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

PubMed

Crompton, Marcus J; Dunstan, R Hugh

2018-05-01

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

Selective Extraction and Purification of Azaspiracids from Blue Mussels ( Mytilus edulis) Using Boric Acid Gel.

PubMed

Miles, Christopher O; Kilcoyne, Jane; McCarron, Pearse; Giddings, Sabrina D; Waaler, Thor; Rundberget, Thomas; Samdal, Ingunn A; Løvberg, Kjersti E

2018-03-21

Azaspiracids belong to a family of more than 50 polyether toxins originating from marine dinoflagellates such as Azadinium spinosum. All of the azaspiracids reported thus far contain a 21,22-dihydroxy group. Boric acid gel can bind selectively to compounds containing vic-diols or α-hydroxycarboxylic acids via formation of reversible boronate complexes. Here we report use of the gel to selectively capture and release azaspiracids from extracts of blue mussels. Analysis of the extracts and fractions by liquid chromatography-tandem mass spectrometry (LC-MS) showed that this procedure resulted in an excellent cleanup of the azaspiracids in the extract. Analysis by enzyme-linked immunoasorbent assay (ELISA) and LC-MS indicated that most azaspiracid analogues were recovered in good yield by this procedure. The capacity of boric acid gel for azaspiracids was at least 50 μg/g, making this procedure suitable for use in the early stages of preparative purification of azaspiracids. In addition to its potential for concentration of dilute samples, the extensive cleanup provided by boric acid gel fractionation of azaspiracids in mussel samples almost eliminated matrix effects during subsequent LC-MS and could be expected to reduce matrix effects during ELISA analysis. The method may therefore prove useful for quantitative analysis of azaspiracids as part of monitoring programs. Although LC-MS data showed that okadaic acid analogues also bound to the gel, this was much less efficient than for azaspiracids under the conditions used. The boric acid gel methodology is potentially applicable to other important groups of natural toxins containing diols including ciguatoxins, palytoxins, pectenotoxins, tetrodotoxin, trichothecenes, and toxin glycosides.

A new procedure for extraction of collagen from modern and archaeological bones for 14C dating.

PubMed

Maspero, F; Sala, S; Fedi, M E; Martini, M; Papagni, A

2011-10-01

Bones are potentially the best age indicators in a stratigraphic study, because they are closely related to the layer in which they are found. Collagen is the most suitable fraction and is the material normally used in radiocarbon dating. Bone contaminants can strongly alter the carbon isotopic fraction values of the samples, so chemical pretreatment for (14)C dating by accelerator mass spectrometry (AMS) is essential. The most widespread method for collagen extraction is based on the Longin procedure, which consists in HCl demineralization to dissolve the inorganic phase of the samples, followed by dissolution of collagen in a weak acid solution. In this work the possible side effects of this procedure on a modern bone are presented; the extracted collagen was analyzed by ATR-IR spectroscopy. An alternative procedure, based on use of HF instead of HCl, to minimize unwanted degradation of the organic fraction, is also given. A study by ATR-IR spectroscopic analysis of collagen collected after different demineralization times and with different acid volumes, and a study of an archaeological sample, are also presented.

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

PubMed

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

2016-02-04

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

Compositional similarities of non-solvent extractable fatty acids from recent marine sediments deposited in differing environments

NASA Astrophysics Data System (ADS)

Nishimura, Mitsugu; Baker, Earl W.

1987-06-01

Five recent sediment samples from a variety of North American continental shelves were analyzed for fatty acids (FAs) in the solvent-extractable (SOLEX) lipids as well as four types of non-solvent extractable (NONEX) lipids. The NONEX lipids were operationally defined by the succession of extraction procedure required to recover them. The complete procedure included (i) very mild acid treatment, (ii) HF digestion and (iii) saponification of the sediment residue following exhaustive solvent extraction. The distribution pattern and various compositional parameters of SOLEX FAs in the five sediments were divided into three different groups, indicating the difference of biological sources and also diagenetic factors and processes among the three groups of samples. Nevertheless, the compositions of the corresponding NONEX FAs after acid treatment were surprisingly very similar. This was also true for the remaining NONEX FA groups in the five sediment samples. The findings implied that most of the NONEX FAs reported here are derived directly from living organisms. It is also concluded that a large part of NONEX FAs are much more resistant to biodegradation than we have thought, so that they can form the large percentage of total lipids with increasing depth of water and sediments.

A simple and efficient ultrasonic-assisted extraction procedure combined with UV-Vis spectrophotometry for the pre-concentration and determination of folic acid (vitamin B9) in various sample matrices.

PubMed

Gürkan, Ramazan; Altunay, Nail

2016-07-01

A simple and efficient ultrasonic-assisted extraction (UAE) procedure has been proposed for the pre-concentration of (2S)-2-[(4-{[(2-amino-4-hydroxypteridin-yl)methyl]amino}phenyl)formamido]pentanedioic acid (folic acid) in vegetables, pharmaceuticals and foods prior to determination at 540 nm using UV-Vis spectrophotometry. The method is based on hydrophobic ternary complex formation of folic acid with silver ions in the presence of cetyltrimethylammonium bromide (CTAB) as a sensitivity enhancer counter ion at pH 7.0, and then extraction into a micellar phase of polyethylene glycol monoalkyl ether (Genapol X-080). The impacts on the extraction efficiency and complex formation of analytical parameters such as sample pH, concentration of silver, concentration of surfactants and extraction time, ultrasonic time and sample volume, were investigated and optimised in detail. The matrix effect on the pre-concentration and determination of folic acid was investigated, and it was observed that the proposed method was highly selective against possible matrix co-extractives. Under optimised conditions, a good linear relationship between the analytical signal and folic acid concentration was obtained in the range of 0.6-180 μg l(-1) with a detection limit of 0.19 μg l(-1) and quantification limit of 0.63 μg l(-1). The applicability was evaluated using samples fortified at different concentration levels, and recoveries higher than 94.1% were obtained. The precision as the percent relative standard deviation (RSD%) was in range of 2.5-3.8% (10 and 40 μg l(-1), n = 5). The proposed method was validated by analysis of two standard reference materials (SRMs) and various real samples, and satisfactory results were obtained.

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.

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.

Phytochemistry of cimicifugic acids and associated bases in Cimicifuga racemosa root extracts.

PubMed

Gödecke, Tanja; Nikolic, Dejan; Lankin, David C; Chen, Shao-Nong; Powell, Sharla L; Dietz, Birgit; Bolton, Judy L; van Breemen, Richard B; Farnsworth, Norman R; Pauli, Guido F

2009-01-01

Earlier studies reported serotonergic activity for cimicifugic acids (CA) isolated from Cimicifuga racemosa. The discovery of strongly basic alkaloids, cimipronidines, from the active extract partition and evaluation of previously employed work-up procedures has led to the hypothesis of strong acid/base association in the extract. Re-isolation of the CAs was desired to permit further detailed studies. Based on the acid/base association hypothesis, a new separation scheme of the active partition was required, which separates acids from associated bases. A new 5-HT(7) bioassay guided work-up procedure was developed that concentrates activity into one partition. The latter was subjected to a new two-step centrifugal partitioning chromatography (CPC) method, which applies pH zone refinement gradient (pHZR CPC) to dissociate the acid/base complexes. The resulting CA fraction was subjected to a second CPC step. Fractions and compounds were monitored by (1)H NMR using a structure-based spin-pattern analysis facilitating dereplication of the known acids. Bioassay results were obtained for the pHZR CPC fractions and for purified CAs. A new CA was characterised. While none of the pure CAs was active, the serotonergic activity was concentrated in a single pHZR CPC fraction, which was subsequently shown to contain low levels of the potent 5-HT(7) ligand, N(omega)-methylserotonin. This study shows that CAs are not responsible for serotonergic activity in black cohosh. New phytochemical methodology (pHZR CPC) and a sensitive dereplication method (LC-MS) led to the identification of N(omega)-methylserotonin as serotonergic active principle. Copyright (c) 2009 John Wiley & Sons, Ltd.

Phytochemistry of Cimicifugic Acids and Associated Bases in Cimicifuga racemosa Root Extracts

PubMed Central

GÖdecke, Tanja; Nikolic, Dejan; Lankin, David C.; Chen, Shao-Nong; Powell, Sharla L.; Dietz, Birgit; Bolton, Judy L.; Van Breemen, Richard B.; Farnsworth, Norman R.; Pauli, Guido F.

2009-01-01

Introduction Earlier studies reported serotonergic activity for cimicifugic acids (CA) isolated from Cimicifuga racemosa. The discovery of strongly basic alkaloids, cimipronidines, from the active extract partition and evaluation of previously employed work-up procedures has led to the hypothesis of strong acid/base association in the extract. Objective Re-isolation of the CAs was desired to permit further detailed studies. Based on the acid/base association hypothesis, a new separation scheme of the active partition was required, which separates acids from associated bases. Methodology A new 5-HT7 bioassay guided work-up procedure was developed that concentrates activity into one partition. The latter was subjected to a new 2-step centrifugal partitioning chromatography (CPC) method, which applies pH zone refinement gradient (pHZR CPC) to dissociate the acid/base complexes. The resulting CA fraction was subjected to a second CPC step. Fractions and compounds were monitored by 1H NMR using a structure based spin-pattern analysis facilitating dereplication of the known acids. Bioassay results were obtained for the pHZR CPC fractions and for purified CAs. Results A new CA was characterized. While none of the pure CAs was active, the serotonergic activity was concentrated in a single pHZR CPC fraction, which was subsequently shown to contain low levels of the potent 5-HT7 ligand, Nω–methylserotonin. Conclusion This study shows that CAs are not responsible for serotonergic activity in black cohosh. New phytochemical methodology (pHZR CPC) and a sensitive dereplication method (LC-MS) led to the identification of Nω–methylserotonin as serotonergic active principle. PMID:19140115

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

PubMed

Szwengiel, Artur; Stachowiak, Barbara

2016-08-01

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

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DERMAL WIPE AND SURFACE WIPE SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.27)

EPA Science Inventory

The method for extracting and preparing a dermal or surface wipe sample for analysis of acidic persistent organic pollutants is summarized in this standard operating procedure. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mas...

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.

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

PubMed

Sheikhian, Leila; Bina, Sedigheh

2016-01-15

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

Determination of Oleanolic and Ursolic Acids in Hedyotis diffusa Using Hyphenated Ultrasound-Assisted Supercritical Carbon Dioxide Extraction and Chromatography

PubMed Central

Hong, Show-Jen

2015-01-01

Oleanolic acid (OA) and ursolic acid (UA) were extracted from Hedyotis diffusa using a hyphenated procedure of ultrasound-assisted and supercritical carbon dioxide (HSC–CO2) extraction at different temperatures, pressures, cosolvent percentages, and SC–CO2 flow rates. The results indicated that these parameters significantly affected the extraction yield. The maximal yields of OA (0.917 mg/g of dry plant) and UA (3.540 mg/g of dry plant) were obtained at a dynamic extraction time of 110 min, a static extraction time of 15 min, 28.2 MPa, and 56°C with a 12.5% (v/v) cosolvent (ethanol/water = 82/18, v/v) and SC–CO2 flowing at 2.3 mL/min (STP). The extracted yields were then analyzed by high performance liquid chromatography (HPLC) to quantify the OA and UA. The present findings revealed that H. diffusa is a potential source of OA and UA. In addition, using the hyphenated procedure for extraction is a promising and alternative process for recovering OA and UA from H. diffusa at high concentrations. PMID:26089939

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.

The enrichment of chlorogenic acid from Eucommia ulmoides leaves extract by mesoporous carbons.

PubMed

Qin, Guotong; Ma, Jing; Wei, Wei; Li, Jaja; Yue, Fangqing

2018-06-15

Herein, we report an efficient separation and enrichment method for chlorogenic acid from crude extracts of Eucommia ulmoides leaves using carbon adsorbents. The effects of the pore structure of the carbon adsorbents on the adsorption capacity were studied. Of the four adsorbents investigated, mesoporous carbon (MC3) showed the highest adsorption capacity (294 mg/g of carbon) for chlorogenic acid due to its high mesopore volume. The static adsorption of CGA on carbon can be accurately described using the Freundlich equation. The kinetics of adsorption follow a pseudo-second-order process. External mass transfer was the controlling step of the adsorption process. Dynamic adsorption on MC3 demonstrated that chlorogenic acid began to break through after 28 bed volumes of extract was loaded. This mesoporous carbon-treatment procedure is safe, economic and has the potential to be scaled up for commercial application. Copyright © 2018 Elsevier B.V. All rights reserved.

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2013 CFR

2013-04-01

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

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2011 CFR

2011-04-01

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

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2012 CFR

2012-04-01

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

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2010 CFR

2010-04-01

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

Process for the extraction of strontium from acidic solutions

DOEpatents

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

1994-09-06

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

Comparison of whole-cell fatty acid (MIDI) or phospholipid fatty acid (PLFA) extractants as biomarkers to profile soil microbial communities.

PubMed

Fernandes, Marcelo F; Saxena, Jyotisna; Dick, Richard P

2013-07-01

The whole-cell lipid extraction to profile microbial communities on soils using fatty acid (FA) biomarkers is commonly done with the two extractants associated with the phospholipid fatty acid (PLFA) or Microbial IDentification Inc. (MIDI) methods. These extractants have very different chemistry and lipid separation procedures, but often shown a similar ability to discriminate soils from various management and vegetation systems. However, the mechanism and the chemistry of the exact suite of FAs extracted by these two methods are poorly understood. Therefore, the objective was to qualitatively and quantitatively compare the MIDI and PLFA microbial profiling methods for detecting microbial community shifts due to soil type or management. Twenty-nine soil samples were collected from a wide range of soil types across Oregon and extracted FAs by each method were analyzed by gas chromatography (GC) and GC-mass spectrometry. Unlike PLFA profiles, which were highly related to microbial FAs, the overall MIDI-FA profiles were highly related to the plant-derived FAs. Plant-associated compounds were quantitatively related to particulate organic matter (POM) and qualitatively related to the standing vegetation at sampling. These FAs were negatively correlated to respiration rate normalized to POM (RespPOM), which increased in systems under more intensive management. A strong negative correlation was found between MIDI-FA to PLFA ratios and total organic carbon (TOC). When the reagents used in MIDI procedure were tested for the limited recovery of MIDI-FAs from soil with high organic matter, the recovery of MIDI-FA microbial signatures sharply decreased with increasing ratios of soil to extractant. Hence, the MIDI method should be used with great caution for interpreting changes in FA profiles due to shifts in microbial communities.

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

Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

PubMed

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2018-01-01

The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

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.

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

PubMed

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

2014-06-15

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

Binary Solvent Extraction of Tocols, γ-Oryzanol, and Ferulic Acid from Rice Bran Using Alkaline Treatment Combined with Ultrasonication.

PubMed

Truong, Hoa Thi; Luu, Phuong Duc; Imamura, Kiyoshi; Matsubara, Takeo; Takahashi, Hideki; Takenaka, Norimichi; Boi, Luu Van; Maeda, Yasuaki

2017-06-21

Alkaline treatment (Alk) combined with ultrasound-assisted extraction (UAE) (Alk+UAE) was examined as a means of extracting tocols and γ-oryzanol from rice bran into an organic phase while simultaneously recovering ferulic acid into an aqueous phase. The tocols and γ-oryzanol/ferulic acid yields were determined using high-performance liquid chromatography with fluorescence and UV detection. The effects of extraction conditions were evaluated by varying the Alk treatment temperature and extraction duration. The maximum yields of tocols and γ-oryzanol were obtained at 25 °C over a time span of 30 min. When the temperature was increased to 80 °C, the yield of ferulic acid increased dramatically, whereas the recovery of γ-oryzanol slightly decreased. Employing the Alk+UAE procedure, the recovered concentrations of tocols, γ-oryzanol, and ferulic acid were in the ranges of 146-518, 1591-3629, and 352-970 μg/g, respectively. These results are in good agreement with those reported for rice bran samples from Thailand.

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.

Subcritical Water Extraction of Amino Acids from Atacama Desert Soils

NASA Technical Reports Server (NTRS)

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

2007-01-01

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

21 CFR 173.280 - Solvent extraction process for citric acid.

Code of Federal Regulations, 2014 CFR

2014-04-01

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

Storage method, drying processes and extraction procedures strongly affect the phenolic fraction of rosemary leaves: an HPLC/DAD/MS study.

PubMed

Mulinacci, N; Innocenti, M; Bellumori, M; Giaccherini, C; Martini, V; Michelozzi, M

2011-07-15

The Rosmarinus officinalis L. is widely known for its numerous applications in the food field but also for the increasing interest in its pharmaceutical properties. Two groups of compounds are mainly responsible for the biological activities of the plant: the volatile fraction and the phenolic constituents. The latter group is mainly constituted by rosmarinic acid, by a flavonoidic fraction and by some diterpenoid compounds structurally derived from the carnosic acid. The aim of our work was to optimize the extractive and analytical procedure for the determination of all the phenolic constituents. Moreover the chemical stability of the main phenols, depending on the storage condition, the different drying procedures and the extraction solvent, have been evaluated. This method allowed to detect up to 29 different constituents at the same time in a relatively short time. The described procedure has the advantage to being able to detect and quantify several classes of compounds, among them numerous minor flavonoids, thus contributing to improving knowledge of the plant. The findings from this study have demonstrated that storing the raw fresh material in the freezer is not appropriate for rosemary, mainly due to the rapid disappearing of the rosmarinic acid during the freezing/thawing process. Regarding the flavonoidic fraction, consistent decrements, were highlighted in the dried samples at room temperature if compared with the fresh leaf. Rosmarinic acid, appeared very sensitive also to mild drying processes. The total diterpenoidic content undergoes to little changes when the leaves are freeze dried or frozen and limited losses are observed working on dried leaves at room temperature. Nevertheless it can be taken in account that this fraction is very sensitive to the water presence during the extraction that favors the conversion of carnosic acid toward it oxidized form carnosol. From our findings, it appear evident that when evaluating the phenolic content in

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.

Analysis of free and bound chlorophenoxy acids in cereals.

PubMed

Lokke, H

1975-06-01

Extraction of the chlorophenoxy acids 2,4-D and dichlorprop in cereals has been examined by analyzing barley from spraying experiments. A procedure has been set up by combination of acid hydrolysis and enzymatic degradation followed by extraction and clean up on either silica gel or basic aluminum oxide. The final determination is based on reaction with diazomethane and subsequently GLC with ECD. This procedure was compared with two different extraction procedures previously described in the literature. The one comparative procedure uses a mixture of 50% diethyl ether/hexane in presence of sulphuric acid and resulted in residues up to ten times lower than found after the combined acid hydrolysis/enzymatic degradation procedure. In the second comparison a direct extraction was made with a mixture of 65% (v/v) acetonitrile in water. No differences were found between this and the combined acid hydrolysis/enzymatic degradation procedure.

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

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.

Optimization of acidic extraction of astaxanthin from Phaffia rhodozyma *

PubMed Central

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

2008-01-01

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

Determination of available phosphorus in soils by using a new extraction procedure and a flow injection amperometric system.

PubMed

Jakmunee, Jaroon; Junsomboon, Jaroon

2009-09-15

A new extraction procedure based on an off-line extraction column was proposed for extracting of available phosphorus from soils. The column was fabricated from a plastic syringe fitted at the bottom with a cotton wool and a piece of filter paper to support a soil sample. An aliquot (50 mL) of extracting solution (0.05 M HCl+0.0125 M H(2)SO(4)) was used to extract the sample under gravity flow and the eluate was collected in a polyethylene bottle. The extract was then analyzed for phosphorus contents by a simple flow injection amperometric system, employing a set of three-way solenoid valves as an injection valve. The method is based on the electrochemical reduction of 12-molybdophosphate which is produced on-line by the reaction of orthophosphate with acidic molybdate and the electrical current produced was directly proportional to the concentration of phosphate in range of 0.1-10.0 mg L(-1) PO(4)-P, with a detection limit of 0.02 mg L(-1). Relative standard for 11 replicate injections of 5 mg L(-1) PO(4)-P was 0.5%. A sample through put of 35 h(-1) was achieved, with consumption of 14 mg KCl, 10mg ammonium molybdate and 0.05 mL H(2)SO(4) per analysis. The detection system does not suffer from the interferences that are encountered in the photometric method such as colored substances, colloids, metal ions, silicate and refractive index effect (Schlieren effect). The results obtained by the column extraction procedure were well correlated with those obtained by the steady-state extraction procedure, but showed slightly higher extraction efficiency.

A biotin-drug extraction and acid dissociation (BEAD) procedure to eliminate matrix and drug interference in a protein complex anti-drug antibody (ADA) isotype specific assay.

PubMed

Niu, Hongmei; Klem, Thomas; Yang, Jinsong; Qiu, Yongchang; Pan, Luying

2017-07-01

Monitoring anti-drug antibody (ADA) responses in patients receiving protein therapeutics treatment is an important safety assessment for regulatory agencies, drug manufacturers, clinicians and patients. Recombinant human IGF-1/IGFBP-3 (rhIGF-1/rhIGFBP-3) is a 1:1 formulation of naturally occurring protein complex. The individual IGF-1 and IGFBP-3 proteins have multiple binding partners in serum matrix with high binding affinity to each other, which presents challenges in ADA assay development. We have developed a biotin-drug extraction with acid dissociation (BEAD) procedure followed by an electrochemiluminescence (ECL) direct assay to overcome matrix and drug interference. The method utilizes two step acid dissociation and excess biotin-drug to extract total ADA, which are further captured by soluble biotin-drug and detected in an ECL semi-homogeneous direct assay format. The pre-treatment method effectively eliminates interference by serum matrix and free drug, and enhances assay sensitivity. The assays passed acceptance criteria for all validation parameters, and have been used for clinical sample Ab testing. This method principle exemplifies a new approach for anti-isotype ADA assays, and could be an effective strategy for neutralizing antibody (NAb), pharmacokinetic (PK) and biomarker analysis in need of overcoming interference factors. Copyright © 2017 Elsevier B.V. All rights reserved.

Extractive fermentation of acetic acid

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

Busche, R.M.

1991-12-31

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

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

PubMed

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

2017-05-01

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

A Procedure for the supercritical fluid extraction of coal samples, with subsequent analysis of extracted hydrocarbons

USGS Publications Warehouse

Kolak, Jonathan J.

2006-01-01

Introduction: This report provides a detailed, step-by-step procedure for conducting extractions with supercritical carbon dioxide (CO2) using the ISCO SFX220 supercritical fluid extraction system. Protocols for the subsequent separation and analysis of extracted hydrocarbons are also included in this report. These procedures were developed under the auspices of the project 'Assessment of Geologic Reservoirs for Carbon Dioxide Sequestration' (see http://pubs.usgs.gov/fs/fs026-03/fs026-03.pdf) to investigate possible environmental ramifications associated with CO2 storage (sequestration) in geologic reservoirs, such as deep (~1 km below land surface) coal beds. Supercritical CO2 has been used previously to extract contaminants from geologic matrices. Pressure-temperature conditions within deep coal beds may render CO2 supercritical. In this context, the ability of supercritical CO2 to extract contaminants from geologic materials may serve to mobilize noxious compounds from coal, possibly complicating storage efforts. There currently exists little information on the physicochemical interactions between supercritical CO2 and coal in this setting. The procedures described herein were developed to improve the understanding of these interactions and provide insight into the fate of CO2 and contaminants during simulated CO2 injections.

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.

Predicting the difficulty of a lead extraction procedure: the LED index.

PubMed

Bontempi, Luca; Vassanelli, Francesca; Cerini, Manuel; D'Aloia, Antonio; Vizzardi, Enrico; Gargaro, Alessio; Chiusso, Francesco; Mamedouv, Rashad; Lipari, Alessandro; Curnis, Antonio

2014-08-01

According to recent surveys, many sites performing permanent lead extractions do not meet the minimum prerequisites concerning personnel training, procedures' volume, or facility requirements. The current Heart Rhythm Society consensus on lead extractions suggests that patients should be referred to more experienced sites when a better outcome could be achieved. The purpose of this study was to develop a score aimed at predicting the difficulty of a lead extraction procedure through the analysis of a high-volume center database. This score could help to discriminate patients who should be sent to a referral site. A total of 889 permanent leads were extracted from 469 patients. All procedures were performed from January 2009 to May 2012 by two expert electrophysiologists, at the University Hospital of Brescia. Factors influencing the difficulty of a procedure were assessed using a univariate and a multivariate logistic regression model. The fluoroscopy time of the procedure was taken as an index of difficulty. A Lead Extraction Difficulty (LED) score was defined, considering the strongest predictors. Overall, 873 of 889 (98.2%) leads were completely removed. Major complications were reported in one patient (0.2%) who manifested cardiac tamponade. Minor complications occurred in six (1.3%) patients. No deaths occurred. Median fluoroscopic time was 8.7 min (3.3-17.3). A procedure was classified as difficult when fluoroscopy time was more than 31.2 min [90th percentile (PCTL)].At a univariate analysis, the number of extracted leads and years from implant were significantly associated with an increased risk of fluoroscopy time above 90th PCTL [odds ratio (OR) 1.51, 95% confidence interval (CI) 1.08-2.11, P = 0.01; and OR 1.19, 95% CI 1.12-1.25, P < 0.001, respectively). After adjusting for patient age and sex, and combining with other covariates potentially influencing the extraction procedure, a multivariate analysis confirmed a 71% increased risk of fluoroscopy time

Antibacterial effect of roselle extracts (Hibiscus sabadariffa), sodium hypochlorite and acetic acid against multidrug-resistant Salmonella strains isolated from tomatoes.

PubMed

Gutiérrez-Alcántara, E J; Rangel-Vargas, E; Gómez-Aldapa, C A; Falfan-Cortes, R N; Rodríguez-Marín, M L; Godínez-Oviedo, A; Cortes-López, H; Castro-Rosas, J

2016-02-01

Antibiotic-resistant Salmonella strains were isolated from saladette and red round type tomatoes, and an analysis done of the antibacterial activity of roselle calyx extracts against any of the identified strains. One hundred saladette tomato samples and 100 red round tomato samples were collected from public markets. Each sample consisted of four whole tomatoes. Salmonella was isolated from the samples by conventional culture procedure. Susceptibility to 16 antibiotics was tested for the isolated Salmonella strains by standard test. The antibacterial effect of four roselle calyx extracts (water, methanol, acetone and ethyl acetate), sodium hypochlorite and acetic acid against antibiotic-resistant Salmonella isolates was evaluated on contaminated tomatoes. Twenty-four Salmonella strains were isolated from 12% of each tomato type. Identified Salmonella serotypes were Typhimurium and Typhi. All isolated strains exhibited resistance to at least three antibiotics and some to as many as 12. Over contaminated tomatoes, the roselle calyx extracts produced a greater reduction (2-2·6 log) in antibiotic-resistant Salmonella strain concentration than sodium hypochlorite and acetic acid. The presence of multidrug-resistant Salmonella in vegetables is a significant public health concern. Multidrug-resistant Salmonella strains were isolated from raw tomatoes purchased in public markets in Mexico and challenged with roselle Hibiscus sabdariffa calyx extracts, sodium hypochlorite and acetic acid. On tomatoes, the extracts caused a greater reduction in the concentration of antibiotic-resistant Salmonella strains than sodium hypochlorite and acetic acid. Roselle calyx extracts are a potentially useful addition to disinfection procedures of raw tomatoes in the field, processing plants, restaurants and homes. © 2015 The Society for Applied Microbiology.

40 CFR 60.648 - Optional procedure for measuring hydrogen sulfide in acid gas-Tutwiler Procedure. 1

Code of Federal Regulations, 2011 CFR

2011-07-01

... hydrogen sulfide in acid gas-Tutwiler Procedure. 1 60.648 Section 60.648 Protection of Environment... procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure. 1 1 Gas Engineers Handbook, Fuel.... In principle, this method consists of titrating hydrogen sulfide in a gas sample directly with a...

40 CFR 60.648 - Optional procedure for measuring hydrogen sulfide in acid gas-Tutwiler Procedure. 1

Code of Federal Regulations, 2010 CFR

2010-07-01

... hydrogen sulfide in acid gas-Tutwiler Procedure. 1 60.648 Section 60.648 Protection of Environment... procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure. 1 1 Gas Engineers Handbook, Fuel.... In principle, this method consists of titrating hydrogen sulfide in a gas sample directly with a...

40 CFR 60.648 - Optional procedure for measuring hydrogen sulfide in acid gas-Tutwiler Procedure. 1

Code of Federal Regulations, 2012 CFR

2012-07-01

... hydrogen sulfide in acid gas-Tutwiler Procedure. 1 60.648 Section 60.648 Protection of Environment... procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure. 1 1 Gas Engineers Handbook, Fuel.... In principle, this method consists of titrating hydrogen sulfide in a gas sample directly with a...

As, Cd, Cr, Ni and Pb pressurized liquid extraction with acetic acid from marine sediment and soil samples

NASA Astrophysics Data System (ADS)

Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; López-Mahía, Purificación; Muniategui-Lorenzo, Soledad; Prada-Rodríguez, Darío; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Adela; Bermejo-Barrera, Pilar

2006-12-01

Rapid leaching procedures by Pressurized Liquid Extraction (PLE) have been developed for As, Cd, Cr, Ni and Pb leaching from environmental matrices (marine sediment and soil samples). The Pressurized Liquid Extraction is completed after 16 min. The released elements by acetic acid Pressurized Liquid Extraction have been evaluated by inductively coupled plasma-optical emission spectrometry. The optimum multi-element leaching conditions when using 5.0 ml stainless steel extraction cells, were: acetic acid concentration 8.0 M, extraction temperature 100 °C, pressure 1500 psi, static time 5 min, flush solvent 60%, two extraction steps and 0.50 g of diatomaceous earth as dispersing agent (diatomaceous earth mass/sample mass ratio of 2). Results have showed that high acetic acid concentrations and high extraction temperatures increase the metal leaching efficiency. Limits of detection (between 0.12 and 0.5 μg g - 1 ) and repeatability of the over-all procedure (around 6.0%) were assessed. Finally, accuracy was studied by analyzing PACS-2 (marine sediment), GBW-07409 (soil), IRANT-12-1-07 (cambisol soil) and IRANT-12-1-08 (luvisol soil) certified reference materials (CRMs). These certified reference materials offer certified concentrations ranges between 2.9 and 26.2 μg g - 1 for As, from 0.068 to 2.85 μg g - 1 for Cd, between 26.4 and 90.7 μg g - 1 for Cr, from 9.3 to 40.0 μg g - 1 for Ni and between 16.3 and 183.0 μg g - 1 for Pb. Recoveries after analysis were between 95.7 and 105.1% for As, 96.2% for Cd, 95.2 and 100.6% for Cr, 95.7 and 103% for Ni and 94.2 and 105.5% for Pb.

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

40 CFR 60.648 - Optional procedure for measuring hydrogen sulfide in acid gas-Tutwiler Procedure. 1

Code of Federal Regulations, 2013 CFR

2013-07-01

... hydrogen sulfide in acid gas-Tutwiler Procedure. 1 60.648 Section 60.648 Protection of Environment..., 2011 § 60.648 Optional procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure. 1 1 Gas... dilute solutions are used. In principle, this method consists of titrating hydrogen sulfide in a gas...

40 CFR 60.648 - Optional procedure for measuring hydrogen sulfide in acid gas-Tutwiler Procedure. 1

Code of Federal Regulations, 2014 CFR

2014-07-01

... hydrogen sulfide in acid gas-Tutwiler Procedure. 1 60.648 Section 60.648 Protection of Environment..., 2011 § 60.648 Optional procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure. 1 1 Gas... dilute solutions are used. In principle, this method consists of titrating hydrogen sulfide in a gas...

Development of a modified cortisol extraction procedure for intermediately sized fish not amenable to whole-body or plasma extraction methods.

PubMed

Guest, Taylor W; Blaylock, Reginald B; Evans, Andrew N

2016-02-01

The corticosteroid hormone cortisol is the central mediator of the teleost stress response. Therefore, the accurate quantification of cortisol in teleost fishes is a vital tool for addressing fundamental questions about an animal's physiological response to environmental stressors. Conventional steroid extraction methods using plasma or whole-body homogenates, however, are inefficient within an intermediate size range of fish that are too small for phlebotomy and too large for whole-body steroid extractions. To assess the potential effects of hatchery-induced stress on survival of fingerling hatchery-reared Spotted Seatrout (Cynoscion nebulosus), we developed a novel extraction procedure for measuring cortisol in intermediately sized fish (50-100 mm in length) that are not amenable to standard cortisol extraction methods. By excising a standardized portion of the caudal peduncle, this tissue extraction procedure allows for a small portion of a larger fish to be sampled for cortisol, while minimizing the potential interference from lipids that may be extracted using whole-body homogenization procedures. Assay precision was comparable to published plasma and whole-body extraction procedures, and cortisol quantification over a wide range of sample dilutions displayed parallelism versus assay standards. Intra-assay %CV was 8.54%, and average recovery of spiked samples was 102%. Also, tissue cortisol levels quantified using this method increase 30 min after handling stress and are significantly correlated with blood values. We conclude that this modified cortisol extraction procedure provides an excellent alternative to plasma and whole-body extraction procedures for intermediately sized fish, and will facilitate the efficient assessment of cortisol in a variety of situations ranging from basic laboratory research to industrial and field-based environmental health applications.

Subcritical water extraction of amino acids from Mars analog soils.

PubMed

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

2018-01-18

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

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

PubMed

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

2016-01-13

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

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Ultrasound-assisted extraction of amino acids from grapes.

PubMed

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

2015-01-01

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

Changes in Corneal Deformation Parameters after Lenticule Creation and Extraction during Small Incision Lenticule Extraction (SMILE) Procedure

PubMed Central

Shen, Yang; Zhao, Jing; Yao, Peijun; Miao, Huamao; Niu, Lingling

2014-01-01

Purpose To investigate the effects of lenticule creation and subsequent corneal lenticule extraction on corneal deformation parameters during small incision lenticule extraction (SMILE) procedure. Materials and Methods In this prospective study, 18 eyes of 10 patients (27.90±7.11 years, −5.64±2.45 diopters) scheduled for SMILE procedure were enrolled. Changes in the corneal deformation parameters, including deformation amplitude (DA), applanation time(AT1 and AT2), applanation length(AL1 and AL2), corneal velocity(CV1 and CV2), peak distance(P.Dist.), radius and intraocular pressure values were measured preoperatively, immediately after lenticule creation and subsequent to corneal lenticule extraction in all eyes with the Corvis Scheimpflug Technology (Corvis ST, OCULUS, Wetzlar, Germany). Repeated measures analysis of variance (ANOVA) with bonferroni-adjusted post hoc comparisons was performed to investigate changes following each step of the procedure. Results All surgical procedures were uneventful. A significant difference was detected among the three time points (pre-operation, post-lenticule creation and post lenticule extraction) for AT1 (P<0.001), AT2 (P = 0.001), DA(P<0.001), and IOP(P = 0.002). Bonferroni-adjusted post hoc comparisons indicated that there was no significant change in AT1, AT2, DA, or IOP after lenticule creation (post hoc P>0.05), but there was a significant change in these parameters following subsequent corneal lenticule extraction (post hoc P<0.01), when compared to values obtained pre-operatively. The scheimpflug camera of the Corvis ST demonstrated the intralamellar small gas bubbles formed from the vaporisation of tissue after lenticule creation and a gray zone was observed between the cap and the residual stromal bed after lenticule extraction. Conclusions There is a significant change in corneal deformation parameters following SMILE procedure. The changes may be caused predominantly by stromal lenticule extraction

Changes in corneal deformation parameters after lenticule creation and extraction during small incision lenticule extraction (SMILE) procedure.

PubMed

Shen, Yang; Zhao, Jing; Yao, Peijun; Miao, Huamao; Niu, Lingling; Wang, Xiaoying; Zhou, Xingtao

2014-01-01

To investigate the effects of lenticule creation and subsequent corneal lenticule extraction on corneal deformation parameters during small incision lenticule extraction (SMILE) procedure. In this prospective study, 18 eyes of 10 patients (27.90 ± 7.11 years, -5.64 ± 2.45 diopters) scheduled for SMILE procedure were enrolled. Changes in the corneal deformation parameters, including deformation amplitude (DA), applanation time(AT1 and AT2), applanation length(AL1 and AL2), corneal velocity(CV1 and CV2), peak distance(P.Dist.), radius and intraocular pressure values were measured preoperatively, immediately after lenticule creation and subsequent to corneal lenticule extraction in all eyes with the Corvis Scheimpflug Technology (Corvis ST, OCULUS, Wetzlar, Germany). Repeated measures analysis of variance (ANOVA) with bonferroni-adjusted post hoc comparisons was performed to investigate changes following each step of the procedure. All surgical procedures were uneventful. A significant difference was detected among the three time points (pre-operation, post-lenticule creation and post lenticule extraction) for AT1 (P<0.001), AT2 (P = 0.001), DA(P<0.001), and IOP(P = 0.002). Bonferroni-adjusted post hoc comparisons indicated that there was no significant change in AT1, AT2, DA, or IOP after lenticule creation (post hoc P>0.05), but there was a significant change in these parameters following subsequent corneal lenticule extraction (post hoc P<0.01), when compared to values obtained pre-operatively. The scheimpflug camera of the Corvis ST demonstrated the intralamellar small gas bubbles formed from the vaporisation of tissue after lenticule creation and a gray zone was observed between the cap and the residual stromal bed after lenticule extraction. There is a significant change in corneal deformation parameters following SMILE procedure. The changes may be caused predominantly by stromal lenticule extraction, while lenticule creation with femtosecond laser may not

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.

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

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

PubMed

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

2004-09-01

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

Analysis of fusaric acid in maize using molecularly imprinted solid phase extraction (MISPE) clean-up and ion-pair LC with diode array UV detection

USDA-ARS?s Scientific Manuscript database

Fusaric acid is a phytotoxin and mycotoxin occasionally found in maize contaminated with Fusarium fungi. A selective sample clean-up procedure was developed to detect fusaric acid in maize using molecularly imprinted solid phase extraction (MISPE) clean-up coupled with ion-pair liquid chromatography...

PROCESS FOR PRODUCING ALKYL ORTHOPHOSPHORIC ACID EXTRACTANTS

DOEpatents

Grinstead, R.R.

1962-01-23

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

Use of topical tranexamic acid or aminocaproic acid to prevent bleeding after major surgical procedures.

PubMed

Ipema, Heather J; Tanzi, Maria G

2012-01-01

To evaluate the literature describing topical use of tranexamic acid or aminocaproic acid for prevention of postoperative bleeding after major surgical procedures. Literature was retrieved through MEDLINE (1946-September 2011) and International Pharmaceutical Abstracts (1970-September 2011) using the terms tranexamic acid, aminocaproic acid, antifibrinolytic, topical, and surgical. In addition, reference citations from publications identified were reviewed. All identified articles in English were evaluated. Clinical trials, case reports, and meta-analyses describing topical use of tranexamic acid or aminocaproic acid to prevent postoperative bleeding were included. A total of 16 publications in the setting of major surgical procedures were included; the majority of data were for tranexamic acid. For cardiac surgery, 4 trials used solutions containing tranexamic acid (1-2.5 g in 100-250 mL of 0.9% NaCl), and 1 trial assessed a solution containing aminocaproic acid (24 g in 250 mL of 0.9% NaCl). These solutions were poured into the chest cavity before sternotomy closure. For orthopedic procedures, all of the data were for topical irrigation solutions containing tranexamic acid (500 mg-3 g in 50-100 mL of 0.9% NaCl) or for intraarticular injections of tranexamic acid (250 mg to 2 g in 20-50 mL of 0.9% sodium chloride, with or without carbazochrome sodium sulfate). Overall, use of topical tranexamic acid or aminocaproic acid reduced postoperative blood loss; however, few studies reported a significant reduction in the number of packed red blood cell transfusions or units given, intensive care unit stay, or length of hospitalization. Topical application of tranexamic acid and aminocaproic acid to decrease postsurgical bleeding after major surgical procedures is a promising strategy. Further data are needed regarding the safety of this hemostatic approach.

Chlorogenic acid stability in pressurized liquid extraction conditions.

PubMed

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

2015-01-01

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

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

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

Lewis, V.P.; Yang, Shangtian

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

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.

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.

A comparison of the compositional differences between humic fractions isolated by the IHSS and exhaustive extraction procedures

NASA Astrophysics Data System (ADS)

Chang, R. R.; Mylotte, R.; Hayes, M. H. B.; Mclnerney, R.; Tzou, Y. M.

2014-03-01

highly ordered hydrocarbon structures that would be expected to have closer associations with the mineral colloids. Although the SEE procedure isolated all of the HAs and FAs from the Yangmingshan soil, extractability of the Hu from the volcanic soil in the DMSO/acid solvent was low (21 %), and contrasted with the much higher yields from temperate and tropical regions. The decreased Hu extraction may arise from its associations with the extensive iron and aluminium hydroxide mineral colloids in the soil. The Hu from this sub-tropical soil was different from the Hus isolated from other soil types, indicating the need to isolate and characterise these recalcitrant organic material in order to understand the organic carbon components in soils in greater detail. Such results would indicate that more attention should be given to mineral colloids in soils, and to the organo/mineral associations that will have an important role in the stabilities of OM in the soil environment.

40 CFR 60.5408 - What is an optional procedure for measuring hydrogen sulfide in acid gas-Tutwiler Procedure?

Code of Federal Regulations, 2013 CFR

2013-07-01

... measuring hydrogen sulfide in acid gas-Tutwiler Procedure? 60.5408 Section 60.5408 Protection of Environment... § 60.5408 What is an optional procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure... of titrating hydrogen sulfide in a gas sample directly with a standard solution of iodine. (b...

40 CFR 60.5408 - What is an optional procedure for measuring hydrogen sulfide in acid gas-Tutwiler Procedure?

Code of Federal Regulations, 2014 CFR

2014-07-01

... measuring hydrogen sulfide in acid gas-Tutwiler Procedure? 60.5408 Section 60.5408 Protection of Environment... § 60.5408 What is an optional procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure... of titrating hydrogen sulfide in a gas sample directly with a standard solution of iodine. (b...

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

NASA Astrophysics Data System (ADS)

Fuller, M.; Huang, Y.

2003-03-01

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

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

PubMed

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

2012-10-01

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

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

PubMed

Nojavan, Saeed; Asadi, Sakine

2016-02-01

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

High-volume extraction of nucleic acids by magnetic bead technology for ultrasensitive detection of bacteria in blood components.

PubMed

Störmer, Melanie; Kleesiek, Knut; Dreier, Jens

2007-01-01

Nucleic acid isolation, the most technically demanding and laborious procedure performed in molecular diagnostics, harbors the potential for improvements in automation. A recent development is the use of magnetic beads covered with nucleic acid-binding matrices. We adapted this technology with a broad-range 23S rRNA real-time reverse transcription (RT)-PCR assay for fast and sensitive detection of bacterial contamination of blood products. We investigated different protocols for an automated high-volume extraction method based on magnetic-separation technology for the extraction of bacterial nucleic acids from platelet concentrates (PCs). We added 2 model bacteria, Staphylococcus epidermidis and Escherichia coli, to a single pool of apheresis-derived, single-donor platelets and assayed the PCs by real-time RT-PCR analysis with an improved primer-probe system and locked nucleic acid technology. Co-amplification of human beta(2)-microglobulin mRNA served as an internal control (IC). We used probit analysis to calculate the minimum concentration of bacteria that would be detected with 95% confidence. For automated magnetic bead-based extraction technology with the real-time RT-PCR, the 95% detection limit was 29 x 10(3) colony-forming units (CFU)/L for S. epidermidis and 22 x 10(3) CFU/L for E. coli. No false-positive results occurred, either due to nucleic acid contamination of reagents or externally during testing of 1030 PCs. High-volume nucleic acid extraction improved the detection limit of the assay. The improvement of the primer-probe system and the integration of an IC make the RT-PCR assay appropriate for bacteria screening of platelets.

Heavy metal speciation in solid-phase materials from a bacterial sulfate reducing bioreactor using sequential extraction procedure combined with acid volatile sulfide analysis.

PubMed

Jong, Tony; Parry, David L

2004-04-01

Heavy metal mobility, bioavailability and toxicity depends largely on the chemical form of metals and ultimately determines potential for environmental pollution. For this reason, determining the chemical form of heavy metals and metalloids, immobilized in sludges by biological mediated sulfate reduction, is important to evaluate their mobility and bioavailability. A modified Tessier sequential extraction procedure (SEP), complemented with acid volatile sulfide (AVS) and simultaneous extracted metals (SEM) measurements, were applied to determine the partitioning of five heavy metals (defined as Fe, Ni, Zn and Cu, and the metalloid As) in anoxic solid-phase material (ASM) from an anaerobic, sulfate reducing bioreactor into six operationally defined fractions. These fractions were water soluble, exchangeable, bound to carbonates (acid soluble), bound to Fe-Mn oxides (reducible), bound to organic matter and sulfides (oxidizable) and residual. It was found that the distribution of Fe, Ni, Zn, Cu and As in ASM was strongly influenced by its association with the above solid fractions. The fraction corresponding to organic matter and sulfides appeared to be the most important scavenging phases of As, Fe, Ni, Zn and Cu in ASM (59.8-86.7%). This result was supported by AVS and SEM (Sigma Zn, Ni and Cu) measurements, which indicated that the heavy metals existed overwhelmingly as sulfides in the organic matter and sulfide fraction. A substantial amount of Fe and Ni at 16.4 and 20.1%, respectively, were also present in the carbonate fraction, while an appreciable portion of As (18.3%) and Zn (19.4%) was bound to Fe-Mn oxides. A significant amount of heavy metals was also associated with the residual fraction, ranging from 2.1% for Zn to 18.8% for As. Based on the average total extractable heavy metal (TEHM) values, the concentration of heavy metals in the ASM was in the order of Cu > Ni > Zn > Fe > As. If the mobility and bioavailability of heavy metals are assumed to be

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

PubMed Central

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

2014-01-01

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

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

PubMed Central

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

2017-01-01

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

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

PubMed

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

2017-10-01

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

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

PubMed

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

2010-09-01

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

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

Code of Federal Regulations, 2010 CFR

2010-04-01

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

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

PubMed

Chen, R; Lee, Y Y

1997-01-01

Lactic acid production from cellulosic biomass by cellulase and Lactobacillus delbrueckii was studied in a fermenter-extractor employing a microporous hollow fiber membrane (MHF). This bioreactor system was operated under a fed-batch mode with continuous removal of lactic acid by anin situ extraction. A tertiary amine (Alamine 336) was used as an extractant for lactic acid. The extraction capacity of Alamine 336 is greatly enhanced by addition of alcohol. Long-chain alcohols serve well for this purpose since they are less toxic to micro-organism. Addition of kerosene, a diluent, was necessary to reduce the solvent viscosity. A solvent mixture of 20% Alamine 336, 40% oleyl alcohol, and 40% kerosene was found to be most effective in the extraction of lactic acid. Progressive change of pH from an initial value of 5.0 down to 4.3 has significantly improved the overall performance of the simultaneous saccharification and extractive fermentation over that of constant pH operation. The change of pH was applied to promote cell growth in the early phase, and extraction in the latter phase.

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.

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

NASA Astrophysics Data System (ADS)

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

2010-03-01

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

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

PubMed

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

2018-04-24

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

An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation.

PubMed

Peters, Sonja; Kaal, Erwin; Horsting, Iwan; Janssen, Hans-Gerd

2012-02-24

A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing 'Micro-extraction in packed sorbent' (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve extraction yields of the more polar analytes and as the methyl donor in the automated in-liner derivatisation method. In this way, a fully automated procedure for the extraction, derivatisation and injection of a wide range of phenolic acids in plasma samples has been obtained. An extensive optimisation of the extraction and derivatisation procedure has been performed. The entire method showed excellent repeatabilities of under 10% and linearities of 0.99 or better for all phenolic acids. The limits of detection of the optimised method for the majority of phenolic acids were 10ng/mL or lower with three phenolic acids having less-favourable detection limits of around 100 ng/mL. Finally, the newly developed method has been applied in a human intervention trial in which the bioavailability of polyphenols from wine and tea was studied. Forty plasma samples could be analysed within 24h in a fully automated method including sample extraction, derivatisation and gas chromatographic analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

Lee, Ilgyu; Han, Jong-In

2015-09-01

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

GC and GC-MS determination of fluoroacetic acid and phenoxy acid herbicides via triphasal extractive pentafluorobenzylation using a polymer-bound phase-transfer catalyst.

PubMed

Miki, A; Tsuchihashi, H; Yamashita, M

1998-01-01

A simple and sensitive gas chromatography and gas chromatography-mass spectrometry (GC-MS) procedure has been developed for fluoroacetic acid (FA) and phenoxy acid herbicides (PAHs) via triphasal extractive pentafluorobenzylation. The triphasal system consisted of an aqueous sample, the extraction solvent toluene containing pentafluorobenzyl bromide as the derivatization reagent, and polymer-bound tri-n-butyl-methylphosphonium bromide as a phase-transfer catalyst, FA spiked in beverages, such as orange juice and milk, was extracted as its pentafluorobenzyl (PFB) derivative under moderate conditions (i.e., at a pH value of 6.5 at 60 degrees C). The detection limits were 0.10-0.20 microgram/mL by GC with electron-capture detection (GC-ECD), and 0.42-0.50 microgram/mL by full-scan GC-MS. PAHs were also detectable in the same manner within the detection limits of 0.05-0.10 microgram/mL by GC-ECD and 0.13-0.25 microgram/mL by full-scan GC-MS. Urine and serum which both contained 2,4-dichlorophenoxyacetic acid could also be analyzed by GC-MS after the triphasal pentafluorobenzylation. The detection limit was 0.20 microgram/mL in the full-scan mode and 10 ng/mL in the selected ion monitoring mode both for the urine and serum.

Addition of Grape Seed Extract Renders Phosphoric Acid a Collagen-stabilizing Etchant.

PubMed

Liu, Y; Dusevich, V; Wang, Y

2014-08-01

Previous studies found that grape seed extract (GSE), which is rich in proanthocyanidins, could protect demineralized dentin collagen from collagenolytic activities following clinically relevant treatment. Because of proanthocyanidin's adverse interference to resin polymerization, it was believed that GSE should be applied and then rinsed off in a separate step, which in effect increases the complexity of the bonding procedure. The present study aimed to investigate the feasibility of combining GSE treatment with phosphoric acid etching to address the issue. It is also the first attempt to formulate collagen-cross-linking dental etchants. Based on Fourier-transformed infrared spectroscopy and digestion assay, it was established that in the presence of 20% to 5% phosphoric acid, 30 sec of GSE treatment rendered demineralized dentin collagen inert to bacterial collagenase digestion. Based on this positive result, the simultaneous dentin etching and collagen protecting of GSE-containing phosphoric acid was evaluated on the premise of a 30-second etching time. According to micro-Raman spectroscopy, the formulation containing 20% phosphoric acid was found to lead to overetching. Based on scanning and transmission electronic microscopy, this same formulation exhibited unsynchronized phosphoric acid and GSE penetration. Therefore, addition of GSE did render phosphoric acid a collagen-stabilizing etchant, but the preferable phosphoric acid concentration should be <20%. © International & American Associations for Dental Research.

Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

PubMed

Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

2016-09-01

In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of magnesium from calcined dolomite ore using hydrochloric acid leaching

NASA Astrophysics Data System (ADS)

Royani, Ahmad; Sulistiyono, Eko; Prasetiyo, Agus Budi; Subagja, Rudi

2018-05-01

Magnesium is widely used in varieties industrial sector. Dolomite is one source of magnesium besides seawater. The extraction of magnesium from dolomite ores can be done by leaching process. In this work, the dolomite leaching to extract magnesium by hydrochloric acid was investigated. The leaching experiments were performed in a spherical glass batch reactor having a capacity of 1000 ml. The effects of the stirring speed, acid concentration, reaction temperature and liquid-solid ratio for each reaction time of 1; 2; and 3 h on the Mg leaching have been evaluated. 5 ml of solution sample were collected from the leached solutions, then it was filtered prior to analysis by ICP OES. The experimental results show that the magnesium extraction increases along with the increase of acid concentration, liquid-solid ratio and temperature. The optimum conditions for magnesium extraction were achieved at temperature 75 °C, extraction time 3 h, the HCl concentration of 2 M, the liquid-solid ratio 20 ml/g and stirring speed of 400 rpm. At this condition 98, 82 % of magnesium were extracted from dolomite. The conclusion obtained from this leaching process is that the magnesium can be extracted from dolomite by using hydrochloric acid solutions.

Alkaline earth cation extraction from acid solution

DOEpatents

Dietz, Mark; Horwitz, E. Philip

2003-01-01

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

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

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

Chen, Rongfu; Lee, Y.Y.

1997-12-31

Lactic acid production from cellulosic biomass by cellulose and Lactobacillus delbrueckii was studied in a fermenter-extractor employing a microporous hollow fiber membrane (NIHF). This bioreactor system was operated under a fed-batch mode with continuous removal of lactic acid by an in situ extraction. A tertiary amine (Alamine 336) was used as an extractant for lactic acid. The extraction capacity of Alamine 336 is greatly enhanced by addition of alcohol. Long-chain alcohols serve well for this purpose since they are less toxic to micro-organism. Addition of kerosene, a diluent, was necessary to reduce the solvent viscosity. A solvent mixture of 20%more » Alamine 336,40% oleyl alcohol, and 40% kerosene was found to be most effective in the extraction of lactic acid. Progressive change of pH from an initial value of 5.0 down to 4.3 has significantly improved the overall performance of the simultaneous saccharification and extractive fermentation over that of constant pH operation. The change of pH was applied to promote cell growth in the early phase, and extraction in the latter phase. 20 refs., 10 figs., 1 tab.« less

Extraction of DNA from forensic-type sexual assault specimens using simple, rapid sonication procedures.

PubMed

Crouse, C A; Ban, J D; D'Alessio, J K

1993-10-01

Sonication procedures for the extraction of DNA from forensic-type semen specimens have been developed, which, when compared to currently utilized sperm DNA extraction techniques, are simple, rapid and result in comparable DNA yields. Sperm DNA extraction by sonication was performed on whole semen, seminal stains, buccal swabs and post-coital specimens. Ultrasound disruption of sperm cells and their ultimate release of cellular DNA has been conducted in the presence of sperm wash buffers followed by organic extraction or Chelex 100 with little or no compromise to DNA quality, quantity or amplifiability. Two advantages of sonication over currently used forensic techniques to extract sperm DNA include 1) sperm DNA extraction that occurs within five minutes of sonication compared with an hour or greater for water bath incubations in classic enzyme digestion DNA extractions and 2) one less preparatory step with the Chelex/sonication protocol and three less steps with the sonication/organic protocol compared with other procedures thus eliminating potential sample-to-sample cross-contamination. Sperm DNA extracted by optimum sonication procedures was used for forensic HLA DQ alpha typing and restriction fragment length polymorphisms analysis without any adverse effects on typing results.

Rapid isolation procedure for Δ9-tetrahydrocannabinolic acid A (THCA) from Cannabis sativa using two flash chromatography systems.

PubMed

Wohlfarth, Ariane; Mahler, Hellmut; Auwärter, Volker

2011-10-15

Two isolation procedures for Δ9-tetrahydrocannabinolic acid A (THCA), the biogenetic precursor in the biosynthesis of the psychoactive Δ9-tetrahydrocannabinol (THC) in the cannabis plant, are presented. Two flash chromatography systems that can be used independently from each other were developed to separate THCA from other compounds of a crude cannabis extract. In both systems UV absorption at 209 and 270 nm was monitored. Purity was finally determined by HPLC-DAD, NMR and GC-MS analysis with a focus on the impurity THC. System 1 consisted of a normal phase silica column (120 g) as well as cyclohexane and acetone--both spiked with the modifier pyridine--as mobile phases. Gradient elution was performed over 15 min. After the chromatographic run the fractions containing THCA fractions were pooled, extracted with hydrochloric acid to eliminate pyridine and evaporated to dryness. Loading 1800 mg cannabis extract yielded 623 mg THCA with a purity of 99.8% and a THC concentration of 0.09%. System 2 was based on a reversed-phase C18 column (150 g) combined with 0.55% formic acid and methanol as mobile phases. A very flat gradient was set over 20 minutes. After pooling the THCA-containing fractions methanol was removed in a rotary evaporator. THCA was re-extracted from the remaining aqueous phase with methyl tert-butyl ether. The organic phase was finally evaporated under high vacuum conditions. Loading 300 mg cannabis extract yielded 51 mg THCA with a purity of 98.8% and a THC concentration of 0.67%. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2010-08-01

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

Aviation accident forensic assessment : comprehensive single-extraction urine screening procedure : final report.

DOT National Transportation Integrated Search

1996-05-01

This paper describes a new single extraction screening procedure that was developed to identify as many drugs as possible in urine, with minimal effort and cost. Urine specimens are hydrolyzed and the specimen is then extracted using commercially pur...

Extraction and analysis of adenosine triphosphate from aquatic environments

USGS Publications Warehouse

Stephens, Doyle W.; Shultz, David J.

1981-01-01

A variety of adenosine triphosphate (ATP) extraction procedures have been investigated for their applicability to samples from aquatic environments. The cold sulfuric-oxalic acid procedure was best suited to samples consisting of water, periphyton, and sediments. Due to cation and fulvic acid interferences, a spike with a known quantity of ATP was necessary to estimate losses when sediments were extracted. Variable colonization densities for periphyton required that several replicates be extracted to characterize acdurately the periphyton community. Extracted samples were stable at room temperature for one to five hours, depending on the ATP concentration, if the pH was below 2. Neutralized samples which were quick frozen and stored at -30°C were stable for months.

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.

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

Membrane protein extraction and purification using styrene-maleic acid (SMA) copolymer: effect of variations in polymer structure.

PubMed

Morrison, Kerrie A; Akram, Aneel; Mathews, Ashlyn; Khan, Zoeya A; Patel, Jaimin H; Zhou, Chumin; Hardy, David J; Moore-Kelly, Charles; Patel, Roshani; Odiba, Victor; Knowles, Tim J; Javed, Masood-Ul-Hassan; Chmel, Nikola P; Dafforn, Timothy R; Rothnie, Alice J

2016-12-01

The use of styrene-maleic acid (SMA) copolymers to extract and purify transmembrane proteins, while retaining their native bilayer environment, overcomes many of the disadvantages associated with conventional detergent-based procedures. This approach has huge potential for the future of membrane protein structural and functional studies. In this investigation, we have systematically tested a range of commercially available SMA polymers, varying in both the ratio of styrene and maleic acid and in total size, for the ability to extract, purify and stabilise transmembrane proteins. Three different membrane proteins (BmrA, LeuT and ZipA), which vary in size and shape, were used. Our results show that several polymers, can be used to extract membrane proteins, comparably to conventional detergents. A styrene:maleic acid ratio of either 2:1 or 3:1, combined with a relatively small average molecular mass (7.5-10 kDa), is optimal for membrane extraction, and this appears to be independent of the protein size, shape or expression system. A subset of polymers were taken forward for purification, functional and stability tests. Following a one-step affinity purification, SMA 2000 was found to be the best choice for yield, purity and function. However, the other polymers offer subtle differences in size and sensitivity to divalent cations that may be useful for a variety of downstream applications. © 2016 The Author(s); published by Portland Press Limited on behalf of the Biochemical Society.

Standard Operating Procedure for the Grinding and Extraction of Lead in Paint using Nitric Acid and a Rotor/Stator System Powered by a High Speed Motor

EPA Science Inventory

This Standard Operating Procedure (SOP) describes a new, rapid, and relatively inexpensive one step procedure which grinds the paint samples removed from the substrate and simultaneously quantitatively extracts the Pb from the paint in only one step in preparation for quantitativ...

Supercritical fluid extraction and characterization of lipids from algae Scenedesmus obliquus

NASA Technical Reports Server (NTRS)

Choi, K. J.; Nakhost, Z.; Krukonis, V. J.; Karel, M.

1987-01-01

Lipids were extracted from a protein concentrate of green algae (Scenedesmus obliquus), using a one-step supercritical carbon dioxide extraction procedure in presence of ethanol as an entrainer, and were characterized. The compositions of neutral lipids, glycolipids, and phospholipids, separated into individual components by column, thin-layer, and gas-liquid chromatography procedures, are presented. Fatty acid composition patterns indicated that the major fatty acids were 16:0, 16:1, 16:2, 16:3, 16:4, 18:1, 18:2, and 18:3. The lipids of S. obliquus were found to contain relatively high concentrations of polyunsaturated fatty acids and essential fatty acids.

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

PubMed

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

2017-12-01

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

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

Treesearch

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

2010-01-01

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

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

PubMed

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

2015-07-29

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

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

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

PubMed

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

2008-01-01

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

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

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

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

2008-07-01

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

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

Nitric Acid and Water Extraction by T2EHDGA in n -Dodecane

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

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

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

Statistical evaluation of fatty acid profile and cholesterol content in fish (common carp) lipids obtained by different sample preparation procedures.

PubMed

Spiric, Aurelija; Trbovic, Dejana; Vranic, Danijela; Djinovic, Jasna; Petronijevic, Radivoj; Matekalo-Sverak, Vesna

2010-07-05

Studies performed on lipid extraction from animal and fish tissues do not provide information on its influence on fatty acid composition of the extracted lipids as well as on cholesterol content. Data presented in this paper indicate the impact of extraction procedures on fatty acid profile of fish lipids extracted by the modified Soxhlet and ASE (accelerated solvent extraction) procedure. Cholesterol was also determined by direct saponification method, too. Student's paired t-test used for comparison of the total fat content in carp fish population obtained by two extraction methods shows that differences between values of the total fat content determined by ASE and modified Soxhlet method are not statistically significant. Values obtained by three different methods (direct saponification, ASE and modified Soxhlet method), used for determination of cholesterol content in carp, were compared by one-way analysis of variance (ANOVA). The obtained results show that modified Soxhlet method gives results which differ significantly from the results obtained by direct saponification and ASE method. However the results obtained by direct saponification and ASE method do not differ significantly from each other. The highest quantities for cholesterol (37.65 to 65.44 mg/100 g) in the analyzed fish muscle were obtained by applying direct saponification method, as less destructive one, followed by ASE (34.16 to 52.60 mg/100 g) and modified Soxhlet extraction method (10.73 to 30.83 mg/100 g). Modified Soxhlet method for extraction of fish lipids gives higher values for n-6 fatty acids than ASE method (t(paired)=3.22 t(c)=2.36), while there is no statistically significant difference in the n-3 content levels between the methods (t(paired)=1.31). The UNSFA/SFA ratio obtained by using modified Soxhlet method is also higher than the ratio obtained using ASE method (t(paired)=4.88 t(c)=2.36). Results of Principal Component Analysis (PCA) showed that the highest positive impact to

A simple one-step ultrasonic-assisted extraction and derivatization method coupling to high-performance liquid chromatographyfor the determination of ε-aminocaproic acid and amino acids in cosmetics.

PubMed

Du, Yuanqi; Xia, Ling; Xiao, Xiaohua; Li, Gongke; Chen, Xiaoguang

2018-06-15

Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE

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

PubMed

Chao, Che-Yi; Yin, Mei-Chin

2009-03-01

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

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

PubMed

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

2015-06-01

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

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

PubMed

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

2009-08-01

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

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

NASA Astrophysics Data System (ADS)

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

2016-02-01

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

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

DTIC Science & Technology

1945-06-08

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

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

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

PubMed

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

2013-04-01

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

Utilization of optimized BCR three-step sequential and dilute HCl single extraction procedures for soil-plant metal transfer predictions in contaminated lands.

PubMed

Kubová, Jana; Matús, Peter; Bujdos, Marek; Hagarová, Ingrid; Medved', Ján

2008-05-30

The prediction of soil metal phytoavailability using the chemical extractions is a conventional approach routinely used in soil testing. The adequacy of such soil tests for this purpose is commonly assessed through a comparison of extraction results with metal contents in relevant plants. In this work, the fractions of selected risk metals (Al, As, Cd, Cu, Fe, Mn, Ni, Pb, Zn) that can be taken up by various plants were obtained by optimized BCR (Community Bureau of Reference) three-step sequential extraction procedure (SEP) and by single 0.5 mol L(-1) HCl extraction. These procedures were validated using five soil and sediment reference materials (SRM 2710, SRM 2711, CRM 483, CRM 701, SRM RTH 912) and applied to significantly different acidified soils for the fractionation of studied metals. The new indicative values of Al, Cd, Cu, Fe, Mn, P, Pb and Zn fractional concentrations for these reference materials were obtained by the dilute HCl single extraction. The influence of various soil genesis, content of essential elements (Ca, Mg, K, P) and different anthropogenic sources of acidification on extraction yields of individual risk metal fractions was investigated. The concentrations of studied elements were determined by atomic spectrometry methods (flame, graphite furnace and hydride generation atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry). It can be concluded that the data of extraction yields from first BCR SEP acid extractable step and soil-plant transfer coefficients can be applied to the prediction of qualitative mobility of selected risk metals in different soil systems.

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

PubMed

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

2005-09-01

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

Carboxylic and Dicarboxylic Acids Extracted from Crushed Magnesium Oxide Single Crystals

NASA Technical Reports Server (NTRS)

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

1998-01-01

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

Carboxylic and dicarboxylic acids extracted from crushed magnesium oxide single crystals

NASA Technical Reports Server (NTRS)

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

1999-01-01

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

Analysis of simulated angiographic procedures. Part 2: extracting efficiency data from audio and video recordings.

PubMed

Duncan, James R; Kline, Benjamin; Glaiberman, Craig B

2007-04-01

To create and test methods of extracting efficiency data from recordings of simulated renal stent procedures. Task analysis was performed and used to design a standardized testing protocol. Five experienced angiographers then performed 16 renal stent simulations using the Simbionix AngioMentor angiographic simulator. Audio and video recordings of these simulations were captured from multiple vantage points. The recordings were synchronized and compiled. A series of efficiency metrics (procedure time, contrast volume, and tool use) were then extracted from the recordings. The intraobserver and interobserver variability of these individual metrics was also assessed. The metrics were converted to costs and aggregated to determine the fixed and variable costs of a procedure segment or the entire procedure. Task analysis and pilot testing led to a standardized testing protocol suitable for performance assessment. Task analysis also identified seven checkpoints that divided the renal stent simulations into six segments. Efficiency metrics for these different segments were extracted from the recordings and showed excellent intra- and interobserver correlations. Analysis of the individual and aggregated efficiency metrics demonstrated large differences between segments as well as between different angiographers. These differences persisted when efficiency was expressed as either total or variable costs. Task analysis facilitated both protocol development and data analysis. Efficiency metrics were readily extracted from recordings of simulated procedures. Aggregating the metrics and dividing the procedure into segments revealed potential insights that could be easily overlooked because the simulator currently does not attempt to aggregate the metrics and only provides data derived from the entire procedure. The data indicate that analysis of simulated angiographic procedures will be a powerful method of assessing performance in interventional radiology.

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.

Simultaneous determination of phenolic acids and flavonoids in rice using solid-phase extraction and RP-HPLC with photodiode array detection.

PubMed

Irakli, Maria N; Samanidou, Victoria F; Biliaderis, Costas G; Papadoyannis, Ioannis N

2012-07-01

An analytical method based on an optimized solid-phase extraction procedure and followed by high-performance liquid chromatography (HPLC) separation with diode array detection was developed and validated for the simultaneous determination of phenolic acids (gallic, protocatechuic, 4-hydroxy-benzoic, vanillic, caffeic, syringic, p-coumaric, ferulic, sinapic, and cinnamic acids), flavanols (catechin and epicatechin), flavonols (myricetin, quercetin, kaempferol, quercetin-3-O-glucoside, hyperoside, and rutin), flavones (luteolin and apigenin) and flavanones (naringenin and hesperidin) in rice flour (Oryza sativa L.). Chromatographic separation was carried out on a PerfectSil Target ODS-3 (250 mm × 4.6 mm, 3 μm) column at temperature 25°C using a mobile phase, consisting of 0.5% (v/v) acetic acid in water, methanol, and acetonitrile at a flow rate 1 mL min(-1) , under gradient elution conditions. Application of optimum extraction conditions, elaborated on both Lichrolut C(18) and Oasis HLB cartridges, have led to extraction of phenolic acids and flavonoids from rice flour with mean recoveries 84.3-113.0%. The developed method was validated in terms of linearity, accuracy, precision, stability, and sensitivity. Repeatability (n = 5) and inter-day precision (n = 4) revealed relative standard deviation (RSD) <13%. The optimized method was successfully applied to the analysis of phenolic acids and flavonoids in pigmented (red and black rice) and non-pigmented rice (brown rice) samples. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of three sequential extraction procedures for arsenic fractionation in highly polluted sites.

PubMed

Wan, Xiang; Dong, Haochen; Feng, Liu; Lin, Zhijia; Luo, Qiuchen

2017-07-01

Three sequential extraction procedures (SEPs) including Tessier, Rauret, and Shiowatana SEPs, were compared for arsenic fractionation using highly polluted soils. In the definition context of exchangeable, reducible, oxidizable and residual fractions, with similar arsenic recovery and reproducibility, Tessier and Rauret SEPs were comparable to each other, whereas Shiowatana SEP showed higher extraction efficiency in all the first three arsenic fractions, although it might overestimate the reducible arsenic. Pot experiment indicated three SEPs all could provide an estimation of the most bioavailable arsenic fraction, and the application of Shiowatana SEP should be preferred. Accordingly, a case study with Shiowatana SEP for a site near a realgar mine area is conducted. The results show that although arsenic in this area presents predominantly in the stable fractions, the sum of most bioavailable fractions was accounted around 11% of total arsenic, and moreover, about another 10% of the total arsenic, the fourth fraction in Shiowatana SEP is likely to be transferred into bioavailable species under suitable conditions, such as strong acid impact, revealing a real major risk source being formed. The study indicated that Shiowatana should be more suitable for arsenic fractionation to provide valuable information in the framework of risk assessment. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

PubMed

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

2008-03-03

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

Development of an efficient fungal DNA extraction method to be used in random amplified polymorphic DNA-PCR analysis to differentiate cyclopiazonic acid mold producers.

PubMed

Sánchez, Beatriz; Rodríguez, Mar; Casado, Eva M; Martín, Alberto; Córdoba, Juan J

2008-12-01

A variety of previously established mechanical and chemical treatments to achieve fungal cell lysis combined with a semiautomatic system operated by a vacuum pump were tested to obtain DNA extract to be directly used in randomly amplified polymorphic DNA (RAPD)-PCR to differentiate cyclopiazonic acid-producing and -nonproducing mold strains. A DNA extraction method that includes digestion with proteinase K and lyticase prior to using a mortar and pestle grinding and a semiautomatic vacuum system yielded DNA of high quality in all the fungal strains and species tested, at concentrations ranging from 17 to 89 ng/microl in 150 microl of the final DNA extract. Two microliters of DNA extracted with this method was directly used for RAPD-PCR using primer (GACA)4. Reproducible RAPD fingerprints showing high differences between producer and nonproducer strains were observed. These differences in the RAPD patterns did not differentiate all the strains tested in clusters by cyclopiazonic acid production but may be very useful to distinguish cyclopiazonic acid producer strains from nonproducer strains by a simple RAPD analysis. Thus, the DNA extracts obtained could be used directly without previous purification and quantification for RAPD analysis to differentiate cyclopiazonic acid producer from nonproducer mold strains. This combined analysis could be adaptable to other toxigenic fungal species to enable differentiation of toxigenic and non-toxigenic molds, a procedure of great interest in food safety.

Determination of homovanillic acid (HVA) in human plasma by HPLC with coulometric detection and a new SPE procedure.

PubMed

Saracino, M A; Mandrioli, R; Mercolini, L; Ferranti, A; Zaimovic, A; Leonardi, C; Raggi, M A

2006-09-11

A sensitive high-performance liquid chromatographic method has been developed for the determination of homovanillic acid (HVA), the main metabolite of dopamine, in human plasma. Analyses were carried out on a reversed-phase column (C8, 250 mm x 4.6 mm i.d., 5 microm) using a mobile phase composed of 10% methanol and 90% aqueous citrate buffer, containing octanesulfonic acid and EDTA at pH 4.8. Coulometric detection was used, setting the guard cell at +0.100 V, the first analytical cell at -0.200 V and the second analytical cell at +0.500 V. A careful solid-phase extraction procedure, based on strong anion exchange (SAX) cartridges (100 mg, 1 mL), was implemented for the pre-treatment of plasma samples. Extraction yield was satisfactory, being the mean value 98.0%. The calibration curve was linear over the concentration range of 0.2-25.0 ng mL(-1) of homovanillic acid. The limit of quantitation (LOQ) was 0.2 ng mL(-1) and the limit of detection (LOD) was 0.1 ng mL(-1). The method was successfully applied to plasma samples from former alcohol, cocaine and heroin addicts. Results were satisfactory in terms of precision and accuracy. Hence, the method is suitable for the determination of homovanillic acid in human plasma.

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

NASA Astrophysics Data System (ADS)

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

2017-08-01

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

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.

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

PubMed

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

2012-06-01

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

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

PubMed

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

2017-08-01

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

Development and characterization of a green procedure for apigenin extraction from Scutellaria barbata D. Don.

PubMed

Yang, Yu-Chiao; Wei, Ming-Chi

2018-06-30

This study compared the use of ultrasound-assisted supercritical CO 2 (USC-CO 2 ) extraction to obtain apigenin-rich extracts from Scutellaria barbata D. Don with that of conventional supercritical CO 2 (SC-CO 2 ) extraction and heat-reflux extraction (HRE), conducted in parallel. This green procedure yielded 20.1% and 31.6% more apigenin than conventional SC-CO 2 extraction and HRE, respectively. Moreover, the extraction time required by the USC-CO 2 procedure, which used milder conditions, was approximately 1.9 times and 2.4 times shorter than that required by conventional SC-CO 2 extraction and HRE, respectively. Furthermore, the theoretical solubility of apigenin in the supercritical fluid system was obtained from the USC-CO 2 dynamic extraction curves and was in good agreement with the calculated values for the three empirical density-based models. The second-order kinetics model was further applied to evaluate the kinetics of USC-CO 2 extraction. The results demonstrated that the selected model allowed the evaluation of the extraction rate and extent of USC-CO 2 extraction. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Determination of aminopolycarboxylic acids in river water by solid-phase extraction on activated charcoal cartridges and gas chromatography with mass spectrometric detection. Method performance characteristics and estimation of the uncertainty.

PubMed

Jiménez, Juan J

2013-04-03

A new sample preparation procedure to determine aminopolycarboxylic acids (ethylenediaminetetraacetic acid, EDTA, nitrilotriacetic acid, NTA, diethylenetriaminepentaacetic acid, DTPA, and cyclohexanediaminetetraacetic acid, CDTA) in river water is described. The procedure consists of the solid-phase extraction of the aminopolycaroxyllic acids on activated charcoal cartridges after increasing the ionic strength and acidifying the sample. The extract was eluted with methanol and the analytes were methylated in presence of BF3/methanol to determine them by GC with mass spectrometric detection. Recoveries were higher than 90% with good repeatabilities and inter-day precision for concentrations close to quantification limits (about 10 μg L(-1)) and higher. It has been verified that the proposed method is robust according to the Youden and Steiner test and free of matrix effects arisen from the presence of organic matter and iron(III) as deduced from statistical tests. A bottom-up approach was followed to estimate the uncertainty of the measured concentration. At concentrations close to 10 μg L(-1) the most relevant step of the method is the calculus of the interpolated concentration which has a high value of relative standard uncertainty. Copyright © 2013 Elsevier B.V. All rights reserved.

Nucleic acid extraction techniques and application to the microchip.

PubMed

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

2009-09-07

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

Procedure optimization for green synthesis of silver nanoparticles by aqueous extract of Eucalyptus oleosa.

PubMed

Pourmortazavi, Seied Mahdi; Taghdiri, Mehdi; Makari, Vajihe; Rahimi-Nasrabadi, Mehdi

2015-02-05

The present study is dealing with the green synthesis of silver nanoparticles using the aqueous extract of Eucalyptus oleosa as a green synthesis procedure without any catalyst, template or surfactant. Colloidal silver nanoparticles were synthesized by reacting aqueous AgNO3 with E. oleosa leaf extract at non-photomediated conditions. The significance of some synthesis conditions such as: silver nitrate concentration, concentration of the plant extract, time of synthesis reaction and temperature of plant extraction procedure on the particle size of synthesized silver particles was investigated and optimized. The participations of the studied factors in controlling the particle size of reduced silver were quantitatively evaluated via analysis of variance (ANOVA). The results of this investigation showed that silver nanoparticles could be synthesized by tuning significant parameters, while performing the synthesis procedure at optimum conditions leads to form silver nanoparticles with 21nm as averaged size. Ultraviolet-visible spectroscopy was used to monitor the development of silver nanoparticles formation. Meanwhile, produced silver nanoparticles were characterized by scanning electron microscopy, energy-dispersive X-ray, and FT-IR techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

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).

Antimicrobial activity and chemical analysis of Microlicia hatschbachii Wurdack (Melastomataceae) extract.

PubMed

Cassiano, Dayse S A; Pacheco, Alessandra G M; da Costa, Mateus M; Almeida, Jackson R G S; Vieira, Ivo J C; Branco, Alexsandro

2014-01-01

Aerial parts of Microlicia hatschbachii were extracted with hexane, and the extract was evaluated for antimicrobial activity by a broth dilution method. After phytochemical procedures: GC-MS identified aliphatic alkanes, carboxylic acids and methyl esters of long-chain fatty acids; and two diterpenoids [labd-8(17)-en-15-oic acid and labd-8(17),13-dien-15-oic acid] were identified by (1)H and (13)C NMR. The antimicrobial activity of the hexane extract could be attributed to the presence of labdanes. This identification is the first reported occurrence of labdane diterpenes in the Melastomataceae family.

Intra-alveolar epsilon-aminocaproic acid for the control of post-extraction bleeding in anticoagulated patients: randomized clinical trial.

PubMed

da Silva, R V; Gadelha, T B; Luiz, R R; Torres, S R

2018-03-27

The aim of this study was to compare the effectiveness of the intra-alveolar administration of epsilon-aminocaproic acid (EACA) and daily gentle rinsing with EACA mouthwash with that of routine postoperative procedures for the control of bleeding after tooth extraction in anticoagulated patients. A randomized clinical trial was conducted involving 52 patients submitted to 140 tooth extractions, assigned randomly to two groups. The intervention group was treated with intra-alveolar administration of EACA immediately after surgery and gentle rinsing with EACA mouthwash during the postoperative period. The control group received routine postoperative recommendations. A single episode of immediate bleeding occurred in the intervention group. Late bleeding episodes occurred in 23 procedures (16.4%): 11 (15.7%) in the intervention group and 12 (17.1%) in the control group. Among the patients with late bleeding, 18 (78.3%) events were classified as moderate and were controlled by the patient applying pressure to a gauze pack placed over the extraction socket. The remaining five cases (21.7%) required re-intervention. No statistically significant difference in the frequency of postoperative bleeding was observed between the groups. Thus, routine measures were as effective for the control of bleeding after simple tooth extractions in anticoagulated patients as the topical administration of EACA. Copyright © 2018 International Association of Oral and Maxillofacial Surgeons. Published by Elsevier Ltd. All rights reserved.

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

PubMed Central

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

2017-01-01

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

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

PubMed

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

2017-10-01

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

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

PubMed

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

2016-05-01

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

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

DOEpatents

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

1984-05-21

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

Current Nucleic Acid Extraction Methods and Their Implications to Point-of-Care Diagnostics.

PubMed

Ali, Nasir; Rampazzo, Rita de Cássia Pontello; Costa, Alexandre Dias Tavares; Krieger, Marco Aurelio

2017-01-01

Nucleic acid extraction (NAE) plays a vital role in molecular biology as the primary step for many downstream applications. Many modifications have been introduced to the original 1869 method. Modern processes are categorized into chemical or mechanical, each with peculiarities that influence their use, especially in point-of-care diagnostics (POC-Dx). POC-Dx is a new approach aiming to replace sophisticated analytical machinery with microanalytical systems, able to be used near the patient, at the point of care or point of need . Although notable efforts have been made, a simple and effective extraction method is still a major challenge for widespread use of POC-Dx. In this review, we dissected the working principle of each of the most common NAE methods, overviewing their advantages and disadvantages, as well their potential for integration in POC-Dx systems. At present, it seems difficult, if not impossible, to establish a procedure which can be universally applied to POC-Dx. We also discuss the effects of the NAE chemicals upon the main plastic polymers used to mass produce POC-Dx systems. We end our review discussing the limitations and challenges that should guide the quest for an efficient extraction method that can be integrated in a POC-Dx system.

Current Nucleic Acid Extraction Methods and Their Implications to Point-of-Care Diagnostics

PubMed Central

Ali, Nasir; Rampazzo, Rita de Cássia Pontello; Krieger, Marco Aurelio

2017-01-01

Nucleic acid extraction (NAE) plays a vital role in molecular biology as the primary step for many downstream applications. Many modifications have been introduced to the original 1869 method. Modern processes are categorized into chemical or mechanical, each with peculiarities that influence their use, especially in point-of-care diagnostics (POC-Dx). POC-Dx is a new approach aiming to replace sophisticated analytical machinery with microanalytical systems, able to be used near the patient, at the point of care or point of need. Although notable efforts have been made, a simple and effective extraction method is still a major challenge for widespread use of POC-Dx. In this review, we dissected the working principle of each of the most common NAE methods, overviewing their advantages and disadvantages, as well their potential for integration in POC-Dx systems. At present, it seems difficult, if not impossible, to establish a procedure which can be universally applied to POC-Dx. We also discuss the effects of the NAE chemicals upon the main plastic polymers used to mass produce POC-Dx systems. We end our review discussing the limitations and challenges that should guide the quest for an efficient extraction method that can be integrated in a POC-Dx system. PMID:28785592

Investigation of the continuous flow of the sample solution on the performance of electromembrane extraction: Comparison with conventional procedure.

PubMed

Nojavan, Saeed; Sirani, Mahsa; Asadi, Sakine

2017-10-01

In this study, electromembrane extraction from a flowing sample solution, termed as continuous-flow electromembrane extraction, was developed and compared with conventional procedures for the determination of four basic drugs in real samples. Experimental parameters affecting the extraction efficiency were further studied and optimized. Under optimum conditions, linearity of continuous-flow procedure was within 8.0-500 ng/mL, while it was wider for conventional procedures (2.0-500 ng/mL). Moreover, repeatability (percentage relative standard deviation) was found to range between 5.6 and 10.4% (n = 3) for the continuous-flow procedure, with a better repeatability than that of conventional procedures (2.3-5.5% (n = 3)). Also, for the continuous-flow procedure, the estimated detection limit (signal-to-noise ratio = 3) was less than 2.4 ng/mL and extraction recoveries were within 8-10%, while the corresponding figures for conventional procedures were less than 0.6 ng/mL and 42-60%, respectively. Thus, the results showed that both continuous flow and conventional procedures were applicable for the extraction of model compounds. However, the conventional procedure was more convenient to use, and thus it was applied to determine sample drugs in real urine and wastewater samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2013-11-01

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

Comparison of extraction induced by emulsion breaking, ultrasonic extraction and wet digestion procedures for determination of metals in edible oil samples in Turkey using ICP-OES.

PubMed

Bakircioglu, Dilek; Kurtulus, Yasemin Bakircioglu; Yurtsever, Selcuk

2013-06-01

The content of elements (Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn) in edible oils (sunflower, hazelnut, canola, corn and olive oils) from Turkey was determined using inductively coupled plasma optical emission spectrometry (ICP-OES) after ultrasonic extraction, wet digestion, and extraction induced by emulsion breaking procedures (EIEB). In order to evaluate the best sample preparation procedure, EIEB procedure was compared by ultrasonic extraction and wet digestion procedures. The results in the samples (minimum-maximum in mgkg(-1)) were : 0.022-0.058, Cr 0.126-7.106, Cu 0.570-4.504, Fe 8.004-12.588, Mn 0.035-0.054, Ni 0.908-2.182, Pb 0.099-0.134 and Zn 2.206-8.982. The EIEB procedure was found to be fast, reliable, simple, and excellent in comparison with the other studied procedures. The recovery test was performed by spiking the samples with known amounts of the metals in the form of organometallic standards and applying the EIEB procedure. The recoveries were in the range of 96-109%. Copyright © 2012 Elsevier Ltd. All rights reserved.

Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

PubMed

Rezende, Helen Cristine; Coelho, Nivia Maria Melo

2014-01-01

An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

The influence of extraction procedure on ion concentrations in sediment pore water

USGS Publications Warehouse

Winger, P.V.; Lasier, P.J.; Jackson, B.P.

1998-01-01

Sediment pore water has the potential to yield important information on sediment quality, but the influence of isolation procedures on the chemistry and toxicity are not completely known and consensus on methods used for the isolation from sediment has not been reached. To provide additional insight into the influence of collection procedures on pore water chemistry, anion (filtered only) and cation concentrations were measured in filtered and unfiltered pore water isolated from four sediments using three different procedures: dialysis, centrifugation and vacuum. Peepers were constructed using 24-cell culture plates and cellulose membranes, and vacuum extractors consisted of fused-glass air stones attached with airline tubing to 60cc syringes. Centrifugation was accomplished at two speeds (2,500 and 10,000 x g) for 30 min in a refrigerated centrifuge maintained at 4?C. Only minor differences in chemical characteristics and cation and anion concentrations were found among the different collecting methods with differences being sediment specific. Filtering of the pore water did not appreciably reduce major cation concentrations, but trace metals (Cu and Pb) were markedly reduced. Although the extraction methods evaluated produced pore waters of similar chemistries, the vacuum extractor provided the following advantages over the other methods: (1) ease of extraction, (2) volumes of pore water isolated, (3) minimal preparation time and (4) least time required for extraction of pore water from multiple samples at one time.

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

PubMed

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

2012-10-01

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

Fractionation of metals by sequential extraction procedures (BCR and Tessier) in soil exposed to fire of wide temperature range

NASA Astrophysics Data System (ADS)

Fajkovic, Hana; Rončević, Sanda; Nemet, Ivan; Prohić, Esad; Leontić-Vazdar, Dana

2017-04-01

sequential extraction procedures. The first step of Tessier and BCR extraction of samples heated at 250°C and 500°C showed increasing trend of elemental concentrations. Results of these steps are especially important since they indicate mobile fraction of the elements (exchangeable, water- and acid-soluble fraction), which can easily affect the environment. Extraction procedures of samples combusted at 850°C showed that decrease in measured elemental content occurred. Some correlation is also noticed between type of organic matter, pH and concentration of analysed elements.

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

PubMed

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

2009-07-01

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

Acidic solvent extraction of gossypol from cottonseed meal

USDA-ARS?s Scientific Manuscript database

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

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

PubMed

García-Salgado, Sara; Quijano, M Ángeles

2016-12-01

Ultrasonic probe sonication (UPS) and microwave-assisted extraction (MAE) were used for rapid single extraction of Cd, Cr, Cu, Ni, Pb, and Zn from soils polluted by former mining activities (Mónica Mine, Bustarviejo, NW Madrid, Spain), using 0.01 mol L -1 calcium chloride (CaCl 2 ), 0.43 mol L -1 acetic acid (CH 3 COOH), and 0.05 mol L -1 ethylenediaminetetraacetic acid (EDTA) at pH 7 as extracting agents. The optimum extraction conditions by UPS consisted of an extraction time of 2 min for both CaCl 2 and EDTA extractions and 15 min for CH 3 COOH extraction, at 30% ultrasound (US) amplitude, whereas in the case of MAE, they consisted of 5 min at 50 °C for both CaCl 2 and EDTA extractions and 15 min at 120 °C for CH 3 COOH extraction. Extractable concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The proposed methods were compared with a reduced version of the corresponding single extraction procedures proposed by the Standards, Measurements and Testing Programme (SM&T). The results obtained showed a great variability on extraction percentages, depending on the metal, the total concentration level and the soil sample, reaching high values in some areas. However, the correlation analysis showed that total concentration is the most relevant factor for element extractability in these soil samples. From the results obtained, the application of the accelerated extraction procedures, such as MAE and UPS, could be considered a useful approach to evaluate rapidly the extractability of the metals studied.

Therapeutic Use of Δ9-THC and Cannabidiol: Evaluation of a New Extraction Procedure for the Preparation of Cannabis-based Olive Oil.

PubMed

Morini, Luca; Porro, Giorgio; Liso, Maurizio; Groppi, Angelo

2017-01-01

Since 2013 Cannabis-based preparations, containing the two main cannabinoids of interest, Δ9-tetrahydrocannabinol (THC), and cannabidiol (CBD), can be used for therapeutic purposes, such as palliative care, neurodegenerative disorder treatment and other therapies. The preparations may consist of a drug partition in sachets, capsules or through the extraction in certified olive oil. The aims of the study were: a) to develop and validate a new liquid chromatographictandem mass spectrometric (LC-MS/MS) method for the identification and quantification of THC and CBD in olive oil; b) to evaluate the extraction efficiency and reproducibility of a new commercial extractor on the market. The olive oil was simply diluted three consecutive times, using organic solvents with increasing polarity index (n-hexane → isopropanol → methanol). The sample was then directly injected into LC-MS/MS system, operating in Multiple Reaction Monitoring Mode, in positive polarization. The method was then fully validated. The method assessed to be linear over the range 0.1-10 ng/µL for both THC and CBD. Imprecision and accuracy were within 12.2% and 16.9% respectively; matrix effects proved to be negligible; THC concentration in oil is stable up to two months at room temperature, whenever kept in the dark. CBD provided a degradation of 30% within ten weeks. The method was then applied to olive oil after sample preparation, in order to evaluate the efficiency of extraction of a new generation instrument. Temperature of extraction is the most relevant factor to be optimized. Indeed, a difference of 2°C (from 94.5°C to 96.5°C, the highest temperature reached in the experiments) of the heating phase, increases the percentage of extraction from 54.2% to 64.0% for THC and from 58.2% to 67.0% for CBD. The amount of THC acid and CBD acid that are decarboxylated during the procedure must be check out in the future. The developed method was simple and fast. The extraction procedure proved to be

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.

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

PubMed

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

2011-10-11

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

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

PubMed Central

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

2011-01-01

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

Efficient production of succinic acid from herbal extraction residue hydrolysate.

PubMed

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

2018-06-15

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

Extraction of uranium from tailings by sulfuric acid leaching with oxidants

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Liquid chromatography mass spectrometry determination of perfluoroalkyl acids in environmental solid extracts after phospholipid removal and on-line turbulent flow chromatography purification.

PubMed

Mazzoni, M; Polesello, S; Rusconi, M; Valsecchi, S

2016-07-01

An on-line TFC (Turbulent Flow Chromatography) clean up procedures coupled with UHPLC-MS/MS (Ultra High Performance Liquid Chromatography Mass Spectrometry) multi-residue method was developed for the simultaneous determination of 8 perfluroalkyl carboxylic acids (PFCA, from 5 to 12 carbon atoms) and 3 perfluoroalkyl sulfonic acids (PFSA, from 4 to 8 carbon atoms) in environmental solid matrices. Fast sample preparation procedure was based on a sonication-assisted extraction with acetonitrile. Phospholipids in biological samples were fully removed by an off-line SPE purification before injection, using HybridSPE(®) Phospholipid Ultra cartridges. The development of the on-line TFC clean-up procedure regarded the choice of the stationary phase, the optimization of the mobile phase composition, flow rate and injected volume. The validation of the optimized method included the evaluation of matrix effects, accuracy and reproducibility. Signal suppression in the analysis of fortified extracts ranged from 1 to 60%, and this problem was overcome by using isotopic dilution. Since no certified reference materials were available for PFAS in these matrices, accuracy was evaluated by recoveries on spiked clam samples which were 98-133% for PFCAs and 40-60% for PFSAs. MLDs and MLQs ranged from 0.03 to 0.3ngg(-1) wet weight and from 0.1 to 0.9ngg(-1) wet weight respectively. Repeatability (intra-day precision) and reproducibility (inter-day precision) showed RSD from 3 to 13% and from 4 to 27% respectively. Validated on-line TFC/UHPLC-MS/MS method has been applied for the determination of perfluoroalkyl acids in different solid matrices (sediment, fish, bivalves and bird yolk). Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2018-01-26

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

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

PubMed

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

2017-02-01

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

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

USDA-ARS?s Scientific Manuscript database

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

The Influence of Lactic Acid Concentration on the Separation of Light Rare Earth Elements by Continuous Liquid-Liquid Extraction with 2-Ethylhexyl Phosphonic Acid Mono-2-ethylhexyl Ester

NASA Astrophysics Data System (ADS)

de Carvalho Gomes, Rafael; Seruff, Luciana Amaral; Scal, Maira Labanca Waineraich; Vera, Ysrael Marrero

2018-02-01

The separation of rare earth elements (REEs) using solvent extraction adding complexing agents appears to be an alternative to saponification of the extractant. We evaluated the effect of lactic acid concentration on didymium (praseodymium and neodymium) and lanthanum extraction with 2-ethylhexyl phosphonic acid mono-2-ethyl hexyl ester [HEH(EHP)] as extractant. First, we investigated in batch experiments the separation of lanthanum (La) and didymium (Pr and Nd) using McCabe-Thiele diagrams to estimate the number of extraction stages when the feed solution was or was not conditioned with lactic acid. Additionally, we conducted continuous liquid-liquid extraction experiments and evaluated the influence of lactic acid concentration on the REE extraction and separation. The tests showed that the extraction percentage of REEs and the separation factor Pr/La increased when the lactic acid concentration increased, but the didymium purity decreased. Lanthanum, praseodymium, and neodymium extraction rate were 23.0, 89.7, and 99.2 pct, respectively, with 1:1 aqueous/organic volume flow rate and feed solution doped with 0.52 mol L-1 lactic acid. The highest didymium purity reached was 92.0 pct with 0.26 mol L-1 lactic acid concentration.

DEVELOPMENTS IN THE SUPERCRITICAL FLUID EXTRACTION OF CHLOROPHENOXY ACID HERBICIDES FROM SOIL SAMPLES

EPA Science Inventory

Extraction of chlorophenoxy acid herbicides from soil samples with supercritical carbon dioxide as extractant and tetrabutylammonium hydroxide and methyl iodide as derivatization agents was investigated. The extraction was carried out at 400 atm and 80 C for 15 min static, follow...

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

PubMed

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

2016-11-01

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

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.

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

NASA Astrophysics Data System (ADS)

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

2015-09-01

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

Carbon and Oxygen Isotope Measurements of Ordinary Chondrite (OC) Meteorites from Antarctica Indicate Distinct Carbonate Species Using a Stepped Acid Extraction Procedure

NASA Technical Reports Server (NTRS)

Evans, Michael E.

2015-01-01

The purpose of this study is to characterize the stable isotope values of terrestrial, secondary carbonate minerals from five Ordinary Chondrite (OC) meteorites collected in Antarctica. These samples were identified and requested from NASA based upon their size, alteration history, and collection proximity to known Martian meteorites. They are also assumed to be carbonate-free before falling to Earth. This research addresses two questions involving Mars carbonates: 1) characterize terrestrial, secondary carbonate isotope values to apply to Martian meteorites for isolating in-situ carbonates, and 2) increase understanding of carbonates formed in cold and arid environments with Antarctica as an analog for Mars. Two samples from each meteorite, each approximately 0.5 grams, were crushed and dissolved in pure phosphoric acid for 3 sequential reactions: a) R times 0 for 1 hour at 30 degrees Centigrade (fine calcite extraction), b) R times 1 for 18 hours at 30 degrees Centigrade (course calcite extraction), and c) R times 2 for 3 hours at 150 degrees Centigrade (siderite and/or magnesite extraction). CO (sub 2) was distilled by freezing with liquid nitrogen from each sample tube, then separated from organics and sulfides with a TRACE GC using a Restek HayeSep Q 80/100 6 foot 2 millimeter stainless column, and then analyzed on a Thermo MAT 253 Isotope Ratio Mass Spectrometer (IRMS) in Dual Inlet mode. This system was built at NASA/JSC over the past 3 years and proof-tested with known carbonate standards to develop procedures, assess yield, and quantify expected error bands. Two distinct species of carbonates are found: 1) calcite, and 2) non-calcite carbonate (future testing will attempt to differentiate siderite from magnesite). Preliminary results indicate the terrestrial carbonates are formed at approximately sigma (sup 13) C equal to plus 5 per mille, which is consistent with atmospheric CO (sub 2) sigma (sup 13) C equal to minus 7 per mille and fractionation of plus

Review of procedures used for the extraction of anti-cancer compounds from tropical plants.

PubMed

Pandey, Saurabh; Shaw, Paul N; Hewavitharana, Amitha K

2015-01-01

Tropical plants are important sources of anti-cancer lead molecules. According to the US National Cancer Institute, out of the 3000 plants identified as active against cancer using in vitro studies, 70% are of tropical origin. The extraction of bioactive compounds from the plant materials is a fundamental step whose efficiency is critical for the success of drug discovery efforts. There has been no review published of the extraction procedures of anti-cancer compounds from tropical plants and hence the following is a critical evaluation of such procedures undertaken prior to the use of these compounds in cancer cell line studies, during the last five years. It presents a comprehensive analysis of all approaches taken to extract anti-cancer compounds from various tropical plants. (Databases searched were PubMed, SciFinder, Web of Knowledge, Scopus, Embase and Google Scholar).

Removal of gallium (III) ions from acidic aqueous solution by supercritical carbon dioxide extraction in the green separation process.

PubMed

Chou, Wei-Lung; Wang, Chih-Ta; Yang, Kai-Chiang; Huang, Yen-Hsiang

2008-12-15

Supercritical carbon dioxide extraction, which is a feasible "green" alternative, was applied in this study as a sample pretreatment step for the removal of gallium (III) ions from acidic aqueous solution. The effect of various process parameters, including various chelating agents, extraction pressure and temperature, dimensionless CO(2) volume, the concentration of the chelating agent, and the pH of the solution, governing the efficiency and throughput of the procedure were systematically investigated. The performance of the various chelating agents from different studies indicated that the extraction efficiency of supercritical CO(2) was in the order: thiopyridine (PySH)>thenoyltrifluoroacetone (TTAH)>acetylacetone (AcAcH). The optimal extraction pressure and temperature for the supercritical CO(2) extraction of gallium (III) with chelating agent PySH were found to be 70 degrees C and 3000psi, respectively. The optimum concentration of the chelating agent was found to be 50ppm. A value of 7.5 was selected as the optimum dimensionless CO(2) volume. The optimum pH of the solution for supercritical CO(2) extraction should fall in the range of 2.0-3.0.

The effect of different solvents and number of extraction steps on the polyphenol content and antioxidant capacity of basil leaves (Ocimum basilicum L.) extracts.

PubMed

Złotek, Urszula; Mikulska, Sylwia; Nagajek, Małgorzata; Świeca, Michał

2016-09-01

The objectives of this study were to determine best conditions for the extraction of phenolic compounds from fresh, frozen and lyophilized basil leaves. The acetone mixtures with the highest addition of acetic acid extracted most of the phenolic compounds when fresh and freeze-dried material have been used. The three times procedure was more effective than once shaking procedure in most of the extracts obtained from fresh basil leaves - unlike the extracts derived from frozen material. Surprisingly, there were not any significant differences in the content of phenolics between the two used procedures in the case of lyophilized basil leaves used for extraction. Additionally, the positive correlation between the phenolic compounds content and antioxidant activity of the studied extracts has been noted. It is concluded that the acetone mixtures were more effective than the methanol ones for polyphenol extraction. The number of extraction steps in most of the cases was also a statistically significant factor affecting the yield of phenolic extraction as well as antioxidant potential of basil leaf extracts.

Vanadium Extraction from Shale via Sulfuric Acid Baking and Leaching

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

PubMed

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

2008-01-01

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

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

PubMed

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

2013-07-26

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

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

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

PubMed

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

2012-11-06

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

Development of extraction procedure for determination of mercury species using SPME-assisted dispersive derivative agent

NASA Astrophysics Data System (ADS)

Abdullah, Md Pauzi; Khalik, Wan Mohd Afiq Wan Mohd; Othman, Mohamed Rozali

2016-11-01

The extraction procedure for determination of low level mercury using solid phase microextraction was successfully carried out. Design of experimental works using factorial design and central composite design were applied to screen and predict the optimum condition for extraction step. In this study, variables namely concentration level (5 % m/v) and volume of derivatization solution (150 µL) has depicted as main effect for controlling the suitability of derivative reagent condition. Maximum of signal response (account as total peak areas for mercury species) was obtained when extraction procedure was set up at pH of water sample (5.8), extraction time (14 min), extraction temperature (43 °C) and stirring rate (450 rpm). Reducing time required to reach equilibrium is new improvement achieved in this study. Detection limit for each species (MeHg 26.17 ngL-1; EtHg 48.84 ngL-1 and IHg 14.11 ngL-1) was calculated lower than our previous work. Recovery, repeatability and reproducibility trial were recorded varied at acceptable range and relative standard deviation was calculated below than 10 %.

Ultrasound-assisted enzymatic hydrolysis for iodinated amino acid extraction from edible seaweed before reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

PubMed

Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

2013-09-27

The combination of reverse phase high performance liquid chromatography (RP-HPLC) with inductively coupled plasma mass spectrometry (ICP-MS) was used for the determination of monoiodotyrosine (MIT) and diiodotyrosine (DIT) in edible seaweed. A sample pre-treatment based on ultrasound assisted enzymatic hydrolysis was optimized for the extraction of these iodinated amino acids. Pancreatin was selected as the most adequate type of enzyme, and parameters affecting the extraction efficiency (pH, temperature, mass of enzyme and extraction time) were evaluated by univariate approaches. In addition, extractable inorganic iodine (iodide) was also quantified by anion exchange high performance liquid chromatography (AE-HPLC) coupled with ICP-MS. The proposed procedure offered limits of detection of 1.1 and 4.3ngg(-1) for MIT and DIT, respectively. Total iodine contents in seaweed, as well as total iodine in enzymatic digests were measured by ICP-MS after microwave assisted alkaline digestion with tetramethylamonium hydroxide (TMAH) for total iodine assessment, and also by treating the pancreatin extracts (extractable total iodine assessment). The optimized procedure was successfully applied to five different types of edible seaweed. The highest total iodine content, and also the highest iodide levels, was found in the brown seaweed Kombu (6646±45μgg(-1)). Regarding iodinated amino acids, Nori (a red seaweed) was by far the one with the highest amount of both species (42±3 and 0.41±0.024μgg(-1) for MIT and DIT, respectively). In general, MIT concentrations were much higher than the amounts of DIT, which suggests that iodine from iodinated proteins in seaweed is most likely bound in the form of MIT residues. Copyright © 2013 Elsevier B.V. All rights reserved.

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

USDA-ARS?s Scientific Manuscript database

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

Rapid Nucleic Acid Extraction and Purification Using a Miniature Ultrasonic Technique

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

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

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

Rapid Nucleic Acid Extraction and Purification Using a Miniature Ultrasonic Technique

DOE PAGES

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

2017-07-21

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

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

PubMed

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

2016-12-01

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

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

PubMed

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

2010-02-01

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

Cytochemical evaluation of the Guard procedure a regressive staining method for demonstrating chromosomal basic proteins. I. Effects of fixation, blocking reactions, selective extractions, and polyacid "differentiation".

PubMed

Cowden, R R; Rasch, E M; Curtis, S K

1976-08-12

Appropriately fixed preparations stained by a modification of the Guard (1959) reaction for "sex chromatin" display selective staining of interphase chromatin and mitotic or meiotic chromosomes. This is a regressive staining method which seems to depend on the selective displacement of an acidic dye from less basic structures, and retention of the dye at more basic sites. The results obtained with the reaction can be controlled by the length of time that the preparations are "differentiated" in solutions containing phosphomolybdic and phosphotungstic acids (polyacids). After three- or four-hour exposures to polyacid solutions, all chromatin is stained. However, with longer differentiation, "condensed" chromatin can be stained preferentially. Of a number of fixatives investigated, only 10% formalin, ethanol-acetic acid (3:1), and Bouin's solution proved useful. Others resulted in diminished specificity or a total loss of selectivity. The most intense staining was obtained after formalin fixation. Less intense dyebinding was observed after fixation in 3:1 - probably due to extraction of some histone fractions-and the least amount of dye was bound in Bouin's-fixed chromatin - probably due to blockage of arginine residues by picric acid. The reaction was not affected by enzymatic removal of nucleic acids or the extraction of lipids. It was diminished by treatment with trypsin or weak acetylation, and it was completely prevented by strong acetylation, deamination, or extraction of basic proteins with HCl. The results presented suggest that the modified Guard (1959) procedure selectively demonstrates basic nucleoproteins. Further, by the use of regressive differentiation in polyacid solutions, the retention of dye in more condensed chromatin can be favored.

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

PubMed Central

Shahrokhi, Nader; Keshavarzi, Zakieh; Khaksari, Mohammad

2015-01-01

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

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

NASA Astrophysics Data System (ADS)

Fidrusli, A.; Suryanto; Mahmood, M.

2018-01-01

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

DEGRADATION OF ERGOTHIONEINE BY CELL-FREE EXTRACTS OF ALCALIGENES FAECALIS II.

PubMed Central

Booth, James S.; Appleman, Milo D.

1963-01-01

Booth, James S. (University of Southern California, Los Angeles) and Milo D. Appleman. Degradation of ergothioneine by cell-free extracts of Alcaligenes faecalis. II. Production of glutamic acid. J. Bacteriol. 85:654–657. 1963.—On the basis of oxidation and paper chromatographic procedures, glutamic acid was identified as the end product of ergothioneine degradation by cell-free extracts of Alcaligenes faecalis. Hydrogen sulfide and ammonia yields were determined. Several differences between the metabolism of whole cells and cell-free extracts were noted. Cleavage of the imidazole ring by cell-free extracts appeared to be hydrolytic rather than oxidative. PMID:14042946

Determining the fatty acid composition in plasma and tissues as fatty acid methyl esters using gas chromatography – a comparison of different derivatization and extraction procedures.

PubMed

Ostermann, Annika I; Müller, Maike; Willenberg, Ina; Schebb, Nils Helge

2014-12-01

Analysis of the fatty acid (FA) composition in biological samples is commonly carried out using gas liquid chromatography (GC) after transesterification to volatile FA methyl esters (FAME). We compared the efficacy of six frequently used protocols for derivatization of different lipid classes as well as for plasma and tissue samples. Transesterification with trimethylsulfonium hydroxide (TMSH) led to insufficient derivatization efficacies for polyunsaturated FAs (PUFA, <50%). Derivatization in presence of potassium hydroxide (KOH) failed at derivatizing free FAs (FFAs). Boron trifluoride (BF3) 7% in hexane/MeOH (1:1) was insufficient for the transesterification of cholesterol ester (CE) as well as triacylglycerols (TGs). In contrast, methanolic hydrochloric acid (HCl) as well as a combination of BF3 with methanolic sodium hydroxide (NaOH+BF3) were suitable for the derivatization of FFAs, polar lipids, TGs, and CEs (derivatization rate >80% for all tested lipids). Regarding plasma samples, all methods led to an overall similar relative FA pattern. However, significant differences were observed, for example, for the relative amount of EPA+DHA (n3-index). Absolute FA plasma concentrations differed considerably among the methods, with low yields for KOH and BF3. We also demonstrate that lipid extraction with tert-butyl methyl ether/methanol (MTBE/MeOH) is as efficient as the classical method according to Bligh and Dyer, making it possible to replace (environmentally) toxic chloroform.We conclude that HCl-catalyzed derivatization in combination with MeOH/MTBE extraction is the most appropriate among the methods tested for the analysis of FA concentrations and FA pattern in small biological samples. A detailed protocol for the analysis of plasma and tissues is included in this article.

Extractive procedure for uranium determination in water samples by liquid scintillation counting.

PubMed

Gomez Escobar, V; Vera Tomé, F; Lozano, J C; Martín Sánchez, A

1998-07-01

An extractive procedure for uranium determination using liquid scintillation counting with the URAEX cocktail is described. Interference from radon and a strong influence of nitrate ion were detected in this procedure. Interference from radium, thorium and polonium emissions were very low when optimal operating conditions were reached. Quenching effects were considered and the minimum detectable activity was evaluated for different sample volumes. Isotopic analysis of samples can be performed using the proposed method. Comparisons with the results obtained with the general procedure used in alpha spectrometry with passivated implanted planar silicon detectors showed good agreement. The proposed procedure is thus suitable for uranium determination in water samples and can be considered as an alternative to the laborious conventional chemical preparations needed for alpha spectrometry methods using semiconductor detectors.

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

PubMed

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

2017-02-23

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

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

PubMed

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

2016-06-01

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

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

Treesearch

Carol Clausen

2004-01-01

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

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

PubMed

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

2016-08-01

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

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

PubMed Central

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

2010-01-01

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

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

PubMed

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

2004-01-01

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

Procedure for extraction of disparate data from maps into computerized data bases

NASA Technical Reports Server (NTRS)

Junkin, B. G.

1979-01-01

A procedure is presented for extracting disparate sources of data from geographic maps and for the conversion of these data into a suitable format for processing on a computer-oriented information system. Several graphic digitizing considerations are included and related to the NASA Earth Resources Laboratory's Digitizer System. Current operating procedures for the Digitizer System are given in a simplified and logical manner. The report serves as a guide to those organizations interested in converting map-based data by using a comparable map digitizing system.

Lactic acid bacterial extract as a biogenic mineral growth modifier

NASA Astrophysics Data System (ADS)

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

2009-04-01

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

Extractive fermentation for enhanced propionic acid production from lactose by Propionibacterium acidipropionici

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

Jin, Z.; Yang, S.T.

1998-05-01

An extractive fermentation process using an amine extractant and a hollow-fiber membrane extractor to selectively remove propionic acid from the fermentation broth was developed to produce propionate from lactose. Compared to the conventional batch fermentation, the extractive fermentation had a much higher productivity ({approximately}1 g/(L{center_dot}h) or 5-fold increase), higher propionate yield (up to 0.66 g/g or more than 20% increase), higher final product concentration (75 g/L or higher), and higher product purity ({approximately}90%). Meanwhile, acetate and succinate productions in the extractive fermentation were significantly reduced. The improved fermentation performance can be attributed to the reduced product inhibition and a possiblemore » metabolic pathway shift to favor more propionic but less acetic and succinic acid production. The process was stable and gave consistent long-term performance over the 1.5-month period studied. The effects of propionate concentration, pH, and amine content in the solvent on the extractive fermentation were also studied and are discussed in this paper.« less

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

PubMed

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

2016-09-12

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

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

PubMed Central

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

2016-01-01

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

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

PubMed

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

2017-02-01

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

SOLVENT EXTRACTION PROCESS FOR THE RECOVERY OF METALS FROM PHOSPHORIC ACID

DOEpatents

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

1958-11-01

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

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

DOEpatents

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

2007-03-27

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

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

DOEpatents

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

2004-06-22

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

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

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

High-performance liquid chromatographic determination of ursodeoxycholic acid after solid phase extraction of blood serum and detection-oriented derivatization.

PubMed

Nobilis, M; Pour, M; Kunes, J; Kopecký, J; Kvĕtina, J; Svoboda, Z; Sládková, K; Vortel, J

2001-03-01

Ursodeoxycholic acid (3 alpha,7 beta-dihydroxy-5 beta-cholanoic acid, UDCA) is a therapeutically applicable bile acid widely used for the dissolution of cholesterol-rich gallstones and in the treatment of chronic liver diseases associated with cholestasis. UDCA is more hydrophilic and less toxic than another therapeutically valuable bile acid, chenodeoxycholic acid (CDCA), the 7 alpha-epimer of UDCA. Procedures for sample preparation and HPLC determination of UDCA in blood serum were developed and validated. A higher homologue of UDCA containing an additional methylene group in the side chain was synthetized and used as an internal standard (IS). Serum samples with IS were diluted with a buffer (pH=7). The bile acids and IS were captured using solid phase extraction (C18 cartridges). The carboxylic group of the analytes was derivatized using 2-bromo-2'-acetonaphthone (a detection-oriented derivatization), and reaction mixtures were analyzed (HPLC with UV 245 nm detection; a 125--4 mm column containing Lichrospher 100 C18, 5 microm; mobile phase: acetonitrile--water, 6:4 (v/v)). Following validation, this method was used for pharmacokinetic studies of UDCA in humans.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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

NASA Astrophysics Data System (ADS)

Bekhterev, V. N.

2016-10-01

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

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

PubMed

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

2016-05-01

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

eCTG: an automatic procedure to extract digital cardiotocographic signals from digital images.

PubMed

Sbrollini, Agnese; Agostinelli, Angela; Marcantoni, Ilaria; Morettini, Micaela; Burattini, Luca; Di Nardo, Francesco; Fioretti, Sandro; Burattini, Laura

2018-03-01

Cardiotocography (CTG), consisting in the simultaneous recording of fetal heart rate (FHR) and maternal uterine contractions (UC), is a popular clinical test to assess fetal health status. Typically, CTG machines provide paper reports that are visually interpreted by clinicians. Consequently, visual CTG interpretation depends on clinician's experience and has a poor reproducibility. The lack of databases containing digital CTG signals has limited number and importance of retrospective studies finalized to set up procedures for automatic CTG analysis that could contrast visual CTG interpretation subjectivity. In order to help overcoming this problem, this study proposes an electronic procedure, termed eCTG, to extract digital CTG signals from digital CTG images, possibly obtainable by scanning paper CTG reports. eCTG was specifically designed to extract digital CTG signals from digital CTG images. It includes four main steps: pre-processing, Otsu's global thresholding, signal extraction and signal calibration. Its validation was performed by means of the "CTU-UHB Intrapartum Cardiotocography Database" by Physionet, that contains digital signals of 552 CTG recordings. Using MATLAB, each signal was plotted and saved as a digital image that was then submitted to eCTG. Digital CTG signals extracted by eCTG were eventually compared to corresponding signals directly available in the database. Comparison occurred in terms of signal similarity (evaluated by the correlation coefficient ρ, and the mean signal error MSE) and clinical features (including FHR baseline and variability; number, amplitude and duration of tachycardia, bradycardia, acceleration and deceleration episodes; number of early, variable, late and prolonged decelerations; and UC number, amplitude, duration and period). The value of ρ between eCTG and reference signals was 0.85 (P < 10 -560 ) for FHR and 0.97 (P < 10 -560 ) for UC. On average, MSE value was 0.00 for both FHR and UC. No CTG feature

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

PubMed

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

2017-07-18

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

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

PubMed

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

2007-01-30

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

Speciation of antimony in airborne particulate matter using ultrasound probe fast extraction and analysis by HPLC-HG-AFS.

PubMed

Bellido-Martín, A; Gómez-Ariza, J L; Smichowsky, P; Sánchez-Rodas, D

2009-09-07

A fast extraction procedure has been developed for Sb(III) and Sb(V) oxoanions speciation in airborne particulate matter samples. Different extraction media (diammonium tartrate, hidroxilammonium clorhidrate, citric acid+ascorbic acid, phosphoric acid and citrate solutions) were tried, with assistance of an ultrasonic probe. The operation power and time of extraction were also optimized. The higher extraction recoveries were obtained with a 100 mmol L(-1) hidroxilammonium clorhidrate aqueous solution assisted by the ultrasound probe operated at 50 W during 3 min. The extracts were analyzed by HPLC-HG-AFS. The chromatographic separation of Sb(III) and Sb(V) was also optimized using diammonium tartrate and phthalic acid as mobile phases. The separation of both Sb species was performed in less than 3 min under isocratic conditions, using a 200 mmol L(-1) diammonium tartrate solution. The proposed extraction procedure and the HPLC-HG-AFS instrumental coupling have been successfully applied to airborne particulate matter samples, with high Sb content, collected in heavy traffic streets from Buenos Aires (Argentina). The results showed the presence of both Sb species at similar concentrations in the ng m(-3) level. The extraction yield was higher than 90% for all the analyzed samples.

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

USDA-ARS?s Scientific Manuscript database

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

Perfluorodecanoic Acid and Lipid Metabolism in the Rat

DTIC Science & Technology

1989-05-25

2. To develop analogous methodologies for perfluorooctanoic acid ( PFOA ), a shorter-chain perfluorinated fatty acid similar to PFDA . 3. To validate...the procedures for the extraction, separation and quantitation of the perfluorinated acids following in vivo administration of either PFDA or PFOA to... Perfluorodecanoic acid ( PFDA ), representative of these in rats killed by cervical dislocation seven days post- perfluorinated fatty acids, resulted in a

Solid-phase extraction using bis(indolyl)methane-modified silica reinforced with multiwalled carbon nanotubes for the simultaneous determination of flavonoids and aromatic organic acid preservatives.

PubMed

Wang, Na; Liao, Yuan; Wang, Jiamin; Tang, Sheng; Shao, Shijun

2015-12-01

A novel bis(indolyl)methane-modified silica reinforced with multiwalled carbon nanotubes sorbent for solid-phase extraction was designed and synthesized by chemical immobilization of nitro-substituted 3,3'-bis(indolyl)methane on silica modified with multiwalled carbon nanotubes. Coupled with high-performance liquid chromatography analysis, the extraction properties of the sorbent were evaluated for flavonoids and aromatic organic acid compounds. Under optimum conditions, the sorbent can simultaneously extract five flavonoids and two aromatic organic acid preservatives in aqueous solutions in a single-step solid-phase extraction procedure. Wide linear ranges were obtained with correlation coefficients (R(2) ) ranging from 0.9843 to 0.9976, and the limits of detection were in the range of 0.5-5 μg/L for the compounds tested. Compared with the silica modified with multiwalled carbon nanotubes sorbent and the nitro-substituted 3,3'-bis(indolyl)methane-modified silica sorbent, the developed sorbent exhibited higher extraction efficiency toward the selected analytes. The synergistic effect of nitro-substituted 3,3'-bis(indolyl)methane and multiwalled carbon nanotubes not only improved the surface-to-volume ratio but also enhanced multiple intermolecular interactions, such as hydrogen bonds, π-π, and hydrophobic interactions, between the new sorbent and the selected analytes. The as-established solid-phase extraction with high-performance liquid chromatography and diode array detection method was successfully applied to the simultaneous determination of flavonoids and aromatic organic acid preservatives in grape juices with recoveries ranging from 83.9 to 112% for all the selected analytes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2014-08-01

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

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

PubMed

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

2017-11-01

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

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

PubMed

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

2015-07-14

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

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

PubMed

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

2012-07-01

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

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

DOEpatents

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

2006-07-11

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

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

DOEpatents

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

2002-01-01

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

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

USGS Publications Warehouse

Krynitsky, A.J.; Stafford, C.J.; Wiemeyer, Stanley N.

1988-01-01

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

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

PubMed Central

Skea, D; Broder, I

1986-01-01

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

Determining gold in water by anion-exchange batch extraction

USGS Publications Warehouse

McHugh, J.B.

1986-01-01

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

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; comparison of a nitric acid in-bottle digestion procedure to other whole-water digestion procedures

USGS Publications Warehouse

Garbarino, John R.; Hoffman, Gerald L.

1999-01-01

A hydrochloric acid in-bottle digestion procedure is used to partially digest wholewater samples prior to determining recoverable elements by various analytical methods. The use of hydrochloric acid is problematic for some methods of analysis because of spectral interference. The inbottle digestion procedure has been modified to eliminate such interference by using nitric acid instead of hydrochloric acid in the digestion. Implications of this modification are evaluated by comparing results for a series of synthetic whole-water samples. Results are also compared with those obtained by using U.S. Environmental Protection Agency (1994) (USEPA) Method 200.2 total-recoverable digestion procedure. Percentage yields that use the nitric acid inbottle digestion procedure are within 10 percent of the hydrochloric acid in-bottle yields for 25 of the 26 elements determined in two of the three synthetic whole-water samples tested. Differences in percentage yields for the third synthetic whole-water sample were greater than 10 percent for 16 of the 26 elements determined. The USEPA method was the most rigorous for solubilizing elements from particulate matter in all three synthetic whole-water samples. Nevertheless, the variability in the percentage yield by using the USEPA digestion procedure was generally greater than the in-bottle digestion procedure, presumably because of the difficulty in controlling the digestion conditions accurately.

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

PubMed

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

2002-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Evaluation of sequential extraction procedures for soluble and insoluble hexavalent chromium compounds in workplace air samples.

PubMed

Ashley, Kevin; Applegate, Gregory T; Marcy, A Dale; Drake, Pamela L; Pierce, Paul A; Carabin, Nathalie; Demange, Martine

2009-02-01

Because toxicities may differ for Cr(VI) compounds of varying solubility, some countries and organizations have promulgated different occupational exposure limits (OELs) for soluble and insoluble hexavalent chromium (Cr(VI)) compounds, and analytical methods are needed to determine these species in workplace air samples. To address this need, international standard methods ASTM D6832 and ISO 16740 have been published that describe sequential extraction techniques for soluble and insoluble Cr(VI) in samples collected from occupational settings. However, no published performance data were previously available for these Cr(VI) sequential extraction procedures. In this work, the sequential extraction methods outlined in the relevant international standards were investigated. The procedures tested involved the use of either deionized water or an ammonium sulfate/ammonium hydroxide buffer solution to target soluble Cr(VI) species. This was followed by extraction in a sodium carbonate/sodium hydroxide buffer solution to dissolve insoluble Cr(VI) compounds. Three-step sequential extraction with (1) water, (2) sulfate buffer and (3) carbonate buffer was also investigated. Sequential extractions were carried out on spiked samples of soluble, sparingly soluble and insoluble Cr(VI) compounds, and analyses were then generally carried out by using the diphenylcarbazide method. Similar experiments were performed on paint pigment samples and on airborne particulate filter samples collected from stainless steel welding. Potential interferences from soluble and insoluble Cr(III) compounds, as well as from Fe(II), were investigated. Interferences from Cr(III) species were generally absent, while the presence of Fe(II) resulted in low Cr(VI) recoveries. Two-step sequential extraction of spiked samples with (first) either water or sulfate buffer, and then carbonate buffer, yielded quantitative recoveries of soluble Cr(VI) and insoluble Cr(VI), respectively. Three-step sequential

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

PubMed

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

2018-04-18

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

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

PubMed

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

2018-02-02

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

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

PubMed

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

2009-04-01

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

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

PubMed

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

2018-03-01

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

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

ERIC Educational Resources Information Center

Brunner, Ulrich

1985-01-01

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

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.

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

PubMed

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

2017-07-10

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

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SOLID FOOD SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.28)

EPA Science Inventory

This SOP describes the extraction and preparation of a solid food sample for analysis of acidic persistent organic pollutants such as acid herbicides, pentachlorphenol, and 3,5,6-trichloro-2-phenol. It covers the extraction, concentration and derivatization of samples that are to...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING LIQUID FOOD SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.29)

EPA Science Inventory

This SOP describes the extraction and preparation of a liquid food sample for analysis of acidic persistent organic pollutants such as acid herbicides, pentachlorphenol, and 3,5,6-trichloro-2-phenol. It covers the extraction, concentration and derivatization of samples that are t...

Effect of Extraction Conditions on the Antioxidant Activity of Olive Wood Extracts

PubMed Central

Pérez-Bonilla, Mercedes; Salido, Sofía; Sánchez, Adolfo; van Beek, Teris A.; Altarejos, Joaquín

2013-01-01

An investigation to optimize the extraction yield and the radical scavenging activity from the agricultural by-product olive tree wood (Olea europaea L., cultivar Picual) using six different extraction protocols was carried out. Four olive wood samples from different geographical origin, and harvesting time have been used for comparison purposes. Among the fifty olive wood extracts obtained in this study, the most active ones were those prepared with ethyl acetate, either through direct extraction or by successive liquid-liquid partitioning procedures, the main components being the secoiridoids oleuropein and ligustroside. An acid hydrolysis pretreatment of olive wood samples before extractions did not improve the results. In the course of this study, two compounds were isolated from the ethanolic extracts of olive wood collected during the olives' harvesting season and identified as (7′′R)-7′′-ethoxyoleuropein (1) and (7′′S)-7′′-ethoxyoleuropein (2). PMID:26904608

Quality control considerations for the determination of acid-volatile sulfide and simultaneously extracted metals in sediments

USGS Publications Warehouse

Brumbaugh, William G.; Arms, Jesse W.

1996-01-01

The determination of acid-volatile sulfide (AVS) and simultaneously extracted metals (SEMs) in sediment by treatment with dilute HCl shows promise as a tool for predicting the potential for metal toxicity to sediment-dwelling organisms. Effective quality control measures must be developed if this method is to become a reliable procedure and to ensure comparability of data. However, establishing quality control measures that assess procedural errors for an operationally defined method can be problematic. For example, preextraction spikes added for assessing the accuracy of AVS and SEMs may be poorly recovered due to adsorption or reaction with sediment constituents. For a variety of sediment types, we found preextraction spikes of sulfide, mercury, and copper to be prone to variable recoveries for the AVS/SEM procedure; recoveries averaged 76.3% (SD, 20.9) for sulfide, 61.9% (39.6) for Hg, and 90.1% (12.7) for Cu. The average recovery was near 100% for preextraction spikes of sediments for Cd, Ni, Pb, and Zn, and the recoveries of preextraction blank spikes for all analytes were consistently 95 to 105%. Binding of Cu or Hg with sulfides is sufficiently strong that 1 N hydrochloric acid will not necessarily keep the spiked metal in the dissolved state. This does not mean that the SEM procedure is invalid for these metals, only that the quality control of procedural error is difficult to assess. However, Hg will generally not be detected when measured as an SEM because of its tendency to adsorb onto sulfide minerals even at extremely low pH. Some reference sediments may be useful for assessing consistency of AVS determinations; we measured 5.97 ± 0.65 μmol/g in National Institute of Standards and Technology (NIST) 1645 and 1.34 ± 0.14 μmol/g in NIST 2704 for repeated determinations conducted over the past 3 years. Apparently, some sediments may contain an oxidation-resistant sulfide component that can release low to moderate AVS when treated with dilute HCl.

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

PubMed

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

2012-08-24

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

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

PubMed

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

2006-01-01

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

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

PubMed

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

2012-01-01

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

Microwave-assisted extraction of coumarin and related compounds from Melilotus officinalis (L.) Pallas as an alternative to Soxhlet and ultrasound-assisted extraction.

PubMed

Martino, Emanuela; Ramaiola, Ilaria; Urbano, Mariangela; Bracco, Francesco; Collina, Simona

2006-09-01

Soxhlet extraction, ultrasound-assisted extraction (USAE) and microwaves-assisted extraction (MAE) in closed system have been investigated to determine the content of coumarin, o-coumaric and melilotic acids in flowering tops of Melilotus officinalis. The extracts were analyzed with an appropriate HPLC procedure. The reproducibility of extraction and of chromatographic analysis was proved. Taking into account the extraction yield, the cost and the time, we studied the effects of extraction variables on the yield of the above-mentioned compounds. Better results were obtained with MAE (50% v/v aqueous ethanol, two heating cycles of 5 min, 50 degrees C). On the basis of the ratio extraction yield/extraction time, we therefore propose MAE as the most efficient method.

Selenium speciation in phosphate mine soils and evaluation of a sequential extraction procedure using XAFS.

PubMed

Favorito, Jessica E; Luxton, Todd P; Eick, Matthew J; Grossl, Paul R

2017-10-01

Selenium is a trace element found in western US soils, where ingestion of Se-accumulating plants has resulted in livestock fatalities. Therefore, a reliable understanding of Se speciation and bioavailability is critical for effective mitigation. Sequential extraction procedures (SEP) are often employed to examine Se phases and speciation in contaminated soils but may be limited by experimental conditions. We examined the validity of a SEP using X-ray absorption spectroscopy (XAS) for both whole and a sequence of extracted soils. The sequence included removal of soluble, PO 4 -extractable, carbonate, amorphous Fe-oxide, crystalline Fe-oxide, organic, and residual Se forms. For whole soils, XANES analyses indicated Se(0) and Se(-II) predominated, with lower amounts of Se(IV) present, related to carbonates and Fe-oxides. Oxidized Se species were more elevated and residual/elemental Se was lower than previous SEP results from ICP-AES suggested. For soils from the SEP sequence, XANES results indicated only partial recovery of carbonate, Fe-oxide and organic Se. This suggests Se was incompletely removed during designated extractions, possibly due to lack of mineral solubilization or reagent specificity. Selenium fractions associated with Fe-oxides were reduced in amount or removed after using hydroxylamine HCl for most soils examined. XANES results indicate partial dissolution of solid-phases may occur during extraction processes. This study demonstrates why precautions should be taken to improve the validity of SEPs. Mineralogical and chemical characterizations should be completed prior to SEP implementation to identify extractable phases or mineral components that may influence extraction effectiveness. Sequential extraction procedures can be appropriately tailored for reliable quantification of speciation in contaminated soils. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Sibuyo, Leah; Widiputri, Diah; Legowo, Evita

2017-01-01

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

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

PubMed

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

2018-01-01

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

Recovery of Uranium from Wet Phosphoric Acid by Solvent Extraction Processes

DOE PAGES

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

2014-11-17

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

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

PubMed

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

2013-01-15

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

Effects of ω-Amino Acids and Related Compounds on Staphylococcal Infections in Mice: a Combined Prophylactic-Therapeutic Procedure 1

PubMed Central

Tsuchiya, Yoshiki; Tanaka, Kinji; Cook, Elton S.; Nutini, Leo G.

1970-01-01

By a short-term combined prophylactic-therapeutic procedure, the following compounds were found to be active against staphylococcal infections in Swiss mice: γ-aminobutyric acid, γ-amino-β-hydroxybutyric acid (GABOB), δ-amino-valeric acid (DAVA), ε-aminocaproic acid (EACA), trans-4-aminomethylcyclohexanecarboxylic acid (trans-AMCHA), taurine, and cysteic acid. Many of these compounds had displayed limited or no activity by a previously used prophylactic procedure. Although DAVA and GABOB were the most potent of the straight-chain ω-amino acids, trans-AMCHA displayed the greatest antistaphylococcic activity of the ω-amino acids thus far investigated. Homocarnosine (γ-aminobutyrl histidine, which also was active by the prophylactic procedure) equalled trans-AMCHA in activity. Taurine was similar in potency to DAVA, and the activity of cysteic acid approximated that of EACA. PMID:5422309

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.

A modal parameter extraction procedure applicable to linear time-invariant dynamic systems

NASA Technical Reports Server (NTRS)

Kurdila, A. J.; Craig, R. R., Jr.

1985-01-01

Modal analysis has emerged as a valuable tool in many phases of the engineering design process. Complex vibration and acoustic problems in new designs can often be remedied through use of the method. Moreover, the technique has been used to enhance the conceptual understanding of structures by serving to verify analytical models. A new modal parameter estimation procedure is presented. The technique is applicable to linear, time-invariant systems and accommodates multiple input excitations. In order to provide a background for the derivation of the method, some modal parameter extraction procedures currently in use are described. Key features implemented in the new technique are elaborated upon.

Extraction of hyaluronic acid (HA) from rooster comb and characterization using flow field-flow fractionation (FlFFF) coupled with multiangle light scattering (MALS).

PubMed

Kang, Dong Young; Kim, Won-Suk; Heo, In Sook; Park, Young Hun; Lee, Seungho

2010-11-01

Hyaluronic acid (HA) was extracted in a relatively large scale from rooster comb using a method similar to that reported previously. The extraction method was modified to simplify and to reduce time and cost in order to accommodate a large-scale extraction. Five hundred grams of frozen rooster combs yielded about 500 mg of dried HA. Extracted HA was characterized using asymmetrical flow field-flow fractionation (AsFlFFF) coupled online to a multiangle light scattering detector and a refractive index detector to determine the molecular size, molecular weight (MW) distribution, and molecular conformation of HA. For characterization of HA, AsFlFFF was operated by a simplified two-step procedure, instead of the conventional three-step procedure, where the first two steps (sample loading and focusing) were combined into one to avoid the adsorption of viscous HA onto the channel membrane. The simplified two-step AsFlFFF yielded reasonably good separations of HA molecules based on their MWs. The weight average MW (M(w) ) and the average root-mean-square (RMS) radius of HA extracted from rooster comb were 1.20×10(6) and 94.7 nm, respectively. When the sample solution was filtered through a 0.45 μm disposable syringe filter, they were reduced down to 3.8×10(5) and 50.1 nm, respectively. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Direct methylation procedure for converting fatty amides to fatty acid methyl esters in feed and digesta samples.

PubMed

Jenkins, T C; Thies, E J; Mosley, E E

2001-05-01

Two direct methylation procedures often used for the analysis of total fatty acids in biological samples were evaluated for their application to samples containing fatty amides. Methylation of 5 mg of oleamide (cis-9-octadecenamide) in a one-step (methanolic HCl for 2 h at 70 degrees C) or a two-step (sodium methoxide for 10 min at 50 degrees C followed by methanolic HCl for 10 min at 80 degrees C) procedure gave 59 and 16% conversions of oleamide to oleic acid, respectively. Oleic acid recovery from oleamide was increased to 100% when the incubation in methanolic HCl was lengthened to 16 h and increased to 103% when the incubation in methoxide was modified to 24 h at 100 degrees C. However, conversion of oleamide to oleic acid in an animal feed sample was incomplete for the modified (24 h) two-step procedure but complete for the modified (16 h) one-step procedure. Unsaturated fatty amides in feed and digesta samples can be converted to fatty acid methyl esters by incubation in methanolic HCl if the time of exposure to the acid catalyst is extended from 2 to 16 h.

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

PubMed Central

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

2016-01-01

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

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

USDA-ARS?s Scientific Manuscript database

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

Method for distinctive estimation of stored acidity forms in acid mine wastes.

PubMed

Li, Jun; Kawashima, Nobuyuki; Fan, Rong; Schumann, Russell C; Gerson, Andrea R; Smart, Roger St C

2014-10-07

Jarosites and schwertmannite can be formed in the unsaturated oxidation zone of sulfide-containing mine waste rock and tailings together with ferrihydrite and goethite. They are also widely found in process wastes from electrometallurgical smelting and metal bioleaching and within drained coastal lowland soils (acid-sulfate soils). These secondary minerals can temporarily store acidity and metals or remove and immobilize contaminants through adsorption, coprecipitation, or structural incorporation, but release both acidity and toxic metals at pH above about 4. Therefore, they have significant relevance to environmental mineralogy through their role in controlling pollutant concentrations and dynamics in contaminated aqueous environments. Most importantly, they have widely different acid release rates at different pHs and strongly affect drainage water acidity dynamics. A procedure for estimation of the amounts of these different forms of nonsulfide stored acidity in mining wastes is required in order to predict acid release rates at any pH. A four-step extraction procedure to quantify jarosite and schwertmannite separately with various soluble sulfate salts has been developed and validated. Corrections to acid potentials and estimation of acid release rates can be reliably based on this method.

Rapid analytical procedure for determination of mineral oils in edible oil by GC-FID.

PubMed

Wrona, Magdalena; Pezo, Davinson; Nerin, Cristina

2013-12-15

A procedure for the determination of mineral oils in edible oil has been fully developed. The procedure consists of using a sulphuric acid-impregnated silica gel (SAISG) glass column to eliminate the fat matter. A chemical combustion of the fatty acids takes place, while the mineral oils are not affected by the sulphuric acid. The column is eluted with hexane using a vacuum pump and the final extract is concentrated and analysed by gas chromatography (GC) with flame ionisation detector (FID). The detection limit (LOD) and the quantification limit (LOQ) in hexane were 0.07 and 0.21 μg g(-1) respectively and the LOQ in vegetable oil was 1 μg g(-1). Only a few minutes were necessary for sample treatment to have a clean extract. The efficiency of the process, measured through the recoveries from spiked samples of edible oil was higher than 95%. The procedure has been applied to determine mineral oil in olive oil from the retailed market. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

PubMed Central

Zarembski, P. M.; Hodgkinson, A.

1965-01-01

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

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

PubMed

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

2015-01-01

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

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

PubMed

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

2008-02-15

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

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

NASA Astrophysics Data System (ADS)

Rhea, James R.; Young, Thomas C.

1987-10-01

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

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

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

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

1987-01-01

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

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

PubMed Central

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

2018-01-01

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

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

PubMed

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

2015-11-01

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

A two-stage extraction procedure for insensitive munition (IM) explosive compounds in soils.

PubMed

Felt, Deborah; Gurtowski, Luke; Nestler, Catherine C; Johnson, Jared; Larson, Steven

2016-12-01

The Department of Defense (DoD) is developing a new category of insensitive munitions (IMs) that are more resistant to detonation or promulgation from external stimuli than traditional munition formulations. The new explosive constituent compounds are 2,4-dinitroanisole (DNAN), nitroguanidine (NQ), and nitrotriazolone (NTO). The production and use of IM formulations may result in interaction of IM component compounds with soil. The chemical properties of these IM compounds present unique challenges for extraction from environmental matrices such as soil. A two-stage extraction procedure was developed and tested using several soil types amended with known concentrations of IM compounds. This procedure incorporates both an acidified phase and an organic phase to account for the chemical properties of the IM compounds. The method detection limits (MDLs) for all IM compounds in all soil types were <5 mg/kg and met non-regulatory risk-based Regional Screening Level (RSL) criteria for soil proposed by the U.S. Army Public Health Center. At defined environmentally relevant concentrations, the average recovery of each IM compound in each soil type was consistent and greater than 85%. The two-stage extraction method decreased the influence of soil composition on IM compound recovery. UV analysis of NTO established an isosbestic point based on varied pH at a detection wavelength of 341 nm. The two-stage soil extraction method is equally effective for traditional munition compounds, a potentially important point when examining soils exposed to both traditional and insensitive munitions. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

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

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

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

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

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

Lin, Yuehe; Liu, Chongxuan; Wu, Hong

2003-03-02

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

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

PubMed

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

2013-01-01

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

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

PubMed

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

2017-09-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Determination of 1-aminocyclopropane-1-carboxylic acid in apple extracts by capillary electrophoresis with laser-induced fluorescence detection.

PubMed

Liu, Xin; Li, Dian-Fan; Wang, Yun; Lu, Ying-Tang

2004-12-17

A rapid and sensitive method for the determination of 1-aminocyclopropane-1-carboxylic acid (ACC) in apple tissues has been described. This method is based on the derivatization of ACC with 3-(2-furoyl)quinoline-2-carboxaldehyde (FQ), and separation and quantification of the resulting FQ-ACC derivative by capillary electrophoresis coupled to laser-induced fluorescence detection (CE-LIF). Our results indicated that ACC derivatized with FQ could be well separated from other interfering amino acids using 20 mM borate buffer (pH 9.35) containing 40 mM sodium dodecyl sulfate and 10 mM Brij 35. The linearity of ACC was determined in the range from 0.05 to 5 microM with a correlation of 0.9967. The concentration detection limit for ACC was 10 nM (signal-to-noise = 3). The sensitivity and selectivity of this described method allows the analysis of ACC in crude apple extracts without extra purification and enrichment procedure.

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

PubMed

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

2017-04-01

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

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.

A novel dual-valve sequential injection manifold (DV-SIA) for automated liquid-liquid extraction. Application for the determination of picric acid.

PubMed

Skrlíková, Jana; Andruch, Vasil; Sklenárová, Hana; Chocholous, Petr; Solich, Petr; Balogh, Ioseph S

2010-05-07

A novel dual-valve sequential injection system (DV-SIA) for online liquid-liquid extraction which resolves the main problems of LLE utilization in SIA has been designed. The main idea behind this new design was to construct an SIA system by connecting two independent units, one for aqueous-organic mixture flow and the second specifically for organic phase flow. As a result, the DV-SIA manifold consists of an Extraction unit and a Detection unit. Processing a mixture of aqueous-organic phase in the Extraction unit and a separated organic phase in the Detection unit solves the problems associated with the change of phases having different affinities to the walls of the Teflon tubing used in the SI-system. The developed manifold is a simple, user-friendly and universal system built entirely from commercially available components. The system can be used for a variety of samples and organic solvents and is simple enough to be easily handled by operators less familiar with flow systems. The efficiency of the DV-SIA system is demonstrated by the extraction of picric acid in the form of an ion associate with 2-[2-(4-methoxy-phenylamino)-vinyl]-1,3,3-trimethyl-3H-indolium reagent, with subsequent spectrophotometric detection. The suggested DV-SIA concept can be expected to stimulate new experiments in analytical laboratories and can be applied to the elaboration of procedures for the determination of other compounds extractable by organic solvents. It could thus form a basis for the design of simple, single-purpose commercial instruments used in LLE procedures. 2010 Elsevier B.V. All rights reserved.

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

PubMed

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

2012-07-01

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

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

PubMed

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

2016-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2013-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1971-01-01

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

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

DOE PAGES

Ellis, Ross J.

2016-08-09

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

A validated solid-liquid extraction method for the HPLC determination of polyphenols in apple tissues Comparison with pressurised liquid extraction.

PubMed

Alonso-Salces, Rosa M; Barranco, Alejandro; Corta, Edurne; Berrueta, Luis A; Gallo, Blanca; Vicente, Francisca

2005-02-15

A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5g of freeze-dried apple tissue with 30mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2g of ascorbic acid/L, for 10min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed.

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

PubMed

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

2011-01-01

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

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

Treesearch

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

2009-01-01

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

Multi-residue analysis of 26 organochlorine pesticides in Alpinia oxyphylla by GC-ECD after solid phase extraction and acid cleanup.

PubMed

Zhao, Xiangsheng; Zhou, Yakui; Kong, Weijun; Gong, Bao; Chen, Deli; Wei, Jianhe; Yang, Meihua

2016-04-01

A simple and effective multi-residue method was developed and validated for the analysis of 26 organochlorine pesticide residues in Alpinia oxyphylla by a gas chromatography with an electron capture detector (GC-ECD). The target pesticides were extracted by sonication and cleaned up with florisil solid phase extraction and sulphuric acid. Some crucial parameters, including extraction solvent and time, sorbent type, elute solvent and concentration of sulphuric acid were optimized to improve the performance of sample preparation procedure. The optimized method gave high sensitivity with detection limit ranging from 0.1 to 2.0μg/kg. Matrix-matched calibration was employed for the quantification, and a wide linear range (from 1.0 to 1000μg/kg) with r(2) values ranging from 0.9971 to 0.9998 was obtained. For the majority of the tested pesticides, the average recoveries were in acceptable range (between 70% and 110%) with relative standard deviation values below 15.0%. Matrix effect was evaluated for target compounds through the study of ratio of peak area obtained in the solvent and blank matrix. The proposed method was applied to simultaneously analyze 26 pesticides in 55 batches of Alpinia oxyphylla samples. 3 samples were found to be positive with four pesticides (α-BHC, quintozene, trans-chlordane and op'-DDD), which were confirmed by gas chromatography-mass spectrometry (GC-MS) in selective ion monitoring (SIM) mode. Copyright © 2016 Elsevier B.V. All rights reserved.

Improved method for extracting lanthanides and actinides from acid solutions

DOEpatents

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

1983-07-26

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

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

PubMed Central

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

2017-01-01

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

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

PubMed Central

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

2017-01-01

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

Extraction of kiwi seed oil: Soxhlet versus four different non-conventional techniques.

PubMed

Cravotto, Giancarlo; Bicchi, Carlo; Mantegna, Stefano; Binello, Arianna; Tomao, Valerie; Chemat, Farid

2011-06-01

Kiwi seed oil has a nutritionally interesting fatty acid profile, but a rather low oxidative stability, which requires careful extraction procedures and adequate packaging and storage. For these reasons and with the aim to achieve process intensification with shorter extraction time, lower energy consumption and higher yields, four different non-conventional techniques were experimented. Kiwi seeds were extracted in hexane using classic Soxhlet as well as under power ultrasound (US), microwaves (MWs; closed vessel) and MW-integrated Soxhlet. Supercritical CO₂ was also employed and compared to the other techniques in term of yield, extraction time, fatty acid profiles and organoleptic properties. All these non-conventional techniques are fast, effective and safe. A sensory evaluation test showed the presence of off-flavours in oil samples extracted by Soxhlet and US, an indicator of partial degradation.

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

PubMed

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

2016-03-01

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

[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

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.

Effect of preparation procedures on intensity of radioautographic labeling is studied

NASA Technical Reports Server (NTRS)

Baserga, R.; Kisieleski, W. E.

1967-01-01

Effects of tissue preparation and extractive procedures on the intensity of radioautographic labeling are presented in terms of mean grain count per cell in cells labeled with tritiated precursors of proteins or nucleic acids. This information would be of interest to medical researchers and cytologists.

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

PubMed Central

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

1988-01-01

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

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

PubMed

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

2017-12-01

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

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

PubMed

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

2016-09-01

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

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

PubMed

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

2008-01-01

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

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

PubMed

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

2011-07-01

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

Hyaluronic Acid Improves Bone Formation in Extraction Sockets With Chronic Pathology: A Pilot Study in Dogs.

PubMed

Kim, Jung-Ju; Song, Hyun Young; Ben Amara, Heithem; Kyung-Rim, Kang; Koo, Ki-Tae

2016-07-01

Previous studies on ridge preservation focusing on fresh extraction sockets using graft materials for ridge preservation procedures have reported a delay in the tissue modeling and remodeling phases. The objective of this study is to evaluate the effect of hyaluronic acid (HA) on healing of infected sockets. Six beagle dogs were used in this study. Both mandibular third premolars were hemisected, and the distal roots were extracted. Subsequently, periodontal and endodontic lesions were induced at the remaining mesial root. After communication of the periodontal lesion, an endodontic periapical lesion was observed at 4 months, and the mesial roots of both the right and left sides were extracted. HA was applied into the socket of the test group, and no treatment was administered to the other group (control group). Three months after extraction of the mesial roots, the dogs were sacrificed, and histologic evaluations were performed. The sockets were filled by mineralized bone (47.80% ± 6.60%) and bone marrow (50.47% ± 6.38%) in the control group, whereas corresponding values were 63.29% ± 9.78% and 34.73% ± 8.97% for the test group, respectively. There was a statistically significant difference between the groups. Reversal lines and a copious lineup of osteoblasts were observed in the middle and apical parts of the sockets in the test group. An infected socket shows delayed healing of the socket wound, and HA, because of its osteoinductive, bacteriostatic, and anti-inflammatory properties, may improve bone formation and accelerate wound healing in infected sockets.

Determination of Acid Herbicides Using Modified QuEChERS with Fast Switching ESI(+)/ESI(-) LC-MS/MS.

PubMed

Sack, Chris; Vonderbrink, John; Smoker, Michael; Smith, Robert E

2015-11-04

A method for the determination of 35 acid herbicides in food matrices was developed, validated, and implemented. It utilizes a modified QuEChERS extraction procedure coupled with quantitation by liquid chromatography tandem mass spectrometry (LC-MS/MS). The acid herbicides analyzed are all organic carboxylic acids, including the older chlorophenoxy acid herbicides such as 2,4-dichlorophenoxyacetic acid (2,4-D), dicamba, 4-chlorophenoxyacetic acid (4-CPA), quinclorac, and many of the newer imidazolinone herbicides such as imazethapyr and imazaquin. In the procedure, 10 mL of water is added to 5 g of sample and then extracted with 1% formic acid in acetonitrile for 1 min. The acetonitrile phase is salted out of the extract by adding sodium chloride and magnesium sulfate, followed by centrifugation. The acetonitrile is diluted 1:1 with water to enable quantitation by LC-MS/MS using fast switching between positive and negative electrospray ionization modes. The average recoveries for all the compounds except aminocyclopyrachlor were 95% with a precision of 8%. The method detection limits for all residues were less than 10 ng/g, and the correlation coefficients for the calibration curves was greater than 0.99 for all but two compounds tested. The method was used successfully for the quantitation of acid herbicides in the FDA's total diet study. The procedure proved to be accurate, precise, linear, sensitive, and rugged.

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

PubMed

Bassel, B A; Curry, M E

1973-11-01

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

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

PubMed

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

2014-11-01

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

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

PubMed

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

2014-12-01

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

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

PubMed

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

2009-08-01

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

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

PubMed

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

2013-11-20

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

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

PubMed

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

1997-11-01

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

Acid extraction by supported liquid membranes containing basic carriers

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

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

1983-01-01

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

Evaluation of an alternative extraction procedure for enterotoxin determination in dairy products.

PubMed

Meyrand, A; Atrache, V; Bavai, C; Montet, M P; Vernozy-Rozand, C

1999-06-01

A concentration protocol based on trichloroacetic acid precipitation was evaluated and compared with the reference method using dialysis concentration. Different quantities of purified staphylococcal enterotoxins were added to pasteurized Camembert-type cheeses. Detection of enterotoxins in these cheeses was performed using an automated detection system. Raw goat milk Camembert-type cheeses involved in a staphylococcal food poisoning were also tested. Both enterotoxin extraction methods allowed detection of the lowest enterotoxin concentration level used in this study (0.5 ng g-1). Compared with the dialysis concentration method, TCA precipitation of staphylococcal enterotoxins was 'user-friendly' and less time-consuming. These results suggest that TCA precipitation is a rapid (1 h), simple and reliable method of extracting enterotoxin from food which gives excellent recovery from dairy products.

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.

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

PubMed

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

2008-05-01

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

A comparison of recovery of virus from wastewaters by beef extract-Celite, ferric chloride, and filter concentration procedures.

PubMed

Dahling, D R; Wright, B A

1988-12-01

An improved concentration method using sample volumes as large as 1500 ml has been developed to monitor for viruses in wastewaters. Non-precipitating dry beef extract powder is added to wastewater samples to give a 3% concentration and mixed until dissolved. This is followed by the addition of Celite as a virus adsorbent. By manipulating pH, viruses are eluted from the Celite in small volumes of phosphate buffer. This procedure was further tested without the aid of the Celite additives using a precipitating beef extract powder and substituting FeCl3 as an alternate reagent for the Celite. Comparison testing was also made with the currently recommended cartridge and disc filter procedures. In all cases, the non-precipitating beef extract-Celite method gave higher recovery rates in highly polluted waters.

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

USDA-ARS?s Scientific Manuscript database

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

Calcium extraction from brine water and seawater using oxalic acid

NASA Astrophysics Data System (ADS)

Natasha, Nadia Chrisayu; Lalasari, Latifa Hanum

2017-01-01

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

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

PubMed

Mubarak, Zaki; Soraya, Cut

2018-01-01

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

Ancient DNA in historical parchments - identifying a procedure for extraction and amplification of genetic material.

PubMed

Lech, T

2016-05-06

Historical parchments in the form of documents, manuscripts, books, or letters, make up a large portion of cultural heritage collections. Their priceless historical value is associated with not only their content, but also the information hidden in the DNA deposited on them. Analyses of ancient DNA (aDNA) retrieved from parchments can be used in various investigations, including, but not limited to, studying their authentication, tracing the development of the culture, diplomacy, and technology, as well as obtaining information on the usage and domestication of animals. This article proposes and verifies a procedure for aDNA recovery from historical parchments and its appropriate preparation for further analyses. This study involved experimental selection of an aDNA extraction method with the highest efficiency and quality of extracted genetic material, from among the multi-stage phenol-chloroform extraction methods, and the modern, column-based techniques that use selective DNA-binding membranes. Moreover, current techniques to amplify entire genetic material were questioned, and the possibility of using mitochondrial DNA for species identification was analyzed. The usefulness of the proposed procedure was successfully confirmed in identification tests of historical parchments dating back to the 13-16th century AD.

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

PubMed

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

2012-12-01

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

Assessment of a geochemical extraction procedure to determine the solid phase fractionation and bioaccessibility of potentially harmful elements in soils: a case study using the NIST 2710 reference soil.