and the total hydrolyzed AAs amount were correlated. Taken together, our findings showed that C-A+F was a promising technique for obtaining extracts of T. molitor larvae with antioxidant activity as potential nutritious functional food.

Application of ionic liquids based enzyme-assisted extraction of chlorogenic acid from Eucommia ulmoides leaves.

PubMed

Liu, Tingting; Sui, Xiaoyu; Li, Li; Zhang, Jie; Liang, Xin; Li, Wenjing; Zhang, Honglian; Fu, Shuang

2016-01-15

A new approach for ionic liquid based enzyme-assisted extraction (ILEAE) of chlorogenic acid (CGA) from Eucommia ulmoides is presented in which enzyme pretreatment was used in ionic liquids aqueous media to enhance extraction yield. For this purpose, the solubility of CGA and the activity of cellulase were investigated in eight 1-alkyl-3-methylimidazolium ionic liquids. Cellulase in 0.5 M [C6mim]Br aqueous solution was found to provide better performance in extraction. The factors of ILEAE procedures including extraction time, extraction phase pH, extraction temperatures and enzyme concentrations were investigated. Moreover, the novel developed approach offered advantages in term of yield and efficiency compared with other conventional extraction techniques. Scanning electronic microscopy of plant samples indicated that cellulase treated cell wall in ionic liquid solution was subjected to extract, which led to more efficient extraction by reducing mass transfer barrier. The proposed ILEAE method would develope a continuous process for enzyme-assisted extraction including enzyme incubation and solvent extraction process. In this research, we propose a novel view for enzyme-assisted extraction of plant active component, besides concentrating on enzyme facilitated cell wall degradation, focusing on improvement of bad permeability of ionic liquids solutions. Copyright © 2015 Elsevier B.V. All rights reserved.

Microwave-assisted extraction of silkworm pupal oil and evaluation of its fatty acid composition, physicochemical properties and antioxidant activities.

PubMed

Hu, Bin; Li, Cheng; Zhang, Zhiqing; Zhao, Qing; Zhu, Yadong; Su, Zhao; Chen, Yizi

2017-09-15

Microwave-assisted extraction (MAE) of oil from silkworm pupae was firstly performed in the present research. The response surface methodology was applied to optimize the parameters for MAE. The yield of oil by MAE was 30.16% under optimal conditions of a mixed solvent consisting of ethanol and n-hexane (1:1, v/v), microwave power (360W), liquid to solid ratio (7.5/1mL/g), microwave time (29min). Moreover, oil extracted by MAE was quantitatively (yield) and qualitatively (fatty acid profile) similar to those obtained using Soxhlet extraction (SE), but oil extracted by MAE exhibited favourable physicochemical properties and oxidation stability. Additionally, oil extracted by MAE had a higher content of total phenolic, and it showed stronger antioxidant activities. Scanning electron microscopy revealed that microwave technique efficiently promoted the release of oil by breaking down the cell structure of silkworm pupae. Therefore, MAE can be an effective method for the silkworm pupal oil extraction. Copyright © 2017 Elsevier Ltd. All rights reserved.

Integrated sample-to-detection chip for nucleic acid test assays.

PubMed

Prakash, R; Pabbaraju, K; Wong, S; Tellier, R; Kaler, K V I S

2016-06-01

Nucleic acid based diagnostic techniques are routinely used for the detection of infectious agents. Most of these assays rely on nucleic acid extraction platforms for the extraction and purification of nucleic acids and a separate real-time PCR platform for quantitative nucleic acid amplification tests (NATs). Several microfluidic lab on chip (LOC) technologies have been developed, where mechanical and chemical methods are used for the extraction and purification of nucleic acids. Microfluidic technologies have also been effectively utilized for chip based real-time PCR assays. However, there are few examples of microfluidic systems which have successfully integrated these two key processes. In this study, we have implemented an electro-actuation based LOC micro-device that leverages multi-frequency actuation of samples and reagents droplets for chip based nucleic acid extraction and real-time, reverse transcription (RT) PCR (qRT-PCR) amplification from clinical samples. Our prototype micro-device combines chemical lysis with electric field assisted isolation of nucleic acid in a four channel parallel processing scheme. Furthermore, a four channel parallel qRT-PCR amplification and detection assay is integrated to deliver the sample-to-detection NAT chip. The NAT chip combines dielectrophoresis and electrostatic/electrowetting actuation methods with resistive micro-heaters and temperature sensors to perform chip based integrated NATs. The two chip modules have been validated using different panels of clinical samples and their performance compared with standard platforms. This study has established that our integrated NAT chip system has a sensitivity and specificity comparable to that of the standard platforms while providing up to 10 fold reduction in sample/reagent volumes.

Determine kind and concentration of eliotropiumsuaveolens, Plantagomajorand Silybummarianum plants ingredients and its effect on some plant pathogenic fungi

NASA Astrophysics Data System (ADS)

Abdlrahmaan, A. J.; Raheem, I. A. Abdul; Latef, R. H.

2018-05-01

A study was conducted in the biology laboratories at Tikrit University to determine the ingredients of three local plants Heliotropiumsuaveolens, Plantagomajor and Silybummarianum and the effect of its extracts on the growth of fungus Fusariumsolani, Fusariumoxysporum and Alternariaalternate. Results analysis by High Performance Liquid Chromotographyte (HPLC) technique showed H. suaveolensplant contain alkaioidic compounds indicine 9.52%, supinine 3.95%, indicine-N-oxide 14.66%, heleurine 33.0%.heliotrine 31.88% and lidelofidine 6.95% and plantago major plant contain salysilic acid 34.93%, kampferol 4.55%, gentisic acid 2.72%, vanilic acid 1.67%, chlorogenetic acid 0.70%, coumaric acid 8.59%, ferulic acid 21.42% and aucubin 9.12%. While S. marinum contained salichristin A 42.24%, salichristin B 14.89%, salidianin 30.23%, silybins A 3.30%, silybins B 2.74%, isosilybins A 4.86% and isosilybins B 1.71%. Extract 20 concentration of H. suavelones and P. major showed high inhibition reached 100%. While S. marinum showed no effect on fungus growth.

Isolation of Purines and Pyrimidines from the Murchison Meteorite Using Sublimation

NASA Technical Reports Server (NTRS)

Glavin, D. P.; Bada, J. L.

2004-01-01

The origin of life on Earth, and possibly on other planets such as Mars, would have required the presence of liquid water and a continuous supply of prebiotic organic compounds. The exogenous delivery of organic matter by asteroids, comets, and carbonaceous meteorites could have contributed to the early Earth s prebiotic inventory by seeding the planet with biologically important organic compounds. A wide variety of prebiotic organic compounds have previously been detected in the Murchison CM type carbonaceous chondrite including amino acids, purines and pyrimidines. These compounds dominate terrestrial biochemistry and are integral components of proteins, DNA and RNA. Several purines including adenine, guanine, hypoxanthine, and xanthine, as well as the pyrimidine uracil, have previously been detected in water or formic acid extracts of Murchison using ion-exclusion chromatography and ultraviolet spectroscopy. However, even after purification of these extracts, the accurate identification and quantification of nucleobases is difficult due to interfering UV absorbing compounds. In order to reduce these effects, we have developed an extraction technique using sublimation to isolate purines and pyrimidines from other non-volatile organic compounds in Murchison acid extracts.

Fatty Acid Composition of Human Follicular Fluid Phospholipids and Fertilization Rate in Assisted Reproductive Techniques

PubMed Central

Shaaker, Maghsod; Rahimipour, Ali; Nouri, Mohammad; Khanaki, Korosh; Darabi, Masoud; Farzadi, Laya; Shahnazi, Vahideh; Mehdizadeh, Amir

2012-01-01

Background: Fatty acids are known to be critically important in multiple biological functions. Phospholipid fatty acids of follicular fluid, an important microenvironment for the development of oocytes, may contribute to the women’s fertility and the efficacy of assisted reproduction techniques. The aim of this study was to investigate the effect of fatty acid composition of follicular fluid phospholipids on women undergoing assisted reproductive techniques. Methods: Follicular fluid samples were obtained from 100 patients, referred to Tabriz Alzahra Hospital. Seventy-nine subjects underwent in vitro fertilization (IVF) and the remaining 21 underwent intracytoplasmic sperm injection (ICSI). Total lipid of follicular fluid was extracted and fatty acids were analyzed by gas-liquid chromatography. Results: Saturated fatty acids (SFA, P = 0.002) and the ratio of SFA to polyunsaturated fatty acids (P = 0.001) were correlated negatively with a number of mature oocytes after age adjustment. Linoleic acid (P = 0.006) was positively correlated, while the level of arachidonic acid was negatively correlated with fertility percentage after adjustment for body mass index, sperm count, sperm motility. Conclusion: Since phospholipids are one of the major components of lipid metabolism, the results of this study highlight the importance of this component in follicular fluid lipid metabolism. Consequently, it is proposed as an index in determination of the rate of success in assisted reproductive techniques such as IVF/ICSI. PMID:23023218

Extraction of Natural Antioxidants from the Thelephora ganbajun Mushroom by an Ultrasound-Assisted Extraction Technique and Evaluation of Antiproliferative Activity of the Extract against Human Cancer Cells.

PubMed

Xu, Dong-Ping; Zheng, Jie; Zhou, Yue; Li, Ya; Li, Sha; Li, Hua-Bin

2016-10-01

The Thelephora ganbajun mushroom has been found to be a potential rich source of natural antioxidants. In this study, an ultrasound-assisted extraction (UAE) technique together with GRAS (generally recognized as safe) solvents (ethanol and water) was used to maximize the extraction of antioxidants from Thelephora ganbajun . Five extraction parameters (ethanol concentration, solvent to solid ratio, extraction time, temperature and ultrasound power) were investigated by single-factor experiments, and then a central composite rotatable design was employed to study interaction of three key extraction parameters. The optimum conditions were as follows: 57.38% ethanol, 70.15 mL/g solvent to solid ratio, 10.58 min extraction time, 40 °C extraction temperature and 500 W ultrasound power. Under the optimum conditions, the antioxidant activity obtained was 346.98 ± 12.19 µmol Trolox/g DW, in accordance with the predicted value of 344.67 µmol Trolox/g DW. Comparison of UAE with conventional maceration and Soxhlet extraction, the UAE method showed stronger extract efficiency in a shorter extraction time. These results showed that UAE was an effective technique to extract antioxidants from Thelephora ganbajun . Furthermore, the extracts obtained under the optimized conditions exhibited antiproliferative activities toward human lung (A549), breast (MCF-7), liver (HepG2) and colon (HT-29) cancer cells, especially for liver and lung cancer cells. In addition, rutin, 2-hydrocinnamic acid and epicatechin were identified in the extract, which might contribute to antioxidant and antiproliferative activities.

Extraction of Natural Antioxidants from the Thelephora ganbajun Mushroom by an Ultrasound-Assisted Extraction Technique and Evaluation of Antiproliferative Activity of the Extract against Human Cancer Cells

PubMed Central

Xu, Dong-Ping; Zheng, Jie; Zhou, Yue; Li, Ya; Li, Sha; Li, Hua-Bin

2016-01-01

The Thelephora ganbajun mushroom has been found to be a potential rich source of natural antioxidants. In this study, an ultrasound-assisted extraction (UAE) technique together with GRAS (generally recognized as safe) solvents (ethanol and water) was used to maximize the extraction of antioxidants from Thelephora ganbajun. Five extraction parameters (ethanol concentration, solvent to solid ratio, extraction time, temperature and ultrasound power) were investigated by single-factor experiments, and then a central composite rotatable design was employed to study interaction of three key extraction parameters. The optimum conditions were as follows: 57.38% ethanol, 70.15 mL/g solvent to solid ratio, 10.58 min extraction time, 40 °C extraction temperature and 500 W ultrasound power. Under the optimum conditions, the antioxidant activity obtained was 346.98 ± 12.19 µmol Trolox/g DW, in accordance with the predicted value of 344.67 µmol Trolox/g DW. Comparison of UAE with conventional maceration and Soxhlet extraction, the UAE method showed stronger extract efficiency in a shorter extraction time. These results showed that UAE was an effective technique to extract antioxidants from Thelephora ganbajun. Furthermore, the extracts obtained under the optimized conditions exhibited antiproliferative activities toward human lung (A549), breast (MCF-7), liver (HepG2) and colon (HT-29) cancer cells, especially for liver and lung cancer cells. In addition, rutin, 2-hydrocinnamic acid and epicatechin were identified in the extract, which might contribute to antioxidant and antiproliferative activities. PMID:27706082

Development of Total Reflection X-ray fluorescence spectrometry quantitative methodologies for elemental characterization of building materials and their degradation products

NASA Astrophysics Data System (ADS)

García-Florentino, Cristina; Maguregui, Maite; Marguí, Eva; Torrent, Laura; Queralt, Ignasi; Madariaga, Juan Manuel

2018-05-01

In this work, a Total Reflection X-ray fluorescence (TXRF) spectrometry based quantitative methodology for elemental characterization of liquid extracts and solids belonging to old building materials and their degradation products from a building of the beginning of 20th century with a high historic cultural value in Getxo, (Basque Country, North of Spain) is proposed. This quantification strategy can be considered a faster methodology comparing to traditional Energy or Wavelength Dispersive X-ray fluorescence (ED-XRF and WD-XRF) spectrometry based methodologies or other techniques such as Inductively Coupled Plasma Mass Spectrometry (ICP-MS). In particular, two kinds of liquid extracts were analysed: (i) water soluble extracts from different mortars and (ii) acid extracts from mortars, black crusts, and calcium carbonate formations. In order to try to avoid the acid extraction step of the materials and their degradation products, it was also studied the TXRF direct measurement of the powdered solid suspensions in water. With this aim, different parameters such as the deposition volume and the measuring time were studied for each kind of samples. Depending on the quantified element, the limits of detection achieved with the TXRF quantitative methodologies for liquid extracts and solids were set around 0.01-1.2 and 2-200 mg/L respectively. The quantification of K, Ca, Ti, Mn, Fe, Zn, Rb, Sr, Sn and Pb in the liquid extracts was proved to be a faster alternative to other more classic quantification techniques (i.e. ICP-MS), accurate enough to obtain information about the composition of the acidic soluble part of the materials and their degradation products. Regarding the solid samples measured as suspensions, it was quite difficult to obtain stable and repetitive suspensions affecting in this way the accuracy of the results. To cope with this problem, correction factors based on the quantitative results obtained using ED-XRF were calculated to improve the accuracy of the TXRF results.

Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

PubMed

Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

2007-11-15

The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

Syringe needle-based sampling coupled with liquid-phase extraction for determination of the three-dimensional distribution of l-ascorbic acid in apples.

PubMed

Tang, Sheng; Lee, Hian Kee

2016-05-15

A novel syringe needle-based sampling approach coupled with liquid-phase extraction (NBS-LPE) was developed and applied to the extraction of l-ascorbic acid (AsA) in apple. In NBS-LPE, only a small amount of apple flesh (ca. 10mg) was sampled directly using a syringe needle and placed in a glass insert for liquid extraction of AsA by 80 μL oxalic acid-acetic acid. The extract was then directly analyzed by liquid chromatography. This new procedure is simple, convenient, almost organic solvent free, and causes far less damage to the fruit. To demonstrate the applicability of NBS-LPE, AsA levels at different sampling points in a single apple were determined to reveal the spatial distribution of the analyte in a three-dimensional model. The results also showed that this method had good sensitivity (limit of detection of 0.0097 mg/100g; limit of quantification of 0.0323 mg/100g), acceptable reproducibility (relative standard deviation of 5.01% (n=6)), a wide linear range of between 0.05 and 50mg/100g, and good linearity (r(2)=0.9921). This interesting extraction technique and modeling approach can be used to measure and monitor a wide range of compounds in various parts of different soft-matrix fruits and vegetables, including single specimens. Copyright © 2015 Elsevier Ltd. All rights reserved.

Coupling of solvent-based de-emulsification dispersive liquid-liquid microextraction with high performance liquid chromatography for simultaneous simple and rapid trace monitoring of 2,4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid.

PubMed

Behbahani, Mohammad; Najafi, Fatemeh; Bagheri, Saman; Bojdi, Majid Kalate; Hassanlou, Parmoon Ghareh; Bagheri, Akbar

2014-04-01

A simple, rapid, and efficient sample pretreatment technique, based on solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME), followed by high performance liquid chromatography (HPLC) has been developed for simultaneous preconcentration and trace detection of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in water and urine samples. Some parameters such as acidity of solution, the amount of salt, type, and volume of extraction solvents, type of disperser/de-emulsifier solvent, and its volume were investigated and optimized. Under optimum extraction conditions, the limits of detections (LODs) of this method for MCPA and 2,4-D were 0.2 and 0.6 μg L(-1) (based on 3S(b)/m) in water and 0.4 and 1.6 μg L(-1) in urine, respectively. Furthermore, dynamic linear range of this method for MCPA and 2,4-D was 1-300 and 2-400 μg L(-1), repectively. Finally, the applicability of the proposed method was evaluated by extraction and determination of the herbicides in urine and different water samples.

Comparison of Acid Titration, Conductivity, Flame Photometry, ICP-MS, and Accelerated Lamellae Formation Techniques in Determining Glass Vial Quality.

PubMed

Fujimori, Kiyoshi; Lee, Hans; Sloey, Christopher; Ricci, Margaret S; Wen, Zai-Qing; Phillips, Joseph; Nashed-Samuel, Yasser

2016-01-01

Certain types of glass vials used as primary containers for liquid formulations of biopharmaceutical drug products have been observed with delamination that produced small glass like flakes termed lamellae under certain conditions during storage. The cause of this delamination is in part related to the glass surface defects, which renders the vials susceptible to flaking, and lamellae are formed during the high-temperature melting and annealing used for vial fabrication and shaping. The current European Pharmacopoeia method to assess glass vial quality utilizes acid titration of vial extract pools to determine hydrolytic resistance or alkalinity. Four alternative techniques with improved throughput, convenience, and/or comprehension were examined by subjecting seven lots of vials to analysis by all techniques. The first three new techniques of conductivity, flame photometry, and inductively coupled plasma mass spectrometry measured the same sample pools as acid titration. All three showed good correlation with alkalinity: conductivity (R(2) = 0.9951), flame photometry sodium (R(2) = 0.9895), and several elements by inductively coupled plasma mass spectrometry [(sodium (R(2) = 0.9869), boron (R(2) = 0.9796), silicon (R(2) = 0.9426), total (R(2) = 0.9639)]. The fourth technique processed the vials under conditions that promote delamination, termed accelerated lamellae formation, and then inspected those vials visually for lamellae. The visual inspection results without the lot with different processing condition correlated well with alkalinity (R(2) = 0.9474). Due to vial processing differences affecting alkalinity measurements and delamination propensity differently, the ratio of silicon and sodium measurements from inductively coupled plasma mass spectrometry was the most informative technique to assess overall vial quality and vial propensity for lamellae formation. The other techniques of conductivity, flame photometry, and accelerated lamellae formation condition may still be suitable for routine screening of vial lots produced under consistent processes. Recently, delamination that produced small glass like flakes termed lamellae has been observed in glass vials that are commonly used as primary containers for pharmaceutical drug products under certain conditions during storage. The main cause of these lamellae was the quality of the glass itself related to the manufacturing process. Current European Pharmacopoeia method to assess glass vial quality utilizes acid titration of vial extract pools to determine hydrolytic resistance or alkalinity. As alternative to the European Pharmacopoeia method, four other techniques were assessed. Three new techniques of conductivity, flame photometry, and inductively coupled plasma mass spectrometry measured the vial extract pool as acid titration to quantify quality, and they demonstrated good correlation with original alkalinity. The fourth technique processed the vials under conditions that promote delamination, termed accelerated lamellae formation, and the vials were then inspected visually for lamellae. The accelerated lamellae formation technique also showed good correlation with alkalinity. Of the new four techniques, inductively coupled plasma mass spectrometry was the most informative technique to assess overall vial quality even with differences in processing between vial lots. Other three techniques were still suitable for routine screening of vial lots produced under consistent processes. © PDA, Inc. 2016.

A Reexamination of Amino Acids in Lunar Soils: Implications for the Survival of Exogenous Organic Material During Impact Delivery

NASA Technical Reports Server (NTRS)

Brinton, Karen L. F.; Bada, Jeffrey L.

1996-01-01

Using a sensitive high performance liquid chromatography technique, we have analyzed both the hot water extract and the acid hydrolyzed hot water extract of lunar soil collected during the Apollo 17 mission. Both free amino acids and those derived from acid labile precursors are present at a level of roughly 15 ppb. Based on the D/L amino acid ratios, the free alanine and aspartic acid observed in the hot water extract can be entirely attributed to terrestrial biogenic contamination. However, in the acid labile fraction, precursors which yield amino acids are apparently present in the lunar soil. The amino acid distribution suggests that the precursor is probably solar wind implanted HCN. We have evaluated our results with regard to the meteoritic input of intact organic compounds to the moon based on an upper limit of less than or equal to 0.3 ppb for alpha-aminoisobutyric acid, a non-protein amino acid which does not generally occur in terrestrial organisms and which is not a major amino acid produced from HCN, but which is a predominant amino acid in many carbonaceous chondrites. We find that the survival of exogenous organic compounds during lunar impact is less than or equal to 0.8%. This result represents an example of minimum organic impact survivability. This is an important first step toward a better understanding of similar processes on Earth and on Mars, and their possible contribution to the budget of prebiotic organic compounds on the primitive Earth.

Solid Phase Micro-extraction (SPME) with In Situ Transesterification: An Easy Method for the Detection of Non-volatile Fatty Acid Derivatives on the Insect Cuticle.

PubMed

Kühbandner, Stephan; Ruther, Joachim

2015-06-01

Triacylglycerides (TAGs) and other non-volatile fatty acid derivatives (NFADs) occur in large amounts in the internal tissues of insects, but their presence on the insect cuticle is controversially discussed. Most studies investigating cuticular lipids of insects involve solvent extraction, which implies the risk of extracting lipids from internal tissues. Here, we present a new method that overcomes this problem. The method employs solid phase micro-extraction (SPME) to sample NFADs by rubbing the SPME fiber over the insect cuticle. Subsequently, the sampled NFADs are transesterified in situ with trimethyl sulfonium hydroxide (TMSH) into more volatile fatty acid methyl esters (FAMEs), which can be analyzed by standard GC/MS. We performed two types of control experiments to enable significant conclusions: (1) to rule out contamination of the GC/MS system with NFADs, and (2) to exclude the presence of free fatty acids on the insect cuticle, which would also furnish FAMEs after TMSH treatment, and thus might simulate the presence of NFADs. In combination with these two essential control experiments, the described SPME technique can be used to detect TAGs and/or other NFADs on the insect cuticle. We analyzed six insect species from four insect orders with our method and compared the results with conventional solvent extraction followed by ex situ transesterification. Several fatty acids typically found as constituents of TAGs were detected by the SPME method on the cuticle of all species analyzed. A comparison of the two methods revealed differences in the fatty acid compositions of the samples. Saturated fatty acids showed by trend higher relative abundances when sampled with the SPME method, while several minor FAMEs were detected only in the solvent extracts. Our study suggests that TAGs and maybe other NFADs are far more common on the insect cuticle than usually thought.

Tigloylshikonin, a new minor Shikonin derivative, from the roots and the commercial root extract of lithospermum erythrorhizon.

PubMed

Ito, Yusai; Onobori, Kenichi; Yamazaki, Takeshi; Kawamura, Yoko

2011-01-01

Tigloylshikonin, a new shikonin derivative esterified with tiglic acid ((E)-2-methylbut-2-enoic acid), was isolated as a minor pigment from a food colorant "Shikon color," a commercial root extract from Lithospermum erythrorhizon SIEBOLD et ZUCCARINI. The structure of tigloylshikonin was elucidated using (1)H, (13)C, the difference nuclear Overhauser effect (NOE), and 2D NMR techniques. Its stereochemistry was determined by chiral-phase HPLC analysis. Tigloylshikonin was also found in the roots of L. erythrorhizon, which indicated that this new shikonin derivative is a typical component of naphthoquinone pigments in the roots of L. erythrorhizon.

Development of a new high-performance liquid chromatography method with diode array and electrospray ionization-mass spectrometry detection for the metabolite fingerprinting of bioactive compounds in Humulus lupulus L.

PubMed

Prencipe, Francesco Pio; Brighenti, Virginia; Rodolfi, Margherita; Mongelli, Andrea; dall'Asta, Chiara; Ganino, Tommaso; Bruni, Renato; Pellati, Federica

2014-07-04

The study was aimed at developing a new analytical method for the metabolite fingerprinting of bioactive compounds in Humulus lupulus L. (hop), together with a simple extraction procedure. Different extraction techniques, including maceration, heat reflux extraction (HRE), ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE), were compared in order to obtain a high yield of the target analytes. Dynamic maceration for 30min with MeOH-HCOOH (99:1, v/v) as the extraction solvent provided the best result in terms of recovery of secondary metabolites. The analysis of hop constituents, including prenylflavonoids and prenylphloroglucinols (bitter acids), was carried out by means of HPLC-UV/DAD, HPLC-ESI-MS and MS(2), using an ion trap mass analyzer. An Ascentis Express C18 column (150mm×3.0mm I.D., 2.7μm) was used for the HPLC analysis, with a mobile phase composed of 0.25% formic acid in both water and acetonitrile, under gradient elution. The method validation was performed to show compliance with ICH guidelines. The validated technique was successfully applied to the phytochemical analysis of ten commercial cultivars and twenty-three wild Italian hop genotypes, thus demonstrating to be a reliable and useful tool for the comprehensive multi-component analysis of hop secondary metabolites. Copyright © 2014 Elsevier B.V. All rights reserved.

Isolation and structural characterization of sugarcane bagasse lignin after dilute phosphoric acid plus steam explosion pretreatment and its effect on cellulose hydrolysis

Treesearch

Jijiao Zeng; Zhaohui Tong; Letian Wang; J.Y. Zhu; Lonnie Ingram

2014-01-01

The structure of lignin after dilute phosphoric acid plus steam explosion pretreatment process of sugarcane bagasse in a pilot scale and the effect of the lignin extracted by ethanol on subsequent cellulose hydrolysis were investigated. The lignin structural changes caused by pretreatment were identified using advanced nondestructive techniques such as gel permeation...

Aroma composition of shalgam: a traditional Turkish lactic acid fermented beverage.

PubMed

Tanguler, Hasan; Selli, Serkan; Sen, Kemal; Cabaroglu, Turgut; Erten, Huseyin

2017-06-01

Shalgam, a traditional red, cloudy and sour soft beverage, is produced by lactic acid fermentation of black carrot, sourdough, salt, bulgur flour, turnip and adequate water. The present study was designed to characterize the volatile compounds of shalgam obtained from different methods. The aroma compounds of shalgams produced by traditional and direct methods, and addition of Lactic acid bateria (LAB) cultures were examined. Volatile components of shalgam samples were extracted by liquid-liquid extraction technique with pentane/dichloromethane and analyzed by gas chromatography-mass spectrometry (GC-MS). Sixty aroma compounds were identified in shalgam samples including 20 terpenes, 9 esters, 9 alcohols, 5 volatile acids, 6 volatile phenols, 5 lactones, 3 naphthalenes, 2 carbonyl compounds and 1 C13-norisoprenoids. It was found that the aroma profiles of shalgams were quite similar. However, the total volatile content of the shalgam samples increased with addition of Lb. plantarum .

Laboratory procedures to generate viral metagenomes.

PubMed

Thurber, Rebecca V; Haynes, Matthew; Breitbart, Mya; Wegley, Linda; Rohwer, Forest

2009-01-01

This collection of laboratory protocols describes the steps to collect viruses from various samples with the specific aim of generating viral metagenome sequence libraries (viromes). Viral metagenomics, the study of uncultured viral nucleic acid sequences from different biomes, relies on several concentration, purification, extraction, sequencing and heuristic bioinformatic methods. No single technique can provide an all-inclusive approach, and therefore the protocols presented here will be discussed in terms of hypothetical projects. However, care must be taken to individualize each step depending on the source and type of viral-particles. This protocol is a description of the processes we have successfully used to: (i) concentrate viral particles from various types of samples, (ii) eliminate contaminating cells and free nucleic acids and (iii) extract, amplify and purify viral nucleic acids. Overall, a sample can be processed to isolate viral nucleic acids suitable for high-throughput sequencing in approximately 1 week.

Extraction and identification of flavonoids from parsley extracts by HPLC analysis

NASA Astrophysics Data System (ADS)

Stan, M.; Soran, M. L.; Varodi, C.; Lung, I.

2012-02-01

Flavonoids are phenolic compounds isolated from a wide variety of plants, and are valuable for their multiple properties, including antioxidant and antimicrobial activities. In the present work, parsley (Petroselinum crispum L.) extracts were obtained by three different extraction techniques: maceration, ultrasonic-assisted and microwave-assisted solvent extractions. The extractions were performed with ethanol-water mixtures in various ratios. From these extracts, flavonoids like the flavones apigenin and luteolin, and the flavonols quercetin and kaempferol were identified using an HPLC Shimadzu apparatus equipped with PDA and MS detectors. The separation method involved a gradient step. The mobile phase consisted of two solvents: acetonitrile and distilled water with 0.1% formic acid. The separation was performed on a RP-C18 column.

Experimental study on thermal hazard of tributyl phosphate-nitric acid mixtures using micro calorimeter technique.

PubMed

Sun, Qi; Jiang, Lin; Gong, Liang; Sun, Jin-Hua

2016-08-15

During PUREX spent nuclear fuel reprocessing, mixture of tributyl phosphate (TBP) and hydrocarbon solvent are employed as organic solvent to extract uranium in consideration of radiation contaminated safety and resource recycling, meanwhile nitric acid is utilized to dissolve the spent fuel into small pieces. However, once TBP contacts with nitric acid or nitrates above 130°C, a heavy "red oil" layer would occur accompanied by thermal runaway reactions, even caused several nuclear safety accident. Considering nitric acid volatility and weak exothermic detection, C80micro calorimeter technique was used in this study to investigate thermal decomposition of TBP mixed with nitric acid. Results show that the concentration of nitric acid greatly influences thermal hazard of the system by direct reactions. Even with a low heating rate, if the concentration of nitric acid increases due to evaporation of water or improper operations, thermal runaway in the closed system could start at a low temperature. Copyright © 2016 Elsevier B.V. All rights reserved.

Subcritical Fluid Extraction of Chinese Quince Seed: Optimization and Product Characterization.

PubMed

Wang, Li; Wu, Min; Liu, Hua-Min; Ma, Yu-Xiang; Wang, Xue-De; Qin, Guang-Yong

2017-03-25

Chinese quince seed (CQS) is an underutilized oil source and a potential source of unsaturated fatty acids and α-tocopherol-rich oil. Subcritical fluid (SCF) extraction is executed at lower pressures and temperatures than the pressures and temperatures used in supercritical fluid extraction. However, no studies on the SCF extraction of CQS oil are reported. Therefore, the objective of this study was to evaluate the use of SCF for the extraction of CQS oil and to compare the use of SCF with the classical Soxhlet (CS) and supercritical CO₂ (SC-CO₂) extraction methods. Response surface methodology (RSM) was used to investigate the extraction conditions: temperature (45-65 °C), time (30-50 min), and solvent/solid ratio (5-15 mL/g). The optimization results showed that the highest yield (27.78%) was obtained at 56.18 °C, 40.20 min, and 12.57 mL/g. The oil extracted by SCF had a higher unsaturated fatty acid content (86.37%-86.75%), higher α-tocopherol content (576.0-847.6 mg/kg), lower acid value (3.97 mg/g), and lower peroxide value (0.02 meq O₂/kg) than extractions using CS and SC-CO 2 methods. The SCF-defatted meal of oilseed exhibited the highest nitrogen solubility index (49.64%) and protein dispersibility index (50.80%), demonstrating that SCF extraction was a promising and efficient technique as an alternative to CS and SC-CO 2 methods, as very mild operating conditions and an eco-friendly solvent can be used in the process with maximum preservation of the quality of the meal.

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.

Dimethyl carbonate-mediated lipid extraction and lipase-catalyzed in situ transesterification for simultaneous preparation of fatty acid methyl esters and glycerol carbonate from Chlorella sp. KR-1 biomass.

PubMed

Jo, Yoon Ju; Lee, Ok Kyung; Lee, Eun Yeol

2014-04-01

Fatty acid methyl esters (FAMEs) and glycerol carbonate were simultaneously prepared from Chlorella sp. KR-1 containing 40.9% (w/w) lipid using a reactive extraction method with dimethyl carbonate (DMC). DMC was used as lipid extraction agent, acyl acceptor for transesterification of the extracted triglycerides, substrate for glycerol carbonate synthesis from glycerol, and reaction medium for the solvent-free reaction system. For 1g of biomass, 367.31 mg of FAMEs and 16.73 mg of glycerol carbonate were obtained under the optimized conditions: DMC to biomass ratio of 10:1 (v/w), water content of 0.5% (v/v), and Novozyme 435 to biomass ratio of 20% (w/w) at 70°C for 24h. The amount of residual glycerol was only in the range of 1-2.5mg. Compared to conventional method, the cost of FAME production with the proposed technique could be reduced by combining lipid extraction with transesterification and omitting the extraction solvent recovery process. Copyright © 2014 Elsevier Ltd. All rights reserved.

Comparison of two novel in-syringe dispersive liquid-liquid microextraction techniques for the determination of iodide in water samples using spectrophotometry.

PubMed

Kaykhaii, Massoud; Sargazi, Mona

2014-01-01

Two new, rapid methodologies have been developed and applied successfully for the determination of trace levels of iodide in real water samples. Both techniques are based on a combination of in-syringe dispersive liquid-liquid microextraction (IS-DLLME) and micro-volume UV-Vis spectrophotometry. In the first technique, iodide is oxidized with nitrous acid to the colorless anion of ICl2(-) at high concentration of hydrochloric acid. Rhodamine B is added and by means of one step IS-DLLME, the ion-pair formed was extracted into toluene and measured spectrophotometrically. Acetone is used as dispersive solvent. The second method is based on the IS-DLLME microextraction of iodide as iodide/1, 10-phenanthroline-iron((II)) chelate cation ion-pair (colored) into nitrobenzene. Methanol was selected as dispersive solvent. Optimal conditions for iodide extraction were determined for both approaches. Methods are compared in terms of analytical parameters such as precision, accuracy, speed and limit of detection. Both methods were successfully applied to determining iodide in tap and river water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

A method for measuring low-weight carboxylic acids from biosolid compost.

PubMed

Himanen, Marina; Latva-Kala, Kyösti; Itävaara, Merja; Hänninen, Kari

2006-01-01

Concentration of low-weight carboxylic acids (LWCA) is one of the important parameters that should be taken into consideration when compost is applied as soil improver for plant cultivation, because high amounts of LWCA can be toxic to plants. The present work describes a method for analysis of LWCA in compost as a useful tool for monitoring compost quality and safety. The method was tested on compost samples of two different ages: 3 (immature) and 6 (mature) months old. Acids from compost samples were extracted at high pH, filtered, and freeze-dried. The dried sodium salts were derivatized with a sulfuric acid-methanol mixture and concentrations of 11 low-weight fatty acids (C1-C10) were analyzed using headspace gas chromatography. The material was analyzed with two analytical techniques: the external calibration method (tested on 11 LWCA) and the standard addition method (tested only on formic, acetic, propionic, butyric, and iso-butyric acids). The two techniques were compared for efficiency of acids quantification. The method allowed good separation and quantification of a wide range of individual acids with high sensitivity at low concentrations. Detection limit for propionic, butyric, caproic, caprylic, and capric acids was 1 mg kg(-1) compost; for formic, acetic, valeric, enanthoic and pelargonic acids it was 5 mg kg(-1) compost; and for iso-butyric acid it was 10 mg kg(-1) compost. Recovery rates of LWCA were higher in 3-mo-old compost (57-99%) than in 6-mo-old compost (29-45%). In comparison with the external calibration technique the standard addition technique proved to be three to four times more precise for older compost and two times for younger compost. Disadvantages of the standard addition technique are that it is more time demanding and laborious.

Development and formulation of Moringa oleifera standardised leaf extract film dressing for wound healing application.

PubMed

Chin, Chai-Yee; Jalil, Juriyati; Ng, Pei Yuen; Ng, Shiow-Fern

2018-02-15

M.oleifera is a medicinal plant traditionally used for skin sores, sore throat and eye infections. Recently, the wound healing property of the leaves of M. oleifera was has been well demonstrated experimentally in both in vivo and in vitro models. However, there is a lack of research which focuses on formulating M.oleifera into a functional wound dressing. In this study, the M.oleifera leaf standardized aqueous extract with highest potency in vitro migration was formulated into a film for wound healing application. Firstly, M. oleifera leaf were extracted in various solvents (aqueous, 50%, 70% and 100% ethanolic extracts) and standardized by reference standards using UHPLC technique. The extracts were then tested for cell migration and proliferation using HDF and HEK cell lines. M. oleifera leaf aqueous extract was then incorporated into alginate-pectin (SA-PC) based film dressing. The film dressings were characterized for the physicochemical properties and the bioactives release from the M. oleifera leaf extract loaded film dressing was also investigated using Franz diffusion cells. All extracts were found to contain vicenin-2, chlorogenic acid, gallic acid, quercetin, kaempferol, rosmarinic acid and rutin. Among all M. oleifera extracts, aqueous standardized leaf extracts showed the highest human dermal fibroblast and human keratinocytes cells proliferation and migration properties. Among the film formulations, SA-PC (3% w/v) composite film dressing containing M. oleifera aqueous leaf extract was found to possess optimal physicochemical properties as wound dressing. A potentially applicable wound dressing formulated as an alginate-pectin film containing aqueous extracts of M. oleifera has been developed. The dressing would be suitable for wounds with moderate exudates. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of Thermoultrasound on the Antioxidant Compounds and Fatty Acid Profile of Blackberry (Rubus fruticosus spp.) Juice.

PubMed

Manríquez-Torres, José de Jesús; Sánchez-Franco, José Antonio; Ramírez-Moreno, Esther; Cruz-Cansino, Nelly Del Socorro; Ariza-Ortega, José Alberto; Torres-Valencia, Jesús Martín

2016-11-29

Blackberry ( Rubus fruticosus spp.) fruit has high antioxidant activity due to its significant content of anthocyanins and antioxidant compounds. Among emerging technologies for food preservation, thermoultrasound is a technique that reduces microbial loads and releases compounds with antioxidant properties. The objective of this study was to determine the antioxidant content and fatty acid profile of blackberry juice subjected to thermoultrasound treatment in comparison to pasteurized juice. Blackberry juice and n -hexane extracts from a control (untreated juice), pasteurized, and thermoultrasonicated samples were evaluated for antioxidant activity, fatty acid profile, and antioxidant content. The juice treated with thermoultrasound exhibited significantly ( p < 0.05) higher levels of total phenols (1011 mg GAE/L), anthocyanins (118 mg Cy-3-GlE/L); antioxidant activity by ABTS (44 mg VCEAC/L) and DPPH (2665 µmol TE/L) in comparison to the control and pasteurized samples. Oil extract from thermoultrasound juice also had the highest antioxidant activity (177.5 mg VCEAC/L and 1802.6 µmol TE/L). The fatty acid profile of the n -hexane extracts showed the presence of myristic, linolenic, stearic, oleic, and linoleic acids and was not affected by the treatments except for stearic acid, whose amount was particularly higher in the control. Our results demonstrated that thermoultrasound can be an alternative technology to pasteurization that maintains and releases antioxidant compounds and preserves the fatty acids of fruit juice.

Highly selective and efficient imprinted polymers based on carboxyl-functionalized magnetic nanoparticles for the extraction of gallic acid from pomegranate rind.

PubMed

Zhang, Junjie; Li, Benqiang; Yue, Huijuan; Wang, Jing; Zheng, Yuansuo

2018-01-01

With the combined surface imprinting technique and immobilized template strategy, molecularly imprinted magnetic nanoparticles were successfully prepared and coupled with high-performance liquid chromatography to selectively separate and determine gallic acid from the pomegranate rind. On the surface of carboxyl-functionalized magnetic nanospheres, thin imprinting shells were formed using dopamine as monomer and crosslinker. The characteristics, polymerization conditions, and adsorption performances of the resultant nanomaterials were investigated in detail. In addition of good crystallinity, satisfactory magnetism, and uniform morphology of the obtained polymers, they had rapid binding kinetics, high adsorption capacity, and favorable reusability. In the mixed solution of four hydroxybenzoic acids, the prepared nanomaterials have an excellent selectivity to gallic acid with an imprinting factor of as high as 17.5. Therefore, the polymers have great potentials in specific extraction and enrichment of gallic acid from the complex natural resources. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Studies on preparative technology and quantitative determination for extracts of total saponin in roof of Panax japonicus].

PubMed

He, Yu-min; Lu, Ke-ming; Yuan, Ding; Zhang, Chang-cheng

2008-11-01

To explore the optimum extraction and purification condition of the total saponins in the root of Panax japonicus (RPJ), and establish its quality control methods. Designed L16 (4(5)) orthogonal test with the extraction rate of total saponins as index, to determine the rational extraction process, and the techniques of water-saturated n-butanol extraction and acetone precipitation were applied to purify the alcohol extract of RPJ. Total saponins were detected by spectrophotometry and its triterpenoidal sapogenin oleanolic acid detected by HPLC. The optimum conditions of total saponins from RPJ was as follows: the material was pulverized, dipped in 60% ethanol aqueous solution as extract solvent at 10 times of volume, and refluxed 3 times for 3 h each time. Extractant of water-saturated n-butanol with extraction times of 3 and precipitant of acetone with precipitation amount of 4-5 times were included in the purification process, which would obtain the quality products. The content of total saponins could reach to 83.48%, and oleanolic acid to 38.30%. The optimized preparative technology is stable, convenient and practical. The extract rate of RPJ was high and steady with this technology, which provided new evidence for industrializing production of the plant and developing new drug.

Isolation and recovery of selected polybrominated diphenyl ethers from human serum and sheep serum: coupling reversed-phase solid-phase disk extraction and liquid-liquid extraction techniques with a capillary gas chromatographic electron capture negative ion mass spectrometric determinative technique.

PubMed

Loconto, Paul R; Isenga, David; O'Keefe, Michael; Knottnerus, Mark

2008-01-01

Polybrominated diphenyl ethers (PBDEs) are isolated and recovered with acceptable percent recoveries from human serum via liquid-liquid extraction and column chromatographic cleanup and fractionation with quantitation using capillary gas chromatography-mass spectrometry with electron capture negative ion and selected ion monitoring. PBDEs are found in unspiked serum. An alternative sample preparation approach is developed using sheep serum that utilizes a formic acid pre-treatment followed by reversed-phase solid-phase disk extraction and normal-phase solid-phase cleanup using acidified silica gel that yields>50% recoveries. When these percent recoveries are combined with a minimized phase ratio for human serum and very low instrument detection limits, method detection limits below 500 parts-per-trillion are realized.

Organic acids in naturally colored surface waters

USGS Publications Warehouse

Lamar, William L.; Goerlitz, D.F.

1966-01-01

Most of the organic matter in naturally colored surface waters consists of a mixture of carboxylic acids or salts of these acids. Many of the acids color the water yellow to brown; however, not all of the acids are colored. These acids range from simple to complex, but predominantly they are nonvolatile polymeric carboxylic acids. The organic acids were recovered from the water by two techniques: continuous liquid-liquid extraction with n-butanol and vacuum evaporation at 50?C (centigrade). The isolated acids were studied by techniques of gas, paper, and column chromatography and infrared spectroscopy. About 10 percent of the acids recovered were volatile or could be made volatile for gas chromatographic analysis. Approximately 30 of these carboxylic acids were isolated, and 13 of them were individually identified. The predominant part of the total acids could not be made volatile for gas chromatographic analysis. Infrared examination of many column chromatographic fractions indicated that these nonvolatile substances are primarily polymeric hydroxy carboxylic acids having aromatic and olefinic unsaturation. The evidence suggests that some of these acids result from polymerization in aqueous solution. Elemental analysis of the sodium fusion products disclosed the absence of nitrogen, sulfur, and halogens.

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

PubMed

Peterson, Eric C; Daugulis, Andrew J

2014-11-01

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

Determination of dissolved aluminum in water samples

USGS Publications Warehouse

Afifi, A.A.

1983-01-01

A technique has been modified for determination of a wide range of concentrations of dissolved aluminum (Al) in water and has been tested. In this technique, aluminum is complexed with 8-hydroxyquinoline at pH 8.3 to minimize interferences, then extracted with methyl isobutyl ketone (MIBK). The extract is analyzed colorimetrically at 395 nm. This technique is used to analyze two forms of monomeric Al, nonlabile (organic complexes) and labile (free, Al, Al sulfate, fluoride and hydroxide complexes). A detection limit 2 ug/L is possible with 25-ml samples and 10-ml extracts. The detection limit can be decreased by increasing the volume of the sample and (or) decreasing the volume of the methyl isobutyl ketone extract. The analytical uncertainty of this method is approximately + or - 5 percent. The standard addition technique provides a recovery test for this technique and ensures precision in samples of low Al concentrations. The average percentage recovery of the added Al plus the amount originally present was 99 percent. Data obtained from analyses of filtered standard solutions indicated that Al is adsorbed on various types of filters. However, the relationship between Al concentrations and adsorption remains linear. A test on standard solutions also indicated that Al is not adsorbed on nitric acid-washed polyethylene and polypropylene bottle wells. (USGS)

The Gabriel Synthesis of Benzylamine

ERIC Educational Resources Information Center

Nigh, W. G.

1975-01-01

Describes an undergraduate organic chemistry laboratory experiment which utilizes the Gabriel Synthesis to demonstrate the acidity of imides and to provide an example of nucleophilic substitution reactions. The experiment also demonstrates the laboratory techniques involved in simple and steam distillation, filtration, extraction, and…

The microwave induced plasma with optical emission spectrometry (MIP-OES) in 23 elements determination in geological samples.

PubMed

Niedzielski, P; Kozak, L; Wachelka, M; Jakubowski, K; Wybieralska, J

2015-01-01

The article presents the optimisation, validation and application of the microwave induced plasma optical emission spectrometry (MIP-OES) dedicated for a routine determination of Ag, Al, B, Ba, Bi, Ca, Cd, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sr, Tl, Zn, in the geological samples. The three procedures of sample preparation has been proposed: sample digestion with the use of hydrofluoric acid for determination of total concentration of elements, extraction by aqua regia for determination of the quasi-total element concentration and extraction by hydrochloric acid solution to determine contents of the elements in acid leachable fraction. The detection limits were on the level 0.001-0.121 mg L(-1) (from 0.010-0.10 to 1.2-12 mg kg(-1) depend on the samples preparation procedure); the precision: 0.20-1.37%; accuracy 85-115% (for recovery for certified standards materials analysis and parallel analysis by independent analytical techniques: X-ray fluorescence (XRF) and flame absorption spectrometry (FAAS)). The conformity of the results obtained by MIP-OES analytical procedures with the results obtained by XRF and FAAS analysis allows to propose the procedures for studies of elemental composition of the fraction of the geological samples. Additionally, the MIP-OES technique is much less expensive than ICP techniques and much less time-consuming than AAS techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

Optimized microwave extraction, characterization and antioxidant capacity of biological polysaccharides from Eucommia ulmoides Oliver leaf.

PubMed

Xu, Jikun; Hou, Huijie; Hu, Jingping; Liu, Bingchuan

2018-04-26

Microwave-induced technique was combined with response surface methodology for optimizing the isolation of polysaccharides from Eucommia ulmoides Oliver leaf. The maximum polysaccharides yield of 12.31% was achieved by microwave extraction at 74 °C for 15 min with a solid to liquid ratio of 1:29 g/mL, which agreed with the predicted value and was 2.9-fold higher than that of the conventional heat-reflux extraction method. The dominant bioactive constituent in extracts was chlorogenic acid (1.3-1.9%), followed by geniposidic acid (1.0-1.7%). The polysaccharides from the optimized extraction had a high molecular weight and polydispersity (M w 38,830 g/mol, M w /M n 2.19), as compared to the fraction prepared in the absence of microwave (M w 12,055 g/mol, M w /M n 1.26). Glucose was the dominant sugar component (38.2-39.1%) of heterogeneous polysaccharides which belonged to a structure of β-type acidic heteropolysaccharides with a glucan group and highly branched degree. The polysaccharides showed a higher DPPH radical scavenging index (0.87-1.22) than BHT (0.41) but lower than BHA (3.56), which can act as a favorable antioxidant in functional food.

Determination of the volatile and semi-volatile secondary metabolites, and aristolochic acids in Aristolochia ringens Vahl.

PubMed

Stashenko, Elena E; Andrés Ordóñez, Sergio; Marín, Néstor Armando; Martínez, Jairo René

2009-10-01

Volatile and semi-volatile secondary metabolites, as well as aristolochic acids (AA), present in leaves, stems, and flowers of Aristolochia ringens were determined by gas chromatography (GC)-mass spectrometry (MS) and high-performance liquid chromatography (HPLC) methods, respectively. Metabolite isolation was performed using different extraction techniques: microwave-assisted hydrodistillation (MWHD), supercritical fluid extraction, and headspace solid-phase microextraction (HS-SPME). The chemical composition of the extracts and oils was established by GC-MS. The determinations of AAI and AAII were conducted by methanolic extraction of different plant parts followed by HPLC analysis. Essential oil yields from leaves and stems were 0.008 +/- 0.0022% and 0.047 +/- 0.0026%, respectively. Aristolochia ringens flowers did not yield essential oil under MWHD. Sesquiterpene hydrocarbons (66%) were the main compounds in the essential oil isolated from leaves whereas monoterpene hydrocarbons (73%) predominated in the stems essential oil. Yields of extracts isolated by SFE from leaves, stems, and flowers were 4 +/- 1.8%, 1.2 +/- 0.25%, and 4 +/- 1.8%, respectively. In vivo HS-SPME of flowers isolated compounds with known unpleasant smells such as volatile aldehydes and short-chain carboxylic acids. HPLC analysis detected the presence of AAII in the flowers of Aristolochia ringens at a concentration of 610 +/- 47 mg/kg of dried flower.

Comparison of the Effects of Blending and Juicing on the Phytochemicals Contents and Antioxidant Capacity of Typical Korean Kernel Fruit Juices

PubMed Central

Pyo, Young-Hee; Jin, Yoo-Jeong; Hwang, Ji-Young

2014-01-01

Four Korean kernel fruit (apple, pear, persimmon, and mandarin orange) juices were obtained by household processing techniques (i.e., blending, juicing). Whole and flesh fractions of each fruit were extracted by a blender or a juicer and then examined for phytochemical content (i.e., organic acids, polyphenol compounds). The antioxidant capacity of each juice was determined by ferric reducing antioxidant power (FRAP) and 2,2-diphenyl-1-picrylhydrazyl (DPPH) assays. Results revealed that juices that had been prepared by blending whole fruits had stronger antioxidant activities and contained larger amounts of phenolic compounds than juices that had been prepared by juicing the flesh fraction of the fruit. However, the concentration of ascorbic acid in apple, pear, and mandarin orange juices was significantly (P<0.05) higher in juice that had been processed by juicing, rather than blending. The juices with the highest ascorbic acid (233.9 mg/serving), total polyphenols (862.3 mg gallic acid equivalents/serving), and flavonoids (295.1 mg quercetin equivalents/serving) concentrations were blended persimmon juice, blended mandarin orange juice, and juiced apple juice, respectively. These results indicate that juice extraction techniques significantly (P<0.05) influences the phytochemical levels and antioxidant capacity of fruit juices. PMID:25054109

Membrane Structure: Spin Labeling and Freeze Etching of Mycoplasma laidlawii*

PubMed Central

Tourtellotte, Mark E.; Branton, Daniel; Keith, Alec

1970-01-01

A spin-labeled fatty acid was incorporated in vivo into the polar lipids of Mycoplasma laidlawii membranes. The electron paramagnetic resonance signal from either intact cells or their extracted lipids reflected the fatty acid composition of the Mycoplasma membranes. Comparison of signals from intact cells, gramicidin-treated cells, heat-treated cells, and extracted lipids indicates that a major portion of the membrane lipids is in a semiviscous hydrocarbon environment. The results also show that the spin label in the intact membrane is slightly but significantly less mobile than it is in protein-free lipid extracts made from these membranes. Correlated electron microscope examinations using the freeze-etch technique reveal particulate components in the hydrophobic region of the membrane. The mobility of the lipids in the intact cell membrane may be influenced by their association with these particles. Images PMID:4316683

Determination of Activity Coefficients of di-(2-ethylhexyl) Phosphoric Acid Dimer in Select Organic Solvents Using Vapor Phase Osmometry

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

Michael F. Gray; Peter Zalupski; Mikael Nilsson

2013-08-01

Effective models for solvent extraction require accurate characterization of the nonideality effects for each component, including the extractants. In this study, the nonideal behavior of the industrial extractant di(2-ethylhexyl) phosphoric acid has been investigated using vapor pressure osmometry (VPO). From the osmometry data, activity coefficients for the HDEHP dimer were obtained based on a formulation of the regular solution theory of Scatchard and Hildebrand, and the Margules two- and three-suffix equations. The results show similarity with a slope-analysis based relation from previous literature, although important differences are highlighted. The work points towards VPO as a useful technique for this typemore » of study, but care must be taken with the choice of standard and method of analysis.« less

Investigation of Diospyros Kaki L.f husk extracts as corrosion inhibitors and bactericide in oil field

PubMed Central

2013-01-01

Background Hydrochloric acid is used in oil-well acidizing commonly for improving the crude oil production of the low-permeable reservoirs, while it is a great challenge for the metal instruments involved in the acidification. Developing natural products as oilfield chemicals is a straight way to find less expensive, green and eco-friendly materials. The great plant resources in Qin-ling and Ba-shan Mountain Area of Shannxi Province enable the investigating of new green oil field chemicals. Diospyros Kaki L.f (persimmon), a famous fruit tree is widely planted in Qin-ling and Ba-shan Mountain Area of Shaanxi Province. It has been found that the crude persimmon extracts are complex mixtures containing vitamins, p-coumaric acid, gallic acid, catechin, flavonoids, carotenoids and condensed tannin and so on, which indicates the extracts of persimmon husk suitable to be used as green and eco-friendly corrosion inhibitors. Findings Extracts of persimmon husk were investigated, by using weight loss and potentiodynamic polarisation techniques, as green and eco-friendly corrosion inhibitors of Q235A steel in 1M HCl. The inhibition efficiency of the extracts varied with extract concentration from 10 to 1,000 mg/L. There are some synergistic effects between the extracts and KI, KSCN and HMTA. Potentiodynamic polarization studies indicate that extracts are mixed-type inhibitors. Besides, the extracts were screened for antibacterial activity against oil field microorganisms, and they showed good to moderate activity against SRB, IB and TGB. Conclusions The inhibition efficiency of the extracts varied with extract concentration from 10 to 1,000 mg/L, and the highest reaches to 65.1% with the con concentration of 1,000 mg/L WE. KI, KSCN and HMTA they can enhance the IE of WE effectively to 97.3% at most, but not effective for KI and KSCN to AE. Tafel polarisation measurements indicate the extracts behave as mixed type inhibitor. Investigation of the antibacterial activity against oil field microorganism showed the extracts can inhibit SRB, IB and TGB with moderate to highly efficiency under 1,000 mg/L, which makes extracts potential to be used as bifunctional oil field chemicals. PMID:23816431

Characteristic vector analysis as a technique for signature extraction of remote ocean color data

NASA Technical Reports Server (NTRS)

Grew, G. W.

1977-01-01

Characteristic vector analysis is being used to extract spectral signatures of suspended matter in the ocean from remote ocean color data collected with MOCS (Multichannel Ocean Color Sensor), a multispectral scanner. Spectral signatures appear to be obtainable either directly from characteristic vectors or through a transformation of these eigenvectors. Quantification of the suspended matter associated with each resulting signature seems feasible using associated coefficients generated by the technique. This paper presents eigenvectors associated with algae, 'sediment', acid waste, sewage sludge, and oil. The results suggest an efficient method of transmitting from satellites multispectral data of pollution in our oceans.

Extending the applicability of pressurized hot water extraction to compounds exhibiting limited water solubility by pH control: curcumin from the turmeric rhizome.

PubMed

Euterpio, Maria Anna; Cavaliere, Chiara; Capriotti, Anna Laura; Crescenzi, Carlo

2011-11-01

Pressurized hot water extraction (PHWE, also known as subcritical water extraction) is commonly considered to be an environmentally friendly extraction technique that could potentially replace traditional methods that use organic solvents. Unfortunately, the applicability of this technique is often limited by the very low water solubility of the target compounds, even at high temperatures. In this paper, the scope for broadening the applicability of PHWE by adjusting the pH of the water used in the extraction is demonstrated in the extraction of curcumin (which exhibits very limited water solubility) from untreated turmeric (Curcuma longa L.) rhizomes. Although poor extraction yields were obtained, even at high temperatures when using degassed water or neutral phosphate buffer as the extraction medium, yields exceeding those obtained by Soxhlet extraction were achieved using highly acidic pH buffers due to curcumin protonation. The influence of the temperature, pH, and buffer concentration on the extraction yield were investigated in detail by means of a series of designed experiments. Optimized conditions for the extraction of curcumin from turmeric by PHWE were estimated at 197 °C using 62 g/L buffer concentration at pH 1.6. The relationships between these variables were subjected to statistical analysis using response surface methodology.

Two simple techniques for the safe Sarcoptes collection and individual mite DNA extraction.

PubMed

Soglia, Dominga; Rambozzi, Luisa; Maione, Sandra; Spalenza, Veronica; Sartore, Stefano; Alasaad, Samer; Sacchi, Paola; Rossi, Luca

2009-10-01

Availability of mites is a recognized limiting factor of biological and genetic investigations of the genus Sarcoptes. Current methods of deoxyribonucleic acid (DNA) extraction from individual mites also need substantial improvement in efficiency and operator friendliness. We have first developed a technique for efficient and safe extraction of living mites from scabietic skin samples (crusts or deep skin scrapings). Its core device is a large plastic syringe connected with a 1.5-ml Eppendorf tube. The source material is introduced in the syringe and the device in a shoe box with the tip half of the tube emerging. Mites migrate towards a heat source during a minimum of 36 h. Then, the tube is detached and the mites utilized without risks for the operators. A second technique allows operator-friendly manipulation of individual mites for DNA extraction. Fixed mites are isolated by adhesion to a small strip of polyvinyl chloride (PVC) adhesive tape operated with tweezers. Then, mite and strip are plunged in the lyses buffer and the sample twice submitted to thermal shock for disruption of the chitinous exoskeleton. Data show that the tape does not interfere with successive DNA extraction with a commercial kit. The corresponding protocol, that we briefly name "PVC adhesive tape + thermal shock + kit DNA extraction," compares favorably with the available ones.

[Composition of chicken and quail eggs].

PubMed

Closa, S J; Marchesich, C; Cabrera, M; Morales, J C

1999-06-01

Qualified food composition data on lipids composition are needed to evaluate intakes as a risk factor in the development of heart disease. Proximal composition, cholesterol and fatty acid content of chicken and quail eggs, usually consumed or traded, were analysed. Proximal composition were determined using AOAC (1984) specific techniques; lipids were extracted by a Folch's modified technique and cholesterol and fatty acids were determined by gas chromatography. Results corroborate the stability of eggs composition. Cholesterol content of quail eggs is similar to chicken eggs, but it is almost the half content of data registered in Handbook 8. Differences may be attributed to the analytical methodology used to obtain them. This study provides data obtained with up-date analytical techniques and accessory information useful for food composition tables.

Profiling ABA metabolites in Nicotiana tabacum L. leaves by ultra-performance liquid chromatography-electrospray tandem mass spectrometry.

PubMed

Turecková, Veronika; Novák, Ondrej; Strnad, Miroslav

2009-11-15

We have developed a simple method for extracting and purifying (+)-abscisic acid (ABA) and eight ABA metabolites--phaseic acid (PA), dihydrophaseic acid (DPA), neophaseic acid (neoPA), ABA-glucose ester (ABAGE), 7'-hydroxy-ABA (7'-OH-ABA), 9'-hydroxy-ABA (9'-OH-ABA), ABAaldehyde, and ABAalcohol--before analysis by a novel technique for these substances, ultra-performance liquid chromatography-electrospray ionisation tandem mass spectrometry (UPLC-ESI-MS/MS). The procedure includes addition of deuterium-labelled standards, extraction with methanol-water-acetic acid (10:89:1, v/v), simple purification by Oasis((R)) HLB cartridges, rapid chromatographic separation by UPLC, and sensitive, accurate quantification by MS/MS in multiple reaction monitoring modes. The detection limits of the technique ranged between 0.1 and 1 pmol for ABAGE and ABA acids in negative ion mode, and 0.01-0.50 pmol for ABAGE, ABAaldehyde, ABAalcohol and the methylated acids in positive ion mode. The fast liquid chromatographic separation and analysis of ABA and its eight measured derivatives by UPLC-ESI-MS/MS provide rapid, accurate and robust quantification of most of the substances, and the low detection limits allow small amounts of tissue (1-5mg) to be used in quantitative analysis. To demonstrate the potential of the technique, we isolated ABA and its metabolites from control and water-stressed tobacco leaf tissues then analysed them by UPLC-ESI-MS/MS. Only ABA, PA, DPA, neoPA, and ABAGE were detected in the samples. PA was the most abundant analyte (ca. 1000 pmol/g f.w.) in both the control and water-stressed tissues, followed by ABAGE and DPA, which were both present at levels ca. 5-fold lower. ABA levels were at least 100-fold lower than PA concentrations, but they increased following the water stress treatment, while ABAGE, PA, and DPA levels decreased. Overall, the technique offers substantial improvements over previously described methods, enabling the detailed, direct study of diverse ABA metabolites in small amounts of plant tissue.

Trace element release from estuarine sediments of South Mosquito Lagoon near Kennedy Space Center

NASA Technical Reports Server (NTRS)

Menon, M. P.; Ghuman, G. S.; Emeh, C. O.

1979-01-01

Analytical partitioning of four trace metals in estuarine sediments collected from eight sites in South Mosquito Lagoon near Kennedy Space Center, in terms of four different categories was accomplished using four different extraction techniques. The concentrations of the four trace metals, Zn, Mn, Cd, and Cu, released in interstitial water extract, 1 N ammonium acetate extract, conc. HCl extract and fusion extract of sediments as well as their concentrations in water samples collected from the same location were determined using flame atomic absorption technique. From the analytical results the percentages of total amount of each metal distributed among four different categories, interstitial water phase, acetate extractable, acid extractable and detrital crystalline material, were determined. Our results suggest that analytical partitioning of trace metals in estuarine sediments may be used to study the mechanism of incorporation of trace metals with sediments from natural waters. A correlation between the seasonal variation in the concentration of acetate extractable trace metals in the sediment and similar variation in their concentration in water was observed. A mechanism for the release of trace metals from estuarine sediments to natural water is also suggested.

A C8-Modified Graphene@mSiO2 Composites Based Method for Quantification of Gallic Acid in Rat Plasma after Oral Administration of Changtai Granule and Its Application to Pharmacokinetics.

PubMed

Xu, Chen; Yu, Yingjia; Ling, Li; Wang, Yang; Zhang, Jundong; Li, Yan; Duan, Gengli

2017-01-01

A rapid, effective extraction technique has been established for measuring the gallic acid in rat plasma by using sandwich-structured graphene/mesoporous silica composites with C 8 -modified interior pore-walls as adsorbent. The unique characteristics of the graphene-silica composites excluded large molecules, like proteins, from the mesopore channels as a result of size exclusion effect, leading to a direct extraction of drug molecules from protein-rich biological samples such as plasma without any other pretreatment procedure. Followed by elution and centrifugation, the gallic acid-absorbed composites were rapidly isolated before LC-MS/MS. Serving as a reliable tool for analysis of Traditional Chinese Medicine: Changtai Granule, the newly developed method was fully validated and successfully applied in the pharmacokinetic study of gallic acid in rat plasma. Extraction recovery, matrix effect and stability were satisfactory in rat plasma. According to the results of pharmacokinetic studies, Changtai Granule exhibited greater adsorption, distribution and clearance properties of gallic acid in the treatment of ulcerative colitis. Hence, this study may offer a valuable alternative to simplify and speed up sample preparation, and be useful for clinical studies of related preparations.

A Rapid and Accurate Extraction Procedure for Analysing Free Amino Acids in Meat Samples by GC-MS

PubMed Central

Barroso, Miguel A.; Ruiz, Jorge; Antequera, Teresa

2015-01-01

This study evaluated the use of a mixer mill as the homogenization tool for the extraction of free amino acids in meat samples, with the main goal of analyzing a large number of samples in the shortest time and minimizing sample amount and solvent volume. Ground samples (0.2 g) were mixed with 1.5 mL HCl 0.1 M and homogenized in the mixer mill. The final biphasic system was separated by centrifugation. The supernatant was deproteinized, derivatized and analyzed by gas chromatography. This procedure showed a high extracting ability, especially in samples with high free amino acid content (recovery = 88.73–104.94%). It also showed a low limit of detection and quantification (3.8 · 10−4–6.6 · 10−4  μg μL−1 and 1.3 · 10−3–2.2 · 10−2  μg μL−1, resp.) for most amino acids, an adequate precision (2.15–20.15% for run-to-run), and a linear response for all amino acids (R 2 = 0.741–0.998) in the range of 1–100 µg mL−1. Moreover, it takes less time and requires lower amount of sample and solvent than conventional techniques. Thus, this is a cost and time efficient tool for homogenizing in the extraction procedure of free amino acids from meat samples, being an adequate option for routine analysis. PMID:25873963

New procedure for extraction of algal lipids from wet biomass: a green clean and scalable process.

PubMed

Dejoye Tanzi, Celine; Abert Vian, Maryline; Chemat, Farid

2013-04-01

A new procedure, called Simultaneous Distillation and Extraction Process (SDEP), for lipid extraction from wet microalgae (Nannochloropsis oculata and Dunaliella salina) was reported. This method does not require a pre-drying of the biomass and employs alternative solvents such as d-limonene, α-pinene and p-cymene. This procedure has been compared with Soxhlet extraction (Sox) and Bligh & Dyer method (B&D). For N. oculata, results showed that SDEP-cymene provided similar lipid yields to B&D (21.45% and 23.78%), while SDEP-limonene and pinene provided lower yields (18.73% and 18.75% respectively). For D. salina, SDEP-pinene provided the maximum lipid yield (3.29%) compared to the other solvents, which is quite close to B&D result (4.03%). No significant differences in terms of distribution of lipid classes and fatty acid composition have been obtained for different techniques. Evaluation of energy consumption indicates a substantial saving in the extraction cost by SDEP compared to the conventional extraction technique, Soxhlet. Copyright © 2013 Elsevier Ltd. All rights reserved.

A Lipid Extraction and Analysis Method for Characterizing Soil Microbes in Experiments with Many Samples

PubMed Central

Oates, Lawrence G.; Read, Harry W.; Gutknecht, Jessica L. M.; Duncan, David S.; Balser, Teri B.; Jackson, Randall D.

2017-01-01

Microbial communities are important drivers and regulators of ecosystem processes. To understand how management of ecosystems may affect microbial communities, a relatively precise but effort-intensive technique to assay microbial community composition is phospholipid fatty acid (PLFA) analysis. PLFA was developed to analyze phospholipid biomarkers, which can be used as indicators of microbial biomass and the composition of broad functional groups of fungi and bacteria. It has commonly been used to compare soils under alternative plant communities, ecology, and management regimes. The PLFA method has been shown to be sensitive to detecting shifts in microbial community composition. An alternative method, fatty acid methyl ester extraction and analysis (MIDI-FA) was developed for rapid extraction of total lipids, without separation of the phospholipid fraction, from pure cultures as a microbial identification technique. This method is rapid but is less suited for soil samples because it lacks an initial step separating soil particles and begins instead with a saponification reaction that likely produces artifacts from the background organic matter in the soil. This article describes a method that increases throughput while balancing effort and accuracy for extraction of lipids from the cell membranes of microorganisms for use in characterizing both total lipids and the relative abundance of indicator lipids to determine soil microbial community structure in studies with many samples. The method combines the accuracy achieved through PLFA profiling by extracting and concentrating soil lipids as a first step, and a reduction in effort by saponifying the organic material extracted and processing with the MIDI-FA method as a second step. PMID:28745639

Chemical speciation and mobilization of copper and zinc in naturally contaminated mine soils with citric and tartaric acids.

PubMed

Pérez-Esteban, Javier; Escolástico, Consuelo; Moliner, Ana; Masaguer, Alberto

2013-01-01

A one-step extraction procedure and a leaching column experiment were performed to assess the effects of citric and tartaric acids on Cu and Zn mobilization in naturally contaminated mine soils to facilitate assisted phytoextraction. A speciation modeling of the soil solution and the metal fractionation of soils were performed to elucidate the chemical processes that affected metal desorption by organic acids. Different extracting solutions were prepared, all of which contained 0.01 M KNO(3) and different concentrations of organic acids: control without organic acids, 0.5 mM citric, 0.5 mM tartaric, 10 mM citric, 10 mM tartaric, and 5 mM citric +5 mM tartaric. The results of the extraction procedure showed that higher concentrations of organic acids increased metal desorption, and citric acid was more effective at facilitating metal desorption than tartaric acid. Metal desorption was mainly influenced by the decreasing pH and the dissolution of Fe and Mn oxides, not by the formation of soluble metal-organic complexes as was predicted by the speciation modeling. The results of the column study reported that low concentrations of organic acids did not significantly increase metal mobilization and that higher doses were also not able to mobilize Zn. However, 5-10 mM citric acid significantly promoted Cu mobilization (from 1 mg kg(-1) in the control to 42 mg kg(-1) with 10 mM citric acid) and reduced the exchangeable (from 21 to 3 mg kg(-1)) and the Fe and Mn oxides (from 443 to 277 mg kg(-1)) fractions. Citric acid could efficiently facilitate assisted phytoextraction techniques. Copyright © 2012 Elsevier Ltd. All rights reserved.

Optimization of total vaporization solid-phase microextraction (TV-SPME) for the determination of lipid profiles of Phormia regina, a forensically important blow fly species.

PubMed

Kranz, William; Carroll, Clinton; Dixon, Darren; Picard, Christine; Goodpaster, John

2017-11-01

A new method has been developed for the determination of fatty acids, sterols, and other lipids which naturally occur within pupae of the blow fly Phormia regina. The method relies upon liquid extraction in non-polar solvent, followed by derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) w/ 1% trimethylchlorsilane (TMCS) carried out inside the sample vial. The analysis is facilitated by total vaporization solid-phase microextraction (TV-SPME), with gas chromatography-mass spectrometry (GC-MS) serving as the instrumentation for analysis. The TV-SPME delivery technique is approximately a factor of five more sensitive than traditional liquid injection, which may alleviate the need for rotary evaporation, reconstitution, collection of high performance liquid chromatography fractions, and many of the other pre-concentration steps that are commonplace in the current literature. Furthermore, the ability to derivatize the liquid extract in a single easy step while increasing sensitivity represents an improvement over current derivatization methods. The most common lipids identified in fly pupae were various saturated and unsaturated fatty acids ranging from lauric acid (12:0) to arachinoic acid (20:4), as well as cholesterol. The concentrations of myristic acid (14:0), palmitelaidic acid (16:2), and palmitoleic acid (16:1) were the most reliable indicators of the age of the pupae. Graphical abstract Blow fly pupae were extracted prior to emerging as adults. The extracts were analyzed via total vaporization solid-phase microextraction (TV-SPME), revealing a complex mixture of lipids that could be associated with the age of the insect. This information may assist in determining a post-mortum interval (PMI) in a death investigation.

A characterization of the antimalarial activity of the bark of Cylicodiscus gabunensis Harms.

PubMed

Aldulaimi, Omar; Uche, Fidelia I; Hameed, Hamza; Mbye, Haddijatou; Ullah, Imran; Drijfhout, Falko; Claridge, Timothy D W; Horrocks, Paul; Li, Wen-Wu

2017-02-23

A decoction of the bark of Cylicodiscus gabunensis Harms is used as a traditional medicine in the treatment of malaria in Nigeria. This study aims to validate the antimalarial potency of this decoction in vitro against Plasmodium falciparum and define potential bioactive constituents within the C. gabunensis bark. A bioassay-guided separation and fractionation protocol was applied to C. gabunensis extracts, exploiting the use of a Malaria Sybr Green I Fluorescence assay method to monitor antiproliferative effects on parasites as well as define 50% inhibition concentrations. Spectroscopic techniques, including GC-MS, TOF LC-MS and 1 H NMR were used to identify phytochemicals present in bioactive fractions. Analogues of gallic acid were synthesized de novo to support the demonstration of the antimalarial action of phenolic acids identified in C. gabunensis bark. In vitro cytotoxicity of plant extracts, fractions and gallate analogues was evaluated against the HepG2 cell line. The antimalarial activity of ethanolic extracts of C. gabunensis bark was confirmed in vitro, with evidence for phenolic acids, primarily gallic acid and close analogues such as ethyl gallate, likely providing this effect. Further fractionation produced the most potent fraction with a 50% inhibitory concentration of 4.7µg/ml. Spectroscopic analysis, including 1 H NMR, LC-MS and GC-MS analysis of this fraction and its acid hydrolyzed products, indicated the presence of conjugates of gallic acid with oligosaccharides. The extracts/fractions and synthetic alkyl and alkenyl gallates showed moderate selectivity against P. falciparum. These results support the use of the bark of C. gabunensis as a traditional medicine in the treatment of human malaria, with phenolic acid oligosaccharide complexes evident in the most bioactive fractions. Copyright © 2017 Elsevier Ireland Ltd. All rights reserved.

Antioxidant activity and total phenolic and flavonoids content variations of leaves extracts of white Horehound (Marrubium vulgare Linné) from three geographical origins.

PubMed

Bouterfas, K; Mehdadi, Z; Elaoufi, M M; Latreche, A; Benchiha, W

2016-11-01

To elucidate the effect of the sampling location of Marrubium vulgare L. leaves on phenolic contents and antioxidant proprieties of flavonoids extracts. M. vulgare L. leaves were collected from three different geographical locations belonging to northwest Algeria: Tessala (mountain region), M'sila forest (coastal region), and Ain Skhouna (steppe region). The flavonoid extraction was achieved using organic solvents with different polarities (methanol, chloroform, ethyl acetate, and hexane). Folin-Ciocalteu colorimetric method was used for quantification of total phenolic contents, and aluminum chloride assay for quantification of total flavonoid contents. The antioxidant properties of flavonoids extract were studied by free l,l-diphenyl-2-picrylhydrazyl radical-scavenging technique. Total phenolic and flavonoids concentrations varied respectively between 40.7 and 160mg gallic acid equivalents/g and 27.4 and 66.3mg catechin equivalents/g. The DPPH free radical-scavenging activity shows that the antioxidant activity of the flavonoid extracts varied significantly (P<0.001) depending on the type of the organic solvent used, and the sampling location. The methanol, chloroform and ethyl acetate extracts exhibited the highest percentages of inhibition unlike to the aqueous and hexane extracts. These percentages are ranged from 54.8 to 98.8% at 1000μg/mL. In general, M'sila forest flavonoids extracts showed the highest free radical inhibition capacity; followed by those of Ain Skhouna and Tessala Mountain. The inhibitory concentration 50 (IC 50 ) ranged from 33.7 to 774μg/mL and often exceeded those recorded by phenolic standards (ascorbic acid, gallic acid, caffeic acid, tannic acid and catechin). The phytochemical screening revealed the presence of some flavonoid classes, such as flavans and flavanols. The results suggested a potent antioxidant activity of M. vulgare flavonoids extracts, which may find its application in feature research for the food and the pharmacological industries. Copyright © 2016 Académie Nationale de Pharmacie. Published by Elsevier Masson SAS. All rights reserved.

Effect of ultrasonic treatment on total phenolic extraction from Lavandula pubescens and its application in palm olein oil industry.

PubMed

Rashed, Marwan M A; Tong, Qunyi; Abdelhai, Mandour H; Gasmalla, Mohammed A A; Ndayishimiye, Jean B; Chen, Long; Ren, Fei

2016-03-01

The aims of the current study were to evaluate the best technique for total phenolic extraction from Lavandula pubescens (Lp) and its application in vegetable oil industries as alternatives of synthetic food additives (TBHQ and BHT). To achieve these aims, three techniques of extraction were used: ultrasonic-microwave (40 kHz, 50 W, microwave power 480 W, 5 min), ultrasonic-homogenizer (20 kHz, 150 W, 5 min) and conventional maceration as a control. By using the Folin-Ciocalteu method, the total phenolic contents (TPC) (mg gallic acid equivalent/g dry matter) were found to be 253.87, 216.96 and 203.41 for ultrasonic-microwave extract, ultrasonic-homogenizer extract and maceration extract, respectively. The ultrasonic-microwave extract achieved the higher scavenger effect of DPPH (90.53%) with EC50 (19.54 μg/mL), and higher inhibition of β-carotene/linoleate emulsion deterioration (94.44%) with IC50 (30.62 μg/mL). The activity of the ultrasonic-microwave treatment could prolong the induction period (18.82 h) and oxidative stability index (1.67) of fresh refined, bleached and deodorized palm olein oil (RBDPOo) according to Rancimat assay. There was an important synergist effect between citric acid and Lp extracts in improving the oxidative stability of fresh RBDPOo. The results of this work also showed that the ultrasonic-microwave assisted extract was the most effective against Gram-positive and Gram-negative strains that were assessed in this study. The uses of ultrasonic-microwave could induce the acoustic cavitation and rupture of plant cells, and this facilitates the flow of solvent into the plant cells and enhances the desorption from the matrix of solid samples, and thus would enhance the efficiency of extraction based on cavitation phenomenon. Copyright © 2015 Elsevier B.V. All rights reserved.

Microextraction techniques for the determination of volatile and semivolatile organic compounds from plants: a review.

PubMed

Yang, Cui; Wang, Juan; Li, Donghao

2013-10-17

Vegetables and fruits are necessary for human health, and traditional Chinese medicine that uses plant materials can cure diseases. Thus, understanding the composition of plant matrix has gained increased attention in recent years. Since plant matrix is very complex, the extraction, separation and quantitation of these chemicals are challenging. In this review we focus on the microextraction techniques used in the determination of volatile and semivolatile organic compounds (such as esters, alcohols, aldehydes, hydrocarbons, ketones, terpenes, sesquiterpene, phenols, acids, plant secondary metabolites and pesticides) from plants (e.g., fruits, vegetables, medicinal plants, tree leaves, etc.). These microextraction techniques include: solid phase microextraction (SPME), stir-bar sorptive extraction (SBSE), single drop microextraction (SDME), hollow fiber liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME), and gas purge microsyringe extraction (GP-MSE). We have taken into consideration papers published from 2008 to the end of January 2013, and provided critical and interpretative review on these techniques, and formulated future trends in microextraction for the determination of volatile and semivolatile compounds from plants. Copyright © 2013 Elsevier B.V. All rights reserved.

Antioxidant activity, phenolic content, and peroxide value of essential oil and extracts of some medicinal and aromatic plants used as condiments and herbal teas in Turkey.

PubMed

Ozcan, Mehmet Musa; Erel, Ozcan; Herken, Emine Etöz

2009-02-01

The antioxidant activity, total peroxide values, and total phenol contents of several medicinal and aromatic plant essential oil and extracts from Turkey were examined. Total phenolic contents were determined using a spectrophotometric technique and calculated as gallic acid equivalents. Total antioxidant activity of essential oil and extracts varied from 0.6853 to 1.3113 and 0.3189 to 0.6119 micromol of Trolox equivalents/g, respectively. The total phenolic content of essential oil ranged from 0.0871 to 0.5919 mg of gallic acid/g dry weight. However, the total phenolic contents of extracts were found to be higher compared with those of essential oils. The amount of total peroxide values of oils varied from 7.31 (pickling herb) to 58.23 (bitter fennel flower) mumol of H(2)O(2)/g. As a result, it is shown that medicinal plant derivatives such as extract and essential oils can be useful as a potential source of total phenol, peroxide, and antioxidant capacity for protection of processed foods.

Automated DNA extraction platforms offer solutions to challenges of assessing microbial biofouling in oil production facilities.

PubMed

Oldham, Athenia L; Drilling, Heather S; Stamps, Blake W; Stevenson, Bradley S; Duncan, Kathleen E

2012-11-20

The analysis of microbial assemblages in industrial, marine, and medical systems can inform decisions regarding quality control or mitigation. Modern molecular approaches to detect, characterize, and quantify microorganisms provide rapid and thorough measures unbiased by the need for cultivation. The requirement of timely extraction of high quality nucleic acids for molecular analysis is faced with specific challenges when used to study the influence of microorganisms on oil production. Production facilities are often ill equipped for nucleic acid extraction techniques, making the preservation and transportation of samples off-site a priority. As a potential solution, the possibility of extracting nucleic acids on-site using automated platforms was tested. The performance of two such platforms, the Fujifilm QuickGene-Mini80™ and Promega Maxwell®16 was compared to a widely used manual extraction kit, MOBIO PowerBiofilm™ DNA Isolation Kit, in terms of ease of operation, DNA quality, and microbial community composition. Three pipeline biofilm samples were chosen for these comparisons; two contained crude oil and corrosion products and the third transported seawater. Overall, the two more automated extraction platforms produced higher DNA yields than the manual approach. DNA quality was evaluated for amplification by quantitative PCR (qPCR) and end-point PCR to generate 454 pyrosequencing libraries for 16S rRNA microbial community analysis. Microbial community structure, as assessed by DGGE analysis and pyrosequencing, was comparable among the three extraction methods. Therefore, the use of automated extraction platforms should enhance the feasibility of rapidly evaluating microbial biofouling at remote locations or those with limited resources.

Automated DNA extraction platforms offer solutions to challenges of assessing microbial biofouling in oil production facilities

PubMed Central

2012-01-01

The analysis of microbial assemblages in industrial, marine, and medical systems can inform decisions regarding quality control or mitigation. Modern molecular approaches to detect, characterize, and quantify microorganisms provide rapid and thorough measures unbiased by the need for cultivation. The requirement of timely extraction of high quality nucleic acids for molecular analysis is faced with specific challenges when used to study the influence of microorganisms on oil production. Production facilities are often ill equipped for nucleic acid extraction techniques, making the preservation and transportation of samples off-site a priority. As a potential solution, the possibility of extracting nucleic acids on-site using automated platforms was tested. The performance of two such platforms, the Fujifilm QuickGene-Mini80™ and Promega Maxwell®16 was compared to a widely used manual extraction kit, MOBIO PowerBiofilm™ DNA Isolation Kit, in terms of ease of operation, DNA quality, and microbial community composition. Three pipeline biofilm samples were chosen for these comparisons; two contained crude oil and corrosion products and the third transported seawater. Overall, the two more automated extraction platforms produced higher DNA yields than the manual approach. DNA quality was evaluated for amplification by quantitative PCR (qPCR) and end-point PCR to generate 454 pyrosequencing libraries for 16S rRNA microbial community analysis. Microbial community structure, as assessed by DGGE analysis and pyrosequencing, was comparable among the three extraction methods. Therefore, the use of automated extraction platforms should enhance the feasibility of rapidly evaluating microbial biofouling at remote locations or those with limited resources. PMID:23168231

The ultrasonic-enhanced factor of mass-transfer coefficient in the supercritical carbon dioxide extraction

NASA Astrophysics Data System (ADS)

Luo, Benyi; Lu, Yigang

2008-10-01

Based on several hypotheses about the process of supercritical carbon dioxide extraction, the onflow around the solute granule is figured out by the Navier-Stocks equation. In combination with the Higbie’s solute infiltration model, the link between the mass-transfer coefficient and the velocity of flow is found. The mass-transfer coefficient with the ultrasonical effect is compared with that without the ultrasonical effect, and then a new parameter named the ultrasonic-enhanced factor of mass-transfer coefficient is brought forward, which describes the mathematical model of the supercritical carbon dioxide extraction process enhanced by ultrasonic. The model gives out the relationships among the ultrasonical power, the ultrasonical frequency, the radius of solute granule and the ultrasonic-enhanced factor of mass-transfer coefficient. The results calculated by this model fit well with the experimental data, including the extraction of Coix Lacryma-jobi Seed Oil (CLSO) and Coix Lacryma-jobi Seed Ester (CLSE) from coix seeds and the extraction of Eicosapentaenoic Acid (EPA) and Docosahexaenoic Acid (DHA) from the alga by means of the ultrasonic-enhanced supercritical carbon dioxide extraction (USFE) and the supercritical carbon dioxide extraction (SFE) respectively. This proves the rationality of the ultrasonic-enhanced factor model. The model provides a theoretical basis for the application of ultrasonic-enhanced supercritical fluid extraction technique.

Extraction and separation of Co(II) and Ni(II) from acidic sulfate solutions using Aliquat 336.

PubMed

Nayl, A A

2010-01-15

Extraction and separation of Co(II) and Ni(II) from acidic sulfate solutions by solvent extraction technique were studied using different forms of Aliquat 336 diluted with kerosene. The extraction percent of each metal ion was found to increase with increasing pH and extractant concentration. Co(II) was preferentially extracted by different forms of Aliquat 336 over Ni(II) under the same extraction conditions. From analysis of the experimental results, the extraction mechanism of R(4)N-forms was proposed with Co(II). It was found that the highest separation factor (S(Co/Ni)) value of 606.7 was obtained with 0.36 M R(4)N-SCN in kerosene from 2.0M H(2)SO(4) solution at pH 4.8 and shaking time of 20 min. Stripping of the two metal ions from the organic phase was also investigated. Based on the experimental results, a separation method was developed and tested to separate high purity Co(II), Ni(II) and Ln(III) from Ni-MH batteries leached by 2.0M H(2)SO(4). Based on the experimental results, a flow sheet was developed and tested and 0.34 g Co, 1.39 g Ln and 5.2g Ni were obtained from the leaching process.

Isolation and Characterization of Phosphatidyl Choline from Spinach Leaves.

ERIC Educational Resources Information Center

Devor, Kenneth A.

1979-01-01

This inexpensive but informative experiment for undergraduate biochemistry students involves isolating phosphatidyl choline from spinach leaves. Emphasis is on introducing students to techniques of lipid extraction, separation of lipids, identification using thin layer chromatography, and identification of fatty acids. Three periods of three hours…

Yield and quality of pectins extractable from the peels of thai mango cultivars depending on fruit ripeness.

PubMed

Sirisakulwat, Suparat; Nagel, Andreas; Sruamsiri, Pittaya; Carle, Reinhold; Neidhart, Sybille

2008-11-26

Pectins, recovered from the peels of four mango ( Mangifera indica L.) cultivars by mimicking industrial techniques, were evaluated in terms of yield, composition, macromolecular properties, and technofunctional quality. Freeze-dried peels of mature-green fruits, after major mesocarp softening, and at full ripeness were extracted using hot acid. The pectins were precipitated in propan-2-ol and their crude yields quantified as alcohol-insoluble substance. Like apple pomace, the dried peels provided hardly acetylated (DAc < 6.3%) rapid-set to ultrarapid-set high-methoxyl pectins at starch-adjusted yields of 11-21 g/100 g. However, despite similar high molecular weight fractions and galacturonic acid/rhamnose ratios, their average molecular weight was markedly reduced by a characteristic, almost monodisperse fraction of 16000-19000. Expanded galactans, indicated by galactose/rhamnose ratios of 15-24 mol/mol, probably represented arabinogalactan side-chain fragments withstanding hot-acid extraction at pH 1.5 and 2.0, as implied by arabinose/galactose ratios of 8-15 and 33-56 mol/100 mol, respectively. Limited galacturonic acid contents made the mango peel pectins less valuable than commercial apple pectins with regard to gelling capacity and thickening properties. Whereas starch and matrix glycan fragments almost completely degraded during ripening, depolymerization of pectins and galactans was insignificant. Technofunctional properties, modulated by extraction at different pH values, were ascribed to structural differences influencing macromolecular entanglements.

Isolation of quercetin and mandelic acid from Aesculus indica fruit and their biological activities.

PubMed

Zahoor, Muhammad; Shafiq, Sadaf; Ullah, Habib; Sadiq, Abdul; Ullah, Farhat

2018-06-26

In this study Aesculus indica fruit was subjected to isolation of phytochemicals. Two antioxidants quercetin and Mandelic acid were isolated in pure state. The free radical scavenging and acetyl choline esterase inhibitory potential of the crude extract and sub fractions were also determined. The antioxidant capacity of crude extract, fractions and isolated compounds were determined by DPPH and ABTS methods. Folin-Ciocalteu reagent method was used to estimate the total phenolic contents and were found to be 78.34 ± 0.96, 44.16 ± 1.05, 65.45 ± 1.29, 37.85 ± 1.44 and 50.23 ± 2.431 (mg/g of gallic acid) in crude extract, ethyl acetate, chloroform, n-hexane and aqueous fractions respectively. The flavonoid concentration in crude extract, ethyl acetate, chloroform, n-hexane and aqueous fraction were; 85.30 ± 1.20, 53.80 ± 1.07, 77.50 ± 1.12, 26.30 ± 1.35 and 37.78 ± 1.25 (mg/g of quercetin) respectively. The chloroform fraction was more potent against enzymes, acetyl choline esterase and butyryl choline esterase (IC 50  = 85 and 160 μg/ml respectively). The phenolic compounds in the crude extract and fractions were determined using HPLC standard method. Chlorogenic acid, quercetin, phloroglucinol, rutin, mandelic acid and hydroxy benzoic acid were detected at retention times 6.005, 10.062, 22.623, 30.597, 35.490 and 36.211 in crude extract and different fractions. The ethyl acetate fraction was rich in the targeted compounds and was therefore subjected to column isolation. The HPLC chromatogram of isolated compounds showed single peak at specified retention times which confirms their isolation in pure state. The isolated compounds were then characterized by FTIR and NMR spectrophotometric techniques. The Aesculus indica fruit extracts showed antioxidant and anticholine esterase inhibitory potentials. Two bioactive compounds were isolated in the pure form ethyl acetate fraction. From results it was concluded that the fruit of this plant could be used to minimize oxidative stress caused by reactive oxygen species.

Alternative to antibiotics against Pseudomonas aeruginosa: Effects of Glycyrrhiza glabra on membrane permeability and inhibition of efflux activity and biofilm formation in Pseudomonas aeruginosa and its in vitro time-kill activity.

PubMed

Chakotiya, Ankita Singh; Tanwar, Ankit; Narula, Alka; Sharma, Rakesh Kumar

2016-09-01

The multi-drug resistance offered by Pseudomonas aeruginosa to antibiotics can be attributed towards its propensity to develop biofilm, modification in cell membrane and to efflux antibacterial drugs. The present study explored the activity of Glycyrrhiza glabra and one of its pure compounds, glycyrrhizic acid against P. aeruginosa and their mechanism of action in terms of the effect on membrane permeability, efflux activity, and biofilm formation were determined. Minimum inhibitory concentrations were determined by using broth dilution technique. The minimum bactericidal concentrations were assessed on agar plate. The MIC of the extract and glycyrrhizic acid was found to be 200 and 100 μg ml(-1), respectively. The MBC was found to be 800 and 400 μg ml(-1) in the case of extract and glycyrrhizic acid, respectively. Time -dependent killing efficacy was also estimated. Flowcytometric analysis with staining methods was used to determine the effect of extract and glycyrrhizic acid at 2 × MIC on different physiological parameters and compared it with the standard (antibiotic). The growth of P. aeruginosa was significantly inhibited by extract and the pure compound. The herbal extract and the glycyrrhic acid were also found to effective in targeting the physiological parameters of the bacteria that involve cell membrane permeabilization, efflux activity, and biofilm formation. This study reports the antipseudomonal action of Glycyrrhiza glabra and one of its compound and provides insight into their mode of action. Copyright © 2016 Elsevier Ltd. All rights reserved.

Solvent extraction of organic acids from stillage for its re-use in ethanol production process.

PubMed

Castro, G A; Caicedo, L A; Alméciga-Díaz, C J; Sanchez, O F

2010-06-01

Stillage re-use in the fermentation stage in ethanol production is a technique used for the reduction of water and fermentation nutrients consumption. However, the inhibitory effect on yeast growth of the by-products and feed components that remains in stillage increases with re-use and reduces the number of possible recycles. Several methods such as ultrafiltration, electrodialysis and advanced oxidation processes have been used in stillage treatment prior its re-use in the fermentation stage. Nevertheless, few studies evaluating the effect of solvent extraction as a stillage treatment option have been performed. In this work, the inhibitory effect of serial stillage recycling over ethanol and biomass production was determined, using acetic acid as a monitoring compound during the fermentation and solvent extraction process. Raw palm oil methyl ester showed the highest acetic acid extraction from the aqueous phase, presenting a distribution coefficient of 3.10 for a 1:1 aqueous phase mixture:solvent ratio. Re-using stillage without treatment allowed up to three recycles with an ethanol production of 53.7 +/- 2.0 g L(-1), which was reduced 25% in the fifth recycle. Alternatively, treated stillage allowed up to five recycles with an ethanol final concentration of 54.7 +/- 1.3 g L(- 1). These results show that reduction of acetic acid concentration by an extraction process with raw palm oil methyl ester before re-using stillage improves the number of recycles without a major effect on ethanol production. The proposed process generates a palm oil methyl ester that contains organic acids, among other by-products, that could be used for product recovery and as an alternative fuel.

Chemometric Profile of Root Extracts of Rhodiola imbricata Edgew. with Hyphenated Gas Chromatography Mass Spectrometric Technique

PubMed Central

Tayade, Amol B.; Dhar, Priyanka; Kumar, Jatinder; Sharma, Manu; Chauhan, Rajinder S.; Chaurasia, Om P.; Srivastava, Ravi B.

2013-01-01

Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo), belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS) technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S); 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl) phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl); α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful results in designing a novel drug. PMID:23326358

[Ganoderma triterpenoids from aqueous extract of Ganoderma lucidum].

PubMed

Che, Xian-Qiang; Li, Shao-Ping; Zhao, Jing

2017-05-01

A new triterpenoid and 18 analogues were isolated from the water extract of Ganoderma lucidum by column chromatographic techniques, including silica gel, ODS, Sephadex LH-20, and HPLC. The new compound was elucidated as 2β-acetoxy-3β,25-dihydroxy-7,11,15-trioxo-lanost-8-en-26-oic acid on the basis of analyses of extensive spectroscopic data and its physicochemical properties. Comparison of NMR data with those reported in literature, the known analogues were determined as ganoderic acid H (2), 12β-acetoxy-3β,7β-dihydroxy-11,15,23-trioxo-lanost-8,16-dien-26-oic acid (3), ganoderenic acid D (4),ganoderic acid C1 (5),ganoderic acid G (6),3β,7β-dihydroxy-11,15,23-trioxo-lanost-8,16-dien-26-oic acid (7),ganoderic acid B (8),ganoderic acid C6 (9),3β,15α-dihydroxy-7,11,23-trioxo-lanost-8,16-dien-26-oic acid (10),ganoderic acid A (11),ganolucidic acid A (12),lucidenic acid E2 (13),lucidenic acid N (14),lucidenic acid P (15), lucidenic acid B (16),lucidenic acid A (17),lucidenic acid C (18),and lucidenic acid L (19), respectively. Compound 1 is new compound and compounds 2-19 have been reported from G. lucidum. The present study enriches the knowledge of the chemical constituent of G. lucidum and completes chemical investigation of water decoction that is traditional use of G. lucidum. Copyright© by the Chinese Pharmaceutical Association.

Simultaneous Extraction Optimization and Analysis of Flavonoids from the Flowers of Tabernaemontana heyneana by High Performance Liquid Chromatography Coupled to Diode Array Detector and Electron Spray Ionization/Mass Spectrometry

PubMed Central

Sathishkumar, Thiyagarajan; Baskar, Ramakrishnan; Aravind, Mohan; Tilak, Suryanarayanan; Deepthi, Sri; Bharathikumar, Vellalore Maruthachalam

2013-01-01

Flavonoids are exploited as antioxidants, antimicrobial, antithrombogenic, antiviral, and antihypercholesterolemic agents. Normally, conventional extraction techniques like soxhlet or shake flask methods provide low yield of flavonoids with structural loss, and thereby, these techniques may be considered as inefficient. In this regard, an attempt was made to optimize the flavonoid extraction using orthogonal design of experiment and subsequent structural elucidation by high-performance liquid chromatography-diode array detector-electron spray ionization/mass spectrometry (HPLC-DAD-ESI/MS) techniques. The shake flask method of flavonoid extraction was observed to provide a yield of 1.2 ± 0.13 (mg/g tissue). With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue). The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction. About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana. The study has also concluded that L16 orthogonal design of experiment is an effective method for the extraction of flavonoid than the shake flask method. PMID:25969771

Spectroscopic methods of process monitoring for safeguards of used nuclear fuel separations

NASA Astrophysics Data System (ADS)

Warburton, Jamie Lee

To support the demonstration of a more proliferation-resistant nuclear fuel processing plant, techniques and instrumentation to allow the real-time, online determination of special nuclear material concentrations in-process must be developed. An ideal materials accountability technique for proliferation resistance should provide nondestructive, realtime, on-line information of metal and ligand concentrations in separations streams without perturbing the process. UV-Visible spectroscopy can be adapted for this precise purpose in solvent extraction-based separations. The primary goal of this project is to understand fundamental URanium EXtraction (UREX) and Plutonium-URanium EXtraction (PUREX) reprocessing chemistry and corresponding UV-Visible spectroscopy for application in process monitoring for safeguards. By evaluating the impact of process conditions, such as acid concentration, metal concentration and flow rate, on the sensitivity of the UV-Visible detection system, the process-monitoring concept is developed from an advanced application of fundamental spectroscopy. Systematic benchtop-scale studies investigated the system relevant to UREX or PUREX type reprocessing systems, encompassing 0.01-1.26 M U and 0.01-8 M HNO3. A laboratory-scale TRansUranic Extraction (TRUEX) demonstration was performed and used both to analyze for potential online monitoring opportunities in the TRUEX process, and to provide the foundation for building and demonstrating a laboratory-scale UREX demonstration. The secondary goal of the project is to simulate a diversion scenario in UREX and successfully detect changes in metal concentration and solution chemistry in a counter current contactor system with a UV-Visible spectroscopic process monitor. UREX uses the same basic solvent extraction flowsheet as PUREX, but has a lower acid concentration throughout and adds acetohydroxamic acid (AHA) as a complexant/reductant to the feed solution to prevent the extraction of Pu. By examining UV-Visible spectra gathered in real time, the objective is to detect the conversion from the UREX process, which does not separate Pu, to the PUREX process, which yields a purified Pu product. The change in process chemistry can be detected in the feed solution, aqueous product or in the raffinate stream by identifying the acid concentration, metal distribution and the presence or absence of AHA. A fiber optic dip probe for UV-Visible spectroscopy was integrated into a bank of three counter-current centrifugal contactors to demonstrate the online process monitoring concept. Nd, Fe and Zr were added to the uranyl nitrate system to explore spectroscopic interferences and identify additional species as candidates for online monitoring. This milestone is a demonstration of the potential of this technique, which lies in the ability to simultaneously and directly monitor the chemical process conditions in a reprocessing plant, providing inspectors with another tool to detect nuclear material diversion attempts. Lastly, dry processing of used nuclear fuel is often used as a head-end step before solvent extraction-based separations such as UREX or TRUEX. A non-aqueous process, used fuel treatment by dry processing generally includes chopping of used fuel rods followed by repeated oxidation-reduction cycles and physical separation of the used fuel from the cladding. Thus, dry processing techniques are investigated and opportunities for online monitoring are proposed for continuation of this work in future studies.

Improved sample preparation of glyphosate and methylphosphonic acid by EPA method 6800A and time-of-flight mass spectrometry using novel solid-phase extraction.

PubMed

Wagner, Rebecca; Wetzel, Stephanie J; Kern, John; Kingston, H M Skip

2012-02-01

The employment of chemical weapons by rogue states and/or terrorist organizations is an ongoing concern in the United States. The quantitative analysis of nerve agents must be rapid and reliable for use in the private and public sectors. Current methods describe a tedious and time-consuming derivatization for gas chromatography-mass spectrometry and liquid chromatography in tandem with mass spectrometry. Two solid-phase extraction (SPE) techniques for the analysis of glyphosate and methylphosphonic acid are described with the utilization of isotopically enriched analytes for quantitation via atmospheric pressure chemical ionization-quadrupole time-of-flight mass spectrometry (APCI-Q-TOF-MS) that does not require derivatization. Solid-phase extraction-isotope dilution mass spectrometry (SPE-IDMS) involves pre-equilibration of a naturally occurring sample with an isotopically enriched standard. The second extraction method, i-Spike, involves loading an isotopically enriched standard onto the SPE column before the naturally occurring sample. The sample and the spike are then co-eluted from the column enabling precise and accurate quantitation via IDMS. The SPE methods in conjunction with IDMS eliminate concerns of incomplete elution, matrix and sorbent effects, and MS drift. For accurate quantitation with IDMS, the isotopic contribution of all atoms in the target molecule must be statistically taken into account. This paper describes two newly developed sample preparation techniques for the analysis of nerve agent surrogates in drinking water as well as statistical probability analysis for proper molecular IDMS. The methods described in this paper demonstrate accurate molecular IDMS using APCI-Q-TOF-MS with limits of quantitation as low as 0.400 mg/kg for glyphosate and 0.031 mg/kg for methylphosphonic acid. Copyright © 2012 John Wiley & Sons, Ltd.

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

PubMed

Sewram, V; Raynor, M W; Mulholland, D A; Raidoo, D M

2001-07-01

In this descriptive study, the superciritical fluid extract of the roots of Clivia miniata L. was tested for uterotonic activity using guinea pig uterine smooth muscle in vitro. Extraction was performed with water modified supercritical carbon dioxide at 400 atm and 80 degrees C. The uterine contractions induced by this extract were compared to those induced by the aqueous extract and found to be active at lower doses. The active compounds were isolated and the structures elucidated by spectroscopic and chromatographic techniques. Both linoleic acid and 5-hydroxymethyl-2-furancarboxaldehyde isolated from the extract were found to induce muscle contractions individually. The pharmacological mode of action of 5-hydroxymethyl-2-furancarboxaldehyde was assessed using two receptor agonists and antagonists. This compound was found to mediate its effect through cholinergic receptors.

SPECTROSCOPIC ONLINE MONITORING FOR PROCESS CONTROL AND SAFEGUARDING OF RADIOCHEMICAL STREAMS

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

Bryan, Samuel A.; Levitskaia, Tatiana G.

2013-09-29

There is a renewed interest worldwide to promote the use of nuclear power and close the nuclear fuel cycle. The long term successful use of nuclear power is critically dependent upon adequate and safe processing and disposition of the used nuclear fuel. Liquid-liquid extraction is a separation technique commonly employed for the processing of the dissolved used nuclear fuel. The instrumentation used to monitor these processes must be robust, require little or no maintenance, and be able to withstand harsh environments such as high radiation fields and aggressive chemical matrices. This paper summarizes application of the absorption and vibrational spectroscopicmore » techniques supplemented by physicochemical measurements for radiochemical process monitoring. In this context, our team experimentally assessed the potential of Raman and spectrophotometric techniques for online real-time monitoring of the U(VI)/nitrate ion/nitric acid and Pu(IV)/Np(V)/Nd(III), respectively, in solutions relevant to spent fuel reprocessing. These techniques demonstrate robust performance in the repetitive batch measurements of each analyte in a wide concentration range using simulant and commercial dissolved spent fuel solutions. Spectroscopic measurements served as training sets for the multivariate data analysis to obtain partial least squares predictive models, which were validated using on-line centrifugal contactor extraction tests. Satisfactory prediction of the analytes concentrations in these preliminary experiments warrants further development of the spectroscopy-based methods for radiochemical process control and safeguarding. Additionally, the ability to identify material intentionally diverted from a liquid-liquid extraction contactor system was successfully tested using on-line process monitoring as a means to detect the amount of material diverted. A chemical diversion and detection from a liquid-liquid extraction scheme was demonstrated using a centrifugal contactor system operating with the simulant PUREX extraction system of Nd(NO3)3/nitric acid aqueous phase and TBP/n-dodecane organic phase. During a continuous extraction experiment, a portion of the feed from a counter-current extraction system was diverted while the spectroscopic on-line process monitoring system was simultaneously measuring the feed, raffinate and organic products streams. The amount observed to be diverted by on-line spectroscopic process monitoring was in excellent agreement with values based from the known mass of sample directly taken (diverted) from system feed solution.« less

Enrichment of the Glycyrrhizic Acid from Licorice Roots (Glycyrrhiza glabra L.) by Isoelectric Focused Adsorptive Bubble Chromatography.

PubMed

Karaoğul, Eyyüp; Parlar, Perihan; Parlar, Harun; Alma, M Hakkı

2016-01-01

The main aim of this study was to enrich glycyrrhizic acid ammonium salt known as one of the main compounds of licorice roots (Glycyrrhiza glabra L.) by isoelectric focused adsorptive bubble separation technique with different foaming agents. In the experiments, four bubble separation parameters were used with β-lactoglobulin, albumin bovine, and starch (soluble) preferred as foaming agents and without additives. The enrichment of glycyrrhizic acid ammonium salt into the foam was influenced by different additive substances. The results showed that highest enrichment values were obtained from β-lactoglobulin as much as 368.3 times. The lowest enrichment values (5.9 times) were determined for the application without additive. After enrichment, each experiment of glycyrrhizic acid ammonium salt confirmed that these substances could be quantitatively enriched into the collection vessel with isoelectric focused adsorptive bubble separation technique. The transfer of glycyrrhizic acid ammonium salt into the foam from standard solution in the presence of additive was more efficient than aqueous licorice extract.

Enrichment of the Glycyrrhizic Acid from Licorice Roots (Glycyrrhiza glabra L.) by Isoelectric Focused Adsorptive Bubble Chromatography

PubMed Central

Karaoğul, Eyyüp; Parlar, Perihan; Parlar, Harun; Alma, M. Hakkı

2016-01-01

The main aim of this study was to enrich glycyrrhizic acid ammonium salt known as one of the main compounds of licorice roots (Glycyrrhiza glabra L.) by isoelectric focused adsorptive bubble separation technique with different foaming agents. In the experiments, four bubble separation parameters were used with β-lactoglobulin, albumin bovine, and starch (soluble) preferred as foaming agents and without additives. The enrichment of glycyrrhizic acid ammonium salt into the foam was influenced by different additive substances. The results showed that highest enrichment values were obtained from β-lactoglobulin as much as 368.3 times. The lowest enrichment values (5.9 times) were determined for the application without additive. After enrichment, each experiment of glycyrrhizic acid ammonium salt confirmed that these substances could be quantitatively enriched into the collection vessel with isoelectric focused adsorptive bubble separation technique. The transfer of glycyrrhizic acid ammonium salt into the foam from standard solution in the presence of additive was more efficient than aqueous licorice extract. PMID:26949562

Stable hydrogen and carbon isotope ratios of extractable hydrocarbons in the Murchison meteorite

NASA Technical Reports Server (NTRS)

Krishnamurthy, R. V.; Epstein, S.; Pizzarello, S.; Cronin, J. R.; Yuen, G. U.

1991-01-01

A fairly fool-proof method to ensure that the compounds isolated from meteorites are truly part of the meteorites and not an artifact introduced by exposure to the terrestrial environment, storage, or handling is presented. The stable carbon and hydrogen isotope ratios in several of the chemical compounds extracted from the Murchison meteorite were measured. The results obtained by studying the amino acids in this meteorite gave very unusual hydrogen and carbon isotope ratios. The technique was extended to the different classes of hydrocarbons and the hydrocarbons were isolated using a variety of separation techniques. The results and methods used in this investigation are described in this two page paper.

Critical points of DNA quantification by real-time PCR – effects of DNA extraction method and sample matrix on quantification of genetically modified organisms

PubMed Central

Cankar, Katarina; Štebih, Dejan; Dreo, Tanja; Žel, Jana; Gruden, Kristina

2006-01-01

Background Real-time PCR is the technique of choice for nucleic acid quantification. In the field of detection of genetically modified organisms (GMOs) quantification of biotech products may be required to fulfil legislative requirements. However, successful quantification depends crucially on the quality of the sample DNA analyzed. Methods for GMO detection are generally validated on certified reference materials that are in the form of powdered grain material, while detection in routine laboratories must be performed on a wide variety of sample matrixes. Due to food processing, the DNA in sample matrixes can be present in low amounts and also degraded. In addition, molecules of plant origin or from other sources that affect PCR amplification of samples will influence the reliability of the quantification. Further, the wide variety of sample matrixes presents a challenge for detection laboratories. The extraction method must ensure high yield and quality of the DNA obtained and must be carefully selected, since even components of DNA extraction solutions can influence PCR reactions. GMO quantification is based on a standard curve, therefore similarity of PCR efficiency for the sample and standard reference material is a prerequisite for exact quantification. Little information on the performance of real-time PCR on samples of different matrixes is available. Results Five commonly used DNA extraction techniques were compared and their suitability for quantitative analysis was assessed. The effect of sample matrix on nucleic acid quantification was assessed by comparing 4 maize and 4 soybean matrixes. In addition 205 maize and soybean samples from routine analysis were analyzed for PCR efficiency to assess variability of PCR performance within each sample matrix. Together with the amount of DNA needed for reliable quantification, PCR efficiency is the crucial parameter determining the reliability of quantitative results, therefore it was chosen as the primary criterion by which to evaluate the quality and performance on different matrixes and extraction techniques. The effect of PCR efficiency on the resulting GMO content is demonstrated. Conclusion The crucial influence of extraction technique and sample matrix properties on the results of GMO quantification is demonstrated. Appropriate extraction techniques for each matrix need to be determined to achieve accurate DNA quantification. Nevertheless, as it is shown that in the area of food and feed testing matrix with certain specificities is impossible to define strict quality controls need to be introduced to monitor PCR. The results of our study are also applicable to other fields of quantitative testing by real-time PCR. PMID:16907967

Acid extraction and purification of recombinant spider silk proteins.

PubMed

Mello, Charlene M; Soares, Jason W; Arcidiacono, Steven; Butler, Michelle M

2004-01-01

A procedure has been developed for the isolation of recombinant spider silk proteins based upon their unique stability and solubilization characteristics. Three recombinant silk proteins, (SpI)7, NcDS, and [(SpI)4/(SpII)1]4, were purified by extraction with organic acids followed by affinity or ion exchange chromatography resulting in 90-95% pure silk solutions. The protein yield of NcDS (15 mg/L culture) and (SpI)7 (35 mg/L) increased 4- and 5-fold, respectively, from previously reported values presumably due to a more complete solubilization of the expressed recombinant protein. [(SpI)4/(SpII)1]4, a hybrid protein based on the repeat sequences of spidroin I and spidroin II, had a yield of 12.4 mg/L. This method is an effective, reproducible technique that has broad applicability for a variety of silk proteins as well as other acid stable biopolymers.

Effect of acidity on the energy level of curcumin dye extracted from Curcuma longa L.

NASA Astrophysics Data System (ADS)

Agustia, Yuda Virgantara; Suyitno, Arifin, Zainal; Sutanto, Bayu

2016-03-01

The purpose of this research is to investigate the effect of acidity on the energy level of curcumin dye. The natural dye, curcumin, was synthesized from Curcuma longa L. using a simple extraction technique. The purification of curcumin dye was conducted in a column of chromatography and its characteristics were studied. Next, the purified curcumin dye was added by benzoic acids until various acidities of 3.0, 3.5, 4.0, 4.5, and 5.0. The absorbance spectra and the functionality groups found in the dyes were detected by ultraviolet-visible spectroscopy and Fourier-transform infrared spectroscopy, respectively. Meanwhile, the energy level of the dyes, EHOMO and ELUMO was measured by cyclic voltammetry. The best energy level of curcumin dye was achieved at pH 3.5 where Ered = -0.37V, ELUMO = -4.28 eV, Eox = 1.15V, EHOMO = -5.83 eV, and Eband gap = 1.55 eV. Therefore, the purified curcumin dye added by benzoic acid was promising for sensitizing the dye-sensitized solar cells.

A comparative mass spectrometric study of fatty acids and metals in some seed extracts.

PubMed

Suvar, Sonia Niculina; Bleiziffer, R; Podea, P; Iordache, A; Voica, C; Zgavarogea, R; Culea, M

A major cause of cardiovascular diseases and cancer is diet content, so the optimization of micronutrients in food is very important. Omega-3 fatty acids supplementation for patients had beneficial effects on subjective global assessment score and metabolic profiles. Fatty acids content and the metal ions in different seeds (e.g. linseed, poppy, grape, hemp, nuts, pumpkin, sesame, watermelon, chia) recommended as food supplements, purchased on the Romanian market, were compared. Gas chromatography coupled to mass spectrometry (GC-MS) was used as an excellent technique for fatty acids identification and quantitation, and inductively coupled plasma mass spectrometer (ICP-MS) for analytical measurements of metals.

The Effect of Salts on Electrospray Ionization of Amino Acids in the Negative Mode

NASA Technical Reports Server (NTRS)

Kim, H. I.; Johnson, P. V.; Beegle, L. W.; Kanik, I.

2004-01-01

The continued search for organics on Mars will require the development of simplified procedures for handling and processing of soil or rock core samples prior to analysis by onboard instrumentation. Extraction of certain organic molecules such as amino acids from rock and soil samples using a liquid solvent (H2O) has been shown to be more efficient (by approximately an order of magnitude) than heat extraction methods. As such, liquid extraction (using H2O) of amino acid molecules from rock cores or regolith material is a prime candidate for the required processing. In this scenario, electrospray ionization (ESI) of the liquid extract would be a natural choice for ionization of the analyte prior to interrogation by one of a variety of potential analytical separation techniques (mass spectroscopy, ion mobility spectroscopy, etc.). Aside from the obvious compatibility of ESI and liquid samples, ESI offers simplicity and a soft ionization capability. In order to demonstrate that liquid extraction and ESI can work as part of an in situ instrument on Mars, we must better understand and quantify the effect salts have on the ESI process. In the current work, we have endeavored to investigate the feasibility and limitations of negative mode ESI of Martian surface samples in the context of sample salt content using ion mobility spectroscopy (IMS).

The use of carrier RNA to enhance DNA extraction from microfluidic-based silica monoliths.

PubMed

Shaw, Kirsty J; Thain, Lauren; Docker, Peter T; Dyer, Charlotte E; Greenman, John; Greenway, Gillian M; Haswell, Stephen J

2009-10-12

DNA extraction was carried out on silica-based monoliths within a microfluidic device. Solid-phase DNA extraction methodology was applied in which the DNA binds to silica in the presence of a chaotropic salt, such as guanidine hydrochloride, and is eluted in a low ionic strength solution, such as water. The addition of poly-A carrier RNA to the chaotropic salt solution resulted in a marked increase in the effective amount of DNA that could be recovered (25ng) compared to the absence of RNA (5ng) using the silica-based monolith. These findings confirm that techniques utilising nucleic acid carrier molecules can enhance DNA extraction methodologies in microfluidic applications.

Complexation of furosemide with fulvic acid extracted from shilajit: a novel approach.

PubMed

Agarwal, Suraj Prakash; Anwer, Mohammad Khalid; Aqil, Mohammad

2008-05-01

The aim of the present work was to complex furosemide (FSM) with fulvic acid (FA) extracted from shilajit with the hope of having a better understanding of the complexation behavior. The effect of FA on the aqueous solubility, dissolution rate, and permeability of FSM was investigated. Different techniques, such as grinding, freeze drying, solvent evaporation, and so forth, were used for the preparation of the complex. The complexes were prepared in molar ratios of 1:1 and 1:2 FSM:FA and were evaluated for drug inclusion, solubility, differential scanning calorimetry, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, dissolution study, and permeation study. These methods confirm the formation of an amorphous inclusion complex of FSM with FA.

Low-Cost 3D Printers Enable High-Quality and Automated Sample Preparation and Molecular Detection

PubMed Central

Chan, Kamfai; Coen, Mauricio; Hardick, Justin; Gaydos, Charlotte A.; Wong, Kah-Yat; Smith, Clayton; Wilson, Scott A.; Vayugundla, Siva Praneeth; Wong, Season

2016-01-01

Most molecular diagnostic assays require upfront sample preparation steps to isolate the target’s nucleic acids, followed by its amplification and detection using various nucleic acid amplification techniques. Because molecular diagnostic methods are generally rather difficult to perform manually without highly trained users, automated and integrated systems are highly desirable but too costly for use at point-of-care or low-resource settings. Here, we showcase the development of a low-cost and rapid nucleic acid isolation and amplification platform by modifying entry-level 3D printers that cost between $400 and $750. Our modifications consisted of replacing the extruder with a tip-comb attachment that houses magnets to conduct magnetic particle-based nucleic acid extraction. We then programmed the 3D printer to conduct motions that can perform high-quality extraction protocols. Up to 12 samples can be processed simultaneously in under 13 minutes and the efficiency of nucleic acid isolation matches well against gold-standard spin-column-based extraction technology. Additionally, we used the 3D printer’s heated bed to supply heat to perform water bath-based polymerase chain reactions (PCRs). Using another attachment to hold PCR tubes, the 3D printer was programmed to automate the process of shuttling PCR tubes between water baths. By eliminating the temperature ramping needed in most commercial thermal cyclers, the run time of a 35-cycle PCR protocol was shortened by 33%. This article demonstrates that for applications in resource-limited settings, expensive nucleic acid extraction devices and thermal cyclers that are used in many central laboratories can be potentially replaced by a device modified from inexpensive entry-level 3D printers. PMID:27362424

Assessment of the antiproliferative and antigenotoxic activity and phytochemical screening of aqueous extracts of Sambucus australis Cham. & Schltdl. (ADOXACEAE).

PubMed

Tedesco, Marília; Kuhn, Andrielle W; Frescura, Viviane Dal-Souto; Boligon, Aline A; Athayde, Margareth L; Tedesco, Solange B; Silva, Antonio C F DA

2017-01-01

The purpose of this study was to evaluate the antiproliferative and antigenotoxic activity of Sambucus australis Cham. & Schltdl. aqueous extracts on the cell cycle of Allium cepa L. as well as determine the phenolic compounds in such extracts. S. australis inflorescences and leaves of two accessions were used for aqueous extract preparation at concentrations: 0.003 g/ml and 0.012 g/ml. A. cepa bulbs were rooted in distilled water and, subsequently, placed in treatments for 24 hours. Rootlets were collected and fixed in modified Carnoy's solution for 24 hours and kept. The squash technique was performed for slide preparation. Root tips were smashed and stained with 2% acetic orcein, and a total of 4000 cells per treatment were analyzed. The phenolic compounds were determined using high-performance liquid chromatography and data was analyzed using the Scott-Knott test. The results show that S. australis aqueous extracts have antiproliferative potential. Besides, the extracts prepared from S. australis leaves of both accessions at a concentration of 0.012 g/ml have shown antigenotoxic activity. The phytochemical analysis allowed us to determine the presence of flavonoids and phenolic acids, of which kaempferol and chrologenic acid were the most predominant compounds in the extracts from the inflorescences and leaves, respectively.

The effects of electrolysis on operational solutions in electromembrane extraction: The role of acceptor solution.

PubMed

Kubáň, Pavel; Boček, Petr

2015-06-12

Fundamental operational principle and instrumental set-up of electromembrane extraction (EME) suggest that electrolysis may play an important role in this recently developed micro-extraction technique. In the present study, the effect of electrolysis in EME is described comprehensively for the first time and it is demonstrated that electrolysis considerably influences EME performance. Micro-electromembrane extraction (μ-EME) across free liquid membrane formed by 1-pentanol was utilized for real-time monitoring of the electrolytically induced changes in composition of μ-EME solutions. These changes were visualized with a set of acid-base indicators. Changes in colours of their aqueous solutions revealed serious variations in their pH values, which occurred within seconds to minutes of the μ-EME process. Variations of up to eight pH units were observed for indicator solutions initially prepared in 1, 5 and 10mM hydrochloric acid. No or only negligible pH changes (less than 0.15 pH unit) were observed for indicator solutions prepared in 50 and 100mM acetic acid demonstrating that initial composition of the aqueous solutions was the crucial parameter. These results were also confirmed by theoretical calculations of maximum pH variations in the solutions, which were based on total electric charge transfers measured in the μ-EME systems, and by exact measurements of their pH values after μ-EMEs. Acceptor solutions that, in the current practice, consist predominantly of low concentrations of strong mineral acids or alkali hydroxides may thus not always ensure adequate EME performance, which was manifested by decrease in extraction recoveries of a basic drug papaverine. A suitable remedy to the observed effects is the application of acceptor solutions containing high concentrations of weak acids or bases. These solutions not only eliminate the decrease in recoveries but also serve well as matrices of extracted samples for subsequent analysis by capillary electrophoresis. Copyright © 2015 Elsevier B.V. All rights reserved.

Measuring bio-oil upgrade intermediates and corrosive species with polarity-matched analytical approaches

DOE PAGES

Connatser, Raynella M.; Lewis, Sr., Samuel Arthur; Keiser, James R.; ...

2014-10-03

Integrating biofuels with conventional petroleum products requires improvements in processing to increase blendability with existing fuels. This work demonstrates analysis techniques for more hydrophilic bio-oil liquids that give improved quantitative and qualitative description of the total acid content and organic acid profiles. To protect infrastructure from damage and reduce the cost associated with upgrading, accurate determination of acid content and representative chemical compound analysis are central imperatives to assessing both the corrosivity and the progress toward removing oxygen and acidity in processed biomass liquids. Established techniques form an ample basis for bio-liquids evaluation. However, early in the upgrading process, themore » unique physical phases and varied hydrophilicity of many pyrolysis liquids can render analytical methods originally designed for use in petroleum-derived oils inadequate. In this work, the water solubility of the organic acids present in bio-oils is exploited in a novel extraction and titration technique followed by analysis on the water-based capillary electrophoresis (CE) platform. The modification of ASTM D664, the standard for Total Acid Number (TAN), to include aqueous carrier solvents improves the utility of that approach for quantifying acid content in hydrophilic bio-oils. Termed AMTAN (modified Total Acid Number), this technique offers 1.2% relative standard deviation and dynamic range comparable to the conventional ASTM method. Furthermore, the results of corrosion product evaluations using several different sources of real bio-oil are discussed in the context of the unique AMTAN and CE analytical approaches developed to facilitate those measurements.« less

Formulation of a fish feed for goldfish with natural astaxanthin extracted from shrimp waste.

PubMed

Weeratunge, W K O V; Perera, B G K

2016-01-01

Astaxanthin is a xanthophyll carotenoid, which exhibits many important biological activities including a high degree of antioxidant capacity (AOC) and antibacterial activity, hence has a significant applicability in food, pharmaceutical and cosmetic industries. An attempt was made towards optimization of astaxanthin extraction conditions using three different extraction conditions and a solvent series, from uncooked, cooked and acid-treated shrimp waste, which is a readily available and cheap source of the pigment. The astaxanthin extracts were analyzed by comparing their UV-visible absorbance spectra and thin layer chromatograms with a standard astaxanthin sample. The percentage of astaxanthin in each crude sample was determined using the Beer-Lambert law. The Folin-Ciocalteu assay and the disk diffusion assay were used to investigate the antioxidant capacities and antibacterial activities of extracted astaxanthin samples respectively. The extracted astaxanthin was incorporated into fish feeds to test its ability to enhance the skin color of goldfish. The best astaxanthin percentage of 68 % was observed with the acetone:ethyl acetate (1:1) solvent system facilitated by maceration of cooked and acid treated shrimp, whereas the best crude yield of 33 % was found to be in the acetone extract of the acid-treated shrimp sample. The highest AOC of 65 µg pyrogallol equivalents/mg was observed for the EtOAc extract obtained by maceration of acid-treated shrimp waste. The highest AOC by sonication and soxhlet extraction methods were also obtained with the EtOAc solvent. The extracts exhibited antibacterial activity against four selected bacterial strains. The newly formulated astaxanthin enriched fish feed was economical and indicated a significant improvement of the skin color and healthiness of goldfish compared to the control feeds. Biologically active astaxanthin can be successfully extracted from shrimp waste in higher percentages. The extraction technique and the solvent used to extract astaxanthin from shrimp waste should be decided depending on the desired outcome and application of astaxanthin. Moreover, the novel astaxanthin enriched fish feed formulated during this study was found to effectively enhance the skin color of goldfish within 10 days, a much shorter feeding period compared to previously reported feeding periods in similar studies.Graphical abstractFormulation of a skin color enhancing fish feed for ornamental fish using crude astaxanthin extracted from shrimp waste.

The impact of wine components on fractionation of Cu and Fe in model wine systems: Macromolecules, phenolic and sulfur compounds.

PubMed

Kontoudakis, Nikolaos; Smith, Mark; Guo, Anque; Smith, Paul A; Scollary, Geoffrey R; Wilkes, Eric N; Clark, Andrew C

2017-08-01

A variety of techniques have been developed with the ability to measure different forms of metals in wine with the ultimate aim of providing a more accurate indicator of metal induced spoilage of wine. This study was conducted in order to identify which wine components influence the measurement of Cu and Fe in their fractionated and/or electrochemically active forms. The measurement techniques involved detection of labile Cu by stripping potentiometry and fractionation of Cu and Fe by sequential solid phase extraction, with detection by inductively coupled plasma-optical emission spectroscopy. The wine components assessed included those extracted from wine (red wine tannin, white wine protein, white wine polysaccharide, red wine polyphenol, white wine polyphenol), and commercially available monomeric compounds, including phenolic compounds and sulfur-containing compounds. For Cu, only hydrogen sulfide, which is known to induce the formation of Cu(I) sulfide, showed any appreciable influence on the fractionation and electrochemical detection of Cu. This form of Cu was also identified as the major component of red and white wines. For Fe, the fractionation was different for red versus white wine, and influenced significantly by extracted red wine polyphenol, (-)-epicatechin, gallic acid and tartaric acid. The wine components showed more influence on Fe at pH4.00 compared to pH3.25. These results enable a targeted use of these techniques in the assessment of metal-induced spoilage of wine. Copyright © 2016 Elsevier Ltd. All rights reserved.

EVALUATION AND APPLICATION OF SOX MEASUREMENT PROCEDURES FOR KRAFT RECOVERY FURNACES

EPA Science Inventory

The objective of this investigation was to determine the sulfuric acid (SO3/H2SO4) and sulfur dioxide (SO2) emissions from kraft recovery furnaces using an extractive sampling system. The Goksoyr and Ross controlled condensation technique was chosen. Equipment was designed and fa...

Facile silicification of plastic surface for bioassays

PubMed Central

Hong, Seonki; Park, Ki Soo; Weissleder, Ralph; Castro, Cesar M.; Lee, Hakho

2017-01-01

We herein report a biomimetic technique to modify plastic substrates for bioassays. The method first places a polydopamine adhesion layer to plastic surface, and then grows conformal silica coating. As proof of principle, we coated plastic microbeads to construct a disposable filter for point-of-care nucleic acid extraction. PMID:28134385

The simultaneous quantitation of ten amino acids in soil extracts by mass fragmentography

NASA Technical Reports Server (NTRS)

Pereira, W. E.; Hoyano, Y.; Reynolds, W. E.; Summons, R. E.; Duffield, A. M.

1972-01-01

A specific and sensitive method for the identification and simultaneous quantitation by mass fragmentography of ten of the amino acids present in soil was developed. The technique uses a computer driven quadrupole mass spectrometer and a commercial preparation of deuterated amino acids is used as internal standards for purposes of quantitation. The results obtained are comparable with those from an amino acid analyzer. In the quadrupole mass spectrometer-computer system up to 25 pre-selected ions may be monitored sequentially. This allows a maximum of 12 different amino acids (one specific ion in each of the undeuterated and deuterated amino acid spectra) to be quantitated. The method is relatively rapid (analysis time of approximately one hour) and is capable of the quantitation of nanogram quantities of amino acids.

Evaluate the role of organic acids in the protection of ligands from radiolytic degradation

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

Miller, Anneka; Mezyk, Stehpen; Peterman, Dean

In the Advanced TALSPEAK process, the bis(2-ethylhexyl)phosphoric acid (HDEHP) extractant used in the traditional TALSPEAK process is replaced by the extractant 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (HEH[EHP]). In addition, the aqueous phase complexant and buffer used in traditional TALSPEAK is replaced with the combination of N-(2-hydroxyethyl)ethylenediamine-N,N’,N’-triacetic acid (HEDTA) and citric acid. In order to evaluate the possible impacts of gamma radiolysis upon the efficacy of the Advanced TALSPEAK flowsheet, aqueous and organic phases corresponding to the extraction section of the proposed flowsheet were irradiated in the INL test loop under an ambient atmosphere. The results of these studies conducted at INL,more » led INL researchers to conclude that the scarcity of values of rate constants for the reaction of hydroxyl radical with the components of the Advanced TALSPEAK process chemistry was severely limiting the interpretation of the results of radiolysis studies performed at the INL. In this work, the rate of reaction of hydroxyl radical with citric acid at several pH values was measured using a competitive pulse radiolysis technique. This report describes those results and is written in completion of milestone M3FT-16IN030102028, the goal of which was to evaluate the role of organic acids in the protection of ligands from radiolytic degradation. The results reported here demonstrate the importance of obtaining hydroxyl radical reaction rate data for the conditions that closely resemble actual solution conditions expected to be used in an actual solvent extraction process. This report describes those results and is written in completion of milestone M3FT-16IN030102028, the goal of which was to evaluate the role of organic acids in the protection of ligands from radiolytic degradation.« less

Potential for utilization of algal biomass for components of the diet in CELSS

NASA Technical Reports Server (NTRS)

Kamarei, A. R.; Nakhost, Z.; Karel, M.

1985-01-01

Techniques which eliminate or reduce the undesirable cell components of algae and enhance the potential nutritional and organoleptic acceptability of algae products are studied. The cell walls, nucleic acids, and pigments and lipids of the green algae Scenedesmus obiliquus need to be removed. The procedures for determining the composition of proteins, pigments and lipids, and moisture and ash are described. Chemical, enzymatic, and physical methods of removing the cell wall to make the algae digestable are analyzed; a homogenization technique is utilized. The problems encountered if algae nucleic acids are ingested directly are discussed; the reduction of DNA and RNA by applying extracellular DNase and RNase to the nucleic acids is examined. The color and flavor of the algae are enhanced with the extraction of pigments and lipids from the algae protein concentration.

Porous extraction paddle: a solid phase extraction technique for studying the urine metabolome

PubMed Central

Shao, Gang; MacNeil, Michael; Yao, Yuanyuan; Giese, Roger W.

2016-01-01

RATIONALE A method was needed to accomplish solid phase extraction of a large urine volume in a convenient way where resources are limited, towards a goal of metabolome and xenobiotic exposome analysis at another, distant location. METHODS A porous extraction paddle (PEP) was set up, comprising a porous nylon bag containing extraction particles that is flattened and immobilized between two stainless steel meshes. Stirring the PEP after attachment to a shaft of a motor mounted on the lid of the jar containing the urine accomplishes extraction. The bag contained a mixture of nonpolar and partly nonpolar particles to extract a diversity of corresponding compounds. RESULTS Elution of a urine-exposed, water-washed PEP with aqueous methanol containing triethylammonium acetate (conditions intended to give a complete elution), followed by MALDI-TOF/TOF-MS, demonstrated that a diversity of compounds had been extracted ranging from uric acid to peptides. CONCLUSION The PEP allows the user to extract a large liquid sample in a jar simply by turning on a motor. The technique will be helpful in conducting metabolomics and xenobiotic exposome studies of urine, encouraging the extraction of large volumes to set up a convenient repository sample (e.g. 2 g of exposed adsorbent in a cryovial) for shipment and re-analysis in various ways in the future, including scaled-up isolation of unknown chemicals for identification. PMID:27624170

Porous extraction paddle: a solid phase extraction technique for studying the urine metabolome.

PubMed

Shao, Gang; MacNeil, Michael; Yao, Yuanyuan; Giese, Roger W

2016-09-14

A method was needed to accomplish solid phase extraction of a large urine volume in a convenient way where resources are limited, towards a goal of metabolome and xenobiotic exposome analysis at another, distant location. A porous extraction paddle (PEP) was set up, comprising a porous nylon bag containing extraction particles that is flattened and immobilized between two stainless steel meshes. Stirring the PEP after attachment to a shaft of a motor mounted on the lid of the jar containing the urine accomplishes extraction. The bag contained a mixture of nonpolar and partly nonpolar particles to extract a diversity of corresponding compounds. Elution of a urine-exposed, water-washed PEP with aqueous methanol containing triethylammonium acetate (conditions intended to give a complete elution), followed by MALDI-TOF/TOF-MS, demonstrated that a diversity of compounds had been extracted ranging from uric acid to peptides. The PEP allows the user to extract a large liquid sample in a jar simply by turning on a motor. The technique will be helpful in conducting metabolomics and xenobiotic exposome studies of urine, encouraging the extraction of large volumes to set up a convenient repository sample (e.g. 2 g of exposed adsorbent in a cryovial) for shipment and re-analysis in various ways in the future, including scaled-up isolation of unknown chemicals for identification. This article is protected by copyright. All rights reserved.

Production and Recovery of Pyruvic Acid: Recent Advances

NASA Astrophysics Data System (ADS)

Pal, Dharm; Keshav, Amit; Mazumdar, Bidyut; Kumar, Awanish; Uslu, Hasan

2017-12-01

Pyruvic acid is an important keto-carboxylic acid and can be manufactured by both chemical synthesis and biotechnological routes. In the present paper an overview of recent developments and challenges in various existing technique for the production and recovery of pyruvic acid from fermentation broth or from waste streams has been presented. The main obstacle in biotechnological production of pyruvic acid is development of suitable microorganism which can provide high yield and selectivity. On the other hand, technical limitation in recovery of pyruvic acid from fermentation broth is that, it could not be separated as other carboxylic acid in the form of salts by addition of alkali. Besides, pyruvic acid cannot be crystallized. Commercial separation by distillation is very expensive because pyruvic acid decomposes at higher temperature. It is also chemically reactive due to its peculiar molecular structure and has tendency to polymerize. Thus, at high concentration the various type of reaction leads to lower yield of the product, and hence, conventional methods are not favorable. Alternate separation technologies viable to both synthetic and biological routes are the current research areas. Latest techniques such as reactive extraction is new to the field of recovery of pyruvic acid. Recent development and future prospects in downstream processing of biochemically produced pyruvic acids has been discussed in this review article.

Green extraction of grape skin phenolics by using deep eutectic solvents.

PubMed

Cvjetko Bubalo, Marina; Ćurko, Natka; Tomašević, Marina; Kovačević Ganić, Karin; Radojčić Redovniković, Ivana

2016-06-01

Conventional extraction techniques for plant phenolics are usually associated with high organic solvent consumption and long extraction times. In order to establish an environmentally friendly extraction method for grape skin phenolics, deep eutectic solvents (DES) as a green alternative to conventional solvents coupled with highly efficient microwave-assisted and ultrasound-assisted extraction methods (MAE and UAE, respectively) have been considered. Initially, screening of five different DES for proposed extraction was performed and choline chloride-based DES containing oxalic acid as a hydrogen bond donor with 25% of water was selected as the most promising one, resulting in more effective extraction of grape skin phenolic compounds compared to conventional solvents. Additionally, in our study, UAE proved to be the best extraction method with extraction efficiency superior to both MAE and conventional extraction method. The knowledge acquired in this study will contribute to further DES implementation in extraction of biologically active compounds from various plant sources. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Study on chemical constituents from Schisandra chinensis stem].

PubMed

Zheng, Li-shi; Du, Shu-shan; Cai, Qian

2014-10-01

To separate and identify the chemical constituents from the stem of Schisandra chinensis. Various chromatographic techniques were used to separate and purify the chemical constituents from 95% ethanol extraction of the stem of Schisandra chinensis. Their structures were elucidated based on the physico-chemical properties and spectral data. Ten compounds were obtained and elucidated as (+)-deoxyschizandrin (1), γ-schizandrin (2), wuweizisu C (3), gomisin N (4), schizandrin (5), anwuweizic acid (6), (-)-dihydroguaiaretic acid (7), tetradecanoic acid (8), β-sitosterol (9) and daucosterol (10). Compounds 6-8 are obtained from the stem of Schisandra chinensis for the first time.

Development of Online Spectroscopic pH Monitoring for Nuclear Fuel Reprocessing Plants: Weak Acid Schemes.

PubMed

Casella, Amanda J; Ahlers, Laura R H; Campbell, Emily L; Levitskaia, Tatiana G; Peterson, James M; Smith, Frances N; Bryan, Samuel A

2015-05-19

In nuclear fuel reprocessing, separating trivalent minor actinides and lanthanide fission products is extremely challenging and often necessitates tight pH control in TALSPEAK (Trivalent Actinide-Lanthanide Separation by Phosphorus reagent Extraction from Aqueous Komplexes) separations. In TALSPEAK and similar advanced processes, aqueous pH is one of the most important factors governing the partitioning of lanthanides and actinides between an aqueous phase containing a polyaminopolycarboxylate complexing agent and a weak carboxylic acid buffer and an organic phase containing an acidic organophosphorus extractant. Real-time pH monitoring would significantly increase confidence in the separation performance. Our research is focused on developing a general method for online determination of the pH of aqueous solutions through chemometric analysis of Raman spectra. Spectroscopic process-monitoring capabilities, incorporated in a counter-current centrifugal contactor bank, provide a pathway for online, real-time measurement of solution pH. The spectroscopic techniques are process-friendly and can be easily configured for online applications, whereas classic potentiometric pH measurements require frequent calibration/maintenance and have poor long-term stability in aggressive chemical and radiation environments. Raman spectroscopy discriminates between the protonated and deprotonated forms of the carboxylic acid buffer, and the chemometric processing of the Raman spectral data with PLS (partial least-squares) regression provides a means to quantify their respective abundances and therefore determine the solution pH. Interpretive quantitative models have been developed and validated under a range of chemical composition and pH conditions using a lactic acid/lactate buffer system. The developed model was applied to new spectra obtained from online spectral measurements during a solvent extraction experiment using a counter-current centrifugal contactor bank. The model predicted the pH of this validation data set within 11% for pH > 2, thus demonstrating that this technique could provide the capability of monitoring pH online in applications such as nuclear fuel reprocessing.

Sustainable rehabilitation of mining waste and acid mine drainage using geochemistry, mine type, mineralogy, texture, ore extraction and climate knowledge.

PubMed

Anawar, Hossain Md

2015-08-01

The oxidative dissolution of sulfidic minerals releases the extremely acidic leachate, sulfate and potentially toxic elements e.g., As, Ag, Cd, Cr, Cu, Hg, Ni, Pb, Sb, Th, U, Zn, etc. from different mine tailings and waste dumps. For the sustainable rehabilitation and disposal of mining waste, the sources and mechanisms of contaminant generation, fate and transport of contaminants should be clearly understood. Therefore, this study has provided a critical review on (1) recent insights in mechanisms of oxidation of sulfidic minerals, (2) environmental contamination by mining waste, and (3) remediation and rehabilitation techniques, and (4) then developed the GEMTEC conceptual model/guide [(bio)-geochemistry-mine type-mineralogy- geological texture-ore extraction process-climatic knowledge)] to provide the new scientific approach and knowledge for remediation of mining wastes and acid mine drainage. This study has suggested the pre-mining geological, geochemical, mineralogical and microtextural characterization of different mineral deposits, and post-mining studies of ore extraction processes, physical, geochemical, mineralogical and microbial reactions, natural attenuation and effect of climate change for sustainable rehabilitation of mining waste. All components of this model should be considered for effective and integrated management of mining waste and acid mine drainage. Copyright © 2015 Elsevier Ltd. All rights reserved.

On-line monitoring of extraction process of Flos Lonicerae Japonicae using near infrared spectroscopy combined with synergy interval PLS and genetic algorithm

NASA Astrophysics Data System (ADS)

Yang, Yue; Wang, Lei; Wu, Yongjiang; Liu, Xuesong; Bi, Yuan; Xiao, Wei; Chen, Yong

2017-07-01

There is a growing need for the effective on-line process monitoring during the manufacture of traditional Chinese medicine to ensure quality consistency. In this study, the potential of near infrared (NIR) spectroscopy technique to monitor the extraction process of Flos Lonicerae Japonicae was investigated. A new algorithm of synergy interval PLS with genetic algorithm (Si-GA-PLS) was proposed for modeling. Four different PLS models, namely Full-PLS, Si-PLS, GA-PLS, and Si-GA-PLS, were established, and their performances in predicting two quality parameters (viz. total acid and soluble solid contents) were compared. In conclusion, Si-GA-PLS model got the best results due to the combination of superiority of Si-PLS and GA. For Si-GA-PLS, the determination coefficient (Rp2) and root-mean-square error for the prediction set (RMSEP) were 0.9561 and 147.6544 μg/ml for total acid, 0.9062 and 0.1078% for soluble solid contents, correspondingly. The overall results demonstrated that the NIR spectroscopy technique combined with Si-GA-PLS calibration is a reliable and non-destructive alternative method for on-line monitoring of the extraction process of TCM on the production scale.

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

PubMed

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

2015-01-01

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

Ultrasonic-assisted enzymatic extraction of phenolics from broccoli (Brassica oleracea L. var. italica) inflorescences and evaluation of antioxidant activity in vitro.

PubMed

Wu, Hao; Zhu, Junxiang; Yang, Long; Wang, Ran; Wang, Chengrong

2015-06-01

An efficient ultrasonic-assisted enzymatic extraction technique was applied to extracting phenolics from broccoli inflorescences without organic solvents. The synergistic model of enzymolysis and ultrasonication simultaneously was selected, and the enzyme combination was optimized by orthogonal test: cellulase 7.5 mg/g FW (fresh weight), pectinase 10 mg/g FW, and papain 1.0 mg/g FW. The operating parameters in ultrasonic-assisted enzymatic extraction were optimized with response surface methodology using Box-Behnken design. The optimal extraction conditions were as follows: ultrasonic power, 440 W; liquid to material ratio, 7.0:1 mL/g; pH value of 6.0 at 54.5 ℃ for 10 min. Under these conditions, the extraction yield of phenolics achieved 1.816 ± 0.0187 mg gallic acid equivalents/gram FW. The free radical scavenging activity of ultrasonic-assisted enzymatic extraction extracts was determined by 1,1-diphenyl-2-picrylhydrazyl·assay with EC50 values of 0.25, and total antioxidant activity was determined by ferric reducing antioxidant power assay with ferric reducing antioxidant power value of 0.998 mmol FeSO4/g compared with the referential ascorbic acid of 1.184 mmol FeSO4/g. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

Preparation of hybrid molecularly imprinted polymer with double-templates for rapid simultaneous purification of theophylline and chlorogenic acid in green tea.

PubMed

Tang, Weiyang; Li, Guizhen; Row, Kyung Ho; Zhu, Tao

2016-05-15

A novel double-templates technique was adopted for solid-phase extraction packing agent, and the obtained hybrid molecularly imprinted polymers with double-templates (theophylline and chlorogenic acid) were characterized by fourier transform infrared and field emission scanning electron microscope. The molecular recognition ability and binding capability for theophylline and chlorogenic acid of polymers was evaluated by static absorption and dynamic adsorption curves. A rapid and accurate approach was established for simultaneous purification of theophylline and chlorogenic acid in green tea by coupling hybrid molecularly imprinted solid-phase extraction with high performance liquid chromatography. With optimization of SPE procedure, a reliable analytical method was developed for highly recognition towards theophylline and chlorogenic acid in green tea with satisfactory extraction recoveries (theophylline: 96.7% and chlorogenic acid: 95.8%). The limit of detection and limit of quantity of the method were 0.01 μg/mL and 0.03 μg/mL for theophylline, 0.05 μg/mL and 0.17 μg/mL for chlorogenic acid, respectively. The recoveries of proposed method at three spiked levels analysis were 98.7-100.8% and 98.3-100.2%, respectively, with the relative standard deviation less than 1.9%. Hybrid molecularly imprinted polymers with double-templates showed good performance for two kinds of targets, and the proposed approach with high affinity of hybrid molecularly imprinted polymers might offer a novel method for the purification of complex samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Trace-fiber color discrimination by electrospray ionization mass spectrometry: a tool for the analysis of dyes extracted from submillimeter nylon fibers.

PubMed

Tuinman, Albert A; Lewis, Linda A; Lewis, Samuel A

2003-06-01

The application of electrospray ionization mass spectrometry (ESI-MS) to trace-fiber color analysis is explored using acidic dyes commonly employed to color nylon-based fibers, as well as extracts from dyed nylon fibers. Qualitative information about constituent dyes and quantitative information about the relative amounts of those dyes present on a single fiber become readily available using this technique. Sample requirements for establishing the color identity of different samples (i.e., comparative trace-fiber analysis) are shown to be submillimeter. Absolute verification of dye mixture identity (beyond the comparison of molecular weights derived from ESI-MS) can be obtained by expanding the technique to include tandem mass spectrometry (ESI-MS/MS). For dyes of unknown origin, the ESI-MS/MS analyses may offer insights into the chemical structure of the compound-information not available from chromatographic techniques alone. This research demonstrates that ESI-MS is viable as a sensitive technique for distinguishing dye constituents extracted from a minute amount of trace-fiber evidence. A protocol is suggested to establish/refute the proposition that two fibers--one of which is available in minute quantity only--are of the same origin.

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

Aortic relaxant activity of Crataegus gracilior Phipps and identification of some of its chemical constituents.

PubMed

Hernández-Pérez, Abigail; Bah, Moustapha; Ibarra-Alvarado, César; Rivero-Cruz, José Fausto; Rojas-Molina, Alejandra; Rojas-Molina, Juana Isela; Cabrera-Luna, José Alejandro

2014-12-15

This study focused on the assessment of the vasorelaxant activity of the organic and aqueous extracts obtained from leaves and fruits of a Mexican hawthorn (Crataegus gracilior) on isolated rat aorta, and on the purification and identification of some of their secondary metabolites by the use of chromatographic and spectroscopic techniques. The results obtained showed that the methanol extract has a significantly more potent and effective vasorelaxant effect than the other tested extracts, with an EC50 = 8.69 ± 4.34 µg/mL and an Emax = 94.6% ± 11.30%, values that are close to that of acetylcholine, the positive control. From the same extract, two major triterpenes were isolated and identified as ursolic and corosolic acids by comparison of their experimental NMR spectroscopic data with those reported in the literature. Chlorogenic acid, rutin, quercetin, kaempferol and (+)-catechin were also identified using HPLC coupled with PDAD. All these compounds have already been proven to possess on their own antihypertensive effect and other benefits on cardiovascular diseases and they can support, at least in part, the traditional use of this plant species.

Rat immunoreactive cholecystokinin (CCK): characterization using two chromatographic techniques.

PubMed

Bacarese-Hamilton, A J; Adrian, T E; Chohan, P; Bloom, S R

1985-06-01

Acid and neutral extracts of rat cerebral cortex and upper small intestine were prepared and the endogenous concentrations of cholecystokinin-like immunoreactivity (CCK-LI) measured by three new CCK-specific radioimmunoassays. The characterization of the immunoreactive CCK molecular forms was undertaken using gel permeation chromatography in the presence of 6 M urea to minimise problems relating to peptide adsorption or aggregation. Reverse-phase high-performance liquid chromatography (HPLC) was also performed on the rat tissue extracts. Rat cortex contained 268 +/- 12 pmol/g CCK-LI, and over 90% resembled the sulphated CCK-8, which was preferentially extracted at neutral pH. In contrast, the rat upper small intestine (97 +/- 8 pmol/g of CCK-LI) contained less than 20% CCK-8, the majority of immunoreactive CCK being of larger molecular size and being preferentially extracted at acid pH. In the small intestine the predominant molecular form(s) was intermediate in size between CCK-33 and CCK-8. Large amounts of CCK-33 and of a molecular form larger than CCK-33 were also detected. It is concluded that post-translational cleavage of CCK differs in rat brain and gut.

Free radical-scavenging activities of Crataegus monogyna extracts.

PubMed

Bernatoniene, Jurga; Masteikova, Rūta; Majiene, Daiva; Savickas, Arūnas; Kevelaitis, Egidijus; Bernatoniene, Rūta; Dvorácková, Katerina; Civinskiene, Genuvaite; Lekas, Raimundas; Vitkevicius, Konradas; Peciūra, Rimantas

2008-01-01

The aim of this study was to investigate antiradical activity of aqueous and ethanolic hawthorn fruit extracts, their flavonoids, and flavonoid combinations. Total amount of phenolic compounds and the constituents of flavonoids were determined using a high-performance liquid chromatography. The antioxidant activity of Crataegus monogyna extracts and flavonoids (chlorogenic acid, hyperoside, rutin, quercetin, vitexin-2O-rhamnoside, epicatechin, catechin, and procyanidin B(2)) quantitatively was determined using the method of spectrophotometry (diphenyl-1-picrylhydrazyl (DPPH.) radical scavenging assay and 2,2'-azino-bis (3-ethylbenzthiazoline-6-sulphonic acid)(ABTS.+) radical cation decolorization assay). The level of tyrosine nitration inhibition was determined using a high-performance liquid chromatography. Ethanolic hawthorn fruit extract contained 182+/-4 mg/100 mL phenolic compounds, i.e. threefold more, as compared to aqueous extract. The antioxidant activity according to DPPH. reduction in the ethanolic extracts was higher 2.3 times (P<0.05). The ABTS.+ technique showed that the effect of ethanolic extracts was by 2.5 times stronger than that of aqueous extracts. Tyrosine nitration inhibition test showed that the effect of ethanolic extracts was by 1.4 times stronger than that of aqueous extracts. The investigation of the antiradical activity of the active constituents in aqueous and ethanolic extracts revealed that epicatechin and catechin contribute to radical-scavenging properties more than other components. Procyanidin B(2) only insignificantly influenced the antiradical activity of the extracts. Both aqueous and ethanolic hawthorn extracts had antiradical activity, but ethanolic extract had stronger free radical-scavenging properties, compared to the aqueous extract. The antioxidant activity of the studied preparations was mostly conditioned by epicatechin and catechin. The individual constituents of both extracts had weaker free radical-scavenging properties than the combination of these substances did.

Three new ursane-type triterpenoids from the stems of Saprosma merrillii.

PubMed

Zhang, Dashuai; Chen, Wenhao; Chen, Wenxing; Song, Xiaoping; Han, Changri; Wang, Yan; Chen, Guangying

2013-11-25

Three new ursane-type triterpenoids, 3α,6α,30-trihydroxy-ursan-28-oic acid (1), 3α,30-dihydroxy-6-oxo-ursan-28-oic acid (2) and 3α,6α,7α,30-tetrahydroxy-ursan-28-oic acid (3), together with one known triterpenoid, betulinic acid (4), one known anthraquinone, 1,7-dihydroxy-2-methylanthraquinone (5), four known phenols, 1,3,5-trimethoxybenzene (6), p-hydroxybenzoic acid (7), syringic acid (8), isovanillin (9), two steroids, sitosterol (10) and daucosterol (11), were isolated from the ethanol extract of the stems of S. merrillii. Their structures were elucidated on the basis of physical and spectral techniques, besides comparison with literature data. Compounds 1-3 showed inhibitory activities against the A549, HEPG2, and B16F10 cell lines.

Optimization of ultrasonic circulating extraction of samara oil from Acer saccharum using combination of Plackett-Burman design and Box-Behnken design.

PubMed

Chen, Fengli; Zhang, Qiang; Fei, Shimin; Gu, Huiyan; Yang, Lei

2017-03-01

In this study, ultrasonic circulating extraction (UCE) technique was firstly and successfully applied for extraction of samara oil from Acer saccharum. The extraction kinetics were fitted and described, and the extraction mechanism was discussed. Through comparison, n-hexane was selected as the extraction solvent, the influence of solvent type on the responses was detailedly interpreted based on the influence of their properties on the occurrence and intensity of cavitation. Seven parameters potentially influencing the extraction yield of samara oil and content of nervonic acid, including ultrasound irradiation time, ultrasound irradiation power, ultrasound temperature, liquid-solid ratio, soaking time, particle size and stirring rate, were screened through Plackett-Burman design to determine the significant variables. Then, three parameters performed statistically significant, including liquid-solid ratio, ultrasound irradiation time and ultrasound irradiation power, were further optimized using Box-Behnken design to predict optimum extraction conditions. Satisfactory yield of samara oil (11.72±0.38%) and content of nervonic acid (5.28±0.18%) were achieved using the optimal conditions. 1% proportion of ethanol in extraction solvent, 120°C of drying temperature and 6.4% moisture were selected and applied for effective extraction. There were no distinct differences in the physicochemical properties of samara oil obtained by UCE and Soxhlet extraction, and the samara oil obtained by UCE exhibited better antioxidant activities. Therefore, UCE method has enormous potential for efficient extraction of edible oil with high quality from plant materials. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of conventional and ultrasonic-assisted extraction on phenolic contents, betacyanin contents, and antioxidant capacity of red dragon fruit (Hylocereus polyrhizus).

PubMed

Ramli, Nurul Shazini; Ismail, Patimah; Rahmat, Asmah

2014-01-01

The aim of this study was to examine the effects of extraction methods on antioxidant capacities of red dragon fruit peel and flesh. Antioxidant capacities were measured using ethylenebenzothiozoline-6-sulfonic acid (ABTS) radical cation assay and ferric reducing antioxidant power assay (FRAP). Total phenolic content (TPC) was determined using Folin-Ciocalteu reagent while quantitative determination of total flavonoid content (TFC) was conducted using aluminium trichloride colorimetric method. Betacyanin content (BC) was measured by spectrophotometer. Red dragon fruit was extracted using conventional (CV) and ultrasonic-assisted extraction (UE) technique to determine the most efficient way of extracting its antioxidant components. Results indicated that UE increased TFC, reduced the extraction yield, BC, and TPC, but exhibited the strongest scavenging activity for the peel of red dragon fruit. In contrast, UE reduced BC, TFC, and scavenging activity but increased the yield for the flesh. Nonetheless, UE slightly increases TPC in flesh. Scavenging activity and reducing power were highly correlated with phenolic and flavonoid compounds. Conversely, the scavenging activity and reducing power were weakly correlated with betacyanin content. This work gives scientific evidences for the consideration of the type of extraction techniques for the peel and flesh of red dragon fruit in applied research and food industry.

Influence of Conventional and Ultrasonic-Assisted Extraction on Phenolic Contents, Betacyanin Contents, and Antioxidant Capacity of Red Dragon Fruit (Hylocereus polyrhizus)

PubMed Central

Ramli, Nurul Shazini; Ismail, Patimah; Rahmat, Asmah

2014-01-01

The aim of this study was to examine the effects of extraction methods on antioxidant capacities of red dragon fruit peel and flesh. Antioxidant capacities were measured using ethylenebenzothiozoline-6-sulfonic acid (ABTS) radical cation assay and ferric reducing antioxidant power assay (FRAP). Total phenolic content (TPC) was determined using Folin-Ciocalteu reagent while quantitative determination of total flavonoid content (TFC) was conducted using aluminium trichloride colorimetric method. Betacyanin content (BC) was measured by spectrophotometer. Red dragon fruit was extracted using conventional (CV) and ultrasonic-assisted extraction (UE) technique to determine the most efficient way of extracting its antioxidant components. Results indicated that UE increased TFC, reduced the extraction yield, BC, and TPC, but exhibited the strongest scavenging activity for the peel of red dragon fruit. In contrast, UE reduced BC, TFC, and scavenging activity but increased the yield for the flesh. Nonetheless, UE slightly increases TPC in flesh. Scavenging activity and reducing power were highly correlated with phenolic and flavonoid compounds. Conversely, the scavenging activity and reducing power were weakly correlated with betacyanin content. This work gives scientific evidences for the consideration of the type of extraction techniques for the peel and flesh of red dragon fruit in applied research and food industry. PMID:25379555

Phytochemical screening, antiglycation and antioxidant activities of whole plant of Boerhavia repens L. from Cholistan, Pakistan.

PubMed

Nazneen, Fariha; Sheikh, Munir A; Jameel, Amir; Rahman, Ziaur

2016-05-01

Present study was aimed to explore a traditionally used indigenous medicinal plant Boerhavia repens (Nyctaginaceae family) of the Cholistan desert, Pakistan. Crude aqueous and methanolic extracts of the whole plant were investigated in vitro for preliminary phytochemical screening, antioxidant and antiglycation activities. Antioxidant activities were determined by total phenolic contents, 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging and inhibition of lipid peroxidation. For antiglycation activities browning production was noted and thiobarbituric acid (TBA) technique was used to determine glycation level. Boerhavia repens expressed considerable amounts of phytochemicals. Extract yield was found to be 4.59%-7.85% g/100g of dry matter with total phenolics ranging from 47.9- 190.77mg/GAE per g for aqueous and methanol extract respectively. Strong inhibitory effect was exhibited by methanolic extract in linoleic acid per oxidation system (86.11%, EC50=0.99mg/mL) and DPPH assay (88.65%, EC50=212.33μg/ml). In term of browning maximum inhibition (81.50%) was exhibited by methanolic extract at 37°C at third week of incubation. Both extracts expressed significant (P>0.05) and comparable inhibition of glycation level. In conclusion, Boerhavia repens showed promising antioxidant and antiglycation activities validating its therapeutic potential.

Facile synthesis of size-tunable gold nanoparticles by pomegranate (Punica granatum) leaf extract: Applications in arsenate sensing

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

Rao, Ashit; Mahajan, Ketakee; Bankar, Ashok

Highlights: ► Pomegranate leaf extracts mediated rapid gold nanoparticle (AuNP) synthesis. ► The phyto-inspired AuNPs were size-tuned and characterized. ► The reducing and capping agents in the extract were identified. ► The nanoparticles reacted specifically with arsenate (V) ions. - Abstract: When pomegranate leaf extracts were incubated with chloroauric acid (HAuCl{sub 4}), gold nanoparticles (AuNPs) were synthesized. These were characterized by a variety of techniques. With an increasing content of the leaf extract, a gradual decrease in size and an increase in monodispersity were observed. Transmission electron microscope (TEM) images showed that the phyto-fabricated AuNPs were surrounded by an amorphousmore » layer. Gallic acid in the extract mediated the reduction and a natural decapeptide capped the nanostructures. Blocking of thiol groups in the decapeptide cysteine residues caused the nanoparticles to aggregate. On interaction with arsenate (V) ions, the UV–vis spectra of the nanoparticles showed a decrease in intensity and a red-shift. Energy dispersive spectra confirmed the presence of arsenate associated with the AuNPs. Thus, by using these AuNPs, a method for sensing the toxic arsenate ions could be developed.« less

Characteristics of Gouda Cheese Supplemented with Chili Pepper Extract Microcapsules

PubMed Central

Nam, Myoung Soo; Bae, Hyoung Churl

2017-01-01

In this study, the physicochemical and sensory properties of Gouda cheese supplemented with microcapsules of chili pepper extract were evaluated. Microcapsules of pepper extract were prepared by coacervation technique using gum acacia-gelatin wall and chili pepper oil core. Changes in pH, lactic acid bacteria (LAB) population, and free amino acid (FAA) content after supplementation of Gouda cheese with chili pepper capsules were monitored during ripening. Texture and sensory characteristics of the Gouda cheese ripened for 6 months were evaluated. The supplementation of pepper extract microcapsules (0.5% or 1%, w/w) did not influence the pH values and LAB content of the Gouda cheese (p<0.05) during the ripening period. While the content of total FAA increased with the ripening process in all the cheese groups (p<0.05), no significant difference (p<0.05) in the content of total FAA was observed among the sample groups at each time point. The addition of pepper extract microcapsules (1%, w/w) to Gouda cheese significantly decreased hardness (p<0.05) and negatively affected sensory attributes in terms of taste and texture (p<0.05). The results demonstrated that supplementation with 0.5% pepper extract microcapsules could provide additional bioactive ingredients, along with maintenance of the quality of Gouda cheese. PMID:29725204

Beef, chicken and lamb fatty acid analysis--a simplified direct bimethylation procedure using freeze-dried material.

PubMed

Lee, M R F; Tweed, J K S; Kim, E J; Scollan, N D

2012-12-01

When fractionation of meat lipids is not required, procedures such as saponification can be used to extract total fatty acids, reducing reliance on toxic organic compounds. However, saponification of muscle fatty acids is laborious, and requires extended heating times, and a second methylation step to convert the extracted fatty acids to fatty acid methyl esters prior to gas chromatography. Therefore the development of a more rapid direct methylation procedure would be of merit. The use of freeze-dried material for analysis is common and allows for greater homogenisation of the sample. The present study investigated the potential of using freeze-dried muscle samples and a direct bimethylation to analyse total fatty acids of meat (beef, chicken and lamb) in comparison with a saponification procedure followed by bimethylation. Both methods compared favourably for all major fatty acids measured. There was a minor difference in relation to the C18:1 trans 10 isomer with a greater (P<0.05) recovery with saponification. However, numerically the difference was small and likely as a result of approaching the limits of isomer identification by single column gas chromatography. Differences (P<0.001) between species were found for all fatty acids measured with no interaction effects. The described technique offers a simplified, quick and reliable alternative to saponification to analyse total fatty acids from muscle samples. Copyright © 2012 Elsevier Ltd. All rights reserved.

Quantitative analysis of myocardial kinetics of 15-p-[iodine-125] iodophenylpentadecanoic acid.

PubMed

DeGrado, T R; Holden, J E; Ng, C K; Raffel, D M; Gatley, S J

1989-07-01

Myocardial extraction and the characteristic tissue clearance of radioactivity following bolus injections of a radioiodinated (125I) long chain fatty acid (LCFA) analog 15-p-iodophenylpentadecanoic acid (IPPA) were examined in the isolated perfused working rat heart. Radioactivity remaining in the heart was monitored with external scintillation probes. A compartmental model which included nonesterified tracer, catabolite, and complex lipid compartments successfully fitted tissue time-radioactivity residue curves, and gave a value for the rate of IPPA oxidation 1.8 times that obtained from steady-state release of tritiated water from labeled palmitic acid. The technique was sensitive to the impairment of LCFA oxidation in hearts of animals treated with the carnitine palmitoyltransferase I inhibitor, 2[5(4-chlorophenyl)pentyl]oxirane-2-carboxylate (POCA). IPPA or similar modified fatty acids may be better than 11C-labeled physiological fatty acids such as palmitate in this type of study, because efflux of unoxidized tracer and catabolite(s) from the heart are kinetically more distinct, and their contributions to the early data can be reliably separated. This technique may be suitable for extension to in vivo measurements with position tomography and appropriate modified fatty acids.

Non-methylene-interrupted fatty acids with Δ5 unsaturation in Sargassum species.

PubMed

Kim, Gwang-Woo; Itabashi, Yutaka

2012-01-01

Detailed fatty acid compositions of five species of the brown algae Sargassum (S. fulvellum, S. horneri, S. boreale, S. thunbergii, and S. yezoense) were determined using silver ion solid phase extraction, gas chromatography (GC), and GC-mass spectrometry (GC-MS) techniques. In addition to a high number of typical saturated and unsaturated fatty acids, the GC-MS spectra of the 4,4-dimethyloxazoline derivatives of fatty acids revealed the occurrence of small amounts of unusual non-methylene-interrupted (NMI) fatty acids with Δ5 unsaturation, namely, 5,9-eicosadienoic (5,9-20:2), 5,11,14-eicosatrienoic (5,11,14-20:3), and 5,11,14,17-eicosatetraenoic (5,11,14,17-20:4) acids. Of these three NMI acids, the 5,9-20:2 acid was found to be the most abundant (0.4%-2.3% of the total fatty acids) and was detected for the first time in algae.

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.

Phenolic compound profiles and antioxidant capacity of Persea americana Mill. peels and seeds of two varieties.

PubMed

Kosińska, Agnieszka; Karamać, Magdalena; Estrella, Isabel; Hernández, Teresa; Bartolomé, Begoña; Dykes, Gary A

2012-05-09

Avocado processing by the food and cosmetic industries yields a considerable amount of phenolic-rich byproduct such as peels and seeds. Utilization of these byproducts would be favorable from an economic point of view. Methanolic (80%) extracts obtained from lyophilized ground peels and seeds of avocado (Persea americana Mill.) of the Hass and Shepard varieties were characterized for their phenolic compound profiles using the HPLC-PAD technique. The structures of the identified compounds were subsequently unambiguously confirmed by ESI-MS. Compositional analysis revealed that the extracts contained four polyphenolic classes: flavanol monomers, proanthocyanidins, hydroxycinnamic acids, and flavonol glycosides. The presence of 3-O-caffeoylquinic acid, 3-O-p-coumaroylquinic acid, and procyanidin A trimers was identified in seeds of both varieties. Intervarietal differences were apparent in the phenolic compound profiles of peels. Peels of the Shepard variety were devoid of (+)-catechin and procyanidin dimers, which were present in the peels of the Hass variety. Peels of both varieties contained 5-O-caffeoylquinic acid and quercetin derivatives. The differences in the phenolic profiles between varietals were also apparent in the different antioxidant activity of the extracts. The peel extracts had a higher total phenolic compound content and antioxidant activity when compared to the seed extracts. The highest TEAC and ORAC values were apparent in peels of the Haas variety in which they amounted to 0.16 and 0.47 mmol Trolox/g DW, respectively. No significant (p > 0.05) differences were apparent between the TEAC values of seeds of the two varieties but the ORAC values differed significantly (p < 0.05). Overall these findings indicate that both the seeds and peel of avocado can be utilized as a functional food ingredient or as an antioxidant additive.

Characterization of pH-fractionated humic acids derived from Chinese weathered coal.

PubMed

Zhang, Shuiqin; Yuan, Liang; Li, Wei; Lin, Zhian; Li, Yanting; Hu, Shuwen; Zhao, Bingqiang

2017-01-01

To reduce the compositional and structural heterogeneity of humic acids (HAs) and achieve better use of HA resources, in this study, we report a new sequential dissolution method for HAs derived from Chinese weathered coal. This method was used to separate HAs into seven fractions by adjusting the pH (3-10) of the extraction solution. The results showed that the HA fractions derived from Chinese weathered coal were concentrated up to 90.31% in the lower pH solutions (3-7). The compositional and structural characteristics of the HA fractions were determined by elemental analysis; ultraviolet-visible (UV-Vis), Fourier transform infrared (FTIR), and solid-state 13 C-nuclear magnetic resonance (NMR) spectroscopies; and other techniques. The results showed significant differences among the HA fractions. The concentrations of the total acidic groups and the carboxyl groups decreased with the increasing pH of the extraction solution. However, the HA fractions derived from extraction solutions with pH 3-4 had relatively lower aromaticity but a higher protonated carbon content. The HA fractions derived from extraction solutions with pH 6-7 had the highest aromaticity and the greatest abundance of COO/N-C=O. This study demonstrated that adjusting the pH of the extraction solution is one way to fractionate HAs from Chinese weathered coal and to obtain HA fractions with compositions and structures that could serve as useful material for study and utilization. Copyright © 2016 Elsevier Ltd. All rights reserved.

RP-HPTLC densitometric determination and validation of vanillin and related phenolic compounds in accelerated solvent extract of Vanilla planifolia*.

PubMed

Sharma, Upendra Kumar; Sharma, Nandini; Gupta, Ajai Prakash; Kumar, Vinod; Sinha, Arun Kumar

2007-12-01

A simple, fast and sensitive RP-HPTLC method is developed for simultaneous quantitative determination of vanillin and related phenolic compounds in ethanolic extracts of Vanilla planifolia pods. In addition to this, the applicability of accelerated solvent extraction (ASE) as an alternative to microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and Soxhlet extraction was also explored for the rapid extraction of phenolic compounds in vanilla pods. Good separation was achieved on aluminium plates precoated with silica gel RP-18 F(254S) in the mobile phase of methanol/water/isopropanol/acetic acid (30:65:2:3, by volume). The method showed good linearity, high precision and good recovery of compounds of interest. ASE showed good extraction efficiency in less time as compared to other techniques for all the phenolic compounds. The present method would be useful for analytical research and for routine analysis of vanilla extracts for their quality control.

Gas chromatographic and mass spectrometric investigations of organic residues from Roman glass unguentaria.

PubMed

Ribechini, Erika; Modugno, Francesca; Colombini, Maria Perla; Evershed, Richard P

2008-03-07

A combination of gas chromatographic (GC) and mass spectrometric (MS) techniques, including direct exposure-MS (DE-MS), high-temperature GC-MS (HTGC-MS) and GC-MS of neutral and acid fractions, was employed to study the composition and recognise origin of the organic materials used to manufacture balm residues surviving in a series of glass unguentaria recovered from excavations of a Roman villa (Villa B) in the ancient town of Oplontis (Naples, Italy). DE-MS provided comprehensive 'fingerprint' information on the solvent soluble components of the contents of the unguentaria, while GC-MS analyses provided detailed molecular compositions, highlighting the presence of a wide range of compound classes including mid- and long-chain fatty acids, long-chain hydroxy-acids, n-alkanols, alkandiols, n-alkanes, long-chain monoesters, phytosterols and diterpenoid acids. Characteristic biomarkers and their distributions indicate the presence of beeswax, Pinaceae resin and another wax, as the main organic constituents of all of the preparations examined. In particular, the occurrence of phytosterols and long-chain monoesters, in which the acyl moiety was not exclusively palmitic acid, suggested the presence of a second waxy-lipid constituent of plant origin. The results are consistent with beeswax being used in the preparation of the cosmetics preserved in the unguentaria, while the other lipids are most likely the residue of some as yet unidentified plant extract(s), possibly deriving from the cuticular waxes of flowers and/or leaves. The composition of the extracts are consistent with the ancient practices of maceration and/or "enfleurage", in which lipid-based materials, such as beeswax, animal fat or vegetables oils, were used to extract aromatic and fragrant substances from resin, flowers, spices and scented wood, in order to produce unguents and balms.

Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples.

PubMed

Fukushima, Romualdo S; Hatfield, Ronald D

2004-06-16

Present analytical methods to quantify lignin in herbaceous plants are not totally satisfactory. A spectrophotometric method, acetyl bromide soluble lignin (ABSL), has been employed to determine lignin concentration in a range of plant materials. In this work, lignin extracted with acidic dioxane was used to develop standard curves and to calculate the derived linear regression equation (slope equals absorptivity value or extinction coefficient) for determining the lignin concentration of respective cell wall samples. This procedure yielded lignin values that were different from those obtained with Klason lignin, acid detergent acid insoluble lignin, or permanganate lignin procedures. Correlations with in vitro dry matter or cell wall digestibility of samples were highest with data from the spectrophotometric technique. The ABSL method employing as standard lignin extracted with acidic dioxane has the potential to be employed as an analytical method to determine lignin concentration in a range of forage materials. It may be useful in developing a quick and easy method to predict in vitro digestibility on the basis of the total lignin content of a sample.

Rapid detection of microbial DNA by a novel isothermal genome exponential amplification reaction (GEAR) assay.

PubMed

Prithiviraj, Jothikumar; Hill, Vincent; Jothikumar, Narayanan

2012-04-20

In this study we report the development of a simple target-specific isothermal nucleic acid amplification technique, termed genome exponential amplification reaction (GEAR). Escherichia coli was selected as the microbial target to demonstrate the GEAR technique as a proof of concept. The GEAR technique uses a set of four primers; in the present study these primers targeted 5 regions on the 16S rRNA gene of E. coli. The outer forward and reverse Tab primer sequences are complementary to each other at their 5' end, whereas their 3' end sequences are complementary to their respective target nucleic acid sequences. The GEAR assay was performed at a constant temperature 60 °C and monitored continuously in a real-time PCR instrument in the presence of an intercalating dye (SYTO 9). The GEAR assay enabled amplification of as few as one colony forming units of E. coli per reaction within 30 min. We also evaluated the GEAR assay for rapid identification of bacterial colonies cultured on agar media directly in the reaction without DNA extraction. Cells from E. coli colonies were picked and added directly to GEAR assay mastermix without prior DNA extraction. DNA in the cells could be amplified, yielding positive results within 15 min. Published by Elsevier Inc.

Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

PubMed

Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

2016-04-01

Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

Pyrogenic transformation of Nannochloropsis oceanica into fatty acid methyl esters without oil extraction for estimating total lipid content.

PubMed

Kim, Jieun; Jung, Jong-Min; Lee, Jechan; Kim, Ki-Hyun; Choi, Tae O; Kim, Jae-Kon; Jeon, Young Jae; Kwon, Eilhann E

2016-07-01

This study fundamentally investigated the pseudo-catalytic transesterification of dried Nannochloropsis oceanica into fatty acid methyl esters (FAMEs) without oil extraction, which was achieved in less than 5min via a thermo-chemical pathway. This study presented that the pseudo-catalytic transesterification reaction was achieved in the presence of silica and that its main driving force was identified as temperature: pores in silica provided the numerous reaction space like a micro-reactor, where the heterogeneous reaction was developed. The introduced FAME derivatization showed an extraordinarily high tolerance of impurities (i.e., pyrolytic products and various extractives). This study also explored the thermal cracking of FAMEs derived from N. oceanica: the thermal cracking of saturated FAMEs was invulnerable at temperatures lower than 400°C. Lastly, this study reported that N. oceanica contained 14.4wt.% of dried N. oceanica and that the introduced methylation technique could be applicable to many research fields sharing the transesterification platform. Copyright © 2016 Elsevier Ltd. All rights reserved.

UFLC/MS-IT-TOF guided isolation of anti-HBV active chlorogenic acid analogues from Artemisia capillaris as a traditional Chinese herb for the treatment of hepatitis.

PubMed

Zhao, Yong; Geng, Chang-An; Ma, Yun-Bao; Huang, Xiao-Yan; Chen, Hao; Cao, Tuan-Wu; He, Kang; Wang, Hao; Zhang, Xue-Mei; Chen, Ji-Jun

2014-10-28

Hepatitis B induced by HBV is a serious health problem. Artemisia capillaris (Yin-Chen) has long been used to treat hepatitis in traditional Chinese medicine. Coumarins, flavonoids and organic acids were revealed as its hepatoprotective and choleretic components, but its anti-HBV active components remain unknown. This current study focused on its anti-HBV active constituents by various chromatographic methods. LC/MS and bioassay-guided fractionation on the active extract of Artemisia capillaris led to the isolation of nine chlorogenic acid analogues. Structures of the isolates were elucidated by MS/MS and NMR techniques. Anti-HBV assay was performed on HepG 2.2.15 cell line in vitro: reduction of HBsAg and HBeAg secretions was measured by an ELISA method; inhibition of HBV DNA replication was monitored by real-time quantitative PCR and cellular toxicity was assessed by a MTT method. The 90% ethanol extract of Artemisia capillaris (Fr. AC) showed significantly inhibitory activity on HBV DNA replication with an IC₅₀ value of 76.1 ± 3.9 μg/mL and low cytotoxic effects (SI>20.1). To clarify its active constituents, the extract was further separated into 3 sub-fractions (AC-1, AC-2 and AC-3), of which Fr. AC-2 was the most active fraction against HBeAg secretion and HBV DNA replication with IC50 values of 44.2 ± 2.8 and 23.2 ± 1.9 μg/mL. Nine chlorogenic acid analogues were detected from the active part (Fr. AC-2) by a LC/MS technique and further separated by a HPLC method. The isolates were determined as chlorogenic acid (1), cryptochlorogenic acid (2), neochlorogenic acid (3), 3,5-dicaffeoylquinic acid (4), 4,5-dicaffeoylquinic acid (5), 3,4-dicaffeoylquinic acid (6), chlorogenic acid methyl ester (7), cryptochlorogenic acid methyl ester (8), neochlorogenic acid methyl ester (9). Compounds 1-6 possessed potent activity against HBV DNA replication with IC50 values in the range of 5.5 ± 0.9-13.7 ± 1.3 μM. Di-caffeoyl analogues (4-6) also exhibited activity against the secretions of HBsAg and HBeAg. Esterified analogues (7-9) showed dramatically decreased anti-HBV activity, indicating that carboxyl group is closely associated to the anti-HBV activity. This investigation was focused on the active fractions of Artemisia capillaris and their active compositions, which showed that Fr. AC-2 was the main active section of Artemisia capillaris and chlorogenic acid analogues were the main constituents contributing to its anti-HBV activity. These results support the ethnopharmacological use of Artemisia capillaris as anti-HBV agents. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Effect of acidity on the energy level of curcumin dye extracted from Curcuma longa L

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

Agustia, Yuda Virgantara, E-mail: yuda.mechanical.engineer@student.uns.ac.id; Suyitno,, E-mail: suyitno@uns.ac.id; Sutanto, Bayu, E-mail: bayu.sutanto@student.uns.ac.id

2016-03-29

The purpose of this research is to investigate the effect of acidity on the energy level of curcumin dye. The natural dye, curcumin, was synthesized from Curcuma longa L. using a simple extraction technique. The purification of curcumin dye was conducted in a column of chromatography and its characteristics were studied. Next, the purified curcumin dye was added by benzoic acids until various acidities of 3.0, 3.5, 4.0, 4.5, and 5.0. The absorbance spectra and the functionality groups found in the dyes were detected by ultraviolet-visible spectroscopy and Fourier-transform infrared spectroscopy, respectively. Meanwhile, the energy level of the dyes, E{submore » HOMO} and E{sub LUMO} was measured by cyclic voltammetry. The best energy level of curcumin dye was achieved at pH 3.5 where E{sub red} = −0.37V, E{sub LUMO} = −4.28 eV, E{sub ox} = 1.15V, E{sub HOMO} = −5.83 eV, and E{sub band} {sub gap} = 1.55 eV. Therefore, the purified curcumin dye added by benzoic acid was promising for sensitizing the dye-sensitized solar cells.« less

Development of a screening method for the determination of 49 priority pollutants in soil

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

Kiang, P.H.; Grob, R.L.

1986-01-01

A screening procedure was develop for the determination of 49 priority pollutants in soil. An extraction procedure followed by the capillary gas chromatographic technique was used. Dual pH solutions with methylene chloride were used as extraction solvent system; no sample clean-up procedure was applied. Both base/neutral and acid fractions were analyzed on the same capillary column (SPB-1). The relative standard deviation for 5.1 ppm (51 ..mu..g/ 10 g) concentration in zero soil was less than 25%.

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

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

The effects of Bombyx mori silk strain and extraction time on the molecular and biological characteristics of sericin.

PubMed

Siritientong, Tippawan; Bonani, Walter; Motta, Antonella; Migliaresi, Claudio; Aramwit, Pornanong

2016-01-01

Sericin was extracted from three strains of Thai Bombyx mori silk cocoons (white shell Chul1/1, greenish shell Chul3/2, and yellow shell Chul4/2) by a high-pressure and high-temperature technique. The characteristics of sericin extracted from different fractions (15, 45, and 60 min extraction process) were compared. No differences in amino acid composition were observed among the three fractions. For all silk strains, sericin extracted from a 15-min process presented the highest molecular weight. The biological potential of the different sericin samples as a bioadditive for 3T3 fibroblast cells was assessed. When comparing sericin extracted from three silk strains, sericin fractions extracted from Chul4/2 improved cell proliferation, while sericin from Chul 1/1 activated Type I collagen production to the highest extent. This study allows the natural variability of sericin obtained from different sources and extraction conditions to be addressed and provides clues for the selection of sericin sources.

In situ Analysis of Organic Compounds on Mars using Chemical Derivatization and Gas Chromatography Mass Spectrometry

NASA Technical Reports Server (NTRS)

Glavin, D. P.; Buch, A.; Cabane, M.; Coll, P.; Navarro-Gonzalez, R.; Mahaffy, P. R.

2005-01-01

One of the core science objectives of NASA's 2009 Mars Science Laboratory (MSL) mission is to determine the past or present habitability of Mars. The search for key organic compounds relevant to terrestrial life will be an important part of that assessment. We have developed a protocol for the analysis of amino acids and carboxylic acids in Mars analogue materials using gas chromatography mass spectrometry (GCMS). As shown, a variety of carboxylic acids were readily identified in soil collected from the Atacama Desert in Chile at part-per-billion levels by GCMS after extraction and chemical derivatization using the reagent N,N-tert.-butyl (dimethylsilyl) trifluoroacetamide (MTBSTFA). Several derivatized amino acids including glycine and alanine were also detected by GCMS in the Atacama soil at lower concentrations (chromatogram not shown). Lacking derivatization capability, the Viking pyrolysis GCMS instruments could not have detected amino acids and carboxylic acids, since these non-volatile compounds require chemical transformation into volatile species that are stable in a GC column. We are currently optimizing the chemical extraction and derivatization technique for in situ GCMS analysis on Mars. Laboratory results of analyses of Atacama Desert samples and other Mars analogue materials using this protocol will be presented.

AMINO ACID ANALYSES OF THE ANTARCTIC CM2 METEORITES ALH 83100 AND LEW 90500 USING LIQUID CHROMATOGRAPHY-TIME OF FLIGHT-MASS SPECTROMETRY

NASA Technical Reports Server (NTRS)

Glavin, D. P.; Dworkin, J. P.; Aubrey, A.; Botta, O.; Doty, J. H., III; Bada, J. L.

2001-01-01

The investigation of organic compounds in primitive carbonaceous meteorites provides a record of the chemical processes that occurred in the early solar system. In particular, amino acids have been shown to be potential indicators in tracing the nature of carbonaceous chondrite parent bodies [ 13. The delivery of amino acids by carbonaceous chondrites to the early Earth could have been any important source of the Earth's prebiotic organic inventory [2]. Over 80 different amino acids have been detected in the Murchison CM2 meteorite, most of them completely non-existent in the terrestrial biosphere [3]. We have optimized a new liquid chromatography-time-of-flight-mass spectrometry (LC-ToF-MS) technique coupled with OPAMAC derivatization in order to detect amino acids in meteorite extracts by UV fluorescence and exact mass simultaneously. The detection limit of the LC-ToF-MS instrument for amino acids is at least 3 orders of magnitude lower than traditional GC-MS techniques. Here we report on the first analyses of amino acids and their enantiomeric abundances in the CM2 carbonaceous meteorites ALH 83100, LEW 90500, and Murchison using this new LC-ToF-MS instrument configuration. Amino acid analyses of any kind for the CM meteorite ALH 83100 have not previously been reported.

Four Different Methods Comparison for Extraction of Astaxanthin from Green Alga Haematococcus pluvialis

PubMed Central

Dong, Shengzhao; Huang, Yi; Zhang, Rui; Wang, Shihui; Liu, Yun

2014-01-01

Haematococcus pluvialis is one of the potent organisms for production of astaxanthin. Up to now, no efficient method has been achieved due to its thick cell wall hindering solvent extraction of astaxanthin. In this study, four different methods, hydrochloric acid pretreatment followed by acetone extraction (HCl-ACE), hexane/isopropanol (6 : 4, v/v) mixture solvents extraction (HEX-IPA), methanol extraction followed by acetone extraction (MET-ACE, 2-step extraction), and soy-oil extraction, were intensively evaluated for extraction of astaxanthin from H. pluvialis. Results showed that HCl-ACE method could obtain the highest oil yield (33.3 ± 1.1%) and astaxanthin content (19.8 ± 1.1%). Quantitative NMR analysis provided the fatty acid chain profiles of total lipid extracts. In all cases, oleyl chains were predominant, and high amounts of polyunsaturated fatty acid chains were observed and the major fatty acid components were oleic acid (13–35%), linoleic acid (37–43%), linolenic acid (20–31%), and total saturated acid (17–28%). DPPH radical scavenging activity of extract obtained by HCl-ACE was 73.2 ± 1.0%, which is the highest amongst the four methods. The reducing power of extract obtained by four extraction methods was also examined. It was concluded that the proposed extraction method of HCl-ACE in this work allowed efficient astaxanthin extractability with high antioxidant properties. PMID:24574909

Four different methods comparison for extraction of astaxanthin from green alga Haematococcus pluvialis.

PubMed

Dong, Shengzhao; Huang, Yi; Zhang, Rui; Wang, Shihui; Liu, Yun

2014-01-01

Haematococcus pluvialis is one of the potent organisms for production of astaxanthin. Up to now, no efficient method has been achieved due to its thick cell wall hindering solvent extraction of astaxanthin. In this study, four different methods, hydrochloric acid pretreatment followed by acetone extraction (HCl-ACE), hexane/isopropanol (6:4, v/v) mixture solvents extraction (HEX-IPA), methanol extraction followed by acetone extraction (MET-ACE, 2-step extraction), and soy-oil extraction, were intensively evaluated for extraction of astaxanthin from H. pluvialis. Results showed that HCl-ACE method could obtain the highest oil yield (33.3±1.1%) and astaxanthin content (19.8±1.1%). Quantitative NMR analysis provided the fatty acid chain profiles of total lipid extracts. In all cases, oleyl chains were predominant, and high amounts of polyunsaturated fatty acid chains were observed and the major fatty acid components were oleic acid (13-35%), linoleic acid (37-43%), linolenic acid (20-31%), and total saturated acid (17-28%). DPPH radical scavenging activity of extract obtained by HCl-ACE was 73.2±1.0%, which is the highest amongst the four methods. The reducing power of extract obtained by four extraction methods was also examined. It was concluded that the proposed extraction method of HCl-ACE in this work allowed efficient astaxanthin extractability with high antioxidant properties.

Converting paper mill sludge into neutral lipids by oleaginous yeast Cryptococcus vishniaccii for biodiesel production.

PubMed

Deeba, Farha; Pruthi, Vikas; Negi, Yuvraj S

2016-08-01

Paper mill sludge (PMS) was assessed as cheap renewable lignocellulosic biomass for lipid production by the oleaginous yeast Cryptococcus vishniaccii (MTCC 232). The sonicated paper mill sludge extract (PMSE) exhibited enhanced lipid yield and lipid content 7.8±0.57g/l, 53.40% in comparison to 5.5±0.8g/l, 40.44% glucose synthetic medium, respectively. The accumulated triglycerides (TAG) inside the lipid droplets (LDs) were converted to biodiesel by transesterification and thoroughly characterized using GC-MS technique. The fatty acid methyl ester (FAME) profile obtained reveals elevated content of oleic acid followed by palmitic acid, linoleic acid and stearic acid with improved oxidative stability related to biodiesel quality. Copyright © 2016 Elsevier Ltd. All rights reserved.

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 quantification of 17 free amino acids in Orthosiphon stamineus (OS) Benth extractsOS extracts were found to be rich in free amino acid contentL-aspartic acid was the major free amino acid in OS water extract while, in OS ethanol, methanol, 50% ethanol and 50% methanol extracts, L-glutamic acid was the major free amino acidL-serine was the minor free amino acid in OS water, ethanol and methanol extracts while, in OS 50% ethanol and 50% methanol extracts, L-threonine had the lowest concentration compared to other amino acid components. Abbreviations used: HPLC-DAD: High-Performance Liquid Chromatography with Diode-Array Detection, OS: Orthosiphon stamineus , OS-W: Orthosiphon stamineus water extract, OS-E: Orthosiphon stamineus ethanol extract, OS-M: Orthosiphon stamineus methanol extract, OS-EW: Orthosiphon stamineus 50% ethanol extract, OS-MW: Orthosiphon stamineus 50% methanol extract, OPA: O-phthaladehyde , SPE: Solid Phase Extraction, UV: Ultraviolet, LOD: Limit of Detection, LOQ: Limit of Quantification, RSD: Relative Standard Deviation.

[Phenolic acid derivatives from Bauhinia glauca subsp. pernervosa].

PubMed

Zhao, Qiao-Li; Wu, Zeng-Bao; Zheng, Zhi-Hui; Lu, Xin-Hua; Liang, Hong; Cheng, Wei; Zhang, Qing-Ying; Zhao, Yu-Ying

2011-08-01

To study the chemical constituents of Bauhinia glauca subsp. pernervosa, eleven phenolic acids were isolated from a 95% ethanol extract by using a combination of various chromatographic techniques including column chromatography over silica gel, ODS, MCI, Sephadex LH-20, and semi-preparative HPLC. By spectroscopic techniques including 1H NMR, 13C NMR, 2D NMR, and HR-ESI-MS, these compounds were identified as isopropyl O-beta-(6'-O-galloyl)-glucopyranoside (1), ethyl O-beta-(6'-O-galloyl)-glucopyranoside (2), 3, 4, 5-trimethoxyphenyl-(6'-O-galloyl)-O-beta-D-glucopyranoside (3), 3, 4, 5-trimethoxyphenyl-beta-D-glucopyranoside (4), gallic acid (5), methyl gallate (6), ethyl gallate (7), protocatechuic acid (8), 3, 5-dimethoxy-4-hydroxybenzoic acid (9), erigeside C (10) and glucosyringic acid (11). Among them, compound 1 is a new polyhydroxyl compound; compounds 2, 10, and 11 were isolated from the genus Bauhinia for the first time, and the other compounds were isolated from the plant for the first time. Compounds 6 and 8 showed significant protein tyrosine phosphatase1B (PTP1B) inhibitory activity in vitro with the IC50 values of 72.3 and 54.1 micromol x L(-1), respectively.

Fourier Transform Infrared Spectroscopy and Multivariate Analysis for Online Monitoring of Dibutyl Phosphate Degradation Product in Tributyl Phosphate/n-Dodecane/Nitric Acid Solvent

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

Tatiana G. Levitskaia; James M. Peterson; Emily L. Campbell

2013-12-01

In liquid–liquid extraction separation processes, accumulation of organic solvent degradation products is detrimental to the process robustness, and frequent solvent analysis is warranted. Our research explores the feasibility of online monitoring of the organic solvents relevant to used nuclear fuel reprocessing. This paper describes the first phase of developing a system for monitoring the tributyl phosphate (TBP)/n-dodecane solvent commonly used to separate used nuclear fuel. In this investigation, the effect of extraction of nitric acid from aqueous solutions of variable concentrations on the quantification of TBP and its major degradation product dibutylphosphoric acid (HDBP) was assessed. Fourier transform infrared (FTIR)more » spectroscopy was used to discriminate between HDBP and TBP in the nitric acid-containing TBP/n-dodecane solvent. Multivariate analysis of the spectral data facilitated the development of regression models for HDBP and TBP quantification in real time, enabling online implementation of the monitoring system. The predictive regression models were validated using TBP/n-dodecane solvent samples subjected to high-dose external ?-irradiation. The predictive models were translated to flow conditions using a hollow fiber FTIR probe installed in a centrifugal contactor extraction apparatus, demonstrating the applicability of the FTIR technique coupled with multivariate analysis for the online monitoring of the organic solvent degradation products.« less

Fourier Transform Infrared Spectroscopy and Multivariate Analysis for Online Monitoring of Dibutyl Phosphate Degradation Product in Tributyl Phosphate /n-Dodecane/Nitric Acid Solvent

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

Levitskaia, Tatiana G.; Peterson, James M.; Campbell, Emily L.

2013-11-05

In liquid-liquid extraction separation processes, accumulation of organic solvent degradation products is detrimental to the process robustness and frequent solvent analysis is warranted. Our research explores feasibility of online monitoring of the organic solvents relevant to used nuclear fuel reprocessing. This paper describes the first phase of developing a system for monitoring the tributyl phosphate (TBP)/n-dodecane solvent commonly used to separate used nuclear fuel. In this investigation, the effect of extraction of nitric acid from aqueous solutions of variable concentrations on the quantification of TBP and its major degradation product dibutyl phosphoric acid (HDBP) was assessed. Fourier Transform Infrared Spectroscopymore » (FTIR) spectroscopy was used to discriminate between HDBP and TBP in the nitric acid-containing TBP/n-dodecane solvent. Multivariate analysis of the spectral data facilitated the development of regression models for HDBP and TBP quantification in real time, enabling online implementation of the monitoring system. The predictive regression models were validated using TBP/n-dodecane solvent samples subjected to the high dose external gamma irradiation. The predictive models were translated to flow conditions using a hollow fiber FTIR probe installed in a centrifugal contactor extraction apparatus demonstrating the applicability of the FTIR technique coupled with multivariate analysis for the online monitoring of the organic solvent degradation products.« less

Extraction and quantitative analysis of iodine in solid and solution matrixes.

PubMed

Brown, Christopher F; Geiszler, Keith N; Vickerman, Tanya S

2005-11-01

129I is a contaminant of interest in the vadose zone and groundwater at numerous federal and privately owned facilities. Several techniques have been utilized to extract iodine from solid matrixes; however, all of them rely on two fundamental approaches: liquid extraction or chemical/heat-facilitated volatilization. While these methods are typically chosen for their ease of implementation, they do not totally dissolve the solid. We defined a method that produces complete solid dissolution and conducted laboratory tests to assess its efficacy to extract iodine from solid matrixes. Testing consisted of potassium nitrate/potassium hydroxide fusion of the sample, followed by sample dissolution in a mixture of sulfuric acid and sodium bisulfite. The fusion extraction method resulted in complete sample dissolution of all solid matrixes tested. Quantitative analysis of 127I and 129I via inductively coupled plasma mass spectrometry showed better than +/-10% accuracy for certified reference standards, with the linear operating range extending more than 3 orders of magnitude (0.005-5 microg/L). Extraction and analysis of four replicates of standard reference material containing 5 microg/g 127I resulted in an average recovery of 98% with a relative deviation of 6%. This simple and cost-effective technique can be applied to solid samples of varying matrixes with little or no adaptation.

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...

The Spermatogenic Effect of Yacon Extract and Its Constituents and Their Inhibition Effect of Testosterone Metabolism

PubMed Central

Park, Jeong Sook; Han, Kun

2013-01-01

We screened the pharmacological effects of a 50% ethanol extract of Yacon tubers and leaves on spermatogenesis in rats. As a result, we found that Yacon tuber extracts increased sperm number and serum testosterone level in rats. It has been reported that the crude extract of Yacon tubers and leaves contain phenolic acids, such as, chlorogenic acid, ferulic acid and caffeic acid by HPLC/MS analysis. We were interested in the contributions made by phenolic acid, particularly chlorogenic acid of Yacon tuber extract to the spermatogenic activity. After administering Yacon tuber extract or chlorogenic acid to rats for 5 weeks, numbers of sperm in epididymis were increased by 34% and 20%, respectively. We also administered ferulic acid, which has been reported to be a metabolite of chlorogenic acid and a constituent of Yacon tuber extract to investigate its spermatogenic activity in rats. Yacon tuber extract and ferulic acid increased sperm numbers by 43% and 37%, respectively. And, Yacon tuber extract, and chlorogenic acid showed significantly inhibition effect of testoeterone degradation in rat liver homogenate. We considered that the spermatogenic effect of Yacon tuber extract might be related to phenolic compounds and their inhibitory effect of testosterone degradation. Yacon showed the possibility as ameliorable agents of infertility by sperm deficiency and late onset hypogonadism syndrome with low level of testosterone. PMID:24009874

Data set for extraction and transesterification of bio-oil from Stoechospermum marginatum, a brown marine algae.

PubMed

Venkatesan, Hariram; Godwin, John J; Sivamani, Seralathan

2017-10-01

The article presents the experimental data on the extraction and transesterification of bio-oil derived from Stoechospermum marginatum, a brown macro marine algae. The samples were collected from Mandapam region, Gulf of Mannar, Tamil Nadu, India. The bio-oil was extracted using Soxhlet technique with a lipid extraction efficiency of 24.4%. Single stage transesterification was adopted due to lower free fatty acid content. The yield of biodiesel was optimized by varying the process parameters. The obtained data showed the optimum process parameters as reaction time 90 min, reaction temperature 65 °C, catalyst concentration 0.50 g and 8:1 M ratio. Furthermore, the data pertaining to the physio-chemical properties of the derived algal biodiesel were also presented.

Phenolic Profile and Antioxidant Activity of Centaurea choulettiana Pomel (Asteraceae) Extracts.

PubMed

Azzouzi, Djihane; Bioud, Kenza; Demirtas, Ibrahim; Gul, Fatih; Sarri, Djamel; Benayache, Samir; Benayache, Fadila; Mekkiou, Ratiba

2016-01-01

This study aimed to quantify phenolic compounds in ethyl acetate and n-butanol extract of Centaurea choulettiana Pomel (Asteraceae) leaves and flowers; compare the antioxidant activity of their extracts, identification and quantification of their phenolic acids. Both organs extracts of Centaurea choulettiana Pomel were investigated and evaluated for their potential antioxidant properties using total phenolics and flavonoids content, DPPH radical scavenging and lipid peroxidation inhibition assays. HPLC-TOF/MS analyses were carried out to identify and quantify some phenolic acids. The amounts of phenolic and flavonoid content were higher in ethyl acetate extract of leaves (325.81 ± 0.038 mgGAE and 263.73 ± 0.004 mgQE /g of extract) respectively. Besides, this extract exhibited the most powerful effect on the DPPH radical scavenging activity with (96.54%), on lipid peroxydation inhibition (64.17%). Ethyl acetate extract of leaves and flowers were found to contain almost the same phenolic compounds, with the leaves having the highest values. Chlorogenic acid was detected in the n-butanol extract of flowers with the highest concentration 17.78 mg/kg plant. The ethyl acetate extract of leaves of Centaurea choulettiana possesses strong antioxidative properties in vitro. They are confirmed by high polyphenols and flavonoids content. The HPLC-TOF/MS analysis reveals the presence of 4-hydroxybenzoic acid, gentisic acid, chlorogenic acid, caffeic acid, vanillic acid, p-Coumaric acid, ferulic acid, salicylic acid and protocatechuic acid. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Green technology approach towards herbal extraction method

NASA Astrophysics Data System (ADS)

Mutalib, Tengku Nur Atiqah Tengku Ab; Hamzah, Zainab; Hashim, Othman; Mat, Hishamudin Che

2015-05-01

The aim of present study was to compare maceration method of selected herbs using green and non-green solvents. Water and d-limonene are a type of green solvents while non-green solvents are chloroform and ethanol. The selected herbs were Clinacanthus nutans leaf and stem, Orthosiphon stamineus leaf and stem, Sesbania grandiflora leaf, Pluchea indica leaf, Morinda citrifolia leaf and Citrus hystrix leaf. The extracts were compared with the determination of total phenolic content. Total phenols were analyzed using a spectrophotometric technique, based on Follin-ciocalteau reagent. Gallic acid was used as standard compound and the total phenols were expressed as mg/g gallic acid equivalent (GAE). The most suitable and effective solvent is water which produced highest total phenol contents compared to other solvents. Among the selected herbs, Orthosiphon stamineus leaves contain high total phenols at 9.087mg/g.

SOLVENT EXTRACTION PROCESS FOR SEPARATING ACTINIDE AND LANTHANIDE METAL VALUES

DOEpatents

Hildebrandt, R.A.; Hyman, H.H.; Vogler, S.

1962-08-14

A process of countercurrently extracting an aqueous mineral acid feed solution for the separation of actinides from lanthanides dissolved therern is described. The feed solution is made acid-defrcient with alkali metal hydroxide prior to.contact with acid extractant; during extraction, however, acid is transferred from organic to aqueous solution and the aqueous solution gradually becomes acid. The acid-deficient phase ' of the process promotes the extraction of the actinides, while the latter acid phase'' of the process improves retention of the lanthanides in the aqueous solution. This provides for an improved separation. (AEC)

Celastrus paniculatus seed water soluble extracts protect against glutamate toxicity in neuronal cultures from rat forebrain.

PubMed

Godkar, Praful B; Gordon, Richard K; Ravindran, Arippa; Doctor, Bhupendra P

2004-08-01

Aqueous extracts of Celastrus paniculatus (CP) seed have been reported to improve learning and memory in rats. In addition, these extracts were shown to have antioxidant properties, augmented endogenous antioxidant enzymes, and decreased lipid peroxidation in rat brain. However, water soluble extracts of CP seed (CP-WSE) have not been evaluated for their neuroprotective effects. In the study reported here, we used enriched forebrain primary neuronal cell (FBNC) cultures to study the neuroprotective effects of three CP-WSE extracts (a room temperature, WF; a hot water, HF; and an acid, AF) on glutamate-induced toxicity. FBNC were pre-treated with the CP-WSE and then with glutamate to evaluate the protection afforded against excitatory amino acid-induced toxicity. The criteria for neuroprotection were based on the effects of CP-WSE on a mitochondrial function test following glutamate-induced neurotoxicity. Pre-treatment of neuronal cells with CP-WSE significantly attenuated glutamate-induced neuronal death. To understand the molecular mechanism of action of CP-WSE, we conducted electrophysiological studies using patch-clamp techniques on N-methyl-D-aspartate (NMDA)-activated whole-cell currents in FBNC. WSE significantly and reversibly inhibited whole-cell currents activated by NMDA. The results suggest that CP-WSE protected neuronal cells against glutamate-induced toxicity by modulating glutamate receptor function.

Characterization by high-performance liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry of the lipid fraction of Spirulina platensis pressurized ethanol extract.

PubMed

Herrero, Miguel; Vicente, María J; Cifuentes, Alejandro; Ibáñez, Elena

2007-01-01

Microalgae have been suggested as a potential source for new functional ingredients, making possible the development of new functional foods from natural origin. Among the natural ingredients, polyunsaturated fatty acids (PUFAs) have generally been identified as an interesting group of compounds with biological activity, mainly related to their anti-inflammatory properties. In this regard, the use of environmentally friendly extraction procedures (e.g. pressurized liquid extraction, PLE) to obtain such natural ingredients is also becoming necessary. In this work, an exhaustive characterization of the lipid fraction of a pressurized ethanolic extract of the microalga Spirulina platensis is carried out. To achieve this objective high-performance liquid chromatography (HPLC) coupled to quadrupole time-of-flight mass spectrometry (QTOF-MS) is employed. The use of the QTOF analyzer allows the selection and isolation of precursor ions as well as providing the high efficiency, sensitivity and mass accuracy required. By means of this powerful hyphenated technique, it was possible to identify several polar lipids in an extract of S. platensis (some of them, to our knowledge, described for the first time in this work), including four free fatty acids, four monogalactosyl monoacylglycerols, three phosphatidylglycerols and two sulfoquinovosyl diacylglycerols.

The effect of lead exposure on fatty acid composition in mouse brain analyzed using pseudo-catalytic derivatization.

PubMed

Jung, Jong-Min; Lee, Jechan; Kim, Ki-Hyun; Jang, In Geon; Song, Jae Gwang; Kang, Kyeongjin; Tack, Filip M G; Oh, Jeong-Ik; Kwon, Eilhann E; Kim, Hyung-Wook

2017-03-01

We performed toxicological study of mice exposed to lead by quantifying fatty acids in brain of the mice. This study suggests that the introduced analytical method had an extremely high tolerance against impurities such as water and extractives; thus, it led to the enhanced resolution in visualizing the spectrum of fatty acid profiles in animal brain. Furthermore, one of the biggest technical advantages achieved in this study was the quantitation of fatty acid methyl ester profiles of mouse brain using a trace amount of sample (e.g., 100 μL mixture). Methanol was screened as the most effective extraction solvent for mouse brain. The behavioral test of the mice before and after lead exposure was conducted to see the effect of lead exposure on fatty acid composition of the mice' brain. The lead exposure led to changes in disease-related behavior of the mice. Also, the lead exposure induced significant alterations of fatty acid profile (C16:0, C 18:0, and C 18:1) in brain of the mice, implicated in pathology of psychiatric diseases. The alteration of fatty acid profile of brain of the mice suggests that the derivatizing technique can be applicable to most research fields associated with the environmental neurotoxins with better resolution in a short time, as compared to the current protocols for lipid analysis. Copyright © 2016 Elsevier Ltd. All rights reserved.

Identification and characterization of hydrocolloid from Cordia myxa leaf.

PubMed

Samavati, Vahid; Lorestani, Mohammad; Joolazadeh, Sajjad

2014-04-01

Hot water extraction technique was employed to extract the hydrocolloid from Cordia myxa leaf (PCM). The optimal conditions for extraction of PCM were determined using response surface methodology. A Box-Behnken design (BBD) was applied to evaluate the effects of three independent variables (extraction time (X1: 1-4 h), extraction temperature (X2: 55-95 °C), and water to raw material ratio (X3: 5-30 ml/g) on the extraction yield of PCM. The content of moisture, water-soluble and water-insoluble ash, crude protein and total phenol were determined in the extracted hydrocolloid by standard methods. The maximum hydrocolloid extraction yield (9.501±0.15%) was achieved by using extraction time of 4.94 h, extraction temperature of 94.91 °C and water to raw material ratio of 21.74 ml/g. The contents of moisture, crude protein, water-soluble and water-insoluble ash and total phenol were 21.63±0.94%, 14.27±0.55%, 3.07±0.16% and 2.61±0.19 mg galic acid/g, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

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 successfully developed and validated for simultaneous determination and quantification of 17 free amino acids in Orthosiphon stamineus (OS) Benth extractsOS extracts were found to be rich in free amino acid contentL-aspartic acid was the major free amino acid in OS water extract while, in OS ethanol, methanol, 50% ethanol and 50% methanol extracts, L-glutamic acid was the major free amino acidL-serine was the minor free amino acid in OS water, ethanol and methanol extracts while, in OS 50% ethanol and 50% methanol extracts, L-threonine had the lowest concentration compared to other amino acid components. Abbreviations used: HPLC-DAD: High-Performance Liquid Chromatography with Diode-Array Detection, OS: Orthosiphon stamineus, OS-W: Orthosiphon stamineus water extract, OS-E: Orthosiphon stamineus ethanol extract, OS-M: Orthosiphon stamineus methanol extract, OS-EW: Orthosiphon stamineus 50% ethanol extract, OS-MW: Orthosiphon stamineus 50% methanol extract, OPA: O-phthaladehyde, SPE: Solid Phase Extraction, UV: Ultraviolet, LOD: Limit of Detection, LOQ: Limit of Quantification, RSD: Relative Standard Deviation. PMID:29142388

Comparison of different extraction procedures for the comprehensive characterization of bioactive phenolic compounds in Rosmarinus officinalis by reversed-phase high-performance liquid chromatography with diode array detection coupled to electrospray time-of-flight mass spectrometry.

PubMed

Borrás Linares, I; Arráez-Román, D; Herrero, M; Ibáñez, E; Segura-Carretero, A; Fernández-Gutiérrez, A

2011-10-21

In the present work, a comparative study between two environmentally friendly and selective extraction techniques, such as supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE) have been carried out focusing in the bioactive phenolic compounds present in Rosmarinus officinalis. For the analysis of the SFE and PLE extracts, a new methodology for qualitative characterization has been developed, based on the use of reversed-phase high-performance liquid chromatography (RP-HPLC), equipped with two different detection systems coupled in series: diode array detector (DAD) and time of flight mass spectrometry (TOF-MS) detector connected via an electrospray ionization interface (ESI). The use of a small particle size C(18) column (1.8 μm) provided a great resolution and made possible the separation of several isomers. Moreover, UV-visible spectrophotometry is a valuable tool for identifying the class of phenolic compounds, whereas MS data enabled to structurally characterize the compounds present in the extracts. The applied methodology was useful for the determination of many well-known phenolic compounds present in R. officinalis, such as carnosol, carnosic acid, rosmadial, rosmanol, genkwanin, homoplantaginin, scutellarein, cirsimaritin and rosmarinic acid, as well as other phenolic compounds present in other species belonging to Lamiaceae family. Copyright © 2011 Elsevier B.V. All rights reserved.

The effect of different extraction techniques on property and bioactivity of polysaccharides from Dioscorea hemsleyi.

PubMed

Zhao, Chengcheng; Li, Xia; Miao, Jing; Jing, Songsong; Li, Xuejiao; Huang, Luqi; Gao, Wenyuan

2017-09-01

The rhizoma of Dioscorea hemsleyi (DH) has been used as a treatment of diabetes in China for hundreds of years. Polysaccharides in DH were extracted by using ultrasonic-assisted extraction (UAE), cold water extraction (CWE), warm water extraction (WWE) and hot water extraction (HWE), separately. Then the different characterizations of four DH polysaccharide (DHP) samples were analyzed by high-performance liquid chromatography (HPLC), high-performance Gel permeation chromatography (HGPC), ultraviolet-visible spectroscopy(UV), fourier transform-infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Their activities in vitro of DHP were compared. Experimental results showed that HWE had the highest yield and large molecular weight. CWE had the highest uronic acid yield and little molecular weight, and its DPPH, AGI and AAI activity were the best. The molecular weight of UAE was small, and its RP and FRAP activity were the best. Four DHP samples had differences in the surface topography, while they all had the typical IR spectra characteristic of polysaccharides. According the correlation analysis, it showed that the more uronic acid and the lower molecular weight was, the higher the antioxidant activity was. The high content of monosaccharide composition of Xyl, Ara, GlcA and GalA, and little molecular weight have good effect on antidiabetic activity. Copyright © 2017 Elsevier B.V. All rights reserved.

Impact of ellagic acid in bone formation after tooth extraction: an experimental study on diabetic rats.

PubMed

Al-Obaidi, Mazen M Jamil; Al-Bayaty, Fouad Hussain; Al Batran, Rami; Hussaini, Jamal; Khor, Goot Heah

2014-01-01

To estimate the impact of ellagic acid (EA) towards healing tooth socket in diabetic animals, after tooth extraction. Twenty-four Sprague Dawley male rats weighing 250-300 g were selected for this study. All animals were intraperitoneally injected with 45 mg/kg (b.w.) of freshly prepared streptozotocin (STZ), to induce diabetic mellitus. Then, the animals were anesthetized, and the upper left central incisor was extracted and the whole extracted sockets were filled with Rosuvastatin (RSV). The rats were separated into three groups, comprising 8 rats each. The first group was considered as normal control group and orally treated with normal saline. The second group was regarded as diabetic control group and orally treated with normal saline, whereas the third group comprised diabetic rats, administrated with EA (50 mg/kg) orally. The maxilla tissue stained by eosin and hematoxylin (H&E) was used for histological examinations and immunohistochemical technique. Fibroblast growth factor (FGF-2) and alkaline phosphatase (ALP) were used to evaluate the healing process in the extracted tooth socket by immunohistochemistry test. The reactions of immunohistochemistry for FGF-2 and ALP presented stronger expression, predominantly in EA treated diabetic rat, than the untreated diabetic rat. These findings suggest that the administration of EA combined with RSV may have accelerated the healing process of the tooth socket of diabetic rats, after tooth extraction.

Stable carbon and nitrogen isotope analysis of avian uric acid.

PubMed

Bird, Michael I; Tait, Elaine; Wurster, Christopher M; Furness, Robert W

2008-11-01

We report results obtained using a new technique developed to measure the stable-isotope composition of uric acid isolated from bird excreta (guano). Results from a diet-switch feeding trial using zebra finches suggest that the delta(13)C of uric acid in the guano equilibrates with the diet of the bird within 3 days of a change in diet, while the equilibration time for delta(15)N may be longer. The average carbon isotope discrimination between uric acid and food before the diet switch was +0.34 +/- 1 per thousand (1sigma) while after the diet switch this increased slightly to +0.83 +/- 0.7 per thousand (1sigma). Nitrogen isotope discrimination was +1.3 +/- 0.3 per thousand (1sigma) and +0.3 +/- 0.3 per thousand (1sigma) before and after the diet switch; however, it is possible that the nitrogen isotope values did not fully equilibrate with diet switch over the course of the experiment. Analyses of other chemical fractions of the guano (organic residue after uric acid extraction and non-uric acid organics solubilised during extraction) suggest a total range of up to 3 per thousand for both delta(13)C and delta(15)N values in individual components of a single bulk guano sample. The analysis of natural samples from a range of terrestrial and marine species demonstrates that the technique yields isotopic compositions consistent with the known diets of the birds. The results from natural samples further demonstrate that multiple samples from the same species collected from the same location yield similar results, while different species from the same location exhibit a range of isotopic compositions indicative of different dietary preferences. Given that many samples of guano can be rapidly collected without any requirement to capture specimens for invasive sampling, the stable-isotope analysis of uric acid offers a new, simple and potentially powerful tool for studying avian ecology and metabolism.

Fast targeted analysis of 132 acidic and neutral drugs and poisons in whole blood using LC-MS/MS.

PubMed

Di Rago, Matthew; Saar, Eva; Rodda, Luke N; Turfus, Sophie; Kotsos, Alex; Gerostamoulos, Dimitri; Drummer, Olaf H

2014-10-01

The aim of this study was to develop an LC-MS/MS based screening technique that covers a broad range of acidic and neutral drugs and poisons by combining a small sample volume and efficient extraction technique with simple automated data processing. After protein precipitation of 100μL of whole blood, 132 common acidic and neutral drugs and poisons including non-steroidal anti-inflammatory drugs, barbiturates, anticonvulsants, antidiabetics, muscle relaxants, diuretics and superwarfarin rodenticides (47 quantitated, 85 reported as detected) were separated using a Shimadzu Prominence HPLC system with a C18 separation column (Kinetex XB-C18, 4.6mm×150mm, 5μm), using gradient elution with a mobile phase of 25mM ammonium acetate buffer (pH 7.5)/acetonitrile. The drugs were detected using an ABSciex(®) API 2000 LC-MS/MS system (ESI+ and -, MRM mode, two transitions per analyte). The method was fully validated in accordance with international guidelines. Quantification data obtained using one-point calibration compared favorably to that using multiple calibrants. The presented LC-MS/MS assay has proven to be applicable for determination of the analytes in blood. The fast and reliable extraction method combined with automated processing gives the opportunity for high throughput and fast turnaround times for forensic and clinical toxicology. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Gastroprotective activity of the hydroethanolic extract and isolated compounds from the leaves of Solanum cernuum Vell.

PubMed

Abreu Miranda, Mariza; Lemos, Marivane; Alves Cowart, Kamila; Rodenburg, Douglas; D McChesney, James; Radwan, Mohamed M; Furtado, Niege Araçari Jacometti Cardoso; Kenupp Bastos, Jairo

2015-08-22

Solanum cernuum Vell. (Solanaceae) is a Brazilian medicinal plant, traditionally known as "panaceia". Its folk name is probably due to its wide range of applications in traditional medicine including the treatment of ulcers. To evaluate the gastroprotective activities of the hydroethanolic extract (ESC) of S. cernuum and its major isolated compounds using in vivo gastric ulcer models. The ESC extract was obtained by maceration followed by percolation of the dried and powdered leaves of S. cernuum in ethanol:water (7:3). The major compounds in the extract were isolated by applying various preparative chromatographic techniques. The gastroprotective activity was evaluated in mice using different gastric ulcer-induced models. The anti-Helicobacter pylori activity was performed using the agar-well diffusion and broth microdilution methods. The ESC extract showed gastroprotective effects in the assay of acute gastric ulcer-induced by HCl/EtOH, nonsteroidal anti-inflammatory drug, and acetic acid-induced chronic ulcer protocols. The results also demonstrated that the gastroprotection induced by ESC extract is related to the activity of nitric oxide and endogenous sulfhydryls, which are important gastroprotective factors. The ESC extract and the alkaloid cernumidine did not show activity against H. pylori in the concentrations tested. The present study showed that the crude extract of S. cernuum possessed gastroprotective activity which corroborating the traditional use of this plant for the treatment of gastric ulcers. The isolated flavonoids, quercitrin and afzelin as well as the phenylpropanoid, isoferulic acid are suggested to be the compounds responsible for the gastroprotective activity of S. cernuum extract. Copyright © 2015. Published by Elsevier Ireland Ltd.

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.

Microwave-assisted extraction and a new determination method for total steroid saponins from Dioscorea zingiberensis C.H. Wright.

PubMed

Ren, Yao; Chen, Yu; Hu, Bohan; Wu, Hui; Lai, Furao; Li, Xiaofeng

2015-12-01

An efficient microwave-assisted extraction (MAE) technique was applied to isolate total steroid saponins from Dioscorea zingiberensis C.H. Wright (DZW). The optimal extracting conditions were established as 75% ethanol as solvent, ratio of solid/liquid 1:20 (g/ml), temperature 75 °C, irradiation power 600 W and three extraction cycles of 6 min each. Scanning electron microscopy (SEM) images of DZW processed by four different extractions provided visual evidence of the disruption effect on DZW. Diosgenin was quantified by HPLC and examined further by LC-ESI/MS after acid hydrolysis. Total steroid saponins were calculated using diosgenin from total steroid saponins. The MAE procedure was optimized, validated and compared with other conventional extraction processes. This report provides a convenient technology for the extraction and quantification of total saponins of DZW combining MAE with HPLC and LC-ESI/MS for the first time. Copyright © 2015 Elsevier Inc. All rights reserved.

In vitro inhibitory effects of Moringa oleifera leaf extract and its major components on chemiluminescence and chemotactic activity of phagocytes.

PubMed

Vongsak, Boonyadist; Gritsanapan, Wandee; Wongkrajang, Yuvadee; Jantan, Ibrahim

2013-11-01

The ethanol extract of Moringa oleifera Lam. leaves and its major constituents, crypto-chlorogenic acid, quercetin 3-O-glucoside and kaempferol 3-O-glucoside, were investigated on the respiratory burst of human whole blood and isolated human polymorphonuclear leukocytes (PMNs) using a luminol-based chemiluminescence assay. The chemotactic migration of PMNs was also investigated using the Boyden chamber technique. The ethanol extract demonstrated inhibitory activities on the oxidative burst and the chemotactic migration of PMNs. Quercetin 3-O-glucoside, crypto-chlorogenic acid, and kaempferol 3-O-glucoside, isolated from the extract, expressed relatively strong inhibitory activity on the oxidative burst of PMNs with IC50 values of 4.1, 6.7 and 7.0 microM, respectively, comparable with that of aspirin. They also demonstrated strong inhibition of chemotatic migration of PMNs with IC50 values of 9.5, 15.9 and 18.2 microM, respectively. The results suggest that M. oleifera leaves could modulate the immune response of human phagocytes, linking to its ethnopharmacological use as an anti-inflammatory agent. The immunomodulating activity of the plant was mainly due to its major components.

Microencapsulation of Garcinia fruit extract by spray drying and its effect on bread quality.

PubMed

Ezhilarasi, Perumal Natarajan; Indrani, Dasappa; Jena, Bhabani Sankar; Anandharamakrishnan, Chinnaswamy

2014-04-01

(-)-Hydroxycitric acid (HCA) is the major acid present in the fruit rinds of certain species of Garcinia. HCA has been reported to have several health benefits. As HCA is highly hygroscopic in nature and thermally sensitive, it is difficult to incorporate in foodstuffs. Hence, Garcinia cowa fruit extract was microencapsulated using three different wall materials such as whey protein isolate (WPI), maltodextrin (MD) and a combination of whey protein isolate and maltodextrin (WPI + MD) by spray drying. Further, these microencapsulated powders were evaluated for their impact on bread quality and HCA retention. Maltodextrin (MD) encapsulates had higher free (86%) and net HCA (90%) recovery. Microencapsulates incorporated breads had enhanced qualitative characteristics and higher HCA content than water extract incorporated bread due to efficient encapsulation during bread baking. Comparatively, bread with MD encapsulates showed softer crumb texture, desirable sensory attributes with considerable volume and higher HCA content. The higher HCA contents of encapsulate incorporated breads were sufficient to claim for functionality of HCA in bread. Comparatively, MD had efficiently encapsulated Garcinia fruit extract during spray drying and bread baking. Spray drying proved to be an excellent encapsulation technique for incorporation into the food system. © 2013 Society of Chemical Industry.

Rapid and simultaneous determination of twenty amino acids in complex biological and food samples by solid-phase microextraction and gas chromatography-mass spectrometry with the aid of experimental design after ethyl chloroformate derivatization.

PubMed

Mudiam, Mohana Krishna Reddy; Ratnasekhar, Ch; Jain, Rajeev; Saxena, Prem Narain; Chauhan, Abhishek; Murthy, R C

2012-10-15

Amino acids play a vital role as intermediates in many important metabolic pathways such as the biosynthesis of nucleotides, vitamins and secondary metabolites. A sensitive and rapid analytical method has been proposed for the first time for the simultaneous determination of twenty amino acids using solid-phase microextraction (SPME). The protein samples were hydrolyzed by 6M HCl under microwave radiation for 120 min. Then the amino acids were derivatized by ethyl chloroformate (ECF) and the ethoxy carbonyl ethyl esters of amino acids formed were extracted using SPME by direct immersion. Finally the extracted analytes on the SPME fiber were desorbed at 260°C and analyzed by gas chromatography-mass spectrometer (GC-MS) in electron ionization mode. Factors which affect the SPME efficiency were screened by Plackett-Burmann design; most significant factors were optimized with response surface methodology. The optimum conditions for SPME are as follows: pH of 1.7, ionic strength of 733 mg, extraction time of 30 min and fiber of divinyl benzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS). The recovery of all the amino acids was found to be in the range of 89.17-100.98%. The limit of detection (LOD) of all derivatized amino acids in urine, hair and soybean was found to be in the range of 0.20-7.52 μg L(-1), 0.21-8.40 μg L(-1) and 0.18-5.62 μg L(-1), respectively. Finally, the proposed technique was successfully applied for the determination of amino acids in complex biological (hair, urine) and food samples (soybean). The method can find wide applications in the routine analysis of amino acids in any biological as well as food samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparison of Oil Content and Fatty Acids Profile of Western Schley, Wichita, and Native Pecan Nuts Cultured in Chihuahua, Mexico.

PubMed

Rivera-Rangel, L R; Aguilera-Campos, K I; García-Triana, A; Ayala-Soto, J G; Chavez-Flores, D; Hernández-Ochoa, L

2018-01-01

Two different extraction processes, Soxhlet and ultrasound, were used to obtain the oil extracts of Western Schley, Wichita, and Native pecan nuts cultured in Chihuahua, Mexico. The aspects evaluated in this study were the extraction yield of the processes and fatty acids' profile of the resulting extracts. Gas chromatography coupled with mass spectrometry (GC-MS) was used to identify and determine the composition percentage of fatty acids present in pecan nuts oils extracted. The results obtained show that higher oil extraction yields were obtained by Soxhlet method with hexane (69.90%) in Wichita varieties. Wichita, Western Schley, and Native pecan nuts from Chihuahua are rich in PUFA (polyunsaturated fatty acids) and MUFA (monounsaturated fatty acids) and have low levels of SFA (saturated fatty acids). The predominant fatty acid present in all pecan nuts oils was linoleic acid followed by oleic acid. Myristic acid, palmitic acid, and linolenic acid were also identified in representative quantities. The results from this study suggest that there are statistically significant differences in the chemical composition of the pecan nuts oils extracted from the varieties cultured in Chihuahua, Mexico, and those cultivated in other regions of the world.

Comparison of Oil Content and Fatty Acids Profile of Western Schley, Wichita, and Native Pecan Nuts Cultured in Chihuahua, Mexico

PubMed Central

Rivera-Rangel, L. R.; Aguilera-Campos, K. I.; García-Triana, A.; Ayala-Soto, J. G.; Chavez-Flores, D.

2018-01-01

Two different extraction processes, Soxhlet and ultrasound, were used to obtain the oil extracts of Western Schley, Wichita, and Native pecan nuts cultured in Chihuahua, Mexico. The aspects evaluated in this study were the extraction yield of the processes and fatty acids' profile of the resulting extracts. Gas chromatography coupled with mass spectrometry (GC-MS) was used to identify and determine the composition percentage of fatty acids present in pecan nuts oils extracted. The results obtained show that higher oil extraction yields were obtained by Soxhlet method with hexane (69.90%) in Wichita varieties. Wichita, Western Schley, and Native pecan nuts from Chihuahua are rich in PUFA (polyunsaturated fatty acids) and MUFA (monounsaturated fatty acids) and have low levels of SFA (saturated fatty acids). The predominant fatty acid present in all pecan nuts oils was linoleic acid followed by oleic acid. Myristic acid, palmitic acid, and linolenic acid were also identified in representative quantities. The results from this study suggest that there are statistically significant differences in the chemical composition of the pecan nuts oils extracted from the varieties cultured in Chihuahua, Mexico, and those cultivated in other regions of the world. PMID:29610686

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...

Metal Cationization Extractive Electrospray Ionization Mass Spectrometry of Compounds Containing Multiple Oxygens

NASA Astrophysics Data System (ADS)

Swanson, Kenneth D.; Spencer, Sandra E.; Glish, Gary L.

2017-06-01

Extractive electrospray ionization is an ambient ionization technique that allows real-time sampling of liquid samples, including organic aerosols. Similar to electrospray ionization, the composition of the electrospray solvent used in extractive electrospray ionization can easily be altered to form metal cationized molecules during ionization simply by adding a metal salt to the electrospray solvent. An increase in sensitivity is observed for some molecules that are lithium, sodium, or silver cationized compared with the protonated molecule formed in extractive electrospray ionization with an acid additive. Tandem mass spectrometry of metal cationized molecules can also significantly improve the ability to identify a compound. Tandem mass spectrometry of lithium and silver cationized molecules can result in an increase in the number and uniqueness of dissociation pathways relative to [M + H]+. These results highlight the potential for extractive electrospray ionization with metal cationization in analyzing complex aerosol mixtures. [Figure not available: see fulltext.

On-line identification of lysergic acid diethylamide (LSD) in tablets using a combination of a sweeping technique and micellar electrokinetic chromatography/77 K fluorescence spectroscopy.

PubMed

Fang, Ching; Liu, Ju-Tsung; Lin, Cheng-Huang

2003-03-01

This work describes a novel method for the accurate determination of lysergic acid diethylamide (LSD) in tablets. A technique involving sweeping-micellar electrokinetic chromatography (MEKC) was used for the initial on-line concentration and separation, after which a cryogenic molecular fluorescence experiment was performed at 77 K. Using this approach, not only the separation of LSD from the tablet extract was achieved, but on-line spectra were readily distinguishable and could be unambiguously assigned. The results are in agreement with analyses by gas chromatography-mass spectrometry (GC-MS). Thus, this method, which was found to be accurate, sensitive and rapid, has the potential for use as a reliable complementary method to GC-MS in such analyses.

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.

New microwave-integrated Soxhlet extraction. An advantageous tool for the extraction of lipids from food products.

PubMed

Virot, Matthieu; Tomao, Valérie; Colnagui, Giulio; Visinoni, Franco; Chemat, Farid

2007-12-07

A new process of Soxhlet extraction assisted by microwave was designed and developed. The process is performed in four steps, which ensures complete, rapid and accurate extraction of the samples. A second-order central composite design (CCD) has been used to investigate the performance of the new device. The results provided by analysis of variance and Pareto chart, indicated that the extraction time was the most important factor followed by the leaching time. The response surface methodology allowed us to determine optimal conditions for olive oil extraction: 13 min of extraction time, 17 min of leaching time, and 720 W of irradiation power. The proposed process is suitable for lipids determination from food. Microwave-integrated Soxhlet (MIS) extraction has been compared with a conventional technique, Soxhlet extraction, for the extraction of oil from olives (Aglandau, Vaucluse, France). The oils extracted by MIS for 32 min were quantitatively (yield) and qualitatively (fatty acid composition) similar to those obtained by conventional Soxhlet extraction for 8 h. MIS is a green technology and appears as a good alternative for the extraction of fat and oils from food products.

Unambiguous detection of astaxanthin and astaxanthin fatty acid esters in krill (Euphausia superba Dana).

PubMed

Grynbaum, Marc David; Hentschel, Petra; Putzbach, Karsten; Rehbein, Jens; Krucker, Manfred; Nicholson, Graeme; Albert, Klaus

2005-09-01

HPLC atmospheric pressure chemical ionization (APCI)/MS, GC MS, HPLC diode array detection (DAD), and NMR were used for the identification of astaxanthin and astaxanthin fatty acid esters in krill (Euphausia superba Dana). Matrix solid phase dispersion was applied for the extraction of the carotenoids. This gentle and expeditious extraction technique for solid and viscous samples leads to distinct higher enrichment rates than the conventional liquid-liquid extraction. The chromatographic separation was achieved employing a C30 RP column that allows the separation of shape-constrained geometrical isomers. A methanol/tert-butylmethyl ether/water gradient was applied. (all-E) Astaxanthin and the geometrical isomers were identified by HPLC APCI/MS, by coelution with isomerized authentical standard, by UV spectroscopy (DAD), and three isomers were unambiguously assigned by microcoil NMR spectroscopy. In this method, microcoils are transversally aligned to the magnetic field and have an increased sensitivity compared to the conventional double-saddle Helmholtz coils, thus enabling the measurement on small samples. The carotenol fatty acid esters were saponified enzymatically with Lipase type VII from Candida rugosa. The fatty acids were detected by GC MS after transesterification, but also without previous derivatization by HPLC APCI/MS. C14:0, C16:0, C16:1, C18:1, C20:0, C20:5, and C22:6 were found in astaxanthin monoesters and in astaxanthin diesters. (all-E) Astaxanthin was identified as the main isomer in six fatty acid ester fractions by NMR. Quantitation was carried out by the method of internal standard. (13-cis) Astaxanthin (70 microg/g), 542 microg/g (all-E) astaxanthin, 36 microg/g unidentified astaxanthin isomer, 62 microg/g (9-cis) astaxanthin, and 7842 microg/g astaxanthin fatty acid esters were found.

Comparison of microwave, ultrasound and accelerated-assisted solvent extraction for recovery of polyphenols from Citrus sinensis peels.

PubMed

Nayak, Balunkeswar; Dahmoune, Farid; Moussi, Kamal; Remini, Hocine; Dairi, Sofiane; Aoun, Omar; Khodir, Madani

2015-11-15

Peel of Citrus sinensis contains significant amounts of bioactive polyphenols that could be used as ingredients for a number of value-added products with health benefits. Extraction of polyphenols from the peels was performed using a microwave-assisted extraction (MAE) technique. The effects of aqueous acetone concentration, microwave power, extraction time and solvent-to-solid ratio on the total phenolic content (TPC), total antioxidant activity (TAA) (using DPPH and ORAC-values) and individual phenolic acids (IPA) were investigated using a response surface method. The TPC, TAA and IPA of peel extracts using MAE was compared with conventional, ultrasound-assisted and accelerated solvent extraction. The maximum predicted TPC under the optimal MAE conditions (51% acetone concentration in water (v/v), 500 W microwave power, 122 s extraction time and 25 mL g(-1) solvent to solid ratio), was 12.20 mg GAE g(-1) DW. The TPC and TAA in MAE extracts were higher than the other three extracts. Copyright © 2015 Elsevier Ltd. All rights reserved.

Determination of Microalgal Lipid Content and Fatty Acid for Biofuel Production

PubMed Central

Chen, Zhipeng; Wang, Lingfeng

2018-01-01

Biofuels produced from microalgal biomass have received growing worldwide recognition as promising alternatives to conventional petroleum-derived fuels. Among the processes involved, the downstream refinement process for the extraction of lipids from biomass greatly influences the sustainability and efficiency of the entire biofuel system. This review summarizes and compares the current techniques for the extraction and measurement of microalgal lipids, including the gravimetric methods using organic solvents, CO2-based solvents, ionic liquids and switchable solvents, Nile red lipid visualization method, sulfo-phospho-vanillin method, and the thin-layer chromatography method. Each method has its own competitive advantages and disadvantages. For example, the organic solvents-based gravimetric method is mostly used and frequently employed as a reference standard to validate other methods, but it requires large amounts of samples and is time-consuming and expensive to recover solvents also with low selectivity towards desired products. The pretreatment approaches which aimed to disrupt cells and support subsequent lipid extraction through bead beating, microwave, ultrasonication, chemical methods, and enzymatic disruption are also introduced. Moreover, the principles and procedures for the production and quantification of fatty acids are finally described in detail, involving the preparation of fatty acid methyl esters and their quantification and composition analysis by gas chromatography.

Quantification of Caffeoylquinic Acids in Coffee Brews by HPLC-DAD

PubMed Central

Moeenfard, Marzieh; Rocha, Lígia; Alves, Arminda

2014-01-01

The influence of different brewing conditions on the concentration of the main caffeoylquinic acids (3-caffeoylquinic acid (3-CQA), 4-caffeoylquinic acid (4-CQA), and 5-caffeoylquinic acid (5-CQA)) was investigated. For this purpose, twenty-four coffee brews were extracted and analyzed using HPLC-DAD at 325 nm. Our findings demonstrate the great impact of brewing techniques on the caffeoylquinic acids (CQAs) content. The major isomer was 3-CQA, accounting for about 50% of the total CQAs, followed by 5-CQA and 4-CQA, accounting for about 24–36% for each one. The total content of CQAs was in the range of 45.79 to 1662.01 mg/L, found in iced cappuccino and pod espresso, respectively. In conclusion, this study demonstrates that coffee brews, in particular those prepared using pressurized methods, can be considered as the potential sources of antioxidants such as CQAs. PMID:25587489

Caffeoyl triterpenes from pear (Pyrus pyrifolia Nakai) fruit peels and their antioxidative activities against oxidation of rat blood plasma.

PubMed

Cho, Jeong-Yong; Kim, Chan Mi; Lee, Hyoung Jae; Lee, Sang-Hyun; Cho, Jeong-An; Kim, Wol-Soo; Park, Keun-Hyung; Moon, Jae-Hak

2013-05-15

Six triterpenes, including three caffeoyl triterpenes, were purified and isolated from pear fruit ( Pyrus pyrifolia Nakai cv. Chuwhangbae) peel extracts using various column chromatography techniques with a guided 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical-scavenging assay. The isolated compounds were identified as betulinic aldehyde (1), lupeol (2), betulinic acid (3), 3-O-cis-caffeoylbetulinic acid (4), 3-O-trans-caffeoylbetulinic acid (5), and 3-O-trans-caffeoyloleanolic acid (6) on the basis of nuclear magnetic resonance spectroscopy and electrospray ionization mass spectrometry. Four compounds (1, 4-6) were identified from Asian pear fruit for the first time. In addition, compounds 4-6, containing a caffeic acid moiety, showed higher DPPH radical-scavenging and suppression effects against copper ion-induced oxidation of rat blood plasma than other compounds without a caffeic acid moiety.

Comparison of Moringa Oleifera seeds oil characterization produced chemically and mechanically

NASA Astrophysics Data System (ADS)

Eman, N. A.; Muhamad, K. N. S.

2016-06-01

It is established that virtually every part of the Moringa oleifera tree (leaves, stem, bark, root, flowers, seeds, and seeds oil) are beneficial in some way with great benefits to human being. The tree is rich in proteins, vitamins, minerals. All Moringa oleifera food products have a very high nutritional value. They are eaten directly as food, as supplements, and as seasonings as well as fodder for animals. The purpose of this research is to investigate the effect of seeds particle size on oil extraction using chemical method (solvent extraction). Also, to compare Moringa oleifera seeds oil properties which are produced chemically (solvent extraction) and mechanically (mechanical press). The Moringa oleifera seeds were grinded, sieved, and the oil was extracted using soxhlet extraction technique with n-Hexane using three different size of sample (2mm, 1mm, and 500μm). The average oil yield was 36.1%, 40.80%, and 41.5% for 2mm, 1mm, and 500μm particle size, respectively. The properties of Moringa oleifera seeds oil were: density of 873 kg/m3, and 880 kg/m3, kinematic viscosity of 42.2mm2/s and 9.12mm2/s for the mechanical and chemical method, respectively. pH, cloud point and pour point were same for oil produced with both methods which is 6, 18°C and 12°C, respectively. For the fatty acids, the oleic acid is present with high percentage of 75.39%, and 73.60% from chemical and mechanical method, respectively. Other fatty acids are present as well in both samples which are (Gadoleic acid, Behenic acid, Palmitic acid) which are with lower percentage of 2.54%, 5.83%, and 5.73%, respectively in chemical method oil, while they present as 2.40%, 6.73%, and 6.04%, respectively in mechanical method oil. In conclusion, the results showed that both methods can produce oil with high quality. Moringa oleifera seeds oil appear to be an acceptable good source for oil rich in oleic acid which is equal to olive oil quality, that can be consumed in Malaysia where the olive oil is imported with high prices. In the same time cultivation of Moringa oleifera tree is considered to be a new source of income for the country and give more job opportunities.

Understanding Thermal Transport in Graded, Layered and Hybrid Materials

DTIC Science & Technology

2014-04-01

interfacial chemistries, including metallic and carbide layers, and; (iv) mimic the observed interface structure on a TDTR specimen by manipulating the...surface carbides , which were extracted from several different composites via acid dissolution of Cu, continued throughout the last 12 months of the...effort. The previously-reported electron probe microanalysis (EPMA) based techniques were employed to estimate the interfacial carbide layer thickness

Prehydrolysis of lignocellulose

DOEpatents

Torget, R.W.; Kadam, K.L.; Hsu, T.A.; Philippidis, G.P.; Wyman, C.E.

1998-01-06

The invention relates to the prehydrolysis of lignocellulose by passing an acidic or alkaline solution through solid lignocellulosic particles with removal of soluble components as they are formed. The technique permits a less severe combination of pH, temperature and time than conventional prehydrolysis. Furthermore, greater extraction of both hemicellulose and lignin occurs simultaneously in the same reactor and under the same conditions. 7 figs.

Prehydrolysis of lignocellulose

DOEpatents

Torget, R.W.; Kadam, K.L.; Hsu, T.A.; Philippidis, G.P.; Wyman, C.E.

1996-04-02

The invention relates to the prehydrolysis of lignocellulose by passing an acidic or alkaline solution through solid lignocellulosic particles with removal of soluble components as they are formed. The technique permits a less severe combination of pH, temperature and time than conventional prehydrolysis. Furthermore, greater extraction of both hemicellulose and lignin occurs simultaneously in the same reactor and under the same conditions. 7 figs.

Prehydrolysis of lignocellulose

DOEpatents

Torget, R.W.; Kadam, K.L.; Hsu, T.A.; Philippidis, G.P.; Wyman, C.E.

1995-06-13

The invention relates to the prehydrolysis of lignocellulose by passing an acidic or alkaline solution through solid lignocellulosic particles with removal of soluble components as they are formed. The technique permits a less severe combination of pH, temperature and time than conventional prehydrolysis. Furthermore, greater extraction of both hemicellulose and lignin occurs simultaneously in the same reactor and under the same conditions. 7 figs.

SEPARATION OF URANYL NITRATE BY EXTRACTION

DOEpatents

Stoughton, R.W.; Steahly, F.L.

1958-08-26

A process is presented for obtaining U/sup 233/ from solutions containing Pa/sup 233/. A carrier precipitate, such as MnO/sub 2/, is formed in such solutions and carries with it the Pa/sup 233/ present. This precipitate is then dissolved in nitric acid and the solution is aged to allow decay of the Pa/ sup 233/ into U/sup 233/. After a sufficient length of time the U/sup 233/ bearing solution is made 2.5 to 4.5 Molar in manganese nitrate by addition thereof, and the solution is then treated with ether to obtain uranyl nitrate by solvent extraction techniques.

Short-term monitoring of aridland lichen cover and biomass using photography and fatty acids

USGS Publications Warehouse

Bowker, M.A.; Johnson, N.C.; Belnap, J.; Koch, G.W.

2008-01-01

Biological soil crust (BSC) communities (composed of lichens, bryophytes, and cyanobacteria) may be more dynamic on short-time scales than previously thought, requiring new and informative short-term monitoring techniques. We used repeat digital photography and image analysis, which revealed a change in area of a dominant BSC lichen, Collema tenax. The data generated correlated well with gross photosynthesis (r=0.57) and carotenoid content (r=0.53), two variables that would be expected to be positively related to lichen area. We also extracted fatty acids from lichen samples and identified useful phospholipid fatty acid (PLFA) indicators for the Collema mycobiont (20:1, 15:0, 23:0), and the Collema photobiont (18:3??3). The 18:3??3 correlated well with chlorophyll a (r=0.66), a more traditional proxy for cyanobacterial biomass. We also compared total PLFA as a proxy for total Collema biomass with our photographically generated areal change data, and found them to be moderately correlated (r=0.44). Areal change proved to be responsive on short-time scales, while fatty acid techniques were information-rich, providing data on biomass of lichens, and both photo- and mycobionts separately, in addition to the physiological status of the mycobiont. Both techniques should be refined and tested in field situations. ?? 2007 Elsevier Ltd. All rights reserved.

Assessment of antioxidant capacities and phenolic contents of nigerian cultivars of onions (Allium cepa L) and garlic (Allium sativum L).

PubMed

Onyeoziri, Ukoha Pius; Romanus, Ekere Nwachukwu; Onyekachukwu, Uzodinma Irene

2016-07-01

This report assessed and compared the antioxidant potentials, quantities of ascorbic acid and phenolic compounds in methanolic extract of varieties of onions and garlic cultivars in Nigeria. The pH and total acidity of the extracts were equally determined. Antioxidancy of the cultivars were analysed using the in vitro assay techniques with 2,2-diphenyl-1-picryl Hydrazyl (DPPH) free radical scavenging and ferric reducing capacity. Ascorbic acid phenolic content were determined by volumetric and Folin-Ciocalteu's method respectively. The pH and total acidity were respectively 5.65 and 0.150mmol/L (red onion), 5.69 and 0.123mmol/L (white onion) and 6.94 and 0.105mmol/L (garlic). Red onion had the highest value of total phenols, ascorbic acid and free radical scavenging activity of 14.25±0.35mg GAE/ml, 229.098mg/100g, 66.44% respectively. In DPPH assay, red and white onion showed higher tendency to inhibit auto-oxidation when compared to garlic. The ferric reducing ability was greatest in garlic and least in white onions. These data indicate that with respect to antioxidant activity, red onion variety has highest health promoting potential among others.

Novel liquid chromatography-mass spectrometry method shows that vitamin E deficiency depletes arachidonic and docosahexaenoic acids in zebrafish (Danio rerio) embryos.

PubMed

Lebold, Katie M; Kirkwood, Jay S; Taylor, Alan W; Choi, Jaewoo; Barton, Carrie L; Miller, Galen W; La Du, Jane; Jump, Donald B; Stevens, Jan Frederik; Tanguay, Robert L; Traber, Maret G

2013-01-01

To test the hypothesis that embryogenesis depends upon α-tocopherol (E) to protect embryo polyunsaturated fatty acids (PUFAs) from lipid peroxidation, new methodologies were applied to measure α-tocopherol and fatty acids in extracts from saponified zebrafish embryos. A solid phase extraction method was developed to separate the analyte classes, using a mixed mode cartridge (reverse phase, π-π bonding, strong anion exchange), then α-tocopherol and cholesterol were measured using standard techniques, while the fatty acids were quantitated using a novel, reverse phase liquid chromatography-mass spectrometry (LC-MS) approach. We also determined if α-tocopherol status alters embryonic lipid peroxidation products by analyzing 24 different oxidized products of arachidonic or docosahexaenoic (DHA) acids in embryos using LC with hybrid quadrupole-time of flight MS. Adult zebrafish were fed E- or E+ diets for 4 months, and then were spawned to obtain E- and E+ embryos. Between 24 and 72 hours post-fertilization (hpf), arachidonic acid decreased 3-times faster in E- (21 pg/h) compared with E+ embryos (7 pg/h, P<0.0001), while both α-tocopherol and DHA concentrations decreased only in E- embryos. At 36 hpf, E- embryos contained double the 5-hydroxy-eicosatetraenoic acids and 7-hydroxy-DHA concentrations, while other hydroxy-lipids remained unchanged. Vitamin E deficiency during embryogenesis depleted DHA and arachidonic acid, and increased hydroxy-fatty acids derived from these PUFA, suggesting that α-tocopherol is necessary to protect these critical fatty acids.

Novel liquid chromatography–mass spectrometry method shows that vitamin E deficiency depletes arachidonic and docosahexaenoic acids in zebrafish (Danio rerio) embryos☆

PubMed Central

Lebold, Katie M.; Kirkwood, Jay S.; Taylor, Alan W.; Choi, Jaewoo; Barton, Carrie L.; Miller, Galen W.; Du, Jane La; Jump, Donald B.; Stevens, Jan Frederik; Tanguay, Robert L.; Traber, Maret G.

2013-01-01

To test the hypothesis that embryogenesis depends upon α-tocopherol (E) to protect embryo polyunsaturated fatty acids (PUFAs) from lipid peroxidation, new methodologies were applied to measure α-tocopherol and fatty acids in extracts from saponified zebrafish embryos. A solid phase extraction method was developed to separate the analyte classes, using a mixed mode cartridge (reverse phase, π–π bonding, strong anion exchange), then α-tocopherol and cholesterol were measured using standard techniques, while the fatty acids were quantitated using a novel, reverse phase liquid chromatography–mass spectrometry (LC–MS) approach. We also determined if α-tocopherol status alters embryonic lipid peroxidation products by analyzing 24 different oxidized products of arachidonic or docosahexaenoic (DHA) acids in embryos using LC with hybrid quadrupole-time of flight MS. Adult zebrafish were fed E− or E+ diets for 4 months, and then were spawned to obtain E− and E+ embryos. Between 24 and 72 hours post-fertilization (hpf), arachidonic acid decreased 3-times faster in E− (21 pg/h) compared with E+ embryos (7 pg/h, P<0.0001), while both α-tocopherol and DHA concentrations decreased only in E− embryos. At 36 hpf, E− embryos contained double the 5-hydroxy-eicosatetraenoic acids and 7-hydroxy-DHA concentrations, while other hydroxy-lipids remained unchanged. Vitamin E deficiency during embryogenesis depleted DHA and arachidonic acid, and increased hydroxy-fatty acids derived from these PUFA, suggesting that α-tocopherol is necessary to protect these critical fatty acids. PMID:24416717

Prevention of artificial dental plaque formation in vitro by plant extracts.

PubMed

Smullen, J; Finney, M; Storey, D M; Foster, H A

2012-10-01

A number of previous studies have shown that plant extracts can inhibit formation of dental plaque. The ability of extracts of Rosmarinus officianalis L., Salvia officianalis L., unfermented cocoa, red grape seed and green tea to inhibit plaque bacteria, glucosyltransferase activity, glucan and plaque formation in an in vitro model using bovine teeth was examined. The antimicrobial activity of the plant extracts against oral bacteria was determined using a standard susceptibility agar dilution technique. Inhibition of growth and acid production from glucose and sucrose by Streptococcus mutans in liquid culture was investigated. Prevention of plaque formation on bovine teeth initiated by Strep. mutans was studied using an artificial mouth. The plant extracts inhibited the growth of oral bacteria and prevented acid production by Strep. mutans. Extracts inhibited glucosyltransferase activity and glucan production and inhibited adhesion to glass. Extracts of R. officianalis L. and S. officianalis L. at 0·25 mg ml(-1) reduced plaque growth by >80%. Green tea extract completely inhibited plaque formation but resulted in a greenish discolouration of the teeth which could not be removed by scrubbing. The plant extracts, particularly those from R. officianalis L. and S. officianalis L., inhibited glucosyltranferase activity, glucan production and plaque formation in vitro. The results suggest that the extracts of R. officianalis L. and S. officianalis L. may be useful as antiplaque agents in foods and dental preparations. Bovine teeth can be used as an alternative to hydroxyapatite for studies of plaque formation, but they need to be carefully sterilized before use. © 2012 The Authors Journal of Applied Microbiology © 2012 The Society for Applied Microbiology.

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.

Nuclear magnetic resonance and high-performance liquid chromatography techniques for the characterization of bioactive compounds from Humulus lupulus L. (hop).

PubMed

Bertelli, Davide; Brighenti, Virginia; Marchetti, Lucia; Reik, Anna; Pellati, Federica

2018-06-01

Humulus lupulus L. (hop) represents one of the most cultivated crops, it being a key ingredient in the brewing process. Many health-related properties have been described for hop extracts, making this plant gain more interest in the field of pharmaceutical and nutraceutical research. Among the analytical tools available for the phytochemical characterization of plant extracts, quantitative nuclear magnetic resonance (qNMR) represents a new and powerful technique. In this ambit, the present study was aimed at the development of a new, simple, and efficient qNMR method for the metabolite fingerprinting of bioactive compounds in hop cones, taking advantage of the novel ERETIC 2 tool. To the best of our knowledge, this is the first attempt to apply this method to complex matrices of natural origin, such as hop extracts. The qNMR method set up in this study was applied to the quantification of both prenylflavonoids and bitter acids in eight hop cultivars. The performance of this analytical method was compared with that of HPLC-UV/DAD, which represents the most frequently used technique in the field of natural product analysis. The quantitative data obtained for hop samples by means of the two aforementioned techniques highlighted that the amount of bioactive compounds was slightly higher when qNMR was applied, although the order of magnitude of the values was the same. The accuracy of qNMR was comparable to that of the chromatographic method, thus proving to be a reliable tool for the analysis of these secondary metabolites in hop extracts. Graphical abstract Graphical abstract related to the extraction and analytical methods applied in this work for the analysis of bioactive compounds in Humulus lupulus L. (hop) cones.

Bioavailability study of a polyphenol-enriched extract from Hibiscus sabdariffa in rats and associated antioxidant status.

PubMed

Fernández-Arroyo, Salvador; Herranz-López, María; Beltrán-Debón, Raúl; Borrás-Linares, Isabel; Barrajón-Catalán, Enrique; Joven, Jorge; Fernández-Gutiérrez, Alberto; Segura-Carretero, Antonio; Micol, Vicente

2012-10-01

The aqueous extracts of Hibiscus sabdariffa have been commonly used in folk medicine. Nevertheless, the compounds or metabolites responsible for its healthy effects have not yet been identified. The major metabolites present in rat plasma after acute ingestion of a polyphenol-enriched Hibiscus sabdariffa extract were characterized and quantified in order to study their bioavailability. The antioxidant status of the plasma samples was also measured through several complementary antioxidant techniques. High-performance liquid chromatography coupled to time-of-flight mass spectrometry (HPLC-ESI-TOF-MS) was used for the bioavailability study. The antioxidant status was measured by ferric reducing ability of plasma method, thiobarbituric acid reactive substances assay, and superoxide dismutase activity assay. Seventeen polyphenols and metabolites have been detected and quantified. Eleven of these compounds were metabolites. Although phenolic acids were found in plasma without any modification in their structures, most flavonols were found as quercetin or kaempferol glucuronide conjugates. Flavonol glucuronide conjugates, which show longer half-life elimination values, are proposed to contribute to the observed lipid peroxidation inhibitory activity in the cellular membranes. By contrast, phenolic acids appear to exert their antioxidant activity through ferric ion reduction and superoxide scavenging at shorter times. We propose that flavonol-conjugated forms (quercetin and kaempferol) may be the compounds responsible for the observed antioxidant effects and contribute to the healthy effects of H. sabdariffa polyphenolic extract. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Lipid composition in a strain of Bacillus subtilis, a producer of iturin A lipopeptides that are active against uropathogenic bacteria.

PubMed

Bernat, Przemysław; Paraszkiewicz, Katarzyna; Siewiera, Paulina; Moryl, Magdalena; Płaza, Grażyna; Chojniak, Joanna

2016-10-01

Urinary tract infections are a common disease in humans. Therefore, new methods are needed to destroy biofilms that are formed by uropathogens. Iturin A lipopeptides (LPs) C14 and C15 are potent biosurfactants synthetized by the Bacillus subtilis I'1a strain. The biological activity of extracted LPs was confirmed by examining extracts from I'1a cultures against uropathogenic bacteria that had been isolated from biofilms on urinary catheters. Compared with cultures of DSM 3257, which produce surfactin at a relatively low level, the extract obtained from strain I'1a exhibited a greater inhibitory effect against both planktonic and sessile forms of Escherichia coli, Serratia marcescens, Enterobacter cloacae, Proteus mirabilis, Citrobacter freundii and Enterococcus faecalis. Moreover, cyclic LP biosurfactants may disturb the integrity of cytoplasmic membranes; therefore, we investigated the effects of synthetized LPs on fatty acids and phospholipids of B. subtilis. LPs and lipids were analyzed using GC-MS, LC-MS/MS and MALDI-TOF/TOF techniques. Compared with B. subtilis DSM 3257, membranes of the I'1a strain were characterized by an increased amount of anteiso fatty acids and a ten-fold higher ratio of phosphatidylglycerol (PG)-to-phosphatidylethanolamine (PE). Interestingly, in cultures of B. subtilis DSM 3257 supplemented with LP extracts of the I'1a strain, the PG-to-PE ratio was fourfold higher, and the amount of anteiso fatty acids was also increased.

Secondary metabolites isolation in natural products chemistry: comparison of two semipreparative chromatographic techniques (high pressure liquid chromatography and high performance thin-layer chromatography).

PubMed

Do, Thi Kieu Tiên; Hadji-Minaglou, Francis; Antoniotti, Sylvain; Fernandez, Xavier

2014-01-17

Chemical investigations on secondary metabolites in natural products chemistry require efficient isolation techniques for characterization purpose as well as for the evaluation of their biological properties. In the case of phytochemical studies, the performance of the techniques is critical (resolution and yield) since the products generally present a narrow range of polarity and physicochemical properties. Several techniques are currently available, but HPLC (preparative and semipreparative) is the most widely used. To compare the performance of semipreparative HPLC and HPTLC for the isolation of secondary metabolites in different types of extracts, we have chosen carvone from spearmint essential oil (Mentha spicata L.), resveratrol from Fallopia multiflora (Thunb.) Haraldson, and rosmarinic acid from rosemary (Rosmarinus officinalis L.) extracts. The comparison was based on the chromatographic separation, the purity and quantity of isolated compounds, the solvent consumption, the duration and the cost of the isolation operations. The results showed that semipreparative HPTLC can in some case offer some advantages over conventional semipreparative HPLC. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Metabolite profiling of Clinacanthus nutans leaves extracts obtained from different drying methods by 1H NMR-based metabolomics

NASA Astrophysics Data System (ADS)

Hashim, Noor Haslinda Noor; Latip, Jalifah; Khatib, Alfi

2016-11-01

The metabolites of Clinacanthus nutans leaves extracts and their dependence on drying process were systematically characterized using 1H nuclear magnetic resonance spectroscopy (NMR) multivariate data analysis. Principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA) were able to distinguish the leaves extracts obtained from different drying methods. The identified metabolites were carbohydrates, amino acid, flavonoids and sulfur glucoside compounds. The major metabolites responsible for the separation in PLS-DA loading plots were lupeol, cycloclinacosides, betulin, cerebrosides and choline. The results showed that the combination of 1H NMR spectroscopy and multivariate data analyses could act as an efficient technique to understand the C. nutans composition and its variation.

Evaluation of Thymus vulgaris plant extract as an eco-friendly corrosion inhibitor for stainless steel 304 in acidic solution by means of electrochemical impedance spectroscopy, electrochemical noise analysis and density functional theory.

PubMed

Ehsani, A; Mahjani, M G; Hosseini, M; Safari, R; Moshrefi, R; Mohammad Shiri, H

2017-03-15

Inhibition performance of Thymus vulgaris plant leaves extract (thyme) as environmentally friendly (green) inhibitor for the corrosion protection of stainless steel (SS) type 304 in 1.0molL -1 HCl solution was studied by potentiodynamic polarization, electrochemical impedance (EIS) and electrochemical noise measurements (EN) techniques. The EN data were analyzed with FFT technique to make the spectral power density plots. The calculations were performed by MATLAB 2014a software. Geometry optimization and calculation of the structural and electronic properties of the molecular system of inhibitor have been carried out using UB3LYP/6-311++G ∗∗ level. Moreover, the results obtained from electrochemical noise analysis were compared with potentiodynamic polarization and electrochemical impedance spectroscopy. All of the used techniques showed positive effect of green inhibitor with increasing inhibitor concentration. Copyright © 2016 Elsevier Inc. All rights reserved.

A highly selective dispersive liquid-liquid microextraction approach based on the unique fluorous affinity for the extraction and detection of per- and polyfluoroalkyl substances coupled with high performance liquid chromatography tandem-mass spectrometry.

PubMed

Wang, Juan; Shi, Yali; Cai, Yaqi

2018-04-06

In the present study, a highly selective fluorous affinity-based dispersive liquid-liquid microextraction (DLLME) technique was developed for the extraction and analysis of per- and polyfluoroalkyl substances (PFASs) followed by high performance liquid chromatography tandem-mass spectrometry. Perfluoro-tert-butanol with multiple C-F bonds was chosen as the extraction solvent, which was injected into the aqueous samples with a dispersive solvent (acetonitrile) in a 120:800 (μL, v/v) mixture for PFASs enrichment. The fluorous affinity-based extraction mechanism was confirmed by the significantly higher extraction recoveries for PFASs containing multiple fluorine atoms than those for compounds with fewer or no fluorine atoms. The extraction recoveries of medium and long-chain PFASs (CF 2  > 5) exceeded 70%, except perfluoroheptanoic acid, while those of short-chain PFASs were lower than 50%, implying that the proposed DLLME may not be suitable for their extraction due to weak fluorous affinity. This highly fluoroselective DLLME technique can greatly decrease the matrix effect that occurs in mass spectrometry detection when applied to the analysis of urine samples. Under the optimum conditions, the relative recoveries of PFASs with CF 2  > 5 ranged from 80.6-121.4% for tap water, river water and urine samples spiked with concentrations of 10, 50 and 100 ng/L. The method limits of quantification for PFASs in water and urine samples were in the range of 0.6-8.7 ng/L. Furthermore, comparable concentrations of PFASs were obtained via DLLME and solid-phase extraction, confirming that the developed DLLME technique is a promising method for the extraction of PFASs in real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Unequivocal glycyrrhizin isomer determination and comparative in vitro bioactivities of root extracts in four Glycyrrhiza species

PubMed Central

Farag, Mohamed A.; Porzel, Andrea; Wessjohann, Ludger A.

2014-01-01

Glycyrrhiza glabra, commonly known as licorice, is a popular herbal supplement used for the treatment of chronic inflammatory conditions and as sweetener in the food industry. This species contains a myriad of phytochemicals including the major saponin glycoside glycyrrhizin (G) of Glycyrrhetinic acid (GA) aglycone. In this study, 2D-ROESY NMR technique was successfully applied for distinguishing 18α and 18β glycyrrhetinic acid (GA). ROESY spectra acquired from G. glabra, Glycyrrhiza uralensis and Glycyrrhiza inflata crude extracts revealed the presence of G in its β-form. Anti-inflammatory activity of four Glycyrrhiza species, G, glabra, G. uralensis, G. inflata, and G. echinata roots was assessed against COX-1 inhibition revealing that phenolics rather than glycyrrhizin are biologically active in this assay. G. inflata exhibits a strong cytotoxic effect against PC3 and HT29 cells lines, whereas other species are inactive. This study presents an effective NMR method for G isomer assignment in licorice extracts that does not require any preliminary chromatography or any other purification step. PMID:25685548

Comprehensive Characterization of Extractable and Nonextractable Phenolic Compounds by High-Performance Liquid Chromatography-Electrospray Ionization-Quadrupole Time-of-Flight of a Grape/Pomegranate Pomace Dietary Supplement.

PubMed

Pérez-Ramírez, Iza F; Reynoso-Camacho, Rosalía; Saura-Calixto, Fulgencio; Pérez-Jiménez, Jara

2018-01-24

Grape and pomegranate are rich sources of phenolic compounds, and their derived products could be used as ingredients for the development of functional foods and dietary supplements. However, the profile of nonextractable or macromolecular phenolic compounds in these samples has not been evaluated. Here, we show a comprehensive characterization of extractable and nonextractable phenolic compounds of a grape/pomegranate pomace dietary supplement using high-performance liquid chromatography-electrospray ionization-quadrupole time-of-flight (HPLC-ESI-QTOF) and matrix-assisted laser desorption/ionization (MALDI)-TOF techniques. The main extractable phenolic compounds were several anthocyanins (principally malvidin 3-O-glucoside) as well as gallotannins and gallagyl derivatives; some phenolic compounds were reported in grape or pomegranate for the first time. Additionally, there was a high proportion of nonextractable phenolic compounds, including vanillic acid, and dihydroxybenzoic acid. Unidentified polymeric structures were detected by MALDI-TOF MS analysis. This study shows that mixed grape and pomegranate pomaces are a source of different classes of phenolic compounds including a high proportion of nonextractable phenolic compounds.

Cholinesterase inhibitory triterpenoids from the bark of Garcinia hombroniana.

PubMed

Jamila, Nargis; Khairuddean, Melati; Yeong, Khaw Kooi; Osman, Hasnah; Murugaiyah, Vikneswaran

2015-02-01

Context: Garcinia hombroniana Pierre, known as manggis hutan in Malaysia is a rich source of xanthones and benzophenones. This study was aimed to isolate and characterize potential cholinesterase inhibitors from the extracts of G. hombroniana bark and investigate their interactions with the enzymes. The dichloromethane extract afforded five triterpenoids which were characterized by NMR and mass spectral techniques. Cholinesterase inhibitory assay and molecular docking were performed to get insight of the inhibitory activity and molecular interactions of the compounds. The compounds were also tested for their antioxidant capacity. The isolated triterpenoids were identified as: 2β-hydroxy-3α-O-caffeoyltaraxar-14-en-28-oic acid (1), taraxerol (2), taraxerone (3), betulin (4) and betulinic acid (5). Compound 1 was the most active dual inhibitor of both AChE and BChE. Compound 1 also showed good antioxidant activities. Compound 1 had dual and moderate inhibitory activity on AChE and BChE worthy for further investigations.

Determination of perfluorinated alkyl acids in corn, popcorn and popcorn bags before and after cooking by focused ultrasound solid-liquid extraction, liquid chromatography and quadrupole-time of flight mass spectrometry.

PubMed

Moreta, Cristina; Tena, María Teresa

2014-08-15

An analytical method is proposed to determine ten perfluorinated alkyl acids (PFAAs) [nine perfluorocarboxylic acids (PFCAs) and perfluorooctane sulfonate (PFOS)] in corn, popcorn and microwave popcorn packaging by focused ultrasound solid-liquid extraction (FUSLE) and ultra high performance liquid chromatography (UHPLC) coupled to quadrupole-time of flight mass spectrometry (QTOF-MS/MS). Selected PFAAs were extracted efficiently in only one 10-s cycle by FUSLE, a simple, safe and inexpensive technique. The developed method was validated for microwave popcorn bags matrix as well as corn and popcorn matrices in terms of linearity, matrix effect error, detection and quantification limits, repeatability and recovery values. The method showed good accuracy with recovery values around 100% except for the lowest chain length PFAAs, satisfactory reproducibility with RSDs under 16%, and sensitivity with limits of detection in the order of hundreds picograms per gram of sample (between 0.2 and 0.7ng/g). This method was also applied to the analysis of six microwave popcorn bags and the popcorn inside before and after cooking. PFCAs contents between 3.50ng/g and 750ng/g were found in bags, being PFHxA (perfluorohexanoic acid) the most abundant of them. However, no PFAAs were detected either corn or popcorn, therefore no migration was assumed. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Demonstration of in situ product recovery of butyric acid via CO2 -facilitated pH swings and medium development in two-phase partitioning bioreactors.

PubMed

Peterson, Eric C; Daugulis, Andrew J

2014-03-01

Production of organic acids in solid-liquid two-phase partitioning bioreactors (TPPBs) is challenging, and highly pH-dependent, as cell growth occurs near neutral pH, while acid sorption occurs only at low pH conditions. CO2 sparging was used to achieve acidic pH swings, facilitating undissociated organic acid uptake without generating osmotic stress inherent in traditional acid/base pH control. A modified cultivation medium was formulated to permit greater pH reduction by CO2 sparging (pH 4.8) compared to typical media (pH 5.3), while still possessing adequate nutrients for extensive cell growth. In situ product recovery (ISPR) of butyric acid (pKa = 4.8) produced by Clostridium tyrobutyricum was achieved through intermittent CO2 sparging while recycling reactor contents through a column packed with absorptive polymer Hytrel® 3078. This polymer was selected on the basis of its composition as a polyether copolymer, and the use of solubility parameters for predicting solute polymer affinity, and was found to have a partition coefficient for butyric acid of 3. Total polymeric extraction of 3.2 g butyric acid with no CO2 mediated pH swings was increased to 4.5 g via CO2 -facilitated pH shifting, despite the buffering capacity of butyric acid, which resists pH shifting. This work shows that CO2 -mediated pH swings have an observable positive effect on organic acid extraction, with improvements well over 150% under optimal conditions in early stage fermentation compared to CO2 -free controls, and this technique can be applied other organic acid fermentations to achieve or improve ISPR. © 2013 Wiley Periodicals, Inc.

Recovery correction technique for NMR spectroscopy of perchloric acid extracts using DL-valine-2,3-d2: validation and application to 5-fluorouracil-induced brain damage.

PubMed

Nakagami, Ryutaro; Yamaguchi, Masayuki; Ezawa, Kenji; Kimura, Sadaaki; Hamamichi, Shusei; Sekine, Norio; Furukawa, Akira; Niitsu, Mamoru; Fujii, Hirofumi

2014-01-01

We explored a recovery correction technique that can correct metabolite loss during perchloric acid (PCA) extraction and minimize inter-assay variance in quantitative (1)H nuclear magnetic resonance (NMR) spectroscopy of the brain and evaluated its efficacy in 5-fluorouracil (5-FU)- and saline-administered rats. We measured the recovery of creatine and dl-valine-2,3-d2 from PCA extract containing both compounds (0.5 to 8 mM). We intravenously administered either 5-FU for 4 days (total, 100 mg/kg body weight) or saline into 2 groups of 11 rats each. We subsequently performed PCA extraction of the whole brain on Day 9, externally adding 7 µmol of dl-valine-2,3-d2. We estimated metabolite concentrations using an NMR spectrometer with recovery correction, correcting metabolite concentrations based on the recovery factor of dl-valine-2,3-d2. For each metabolite concentration, we calculated the coefficient of variation (CEV) and compared differences between the 2 groups using unpaired t-test. Equivalent recoveries of dl-valine-2,3-d2 (89.4 ± 3.9%) and creatine (89.7 ± 3.9%) in the PCA extract of the mixed solution indicated the suitability of dl-valine-2,3-d2 as an internal reference. In the rat study, recovery of dl-valine-2,3-d2 was 90.6 ± 9.2%. Nine major metabolite concentrations adjusted by recovery of dl-valine-2,3-d2 in saline-administered rats were comparable to data in the literature. CEVs of these metabolites were reduced from 10 to 17% before to 7 to 16% after correction. The significance of differences in alanine and taurine between the 5-FU- and saline-administered groups was determined only after recovery correction (0.75 ± 0.12 versus 0.86 ± 0.07 for alanine; 5.17 ± 0.59 versus 5.66 ± 0.42 for taurine [µmol/g brain tissue]; P < 0.05). A new recovery correction technique corrected metabolite loss during PCA extraction, minimized inter-assay variance in quantitative (1)H NMR spectroscopy of brain tissue, and effectively detected inter-group differences in concentrations of brain metabolites between 5-FU- and saline-administered rats.

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.

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

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

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

1995-12-31

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

Characterization of bacterial diversity in an atrazine degrading enrichment culture and degradation of atrazine, cyanuric acid and biuret in industrial wastewater.

PubMed

Dutta, Anirban; Vasudevan, Venugopal; Nain, Lata; Singh, Neera

2016-01-01

An enrichment culture was used to study atrazine degradation in mineral salt medium (MSM) (T1), MSM+soil extract (1:1, v/v) (T2) and soil extract (T3). Results suggested that enrichment culture required soil extract to degrade atrazine, as after second sequential transfer only partial atrazine degradation was observed in T1 treatment while atrazine was completely degraded in T2 and T3 treatments even after fourth transfer. Culture independent polymerase chain reaction-denaturing gradient gel electrophoresis (PCR-DGGE) technique confirmed selective enrichment of genus Bacillus along with Pseudomonas and Burkholderia. Degradation of atrazine/metabolites in the industrial wastewater was studied at different initial concentrations of the contaminants [wastewater-water (v/v) ratio: T1, 1:9; T2, 2:8; T3, 3:7; T4, 5:5 and T5, undiluted effluent]. The initial concentrations of atrazine, cyanuric acid and biuret ranged between 5.32 and 53.92 µg mL(-1), 265.6 and 1805.2 µg mL(-1) and 1.85 and 16.12 µg mL(-1), respectively. The enrichment culture was able to completely degrade atrazine, cyanuric acid and biuret up to T4 treatment, while no appreciable degradation of contaminants was observed in the undiluted effluent (T5). Inability of enrichment culture to degrade atrazine/metabolites might be due to high concentrations of cyanuric acid. Therefore, a separate study on cyanuric acid degradation suggested: (i) no appreciable cyanuric acid degradation with accumulation of an unidentified metabolite in the medium where cyanuric acid was supplemented as the sole source of carbon and nitrogen; (ii) partial cyanuric acid degradation with accumulation of unidentified metabolite in the medium containing additional nitrogen source; and (iii) complete cyanuric acid degradation in the medium supplemented with an additional carbon source. This unidentified metabolite observed during cyanuric acid degradation and also detected in the enrichment culture inoculated wastewater samples, however, was degraded up to T4 treatments and was persistent in the T5 treatment. Probably, accumulation of this metabolite inhibited atrazine/cyanuric acid degradation by the enrichment culture in undiluted wastewater.

Chemical composition and antioxidant capacities of phytococktail extracts from trans-Himalayan cold desert

PubMed Central

2013-01-01

Background Himalayan plants are widely used in traditional system of medicine both as prophylactics and therapeutics for high altitude maladies. Our aim was to evaluate the antioxidant capacities and bioactive compounds of methanol and n-hexane extracts of the phytococktail comprising of sea buckthorn (Hippophae rhamnoides), apricot (Prunus armeniaca) and roseroot (Rhodiola imbricata) from trans-Himalaya. Methods The 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS) and nitric oxide (NO) radical scavenging capacities and lipid peroxidation inhibition (LPI) property of the extracts were determined. Total antioxidant power was determined by ferric reducing/antioxidant power (FRAP) assay. Total polyphenol, flavonoid, flavonol, proanthocyanidin and carotenoid were also estimated for both extracts. We have identified and quantified the phyto-chemotypes present in the methanol and n-hexane extracts by hyphenated gas chromatography/mass spectrometry (GC/MS) technique. Results Antioxidant capacity assays using DPPH, ABTS, NO, LPI and FRAP exhibited analogous results where the phytococktail showed high antioxidant action. The phytococktail was also found to possess high quantity of total polyphenol, flavonoid, flavonol and carotenoid. A significant and linear correlation was found between the antioxidant capacities and bioactive principles. A total of 32 phyto-chemotypes were identified from these extracts by GC/MS chemometric fingerprinting. Major phyto-chemotypes identified by GC/MS were glycosides, phenylpropanoids and derivatives, terpenoids, alkaloids, phytosterols, fatty acids and esters, alkaloids and derivatives, organic acid esters and aromatic ethers with positive biological and pharmacological actions. Conclusion The phytococktail extracts were found to contain considerable amount of diverse bioactive compounds with high antioxidant capacities. The presence of hydrophilic and lipophilic antioxidants in the phytococktail could have contributed to the higher antioxidant values. Hence, the phytococktail could be used as natural source of antioxidants to ameliorate disorders associated with oxidative stress. PMID:24098968

Remediation of lead-contaminated soils

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

Peters, R.W.; Shem, L.

1992-01-01

Excavation and transport of soil contaminated with heavy metals has generally been the standard remediation technique for treatment of heavy-metal-contaminated soils. This approach is not a permanent solution; moreover, off-site shipment and disposal of contaminated soil involves high expense, liability, and appropriate regulatory approval. Recently, a number of other techniques have been investigated for treating such contaminated sites, including flotation, solidification/stabilization, vitrification, and chemical extraction. This paper reports the results of a laboratory investigation determining the efficiency of using chelating agents to extract lead from contaminated soils. Lead concentrations in the soils ranged from 500 to 10,000 mg/kg. Ethylenediaminetetraacetic acidmore » (EDTA) and nitrilotriacetic acid (NTA) were examined for their potential extractive capabilities. Concentrations of the chelating agents ranged from 0.01 to 0.10 M. The pH of the suspensions in which the extractions were performed ranged from 4 to 12. Results showed that the removal of lead using NTA and water was ph-dependent, whereas the removal of lead using EDTA was ph-insensitive. Maximum removals of lead were 68.7%,19.1%, and 7.3% using EDTA, NTA, and water, respectively (as compared with initial lead concentrations).« less

Remediation of lead-contaminated soils

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

Peters, R.W.; Shem, L.

1992-09-01

Excavation and transport of soil contaminated with heavy metals has generally been the standard remediation technique for treatment of heavy-metal-contaminated soils. This approach is not a permanent solution; moreover, off-site shipment and disposal of contaminated soil involves high expense, liability, and appropriate regulatory approval. Recently, a number of other techniques have been investigated for treating such contaminated sites, including flotation, solidification/stabilization, vitrification, and chemical extraction. This paper reports the results of a laboratory investigation determining the efficiency of using chelating agents to extract lead from contaminated soils. Lead concentrations in the soils ranged from 500 to 10,000 mg/kg. Ethylenediaminetetraacetic acidmore » (EDTA) and nitrilotriacetic acid (NTA) were examined for their potential extractive capabilities. Concentrations of the chelating agents ranged from 0.01 to 0.10 M. The pH of the suspensions in which the extractions were performed ranged from 4 to 12. Results showed that the removal of lead using NTA and water was ph-dependent, whereas the removal of lead using EDTA was ph-insensitive. Maximum removals of lead were 68.7%,19.1%, and 7.3% using EDTA, NTA, and water, respectively (as compared with initial lead concentrations).« less

Rapid characterization of chlorogenic acids in Duhaldea nervosa based on ultra-high-performance liquid chromatography-linear trap quadropole-Orbitrap-mass spectrometry and mass spectral trees similarity filter technique.

PubMed

Liu, Lianghong; Zhang, Jiayu; Zheng, Binjie; Guan, Ying; Wang, Liting; Chen, Lei; Cai, Wei

2018-04-01

Duhaldea nervosa (Wallich ex Candolle) A. Anderberg has been traditionally used as a food spice and also in folk medicine for treating traumatic injury and relieving rheumatism, especially accelerating the healing of a fracture. However, so far as we are aware, the chemical constituents have not been fully investigated. In this study, a practical method of mass spectral trees similarity filter, a data-mining technique, was developed and evaluated for the rapid detection and identification complicated constituents based on ultra-high-performance liquid chromatography-linear trap quadropole-Orbitrap-mass spectrometry. Finally, a total of 47 chlorogenic acids, including 19 monoacyl-quinic acids, 22 diacyl-quinic acids, and six triacyl-quinic acids, were unambiguously or tentatively identified based on their accurate mass measurement, chromatographic retention, MS n spectra, and bibliography data. To our best knowledge, it is the first time to report the chlorogenic acids of D. nervosa, which would be beneficial for the further material basis and quality research. Meanwhile, this mass spectral trees similarity filter method could be envisioned to exhibit a wide application for the identification of complicated components from botanical extracts. © 2018 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.

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.

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.

Effect of Gibberellic Acid on the Plasticity and Elasticity of Avena Stem Segments 1

PubMed Central

Adams, Paul A.; Montague, Michael J.; Tepfer, Mark; Rayle, David L.; Ikuma, Hiroshi; Kaufman, Peter B.

1975-01-01

Extensibility characteristics of Avena stem segments treated with gibberellic acid (GA) were investigated in living internodes using a microgrowth method and in partially extracted cell walls subjected to Instron extensometer analysis. Both techniques showed that treatment with GA greatly increases internodal plasticity, but has virtually no effect on internodal elasticity. The increase in plasticity occurred 1 to 2 hours after the initiation of hormone treatment, which is similar to the time of onset of GA-enhanced growth and cell wall synthesis. Cycloheximide was shown to inhibit the effect of GA on plasticity. PMID:16659388

Isoelectric focusing of proteins and peptides

NASA Technical Reports Server (NTRS)

Egen, N.

1979-01-01

Egg-white solution was chosen as the reference solution in order to assess the effects of operational parameters (voltage, flow rate, ampholine pH range and concentration, and protein concentration) of the RIEF apparatus on protein resolution. Topics of discussion include: (1) comparison of RIEF apparatus to conventional IEF techniques (column and PAG) with respect to resolution and throughput; (2) peptide and protein separation (AHF, Thymosin - Fraction 5, vasoactive peptide, L-asparaginase and ACP); and (3) detection of peptides - dansyl derivatives of amino acids and peptides, post-focusing fluorescent labeling of amino acids, peptides and proteins, and ampholine extraction from focused gels.

Temporal Variations of Organic Acids in Sumac Fruit

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

Robbins, C.; Mulcahy, F.; Somayajula, K.

2006-10-01

Extracts from staghorn sumac (Rhus typhina) fruits were obtained from fresh fruits obtained from June to October in two successive years. Total acidity, pH, and concentrations of malic and succinic acids determined using liquid chromatography were measured for each extract. Acidity and acid concentrations reached their maxima in late July, and declined slowly thereafter. Malic and succinic acid concentrations in the extracts reached maxima of about 4 and 0.2% (expressed per unit weight of fruit), respectively. Malic and succinic acids were the only organic acids observed in the extracts, and mass balance determinations indicate that these acids are most likelymore » the only ones present in appreciable amounts.« less

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

Classification of bacteria by simultaneous methylation-solid phase microextraction and gas chromatography/mass spectrometry analysis of fatty acid methyl esters.

PubMed

Lu, Yao; Harrington, Peter B

2010-08-01

Direct methylation and solid-phase microextraction (SPME) were used as a sample preparation technique for classification of bacteria based on fatty acid methyl ester (FAME) profiles. Methanolic tetramethylammonium hydroxide was applied as a dual-function reagent to saponify and derivatize whole-cell bacterial fatty acids into FAMEs in one step, and SPME was used to extract the bacterial FAMEs from the headspace. Compared with traditional alkaline saponification and sample preparation using liquid-liquid extraction, the method presented in this work avoids using comparatively large amounts of inorganic and organic solvents and greatly decreases the sample preparation time as well. Characteristic gas chromatography/mass spectrometry (GC/MS) of FAME profiles was achieved for six bacterial species. The difference between Gram-positive and Gram-negative bacteria was clearly visualized with the application of principal component analysis of the GC/MS data of bacterial FAMEs. A cross-validation study using ten bootstrap Latin partitions and the fuzzy rule building expert system demonstrated 87 +/- 3% correct classification efficiency.

Induction of apoptosis against cancer cell lines by four ascomycetes (endophytes) from Malaysian rainforest.

PubMed

Hazalin, Nurul Aqmar Mohamad Nor; Ramasamy, Kalavathy; Lim, Siong Meng; Cole, Anthony L J; Majeed, Abu Bakar Abdul

2012-05-15

Endophytic fungi have been shown to be a promising source of biologically active natural products. In the present study, extracts of four endophytic fungi isolated from plants of the National Park, Pahang were evaluated for their cytotoxic activity and the nature of their active compounds determined. Those extracts exhibiting activity with IC(50) values less than 17 μg/ml against HCT116, MCF-7 and K562 cell lines were shown to induce apoptosis in these cell lines. Molecular analysis, based on sequences of the rDNA internal transcribed spacers ITS1 and ITS4, revealed all four endophytic fungi to be ascomycetes: three sordariomycetes and a dothideomycete. Six known compounds, cytochalasin J, dechlorogriseofulvin, demethylharzianic-acid, griseofulvin, harzianic acid and 2-hexylidene-3-methyl-succinic acid were identified from a rapid dereplication technique for fungal metabolites using an in-house UV library. The results from the present study suggest the potential of endophytic fungi as cytotoxic agents, and there is an indication that the isolates contain bioactive compounds that mainly kill cancer cells by apoptosis. Copyright © 2012 Elsevier GmbH. All rights reserved.

Biosynthesis, characterization and enzymatic transesterification of single cell oil of Mucor circinelloides--a sustainable pathway for biofuel production.

PubMed

Carvalho, Ana K F; Rivaldi, Juan D; Barbosa, Jayne C; de Castro, Heizir F

2015-04-01

The filamentous fungus Mucor circinelloides URM 4182 was tested to determine its ability to produce single-cell oil suitable for obtaining biodiesel. Cell growth and lipid accumulation were investigated in a medium containing glucose as the main carbon source. A microwave-assisted ethanol extraction technique (microwave power ⩽200 W, 50-60 °C) was established and applied to lipid extraction from the fungal hyphae to obtain high lipid concentration (44%wt) of the dry biomass, which was considerably higher than the quantity obtained by classical solvent methods. The lipid profile showed a considerable amount of oleic acid (39.3%wt), palmitic acid (22.2%wt) and γ-linoleic acid (10.8%wt). Biodiesel was produced by transesterification of the single-cell oil with ethanol using a immobilized lipase from Candida antarctica (Novozym® 435) as the catalyst. (1)H NMR and HPLC analyses confirmed conversion of 93% of the single-cell oil from M. circinelloides into ethyl esters (FAEE). Copyright © 2015 Elsevier Ltd. All rights reserved.

Tabletted microspheres containing Cynara scolymus (var. Spinoso sardo) extract for the preparation of controlled release nutraceutical matrices.

PubMed

Gavini, E; Alamanni, M C; Cossu, M; Giunchedi, P

2005-08-01

Controlled release dosage forms based on tabletted microspheres containing fresh artichoke Cynara scolymus extract were performed for the oral administration of a nutritional supplement. Microspheres were prepared using a spray-drying technique; lactose or hypromellose have been chosen as excipients. Microspheres were characterized in terms of encapsulated extract content, size and morphology. Qualitative and quantitative composition of the extract before and after the spray process was determined. Compressed matrices (tablets) were prepared by direct compression of the spray-dried microspheres. In vitro release tests of microparticles and tablets prepared were carried out in both acidic and neutral media. Spray-drying is a good method to prepare microspheres containing the artichoke extract. The microspheres encapsulate an amount of extract close to the theoretical value. Particle size analyses indicate that the microparticles have dvs of approximately 6-7 microm. Electronic microscopy observations reveal that particles based on lactose have spherical shape and particles containing hypromellose are almost collapsed. The hydroalcoholic extract is stable to the microsphere production process: its polyphenolic composition (qualitative and quantitative) did not change after spraying. In vitro release studies show that microparticles characterized by a quick polyphenolic release both in acidic and neutral media due to the high water solubility of the carrier lactose. On the contrary, microspheres based hypromellose release only 20% of the loaded extract at pH 1.2 in 2 h and the total amount of polyphenols is released only after about further 6 h at pH 6.8. Matrices prepared tabletting lactose microspheres and hypromellose microparticles in the weight ratio 1:1 show a slow release rate, that lasts approximately 24 h. This one-a-day sustained release formulation containing Cynara scolymus extract could be proposed as a nutraceutical controlled release dosage form for oral administration.

Monitoring of Soil Remediation Process in the Metal Mining Area

NASA Astrophysics Data System (ADS)

Kim, Kyoung-Woong; Ko, Myoung-Soo; Han, Hyeop-jo; Lee, Sang-Ho; Na, So-Young

2016-04-01

Stabilization using proper additives is an effective soil remediation technique to reduce As mobility in soil. Several researches have reported that Fe-containing materials such as amorphous Fe-oxides, goethite and hematite were effective in As immobilization and therefore acid mine drainage sludge (AMDS) may be potential material for As immobilization. The AMDS is the by-product from electrochemical treatment of acid mine drainage and mainly contains Fe-oxide. The Chungyang area in Korea is located in the vicinity of the huge abandoned Au-Ag Gubong mine which was closed in the 1970s. Large amounts of mine tailings have been remained without proper treatment and the mobilization of mine tailings can be manly occurred during the summer heavy rainfall season. Soil contamination from this mobilization may become an urgent issue because it can cause the contamination of groundwater and crop plants in sequence. In order to reduce the mobilization of the mine tailings, the pilot scale study of in-situ stabilization using AMDS was applied after the batch and column experiments in the lab. For the monitoring of stabilization process, we used to determine the As concentration in crop plants grown on the field site but it is not easily applicable because of time and cost. Therefore, we may need simple monitoring technique to measure the mobility or leachability which can be comparable with As concentration in crop plants. We compared several extraction methods to suggest the representative single extraction method for the monitoring of soil stabilization efficiency. Several selected extraction methods were examined and Mehlich 3 extraction method using the mixture of NH4F, EDTA, NH4NO3, CH3COOH and HNO3 was selected as the best predictor of the leachability or mobility of As in the soil remediation process.

A new tunable dispersive liquid-liquid micro extraction method developed for the simultaneous preconcentration of lead and cadmium from lakes water: a multivariate study

NASA Astrophysics Data System (ADS)

Bilal, Muhammad; Kazi, Tasneem Gul; Afridi, Hassan Imran; Ali, Jamshed; Baig, Jameel Ahmed; Arain, Mohammad Balal; Khan, Mustafa

2017-08-01

A green tunable dispersive liquid-liquid micro extraction (TDLLME) technique was established for the simultaneous enrichment of lead (Pb) and cadmium (Cd) from different lakes water before analysis by flame atomic absorption spectrometry (FAAS). A solvent known as tunable polarity solvent (TPS), mixture of 1,8-diazabicyclo-[5.4.0]-undec-7-ene (DBU) and 1-decanol, has been employed as extractant in aqueous medium. In first step this mixture can be made polar by slowly bubbling the antisolvent trigger (CO2) through the solution, which makes a monophasic solution. During this step hydrophobic complexes of the metals with 8-hydroxy quinoline (8-HQ) were extracted by TPS. Then the mixture was switched back to hydrophobic one by heating and/or bubbling nitrogen, turning the mixture into two phases again. In second phase the metals were leached out from the complexes entrapped in TPS, by treating with a solution of nitric acid and exposing the mixture to CO2, which switched the mixture into single phase. Then N2 purging and/or heating again turned the mixture into two phases. The acidic aqueous phase containing the metals was introduced to FAAS for analysis, whereas TPS was recycled for next experiment. Different parameters, affecting the efficiency the technique, were optimized by multivariate approach. The method was applied to certified reference material of water and to a real sample spiked with standards of known concentration, to confirm its validity and accuracy. LOD obtained for Pb and Cd were 0.560 and 0.056 μg L- 1 respectively. The developed method was applied successfully to the real water samples of two lakes of Sindh, Pakistan.

Development of water-phase derivatization followed by solid-phase microextraction and gas chromatography/mass spectrometry for fast determination of valproic acid in human plasma.

PubMed

Deng, Chunhui; Li, Ning; Ji, Jie; Yang, Bei; Duan, Gengli; Zhang, Xiangmin

2006-01-01

In this study, a simple, rapid, and sensitive method was developed and validated for the quantification of valproic acid (VPA), an antiepileptic drug, in human plasma, which was based on water-phase derivatization followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS). In the proposed method, VPA in plasma was rapidly derivatized with a mixture of isobutyl chloroformate, ethanol and pyridine under mild conditions (room temperature, aqueous medium), and the VPA ethyl ester formed was headspace-extracted and simultaneously concentrated using the SPME technique. Finally, the analyte extracted on SPME fiber was analyzed by GC/MS. The experimental parameters and method validations were studied. The optimal conditions were obtained: PDMS fiber, stirring rate of 1100 rpm, sample temperature of 80 degrees C, extraction time of 20 min, NaCl concentration of 30%. The proposed method had a limit of quantification (0.3 microg/mL), good recovery (89-97%) and precision (RSD value less than 10%). Because the proposed method combined a rapid water-phase derivatization with a fast, simple and solvent-free sample extraction and concentration technique of SPME, the sample preparation time was less than 25 min. This much shortens the whole analysis time of VPA in plasma. The validated method has been successfully used to analyze VPA in human plasma samples for application in pharmacokinetic studies. All these results show that water-phase derivatization followed by HS-SPME and GC/MS is an alternative and powerful method for fast determination of VPA in biological fluids. Copyright 2006 John Wiley & Sons, Ltd.

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.

Consequence of the antioxidant activities and tyrosinase inhibitory effects of various extracts from the fruiting bodies of Pleurotus ferulae

PubMed Central

Alam, Nuhu; Yoon, Ki Nam; Lee, Jae Seong; Cho, Hae Jin; Lee, Tae Soo

2011-01-01

This study was initiated to screen the antioxidant activities, tyrosinase inhibitory effects on the fruiting bodies of Pleurotus ferulae extracted with acetone, methanol and hot water. The antioxidant activities were performed on β-carotene–linoleic acid, reducing power, DPPH, ferrous ions chelating abilities, and xanthine oxidase. In addition to this, phenolic compounds were also analyzed. The methanolic extract showed the strongest β-carotene–linoleic acid inhibition and high reducing power as compared to other extracts. The scavenging effects on DPPH radicals, the acetonic and methanolic extracts were more effective than hot water extracts. The strongest chelating effect was obtained from the methanolic extract as compared to the tested synthetic antioxidant. Gallic acid, protocatechuic acid, caffeic acid, vanillin, ferulic acid, naringin, resveratrol, naringenin, hesperetin, formononetin and biochanin-A were detected from acetonitrile and hydrochloric acid (5:1) solvent extract. Xanthine oxidase and tyrosinase inhibitory activities of acetonic, methanolic, and hot water extracts of P. ferulae increased with increasing concentration. The results suggested that consumption of P. ferulae might be beneficial to the antioxidant, xanthine oxidase, and tyrosinase protection system of the human body against oxidative damage and others complications. PMID:23961169

Reverse micelle-mediated dispersive liquid-liquid microextraction of 2,4-dichlorophenoxyacetic acid and 4-chloro-2-methylphenoxyacetic acid.

PubMed

Tayyebi, Moslem; Yamini, Yadollah; Moradi, Morteza

2012-09-01

A supramolecular solvent consisting of reverse micelles of decanoic acid, dispersed in a continuous phase of tetrahydrofuran:water, was proposed as an efficient microextraction technique for extraction of selected chlorophenoxy acid herbicides from water samples prior to high-performance liquid chromatography UV determination. The disperser solvent (1.0 mL tetrahydrofuran) containing 20 mg decanoic acid was rapidly injected into 10.0 mL of water sample. After centrifugation, the reverse micelle-rich phase (25 ± 0.5 μL) was floated at top of the home-designed centrifuge tube. The solvent was collected and 20 μL of it was injected into high-performance liquid chromatography for analysis. The results showed that the in situ solvent formation and extraction process can be completed in a few seconds. Under the optimal conditions, limits of detection of the method for 4-chloro-2-methylphenoxyacetic acid and 2,4-dichlorophenoxyacetic acid were in the range of 0.5-0.8 μg L(-1) and the repeatability of the proposed method, expressed as relative standard deviation, varied in the range of 2.5-3.2%. Linearity was found to be in the range of 1-200 μg L(-1) and the preconcentration factors were between 148 and 157. The mean percentage recoveries exceeded 92.0% for all the spiking levels in real water samples. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

Measurement of non-enteric emission fluxes of volatile fatty acids from a California dairy by solid phase micro-extraction with gas chromatography/mass spectrometry

NASA Astrophysics Data System (ADS)

Alanis, Phillip; Sorenson, Mark; Beene, Matt; Krauter, Charles; Shamp, Brian; Hasson, Alam S.

Dairies are a major source of volatile organic compounds (VOCs) in California's San Joaquin Valley; a region that experiences high ozone levels during summer. Short-chain carboxylic acids, or volatile fatty acids (VFAs), are believed to make up a large fraction of VOC emissions from these facilities, although there are few studies to substantiate this. In this work, a method using a flux chamber coupled to solid phase micro-extraction (SPME) fibers followed by analysis using gas chromatography/mass spectrometry was developed to quantify emissions of six VFAs (acetic acid, propanoic acid, butanoic acid, pentanoic acid, hexanoic acid and 3-methyl butanoic acid) from non-enteric sources. The technique was then used to quantify VFA fluxes from a small dairy located on the campus of California State University Fresno. Both animal feed and animal waste are found to be major sources of VFAs, with acetic acid contributing 70-90% of emissions from the sources tested. Measured total acid fluxes during spring (with an average temperature of 20 °C) were 1.84 ± 0.01, 1.06 ± 0.08, (1.3 ± 0.5) × 10 -2, (1.7 ± 0.2) × 10 -2 and (1.2 ± 0.5) × 10 -2 g m -2 h -1 from silage, total mixed rations, flushing lane, open lot and lagoon sources, respectively. VFA emissions from the sources tested total 390 ± 80 g h -1. The data indicate high fluxes of VFAs from dairy facilities, but differences in the design and operation of dairies in the San Joaquin Valley as well as seasonal variations mean that additional measurements must be made to accurately determine emissions inventories for the region.

Investigation of aggregation in solvent extraction of lanthanides by acidic extractants (organophosphorus and naphthenic acid)

USGS Publications Warehouse

Zhou, N.; Wu, J.; Yu, Z.; Neuman, R.D.; Wang, D.; Xu, G.

1997-01-01

Three acidic extractants (I) di(2-ethylhexyl) phosphoric acid (HDEHP), (II) 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (HEHPEHE) and (III) naphthenic acid were employed in preparing the samples for the characterization of the coordination structure of lanthanide-extractant complexes and the physicochemical nature of aggregates formed in the organic diluent of the solvent extraction systems. Photo correlation spectroscopy (PCS) results on the aggregates formed by the partially saponified HDEHP in n-heptane showed that the hydrodynamic radius of the aggregates was comparable to the molecular dimensions of HDEHP. The addition of 2-octanol into the diluent, by which the mixed solvent was formed, increased the dimensions of the corresponding aggregates. Aggregates formed from the lanthanide ions and HDEHP in the organic phase of the extraction systems were found very unstable. In the case of naphthenic acid, PCS data showed the formation of w/o microemulsion from the saponified naphthenic acid in the mixed solvent. The extraction of lanthanides by the saponified naphthenic acid in the mixed solvent under the given experimental conditions was a process of destruction of the w/o microemulsion. A possible mechanism of the breakdown of the w/o microemulsion droplets is discussed.

[Determination of estrogen residues in drinking water by on-line solid phase extraction based on sol-gel technique coupled with high performance liquid chromatography].

PubMed

Li, Longfei; Su, Min; Shi, Xiaolei; Wang, Yana; Wang, Minmin; He, Jinxing

2014-02-01

A method for the determination of diethylstilbestrol (DES), hexestrol (HEX) and dienestrol (DS) residues in drinking water was established by on-line solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). The material synthesized on the base of sol-gel technology was employed as adsorbent. This material was prepared using 3-aminopropyltriethoxysilane (APTES) as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and acetic acid as the initiator. The synthesized adsorbent showed outstanding property for the estrogen extraction. The estrogen can be caught effectively from water samples and the extraction can be achieved rapidly. Some important parameters, such as pH of sample solution, eluent solvents, loading flow rate, which might influence extraction efficiency, were optimized. The results indicated that the limit of detection (S/N = 3) of the developed method could reach 0.07-0.13 microg/L under the conditions of pH 7.0 of sample solution, methanol and 1% (v/v) acetic acid aqueous solution as the eluent solvent and the loading flow rate of 2 mL/min. The recoveries of the three estrogens from the water samples at three spiked levels ranged from 82.31% to 99.43% with RSD of 1.61%-7.15%. The method was simple, rapid, and suitable to detect the trace residues of estrogens in drinking water.

In vitro fermentation characteristics of two mushroom species, an herb, and their polysaccharide fractions, using chicken cecal contents as inoculum.

PubMed

Guo, F C; Williams, B A; Kwakkel, R P; Verstegen, M W A

2003-10-01

In vitro fermentabilities of two mushrooms (Lentinus edodes--LenS; Tremella fuciformis--TreS), an herb (Astragalus membranaceus--AstS), and their polysaccharide fractions (LenE, TreE, and AstE) were investigated using microflora from chicken ceca. Polysaccharides were extracted using the hot water method. The mushrooms had lower polysaccharide yields (8 to 10%) than the herb (31%). Fermentation kinetics were determined using the in vitro cumulative gas production technique. End-products, such as gas, volatile fatty acids (VFA), and ammonia, were also determined. The gas profiles of intact materials were similar for AstS and LenS. The TreS had a diphasic digestion pattern. The extracts had similar profiles to the intact materials though gas production rates were faster. Intact materials tended to produce less VFA than the extracts though LenS and AstE had the highest total VFA production overall. Intact materials contained more protein than the extracts, and therefore resulted in more branched-chain fatty acids and ammonia. Fermentation kinetics and end-point products demonstrated differences in availability of substrates between the mushrooms and herb. These medicinal mushroom and herb materials, particularly their polysaccharide extracts, show promise in altering microbial activities and composition in chicken ceca. In vivo experiments are necessary for confirmation of this hypothesis.

Anti-inflammatory, Antipyretic, and Antinociceptive Effects of a Cressa cretica Aqueous Extract.

PubMed

Abdallah, Heba Mohammed Ibrahim; Elshamy, Abdelsamed Ibrahim; El Gendy, Abd El-Nasser Gaber; Abd El-Gawad, Ahmed Mohamed; Omer, Elsayed Abouelfotowh; De Leo, Marinella; Pistelli, Luisa

2017-11-01

Cressa cretica is a widely grown halophytic plant traditionally used for the treatment of different ailments. Previous investigations reported its biological activity on a wide spectrum of diseases. In this study, in vivo antinociceptive, anti-inflammatory, and antipyretic activities of C. cretica aqueous extract whole plant were evaluated. In addition, the total polyphenol content, the total flavonoid content, and the chemical characterization of the extract were performed. C. cretica showed writhing inhibition in acetic acid-induced peripheral nociception of 43 and 48 % at doses of 50 and 100 mg/kg, respectively. The same doses increased latency time in a hot plate model of central analgesia by 66 and 78 % compared to the control group, respectively. The acute anti-inflammatory effect of the extract was explored in the carrageenan-induced rat hind paw test. The inhibition of paw volume was better than that of the standard drug indomethacin. C. cretica significantly decreased rectal temperature in the rats injected with Brewer's yeast. C. cretica aqueous extract showed both central and peripheral antinociceptive activities and was effective as an anti-inflammatory and antipyretic. Phenolic compounds, including chlorogenic acids and flavonol glycosides, were identified by HPLC-PDA-ESI-MS techniques. These findings indicate the medicinal importance of this traditionally used plant as a therapeutic remedy for different ailments. Georg Thieme Verlag KG Stuttgart · New York.

Production of secondary metabolites by some terverticillate penicillia on carbohydrate-rich and meat substrates.

PubMed

Núñez, Félix; Westphal, Carmen D; Bermúdez, Elena; Asensio, Miguel A

2007-12-01

Most terverticillate penicillia isolated from dry-cured meat products are toxigenic, but their ability to produce hazardous metabolites on meat-based substrates is not well known. The production of extrolites by selected terverticillate penicillia isolated from dry-cured ham has been studied on carbohydrate-rich media (malt extract agar, Czapek yeast autolysate agar, rice extract agar, and rice), meat extract triolein salt agar, and ham slices. Chloroform extracts from the selected strains grown on malt extract agar were toxic for the brine shrimp (Artemia salina) larvae and VERO cells at a concentration of 2 mg/ml, but 0.02 mg/ml produced no toxic effect. Analysis by high-pressure liquid chromatography (HPLC) coupled with photodiode array detection (DAD) or with mass spectrometry (MS) and an atmospheric pressure chemical ionization (APCI) source revealed different biologically active metabolites: cyclopiazonic acid and rugulovasine A from Penicillium commune; verrucosidin, anacine, puberuline, verrucofortine, and viridicatols from Penicillium polonicum; arisugacin and viridicatols from Penicillium echinulatum; and compactin and viridicatols from Penicillium solitum. Most of these metabolites, including the amino acid-derived compounds, were produced in the media containing high levels of carbohydrates. High concentrations of nitrogen compounds in the medium does not imply a greater production of the metabolites studied, not even those derived from the amino acids. However, molds growing on dry-cured ham are able to synthesize limited amounts of some secondary metabolites, a fact not previously reported. The combination of HPLC coupled with DAD and MS-APCI was useful for identification of closely related terverticillate Penicillium species from dry-cured ham. These techniques could be used to characterize the risk associated with the potential production of secondary metabolites in cured meats.

Features of the Thermodynamics of Trivalent Lanthanide/Actinide Distribution Reactions by Tri-n-Octylphosphine Oxide and Bis(2-EthylHexyl) Phosphoric Acid

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

Travis S. Grimes; Peter R. Zalupski

2014-11-01

A new methodology has been developed to study the thermochemical features of the biphasic transfer reactions of trisnitrato complexes of lanthanides and americium by a mono-functional solvating ligand (tri-n-octyl phosphine oxide - TOPO). Stability constants for successive nitrato complexes (M(NO3)x3-x (aq) where M is Eu3+, Am3+ or Cm3+) were determined to assist in the calculation of the extraction constant, Kex, for the metal ions under study. Enthalpies of extraction (?Hextr) for the lanthanide series (excluding Pm3+) and Am3+ by TOPO have been measured using isothermal titration calorimetry. The observed ?Hextr were found to be constant at ~29 kJ mol-1across themore » series from La3+-Er3+, with a slight decrease observed from Tm3+-Lu3+. These heats were found to be consistent with enthalpies determined using van ’t Hoff analysis of temperature dependent extraction studies. A complete set of thermodynamic parameters (?G, ?H, ?S) was calculated for Eu(NO3)3, Am(NO3)3 and Cm(NO3)3 extraction by TOPO and Am3+ and Cm3+ extraction by bis(2-ethylhexyl) phosphoric acid (HDEHP). A discussion comparing the energetics of these systems is offered. The measured biphasic extraction heats for the transplutonium elements, ?Hextr, presented in these studies are the first ever direct measurements offered using two-phase calorimetric techniques.« less

Impact of Ellagic Acid in Bone Formation after Tooth Extraction: An Experimental Study on Diabetic Rats

PubMed Central

Al-Obaidi, Mazen M. Jamil; Al-Bayaty, Fouad Hussain; Hussaini, Jamal; Khor, Goot Heah

2014-01-01

Objectives. To estimate the impact of ellagic acid (EA) towards healing tooth socket in diabetic animals, after tooth extraction. Methods. Twenty-four Sprague Dawley male rats weighing 250–300 g were selected for this study. All animals were intraperitoneally injected with 45 mg/kg (b.w.) of freshly prepared streptozotocin (STZ), to induce diabetic mellitus. Then, the animals were anesthetized, and the upper left central incisor was extracted and the whole extracted sockets were filled with Rosuvastatin (RSV). The rats were separated into three groups, comprising 8 rats each. The first group was considered as normal control group and orally treated with normal saline. The second group was regarded as diabetic control group and orally treated with normal saline, whereas the third group comprised diabetic rats, administrated with EA (50 mg/kg) orally. The maxilla tissue stained by eosin and hematoxylin (H&E) was used for histological examinations and immunohistochemical technique. Fibroblast growth factor (FGF-2) and alkaline phosphatase (ALP) were used to evaluate the healing process in the extracted tooth socket by immunohistochemistry test. Results. The reactions of immunohistochemistry for FGF-2 and ALP presented stronger expression, predominantly in EA treated diabetic rat, than the untreated diabetic rat. Conclusion. These findings suggest that the administration of EA combined with RSV may have accelerated the healing process of the tooth socket of diabetic rats, after tooth extraction. PMID:25485304

Antimicrobial activity of fatty acid methyl esters of some members of Chenopodiaceae.

PubMed

Chandrasekaran, Manivachagam; Kannathasan, Krishnan; Venkatesalu, Venugopalan

2008-01-01

Fatty acid methyl ester (FAME) extracts of four halophytic plants, viz. Arthrocnemum indicum, Salicornia brachiata, Suaeda maritima and Suaeda monoica belonging to the family Chenopodiaceae, were prepared and their composition was analyzed by GC-MS. The FAME extracts were also screened for antibacterial and antifungal activities. The GC-MS analysis revealed the presence of more saturated fatty acids than unsaturated fatty acids. Among the fatty acids analyzed, the relative percentage of lauric acid was high in S. brachiata (61.85%). The FAME extract of S. brachiata showed the highest antibacterial and antifungal activities among the extracts tested. The other three extracts showed potent antibacterial and moderate anticandidal activities.

Detection of a nuclear, EBNA-type antigen in apparently EBNA-negative Herpesvirus papio (HVP)-transformed lymphoid lines by the acid-fixed nuclear binding technique.

PubMed

Ohno, S; Luka, J; Falk, L; Klein, G

1977-12-15

In agreement with the findings of previous authors, we could not detect a virally determined nuclear antigen in Herpesvirus papio (HVP)-transformed baboon lymphoid lines by anticomplementary staining in situ, as for EBNA. However, by means of our recently developed acid-fixed nuclear binding technique an EBNA-like antigen could be readily demonstrated, after extraction from both producer and non-producer lines. We propose to designate the antigen as HUPNA. It can be detected by a human anti-EBNA antibody, suggesting cross-reactivity, if not identity, between EBNA and HUPNA. HVP-DNA carrying non-producer lines, negative for in situ ACIF stainability but capable of yielding HUPNA by the nuclear binding technique, can be superinfected with EBV, with brilliant EBNA expression as the result, suggesting that the defective in situ staining is a property associated with the baboon HVP, rather than the baboon lymphoid cell per se.

Universal nucleic acids sample preparation method for cells, spores and their mixture

DOEpatents

Bavykin, Sergei [Darien, IL

2011-01-18

The present invention relates to a method for extracting nucleic acids from biological samples. More specifically the invention relates to a universal method for extracting nucleic acids from unidentified biological samples. An advantage of the presently invented method is its ability to effectively and efficiently extract nucleic acids from a variety of different cell types including but not limited to prokaryotic or eukaryotic cells and/or recalcitrant organisms (i.e. spores). Unlike prior art methods which are focused on extracting nucleic acids from vegetative cell or spores, the present invention effectively extracts nucleic acids from spores, multiple cell types or mixtures thereof using a single method. Important that the invented method has demonstrated an ability to extract nucleic acids from spores and vegetative bacterial cells with similar levels effectiveness. The invented method employs a multi-step protocol which erodes the cell structure of the biological sample, isolates, labels, fragments nucleic acids and purifies labeled samples from the excess of dye.

A simplified extraction schema to for the analytical characterization of apple orchard soils

NASA Astrophysics Data System (ADS)

Sager, Manfred

2014-05-01

In agriculture, soil analysis is mainly done to monitor available nutrients as well contaminants, in order to find the optimum fertilization resp. remediation strategy. Traditionally, available nutrients in soils have been obtained from a series of different extractions, some just for one single parameter. In order to simplify the entire procedures, multi-element techniques, like ICP-OES and ICP-MS, have been applied to a sequence of extracts obtained with 0,16M acetic acid and 0,1M oxalate buffer pH 3, which are more suitable for the plasma than traditional salt extractant solutions. Dilute acetic acid should characterize exchangeables plus carbonates, and oxalate buffer the pedogenic oxides. Aqua regia extractions in glass have been replaced by pressure digestion with KClO3 in dilute nitric acid, which yields results equivalent to aqua regia, and additionally permits the determination of total sulfur, as well as acid-leachable boron and silicon. Total digestion was done in PTFE beakers by fuming with HNO3/HClO4, subsequently with HF, and final uptake in 1+1 HCl. The results of total digestion could be verified by XRF analysis of the solid, Ti recovery was the most critical item. The method was applied to 34 soils from apple orchards of different soil types and climatic zones. P and K obtained from standard acetate-lactate extract as well as B obtained from the Baron extract correlated with the results from the acetic acid extract better than 0,9. Just Mg from the CaCl2 extract (Schachtschabel) was independent from all other Mg fractions. The results for Ca, Cu, Mg, Mn, Sr, Pb and Zn obtained from KClO3 digest and from totals, were strongly correlated. The Rare Earth elements formed a strongly intercorrelated group as well after total digestion as in the oxalate leach. Factor analysis was utilized to prove if the obtained fractions part into groups in a geochemically feasible way. The fraction mobilized by dilute acetic acid contained Ca-Mg-carbonates as well as the minority elements Al-B-Ba-K-Na-S in the first factor, whereas Fe-Mn-Ti-La-Li-Sr-Y formed a group of its own. Both groups were rather independent from nutrient P as well as from the pedogenic oxides, obtained from Al-Fe-Mn-Ti released in oxalate. The oxalate soluble fraction was independent form available nutrient levels, and parted into 5 groups, of which one contained the anions B-S-Si, another one the contaminants As-Cd-Pb. Finally, the relations of these soil data to apple leaves from May and August, apple blossom leaves and apple fruits grown at these sites will be discussed, covering 50 varieties. The proposed method permits to obtain informations about common cations including trace elements, and the non-metals phosphorus, silicon, sulfur, boron and iodine simultaneously, which could be a gate to find new relations among them.

Identification of COX inhibitors in the hexane extract of Japanese horse chestnut (Aesculus turbinata) seeds.

PubMed

Sato, Itaru; Kofujita, Hisayoshi; Tsuda, Shuji

2007-07-01

Japanese horse chestnut (Aesculus turbinata) seed extract inhibits the activity of cyclooxygenase (COX), but its active constituents have not been identified. In the present study, COX inhibitors were isolated from the hexane extract of this seed by means of 4 steps of liquid chromatography and were identified by gas chromatography/mass spectrometry and nuclear magnetic resonance. The COX inhibitors in the extract of Japanese horse chestnut seeds were identified as linoleic acid, linolenic acid, and oleic acid. Their efficacies were in the following order: linolenic acid = linoleic acid > oleic acid. These active constituents are C18 unsaturated fatty acids; stearic acid, a C18 saturated fatty acid, had no activity. Linolenic acid and linoleic acid had high selectivity toward COX-2 (selectivity index = 10), whereas oleic acid had no selectivity. Considering the efficacy and yield of each fatty acid, linoleic acid may be the principal COX inhibitor in this seed.

Recent advances in rapid and nondestructive determination of fat content and fatty acids composition of muscle foods.

PubMed

Tao, Feifei; Ngadi, Michael

2018-06-13

Conventional methods for determining fat content and fatty acids (FAs) composition are generally based on the solvent extraction and gas chromatography techniques, respectively, which are time consuming, laborious, destructive to samples and require use of hazard solvents. These disadvantages make them impossible for large-scale detection or being applied to the production line of meat factories. In this context, the great necessity of developing rapid and nondestructive techniques for fat and FAs analyses has been highlighted. Measurement techniques based on near-infrared spectroscopy, Raman spectroscopy, nuclear magnetic resonance and hyperspectral imaging have provided interesting and promising results for fat and FAs prediction in varieties of foods. Thus, the goal of this article is to give an overview of the current research progress in application of the four important techniques for fat and FAs analyses of muscle foods, which consist of pork, beef, lamb, chicken meat, fish and fish oil. The measurement techniques are described in terms of their working principles, features, and application advantages. Research advances for these techniques for specific food are summarized in detail and the factors influencing their modeling results are discussed. Perspectives on the current situation, future trends and challenges associated with the measurement techniques are also discussed.

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.

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-performance relationship that can be used to guide molecular designs of HRE extraction in future.

STUDIES ON CHEMICAL COMPOSITION AND ANTIMICROBIAL ACTIVITIES OF BIOACTIVE MOLECULES FROM DATE PALM (PHOENIXDACTYLIFERA L.) POLLENS AND SEEDS.

PubMed

Bentrad, Najla; Gaceb-Terrak, Rabéa; Benmalek, Yamina; Rahmania, Fatma

2017-01-01

Natural resources have been the crucial origin of chemical elements. They have been used in many traditions as alternative medicines. The chemical profiling of some plant extracts and essential oils related to different plants were followed to unveil their most active components. In this paper, Phoenix dactilyfera L was selected as a host plant to investigate the composition of different organs with different cultivars. The antibacterial and antifungal activities of the extracts have been tested using different techniques, including optical density and GC/MS analyses of the natural extracts. GC/MS analysis revealed the presence of abundant oleic (36.69%) and lauric (20.49%) acids in date seeds. However, the pollen contains a high amount of palmitic (22.27 %), linoleic (33.4%) and linolenic (17.055%) acids. Moreover, the largest inhibition zone is obtained with the organic extract of Deglet Nour which showed a strong antibacterial activity against Escherichia coli and pollen extract showed also a strong inhibition against Escherichia coli , Staphylococcus aureus , S. aureus MRSA and Enterococcus faecalis . Aqueous extracts of date palm seeds of and pollen seem to have a fongitoxique activity from a concentration of 6 mg.mL -1 and 12mg.mL -1 of cyanidine; as well as the organic extracts of pollen with a concentration of 90 μg.mL" 1 induce an inhibition to the growth of five special forms of Fusarium oxysporum . The bioactive compounds of date palm can be used for drug development and in the food industry.

STUDIES ON CHEMICAL COMPOSITION AND ANTIMICROBIAL ACTIVITIES OF BIOACTIVE MOLECULES FROM DATE PALM (PHOENIXDACTYLIFERA L.) POLLENS AND SEEDS

PubMed Central

Bentrad, Najla; Gaceb-Terrak, Rabéa; Benmalek, Yamina; Rahmania, Fatma

2017-01-01

Background: Natural resources have been the crucial origin of chemical elements. They have been used in many traditions as alternative medicines. The chemical profiling of some plant extracts and essential oils related to different plants were followed to unveil their most active components. In this paper, Phoenix dactilyfera L was selected as a host plant to investigate the composition of different organs with different cultivars. Materials and method: The antibacterial and antifungal activities of the extracts have been tested using different techniques, including optical density and GC/MS analyses of the natural extracts. Results: GC/MS analysis revealed the presence of abundant oleic (36.69%) and lauric (20.49%) acids in date seeds. However, the pollen contains a high amount of palmitic (22.27 %), linoleic (33.4%) and linolenic (17.055%) acids. Moreover, the largest inhibition zone is obtained with the organic extract of Deglet Nour which showed a strong antibacterial activity against Escherichia coli and pollen extract showed also a strong inhibition against Escherichia coli, Staphylococcus aureus, S. aureus MRSA and Enterococcus faecalis. Aqueous extracts of date palm seeds of and pollen seem to have a fongitoxique activity from a concentration of 6 mg.mL-1 and 12mg.mL-1 of cyanidine; as well as the organic extracts of pollen with a concentration of 90 μg.mL”1 induce an inhibition to the growth of five special forms of Fusarium oxysporum. Conclusion: The bioactive compounds of date palm can be used for drug development and in the food industry. PMID:28480436

Antioxidant and Antifungal Activity of Extracts of the Aerial Parts of Thymus capitatus (L.) Hoffmanns Against Four Phytopathogenic Fungi of Citrus sinensis

PubMed Central

Tabti, Leila; Dib, Mohammed El Amine; Gaouar, Nassira; Samira, Bouayad; Tabti, Boufeldja

2014-01-01

Background: Many medicinal plants from the Lamiaceae family can be easily found in Algeria. These plants have been used as traditional medicines by local ethnic groups. Thymus capitatus is known in Algeria as "Zaatar" and has been commonly used as a spice, and reported to have many biological effects. Objectives: This paper focused on the assessment of the antioxidant potential and antifungal activity of essential oil and solvent extracts of T. capitatus against the growth of certain fungi. Materials and Methods: Essential oil, ethanol and hexane extracts of T. capitatus were tested for their antioxidant and antifungal activities. The 2, 2-diphenyl-1-picrylhydrazyl (DPPH) assay was used to determine the free radical quenching capacity. Antifungal activity was assessed using the radial growth technique. Results: DPPH free radical scavenging effect of the extracts was compared with standard antioxidant ascorbic acid and showed significant results. The ethanol extract showed high activity at the concentration of 80 g/mL, but less than the standard ascorbic acid. The essential oil was effective against all the fungi used in the experiment. The highest inhibitory effect on the growth of Aspergillus niger, Aspergillus oryzae, Penicillium digitatum, and Fusarium solani was exhibited by the essential oil at concentrations between 0.1 and 0.5 μg/mL. Conclusions: These findings demonstrated that ethanol extract obtained from T. capitatus is a potential source of natural antioxidant, while the essential oil extract can be exploited as an ideal alternative to synthetic fungicides for use in the treatment of many fungal phytopathogens. PMID:24644439

Effects of Pre-Converted Nitrite from Red Beet and Ascorbic Acid on Quality Characteristics in Meat Emulsions

PubMed Central

Kim, Hyun-Wook; Hwang, Ko-Eun

2017-01-01

We investigated the effects of fermented red beet extract and ascorbic acid on color development in meat emulsions. The pH of meat emulsions containing red beet extract decreased with an increase in the amount of extract added. The redness of the treated meat emulsions was higher than that of the control with no added nitrite or fermented red beet extract (p<0.05), though the redness of the meat emulsions treated with fermented red beet extract only was lower than in that treated with both fermented red beet extract and ascorbic acid (p<0.05). The highest VBN, TBARS, and total viable count values were observed in the control, and these values in the meat emulsions treated with fermented red beet extract were higher than in that treated with both fermented red beet extract and ascorbic acid (p<0.05). E. coli and coliform bacteria were not found in any of the meat emulsions tested. Treatment T2, containing nitrite and ascorbic acid, had the highest overall acceptability score (p<0.05); however, there was no significant difference between the T2 treatment and the T6 treatment, which contained 10% pre-converted nitrite from red beet extract and 0.05% ascorbic acid (p>0.05). The residual nitrite content of the meat emulsions treated with ascorbic acid was lower than in those treated without ascorbic acid (p<0.05). Thus, the combination of fermented red beet extract and ascorbic acid could be a viable alternative to synthetic nitrite for the stability of color development in meat emulsions. PMID:28515652

Effects of Pre-Converted Nitrite from Red Beet and Ascorbic Acid on Quality Characteristics in Meat Emulsions.

PubMed

Choi, Yun-Sang; Kim, Tae-Kyung; Jeon, Ki-Hong; Park, Jong-Dae; Kim, Hyun-Wook; Hwang, Ko-Eun; Kim, Young-Boong

2017-01-01

We investigated the effects of fermented red beet extract and ascorbic acid on color development in meat emulsions. The pH of meat emulsions containing red beet extract decreased with an increase in the amount of extract added. The redness of the treated meat emulsions was higher than that of the control with no added nitrite or fermented red beet extract ( p <0.05), though the redness of the meat emulsions treated with fermented red beet extract only was lower than in that treated with both fermented red beet extract and ascorbic acid ( p <0.05). The highest VBN, TBARS, and total viable count values were observed in the control, and these values in the meat emulsions treated with fermented red beet extract were higher than in that treated with both fermented red beet extract and ascorbic acid ( p <0.05). E. coli and coliform bacteria were not found in any of the meat emulsions tested. Treatment T2, containing nitrite and ascorbic acid, had the highest overall acceptability score ( p <0.05); however, there was no significant difference between the T2 treatment and the T6 treatment, which contained 10% pre-converted nitrite from red beet extract and 0.05% ascorbic acid ( p >0.05). The residual nitrite content of the meat emulsions treated with ascorbic acid was lower than in those treated without ascorbic acid ( p <0.05). Thus, the combination of fermented red beet extract and ascorbic acid could be a viable alternative to synthetic nitrite for the stability of color development in meat emulsions.

Assessment of Antioxidant and Phenolic Compound Concentrations as well as Xanthine Oxidase and Tyrosinase Inhibitory Properties of Different Extracts of Pleurotus citrinopileatus Fruiting Bodies

PubMed Central

Alam, Nuhu; Yoon, Ki Nam; Lee, Kyung Rim; Kim, Hye Young; Shin, Pyung Gyun; Cheong, Jong Chun; Yoo, Young Bok; Shim, Mi Ja; Lee, Min Woong

2011-01-01

Cellular damage caused by reactive oxygen species has been implicated in several diseases, thus establishing a significant role for antioxidants in maintaining human health. Acetone, methanol, and hot water extracts of Pleurotus citrinopileatus were evaluated for their antioxidant activities against β-carotene-linoleic acid and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radicals, reducing power, ferrous ion-chelating abilities, and xanthine oxidase inhibitory activities. In addition, the tyrosinase inhibitory effects and phenolic compound contents of the extracts were also analyzed. Methanol and acetone extracts of P. citrinopileatus showed stronger inhibition of β-carotene-linoleic acid compared to the hot water extract. Methanol extract (8 mg/mL) showed a significantly high reducing power of 2.92 compared to the other extracts. The hot water extract was more effective than the acetone and methanole extracts for scavenging DPPH radicals. The strongest chelating effect (92.72%) was obtained with 1.0 mg/mL of acetone extract. High performance liquid chromatography analysis detected eight phenolic compounds, including gallic acid, protocatechuic acid, chlorogenic acid, ferulic acid, naringenin, hesperetin, formononetin, and biochanin-A, in an acetonitrile and hydrochloric acid (5 : 1) solvent extract. Xanthine oxidase and tyrosinase inhibitory activities of the acetone, methanol, and hot water extracts increased with increasing concentration. This study suggests that fruiting bodies of P. citrinopileatus can potentially be used as a readily accessible source of natural antioxidants. PMID:22783067

Phytochemical composition and in vitro pharmacological activity of two rose hip (Rosa canina L.) preparations.

PubMed

Wenzig, E M; Widowitz, U; Kunert, O; Chrubasik, S; Bucar, F; Knauder, E; Bauer, R

2008-10-01

The aim of the present study was to compare powdered rose hip with and without fruits (Rosae pseudofructus cum/sine fructibus, Rosa canina L., Rosaceae) with regard to their phytochemical profile and their in vitro anti-inflammatory and radical-scavenging properties. The two powders were subsequently extracted with solvents of increasing polarity and tested for inhibition of cyclooxygenase (COX-1, COX-2) and of 5-LOX-mediated leukotriene B(4) (LTB(4)) formation as well as for DPPH-radical-scavenging capacity. While the water and methanol extracts were inactive in the COX-1, COX-2 and LTB(4) inhibition assays, the n-hexane and the dichloromethane extracts inhibited all three enzymes. In the active extracts, the triterpenoic acids ursolic acid, oleanolic acid and betulinic acid were identified, although only in minute amounts. Furthermore, oleic, linoleic and alpha-linolenic acid were identified apart from several saturated fatty acids. Even though unsaturated fatty acids are known to be good inhibitors of COX-1, COX-2 and LT formation, no clear correlation between their concentration in the extracts and their activity was found. We suggest that other, yet unidentified, lipophilic constituents might play a more important role for the observed in vitro inhibitory activity on arachidonic acid metabolism. Some of the extracts also showed considerable DPPH radical scavenging activity, the methanolic extracts being most potent. The radical scavenging activity of the extracts correlated very well with their total phenolic content, while ascorbic acid contributes only little to the radical-scavenging activity due to its low concentration present in the extracts. In summary, extracts derived from powdered rose hip without fruits were more effective in all assays carried out compared with extracts derived from powdered rose hip with fruits.

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.

Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

NASA Astrophysics Data System (ADS)

Oliveira, J. M.; Carvalho, F. P.

2006-01-01

A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom® and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample).

Comparison of the Composition and Antioxidant Activities of Phenolics from the Fruiting Bodies of Cultivated Asian Culinary-Medicinal Mushrooms.

PubMed

Lin, Shaoling; Ching, Lai Tsz; Ke, Xinxin; Cheung, Peter Chi Keung

2016-01-01

The composition profile and the antioxidant properties of phenolics in water extracts obtained from the fresh fruiting bodies of 4 common cultivated Asian edible mushrooms-Agrocybe aegerita, Pleurotus ostreatus, P. eryngii, and Pholiota nameko were compared. The water extract from A. aegerita (AaE) had the highest total phenolic content (TPC) at 54.18 ± 0.27 gallic acid equivalents (μmol/L)/mg extract (P < 0.05), as measured by the Folin-Ciocalteu method, and consisted of the largest number (including gallic acid, protocatechuic acid, chlorogenic acid, ferulic acid, and sinapic acid) and total amounts of phenolic acids identified by Fourier transform-ion cyclotron resonance mass spectrometry. The water extract of Ph. nameko was found to have the second-highest TPC (43.55 ± 0.10 gallic acid equivalents [μmol/L]/mg extract), followed by the water extract of P. eryngii and the water extract of P. ostreatus (39.55 ± 0.25 and 39.02 ± 0.30 gallic acid equivalents/mg extract, respectively). The scavenging activities of the water extracts from these mushrooms were evaluated against 2,2-diphenyl-l-(2,4,6-trinitrophenyl) hydrazyl diphenylpicrylhydrazyl (DPPH), superoxide anion radicals, hydroxyl radicals, and hydrogen peroxide. Based on halfmaximal effective concentrations, AaE was more effective in scavenging hydrogen peroxide (<0.05), followed by DPPH (0.51 mg/mL), superoxide anion radicals (0.85 mg/mL) and hydroxyl radicals (5.94 mg/mL), then the other mushroom water extracts. The differences in the half-maximal effective concentrations of individual mushroom water extracts were probably the result of the different numbers and amounts of individual phenolic acids in the extracts. The antioxidant activities of the mushroom water extracts were correlated with their TPC. The strongest antioxidant properties of AaE were consistent with its highest TPC and with the largest number and amount of phenolics identified in the extract. These results indicated that cultivated edible mushrooms could be a potential source of natural antioxidants with free radical scavenging properties for application as a functional food ingredient.

Production and purification of anti-bacterial biometabolite from wild-type Lactobacillus, isolated from fermented bamboo shoot: future suggestions and a proposed system for secondary metabolite onsite recovery during continuous fermentation.

PubMed

Badwaik, Laxmikant S; Borah, Pallab Kumar; Deka, Sankar C

2015-02-01

Wild-type lactobacillus isolated form Khorisa, a fermented bamboo shoot product of Assam, India were evaluated for production anti-bacterial secondary biometabolites, against Staphylococcus aureus. Submerged fermentation technique was used for the production of secondary anti-microbial biometabolite by a single wild-type lactobacillus strain, which tested positive for the release of anti-bacterial factor(s). Crude cell-free supernatant was obtained, followed by extraction in water-immiscible solvents viz., chloroform, hexane, petroleum ether. Chloroform extract of cell-free crude supernatant showed maximum yield (0.054 g/ml) and inhibited all indicator bacterial strains viz., Escherichia coli, Staphylococcus aureus, and Bacillus cereus. Yields of hexane and petroleum ether extract were 0.052 and 0.026 g/ml, respectively. Minimum lethal dose concentration assay of the chloroform extract showed LDmin values at 27, 1.68, and 1.68 mg/ml for E. coli, S. aureus, and B. cereus, respectively. Kill time for all the indicator bacterial strains were less than 12 h. The efficacy of the anti-bacterial substance seemed to depend on the presence of organic acids, particularly lactic acid. Conceptual-based suggestion for the development of an onsite secondary metabolites recovery system during continuous fermentation has also been attempted.

Antimicrobial and Antibiofilm Activities of Citrus Water-Extracts Obtained by Microwave-Assisted and Conventional Methods.

PubMed

Caputo, Leonardo; Quintieri, Laura; Cavalluzzi, Maria Maddalena; Lentini, Giovanni; Habtemariam, Solomon

2018-06-17

Citrus pomace is a huge agro-food industrial waste mostly composed of peels and traditionally used as compost or animal feed. Owing to its high content of compounds beneficial to humans (e.g., flavonoids, phenol-like acids, and terpenoids), citrus waste is increasingly used to produce valuable supplements, fragrance, or antimicrobials. However, such processes require sustainable and efficient extraction strategies by solvent-free techniques for environmentally-friendly good practices. In this work, we evaluated the antimicrobial and antibiofilm activity of water extracts of three citrus peels (orange, lemon, and citron) against ten different sanitary relevant bacteria. Both conventional extraction methods using hot water (HWE) and microwave-assisted extraction (MAE) were used. Even though no extract fully inhibited the growth of the target bacteria, these latter (mostly pseudomonads) showed a significant reduction in biofilm biomass. The most active extracts were obtained from orange and lemon peel by using MAE at 100 °C for 8 min. These results showed that citrus peel water infusions by MAE may reduce biofilm formation possibly enhancing the susceptibility of sanitary-related bacteria to disinfection procedures.

Automated Desalting Apparatus

NASA Technical Reports Server (NTRS)

Spencer, Maegan K.; Liu, De-Ling; Kanik, Isik; Beegle, Luther

2010-01-01

Because salt and metals can mask the signature of a variety of organic molecules (like amino acids) in any given sample, an automated system to purify complex field samples has been created for the analytical techniques of electrospray ionization/ mass spectroscopy (ESI/MS), capillary electrophoresis (CE), and biological assays where unique identification requires at least some processing of complex samples. This development allows for automated sample preparation in the laboratory and analysis of complex samples in the field with multiple types of analytical instruments. Rather than using tedious, exacting protocols for desalting samples by hand, this innovation, called the Automated Sample Processing System (ASPS), takes analytes that have been extracted through high-temperature solvent extraction and introduces them into the desalting column. After 20 minutes, the eluent is produced. This clear liquid can then be directly analyzed by the techniques listed above. The current apparatus including the computer and power supplies is sturdy, has an approximate mass of 10 kg, and a volume of about 20 20 20 cm, and is undergoing further miniaturization. This system currently targets amino acids. For these molecules, a slurry of 1 g cation exchange resin in deionized water is packed into a column of the apparatus. Initial generation of the resin is done by flowing sequentially 2.3 bed volumes of 2N NaOH and 2N HCl (1 mL each) to rinse the resin, followed by .5 mL of deionized water. This makes the pH of the resin near neutral, and eliminates cross sample contamination. Afterward, 2.3 mL of extracted sample is then loaded into the column onto the top of the resin bed. Because the column is packed tightly, the sample can be applied without disturbing the resin bed. This is a vital step needed to ensure that the analytes adhere to the resin. After the sample is drained, oxalic acid (1 mL, pH 1.6-1.8, adjusted with NH4OH) is pumped into the column. Oxalic acid works as a chelating reagent to bring out metal ions, such as calcium and iron, which would otherwise interfere with amino acid analysis. After oxalic acid, 1 mL 0.01 N HCl and 1 mL deionized water is used to sequentially rinse the resin. Finally, the amino acids attached to the resin, and the analytes are eluted using 2.5 M NH4OH (1 mL), and the NH4OH eluent is collected in a vial for analysis.

Ultrasound-assisted analyte extraction for the determination of sulfate and elemental sulfur in zinc sulfide by different liquid chromatography techniques.

PubMed

Dash, K; Thangavel, S; Krishnamurthy, N V; Rao, S V; Karunasagar, D; Arunachalam, J

2005-04-01

The speciation and determination of sulfate (SO4(2-)) and elemental sulfur (S degree) in zinc sulfide (ZnS) using ion-chromatography (IC) and reversed-phase liquid chromatography (RPLC) respectively is described. Three sample pretreatment approaches were employed with the aim of determining sulfate: (i) conventional water extraction of the analyte; (ii) solid-liquid aqueous extraction with an ultrasonic probe; and (iii) elimination of the zinc sulfide matrix via ion-exchange dissolution (IED). The separation of sulfate was carried out by an anion-exchange column (IonPac AS17), followed by suppressed conductivity detection. Elemental sulfur was extracted ultrasonically from the acid treated sample solution into chloroform and separated on a reversed phase HPLC column equipped with a diode array detector (DAD) at 264 nm. The achievable solid detection limits for sulfate and sulfur were 35 and 10 microg g(-1) respectively.

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®.

Optimization of ultrasound-assisted extraction of crude oil from winter melon (Benincasa hispida) seed using response surface methodology and evaluation of its antioxidant activity, total phenolic content and fatty acid composition.

PubMed

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

2012-10-08

In the present study, ultrasound-assisted extraction of crude oil from winter melon seeds was investigated through response surface methodology (RSM). Process variables were power level (25-75%), temperature (45-55 °C) and sonication time (20-40 min). It was found that all process variables have significant (p < 0.05) effects on the response variable. A central composite design (CCD) was used to determine the optimum process conditions. Optimal conditions were identified as 65% power level, 52 °C temperature and 36 min sonication time for maximum crude yield (108.62 mg-extract/g-dried matter). The antioxidant activity, total phenolic content and fatty acid composition of extract obtained under optimized conditions were determined and compared with those of oil obtained by the Soxhlet method. It was found that crude extract yield (CEY) of ultrasound-assisted extraction was lower than that of the Soxhlet method, whereas antioxidant activity and total phenolic content of the extract obtained by ultrasound-assisted extraction were clearly higher than those of the Soxhlet extract. Furthermore, both extracts were rich in unsaturated fatty acids. The major fatty acids of the both extracts were linoleic acid and oleic acid.

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.

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.

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.

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...

The 1984 NASA/ASEE summer faculty fellowship program

NASA Technical Reports Server (NTRS)

1984-01-01

The assessment of forest productivity and associated nitrogen flux in a number of conifer ecosystems is described. As a base line study of acid precipitation in the Sierra Nevada, involved is the extraction and integration of a number of data planes describing the terrain, soils, lithology, vegetation cover and structure, and microclimate of the region. The development of automated techniques to extract topographic networks (stream canyons and ridge lines) for use as a landscrape skeleton to organize and integrate data sets into an efficient geographical information system is examined. The software is written in both FORTRAN and C, and is portable to a number of different computer environments with minimal modification.

Organic chemistry of Murchison meteorite: Carbon isotopic fractionation

NASA Technical Reports Server (NTRS)

Yuen, G. U.; Blair, N. E.; Desmarais, D. J.; Cronin, J. R.; Chang, S.

1986-01-01

The carbon isotopic composition of individual organic compounds of meteoritic origin remains unknown, as most reported carbon isotopic ratios are for bulk carbon or solvent extractable fractions. The researchers managed to determine the carbon isotopic ratios for individual hydrocarbons and monocarboxylic acids isolated from a Murchison sample by a freeze-thaw-ultrasonication technique. The abundances of monocarboxylic acids and saturated hydrocarbons decreased with increasing carbon number and the acids are more abundant than the hydrocarbon with the same carbon number. For both classes of compounds, the C-13 to C-12 ratios decreased with increasing carbon number in a roughly parallel manner, and each carboxylic acid exhibits a higher isotopic number than the hydrocarbon containing the same number of carbon atoms. These trends are consistent with a kinetically controlled synthesis of higher homologues for lower ones.

Carbon Isotope Characterization of Organic Intermediaries in Hydrothermal Hydrocarbon Synthesis by Pyrolysis-GC-MS-C-IRMS

NASA Technical Reports Server (NTRS)

Socki, Richard A.; Fu, Qi; Niles, Paul B.

2010-01-01

We report results of experiments designed to characterize the carbon isotope composition of intermediate organic compounds produced as a result of mineral surface catalyzed reactions. The impetus for this work stems from recently reported detection of methane in the Martian atmosphere coupled with evidence showing extensive water-rock interaction during Martian history. Abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions may be one possible process responsible for methane generation on Mars, and measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible isotope measurements. Our isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-Combustion-Isotope Ratio Mass Specrometry (Py-GC-MS-C-IRMS). Others have conducted similar pyrolysis-IRMS experiments on low molecular weight organic acids (Dias, et al, Organic Geochemistry, 33 [2002]). Our technique differs in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of the organic compounds. A sample of carboxylic acid (mixture of C1 through C6) was pyrolyzed at 100 XC and passed through the GC-MS-C-IRMS (combusted at 940 XC). In order to test the reliability of our technique we compared the _13C composition of different molecular weight organic acids (from C1 through C6) extracted individually by the traditional sealed-tube cupric oxide combustion (940 XC) method with the _13C produced by our pyrolysis technique. Our data indicate that an average 4.3. +/-0.5. (V-PDB) apparent isotopic fractionation accompanies the pyrolysis extractions. We postulate that this isotope offset could be the result of incomplete thermal desorption during pyrolysis. We are continuing to investigate the reliability of this pyrolysis technique for correcting carbon isotope measurements of mineral surface catalyzed organic compounds.

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

Supercritical Carbon Dioxide Extraction of Flavonoids from Pomelo (Citrus grandis (L.) Osbeck) Peel and Their Antioxidant Activity

PubMed Central

He, Jin-Zhe; Shao, Ping; Liu, Jian-Hua; Ru, Qiao-Mei

2012-01-01

Supercritical carbon dioxide (SC-CO2) extraction of flavonoids from pomelo (Citrus grandis (L.) Osbeck) peel and their antioxidant activity were investigated. Box-Behnken design combined with response surface methodology was employed to maximize the extraction yield of flavonoids. Correlation analysis of the mathematical-regression model indicated that a quadratic polynomial model could be used to optimize the SC-CO2 extraction of flavonoids. The optimal conditions for obtaining the highest extraction yield of flavonoids from pomelo peel were a temperature of 80 °C, a pressure of 39 MPa and a static extraction time of 49 min in the presence of 85% ethanol as modifier. Under these conditions, the experimental yield was 2.37%, which matched positively with the value predicted by the model. Furthermore, flavonoids obtained by SC-CO2 extraction showed a higher scavenging activity on hydroxyl, 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2′-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS) radicals than those obtained by conventional solvent extraction (CSE). Therefore, SC-CO2 extraction can be considered as a suitable technique for the obtainment of flavonoids from pomelo peel. PMID:23202938

Hemicelluloses prior to aspen chemithermomechanical pulping: pre-extraction, separation, and characterization.

PubMed

Liu, Wei; Hou, Qingxi; Mao, Changbin; Yuan, Zhirun; Li, Kecheng

2012-05-16

A portion of hemicelluloses and acetic acid can be pre-extracted with dilute sulfuric acid prior to the aspen chemithermomechanical pulp process. The streams collected from the second press-impregnation stage after acid pre-extraction contain a significant amount of acid pre-extracted hemicelluloses. Most of the total sugars obtained from the pressate were xylan, in which xylan was further hydrolyzed to sugar monomers under the acid pre-extraction condition. To fully understand the characteristics of hemicelluloses yielded prior to pulping, the pre-extracted hemicelluloses were separated and characterized by FT-IR, (1)H NMR, and thermogravimetric analysis in this study. Most of the FT-IR bonds from the hemicelluloses agreed well with the other two spectra of birch xylan and CA0050 xylan, except a new absorption at 1734 cm(-1) contributed to acetyl groups. The hemicelluloses obtained from acid pre-extraction began to decompose significantly at about 225 °C, slightly lower in comparison with organosolv and alkaline hemicelluloses reported in the literature.

Screening of plant extracts for antimicrobial activity against bacteria and yeasts with dermatological relevance.

PubMed

Weckesser, S; Engel, K; Simon-Haarhaus, B; Wittmer, A; Pelz, K; Schempp, C M

2007-08-01

There is cumulative resistance against antibiotics of many bacteria. Therefore, the development of new antiseptics and antimicrobial agents for the treatment of skin infections is of increasing interest. We have screened six plant extracts and isolated compounds for antimicrobial effects on bacteria and yeasts with dermatological relevance. The following plant extracts have been tested: Gentiana lutea, Harpagophytum procumbens, Boswellia serrata (dry extracts), Usnea barbata, Rosmarinus officinalis and Salvia officinalis (supercritical carbon dioxide [CO2] extracts). Additionally, the following characteristic plant substances were tested: usnic acid, carnosol, carnosic acid, ursolic acid, oleanolic acid, harpagoside, boswellic acid and gentiopicroside. The extracts and compounds were tested against 29 aerobic and anaerobic bacteria and yeasts in the agar dilution test. U. barbata-extract and usnic acid were the most active compounds, especially in anaerobic bacteria. Usnea CO2-extract effectively inhibited the growth of several Gram-positive bacteria like Staphylococcus aureus (including methicillin-resistant strains - MRSA), Propionibacterium acnes and Corynebacterium species. Growth of the dimorphic yeast Malassezia furfur was also inhibited by Usnea-extract. Besides the Usnea-extract, Rosmarinus-, Salvia-, Boswellia- and Harpagophytum-extracts proved to be effective against a panel of bacteria. It is concluded that due to their antimicrobial effects some of the plant extracts may be used for the topical treatment of skin disorders like acne vulgaris and seborrhoic eczema.

[Effect of phosphate and organic acid addition on passivation of simulated Pb contaminated soil and the stability of the product].

PubMed

Zuo, Ji-Chao; Gao, Ting-Ting; Su, Xiao-Juan; Wan, Tian-Ying; Hu, Hong-Qing

2014-10-01

Organic acids can improve the phosphorus availability, influence the immobilization of heavy metals in soil, and has very complicated function in phosphorus activation and heavy metal passivation. This research took simulated Pb contaminated soil as material, phosphate and citric acid as remediation matter, adopted BCR continuous extraction, 0.01 mol · L(-1) CaCl2 and toxicity characteristic leaching procedure (TCLP) to evaluate the remediation effect. Besides, malic acid and NaNO3 were taken as desorption reagents to discuss the stability of the phosphorus-citric acid-Pb system. The results showed that: in the absence of citric acid, the amount of acid extracted Pb decreased along with the increase of P concentration; when the P concentration was 100 and 400 mg · kg(-1), acid extractable Pb increased with the increasing of citric acid concentration. However, residual Pb changed in the opposite direction from acid extractable Pb. The phenomenon showed that P improved the bioavailability of Pb, while citric acid had the opposite effect. With a certain organic acid concentration, extractable Pb contents extracted by 0.01 mol · L(-1) CaCl2 and TCLP both decreased with the increasing P concentration, therefore, P had immobilization effect on Pb in contaminated soil. But at a fixed P concentration, extractable Pb contents by 0.01 mol · L(-1) CaCl2 and TCLP changed in the opposite trend with the increasing citric acid concentration. The desorption rate of Pb in soil increased with the increasing malic acid concentration, the decreasing pH and the increasing ionic strength. The desorption extent of Pb in soil with P only was lower than that with both P and citric acid. But the stability of Pb passivated by the former was higher.

Anti-Escherichia coli activity of extracts from Schinus terebinthifolius fruits and leaves.

PubMed

da Silva, Jessica H S; Simas, Naomi K; Alviano, Celuta S; Alviano, Daniela S; Ventura, José A; de Lima, Eliandro J; Seabra, Sergio H; Kuster, Ricardo M

2018-06-01

Ethanol extracts obtained from Schinus terebinthifolius Raddi fruits and leaves were active against Escherichia coli with MIC of 78 μg mL -1 for both extracts. Phytochemical analyses revealed a major presence of phenolic acids, tannins, fatty acids and acid triterpenes in the leaves and phenolic acids, fatty acids, acid triterpenes and biflavonoids in the fruits. Major compounds isolated from the plant, such as the acid triterpene schinol, the phenolic acid derivative ethyl gallate and the biflavonoids agathisflavone and tetrahydroamentoflavone, showed very little activity against E. coli. Bioautography of the ethanol extracts on silica gel plate showed inhibition zones for E. coli. They were removed from the plate and the compounds identified as a mixture of myristic, pentadecanoic, palmitic, heptadecanoic, stearic, nonadecanoic, eicosanoic, heneicosanoic and behenic fatty acids.

Identification of the soluble HVP-associated antigen of the lymphoblastoid cell line established from lymphomatous baboon (Papio hamadryas).

PubMed

Voevodin, A F; Lapin, B A; Agrba, V Z; Timanovskaya, V V

1978-01-01

A new technique (indirect double immunodiffusion) for detection of EBV-associated soluble antigen and corresponding antibodies has been developed. This technique includes three steps: 1) simple double immunodiffusion with extracts of Raji cells (or other EBV-genome positive cells) and human sera containing antibodies against EBV-associated soluble antigen; 2) extensive washing and treatment with anti-human globulin; 3) extensive washing and treatment with tannic acid. Using this test it was shown that the soluble antigen indistinguishable from EBV-associated soluble antigen was present in KMPG-1 cells producing HVP.

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.

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.

Phytotoxic activity and chemical composition of Cassia absus seeds and aerial parts.

PubMed

Zribi, I; Sbai, H; Ghezal, N; Richard, G; Trisman, D; Fauconnier, M L; Haouala, R

2017-12-01

The present study was conducted to assess the phytotoxic potential and the phytochemical composition of Cassia absus. Aqueous extracts caused significant reduction in root growth of Lactuca sativa. Seed extract was more effective than aerial part extract. Successive extractions of this plant were performed using solvents with increasing polarities. The methanolic seed extract exerted strong phytotoxic effect on seedling growth, followed by petroleum ether extract of the aerial part. The phytochemical investigation showed that among the organic extracts, methanol extracts of seeds and aerial parts contained the highest amounts of total phenolics and proanthocyanidins. Seeds were rich in linoleic acid followed by palmitic acids. Palmitic, stearic and arachidic acids were the major fatty acids in aerial parts. HPLC-DAD analysis of the methanolic extracts revealed the presence of luteolin in C. absus aerial parts.

INVESTIGATION OF CE/LIF AS A TOOL IN THE ...

EPA Pesticide Factsheets

The investigation of emerging contaminant issues is a proactive effort in environmental analysis. As a part of this effort, sewage effluent is of current analytical interest because of the presence of pharmaceuticals and their metabolites and personal care products The environmental impact of these components is still under investigation but their constant perfusion into receiving waters and their potential effect on biota is of concern. This paper examines a tool for the characterization of sewage effluent using capillary electrophoresis/laser-induced fluorescence (CE/LIF) with a frequency-doubled laser operated in the ultraviolet (UV). Fluorescent acidic analytes are targeted because they present special problems for techniques such as gas chromatography/mass spectrometry (GC/MS) but are readily accessible to CE/LIF. As an example of the application of this tool, salicylic acid is determined near the 100 ng/L level in sewage effluent. Salicylic acid is a metabolite of various analgesics Relatively stable in the environment, it is a common contaminant of municipal sewage systems. Salicylic acid was recovered from freshly collected samples of the effluent by liquid-liquid extraction as part of a broad characterization effort. Confirmation of identity was by electron ionization GC/MS after conversion of the salicylic acid to the methyl ester by means of trimethylsilyidiazomethane CE/LIF in the UV has revealed more than 50 individual peaks in the extract and a bac

Effect of various solvent on the specific amino acids of black soybean (Glycine soja) sprout

NASA Astrophysics Data System (ADS)

Kanetro, B.; Slamet, A.; Wazyka, A.

2018-01-01

The objective of this research was to study the effect of various solvent extractions on the specific amino acids as small peptide or free amino acids that was contained in the extract after removal of the macromolecule protein of black soybean sprouts. The experimental design of this research was randomized complete design with one factor, which was the three various solvent, i.e. hexane, ethanol and water. The black soybean seed was germinated for 36 h. The small peptide and free amino acids of black soybean sprout were isolated at 3 various of solvents extraction, and then the macromolecule proteins in the extracts were precipitated at the pH 4. The extracts of black soybean sprout after removal of the macromolecule protein were analysed by HPLC to determine the profile of amino acids for stimulation of insulin secretion. The result of this research showed that the extracts contained the small peptide and free amino acid for stimulation of insulin secretion. The best solvent extraction was water that was due to the content of Leu, Arg, Ala, Phe, Ile, and Lys of water extract was higher than hexane and ethanol extracts.

Some phenolic compounds of extracts obtained from Origanum species growing in Turkey.

PubMed

Ozkan, Gülcan; Ozcan, Mehmet Musa

2014-08-01

Caffeic acid, rosmarinic acid, rutin, apigenin 7-O-glucoside, apigenin, and acesetin were the main phenolic compounds of Origanum onites extracts in all applications. While acesetin contents ranged from 133.59 mg/100 g (U1) to 437.25 mg/100 g (S3), rosmarinic acid changed between 215.94 mg/100 g (U4) and 1120.56 mg/100 g (S2) in Origanum vulgare L. subsp. hirtum (Link) Ietsw. Both rosmarinic acid and acesetin were not found in U5 application. Only caffeic acid (19.39 mg/100 g) was found in U5 application. Rosmarinic acid contents of O. onites extract changed between 158.62 mg/100 g (U5) and 799.87 mg/100 g (S2). Generally, dominant phenolic compound of Origanum extracts was rosmarinic acid compared with other extracts. In addition, methanol:water:acetic acid mixture (S2) (95:4.5:0.5) was found as the best application. Phenolic contents of extracts obtained with U series mixtures were found low.

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.

Distribution and enantiomeric composition of amino acids in the Murchison meteorite

NASA Technical Reports Server (NTRS)

Engel, M. H.; Nagy, B.

1982-01-01

Studies of the amino acid contents and enantiomeric compositions of a single stone from the Murchison meteorite are reported. Water-extracted and 6M HCl-extracted samples from the meteorite interior of meteorite fragments were analyzed by gas chromatography and combined gas chromatography-chemical ionization mass spectrometry. Examination of the D/L ratios of glutamic acid, aspartic acid, proline, leucine and alanine reveals those amino acids extractable by water to be partially racemized, whereas the acid-extracted amino acids were less racemized. The amino acid composition of the stone is similar to those previously reported, including the absence of serine, threonine, tyrosine phenylalanine and methionine and the presence of unusual amino acids including such as isovaline, alpha-aminoisobutyric acid and pseudoleucine. It is concluded that the most likely mechanism accounting for the occurrence of nonracemic amino acid mixtures in the Murchison meteorite is by extraterrestrial stereoselective synthesis or decomposition reactions.

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.

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.

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.

Rapid determination of amino acids in neonatal blood samples based on derivatization with isobutyl chloroformate followed by solid-phase microextraction and gas chromatography/mass spectrometry.

PubMed

Deng, Chunhui; Li, Ning; Zhang, Xiangmin

2004-01-01

The purpose of this study was to develop a simple, rapid and sensitive analytical method for determination of amino acids in neonatal blood samples. The developed method involves the employment of derivatization and a solid-phase microextraction (SPME) technique together with gas chromatography/mass spectrometry (GC/MS). Amino acids in blood samples were derivatized by a mixture of isobutyl chloroformate, methanol and pyridine, and the N(O,S)-alkoxycarbonyl alkyl esters thus formed were headspace extracted by a SPME fiber. Finally, the extracted analytes on the fiber were desorbed and detected by GC/MS in electron impact (EI) mode. L-Valine, L-leucine, L-isoleucine, L-phenylanaline and L-tyrosine in blood samples were quantitatively analyzed by measurement of the corresponding N(O,S)-alkoxycarbonyl alkyl esters using an external standard method. SPME conditions were optimized, and the method was validated. The method was applied to diagnosis of neonatal phenylkenuria (PKU) and maple syrup urine disease (MSUD) by the analyses of five amino acids in blood samples. The results showed that the proposed method is a potentially powerful tool for simultaneous screening for neonatal PKU and MSUD. Copyright (c) 2004 John Wiley & Sons, Ltd.

Fatty acid methyl ester (FAME) technology for monitoring biological foaming in activated sludge: full scale plant verification.

PubMed

Lee, J W; Cha, D K; Kim, I; Son, A; Ahn, K H

2008-02-01

Fatty acid methyl ester (FAME) technology was evaluated as a monitoring tool for quantification of Gordonia amarae in activated sludge systems. The fatty acid, 19:1 alcohol, which was identified as a unique fatty acid in G. amarae was not only confirmed to be present in foaming plant samples, but the quantity of the signature peak correlated closely with the degree of foaming. Foaming potential experiment provided a range of critical foaming levels that corresponded to G. amarae population. This range of critical Gordonia levels was correlated to the threshold signature FAME amount. Six full-scale wastewater treatment plants were selected based on a survey to participate in our full-scale study to evaluate the potential application of the FAME technique as the Gordonia monitoring tool. Greater amounts of signature FAME were extracted from the mixed liquor samples obtained from treatment plants experiencing Gordonia foaming problems. The amounts of signature FAME correlated well with the conventional filamentous counting technique. These results demonstrated that the relative abundance of the signature FAMEs can be used to quantitatively monitor the abundance of foam-causing microorganism in activated sludge.

A new method for the determination of short-chain fatty acids from the aliphatic series in wines by headspace solid-phase microextraction-gas chromatography-ion trap mass spectrometry.

PubMed

Olivero, Sergio J Pérez; Trujillo, Juan P Pérez

2011-06-24

A new analytical method for the determination of nine short-chain fatty acids (acetic, propionic, isobutyric, butyric, isovaleric, 2-methylbutyric, hexanoic, octanoic and decanoic acids) in wines using the automated HS/SPME-GC-ITMS technique was developed and optimised. Five different SPME fibers were tested and the influence of different factors such as temperature and time of extraction, temperature and time of desorption, pH, strength ionic, tannins, anthocyans, SO(2), sugar and ethanol content were studied and optimised using model solutions. Some analytes showed matrix effect so a study of recoveries was performed. The proposed HS/SPME-GC-ITMS method, that covers the concentration range of the different analytes in wines, showed wide linear ranges, values of repeatability and reproducibility lower than 4.0% of RSD and detection limits between 3 and 257 μgL(-1), lower than the olfactory thresholds. The optimised method is a suitable technique for the quantitative analysis of short-chain fatty acids from the aliphatic series in real samples of white, rose and red wines. Copyright © 2011 Elsevier B.V. All rights reserved.

Biomimetic synthesis of silver nanoparticles by Citrus limon (lemon) aqueous extract and theoretical prediction of particle size.

PubMed

Prathna, T C; Chandrasekaran, N; Raichur, Ashok M; Mukherjee, Amitava

2011-01-01

In the present study, silver nanoparticles were rapidly synthesized at room temperature by treating silver ions with the Citrus limon (lemon) extract. The effect of various process parameters like the reductant concentration, mixing ratio of the reactants and the concentration of silver nitrate were studied in detail. In the standardized process, 10(-2)M silver nitrate solution was interacted for 4h with lemon juice (2% citric acid concentration and 0.5% ascorbic acid concentration) in the ratio of 1:4 (vol:vol). The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance as determined by UV-Visible spectra in the range of 400-500 nm. X-ray diffraction analysis revealed the distinctive facets (111, 200, 220, 222 and 311 planes) of silver nanoparticles. We found that citric acid was the principal reducing agent for the nanosynthesis process. FT-IR spectral studies demonstrated citric acid as the probable stabilizing agent. Silver nanoparticles below 50 nm with spherical and spheroidal shape were observed from transmission electron microscopy. The correlation between absorption maxima and particle sizes were derived for different UV-Visible absorption maxima (corresponding to different citric acid concentrations) employing "MiePlot v. 3.4". The theoretical particle size corresponding to 2% citric acid concentration was compared to those obtained by various experimental techniques like X-ray diffraction analysis, atomic force microscopy, and transmission electron microscopy. Copyright © 2010 Elsevier B.V. All rights reserved.

THE SOLVENT EXTRACTION OF NITROSYLRUTHENIUM BY TRILAURYLAMINE IN NITRATE SYSTEM. Summary Report for the Period, July 1, 1960 to March 31, 1962

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

Skavdahl, R.E.; Mason, E.A.

1962-06-01

An investigation of the solvent extraction characteristics of the nitro and nitrato complexes of nitrosylruthenium in nitric acid- sodium nitrate aqueous media was conducted. As the organic extractant phase, a solution of trilaurylamine (TLA) in toluene was utilized. In addition to the usual process parameter variation tyne of experiment, a rapid dilution type of experiment was used extensively to determine qualitative and semiquantitative results regarding the degree of extractability and concentration of the more extractable species of the nitrato complexes of nitrosylruthenium. It was found that the acids of the tetra-nitrato and pentanitrato complexes were the more extractable species formore » that set of complexes and that the acid of the penta-nitrato complex was the more extractable of the two. It was observed that for freshly prepared solutions, the dinitro complex of nitrosylruthenium was much more extractable than the gross nitrato complexes solutions. Nitro complexes in general, and the dinitro complex in particular, may be the controlling agent in ruthenium decontamination of spent nuclear fuel processed by solvent extraction methods. The experimental results from both sets of complexes could be more meaningfully correlated on the basis of unbound nitric acid concentration in the organic phase than on the basis of nitric acid concentration in the aqueous phase. The extraction of nitric acid by TLA from nitric acid-sodium nitrate aqueous solutions was investigated and the results correlated on the basis of activity of the undissociated nitric acid in the aqueous phase. (auth)« less

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

Casella, Amanda J.; Hylden, Laura R.; Campbell, Emily L.

Knowledge of real-time solution properties and composition is a necessity for any spent nuclear fuel reprocessing method. Metal-ligand speciation in aqueous solutions derived from the dissolved commercial spent fuel is highly dependent upon the acid concentration/pH, which influences extraction efficiency and the resulting speciation in the organic phase. Spectroscopic process monitoring capabilities, incorporated in a counter current centrifugal contactor bank, provide a pathway for on-line real-time measurement of solution pH. The spectroscopic techniques are process-friendly and can be easily configured for on-line applications, while classic potentiometric pH measurements require frequent calibration/maintenance and have poor long-term stability in aggressive chemical andmore » radiation environments. Our research is focused on developing a general method for on-line determination of pH of aqueous solutions through chemometric analysis of Raman spectra. Interpretive quantitative models have been developed and validated under the range of chemical composition and pH using a lactic acid/lactate buffer system. The developed model was applied to spectra obtained on-line during solvent extractions performed in a centrifugal contactor bank. The model predicted the pH within 11% for pH > 2, thus demonstrating that this technique could provide the capability of monitoring pH on-line in applications such as nuclear fuel reprocessing.« less

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.

Mugil cephalus roe oil obtained by supercritical fluid extraction affects the lipid profile and viability in cancer HeLa and B16F10 cells.

PubMed

Rosa, A; Piras, A; Nieddu, M; Putzu, D; Cesare Marincola, F; Falchi, A M

2016-09-14

We explored the changes in viability and lipid profile occurring in cancer cells, murine melanoma cells (B16F10 cells) and human cervical carcinoma cells (HeLa cells), when exposed to 24 h-treatments with an n-3 PUFA-rich oil obtained by supercritical extraction with CO2 from Mugil cephalus processed roe (bottarga). The composition of the major lipid classes of bottarga oil was determined by the (13)C NMR technique. Reversed-phase HPLC with DAD/ELSD detection was performed to analyze cells' total fatty acid profile and the levels of phospholipids, total/free cholesterol, triacylglycerols, and cholesteryl esters. Cell-based fluorescent measurements of intracellular membranes and lipid droplets were performed on bottarga oil-treated cells using the Nile red staining technique. The treatments of cancer cells with bottarga oil reduced the viability and affected the fatty acid profile, with a significant n-3 PUFA increase in treated cells. Mullet roe oil uptake modulated the cancer cell lipid composition, inducing a remarkable incorporation of health beneficial n-3 PUFA in the polar and neutral lipid fractions. Bottarga oil treatment influenced the synthesis of intracellular membranes and accumulation of cytoplasmic lipid droplets in cancer cells.

Bioassay-directed fractionation of organic compounds associated with airborne particulate matter; An interseasonal study

NASA Astrophysics Data System (ADS)

Greenberg, Arthur; Lwo, Jung-Hen; Antherholt, Thomas B.; Rosen, Robert; Hartman, Thomas; Butler, James; Louis, Judy

Bioassay-directed fractionation based upon a modification of a published technique is applied to the study of three seasonal composites of dichloromethane extracts of inhalable particulate matter collected in Newarks, New Jersey The "profiles" of mass distribution and Salmonella TA98 mutagenic activity vs polarity are similar for the three seasons. Only at the second and especially the third fractionation levels are significant differents seen with a slight shift toward more polar compounds during summer. In all three seasons, polar neutral compounds make the greatest contribution toward mutagenic activity. Hydroxynitropolyciclic aromatic hydrocarbons are difficult to analyse by GC/MS) (El and negative chemical ionization), but HPLC/UV appears to be useful. A number of techniques are emplited in the analysis of specific compounds and classes of compounds. Subsequent acetone extraction of filters yields highly polar mutagens where the acidic fractions account for most of the mutagenic activity. These compounds show significantly enhanced mutagenic activity with TA100 relative to TA98 suggesting the presence of highly polar, acidic substances that are strong alkylating agents. The compound 2-acetoxyl-1-nitronaphthalene, found in fresh diesel particalates, is shown to hydrolyse during fractionation, thus introducing a note of caution into the use of such procedures.

Quality control of herbs: determination of amino acids in Althaea officinalis, Matricaria chamomilla and Taraxacum officinale.

PubMed

Qureshi, Muhammad Nasimullah; Stecher, Guenther; Bonn, Guenther Karl

2014-05-01

Analysis of raw materials and final products need reliable methods for the standardization of natural product drugs. Legal guideline also emphasizes on the qualitative and quantitative analyses of the plant constituents in an herbal product. In this study, thin layer chromatography (TLC) and amino acid analyzer was used for the determination of amino acids in plant extracts. Samples for this study were standards and aqueous extracts from Althaea officinalis, Matricaria chamomilla and Taraxacum officinale. Different amino acids in the extracts were detected through TLC. An automatic amino acid analyzer was used for the quantification of amino acids in the plant extracts under study.

Chemical Composition Analysis of Extracts from Ficus Hirta Using Supercritical Fluid

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Antibacterial and anti-inflammatory finishing of cotton by microencapsulation using three marine organisms.

PubMed

El-Rafie, H M; El-Rafie, M H; AbdElsalam, H M; El-Sayed, W A

2016-05-01

This work is a small effort in the production of an eco-friendly natural based antibacterial and anti-inflammatory finished cotton fabrics using the ethanolic extracts (Ex) of the sea grass Halophila stipulacea (H. stipulacea) and marine macroalgae [Colbomenia sinuosa (C. sinuosa) and Ulva fasciata (U. fasciata)]. The extracts were phytochemically screened for their constituents. These extracts were used to finish cotton fabrics by a variety of methods. Concerning this, fabrics (F) were singly treated with ethanolic extracts (ExF) of these marine organisms by the dip technique and the extract encapsulated with sodium alginate or meypro gum. The encapsulated fabric (EnF) was further finished individually with citric acid (CA), (EnF/CA) and mono-tert-butyl ether of glycerol (MTBG) binder (EnF/Bin) by the pad-dry-cure technique. The fabrics so-finished were evaluated for their antibacterial and anti-inflammatory activities without washing (control) and after different washing cycles. The results obtained showed that, both EnF/CA and EnF/Bin inhibit the bacterial growth by about 90% after 10 washing cycles for both Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). The anti-inflammatory activity, the potency% reached to 88.3% for the fabric encapsulated with microcapsules of sodium alginate/H. stipulacea sea grass and the EnF/CA. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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.

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.

Comparison of in situ DGT measurement with ex situ methods for predicting cadmium bioavailability in soils with combined pollution to biotas.

PubMed

Wang, Peifang; Liu, Cui; Yao, Yu; Wang, Chao; Wang, Teng; Yuan, Ye; Hou, Jun

2017-05-01

To assess the capabilities of the different techniques in predicting Cadmium (Cd) bioavailability in Cd-contaminated soils with the addition of Zn, one in situ technique (diffusive gradients in thin films; DGT) was compared with soil solution concentration and four widely used single-step extraction methods (acetic acid, EDTA, sodium acetate and CaCl 2 ). Wheat and maize were selected as tested species. The results demonstrated that single Cd-polluted soils inhibited the growth of wheat and maize significantly compared with control plants; the shoot and root biomasses of the plants both dropped significantly (P < 0.05). The addition of Zn exhibited a strong antagonism to the physiological toxicity induced by Cd. The Pearson correlation coefficient presented positive correlations (P < 0.01, R > 0.9) between Cd concentrations in two plants and Cd bioavailability indicated by each method in soils. Consequently, the results indicated that the DGT technique could be regarded as a good predictor of Cd bioavailability to plants, comparable to soil solution concentration and the four single-step extraction methods. Because the DGT technique can offer in situ data, it is expected to be widely used in more areas.

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 latency period to the onset of seizure. Phenytoin showed interaction only with the ethanolic valerian extracts. Valerenic acid and valerian extracts have anticonvulsant properties in adult zebrafish. Valerian extracts markedly enhanced the anticonvulsant effect of both clonazepam and phenytoin, and could contribute to therapy of epileptic patients.

Direct technique for monitoring lipid oxidation in water-in-oil emulsions based on micro-calorimetry.

PubMed

Dridi, Wafa; Toutain, Jean; Sommier, Alain; Essafi, Wafa; Leal-Calderon, Fernando; Cansell, Maud

2017-09-01

An experimental device based on the measurement of the heat flux dissipated during chemical reactions, previously validated for monitoring lipid oxidation in plant oils, was extended to follow lipid oxidation in water-in-oil emulsions. Firstly, validation of the approach was performed by correlating conjugated diene concentrations measured by spectrophotometry and the heat flux dissipated by oxidation reactions and measured directly in water-in-oil emulsions, in isothermal conditions at 60°C. Secondly, several emulsions based on plant oils differing in their n-3 fatty acid content were compared. The oxidability parameter derived from the enthalpy curves reflected the α-linolenic acid proportion in the oils. On the whole, the micro-calorimetry technique provides a sensitive method to assess lipid oxidation in water-in-oil emulsions without requiring any phase extraction. Copyright © 2017 Elsevier Ltd. All rights reserved.

Leukotriene B4 catabolism: quantitation of leukotriene B4 and its omega-oxidation products by reversed-phase high-performance liquid chromatography.

PubMed

Shak, S

1987-01-01

LTB4 and its omega-oxidation products may be rapidly, sensitively, and specifically quantitated by the methods of solid-phase extraction and reversed-phase high-performance liquid chromatography (HPLC), which are described in this chapter. Although other techniques, such as radioimmunoassay or gas chromatography-mass spectrometry, may be utilized for quantitative analysis of the lipoxygenase products of arachidonic acid, only the technique of reversed-phase HPLC can quantitate as many as 10 metabolites in a single analysis, without prior derivatization. In this chapter, we also reviewed the chromatographic theory which we utilized in order to optimize reversed-phase HPLC analysis of LTB4 and its omega-oxidation products. With this information and a gradient HPLC system, it is possible for any investigator to develop a powerful assay for the potent inflammatory mediator, LTB4, or for any other lipoxygenase product of arachidonic acid.

DNA stable-isotope probing (DNA-SIP).

PubMed

Dunford, Eric A; Neufeld, Josh D

2010-08-02

DNA stable-isotope probing (DNA-SIP) is a powerful technique for identifying active microorganisms that assimilate particular carbon substrates and nutrients into cellular biomass. As such, this cultivation-independent technique has been an important methodology for assigning metabolic function to the diverse communities inhabiting a wide range of terrestrial and aquatic environments. Following the incubation of an environmental sample with stable-isotope labelled compounds, extracted nucleic acid is subjected to density gradient ultracentrifugation and subsequent gradient fractionation to separate nucleic acids of differing densities. Purification of DNA from cesium chloride retrieves labelled and unlabelled DNA for subsequent molecular characterization (e.g. fingerprinting, microarrays, clone libraries, metagenomics). This JoVE video protocol provides visual step-by-step explanations of the protocol for density gradient ultracentrifugation, gradient fractionation and recovery of labelled DNA. The protocol also includes sample SIP data and highlights important tips and cautions that must be considered to ensure a successful DNA-SIP analysis.

1H NMR study of fermented cocoa (Theobroma cacao L.) beans.

PubMed

Caligiani, Augusta; Acquotti, Domenico; Cirlini, Martina; Palla, Gerardo

2010-12-08

This study reports for the first time the metabolic profile of cocoa (Theobroma cacao L.) beans using the (1)H NMR technique applied to polar extracts of fermented cocoa beans. The simultaneous detection and quantification of amino acids, polyalcohols, organic acids, sugars, methylxanthines, catechins, and phenols were obtained by assigning the major signals of the spectra for different varieties of cocoa beans (Forastero, Criollo, and Trinitario) from different countries (Ecuador, Ghana, Grenada, and Trinidad). The data set obtained, representative of all classes of soluble compounds of cocoa, was useful to characterize the fermented cocoa beans as a function of the variety and geographic origin.

Multivariate data analysis and metabolic profiling of artemisinin and related compounds in high yielding varieties of Artemisia annua field-grown in Madagascar.

PubMed

Suberu, John; Gromski, Piotr S; Nordon, Alison; Lapkin, Alexei

2016-01-05

An improved liquid chromatography-tandem mass spectrometry (LC-MS/MS) protocol for rapid analysis of co-metabolites of A. annua in raw extracts was developed and extensively characterized. The new method was used to analyse metabolic profiles of 13 varieties of A. annua from an in-field growth programme in Madagascar. Several multivariate data analysis techniques consistently show the association of artemisinin with dihydroartemisinic acid. These data support the hypothesis of dihydroartemisinic acid being the late stage precursor to artemisinin in its biosynthetic pathway. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

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...

Chromatographic and mass spectrometric characterization of essential oils and extracts from Lippia (Verbenaceae) aromatic plants.

PubMed

Stashenko, Elena E; Martínez, Jairo R; Cala, Mónica P; Durán, Diego C; Caballero, Deyanira

2013-01-01

Analytical methodologies based on GC and HPLC were developed for the separation and quantification of carnosic acid, ursolic acid, caffeic acid, p-coumaric acid, rosmarinic acid, apigenin, luteolin, quercetin, kaempferol, naringenin, and pinocembrin. These methods were used to characterize essential oils and extracts obtained by solvent (methanol) and by supercritical fluid (CO(2)) extraction from stems and leaves of Lippia (Verbenaceae family) aromatic plants (Lippia alba, Lippia origanoides, Lippia micromera, Lippia americana, Lippia graveolens, and Lippia citriodora). Supercritical CO(2) extraction isolated solely pinocembrin and narigenin from three L. origanoides chemotypes. Solvent extracts possessed a more varied composition that additionally included apigenin, quercetin, and luteolin. Solvent extraction afforded higher overall flavonoid yields from all species in comparison with supercritical CO(2) extraction. Pinocembrin was determined in L. origanoides extract at a concentration of 30 mg/g of plant material, which is more than ten times higher than the amount at which polyphenols are regularly found in aromatic plant extracts. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Efficient Accumulation and In Vitro Antitumor Activities of Triterpene Acids from Submerged Batch--Cultured Lingzhi or Reishi Medicinal Mushroom, Ganoderma lucidum (Agaricomycetes).

PubMed

Wang, Xiao-Ling; Ding, Zhong-Yang; Zhao, Yan; Liu, Gao-Qiang; Zhou, Guo-Ying

2017-01-01

Triterpene acids are among the major bioactive constituents of lucidum. However, submerged fermentation techniques for isolating triterpene acids from G. lucidum have not been optimized for commercial use, and the antitumor activity of the mycelial triterpene acids needs to be further proven. The aim of this work was to optimize the conditions for G. lucidum culture with respect to triterpene acid production, scaling up the process, and examining the in vitro antitumor activity of mycelial triterpene acids. The key conditions (i.e., initial pH, fermentation temperature, and rotation speed) were optimized using response surface methodology, and the in vitro antitumor activity was evaluated using the MTT method. The optimum key fermentation conditions for triterpene acid production were pH 6.0; rotation speed, 161.9 rpm; and temperature, 30.1°C, resulting in a triterpene acid yield of 291.0 mg/L in the validation experiment in a 5-L stirred bioreactor; this yield represented a 70.8% increase in titer compared with the nonoptimized conditions. Furthermore, the optimized conditions were then successfully scaled up to a production scale of 200 L, and a triterpene productivity of 47.9 mg/L/day was achieved, which is, to our knowledge, the highest reported in the large-scale fermentation of G. lucidum. In addition, the mycelial triterpene acids were found to be cytotoxic to the SMMC-7721 and SW620 cell lines in vitro. Chemical analysis showed that the key active triterpene acid compounds, ganoderic acids T and Me, predominated in the extract, at 69.2 and 41.6 mg/g, respectively. Thus, this work develops a simple and feasible batch fermentation technique for the large-scale production of antitumor triterpene acids from G. lucidum.

HPLC-PDA analysis and anti-inflammatory effects of Mori Cortex Radicis.

PubMed

Seo, Chang-Seob; Lim, Hye-Sun; Jeong, Soo-Jin; Ha, Hyekyung; Shin, Hyeun-Kyoo

2013-10-01

Mori Cortex Radicis (MCR, Moraceae) is used traditionally in the treatment ofjaundice, hematemesis, edema, and pollakisuria in Korea. In this study, the antiinflammatory effects of MCR extract were investigated using RAW 264.7 cells. The simultaneous analysis of five components present (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, and p-coumaric acid) in the MCR extract was performed using high-performance liquid chromatography (HPLC) coupled with photodiode array (PDA) detection. We determined the effects of MCR extract and its components on the production of nitric oxide (NO), prostaglandin E2 (PGE2), and mRNA expression of cyclooxygenase-2 (COX-2) in RAW 264.7 cells. MCR extract suppressed the production of NO and PGE2 in RAW 264.7 cells in a dose-dependent manner. None of the five components of the MCR extract had any influence on the production of NO. However, caffeic acid and p-coumaric acid inhibited the production of PGE2 and mRNA expression of COX-2 in RAW 264.7 cells. Our results suggest that MCR extract may offer potential as a therapeutic agent for the treatment of inflammation. The method we have established will help to improve the quality control of MCR extracts.

Extraction of amino acids from aerogel for analysis by capillary electrophoresis. Implications for a mission concept to Enceladus' Plume.

PubMed

Mora, Maria F; Jones, Steve M; Creamer, Jessica; Willis, Peter A

2018-02-01

Ocean worlds like Europa and Enceladus in the outer solar system are prime targets in the search for life beyond Earth. Enceladus is particularly interesting due to the presence of a water plume ejecting from the south polar region. The recent discovery of H 2 in the plume, in addition to the presence of previously observed organic compounds, highlights the possibility of life in this moon. The plume provides materials from the underlying ocean that could be collected simply by flying through it. The presence of the plume means that material from the ocean is available for collection during a flyby, without the need for landing or complex sample handling operations such as scooping or drilling. An attractive approach to preserve the organics in particles collected during flyby encounters would be to utilize silica aerogel, the material used to collect particles at hypervelocity during the Stardust mission. Here we demonstrate amino acids can be extracted from aerogel simply by adding water. This simple liquid extraction method could be implemented during a mission prior to analysis with a liquid-based technique like capillary electrophoresis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of perfluorinated compounds in fish fillet homogenates: method validation and application to fillet homogenates from the Mississippi River.

PubMed

Malinsky, Michelle Duval; Jacoby, Cliffton B; Reagen, William K

2011-01-10

We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7-C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill (Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100±13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented. Copyright © 2010 Elsevier B.V. All rights reserved.

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.

Recovering Bioactive Compounds from Olive Oil Filter Cake by Advanced Extraction Techniques

PubMed Central

Lozano-Sánchez, Jesús; Castro-Puyana, María; Mendiola, Jose A.; Segura-Carretero, Antonio; Cifuentes, Alejandro; Ibáñez, Elena

2014-01-01

The potential of by-products generated during extra-virgin olive oil (EVOO) filtration as a natural source of phenolic compounds (with demonstrated bioactivity) has been evaluated using pressurized liquid extraction (PLE) and considering mixtures of two GRAS (generally recognized as safe) solvents (ethanol and water) at temperatures ranging from 40 to 175 °C. The extracts were characterized by high-performance liquid chromatography (HPLC) coupled to diode array detection (DAD) and electrospray time-of-flight mass spectrometry (HPLC-DAD-ESI-TOF/MS) to determine the phenolic-composition of the filter cake. The best isolation procedure to extract the phenolic fraction from the filter cake was accomplished using ethanol and water (50:50, v/v) at 120 °C. The main phenolic compounds identified in the samples were characterized as phenolic alcohols or derivatives (hydroxytyrosol and its oxidation product), secoiridoids (decarboxymethylated and hydroxylated forms of oleuropein and ligstroside aglycones), flavones (luteolin and apigenin) and elenolic acid derivatives. The PLE extraction process can be applied to produce enriched extracts with applications as bioactive food ingredients, as well as nutraceuticals. PMID:25226536

Biological, chemical and in silico fingerprints of Dianthus calocephalus Boiss.: A novel source for rutin.

PubMed

Uysal, Sengul; Aktumsek, Abdurrahman; Picot-Allain, Carene M N; Unuvar, Hamiyet; Mollica, Adriano; Georgiev, Milen I; Zengin, Gokhan; Mahomoodally, Mohamad Fawzi

2018-03-01

Extracts (methanol, ethyl acetate, and water) from Dianthus calocephalus Boiss. prepared by different extraction techniques (maceration, Soxhlet, and ultrasonication) were studied for possible inhibitory action against key enzymes (α-amylase, α-glucosidase, acetyl cholinesterase, butyryl cholinesterase, and tyrosinase). Antioxidant potential was established using a battery of assays and phenolic compounds profiled by RP-HPLC. Binding pose of tyrosinase with rutin was studied by means of molecular docking. Methanol extracts showed the highest phenolic (39.35-40.25 mgGAE/g) content and rich in rutin (61.38-72.07 mg/g extract). Ethyl acetate extracts of D. calocephalus were potent inhibitors of acetyl (1.45-1.48 mgGALAE/g) and butyryl (2.44-2.74 mgGALAE/g) cholinesterases. Docking studies showed that rutin interacts with the side chains of the key amino acid residues and to the copper atom found at the active site of tyrosinase. Methanol extracts showed highest antioxidant capacity. D. calocephalus showed interesting biological properties that could be further studied to manage diabetes, neurodegenerative diseases, Alzheimer's disease, and hyperpigmentation. Copyright © 2018 Elsevier Ltd. All rights reserved.

Investigation of cloud point extraction for the analysis of metallic nanoparticles in a soil matrix

PubMed Central

Hadri, Hind El; Hackley, Vincent A.

2017-01-01

The characterization of manufactured nanoparticles (MNPs) in environmental samples is necessary to assess their behavior, fate and potential toxicity. Several techniques are available, but the limit of detection (LOD) is often too high for environmentally relevant concentrations. Therefore, pre-concentration of MNPs is an important component in the sample preparation step, in order to apply analytical tools with a LOD higher than the ng kg−1 level. The objective of this study was to explore cloud point extraction (CPE) as a viable method to pre-concentrate gold nanoparticles (AuNPs), as a model MNP, spiked into a soil extract matrix. To that end, different extraction conditions and surface coatings were evaluated in a simple matrix. The CPE method was then applied to soil extract samples spiked with AuNPs. Total gold, determined by inductively coupled plasma mass spectrometry (ICP-MS) following acid digestion, yielded a recovery greater than 90 %. The first known application of single particle ICP-MS and asymmetric flow field-flow fractionation to evaluate the preservation of the AuNP physical state following CPE extraction is demonstrated. PMID:28507763