The extraction of essential oil from patchouli leaves (Pogostemon cablin Benth) using microwave hydrodistillation and solvent-free microwave extraction methods

NASA Astrophysics Data System (ADS)

Putri, D. K. Y.; Kusuma, H. S.; Syahputra, M. E.; Parasandi, D.; Mahfud, M.

2017-12-01

Patchouli plant (Pogostemon cablin Benth) is one of the important essential oil-producing plant, contributes more than 50% of total exports of Indonesia’s essential oil. However, the extraction of patchouli oil that has been done in Indonesia is generally still used conventional methods that require enormous amount of energy, high solvent usage, and long time of extraction. Therefore, in this study, patchouli oil extraction was carried out by using microwave hydrodistillation and solvent-free microwave extraction methods. Based on this research, it is known that the extraction of patchouli oil using microwave hydrodistillation method with longer extraction time (240 min) only produced patchouli oil’s yield 1.2 times greater than solvent-free microwave extraction method which require faster extraction time (120 min). Otherwise the analysis of electric consumption and the environmental impact, the solvent-free microwave extraction method showed a smaller amount when compared with microwave hydrodistillation method. It is conclude that the use of solvent-free microwave extraction method for patchouli oil extraction is suitably method as a new green technique.

Ultrahigh pressure extraction of bioactive compounds from plants-A review.

PubMed

Xi, Jun

2017-04-13

Extraction of bioactive compounds from plants is one of the most important research areas for pharmaceutical and food industries. Conventional extraction techniques are usually associated with longer extraction times, lower yields, more organic solvent consumption, and poor extraction efficiency. A novel extraction technique, ultrahigh pressure extraction, has been developed for the extraction of bioactive compounds from plants, in order to shorten the extraction time, decrease the solvent consumption, increase the extraction yields, and enhance the quality of extracts. The mild processing temperature of ultrahigh pressure extraction may lead to an enhanced extraction of thermolabile bioactive ingredients. A critical review is conducted to introduce the different aspects of ultrahigh pressure extraction of plants bioactive compounds, including principles and mechanisms, the important parameters influencing its performance, comparison of ultrahigh pressure extraction with other extraction techniques, advantages, and disadvantages. The future opportunities of ultrahigh pressure extraction are also discussed.

EVALUATION OF ANALYTICAL METHODS FOR DETERMINING PESTICIDES IN BABY FOOD

EPA Science Inventory

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

RESOURCES CONSERVATIONS COMPANY - B.E.S.T. SOLVENT EXTRACTION TECHNOLOGY - APPLICATIONS ANALYSIS REPORT

EPA Science Inventory

This document is an evaluation of the performance of the Resources Conservation Company (RCC) Basic Extractive Sludge Treatment (B.E.S.T.®) solvent extraction technology and its applicability as a treatment technique for soils, sediments, and sludges contaminated with organics. B...

Microwave-assisted extraction of total bioactive saponin fraction from Gymnema sylvestre with reference to gymnemagenin: a potential biomarker.

PubMed

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

2009-01-01

To develop a fast and ecofriendly microwave assisted extraction (MAE) technique for the effective and exhaustive extraction of gymnemagenin as an indicative biomarker for the quality control of Gymnema sylvestre. Several extraction parameters such as microwave power, extraction time, solvent composition, pre-leaching time, loading ratio and extraction cycle were studied for the determination of the optimum extraction condition. Scanning electron micrographs were obtained to elucidate the mechanism of extraction. The final optimum extraction conditions as obtained from the study were: 40% microwave power, 6 min irradiation time, 85% v/v methanol as the extraction solvent, 15 min pre-leaching time and 25 : 1 (mL/g) as the solvent-to-material loading ratio. The proposed extraction technique produced a maximum yield of 4.3% w/w gymnemagenin in 6 min which was 1.3, 2.5 and 1.95 times more efficient than 6 h of heat reflux, 24 h of maceration and stirring extraction, respectively. A synergistic heat and mass transfer theory was also proposed to support the extraction mechanism. Comparison with conventional extraction methods revealed that MAE could save considerable amounts of time and energy, whilst the reduction of volume of organic solvent consumed provides an ecofriendly feature.

Conventional and accelerated-solvent extractions of green tea (camellia sinensis) for metabolomics-based chemometrics.

PubMed

Kellogg, Joshua J; Wallace, Emily D; Graf, Tyler N; Oberlies, Nicholas H; Cech, Nadja B

2017-10-25

Metabolomics has emerged as an important analytical technique for multiple applications. The value of information obtained from metabolomics analysis depends on the degree to which the entire metabolome is present and the reliability of sample treatment to ensure reproducibility across the study. The purpose of this study was to compare methods of preparing complex botanical extract samples prior to metabolomics profiling. Two extraction methodologies, accelerated solvent extraction and a conventional solvent maceration, were compared using commercial green tea [Camellia sinensis (L.) Kuntze (Theaceae)] products as a test case. The accelerated solvent protocol was first evaluated to ascertain critical factors influencing extraction using a D-optimal experimental design study. The accelerated solvent and conventional extraction methods yielded similar metabolite profiles for the green tea samples studied. The accelerated solvent extraction yielded higher total amounts of extracted catechins, was more reproducible, and required less active bench time to prepare the samples. This study demonstrates the effectiveness of accelerated solvent as an efficient methodology for metabolomics studies. Copyright © 2017. Published by Elsevier B.V.

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

PubMed

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

2016-06-01

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

Comparison on extraction yield of sennoside A and sennoside B from senna (Cassia angustifolia) using conventional and non conventional extraction techniques and their quantification using a validated HPLC-PDA detection method.

PubMed

Dhanani, Tushar; Singh, Raghuraj; Reddy, Nagaraja; Trivedi, A; Kumar, Satyanshu

2017-05-01

Senna is an important medicinal plant and is used in many Ayurvedic formulations. Dianthraquinone glucosides are the main bioactive phytochemicals present in leaves and pods of senna. The extraction efficiency in terms of yield and composition of the extract of senna prepared using both conventional (cold percolation at room temperature and refluxing) and non conventional (ultrasound and microwave assisted solvent extraction as well as supercritical fluid extraction) techniques were compared in the present study. Also a rapid reverse phase HPLC-PDA detection method was developed and validated for the simultaneous determination of sennoside A and sennoside B in the different extracts of senna leaves. Ultrasound and microwave assisted solvent extraction techniques were more effective in terms of yield and composition of the extracts compared to cold percolation at room temperature and refluxing methods of extraction.

Comparison of microwave hydrodistillation and solvent-free microwave extraction of essential oil from Melaleuca leucadendra Linn

NASA Astrophysics Data System (ADS)

Ismanto, A. W.; Kusuma, H. S.; Mahfud, M.

2017-12-01

The comparison of solvent-free microwave extraction (SFME) and microwave hydrodistillation (MHD) in the extraction of essential oil from Melaleuca leucadendra Linn. was examined. Dry cajuput leaves were used in this study. The purpose of this study is also to determine optimal condition (microwave power). The relative electric consumption of SFME and MHD methods are both showing 0,1627 kWh/g and 0,3279 kWh/g. The results showed that solvent-free microwave extraction methods able to reduce energy consumption and can be regarded as a green technique for extraction of cajuput oil.

Green bio-oil extraction for oil crops

NASA Astrophysics Data System (ADS)

Zainab, H.; Nurfatirah, N.; Norfaezah, A.; Othman, H.

2016-06-01

The move towards a green bio-oil extraction technique is highlighted in this paper. The commonly practised organic solvent oil extraction technique could be replaced with a modified microwave extraction. Jatropha seeds (Jatropha curcas) were used to extract bio-oil. Clean samples were heated in an oven at 110 ° C for 24 hours to remove moisture content and ground to obtain particle size smaller than 500μm. Extraction was carried out at different extraction times 15 min, 30 min, 45 min, 60 min and 120 min to determine oil yield. The biooil yield obtained from microwave assisted extraction system at 90 minutes was 36% while that from soxhlet extraction for 6 hours was 42%. Bio-oil extracted using the microwave assisted extraction (MAE) system could enhance yield of bio-oil compared to soxhlet extraction. The MAE extraction system is rapid using only water as solvent which is a nonhazardous, environment-friendly technique compared to soxhlet extraction (SE) method using hexane as solvent. Thus, this is a green technique of bio-oil extraction using only water as extractant. Bio-oil extraction from the pyrolysis of empty fruit bunch (EFB), a biomass waste from oil palm crop, was enhanced using a biocatalyst derived from seashell waste. Oil yield for non-catalytic extraction was 43.8% while addition of seashell based biocatalyst was 44.6%. Oil yield for non-catalytic extraction was 43.8% while with addition of seashell-based biocatalyst was 44.6%. The pH of bio-oil increased from 3.5 to 4.3. The viscosity of bio-oil obtained by catalytic means increased from 20.5 to 37.8 cP. A rapid and environment friendly extraction technique is preferable to enhance bio-oil yield. The microwave assisted approach is a green, rapid and environmental friendly extraction technique for the production of bio-oil bearing crops.

In-tube electro-membrane extraction with a sub-microliter organic solvent consumption as an efficient technique for synthetic food dyes determination in foodstuff samples.

PubMed

Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Asghari, Alireza; Abdossalami asl, Yousef

2015-09-04

A simple and efficient extraction technique with a sub-microliter organic solvent consumption termed as in-tube electro-membrane extraction (IEME) is introduced. This method is based upon the electro-kinetic migration of ionized compounds by the application of an electrical potential difference. For this purpose, a thin polypropylene (PP) sheet placed inside a tube acts as a support for the membrane solvent, and 30μL of an aqueous acceptor solution is separated by this solvent from 1.2mL of an aqueous donor solution. This method yielded high extraction recoveries (63-81%), and the consumption of the organic solvent used was only 0.5μL. By performing this method, the purification is high, and the utilization of the organic solvent, used as a mediator, is very simple and repeatable. The proposed method was evaluated by extraction of four synthetic food dyes (Amaranth, Ponceau 4R, Allura Red, and Carmoisine) as the model analytes. Optimization of variables affecting the method was carried out in order to achieve the best extraction efficiency. These variables were the type of membrane solvent, applied extraction voltage, extraction time, pH range, and concentration of salt added. Under the optimized conditions, IEME-HPLC-UV provided a good linearity in the range of 1.00-800ngmL(-1), low limits of detection (0.3-1ngmL(-1)), and good extraction repeatabilities (RSDs below 5.2%, n=5). It seems that this design is a proper one for the automation of the method. Also the consumption of the organic solvent in a sub-microliter scale, and its simplicity, high efficiency, and high purification can help one getting closer to the objectives of the green chemistry. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

USGS Publications Warehouse

Steinheimer, T.R.; Brooks, M.G.

1984-01-01

A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth.

PubMed

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-09-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%).

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth#

PubMed Central

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-01-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%). PMID:27604860

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

PubMed

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

2017-03-29

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

Chemical composition and antibacterial activity of Cordia verbenacea extracts obtained by different methods.

PubMed

Michielin, Eliane M Z; Salvador, Ana A; Riehl, Carlos A S; Smânia, Artur; Smânia, Elza F A; Ferreira, Sandra R S

2009-12-01

The present study describes the chemical composition and the antibacterial activity of extracts from Cordia verbenacea DC (Borraginaceae), a traditional medicinal plant that grows widely along the southeastern coast of Brazil. The extracts were obtained using different extraction techniques: high-pressure operations and low-pressure methods. The high-pressure technique was applied to obtain C. verbenacea extracts using pure CO(2) and CO(2) with co-solvent at pressures up to 30MPa and temperatures of 30, 40 and 50 degrees C. Organic solvents such as n-hexane, ethyl acetate, ethanol, acetone and dichloromethane were used to obtain extracts by low-pressure processes. The antibacterial activity of the extracts was also subjected to screening against four strains of bacteria using the agar dilution method. The extraction yields were up to 5.0% w/w and up to 8.6% w/w for supercritical fluid extraction with pure CO(2) and with ethyl acetate as co-solvent, respectively, while the low-pressure extraction indicates yields up to 24.0% w/w in the soxhlet extraction using water and aqueous mixture with 50% ethanol as solvents. The inhibitory activity of the extracts in gram-positive bacteria was significantly higher than in gram-negative. The quantification and the identification of the extracts recovered were accomplished using GC/MS analysis. The most important components identified in the extract were artemetin, beta-sitosterol, alpha-humulene and beta-caryophyllene, among others.

An effective vacuum assisted extraction method for the optimization of labdane diterpenoids from Andrographis paniculata by response surface methodology.

PubMed

Wang, Ya-Qi; Wu, Zhen-Feng; Ke, Gang; Yang, Ming

2014-12-31

An effective vacuum assisted extraction (VAE) technique was proposed for the first time and applied to extract bioactive components from Andrographis paniculata. The process was carefully optimized by response surface methodology (RSM). Under the optimized experimental conditions, the best results were obtained using a boiling temperature of 65 °C, 50% ethanol concentration, 16 min of extraction time, one extraction cycles and a 12:1 liquid-solid ratio. Compared with conventional ultrasonic assisted extraction and heat reflux extraction, the VAE technique gave shorter extraction times and remarkable higher extraction efficiency, which indicated that a certain degree of vacuum gave the solvent a better penetration of the solvent into the pores and between the matrix particles, and enhanced the process of mass transfer. The present results demonstrated that VAE is an efficient, simple and fast method for extracting bioactive components from A. paniculata, which shows great potential for becoming an alternative technique for industrial scale-up applications.

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

PubMed

Regel-Rosocka, Magdalena

2010-05-15

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

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

EPA Science Inventory

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

Review of online coupling of sample preparation techniques with liquid chromatography.

PubMed

Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

2014-03-07

Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

A high-throughput platform for low-volume high-temperature/pressure sealed vessel solvent extractions.

PubMed

Damm, Markus; Kappe, C Oliver

2011-11-30

A high-throughput platform for performing parallel solvent extractions in sealed HPLC/GC vials inside a microwave reactor is described. The system consist of a strongly microwave-absorbing silicon carbide plate with 20 cylindrical wells of appropriate dimensions to be fitted with standard HPLC/GC autosampler vials serving as extraction vessels. Due to the possibility of heating up to four heating platforms simultaneously (80 vials), efficient parallel analytical-scale solvent extractions can be performed using volumes of 0.5-1.5 mL at a maximum temperature/pressure limit of 200°C/20 bar. Since the extraction and subsequent analysis by either gas chromatography or liquid chromatography coupled with mass detection (GC-MS or LC-MS) is performed directly from the autosampler vial, errors caused by sample transfer can be minimized. The platform was evaluated for the extraction and quantification of caffeine from commercial coffee powders assessing different solvent types, extraction temperatures and times. For example, 141±11 μg caffeine (5 mg coffee powder) were extracted during a single extraction cycle using methanol as extraction solvent, whereas only 90±11 were obtained performing the extraction in methylene chloride, applying the same reaction conditions (90°C, 10 min). In multiple extraction experiments a total of ~150 μg caffeine was extracted from 5 mg commercial coffee powder. In addition to the quantitative caffeine determination, a comparative qualitative analysis of the liquid phase coffee extracts and the headspace volatiles was performed, placing special emphasis on headspace analysis using solid-phase microextraction (SPME) techniques. The miniaturized parallel extraction technique introduced herein allows solvent extractions to be performed at significantly expanded temperature/pressure limits and shortened extraction times, using standard HPLC autosampler vials as reaction vessels. Remarkable differences regarding peak pattern and main peaks were observed when low-temperature extraction (60°C) and high-temperature extraction (160°C) are compared prior to headspace-SPME-GC-MS performed in the same HPLC/GC vials. Copyright © 2011 Elsevier B.V. All rights reserved.

Design of experiment approach for the process optimisation of microwave assisted extraction of lupeol from Ficus racemosa leaves using response surface methodology.

PubMed

Das, Anup Kumar; Mandal, Vivekananda; Mandal, Subhash C

2013-01-01

Triterpenoids are a group of important phytocomponents from Ficus racemosa (syn. Ficus glomerata Roxb.) that are known to possess diverse pharmacological activities and which have prompted the development of various extraction techniques and strategies for its better utilisation. To develop an effective, rapid and ecofriendly microwave-assisted extraction (MAE) strategy to optimise the extraction of a potent bioactive triterpenoid compound, lupeol, from young leaves of Ficus racemosa using response surface methodology (RSM) for industrial scale-up. Initially a Plackett-Burman design matrix was applied to identify the most significant extraction variables amongst microwave power, irradiation time, particle size, solvent:sample ratio loading, varying solvent strength and pre-leaching time on lupeol extraction. Among the six variables tested, microwave power, irradiation time and solvent-sample/loading ratio were found to have a significant effect (P < 0.05) on lupeol extraction and were fitted to a Box-Behnken-design-generated quadratic polynomial equation to predict optimal extraction conditions as well as to locate operability regions with maximum yield. The optimal conditions were microwave power of 65.67% of 700 W, extraction time of 4.27 min and solvent-sample ratio loading of 21.33 mL/g. Confirmation trials under the optimal conditions gave an experimental yield (18.52 µg/g of dry leaves) close to the RSM predicted value of 18.71 µg/g. Under the optimal conditions the mathematical model was found to be well fitted with the experimental data. The MAE was found to be a more rapid, convenient and appropriate extraction method, with a higher yield and lower solvent consumption when compared with conventional extraction techniques. Copyright © 2012 John Wiley & Sons, Ltd.

Evaluation of extraction protocols for anti-diabetic phytochemical substances from medicinal plants.

PubMed

Okoduwa, Stanley Irobekhian Reuben; Umar, Ismaila A; James, Dorcas B; Inuwa, Hajara M; Habila, James D

2016-12-15

To examine the efficacy of three extraction techniques: Soxhlet-extraction (SE), cold-maceration (CM) and microwave-assisted-extraction (MAE) using 80% methanol as solvent. The study was performed on each of 50 g of Vernonia amygdalina (VA) and Occimum gratissimum (OG) leaves respectively. The percentage yield, duration of extraction, volume of solvent used, qualitative and quantitative phytoconstituents present was compared. The biological activities (hypoglycemic effect) were investigated using albino wistar rat model of diabetes mellitus ( n = 36) with a combined dose (1:1) of the two plants leaf extracts (250 mg/kg b.w.) from the three methods. The extracts were administered orally, once daily for 21 d. In this report, the percentage VA extract yield from MAE was highest (20.9% ± 1.05%) within 39 min using 250 mL of solvent, when compared to the CM (14.35% ± 0.28%) within 4320 min using 900 mL of solvent and SE (15.75% ± 0.71%) within 265 min using 500 mL of solvent. The percentage differences in OG extract yield between: MAE vs SE was 41.05%; MAE vs CM was 46.81% and SE vs CM was 9.77%. The qualitative chemical analysis of the two plants showed no difference in the various phytoconstituents tested, but differs quantitatively in the amount of the individual phytoconstituents, as MAE had significantly high yield ( P > 0.05) on phenolics, saponins and tannins. SE technique gave significantly high yield ( P > 0.05) on alkaloid, while CM gave significant high yield on flavonoids. The extracts from CM exhibited a significantly ( P > 0.05) better hypoglycemic activity within the first 14-d of treatment (43.3% ± 3.62%) when compared to MAE (36.5% ± 0.08%) and SE methods (33.3% ± 1.60%). However, the percentage hypoglycemic activity, 21 d post-treatment with 250 mg/kg b.w. extract from MAE was 72.6% ± 1.03% and it was more comparable to 10 mg/kg b.w. glibenclamide treated group (75.0% ± 0.73%), unlike the SE (69.5% ± 0.71%) and CM (69.1% ± 1.03%). CM technique produces extract with better hypoglycemic activity, whereas; MAE is a better option for high yield of phytoconstituents using less solvent within a short time.

Evaluation of extraction protocols for anti-diabetic phytochemical substances from medicinal plants

PubMed Central

Okoduwa, Stanley Irobekhian Reuben; Umar, Ismaila A; James, Dorcas B; Inuwa, Hajara M; Habila, James D

2016-01-01

AIM To examine the efficacy of three extraction techniques: Soxhlet-extraction (SE), cold-maceration (CM) and microwave-assisted-extraction (MAE) using 80% methanol as solvent. METHODS The study was performed on each of 50 g of Vernonia amygdalina (VA) and Occimum gratissimum (OG) leaves respectively. The percentage yield, duration of extraction, volume of solvent used, qualitative and quantitative phytoconstituents present was compared. The biological activities (hypoglycemic effect) were investigated using albino wistar rat model of diabetes mellitus (n = 36) with a combined dose (1:1) of the two plants leaf extracts (250 mg/kg b.w.) from the three methods. The extracts were administered orally, once daily for 21 d. RESULTS In this report, the percentage VA extract yield from MAE was highest (20.9% ± 1.05%) within 39 min using 250 mL of solvent, when compared to the CM (14.35% ± 0.28%) within 4320 min using 900 mL of solvent and SE (15.75% ± 0.71%) within 265 min using 500 mL of solvent. The percentage differences in OG extract yield between: MAE vs SE was 41.05%; MAE vs CM was 46.81% and SE vs CM was 9.77%. The qualitative chemical analysis of the two plants showed no difference in the various phytoconstituents tested, but differs quantitatively in the amount of the individual phytoconstituents, as MAE had significantly high yield (P > 0.05) on phenolics, saponins and tannins. SE technique gave significantly high yield (P > 0.05) on alkaloid, while CM gave significant high yield on flavonoids. The extracts from CM exhibited a significantly (P > 0.05) better hypoglycemic activity within the first 14-d of treatment (43.3% ± 3.62%) when compared to MAE (36.5% ± 0.08%) and SE methods (33.3% ± 1.60%). However, the percentage hypoglycemic activity, 21 d post-treatment with 250 mg/kg b.w. extract from MAE was 72.6% ± 1.03% and it was more comparable to 10 mg/kg b.w. glibenclamide treated group (75.0% ± 0.73%), unlike the SE (69.5% ± 0.71%) and CM (69.1% ± 1.03%). CONCLUSION CM technique produces extract with better hypoglycemic activity, whereas; MAE is a better option for high yield of phytoconstituents using less solvent within a short time. PMID:28031778

Solvent-free microwave extraction of essential oil from aromatic herbs: from laboratory to pilot and industrial scale.

PubMed

Filly, Aurore; Fernandez, Xavier; Minuti, Matteo; Visinoni, Francesco; Cravotto, Giancarlo; Chemat, Farid

2014-05-01

Solvent-free microwave extraction (SFME) has been proposed as a green method for the extraction of essential oil from aromatic herbs that are extensively used in the food industry. This technique is a combination of microwave heating and dry distillation performed at atmospheric pressure without any added solvent or water. The isolation and concentration of volatile compounds is performed in a single stage. In this work, SFME and a conventional technique, hydro-distillation HD (Clevenger apparatus), are used for the extraction of essential oil from rosemary (Rosmarinus officinalis L.) and are compared. This preliminary laboratory study shows that essential oils extracted by SFME in 30min were quantitatively (yield and kinetics profile) and qualitatively (aromatic profile) similar to those obtained using conventional hydro-distillation in 2h. Experiments performed in a 75L pilot microwave reactor prove the feasibility of SFME up scaling and potential industrial applications. Copyright © 2013 Elsevier Ltd. All rights reserved.

Ionic liquid solutions as extractive solvents for value-added compounds from biomass

PubMed Central

Passos, Helena; Freire, Mara G.; Coutinho, João A. P.

2014-01-01

In the past few years, the number of studies regarding the application of ionic liquids (ILs) as alternative solvents to extract value-added compounds from biomass has been growing. Based on an extended compilation and analysis of the data hitherto reported, the main objective of this review is to provide an overview on the use of ILs and their mixtures with molecular solvents for the extraction of value-added compounds present in natural sources. The ILs (or IL solutions) investigated as solvents for the extraction of natural compounds, such as alkaloids, flavonoids, terpenoids, lipids, among others, are outlined. The extraction techniques employed, namely solid–liquid extraction, and microwave-assisted and ultrasound-assisted extractions, are emphasized and discussed in terms of extraction yields and purification factors. Furthermore, the evaluation of the IL chemical structure and the optimization of the process conditions (IL concentration, temperature, biomass–solvent ratio, etc.) are critically addressed. Major conclusions on the role of the ILs towards the extraction mechanisms and improved extraction yields are additionally provided. The isolation and recovery procedures of the value-added compounds are ascertained as well as some scattered strategies already reported for the IL solvent recovery and reusability. Finally, a critical analysis on the economic impact versus the extraction performance of IL-based methodologies was also carried out and is here presented and discussed. PMID:25516718

Ionic liquid solutions as extractive solvents for value-added compounds from biomass.

PubMed

Passos, Helena; Freire, Mara G; Coutinho, João A P

2014-12-01

In the past few years, the number of studies regarding the application of ionic liquids (ILs) as alternative solvents to extract value-added compounds from biomass has been growing. Based on an extended compilation and analysis of the data hitherto reported, the main objective of this review is to provide an overview on the use of ILs and their mixtures with molecular solvents for the extraction of value-added compounds present in natural sources. The ILs (or IL solutions) investigated as solvents for the extraction of natural compounds, such as alkaloids, flavonoids, terpenoids, lipids, among others, are outlined. The extraction techniques employed, namely solid-liquid extraction, and microwave-assisted and ultrasound-assisted extractions, are emphasized and discussed in terms of extraction yields and purification factors. Furthermore, the evaluation of the IL chemical structure and the optimization of the process conditions (IL concentration, temperature, biomass-solvent ratio, etc.) are critically addressed. Major conclusions on the role of the ILs towards the extraction mechanisms and improved extraction yields are additionally provided. The isolation and recovery procedures of the value-added compounds are ascertained as well as some scattered strategies already reported for the IL solvent recovery and reusability. Finally, a critical analysis on the economic impact versus the extraction performance of IL-based methodologies was also carried out and is here presented and discussed.

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

PubMed

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

2016-10-01

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

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

PubMed Central

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

2016-01-01

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

Solvent extraction of gold using ionic liquid based process

NASA Astrophysics Data System (ADS)

Makertihartha, I. G. B. N.; Zunita, Megawati; Rizki, Z.; Dharmawijaya, P. T.

2017-01-01

In decades, many research and mineral processing industries are using solvent extraction technology for metal ions separation. Solvent extraction technique has been used for the purification of precious metals such as Au and Pd, and base metals such as Cu, Zn and Cd. This process uses organic compounds as solvent. Organic solvents have some undesired properties i.e. toxic, volatile, excessive used, flammable, difficult to recycle, low reusability, low Au recovery, together with the problems related to the disposal of spent extractants and diluents, even the costs associated with these processes are relatively expensive. Therefore, a lot of research have boosted into the development of safe and environmentally friendly process for Au separation. Ionic liquids (ILs) are the potential alternative for gold extraction because they possess several desirable properties, such as a the ability to expanse temperature process up to 300°C, good solvent properties for a wide range of metal ions, high selectivity, low vapor pressures, stability up to 200°C, easy preparation, environmentally friendly (commonly called as "green solvent"), and relatively low cost. This review paper is focused in investigate of some ILs that have the potentials as solvent in extraction of Au from mineral/metal alloy at various conditions (pH, temperature, and pressure). Performances of ILs extraction of Au are studied in depth, i.e. structural relationship of ILs with capability to separate Au from metal ions aggregate. Optimal extraction conditon in order to gain high percent of Au in mineral processing is also investigated.

Comparisons between conventional, ultrasound-assisted and microwave-assisted methods for extraction of anthraquinones from Heterophyllaea pustulata Hook f. (Rubiaceae).

PubMed

Barrera Vázquez, M F; Comini, L R; Martini, R E; Núñez Montoya, S C; Bottini, S; Cabrera, J L

2014-03-01

This work reports a comparative study about extraction methods used to obtain anthraquinones (AQs) from stems and leaves of Heterophyllae pustulata Hook (Rubiáceae). One of the conventional procedures used to extract these metabolites from a vegetable matrix is by successive Soxhlet extractions with solvents of increasing polarity: starting with hexane to eliminate chlorophylls and fatty components, following by benzene and finally ethyl acetate. However, this technique shows a low extraction yield of total AQs, and consumes large quantities of solvent and time. Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) have been investigated as alternative methods to extract these compounds, using the same sequence of solvents. It was found that UAE increases the extraction yield of total AQs and reduces the time and amount of solvent used. Nevertheless, the combination UAE with benzene, plus MAE with ethyl acetate at a constant power of 900 W showed the best results. A higher yield of total AQs was obtained in less time and using the same amount of solvent that UAE. The optimal conditions for this latter procedure were UAE with benzene at 50 °C during 60 min, followed by MAE at 900 W during 15 min using ethyl acetate as extraction solvent. Copyright © 2013 Elsevier B.V. All rights reserved.

Using GC-FID to Quantify the Removal of 4-sec-Butylphenol from NGS Solvent by NaOH

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

Sloop, Jr., Frederick V.; Moyer, Bruce A.

2014-12-01

A caustic wash of the solvent used in the Next-Generation Caustic-Side Solvent Extraction (NG-CSSX) process was found to remove the modifier breakdown product 4-sec-butylphenol (SBP) with varying efficiency depending on the aqueous NaOH concentration. Recent efforts at ORNL have aimed at characterizing the flowsheet chemistry and reducing the technical uncertainties of the NG-CSSX process. One technical uncertainty has been the efficacy of caustic washing of the solvent for the removal of lipophilic anions, in particular, the efficient removal of SBP, an important degradation product of the solvent modifier, Cs-7SB. In order to make this determination, it was necessary to developmore » a sensitive and reliable analytical technique for the detection and quantitation of SBP. This report recounts the development of a GC-FID-based (Gas Chromatography Flame Ionization Detection) technique for analyzing SBP and the utilization of the technique to subsequently confirm the ability of the caustic wash to efficiently remove SBP from the Next Generation Solvent (NGS) used in NG-CSSX. In particular, the developed technique was used to monitor the amount of SBP removed from a simple solvent and the full NGS by contact with sodium hydroxide wash solutions over a range of concentrations. The results show that caustic washing removes SBP with effectively the same efficiency as it did in the original Caustic-Side Solvent Extraction (CSSX) process.« less

Dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by high-performance liquid chromatography with ultraviolet detection and liquid chromatography-tandem mass spectrometry for the determination of triclosan and 2,4-dichlorophenol in water samples.

PubMed

Zheng, Cao; Zhao, Jing; Bao, Peng; Gao, Jin; He, Jin

2011-06-24

A novel, simple and efficient dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) technique coupled with high-performance liquid chromatography with ultraviolet detection (HPLC-UV) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of triclosan and its degradation product 2,4-dichlorophenol in real water samples. The extraction solvent used in this work is of low density, low volatility, low toxicity and proper melting point around room temperature. The extractant droplets can be collected easily by solidifying it at a lower temperature. Parameters that affect the extraction efficiency, including type and volume of extraction solvent and dispersive solvent, salt effect, pH and extraction time, were investigated and optimized in a 5 mL sample system by HPLC-UV. Under the optimum conditions (extraction solvent: 12 μL of 1-dodecanol; dispersive solvent: 300 of μL acetonitrile; sample pH: 6.0; extraction time: 1 min), the limits of detection (LODs) of the pretreatment method combined with LC-MS/MS were in the range of 0.002-0.02 μg L(-1) which are lower than or comparable with other reported approaches applied to the determination of the same compounds. Wide linearities, good precisions and satisfactory relative recoveries were also obtained. The proposed technique was successfully applied to determine triclosan and 2,4-dichlorophenol in real water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Comparison of microwave, ultrasound and accelerated-assisted solvent extraction for recovery of polyphenols from Citrus sinensis peels.

PubMed

Nayak, Balunkeswar; Dahmoune, Farid; Moussi, Kamal; Remini, Hocine; Dairi, Sofiane; Aoun, Omar; Khodir, Madani

2015-11-15

Peel of Citrus sinensis contains significant amounts of bioactive polyphenols that could be used as ingredients for a number of value-added products with health benefits. Extraction of polyphenols from the peels was performed using a microwave-assisted extraction (MAE) technique. The effects of aqueous acetone concentration, microwave power, extraction time and solvent-to-solid ratio on the total phenolic content (TPC), total antioxidant activity (TAA) (using DPPH and ORAC-values) and individual phenolic acids (IPA) were investigated using a response surface method. The TPC, TAA and IPA of peel extracts using MAE was compared with conventional, ultrasound-assisted and accelerated solvent extraction. The maximum predicted TPC under the optimal MAE conditions (51% acetone concentration in water (v/v), 500 W microwave power, 122 s extraction time and 25 mL g(-1) solvent to solid ratio), was 12.20 mg GAE g(-1) DW. The TPC and TAA in MAE extracts were higher than the other three extracts. Copyright © 2015 Elsevier Ltd. All rights reserved.

Comparison of solvent/derivatization agent systems for determination of extractable toluene diisocyanate from flexible polyurethane foam.

PubMed

Vangronsveld, Erik; Berckmans, Steven; Spence, Mark

2013-06-01

Flexible polyurethane foam (FPF) is produced from the reaction of toluene diisocyanate (TDI) and polyols. Limited and conflicting results exist in the literature concerning the presence of unreacted TDI remaining in FPF as determined by various solvent extraction and analysis techniques. This study reports investigations into the effect of several solvent/derivatization agent combinations on extractable TDI results and suggests a preferred method. The suggested preferred method employs a syringe-based multiple extraction of foam samples with a toluene solution of 1-(2-methoxyphenyl)-piperazine. Extracts are analyzed by liquid chromatography using an ion trap mass spectrometry detection technique. Detection limits of the method are ~10ng TDI g(-1) foam (10 ppb, w/w) for each TDI isomer (i.e. 2,4-TDI and 2,6-TDI). The method was evaluated by a three-laboratory interlaboratory comparison using two representative foam samples. The total extractable TDI results found by the three labs for the two foams were in good agreement (relative standard deviation of the mean of 30-40%). The method has utility as a basis for comparing FPFs, but the interpretation of extractable TDI results using any solvent as the true value for 'free' or 'unreacted' TDI in the foam is problematic, as demonstrated by the difference in the extracted TDI results from the different extraction systems studied. Further, a consideration of polyurethane foam chemistry raises the possibility that extractable TDI may result from decomposition of parts of the foam structure (e.g. dimers, biurets, and allophanates) by the extraction system.

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

PubMed

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

2010-06-01

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

Identification of nonvolatile coal derived products via chromatography coupled with on-line FTIR detection. Quarterly progress report, March 1-May 31, 1985. [C/sub 2/H/sub 2/ extracts of ground coal, coffee and paprika

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

Taylor, L.T.

Because it has been our goal to interface the supercritical fluid chromatograph with a Fourier transform infrared spectrometer we have initially chosen packed columns due to their increased sample capacities, and supercritical CO/sub 2/ because of its infrared transparency. This paper compares two sampling techniques that can be utilized in packed column supercritical fluid Chromatography (SFC). Traditional sample introduction is accomplished using an injector with a sample loop. The loop is filled with the appropriate amount of material, and subsequently inserted into the mobile phase path. In most cases the sample must be either dissolved or extracted into an appropriatemore » solvent for such sample introduction. Note that unlike HPLC, where the solvent can be the same as the mobile phase, traditional sampling with SFC must use a solvent that is very different from the mobile phase. As a result, solvent peaks are almost always present, especially with universal detectors like FTIR. An alternative method is described here whereby both extraction of the sample and introduction of the extract onto the column is accomplished on-line using only the supercritical fluid mobile phase. This sampling technique is made possible by a simple valving scheme which ties directly the extraction vessel, the injector, the packed column and the detector. This technique has several advantages over the traditional methods, not the least of which is the absence of a large amount of foreign solvent introduced on the column. 11 refs., 7 figs.« less

Development of dispersive liquid-liquid microextraction technique using ternary solvents mixture followed by heating for the rapid and sensitive analysis of phthalate esters and di(2-ethylhexyl) adipate.

PubMed

Farajzadeh, Mir Ali; Khoshmaram, Leila

2015-01-30

In this study, for the first time, a dispersive liquid-liquid microextraction technique using a ternary solvent mixture is reported. In order to extract five phthalate esters and di(2-ethylhexyl) adipate with different polarities from aqueous samples, a simplex centroid experimental design method was used to select an optimal mixture of ternary solvents prior to gas chromatographyflame ionization detection. In this work, dimethyl formamide as a disperser solvent containing dichloromethane, chloroform, and carbon tetrachloride as a ternary extraction solvent mixture is injected into sample solution and a cloudy solution is formed. After centrifuging, 250μL of the obtained sedimented phase was transferred into another tube and 5μL DMF was added to it. Then, the tube was heated in a water bath at 75°C for 5min in order to evaporate the main portion of the extraction solvents. Finally, 2μL of the remained phase is injected into the separation system. Under the optimum extraction conditions, the method shows wide linear ranges and low limits of detection and quantification between 0.03-0.15 and 0.09-0.55μgL(-1), respectively. Enrichment factors and extraction recoveries are in the ranges of 980-4500 and 20-90%, respectively. The method is successfully applied in the determination of the target analytes in mineral water, soda, lemon juice, vinegar, dough, and yogurt packed in plastic packages. Copyright © 2014 Elsevier B.V. All rights reserved.

Dialysis Extraction for Chromatography

NASA Technical Reports Server (NTRS)

Jahnsen, V. J.

1985-01-01

Chromatographic-sample pretreatment by dialysis detects traces of organic contaminants in water samples analyzed in field with minimal analysis equipment and minimal quantities of solvent. Technique also of value wherever aqueous sample and solvent must not make direct contact.

The extraction and chromatographic determination of the essentials oils from Ocimum basilicum L. by different techniques

NASA Astrophysics Data System (ADS)

Loredana Soran, Maria; Codruta Cobzac, Simona; Varodi, Codruta; Lung, Ildiko; Surducan, Emanoil; Surducan, Vasile

2009-08-01

Three different techniques (maceration, sonication and extraction in microwave field) were used for extraction of essential oils from Ocimum basilicum L. The extracts were analyzed by TLC/HPTLC technique and the fingerprint informations were obtained. The GC-FID was used to characterized the extraction efficiency and for identify the terpenic bioactive compounds. The most efficient extraction technique was maceration followed by microwave and ultrasound. The best extraction solvent system was ethyl ether + ethanol (1:1, v/v). The main compounds identified in Ocimum basilicum L. extracts were: α and β-pinene (mixture), limonene, citronellol, and geraniol.

Extraction of organic compounds with room temperature ionic liquids.

PubMed

Poole, Colin F; Poole, Salwa K

2010-04-16

Room temperature ionic liquids are novel solvents with a rather specific blend of physical and solution properties that makes them of interest for applications in separation science. They are good solvents for a wide range of compounds in which they behave as polar solvents. Their physical properties of note that distinguish them from conventional organic solvents are a negligible vapor pressure, high thermal stability, and relatively high viscosity. They can form biphasic systems with water or low polarity organic solvents and gases suitable for use in liquid-liquid and gas-liquid partition systems. An analysis of partition coefficients for varied compounds in these systems allows characterization of solvent selectivity using the solvation parameter model, which together with spectroscopic studies of solvent effects on probe substances, results in a detailed picture of solvent behavior. These studies indicate that the solution properties of ionic liquids are similar to those of polar organic solvents. Practical applications of ionic liquids in sample preparation include extractive distillation, aqueous biphasic systems, liquid-liquid extraction, liquid-phase microextraction, supported liquid membrane extraction, matrix solvents for headspace analysis, and micellar extraction. The specific advantages and limitations of ionic liquids in these studies is discussed with a view to defining future uses and the need not to neglect the identification of new room temperature ionic liquids with physical and solution properties tailored to the needs of specific sample preparation techniques. The defining feature of the special nature of ionic liquids is not their solution or physical properties viewed separately but their unique combinations when taken together compared with traditional organic solvents. Copyright 2009 Elsevier B.V. All rights reserved.

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

PubMed

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

2013-03-01

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

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

PubMed

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

2014-12-01

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

Enzyme assisted extraction of biomolecules as an approach to novel extraction technology: A review.

PubMed

Nadar, Shamraja S; Rao, Priyanka; Rathod, Virendra K

2018-06-01

An interest in the development of extraction techniques of biomolecules from various natural sources has increased in recent years due to their potential applications particularly for food and nutraceutical purposes. The presence of polysaccharides such as hemicelluloses, starch, pectin inside the cell wall, reduces the extraction efficiency of conventional extraction techniques. Conventional techniques also suffer from low extraction yields, time inefficiency and inferior extract quality due to traces of organic solvents present in them. Hence, there is a need of the green and novel extraction methods to recover biomolecules. The present review provides a holistic insight to various aspects related to enzyme aided extraction. Applications of enzymes in the recovery of various biomolecules such as polyphenols, oils, polysaccharides, flavours and colorants have been highlighted. Additionally, the employment of hyphenated extraction technologies can overcome some of the major drawbacks of enzyme based extraction such as longer extraction time and immoderate use of solvents. This review also includes hyphenated intensification techniques by coupling conventional methods with ultrasound, microwave, high pressure and supercritical carbon dioxide. The last section gives an insight on application of enzyme immobilization as a strategy for large scale extraction. Immobilization of enzymes on magnetic nanoparticles can be employed to enhance the operational performance of the system by multiple use of expensive enzymes making them industrially and economically feasible. Copyright © 2018 Elsevier Ltd. All rights reserved.

[Determination of benzo(alpha)pyrene in food with microwave-assisted extraction].

PubMed

Zhou, Na; Luo, He-Dong; Li, Na; Li, Yao-Qun

2014-03-01

Coupling derivative technique and constant-energy synchronous fluorescence scanning technique, a method of determining benzo[alpha] pyrene in foods by second derivative constant-energy synchronous spectrofluorimetry after microwave-assisted treatment of samples was established using domestic microwave oven. The main factors of influencing the efficiency of microwave extraction were discussed, including the extraction solvent types and amounts, the microwave extraction time, microwave radiation power and cooling time. And the comparison with ultrasonic extraction was made. Low-fat food samples, which were just microwave-extracted with mixed-solvents, could be analyzed immediately by the spectrofluorimetric technique. For high-fat food samples, microwave-assisted saponification and extraction were made at the same time, thus simplifying operation steps and reducing sample analysis time. So the whole sample analysis process could be completed within one hour. This method was simple, rapid and inexpensive. In consequence, it was applied to determine benzo(a)pyrene in food with good reproducibility and the recoveries of benzo(alpha) pyrene ranged from 90.0% to 105.0% for the low fat samples and 83.3% to 94.6% for high-fat samples.

Efficient purification of paclitaxel from yews using high-performance displacement chromatography technique.

PubMed

Watchueng, Jean; Kamnaing, Pierre; Gao, Jin-Ming; Kiyota, Taira; Yeboah, Faustinus; Konishi, Yasuo

2011-05-20

Paclitaxel was purified using high-performance displacement chromatography (HPDC) technique, but not by the mechanism of HPDC. On small scale, paclitaxel was extracted with methanol from dry needles of Taxus canadensis and was enriched by extracting with chloroform after removing water-soluble hydrophilic components and hexane-soluble hydrophobic components. Then, 93-99% purity of paclitaxel was obtained using the HPDC technique. On large scale, taxanes were enriched by solvent partitioning between acetic acid/MeOH/H(2)O and hexane and extracted with CH(2)Cl(2). Taxanes except paclitaxel were further removed by extracting with methanol-water-trifluoroacetic acid (1.0:98.9:0.1, v/v/v). Applying HPDC technique to water-insoluble substances is problematic as this method requires a highly aqueous solvent system. In order to overcome this incompatibility, a system was set up where paclitaxel, although in low concentration, was extracted by methanol-water-trifluoroacetic acid (10.0:89.9:0.1, v/v/v). Recycling the extracting solvent to ensure minimal volume, the extracted paclitaxel was adsorbed on a C(18) trap column. A C(18) column of 4.6mm internal diameter was then connected to the trap column. The HPDC technique was thus carried out using an isocratic acetonitrile-water-trifluoroacetic acid (30.0:69.9:0.1, v/v/v) mobile phase consisting of a displacer cetylpyridinium trifluoroacetate (3mg/mL). Paclitaxel was co-eluted with the displacer and spontaneously crystallized. The crystal (114mg) showed 99.4% purity and only 10% of paclitaxel in the starting crude extract was lost during the enrichment/purification processes. This large scale purification method was successfully applied to purify paclitaxel from Chinese yew in small scale, suggesting general applicability of the method. This is the first report of purifying a water-insoluble natural product using HPDC technique. Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

PubMed

Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

2015-05-01

A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (<10%) for phenols. Four real soil samples were analyzed by the proposed method to assess its applicability. Experimental results showed that the soil samples were free of our target compounds, and average recoveries were in the range of 87.9-110%. These findings indicate that accelerated solvent extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of polycyclic aromatic hydrocarbons in sediment reference materials by microwave-assisted extraction.

PubMed

Shu, Y Y; Lao, R C; Chiu, C H; Turle, R

2000-12-01

The microwave-assisted extraction (MAE) of polycyclic aromatic hydrocarbons (PAHs) from harbor sediment reference material EC-1, marine sediment reference material HS-2 and PAH-spiked river bed soil was conducted. The extraction conditions for EC-1 were carried out at 70 degrees C and 100 degrees C under pressure in closed vessels with cyclohexane acetone (1:1), cyclohexane-water (3:1), hexane acetone (1:1), and hexane-water (3:1) for 10 min. A comparison between MAE and a 16-h Soxhlet extraction (SX) method showed that both techniques gave comparable results with certified values. MAE has advantages over the currently used Soxhlet technique due to a faster extraction time and lower quantity of solvent used. The consumption of organic solvent of the microwave method was less than one-tenth compared to Soxhlet.

Production of proteases from organic wastes by solid-state fermentation: downstream and zero waste strategies.

PubMed

Marín, Maria; Artola, Adriana; Sánchez, Antoni

2018-04-01

Production of enzymes through solid-state fermentation (SSF) of agro-industrial wastes reports high productivity with low investment. The extraction of the final product from the solid waste and solid disposal represent the main cost of the process. In this work, the complete downstream processes of SSF of two industrial residues for the production of proteases, soy fibre (SF) and a mixture of hair and sludge (HS), were studied in terms of activity recovery, using different extraction parameters (extracting solvent, ratio solid: solvent and extraction mode). Activity after lyophilisation was tested. Solid waste valorisation after extraction was studied using respiration techniques and biogas production tests, as part of a zero waste strategy. Results showed a maximum extraction yield of 91% for SF and 121% for HS, both in agitated mode and distilled water as extraction agent. An average activity recovery of 95 ± 6 and 94 ± 6% for SF and HS, respectively, was obtained after lyophilisation and redissolution. To reduce the cost of extraction, a ratio 1:3 w : v solid-solvent in static mode is advised for SF, and 1:2 w : v extraction ratio in agitated mode for HS, both with distilled water as extracting agent. Both composting and anaerobic digestion are suitable techniques for valorisation of the waste material.

Microwave-assisted extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb.

PubMed

Zhang, Fan; Yang, Yi; Su, Ping; Guo, Zhenku

2009-01-01

Euonymus alatus (Thunb.) has been used as one of traditional Chinese medicines for several thousand years. Conventional methods for the extraction of rutin and quercetin from E. alatus, including solvent extraction, Soxhlet extraction and heat reflux extraction are characterised by long extraction times and consumption of large amounts of solvents. To develop a simple and rapid method for the extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb using microwave-assisted extraction (MAE) technique. MAE experiments were performed with a multimode microwave extraction system. The experimental variables that affect the MAE process, such as the concentration of ethanol solution, extractant volume, microwave power and extraction time were optimised. Yields were determined by HPLC. The results were compared with that obtained by classical Soxhlet and ultrasonic-assisted extraction (UAE). From the optimised conditions for MAE of rutin and quercetin it can be concluded that the solvent is 50% ethanol (v/v) solution, the extractant volume is 40 mL, microwave power is 170 W and irradiation time is 6 min. Compared with Soxhlet extraction and ultrasonic extraction, microwave extraction is a rapid method with a higher yield and lower solvent consumption. The results showed that MAE can be used as an efficient and rapid method for the extraction of the active components from plants.

A modified method for determining tannin-protein precipitation capacity using accelerated solvent extraction (ASE) and microplate gel filtration.

PubMed

McArt, Scott H; Spalinger, Donald E; Kennish, John M; Collins, William B

2006-06-01

The protein precipitation assay used by Robbins et al., (1987) Ecology 68:98-107 has been shown to predict successfully the reduction in protein availability to some ruminants due to tannins. The procedure, however, is expensive and laborious, which limits its utility, especially for quantitative ecological or nutritional applications where large numbers of assays may be required. We have modified the method to decrease its cost and increase laboratory efficiency by: (1) automating the extraction by using Accelerated Solvent Extraction (ASE); and (2) by scaling and automating the precipitation reaction, chromatography, and spectrometry with microplate gel filtration and an automated UV-VIS microplate spectrometer. ASE extraction is shown to be as effective at extracting tannins as the hot methanol technique. Additionally, the microplate assay is sensitive and precise. We show that the results from the new technique correspond in a nearly 1:1 relationship to the results of the previous technique. Hence, this method could reliably replace the older method with no loss in relevance to herbivore protein digestion. Moreover, the ASE extraction technique should be applicable to other tannin-protein precipitation assays and possibly other phenolic assays.

Bio-refinery of orange peels waste: a new concept based on integrated green and solvent free extraction processes using ultrasound and microwave techniques to obtain essential oil, polyphenols and pectin.

PubMed

Boukroufa, Meryem; Boutekedjiret, Chahrazed; Petigny, Loïc; Rakotomanomana, Njara; Chemat, Farid

2015-05-01

In this study, extraction of essential oil, polyphenols and pectin from orange peel has been optimized using microwave and ultrasound technology without adding any solvent but only "in situ" water which was recycled and used as solvent. The essential oil extraction performed by Microwave Hydrodiffusion and Gravity (MHG) was optimized and compared to steam distillation extraction (SD). No significant changes in yield were noticed: 4.22 ± 0.03% and 4.16 ± 0.05% for MHG and SD, respectively. After extraction of essential oil, residual water of plant obtained after MHG extraction was used as solvent for polyphenols and pectin extraction from MHG residues. Polyphenols extraction was performed by ultrasound-assisted extraction (UAE) and conventional extraction (CE). Response surface methodology (RSM) using central composite designs (CCD) approach was launched to investigate the influence of process variables on the ultrasound-assisted extraction (UAE). The statistical analysis revealed that the optimized conditions of ultrasound power and temperature were 0.956 W/cm(2) and 59.83°C giving a polyphenol yield of 50.02 mgGA/100 g dm. Compared with the conventional extraction (CE), the UAE gave an increase of 30% in TPC yield. Pectin was extracted by conventional and microwave assisted extraction. This technique gives a maximal yield of 24.2% for microwave power of 500 W in only 3 min whereas conventional extraction gives 18.32% in 120 min. Combination of microwave, ultrasound and the recycled "in situ" water of citrus peels allow us to obtain high added values compounds in shorter time and managed to make a closed loop using only natural resources provided by the plant which makes the whole process intensified in term of time and energy saving, cleanliness and reduced waste water. Copyright © 2014 Elsevier B.V. All rights reserved.

Effects of moisture content in cigar tobacco on nicotine extraction. Similarity between soxhlet and focused open-vessel microwave-assisted techniques.

PubMed

Ng, Lay-Keow; Hupé, Michel

2003-09-05

The effects of tobacco moisture on nicotine yield were investigated in this study. Soxhlet and microwave-assisted techniques were used to extract nicotine from cigar fillers of varying moisture contents (5-20%), using a polar (methanol) and a non-polar (isooctane) solvent. The extracts were analyzed by a gas chromatograph equipped with a flame-ionization detector. For both extraction techniques, higher nicotine yields were consistently obtained with methanol than with isooctane from the same samples. Solubility of nicotine salts in methanol but not in isooctane is the major cause of this observation. Moreover, pronounced effects of the tobacco moisture content on extraction efficiency were observed with isooctane but not with methanol. For microwave assisted extraction (MAE) with isooctane, nicotine yield increased from 3 to 70% as the moisture level in tobacco was raised from 3 to 13%, and leveled off thereafter. Similar observations were made with Soxhlet extraction. While MAE results were rationalized by the known cell-rupture process, a mechanism based on the interaction between the solvents and the structural components of the plant cells has been proposed to account for the observations made with Soxhlet extraction.

Comparison of yield, composition, and antioxidant activity of turmeric (Curcuma longa L.) extracts obtained using various techniques.

PubMed

Braga, Mara E M; Leal, Patrícia F; Carvalho, João E; Meireles, M Angela A

2003-10-22

Turmeric extracts were obtained from two lots of raw material (M and S) using various techniques: hydrodistillation, low pressure solvent extraction, Soxhlet, and supercritical extraction using carbon dioxide and cosolvents. The solvents and cosolvents tested were ethanol, isopropyl alcohol, and their mixture in equal proportions. The composition of the extracts was determined by gas chromatography-flame ionization detection (GC-FID) and UV. The largest yield (27%, weight) was obtained in the Soxhlet extraction (turmeric (S), ethanol = 1:100); the lowest yield was detected in the hydrodistillation process (2.1%). For the supercritical extraction, the best cosolvent was a mixture of ethanol and isopropyl alcohol. Sixty percent of the light fraction of the extracts consisted of ar-turmerone, (Z)-gamma-atlantone, and (E)-gamma-atlantone, except for the Soxhlet extracts (1:100, ethanol), for which only ar-turmeronol and (Z)-alpha-atlantone were detected. The maximum amount of curcuminoids (8.43%) was obtained using Soxhlet extraction (ethanol/isopropyl alcohol). The Soxhlet and low pressure extract exhibited the strongest antioxidant activities.

Multi-residue method for determination of 58 pesticides, pharmaceuticals and personal care products in water using solvent demulsification dispersive liquid-liquid microextraction combined with liquid chromatography-tandem mass spectrometry.

PubMed

Caldas, Sergiane Souza; Rombaldi, Caroline; Arias, Jean Lucas de Oliveira; Marube, Liziane Cardoso; Primel, Ednei Gilberto

2016-01-01

A rapid and efficient sample pretreatment using solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was studied for the extraction of 58 pharmaceuticals and personal care products (PPCPs) and pesticides from water samples. Type and volume of extraction and disperser solvents, pH, salt addition, amount of salt and type of demulsification solvent were evaluated. Limits of quantification (LOQ) in the range from 0.0125 to 1.25 µg L(-1) were reached, and linearity was in the range from the LOQ of each compound to 25 μg L(-1). Recoveries ranged from 60% to 120% for 84% of the compounds, with relative standard deviations lower than 29%. The proposed method demonstrated, for the first time, that sample preparation by SD-DLLME with determination by LC-MS/MS can be successfully used for the simultaneous extraction of 32 pesticides and 26 PPCPs from water samples. The entire procedure, including the extraction of 58 organic compounds from the aqueous sample solution and the breaking up of the emulsion after extraction with water, rather than with an organic solvent, was environmentally friendly. In addition, this technique was less expensive and faster than traditional techniques. Finally, the analytical method under study was successfully applied to the analysis of all 58 pesticides and PPCPs in surface water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Method 1664: N-hexane extractable material (hem) and silica gel treated n-hexane extractable material (SGT-HEM) by extraction and gravimetry (oil and grease and total petroleum hydrocarbons), April 1995

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

NONE

Method 1664 was developed by the United States Environmental Protection Agency Office of Science and Technology to replace previously used gravimetric procedures that employed Freon-113, a Class I CFC, as the extraction solvent for the determination of oil and grease and petroleum hydrocarbons. Method 1664 is a performance-based method applicable to aqueous matrices that requires the use of n-hexane as the extraction solvent and gravimetry as the determinative technique. In addition, QC procedures designed to monitor precision and accuracy have been incorporated into Method 1664.

Ambient Mass Spectrometry Imaging Using Direct Liquid Extraction Techniques

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

Laskin, Julia; Lanekoff, Ingela

2015-11-13

Mass spectrometry imaging (MSI) is a powerful analytical technique that enables label-free spatial localization and identification of molecules in complex samples.1-4 MSI applications range from forensics5 to clinical research6 and from understanding microbial communication7-8 to imaging biomolecules in tissues.1, 9-10 Recently, MSI protocols have been reviewed.11 Ambient ionization techniques enable direct analysis of complex samples under atmospheric pressure without special sample pretreatment.3, 12-16 In fact, in ambient ionization mass spectrometry, sample processing (e.g., extraction, dilution, preconcentration, or desorption) occurs during the analysis.17 This substantially speeds up analysis and eliminates any possible effects of sample preparation on the localization of moleculesmore » in the sample.3, 8, 12-14, 18-20 Venter and co-workers have classified ambient ionization techniques into three major categories based on the sample processing steps involved: 1) liquid extraction techniques, in which analyte molecules are removed from the sample and extracted into a solvent prior to ionization; 2) desorption techniques capable of generating free ions directly from substrates; and 3) desorption techniques that produce larger particles subsequently captured by an electrospray plume and ionized.17 This review focuses on localized analysis and ambient imaging of complex samples using a subset of ambient ionization methods broadly defined as “liquid extraction techniques” based on the classification introduced by Venter and co-workers.17 Specifically, we include techniques where analyte molecules are desorbed from solid or liquid samples using charged droplet bombardment, liquid extraction, physisorption, chemisorption, mechanical force, laser ablation, or laser capture microdissection. Analyte extraction is followed by soft ionization that generates ions corresponding to intact species. Some of the key advantages of liquid extraction techniques include the ease of operation, ability to analyze samples in their native environments, speed of analysis, and ability to tune the extraction solvent composition to a problem at hand. For example, solvent composition may be optimized for efficient extraction of different classes of analytes from the sample or for quantification or online derivatization through reactive analysis. In this review, we will: 1) introduce individual liquid extraction techniques capable of localized analysis and imaging, 2) describe approaches for quantitative MSI experiments free of matrix effects, 3) discuss advantages of reactive analysis for MSI experiments, and 4) highlight selected applications (published between 2012 and 2015) that focus on imaging and spatial profiling of molecules in complex biological and environmental samples.« less

Downstream Processing of Synechocystis for Biofuel Production

NASA Astrophysics Data System (ADS)

Sheng, Jie

Lipids and free fatty acids (FFA) from cyanobacterium Synechocystis can be used for biofuel (e.g. biodiesel or renewable diesel) production. In order to utilize and scale up this technique, downstream processes including culturing and harvest, cell disruption, and extraction were studied. Several solvents/solvent systems were screened for lipid extraction from Synechocystis. Chloroform + methanol-based Folch and Bligh & Dyer methods were proved to be "gold standard" for small-scale analysis due to their highest lipid recoveries that were confirmed by their penetration of the cell membranes, higher polarity, and stronger interaction with hydrogen bonds. Less toxic solvents, such as methanol and MTBE, or direct transesterification of biomass (without preextraction step) gave only slightly lower lipid-extraction yields and can be considered for large-scale application. Sustained exposure to high and low temperature extremes severely lowered the biomass and lipid productivity. Temperature stress also triggered changes of lipid quality such as the degree of unsaturation; thus, it affected the productivities and quality of Synechocystis-derived biofuel. Pulsed electric field (PEF) was evaluated for cell disruption prior to lipid extraction. A treatment intensity > 35 kWh/m3 caused significant damage to the plasma membrane, cell wall, and thylakoid membrane, and it even led to complete disruption of some cells into fragments. Treatment by PEF enhanced the potential for the low-toxicity solvent isopropanol to access lipid molecules during subsequent solvent extraction, leading to lower usage of isopropanol for the same extraction efficiency. Other cell-disruption methods also were tested. Distinct disruption effects to the cell envelope, plasma membrane, and thylakoid membranes were observed that were related to extraction efficiency. Microwave and ultrasound had significant enhancement of lipid extraction. Autoclaving, ultrasound, and French press caused significant release of lipid into the medium, which may increase solvent usage and make medium recycling difficult. Production of excreted FFA by mutant Synechocystis has the potential of reducing the complexity of downstream processing. Major problems, such as FFA precipitation and biodegradation by scavengers, account for FFA loss in operation. Even a low concentration of FFA scavengers could consume FFA at a high rate that outpaced FFA production rate. Potential strategies to overcome FFA loss include high pH, adsorptive resin, and sterilization techniques.

A surprising method for green extraction of essential oil from dry spices: Microwave dry-diffusion and gravity.

PubMed

Farhat, Asma; Fabiano-Tixier, Anne-Sylvie; Visinoni, Franco; Romdhane, Mehrez; Chemat, Farid

2010-11-19

Without adding any solvent or water, we proposed a novel and green approach for the extraction of secondary metabolites from dried plant materials. This "solvent, water and vapor free" approach based on a simple principle involves the application of microwave irradiation and earth gravity to extract the essential oil from dried caraway seeds. Microwave dry-diffusion and gravity (MDG) has been compared with a conventional technique, hydrodistillation (HD), for the extraction of essential oil from dried caraway seeds. Essential oils isolated by MDG were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained by HD, but MDG was better than HD in terms of rapidity (45min versus 300min), energy saving, and cleanliness. The present apparatus permits fast and efficient extraction, reduces waste, avoids water and solvent consumption, and allows substantial energy savings. Copyright © 2010 Elsevier B.V. All rights reserved.

Determination of zearalenone and its metabolites in endometrial cancer by coupled separation techniques.

PubMed

Gadzała-Kopciuch, Renata; Cendrowski, Krzysztof; Cesarz, Anna; Kiełbasa, Paweł; Buszewski, Bogusław

2011-10-01

This study presents a selective method of isolation of zearalenone (ZON) and its metabolite, α-zearalenol (α-ZOL), in neoplastically changed human tissue by accelerated solvent and ultrasonic extractions using a mixture of acetonitrile/water (84/16% v/v) as the extraction solvent. Extraction effectiveness was determined through the selection of parameters (composition of the solvent mixture, temperature, pressure, number of cycles) with tissue contamination at the level of nanograms per gram. The produced acetonitrile/water extracts were purified, and analytes were enriched in columns packed with homemade molecularly imprinted polymers. Purified extracts were determined by liquid chromatography (LC) coupled with different detection systems (diode array detection--DAD and mass spectrometry--MS) involving the Ascentis RP-Amide as a stationary phase and gradient elution. The combination of UE-MISPE-LC (ultrasonic extraction--molecularly imprinted solid-phase extraction--liquid chromatography) produced high (R≈95-98%) and repeatable (RSD<3%) recovery values for ZON and α-ZOL. © The Author(s) 2011. This article is published with open access at Springerlink.com

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

Moyer, Bruce A.

The North American industry has employed major solvent-extraction processes to support a wide range of separations including but not limited to chemical, metallurgical, nuclear, biochemical, pharmaceutical, and petroleum applications. The knowledge enabling these separations has been obtained through fundamental studies in academe, government and industry. The International Solvent Extraction Conferences have been and continue to be a major gathering of scientists, engineers, operators, and vendors from around the world, who present new findings since the last meeting, exchange ideas, make business contacts, and conduct collegial discussions. The ISEC 2008 program emphasizes fundamentals to industrial applications of solvent extraction, particularly howmore » this broad spectrum of activities is interconnected and has led to the implementation of novel processes. The oral and poster sessions have been organized into seven topics: Fundamentals; Novel Reagents, Materials and Techniques; Nuclear Fuel Reprocessing; Hydrometallurgy and Metals Extraction; Analytical and Preparative Applications; Biotechnology, Pharmaceuticals, Life-Science Products, and Organic Products; and Process Chemistry and Engineering. Over 350 abstracts were received, resulting in more than 260 manuscripts published in these proceedings. Five outstanding plenary presentations have been identified, with five parallel sessions for oral presentations and posters. In recognition of the major role solvent extraction (SX) plays in the hydrometallurgical and nuclear industries, these proceedings begin with sections focusing on hydrometallurgy, process chemistry, and engineering. More fundamental topics follow, including sections on novel reagents, materials, and techniques, featuring novel applications in analytical and biotechnology areas. Despite the diversity of topics and ideas represented, however, the primary focus of the ISEC community continues to be metals extraction. Four papers from these proceedings have been entered already in INIS in the form of individual reports. Among the remaining papers, 60 have been selected from the following sessions: Plenary Lectures, Hydrometallurgy and Metals Extraction, Nuclear Fuel Reprocessing, Analytical and Preparative Applications, Fundamentals, and Novel Reagents, Materials, and Techniques.« less

Extraction and identification of flavonoids from parsley extracts by HPLC analysis

NASA Astrophysics Data System (ADS)

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

2012-02-01

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

Development of Solvent Extraction Approach to Recycle Enriched Molybdenum Material

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

Tkac, Peter; Brown, M. Alex; Sen, Sujat

2016-06-01

Argonne National Laboratory, in cooperation with Oak Ridge National Laboratory and NorthStar Medical Technologies, LLC, is developing a recycling process for a solution containing valuable Mo-100 or Mo-98 enriched material. Previously, Argonne had developed a recycle process using a precipitation technique. However, this process is labor intensive and can lead to production of large volumes of highly corrosive waste. This report discusses an alternative process to recover enriched Mo in the form of ammonium heptamolybdate by using solvent extraction. Small-scale experiments determined the optimal conditions for effective extraction of high Mo concentrations. Methods were developed for removal of ammonium chloridemore » from the molybdenum product of the solvent extraction process. In large-scale experiments, very good purification from potassium and other elements was observed with very high recovery yields (~98%).« less

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

PubMed

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

2015-03-01

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

Automation of static and dynamic non-dispersive liquid phase microextraction. Part 1: Approaches based on extractant drop-, plug-, film- and microflow-formation.

PubMed

Alexovič, Michal; Horstkotte, Burkhard; Solich, Petr; Sabo, Ján

2016-02-04

Simplicity, effectiveness, swiftness, and environmental friendliness - these are the typical requirements for the state of the art development of green analytical techniques. Liquid phase microextraction (LPME) stands for a family of elegant sample pretreatment and analyte preconcentration techniques preserving these principles in numerous applications. By using only fractions of solvent and sample compared to classical liquid-liquid extraction, the extraction kinetics, the preconcentration factor, and the cost efficiency can be increased. Moreover, significant improvements can be made by automation, which is still a hot topic in analytical chemistry. This review surveys comprehensively and in two parts the developments of automation of non-dispersive LPME methodologies performed in static and dynamic modes. Their advantages and limitations and the reported analytical performances are discussed and put into perspective with the corresponding manual procedures. The automation strategies, techniques, and their operation advantages as well as their potentials are further described and discussed. In this first part, an introduction to LPME and their static and dynamic operation modes as well as their automation methodologies is given. The LPME techniques are classified according to the different approaches of protection of the extraction solvent using either a tip-like (needle/tube/rod) support (drop-based approaches), a wall support (film-based approaches), or microfluidic devices. In the second part, the LPME techniques based on porous supports for the extraction solvent such as membranes and porous media are overviewed. An outlook on future demands and perspectives in this promising area of analytical chemistry is finally given. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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

2017-05-01

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

Microwave-Assisted Extraction of Fucoidan from Marine Algae.

PubMed

Mussatto, Solange I

2015-01-01

Microwave-assisted extraction (MAE) is a technique that can be applied to extract compounds from different natural resources. In this chapter, the use of this technique to extract fucoidan from marine algae is described. The method involves a closed MAE system, ultrapure water as extraction solvent, and suitable conditions of time, pressure, and algal biomass/water ratio. By using this procedure under the specified conditions, the penetration of the electromagnetic waves into the material structure occurs in an efficient manner, generating a distributed heat source that promotes the fucoidan extraction from the algal biomass.

Micro-Raman Technology to Interrogate Two-Phase Extraction on a Microfluidic Device.

PubMed

Nelson, Gilbert L; Asmussen, Susan E; Lines, Amanda M; Casella, Amanda J; Bottenus, Danny R; Clark, Sue B; Bryan, Samuel A

2018-05-21

Microfluidic devices provide ideal environments to study solvent extraction. When droplets form and generate plug flow down the microfluidic channel, the device acts as a microreactor in which the kinetics of chemical reactions and interfacial transfer can be examined. Here, we present a methodology that combines chemometric analysis with online micro-Raman spectroscopy to monitor biphasic extractions within a microfluidic device. Among the many benefits of microreactors is the ability to maintain small sample volumes, which is especially important when studying solvent extraction in harsh environments, such as in separations related to the nuclear fuel cycle. In solvent extraction, the efficiency of the process depends on complex formation and rates of transfer in biphasic systems. Thus, it is important to understand the kinetic parameters in an extraction system to maintain a high efficiency and effectivity of the process. This monitoring provided concentration measurements in both organic and aqueous plugs as they were pumped through the microfluidic channel. The biphasic system studied was comprised of HNO 3 as the aqueous phase and 30% (v/v) tributyl phosphate in n-dodecane comprised the organic phase, which simulated the plutonium uranium reduction extraction (PUREX) process. Using pre-equilibrated solutions (post extraction), the validity of the technique and methodology is illustrated. Following this validation, solutions that were not equilibrated were examined and the kinetics of interfacial mass transfer within the biphasic system were established. Kinetic results of extraction were compared to kinetics already determined on a macro scale to prove the efficacy of the technique.

A combination strategy for extraction and isolation of multi-component natural products by systematic two-phase solvent extraction-(13)C nuclear magnetic resonance pattern recognition and following conical counter-current chromatography separation: Podophyllotoxins and flavonoids from Dysosma versipellis (Hance) as examples.

PubMed

Yang, Zhi; Wu, Youqian; Wu, Shihua

2016-01-29

Despite of substantial developments of extraction and separation techniques, isolation of natural products from natural resources is still a challenging task. In this work, an efficient strategy for extraction and isolation of multi-component natural products has been successfully developed by combination of systematic two-phase liquid-liquid extraction-(13)C NMR pattern recognition and following conical counter-current chromatography separation. A small-scale crude sample was first distributed into 9 systematic hexane-ethyl acetate-methanol-water (HEMWat) two-phase solvent systems for determination of the optimum extraction solvents and partition coefficients of the prominent components. Then, the optimized solvent systems were used in succession to enrich the hydrophilic and lipophilic components from the large-scale crude sample. At last, the enriched components samples were further purified by a new conical counter-current chromatography (CCC). Due to the use of (13)C NMR pattern recognition, the kinds and structures of major components in the solvent extracts could be predicted. Therefore, the method could collect simultaneously the partition coefficients and the structural information of components in the selected two-phase solvents. As an example, a cytotoxic extract of podophyllotoxins and flavonoids from Dysosma versipellis (Hance) was selected. After the systematic HEMWat system solvent extraction and (13)C NMR pattern recognition analyses, the crude extract of D. versipellis was first degreased by the upper phase of HEMWat system (9:1:9:1, v/v), and then distributed in the two phases of the system of HEMWat (2:8:2:8, v/v) to obtain the hydrophilic lower phase extract and lipophilic upper phase extract, respectively. These extracts were further separated by conical CCC with the HEMWat systems (1:9:1:9 and 4:6:4:6, v/v). As results, total 17 cytotoxic compounds were isolated and identified. In general, whole results suggested that the strategy was very efficient for the systematic extraction and isolation of biological active components from the complex biomaterials. Copyright © 2016 Elsevier B.V. All rights reserved.

Green technology approach towards herbal extraction method

NASA Astrophysics Data System (ADS)

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

2015-05-01

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

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

PubMed

Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-06-01

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

Extraction of polycyclic aromatic hydrocarbons and organochlorine pesticides from soils: a comparison between Soxhlet extraction, microwave-assisted extraction and accelerated solvent extraction techniques.

PubMed

Wang, Wentao; Meng, Bingjun; Lu, Xiaoxia; Liu, Yu; Tao, Shu

2007-10-29

The methods of simultaneous extraction of polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs) from soils using Soxhlet extraction, microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) were established, and the extraction efficiencies using the three methods were systemically compared from procedural blank, limits of detection and quantification, method recovery and reproducibility, method chromatogram and other factors. In addition, soils with different total organic carbon contents were used to test the extraction efficiencies of the three methods. The results showed that the values obtained in this study were comparable with the values reported by other studies. In some respects such as method recovery and reproducibility, there were no significant differences among the three methods for the extraction of PAHs and OCPs. In some respects such as procedural blank and limits of detection and quantification, there were significant differences among the three methods. Overall, ASE had the best extraction efficiency compared to MAE and Soxhlet extraction, and the extraction efficiencies of MAE and Soxhlet extraction were comparable to each other depending on the property such as TOC content of the studied soil. Considering other factors such as solvent consumption and extraction time, ASE and MAE are preferable to Soxhlet extraction.

Bubbles in solvent microextraction: the influence of intentionally introduced bubbles on extraction efficiency.

PubMed

Williams, D Bradley G; George, Mosotho J; Meyer, Riaan; Marjanovic, Ljiljana

2011-09-01

Significant improvements to microdrop extractions of triazine pesticides are realized by the intentional incorporation of an air bubble into the solvent microdroplet used in this microextraction technique. The increase is attributed partly to greater droplet surface area resulting from the air bubble being incorporated into the solvent droplet as opposed to it sitting thereon and partly to thin film phenomena. The method is useful at nanogram/liter levels (LOD 0.002-0.012 μg/L, LOQ 0.007-0.039 μg/L), is precise (7-12% at 10 μg/L concentration level), and is validated against certified reference materials containing 0.5 and 5.0 μg/L analyte. It tolerates water and fruit juice as matrixes without serious matrix effects. This new development brings a simple, inexpensive, and efficient preconcentration technique to bear which rivals solid phase microextraction methods.

An evaporation-assisted dispersive liquid-liquid microextraction technique as a simple tool for high performance liquid chromatography tandem-mass spectrometry determination of insecticides in wine.

PubMed

Timofeeva, Irina; Kanashina, Daria; Moskvin, Leonid; Bulatov, Andrey

2017-08-25

A sample pre-treatment technique based on evaporation-assisted dispersive liquid-liquid microextraction (EVA-DLLME), followed by HPLC-MS/MS has been developed for the determination of organophosphate insecticides (malathion, diazinon, phosalone) in wine samples. The procedure includes the addition of mixture of organic solvents (with density higher than water), consisting of the extraction (low density) and volatile (high density) solvents, to aqueous sample followed by heating of the mixture obtained, what promotes the volatile solvent evaporation and moving extraction solvent droplets from down to top of the aqueous sample and, as a consequence, microextraction of target analytes. To initiate the evaporation process an initiator is required. It was established that hexanol (extraction solvent) and dichloromethane (volatile solvent) mixture (1:1, v/v) provides effective microextraction of the insecticides from wine samples with recovery from 92 to 103%. The conditions of insecticides' microextraction such as selection of extraction solvent, ratio of hexanol/dichloromethane and hexanol/sample, type and concentration of initiator, and effect of ethanol as one of the main components of wine have been studied. Under optimal experimental conditions the linear detection ranges were found to be 10 -7 -10 -3 gL -1 for malathion, 10 -9 -10 -4 gL -1 for diazinon, and 10 -6 -10 -2 gL -1 for phosalone. The LODs, calculated from a blank test, based on 3σ, found to be 3×10 -8 gL -1 for malathion, 3×10 -10 gL -1 for diazinon and 3×10 -7 gL -1 for phosalone. The advantages of EVA-DLLME are the rapidity, simplicity, high sample throughput and low cost. As an outcome, the analytical results agreed fairly well with the results obtained by a reference GC-MS method. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of the effect of extraction solvent and organ selection on the chemical profile of Astragalus spinosus using HPTLC- multivariate image analysis.

PubMed

Shawky, Eman; Selim, Dina A

2017-09-01

The evaluation of extraction protocols for untargeted and targeted metabolomics was implemented for root and aerial organs of Astragalus spinosus in this work. The efficiency and complementarity of commonly used extraction solvents, namely petroleum ether, methylene chloride, ethyl acetate and n-butanol were considered for method evaluation using chemometric techniques in conjunction with new, simple, and fast high performance thin layer chromatography (HPTLC) method for fingerprint analysis by extracting information from a digitalized HPTLC plate using ImageJ software. A targeted approach was furtherly implemented by developing and validating an HPTLC method allowing the quantification of three saponin glycosides. The results of untargeted and targeted principle component analysis (PCA) and hierarchical cluster analysis (HCA) revealed that the apparent saponins profile seems to depend on a combined effect of matrix composition and the properties of the selected solvent for extraction, where both the biological matrix of the investigated plant organs, as well as the extraction solvent can influence the precision of metabolite abundances. Although, the aerial part is frequently discarded as waste, it is shown hereby that it has similar chemical profile compared to the medicinal part, roots, yet a different extraction solvents pattern is recognized between the two organs which can be attributed to the differences in the composition, permeability or accessibility of the sample matrix/organ tissues, rather than the chemical structures of the detected metabolites. Copyright © 2017 Elsevier B.V. All rights reserved.

Molecular-Scale Investigation of Heavy Metal Ions at a Charged Langmuir Monolayer

NASA Astrophysics Data System (ADS)

Rock, William; Qiao, Baofu; Uysal, Ahmet; Bu, Wei; Lin, Binhua

Solvent extraction - the surfactant-aided preferential transfer of a species from an aqueous to an organic phase - is an important technique used in heavy and precious metal refining and reprocessing. Solvent extraction requires transfer through an oil/water interface, and interfacial interactions are expected to control transfer kinetics and phase stability, yet these key interactions are poorly understood. Langmuir monolayers with charged headgroups atop concentrated salt solutions containing heavy metal ions act as a model of solvent extraction interfaces; studies of ions at a charged surface are also fundamentally important to many other phenomena including protein solvation, mineral surface chemistry, and electrochemistry. We probe these charged interfaces using a variety of surface-sensitive techniques - vibrational sum frequency generation (VSFG) spectroscopy, x-ray reflectivity (XRR), x-ray fluorescence near total reflection (XFNTR), and grazing incidence diffraction (GID). We integrate experiments with Molecular Dynamics (MD) simulations to uncover the molecular-level interfacial structure. This work is supported by the U.S. DOE, BES, Contract DE-AC02-06CH11357. ChemMatCARS is supported by NSF/CHE-1346572.

A Review of Enzymatic Transesterification of Microalgal Oil-Based Biodiesel Using Supercritical Technology

PubMed Central

Taher, Hanifa; Al-Zuhair, Sulaiman; Al-Marzouqi, Ali H.; Haik, Yousef; Farid, Mohammed M.

2011-01-01

Biodiesel is considered a promising replacement to petroleum-derived diesel. Using oils extracted from agricultural crops competes with their use as food and cannot realistically satisfy the global demand of diesel-fuel requirements. On the other hand, microalgae, which have a much higher oil yield per hectare, compared to oil crops, appear to be a source that has the potential to completely replace fossil diesel. Microalgae oil extraction is a major step in the overall biodiesel production process. Recently, supercritical carbon dioxide (SC-CO2) has been proposed to replace conventional solvent extraction techniques because it is nontoxic, nonhazardous, chemically stable, and inexpensive. It uses environmentally acceptable solvent, which can easily be separated from the products. In addition, the use of SC-CO2 as a reaction media has also been proposed to eliminate the inhibition limitations that encounter biodiesel production reaction using immobilized enzyme as a catalyst. Furthermore, using SC-CO2 allows easy separation of the product. In this paper, conventional biodiesel production with first generation feedstock, using chemical catalysts and solvent-extraction, is compared to new technologies with an emphasis on using microalgae, immobilized lipase, and SC-CO2 as an extraction solvent and reaction media. PMID:21915372

Optimization of extraction of linarin from Flos chrysanthemi indici by response surface methodology and artificial neural network.

PubMed

Pan, Hongye; Zhang, Qing; Cui, Keke; Chen, Guoquan; Liu, Xuesong; Wang, Longhu

2017-05-01

The extraction of linarin from Flos chrysanthemi indici by ethanol was investigated. Two modeling techniques, response surface methodology and artificial neural network, were adopted to optimize the process parameters, such as, ethanol concentration, extraction period, extraction frequency, and solvent to material ratio. We showed that both methods provided good predictions, but artificial neural network provided a better and more accurate result. The optimum process parameters include, ethanol concentration of 74%, extraction period of 2 h, extraction three times, solvent to material ratio of 12 mL/g. The experiment yield of linarin was 90.5% that deviated less than 1.6% from that obtained by predicted result. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of aroma compounds in apple cider using solvent-assisted flavor evaporation and headspace solid-phase microextraction.

PubMed

Xu, Yan; Fan, Wenlai; Qian, Michael C

2007-04-18

The aroma-active compounds in two apple ciders were identified using gas chromatography-olfactometry (GC-O) and GC-mass spectrometry (MS) techniques. The volatile compounds were extracted using solvent-assisted flavor evaporation (SAFE) and headspace solid-phase microextraction (HS-SPME). On the basis of odor intensity, the most important aroma compounds in the two apple cider samples were 2-phenylethanol, butanoic acid, octanoic acid, 2-methylbutanoic acid, 2-phenylethyl acetate, ethyl 2-methylbutanoate, ethyl butanoate, ethyl hexanoate, 4-ethylguaiacol, eugenol, and 4-vinylphenol. Sulfur-containing compounds, terpene derivatives, and lactones were also detected in ciders. Although most of the aroma compounds were common in both ciders, the aroma intensities were different. Comparison of extraction techniques showed that the SAFE technique had a higher recovery for acids and hydroxy-containing compounds, whereas the HS-SPME technique had a higher recovery for esters and highly volatile compounds.

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

PubMed Central

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

2005-01-01

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

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.

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.

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

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

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

2013-12-01

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

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

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

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

2013-11-05

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

Solvent-assisted stir bar sorptive extraction by using swollen polydimethylsiloxane for enhanced recovery of polar solutes in aqueous samples: Application to aroma compounds in beer and pesticides in wine.

PubMed

Ochiai, Nobuo; Sasamoto, Kikuo; David, Frank; Sandra, Pat

2016-07-15

A novel solvent-assisted stir bar sorptive extraction (SA-SBSE) technique was developed for enhanced recovery of polar solutes in aqueous samples. A conventional PDMS stir bar was swollen in several solvents with log Kow ranging from 1.0 to 3.5 while stirring for 30min prior to extraction. After extraction, thermal desorption - gas chromatography - (tandem) mass spectrometry (TD-GC-(MS/)MS) or liquid desorption - large volume injection (LD-LVI)-GC-MS were performed. An initial study involved investigation of potential solvents for SA-SBSE by weighing of the residual solvent in the swollen PDMS stir bar before and after extraction. Compared to conventional SBSE, SA-SBSE using diethyl ether, methyl isobutyl ketone, dichloromethane, diisopropyl ether and toluene provided higher recoveries from water samples for test solutes with log Kow<2.5. For SA-SBSE using dichloromethane, recoveries were improved by factors of 1.4-4.1, while maintaining or even improving the recoveries for test solutes with log Kow>2.5. The performance of the SA-SBSE method using dichloromethane, diisopropyl ether, and cyclohexane is illustrated with analyses of aroma compounds in beer and of pesticides in wine. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Solvent and solute ingress into hydrogels resolved by a combination of imaging techniques

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

Wagner, D.; Burbach, J.; Egelhaaf, S. U.

2016-05-28

Using simultaneous neutron, fluorescence, and optical brightfield transmission imaging, the diffusion of solvent, fluorescent dyes, and macromolecules into a crosslinked polyacrylamide hydrogel was investigated. This novel combination of different imaging techniques enables us to distinguish the movements of the solvent and fluorescent molecules. Additionally, the swelling or deswelling of the hydrogels can be monitored. From the sequence of images, dye and solvent concentrations were extracted spatially and temporally resolved. Diffusion equations and different boundary conditions, represented by different models, were used to quantitatively analyze the temporal evolution of these concentration profiles and to determine the diffusion coefficients of solvent andmore » solutes. Solute size and network properties were varied and their effect was investigated. Increasing the crosslinking ratio or partially drying the hydrogel was found to hinder solute diffusion due to the reduced pore size. By contrast, solvent diffusion seemed to be slightly faster if the hydrogel was only partially swollen and hence solvent uptake enhanced.« less

In-syringe demulsified dispersive liquid-liquid microextraction and high performance liquid chromatography-mass spectrometry for the determination of trace fungicides in environmental water samples.

PubMed

Xia, Yating; Cheng, Min; Guo, Feng; Wang, Xiangfang; Cheng, Jing

2012-04-29

An in-syringe demulsified dispersive liquid-liquid microextraction (ISD-DLLME) technique was developed using low-density extraction solvents for the highly sensitive determination of the three trace fungicides (azoxystrobin, diethofencarb and pyrimethanil) in water samples by high performance liquid chromatography-mass spectrometry chromatography-diode array detector/electrospray ionisation mass spectrometry. In the proposed technique, a 5-mL syringe was used as an extraction, separation and preconcentration container. The emulsion was obtained after the mixture of toluene (extraction solvent) and methanol (dispersive solvent) was injected into the aqueous bulk of the syringe. The obtained emulsion cleared into two phases without centrifugation, when an aliquot of methanol was introduced as a demulsifier. The separated floating organic extraction solvent was impelled and collected into a pipette tip fitted to the tip of the syringe. Under the optimal conditions, the enrichment factors for azoxystrobin, diethofencarb and pyrimethanil were 239, 200, 195, respectively. The limits of detection, calculated as three times the signal-to-noise ratio (SN(-1)), were 0.026 μg L(-1) for azoxystrobin, 0.071 μg L(-1) for diethofencarb and 0.040 μg L(-1) for pyrimethanil. The repeatability study was carried out by extracting the spiked water samples at concentration levels of 0.02 μg mL(-1) for all the three fungicides. The relative standard deviations varied between 4.9 and 8.2% (n=5). The recoveries of all the three fungicides from tap, lake and rain water samples at spiking levels of 0.2, 1, 5 μg L(-1) were in the range of 90.0-105.0%, 86.0-114.0% and 88.6-110.0%, respectively. The proposed ISD-DLLME technique was demonstrated to be simple, practical and efficient for the determination of different kinds of fungicide residues in real water samples. Copyright © 2012. Published by Elsevier B.V.

Extraction and preconcentration of residual solvents in pharmaceuticals using dynamic headspace-liquid phase microextraction and their determination by gas chromatography-flame ionization detection.

PubMed

Farajzadeh, Mir Ali; Dehghani, Hamideh; Yadeghari, Adeleh; Khoshmaram, Leila

2017-02-01

The present study describes a microextraction and determination method for analyzing residual solvents in pharmaceutical products using dynamic headspace-liquid phase microextraction technique followed by gas chromatography-flame ionization detection. In this method dimethyl sulfoxide (μL level) placed into a GC liner-shaped extraction vessel is used as a collection/extraction solvent. Then the liner is exposed to the headspace of a vial containing the sample solution. The effect of different parameters influencing the microextraction procedure including collection/extraction solvent type and its volume, ionic strength, extraction time, extraction temperature and concentration of NaOH solution used in dissolving the studied pharmaceuticals are investigated and optimized. Under the optimum extraction conditions, the method showed wide linear ranges between 0.5 and 5000 mg L -1 . The other analytical parameters were obtained in the following ranges: enrichment factors 240-327, extraction recoveries 72-98% and limits of detection 0.1-0.8 mg L -1 in solution and 0.6-3.2 μg g -1 in solid. Relative standard deviations for the extraction of 100 mg L -1 of each analyte were obtained in the ranges of 4-7 and 5-8% for intra-day (n = 6) and inter-day (n = 4) respectively. Finally the target analytes were determined in different samples such as erythromycin, azithromycin, cefalexin, amoxicillin and co-amoxiclav by the proposed method. Copyright © 2016 John Wiley & Sons, Ltd.

Total lipid extraction of homogenized and intact lean fish muscles using pressurized fluid extraction and batch extraction techniques.

PubMed

Isaac, Giorgis; Waldebäck, Monica; Eriksson, Ulla; Odham, Göran; Markides, Karin E

2005-07-13

The reliability and efficiency of pressurized fluid extraction (PFE) technique for the extraction of total lipid content from cod and the effect of sample treatment on the extraction efficiency have been evaluated. The results were compared with two liquid-liquid extraction methods, traditional and modified methods according to Jensen. Optimum conditions were found to be with 2-propanol/n-hexane (65:35, v/v) as a first and n-hexane/diethyl ether (90:10, v/v) as a second solvent, 115 degrees C, and 10 min of static time. PFE extracts were cleaned up using the same procedure as in the methods according to Jensen. When total lipid yields obtained from homogenized cod muscle using PFE were compared yields obtained with original and modified Jensen methods, PFE gave significantly higher yields, approximately 10% higher (t test, P < 0.05). Infrared and NMR spectroscopy suggested that the additional material that inflates the gravimetric results is rather homogeneous and is primarily consists of phospholipid with headgroups of inositidic and/or glycosidic nature. The comparative study demonstrated that PFE is an alternative suitable technique to extract total lipid content from homogenized cod (lean fish) and herring (fat fish) muscle showing a precision comparable to that obtained with the traditional and modified Jensen methods. Despite the necessary cleanup step, PFE showed important advantages in the solvent consumption was cut by approximately 50% and automated extraction was possible.

MICROWAVE-ASSISTED EXTRACTION OF ORGANIC COMPOUNDS FROM STANDARD REFERENCE SOILS AND SEDIMENTS

EPA Science Inventory

As part of an ongoing evaluation of new sample preparation techniques by the U.S. Environmental Protection Agency (EPA), especially those that minimize waste solvents, microwave-assisted extraction (MAE) of organic compounds from solid materials (or "matrices") was evaluated. Six...

Ionic liquid-based ultrasonic/microwave-assisted extraction combined with UPLC-MS-MS for the determination of tannins in Galla chinensis.

PubMed

Lu, Chunxia; Wang, Hongxin; Lv, Wenping; Ma, Chaoyang; Lou, Zaixiang; Xie, Jun; Liu, Bo

2012-01-01

Ionic liquid was used as extraction solvents and applied to the extraction of tannins from Galla chinensis in the simultaneous ultrasonic- and microwave-assisted extraction (UMAE) technique. Several parameters of UMAE were optimised, and the results were compared with of the conventional extraction techniques. Under optimal conditions, the content of tannins was 630.2 ± 12.1 mg g⁻¹. Compared with the conventional heat-reflux extraction, maceration extraction, regular ultrasound- and microwave-assisted extraction, the proposed approach exhibited higher efficiency (11.7-22.0% enhanced) and shorter extraction time (from 6 h to 1 min). The tannins were then identified by ultraperformance liquid chromatography tandem mass spectrometry. This study suggests that ionic liquid-based UMAE is an efficient, rapid, simple and green sample preparation technique.

Effect of three extraction techniques on submitochondrial particle and Microtox bioassays for airborne particulate matter.

PubMed

Torres-Pérez, Mónica I; Jiménez-Velez, Braulio D; Mansilla-Rivera, Imar; Rodríguez-Sierra, Carlos J

2005-03-01

The effect that three extraction techniques (e.g., Soxhlet, ultrasound and microwave-assisted extraction) have on the toxicity, as measured by submitochondrial particle (SMP) and Microtox assays, of organic extracts was compared from three sources of airborne particulate matter (APM). The extraction technique influenced the toxicity response of APM extracts and it was dependent on the bioassay method, and APM sample source. APM extracts from microwave-assisted extraction (MAE) were similar or more toxic than the conventional extraction techniques of Soxhlet and ultrasound, thus, providing an alternate extraction method. The microwave extraction technique has the advantage of using less solvent volume, less extraction time, and the capacity to simultaneously extract twelve samples. The ordering of APM toxicity was generally urban dust > diesel dust > PM10 (particles with diameter < 10 microm), thus, reflecting different chemical composition of the samples. This study is the first to report the suitability of two standard in-vitro bioassays for the future toxicological characterization of APM collected from Puerto Rico, with the SMP generally showing better sensitivity to the well-known Microtox bioassay.

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

PubMed

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

2015-04-01

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

Supercritical fluid extraction and processing of foods

USDA-ARS?s Scientific Manuscript database

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

Gas flow headspace liquid phase microextraction.

PubMed

Yang, Cui; Qiu, Jinxue; Ren, Chunyan; Piao, Xiangfan; Li, Xifeng; Wu, Xue; Li, Donghao

2009-11-06

There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

Use of Innovative (Micro)Extraction Techniques to Characterise Harpagophytum procumbens Root and its Commercial Food Supplements.

PubMed

Diuzheva, Alina; Carradori, Simone; Andruch, Vasil; Locatelli, Marcello; De Luca, Elisa; Tiecco, Matteo; Germani, Raimondo; Menghini, Luigi; Nocentini, Alessio; Gratteri, Paola; Campestre, Cristina

2018-05-01

For the determination of harpagoside and the wide phenolic pattern in Harpagophytum procumbens root and its commercial food supplements, dispersive liquid-liquid microextraction (DLLME), ultrasound-assisted DLLME (UA-DLLME), and sugaring-out liquid-liquid extraction (SULLE) were tested and compared. In order to optimise the extraction efficiency, DLLME and UA-DLLME were performed in different solvents (water and aqueous solutions of glucose, β-cyclodextrin, (2-hydroxypropyl)-β-cyclodextrin, sodium chloride, natural deep eutectic solvent, and ionic liquid). The plant material was ground and sieved to obtain a uniform granulometry before extraction. Commercial food supplements, containing H. procumbens are commercially available in Italy. The most effective sodium chloride-aided-DLLME was then optimised and applied for analyses followed by HPLC-PDA. For comparison, microwave-assisted extraction was performed using the same solvents and the best results were obtained using 1% of β-cyclodextrin or 15% of sodium chloride. All commercial samples respected the European Pharmacopoeia monograph for this plant material, showing a harpagoside content ≥ 1.2%. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Screening of Indian Lingzhi or Reishi Medicinal Mushroom, Ganoderma lucidum (Agaricomycetes): A UPC2-SQD-MS Approach.

PubMed

Bhardwaj, Anuja; Srivastava, Mousami; Pal, Mamta; Sharma, Yogesh Kumar; Bhattacharya, Saikat; Tulsawani, Rajkumar; Sugadev, Ragumani; Misra, Kshipra

2016-01-01

Oriental medicinal mushroom Ganoderma lucidum has been widely used for the promotion of health and longevity owing to its various bioactive constituents. Therefore, comprehending metabolomics of different G. lucidum parts could be of paramount importance for investigating their pharmacological properties. Ultra-performance convergence chromatography (UPC2) along with mass spectrometry (MS) is an emerging technique that has not yet been applied for metabolite profiling of G. lucidum. This study has been undertaken to establish metabolomics of the aqueous extracts of mycelium (GLM), fruiting body (GLF), and their mixture (GLMF) using ultra-performance convergence chromatography single quadrupole mass spectrometry (UPC2-SQD-MS). Aqueous extracts of G. lucidum prepared using an accelerated solvent extraction technique have been characterized for their mycochemical activities in terms of total flavonoid content, 1,1-diphenyl-2-picryl-hydrazyl scavenging activity, and ferric ion reducing antioxidant power. The UPC2-SQD-MS technique has been used for the first time for metabolite profiling of G. lucidum on a Princeton Diol column (4.6 × 250 mm; 5 µm) using supercritical CO2 (solvent) and 20 mM ammonium acetate in methanol (co-solvent). In the present study, UPC2-SQD-MS was found to be a rapid, efficient, and high-throughput analytical technique, whose coupling to principal component analysis (PCA) and phytochemical evaluation could be used as a powerful tool for elucidating metabolite diversity between mycelium and fruiting body of G. lucidum. PCA showed a clear distinction in the metabolite compositions of the samples. Mycochemical studies revealed that overall GLF possessed better antioxidant properties among the aqueous extracts of G. lucidum.

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

PubMed

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

2017-02-01

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

Extraction, isolation, and aromatase inhibitory evaluation of low-polar ginsenosides from Panax ginseng leaves.

PubMed

Zhang, Yuchi; Zhang, Jianxu; Liu, Chunming; Yu, Min; Li, Sainan

2017-02-03

A hyphenated accelerated solvent extraction (ASE) technique was elaborately coupled with centrifugal partition chromatography (CPC), ultra-high-performance liquid chromatography (UHPLC), and photo-diode array detector (PDA). This approach was applied to obtain low-polar ginsenoside fractions from the leaves of Panax ginseng. The CPC fractions were isolated and analyzed using the hyphenated technique, and followed by testing and evaluation of their aromatase inhibitory effects. Subsequently, the aromatase inhibition rates of the compositions in the CPC fractions were calculated using a multivariable linear regression model. A biphasic ethyl acetate/n-butanol/ethanol/water solvent system with respective volume ratios of 10:2:2:8 was used for the ASE and CPC separation of 200g of leaves of P. ginseng raw material. The (lower) aqueous phase of the abovementioned solvent system was used as the extraction solvent. The ginsenosides were subjected to ASE, and the extraction solution was pumped into the sample loop and then directly into the CPC column. The CPC fractions were collected and monitored by an online UHPLC/PDA system at 5-min intervals. The aromatase inhibitory activities of CPC fractions were analyzed by a fluorescence method, with mathematical calculations indicating that the inhibition rates of ginsenosides Rk 1 , Rg 5 , Rs 5 , 20R-Rg 3 , and Rs 4 exceeded 50.00%; indicating that the aforementioned chemical compounds have potential for further development. The results were validated by comparison with authentic standards, indicating that the method used in this research was accurate and advantageous for matrix analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Optimization of in-cell accelerated solvent extraction technique for the determination of organochlorine pesticides in river sediments.

PubMed

Duodu, Godfred Odame; Goonetilleke, Ashantha; Ayoko, Godwin A

2016-04-01

Organochlorine pesticides (OCPs) are ubiquitous environmental contaminants with adverse impacts on aquatic biota, wildlife and human health even at low concentrations. However, conventional methods for their determination in river sediments are resource intensive. This paper presents an approach that is rapid and also reliable for the detection of OCPs. Accelerated Solvent Extraction (ASE) with in-cell silica gel clean-up followed by Triple Quadrupole Gas Chromatograph Mass Spectrometry (GCMS/MS) was used to recover OCPs from sediment samples. Variables such as temperature, solvent ratio, adsorbent mass and extraction cycle were evaluated and optimized for the extraction. With the exception of Aldrin, which was unaffected by any of the variables evaluated, the recovery of OCPs from sediment samples was largely influenced by solvent ratio and adsorbent mass and, to some extent, the number of cycles and temperature. The optimized conditions for OCPs extraction in sediment with good recoveries were determined to be 4 cycles, 4.5 g of silica gel, 105 °C, and 4:3 v/v DCM: hexane mixture. With the exception of two compounds (α-BHC and Aldrin) whose recoveries were low (59.73 and 47.66% respectively), the recovery of the other pesticides were in the range 85.35-117.97% with precision <10% RSD. The method developed significantly reduces sample preparation time, the amount of solvent used, matrix interference, and is highly sensitive and selective. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of lutein from green tea and green tea by-products using accelerated solvent extraction and UPLC.

PubMed

Heo, Ji-Young; Kim, Suna; Kang, Jae-Hyun; Moon, Bokyung

2014-05-01

We aimed to identify the optimum conditions for the extraction of lutein from green tea using accelerated solvent extraction, and achieve improved analytical resolution and sensitivity between lutein and zeaxanthin using an ultra performance liquid chromatography (UPLC) system. The optimized method employed 80% ethanol as the extraction solvent, 160 °C as the temperature, 2 static cycles, and 5 min of static time. In the validation of the UPLC method, recovery was found to be in the range approximately 93.73 to 108.79%, with a correlation coefficient of 0.9974 and a relative standard deviation of <9.29% in inter- and intraday precision analyses. Finally, the lutein contents of green tea and green tea by-products were measured as 32.67 ± 0.70 and 18.18 ± 0.68 mg/100g dw, respectively. Furthermore, we verified that green tea by-products, which are discarded after producing green tea beverages, might be used as a great resource for massive lutein production. We have demonstrated that the common problem of inadequate resolution between lutein and zeaxanthin during carotenoid analyses can be overcome by optimizing the combined techniques of accelerated solvent extraction and ultra performance liquid chromatography (UPLC). UPLC was highly effective for saving time, solvent, and labor, as well as providing better resolution. The results in this study demonstrated that green tea by-products could be used as new sources for industrial lutein production owing to their massive production during the extraction of green tea beverages. © 2014 Institute of Food Technologists®

Isolation and Analysis of Essential Oils from Spices

ERIC Educational Resources Information Center

O'Shea, Stephen K.; Von Riesen, Daniel D.; Rossi, Lauren L.

2012-01-01

Natural product isolation and analysis provide an opportunity to present a variety of experimental techniques to undergraduate students in introductory organic chemistry. Eugenol, anethole, and carvone were extracted from six common spices using steam-distillation and diethyl ether as the extraction solvent. Students assessed the purity of their…

Central composite rotatable design for investigation of microwave-assisted extraction of ginger (Zingiber officinale)

NASA Astrophysics Data System (ADS)

Fadzilah, R. Hanum; Sobhana, B. Arianto; Mahfud, M.

2015-12-01

Microwave-assisted extraction technique was employed to extract essential oil from ginger. The optimal condition for microwave assisted extraction of ginger were determined by resposnse surface methodology. A central composite rotatable design was applied to evaluate the effects of three independent variables. The variables is were microwave power 400 - 800W as X1, feed solvent ratio of 0.33 -0.467 as X2 and feed size 1 cm, 0.25 cm and less than 0.2 cm as X3. The correlation analysis of mathematical modelling indicated that quadratic polynomial could be employed to optimize microwave assisted extraction of ginger. The optimal conditions to obtain highest yield of essential oil were : microwave power 597,163 W : feed solvent ratio and size of feed less than 0.2 cm.

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

PubMed

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

2007-12-01

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

Development of "ultrasound-assisted dynamic extraction" and its combination with CCC and CPC for simultaneous extraction and isolation of phytochemicals.

PubMed

Zhang, Yuchi; Liu, Chunming; Li, Jing; Qi, Yanjuan; Li, Yuchun; Li, Sainan

2015-09-01

A new method for the extraction of medicinal herbs termed ultrasonic-assisted dynamic extraction (UADE) was designed and evaluated. This technique was coupled with counter-current chromatography (CCC) and centrifugal partition chromatography (CPC) and then applied to the continuous extraction and online isolation of chemical constituents from Paeonia lactiflora Pall (white peony) roots. The mechanical parameters, including the pitch and diameter of the shaft, were optimized by means of mathematical modeling. Furthermore, the configuration and mechanism of online UADE coupled with CCC and CPC were elaborated. The stationary phases of the two-phase solvent systems from CCC and CPC were utilized as the UADE solution. The extraction solution was pumped into the sample loop and then introduced into the CCC column; the target compounds were eluted with the lower aqueous phase of the two-phase solvent system. During the CCC separation, the extraction solution was continuously fed in the sample loop by turning the ten-port valve; the extraction solution was then pumped into the CPC column and eluted by the mobile phase of the two-phase solvent system mentioned above. When the first cycle of the UADE/CCC/CPC was completed, the second cycle experiment could be carried out, and so on. Four target compounds (albiflorin, benzoylpaeoniflorin, paeoniflorin, and galloylpaeoniflorin) with purities above 94.96% were successfully extracted and isolated online using the two-phase solvent system comprising ethyl acetate-n-butanol-ethanol-water (1:3.5:2:4.5, v/v/v/v). Compared with conventional extraction methods, the instrumental setup of the present method offers the advantages of automation and systematic extraction and isolation of natural products. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

Determination of low methylmercury concentrations in peat soil samples by isotope dilution GC-ICP-MS using distillation and solvent extraction methods.

PubMed

Pietilä, Heidi; Perämäki, Paavo; Piispanen, Juha; Starr, Mike; Nieminen, Tiina; Kantola, Marjatta; Ukonmaanaho, Liisa

2015-04-01

Most often, only total mercury concentrations in soil samples are determined in environmental studies. However, the determination of extremely toxic methylmercury (MeHg) in addition to the total mercury is critical to understand the biogeochemistry of mercury in the environment. In this study, N2-assisted distillation and acidic KBr/CuSO4 solvent extraction methods were applied to isolate MeHg from wet peat soil samples collected from boreal forest catchments. Determination of MeHg was performed using a purge and trap GC-ICP-MS technique with a species-specific isotope dilution quantification. Distillation is known to be more prone to artificial MeHg formation compared to solvent extraction which may result in the erroneous MeHg results, especially with samples containing high amounts of inorganic mercury. However, methylation of inorganic mercury during the distillation step had no effect on the reliability of the final MeHg results when natural peat soil samples were distilled. MeHg concentrations determined in peat soil samples after distillation were compared to those determined after the solvent extraction method. MeHg concentrations in peat soil samples varied from 0.8 to 18 μg kg(-1) (dry weight) and the results obtained with the two different methods did not differ significantly (p=0.05). The distillation method with an isotope dilution GC-ICP-MS was shown to be a reliable method for the determination of low MeHg concentrations in unpolluted soil samples. Furthermore, the distillation method is solvent-free and less time-consuming and labor-intensive when compared to the solvent extraction method. Copyright © 2014 Elsevier Ltd. All rights reserved.

A comparative study of Averrhoabilimbi extraction method

NASA Astrophysics Data System (ADS)

Zulhaimi, H. I.; Rosli, I. R.; Kasim, K. F.; Akmal, H. Muhammad; Nuradibah, M. A.; Sam, S. T.

2017-09-01

In recent year, bioactive compound in plant has become a limelight in the food and pharmaceutical market, leading to research interest to implement effective technologies for extracting bioactive substance. Therefore, this study is focusing on extraction of Averrhoabilimbi by different extraction technique namely, maceration and ultrasound-assisted extraction. Fewplant partsof Averrhoabilimbiweretaken as extraction samples which are fruits, leaves and twig. Different solvents such as methanol, ethanol and distilled water were utilized in the process. Fruit extractsresult in highest extraction yield compared to other plant parts. Ethanol and distilled water have significant role compared to methanol in all parts and both extraction technique. The result also shows that ultrasound-assisted extraction gave comparable result with maceration. Besides, the shorter period on extraction process gives useful in term of implementation to industries.

Improved solvent-free microwave extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim.

PubMed

Wang, Ziming; Ding, Lan; Li, Tiechun; Zhou, Xin; Wang, Lu; Zhang, Hanqi; Liu, Li; Li, Ying; Liu, Zhihong; Wang, Hongju; Zeng, Hong; He, Hui

2006-01-13

Solvent-free microwave extraction (SFME) is a recently developed green technique which is performed in atmospheric conditions without adding any solvent or water. SFME has already been applied to extraction of essential oil from fresh plant materials or dried materials prior moistened. The essential oil is evaporated by the in situ water in the plant materials. In this paper, it was observed that an improved SFME, in which a kind of microwave absorption solid medium, such as carbonyl iron powders (CIP), was added and mixed with the sample, can be applied to extraction of essential oil from the dried plant materials without any pretreatment. Because the microwave absorption capacity of CIP is much better than that of water, the extraction time while using the improved SFME is no more than 30 min using a microwave power of 85 W. Compared to the conventional SFME, the advantages of improved SFME were to speed up the extraction rate and need no pretreatment. Improved SFME has been compared with conventional SFME, microwave-assisted hydrodistillation (MAHD) and conventional hydrodistillation (HD) for the extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim. By using GC-MS system the compositions of essential oil extracted by applying four kinds of extraction methods were identified. There was no obvious difference in the quality of essential oils obtained by the four kinds of extraction methods.

Comparison Pore Aggregate Levels After Extraction With Solvents Pertamax Plus And Gasoline

NASA Astrophysics Data System (ADS)

Anggraini, Muthia

2017-12-01

Loss of asphalt content extraction results become problems in Field Work For implementing parties. The use of solvents with high octane (pertamax plus) for the extraction, dissolving the asphalt more than gasoline. By comparing the levels of aggregate pores after using solvent extraction pertamax plus compared to gasoline could answer that pertamax plus more solvent dissolves the bitumen compared to gasoline. This study aims to obtain comparative levels of porous aggregate mix AC-WC after using solvent extraction pertamax plus compared to gasoline. This study uses the aggregate that has been extracted from the production of asphalt mixtures, when finisher and after compaction field. The method used is the assay of coarse and fine aggregate pores, extraction of bitumen content to separate the aggregate with bitumen. Results of testing the total absorption after extraction using a solvent preta max plus in the production of asphalt mixtures 0.80%, while gasoline solvent 0.67% deviation occurs 0.13%. In the finisher after the solvent extraction preta max plus 0.77%, while 0.67% gasoline solvent occurs deviation of 0.1%. At the core after extraction and solvent pertamax plus 0.71%, while gasoline solvent 0.60% 0.11% deviation occurs. The total water absorption after extraction using a solvent pertamax plus greater than gasoline. This proves that the solvent dissolves pertamax plus more asphalt than gasoline.

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

PubMed

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

2018-04-01

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

Comparison between several techniques of olive tree bark extraction (Tunisian Chemlali variety).

PubMed

Issaoui, Aimen; Ksibi, Hatem; Ksibi, Mohamed

2017-01-01

In order to better understand the chemical composition of the olive tree bark of Tunisian chemlali variety (Olea europaea cv. 'Chemlali'), this material was extracted by different ways. Compositions of extracts were used at best-selected conditions for each technique, and characterised using HPLC, LC/MS and GC-MS techniques. Analyses are conducted to an important variety of high carbon number compounds such as aliphatic compounds as nanocosane and heptacosane, and molecules with high value added tax (VAT) which can be classified as follows: diterpenes as phytol, triterpenes as squalene and also esters as Benzyl cinnamate. Hydrodistillation at high pressure seems to be a very common method to get a wide variety of compounds, the results are better than the ones obtained using supercritical fluid extraction and solvent extraction.

Evaluation of micro-colorimetric lipid determination method with samples prepared using sonication and accelerated solvent extraction methods

EPA Science Inventory

Two common laboratory extraction techniques were evaluated for routine use with the micro-colorimetric lipid determination method developed by Van Handel (1985) [E. Van Handel, J. Am. Mosq. Control Assoc. 1(1985) 302] and recently validated for small samples by Inouye and Lotufo ...

Optimization of antibacterial activity by Gold-Thread (Coptidis Rhizoma Franch) against Streptococcus mutans using evolutionary operation-factorial design technique.

PubMed

Choi, Ung-Kyu; Kim, Mi-Hyang; Lee, Nan-Hee

2007-11-01

This study was conducted to find the optimum extraction condition of Gold-Thread for antibacterial activity against Streptococcus mutans using The evolutionary operation-factorial design technique. Higher antibacterial activity was achieved in a higher extraction temperature (R2 = -0.79) and in a longer extraction time (R2 = -0.71). Antibacterial activity was not affected by differentiation of the ethanol concentration in the extraction solvent (R2 = -0.12). The maximum antibacterial activity of clove against S. mutans determined by the EVOP-factorial technique was obtained at 80 degrees C extraction temperature, 26 h extraction time, and 50% ethanol concentration. The population of S. mutans decreased from 6.110 logCFU/ml in the initial set to 4.125 logCFU/ml in the third set.

Ultrasound-assisted surfactant-enhanced emulsification microextraction based on the solidification of a floating organic droplet used for the simultaneous determination of six fungicide residues in juices and red wine.

PubMed

You, Xiangwei; Wang, Suli; Liu, Fengmao; Shi, Kaiwei

2013-07-26

A novel ultrasound-assisted surfactant-enhanced emulsification microextraction technique based on the solidification of a floating organic droplet followed by high performance liquid chromatography with diode array detection was developed for simultaneous determination of six fungicide residues in juices and red wine samples. The low-toxicity solvent, 1-dodecanol, was used as an extraction solvent. For its low density and proper melting point near room temperature, the extractant droplet was collected easily by solidifying it at a low temperature. The surfactant, Tween 80, was used as an emulsifier to enhance the dispersion of the water-immiscible extraction solvent into an aqueous phase, which hastened the mass-transfer of the analytes. Organic dispersive solvent typically required in common dispersive liquid-liquid microextraction methods was not used in the proposed method. Some parameters (e.g., the type and volume of extraction solvent, the type and concentration of surfactant, ultrasound extraction time, salt addition, and volume of samples) that affect the extraction efficiency were optimized. The proposed method showed a good linearity within the range of 5μgL(-1)-1000μgL(-1), with the correlation coefficients (γ) higher than 0.9969. The limits of detection for the method ranged from 0.4μgL(-1) to 1.4μgL(-1). Further, this simple, practical, sensitive, and environmentally friendly method was successfully applied to determine the target fungicides in juice and red wine samples. The recoveries of the target fungicides in red wine and fruit juice samples were 79.5%-113.4%, with relative standard deviations that ranged from 0.4% to 12.3%. Copyright © 2013 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Box-Behnken design for investigation of microwave-assisted extraction of patchouli oil

NASA Astrophysics Data System (ADS)

Kusuma, Heri Septya; Mahfud, Mahfud

2015-12-01

Microwave-assisted extraction (MAE) technique was employed to extract the essential oil from patchouli (Pogostemon cablin). The optimal conditions for microwave-assisted extraction of patchouli oil were determined by response surface methodology. A Box-Behnken design (BBD) was applied to evaluate the effects of three independent variables (microwave power (A: 400-800 W), plant material to solvent ratio (B: 0.10-0.20 g mL-1) and extraction time (C: 20-60 min)) on the extraction yield of patchouli oil. The correlation analysis of the mathematical-regression model indicated that quadratic polynomial model could be employed to optimize the microwave extraction of patchouli oil. The optimal extraction conditions of patchouli oil was microwave power 634.024 W, plant material to solvent ratio 0.147648 g ml-1 and extraction time 51.6174 min. The maximum patchouli oil yield was 2.80516% under these optimal conditions. Under the extraction condition, the experimental values agreed with the predicted results by analysis of variance. It indicated high fitness of the model used and the success of response surface methodology for optimizing and reflect the expected extraction condition.

Rapid determination of caffeine in one drop of beverages and foods using drop-to-drop solvent microextraction with gas chromatography/mass spectrometry.

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2007-11-02

A simple and rapid sample cleanup and preconcentration method for the quantitative determination of caffeine in one drop of beverages and foods by gas chromatography/mass spectrometry (GC/MS) has been proposed using drop-to-drop solvent microextraction (DDSME). The best optimum experimental conditions for DDSME were: chloroform as the extraction solvent, 5 min extraction time, 0.5 microL exposure volume of the extraction phase and no salt addition at room temperature. The optimized methodology exhibited good linearity between 0.05 and 5.0 microg/mL with correlation coefficient of 0.980. The relative standard deviation (RSD) and limits of detection (LOD) of the DDSME/GC/MS method were 4.4% and 4.0 ng/mL, respectively. Relative recovery of caffeine in beverages and foods were found to be 96.6-101%, which showing good reliability of this method. This DDSME excludes the major disadvantages of conventional method of caffeine extraction, like large amount of organic solvent and sample consumption and long sample pre-treatment process. So, this approach proves that the DDSME/GC/MS technique can be applied as a simple, fast and feasible diagnosis tool for environmental, food and biological application for extremely small amount of real sample analysis.

Determination of Microalgal Lipid Content and Fatty Acid for Biofuel Production

PubMed Central

Chen, Zhipeng; Wang, Lingfeng

2018-01-01

Biofuels produced from microalgal biomass have received growing worldwide recognition as promising alternatives to conventional petroleum-derived fuels. Among the processes involved, the downstream refinement process for the extraction of lipids from biomass greatly influences the sustainability and efficiency of the entire biofuel system. This review summarizes and compares the current techniques for the extraction and measurement of microalgal lipids, including the gravimetric methods using organic solvents, CO2-based solvents, ionic liquids and switchable solvents, Nile red lipid visualization method, sulfo-phospho-vanillin method, and the thin-layer chromatography method. Each method has its own competitive advantages and disadvantages. For example, the organic solvents-based gravimetric method is mostly used and frequently employed as a reference standard to validate other methods, but it requires large amounts of samples and is time-consuming and expensive to recover solvents also with low selectivity towards desired products. The pretreatment approaches which aimed to disrupt cells and support subsequent lipid extraction through bead beating, microwave, ultrasonication, chemical methods, and enzymatic disruption are also introduced. Moreover, the principles and procedures for the production and quantification of fatty acids are finally described in detail, involving the preparation of fatty acid methyl esters and their quantification and composition analysis by gas chromatography.

Supercritical Fluid Extraction of Biogenic SOA in Northern Michigan

NASA Astrophysics Data System (ADS)

Flores, R. M.; Doskey, P. V.; Perlinger, J. A.

2010-12-01

Secondary organic aerosols (SOA) are formed by photooxidation of volatile organic compounds (VOCs) and nucleation and condensation of the oxygenated products. On a global scale, monoaromatic hydrocarbons of anthropogenic origin are estimated to be the source of 12% of the SOA while biogenic emissions of isoprene (C5H8), monoterpenes (C10H16), and sesquiterpenes (C15H24) are estimated to be the source of 46, 29 and 7% of SOA, respectively. The functional groups of organic substances comprising SOA (i.e., hydroxyl, carbonyl, carboxylic acid, sulfate, and nitrate) complicate sample processing, analysis, and identification of the characteristic aerosol products of VOC oxidation pathways. Only a very small fraction of the organic molecular species in SOA have been identified due to the complexity of precursor oxidation reactions and the need for (1) methodologies that are less labor intensive and suitable for thermally labile compounds and (2) analytic instrumentation that provides more complete resolution of complex mixtures for sensitive detection of molecular species. Extraction techniques commonly used include solvent extraction, which requires large amounts of solvent and is labor intensive and thermal desorption, which evolves organic substances from aerosol at temperatures not suitable for thermally labile compounds. A promising technique that does not involve sample processing with solvents or high temperatures is supercritical fluid extraction (SFE). In this work, the composition of biogenic SOA was studied in Northern Michigan. Aerosol samples were collected on quartz fiber filters with a high-volume air sampler and extracted with supercritical CO2. Carboxylic and hydroxyl compounds were derivatized during static extraction conditions and identified by comprehensive two dimensional gas chromatography with time-of-flight mass spectrometric detection (GC×GC-TOFMS). The overall goal of the research is to couple the post-collection analytic scheme developed here with a rapid sampling technique to evaluate SOA produced from a variety of biogenic and anthropogenic sources of precursors in the Midwestern United States.

A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

PubMed

Kahe, Hadi; Chamsaz, Mahmoud

2016-11-01

A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L -1 Bi (III) with a limit of detection (LOD) of 0.16 μg L -1 (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L -1 of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

Applications of derivatization reactions to trace organic compounds during sample preparation based on pressurized liquid extraction.

PubMed

Carro, Antonia M; González, Paula; Lorenzo, Rosa A

2013-06-28

Pressurized liquid extraction (PLE) is an exhaustive technique used for the extraction of analytes from solid samples. Temperature, pressure, solvent type and volume, and the addition of other reagents notably influence the efficiency of the extraction. The analytical applications of this technique can be improved by coupling with appropriate derivatization reactions. The aim of this review is to discuss the recent applications of the sequential combination of PLE with derivatization and the approaches that involve simultaneous extraction and in situ derivatization. The potential of the latest developments to the trace analysis of environmental, food and biological samples is also analyzed. Copyright © 2013 Elsevier B.V. All rights reserved.

Conversion and Extraction of Insoluble Organic Materials in Meteorites

NASA Technical Reports Server (NTRS)

Locke, Darren R.; Burton, Aaron S.; Niles, Paul B.

2016-01-01

We endeavor to develop and implement methods in our laboratory to convert and extract insoluble organic materials (IOM) from low car-bon bearing meteorites (such as ordinary chondrites) and Precambrian terrestrial rocks for the purpose of determining IOM structure and prebiotic chemistries preserved in these types of samples. The general scheme of converting and extracting IOM in samples is summarized in Figure 1. First, powdered samples are solvent extracted in a micro-Soxhlet apparatus multiple times using solvents ranging from non-polar to polar (hexane - non-polar, dichloromethane - non-polar to polar, methanol - polar protic, and acetonitrile - polar aprotic). Second, solid residue from solvent extractions is processed using strong acids, hydrochloric and hydrofluoric, to dissolve minerals and isolate IOM. Third, the isolated IOM is subjected to both thermal (pyrolysis) and chemical (oxidation) degradation to release compounds from the macromolecular material. Finally, products from oxidation and pyrolysis are analyzed by gas chromatography - mass spectrometry (GCMS). We are working toward an integrated method and analysis scheme that will allow us to determine prebiotic chemistries in ordinary chondrites and Precambrian terrestrial rocks. Powerful techniques that we are including are stepwise, flash, and gradual pyrolysis and ruthenium tetroxide oxidation. More details of the integrated scheme will be presented.

Lipid Extraction Techniques for Stable Isotope Analysis and Ecological Assays.

PubMed

Elliott, Kyle H; Roth, James D; Crook, Kevin

2017-01-01

Lipid extraction is an important component of many ecological and ecotoxicological measurements. For instance, percent lipid is often used as a measure of body condition, under the assumption that those individuals with higher lipid reserves are healthier. Likewise, lipids are depleted in 13 C compared with protein, and it is consequently a routine to remove lipids prior to measuring carbon isotopes in ecological studies so that variation in lipid content does not obscure variation in diet. We provide detailed methods for two different protocols for lipid extraction: Soxhlet apparatus and manual distillation. We also provide methods for polar and nonpolar solvents. Neutral (nonpolar) solvents remove some lipids but few non-lipid compounds, whereas polar solvents remove most lipids but also many non-lipid compounds. We discuss each of the methods and provide guidelines for best practices. We recommend that, for stable isotope analysis, researchers test for a relationship between the change in carbon stable isotope ratio and the amount of lipid extracted to see if the degree of extraction has an impact on isotope ratios. Stable isotope analysis is widely used by ecologists, and we provide a detailed methodology that minimizes known biases.

Ultrasound assisted extraction of food and natural products. Mechanisms, techniques, combinations, protocols and applications. A review.

PubMed

Chemat, Farid; Rombaut, Natacha; Sicaire, Anne-Gaëlle; Meullemiestre, Alice; Fabiano-Tixier, Anne-Sylvie; Abert-Vian, Maryline

2017-01-01

This review presents a complete picture of current knowledge on ultrasound-assisted extraction (UAE) in food ingredients and products, nutraceutics, cosmetic, pharmaceutical and bioenergy applications. It provides the necessary theoretical background and some details about extraction by ultrasound, the techniques and their combinations, the mechanisms (fragmentation, erosion, capillarity, detexturation, and sonoporation), applications from laboratory to industry, security, and environmental impacts. In addition, the ultrasound extraction procedures and the important parameters influencing its performance are also included, together with the advantages and the drawbacks of each UAE techniques. Ultrasound-assisted extraction is a research topic, which affects several fields of modern plant-based chemistry. All the reported applications have shown that ultrasound-assisted extraction is a green and economically viable alternative to conventional techniques for food and natural products. The main benefits are decrease of extraction and processing time, the amount of energy and solvents used, unit operations, and CO 2 emissions. Copyright © 2016 Elsevier B.V. All rights reserved.

Application of non-ionic surfactant as a developed method for the enhancement of two-phase solvent bar microextraction for the simultaneous determination of three phthalate esters from water samples.

PubMed

Bandforuzi, Samereh Ranjbar; Hadjmohammadi, Mohammad Reza

2018-08-03

The extraction of phthalate esters (PEs) from aqueous matrices using two-phase solvent bar microextraction by organic micellar phase was investigated. A short hollow fiber immobilized with reverse micelles of Brij 35 surfactant in 1-octanol was served as the solvent bar for microextraction. Experimental results show that the extraction efficiency were much higher using two-phase solvent bar microextraction based on non-ionic surfactant than conventional two-phase solvent bar microextraction because of a positive effect of surfactant-containing extraction phase in promoting the partition process by non-ionic intermolecular forces such as polar and hydrophobicity interactions. The nature of the extraction solvent, type and concentration of non-ionic surfactant, extraction time, sample pH, temperature, stirring rate and ionic strength were the effecting parameters which optimized to obtain the highest extraction recovery. Analysis of recovered analytes was carried out with high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV). Under the optimum conditions, linearity was observed in the range of 1-800 ng mL -1 for dimethylphthalate (DMP) and 0.5-800 ng mL -1 for diethylphthalate (DEP) and di-n-butyl phthalate (DBP) with correlation determination values above 0.99 for them. The limits of detection and quantification were ranged from 0.012 to 0.03 ng mL -1 and 0.04-0.1 ng mL -1 , respectively. The ranges of intra-day and inter-day RSD (n = 3) at 20 ng mL -1 of PEs were 1.8-2.1% and 2.1-2.6%, respectively. Results showed that developed method can be a very powerful, innovative and promising sample preparation technique in PEs analysis from environmental and drinking water samples. Copyright © 2018. Published by Elsevier B.V.

Extrusion of xylans extracted from corn cobs into biodegradable polymeric materials.

PubMed

Bahcegul, Erinc; Akinalan, Busra; Toraman, Hilal E; Erdemir, Duygu; Ozkan, Necati; Bakir, Ufuk

2013-12-01

Solvent casting technique, which comprises multiple energy demanding steps including the dissolution of a polymer in a solvent followed by the evaporation of the solvent from the polymer solution, is currently the main technique for the production of xylan based polymeric materials. The present study shows that sufficient water content renders arabinoglucuronoxylan (AGX) polymers extrudable, enabling the production of AGX based polymeric materials in a single step via extrusion, which is economically advantageous to solvent casting process for mass production. AGX polymers with water content of 27% were found to yield extrudates at an extrusion temperature of 90°C. The extruded strips showed very good mechanical properties with an ultimate tensile strength of 76 ± 6 MPa and elongation at break value of 35 ± 8%, which were superior to the mechanical properties of the strips obtained from polylactic acid. Copyright © 2013 Elsevier Ltd. All rights reserved.

Polyphenolic Content, Antioxidant and Antimicrobial Activities of Vernonia mespilifolia Less. Used in Folk Medicine in the Eastern Cape Province, South Africa

PubMed Central

Afolayan, Anthony Jide

2018-01-01

Vernonia mespilifolia Less. is a shrub of the Asteraceae family used in the South African traditional medicine system for the management of weight loss, hypertension, and heartwater disease. There is a need for scientific evaluation to validate its ethnomedicinal usage. In vitro assays were conducted to evaluate the polyphenolic content, antioxidant and antimicrobial properties of different solvent extracts (acetone, aqueous, and ethanol) of the whole plant of Vernonia mespilifolia spectrophotometric and agar dilution techniques, respectively. The result revealed varying amounts of polyphenolics in the different solvent extracts corresponding to the antioxidant activities. Also, only the acetone and ethanol extracts inhibited the growth of the selected bacteria and fungi. These findings reveal that the extracts have strong bioactive compounds and hence support its ethnomedicinal application. PMID:29756461

Extraction and isotopic analysis of medium molecular weight hydrocarbons from Murchison using supercritical carbon dioxide

NASA Technical Reports Server (NTRS)

Gilmour, Iain; Pillinger, Colin

1993-01-01

The large variety of organic compounds present in carbonaceous chondrites poses particular problems in their analysis not the least of which is terrestrial contamination. Conventional analytical approaches employ simple chromatographic techniques to fractionate the extractable compounds into broad classes of similar chemical structure. However, the use of organic solvents and their subsequent removal by evaporation results in the depletion or loss of semi-volatile compounds as well as requiring considerable preparative work to assure solvent purity. Supercritical fluids have been shown to provide a powerful alternative to conventional liquid organic solvents used for analytical extractions. A sample of Murchison from the Field Museum was analyzed. Two interior fragments were used; the first (2.85 g) was crushed in an agate pestel and mortar to a grain size of ca. 50-100 micron, the second (1.80 g) was broken into chips 3-8 mm in size. Each sample was loaded into a stainless steel bomb and placed in the extraction chamber of an Isco supercritical fluid extractor maintained at 35 C. High purity (99.9995 percent) carbon dioxide was used and was pressurized using an Isco syringe pump. The samples were extracted dynamically by flowing CO2 under pressure through the bomb and venting via a 50 micron fused filica capillary into 5 mls of hexane used as a collection solvent. The hexane was maintained at a temperature of 0.5 C. A series of extractions were done on each sample using CO2 of increasing density. The principal components extracted in each fraction are summarized.

Extraction and isotopic analysis of medium molecular weight hydrocarbons from Murchison using supercritical carbon dioxide

NASA Astrophysics Data System (ADS)

Gilmour, Iain; Pillinger, Colin

1993-03-01

The large variety of organic compounds present in carbonaceous chondrites poses particular problems in their analysis not the least of which is terrestrial contamination. Conventional analytical approaches employ simple chromatographic techniques to fractionate the extractable compounds into broad classes of similar chemical structure. However, the use of organic solvents and their subsequent removal by evaporation results in the depletion or loss of semi-volatile compounds as well as requiring considerable preparative work to assure solvent purity. Supercritical fluids have been shown to provide a powerful alternative to conventional liquid organic solvents used for analytical extractions. A sample of Murchison from the Field Museum was analyzed. Two interior fragments were used; the first (2.85 g) was crushed in an agate pestel and mortar to a grain size of ca. 50-100 micron, the second (1.80 g) was broken into chips 3-8 mm in size. Each sample was loaded into a stainless steel bomb and placed in the extraction chamber of an Isco supercritical fluid extractor maintained at 35 C. High purity (99.9995 percent) carbon dioxide was used and was pressurized using an Isco syringe pump. The samples were extracted dynamically by flowing CO2 under pressure through the bomb and venting via a 50 micron fused filica capillary into 5 mls of hexane used as a collection solvent. The hexane was maintained at a temperature of 0.5 C. A series of extractions were done on each sample using CO2 of increasing density. The principal components extracted in each fraction are summarized.

A highly selective and sensitive ultrasonic assisted dispersive liquid phase microextraction based on deep eutectic solvent for determination of cadmium in food and water samples prior to electrothermal atomic absorption spectrometry.

PubMed

Zounr, Rizwan Ali; Tuzen, Mustafa; Deligonul, Nihal; Khuhawar, Muhammad Yar

2018-07-01

A simple, fast, green, sensitive and selective ultrasonic assisted deep eutectic solvent liquid-phase microextraction technique was used for preconcentration and extraction of cadmium (Cd) in water and food samples by electrothermal atomic absorption spectrometry (ETAAS). In this technique, a synthesized reagent (Z)-N-(3,5-diphenyl-1H-pyrrol-2-yl)-3,5-diphenyl-2H-pyrrol-2-imine (Azo) was used as a complexing agent for Cd. The main factors effecting the pre-concentration and extraction of Cd such as effect of pH, type and composition of deep eutectic solvent (DES), volume of DES, volume of complexing agent, volume of tetrahydrofuran (THF) and ultrasonication time have been examined in detail. At optimum conditions the value of pH and molar ratio of DES were found to be 6.0 and 1:4 (ChCl:Ph), respectively. The detection limit (LOD), limit of quantification (LOQ), relative standard deviation (RSD) and preconcentration factor (PF) were observed as 0.023 ng L -1 , 0.161 ng L -1 , 3.1% and 100, correspondingly. Validation of the developed technique was observed by extraction of Cd in certified reference materials (CRMs) and observed results were successfully compared with certified values. The developed procedure was practiced to various food, beverage and water samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

A microfluidic study of liquid-liquid extraction mediated by carbon dioxide.

PubMed

Lestari, Gabriella; Salari, Alinaghi; Abolhasani, Milad; Kumacheva, Eugenia

2016-07-05

Liquid-liquid extraction is an important separation and purification method; however, it faces a challenge in reducing the energy consumption and the environmental impact of solvent (extractant) recovery. The reversible chemical reactions of switchable solvents (nitrogenous bases) with carbon dioxide (CO2) can be implemented in reactive liquid-liquid extraction to significantly reduce the cost and energy requirements of solvent recovery. The development of new effective switchable solvents reacting with CO2 and the optimization of extraction conditions rely on the ability to evaluate and screen the performance of switchable solvents in extraction processes. We report a microfluidic strategy for time- and labour-efficient studies of CO2-mediated solvent extraction. The platform utilizes a liquid segment containing an aqueous extractant droplet and a droplet of a solution of a switchable solvent in a non-polar liquid, with gaseous CO2 supplied to the segment from both sides. Following the reaction of the switchable solvent with CO2, the solvent becomes hydrophilic and transfers from the non-polar solvent to the aqueous droplet. By monitoring the time-dependent variation in droplet volumes, we determined the efficiency and extraction time for the CO2-mediated extraction of different nitrogenous bases in a broad experimental parameter space. The platform enables a significant reduction in the amount of switchable solvents used in these studies, provides accurate temporal characterization of the liquid-liquid extraction process, and offers the capability of high-throughput screening of switchable solvents.

Antifouling booster biocide extraction from marine sediments: a fast and simple method based on vortex-assisted matrix solid-phase extraction.

PubMed

Caldas, Sergiane Souza; Soares, Bruno Meira; Abreu, Fiamma; Castro, Ítalo Braga; Fillmann, Gilberto; Primel, Ednei Gilberto

2018-03-01

This paper reports the development of an analytical method employing vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of diuron, Irgarol 1051, TCMTB (2-thiocyanomethylthiobenzothiazole), DCOIT (4,5-dichloro-2-n-octyl-3-(2H)-isothiazolin-3-one), and dichlofluanid from sediment samples. Separation and determination were performed by liquid chromatography tandem-mass spectrometry. Important MSPD parameters, such as sample mass, mass of C18, and type and volume of extraction solvent, were investigated by response surface methodology. Quantitative recoveries were obtained with 2.0 g of sediment sample, 0.25 g of C18 as the solid support, and 10 mL of methanol as the extraction solvent. The MSPD method was suitable for the extraction and determination of antifouling biocides in sediment samples, with recoveries between 61 and 103% and a relative standard deviation lower than 19%. Limits of quantification between 0.5 and 5 ng g -1 were obtained. Vortex-assisted MPSD was shown to be fast and easy to use, with the advantages of low cost and reduced solvent consumption compared to the commonly employed techniques for the extraction of booster biocides from sediment samples. Finally, the developed method was applied to real samples. Results revealed that the developed extraction method is effective and simple, thus allowing the determination of biocides in sediment samples.

Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

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

C.J. Miller; G. Elias; N.C. Schmitt

2010-06-01

High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to specifically identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol using no sample cleanup prior to analysis. The methanol extracts were injected directly into several different column types and analyzed by HPLC-UV and/or GC-ECD. This paper describes general screening methods that weremore » used to determine the presence of explosives in unknown samples and techniques that have been optimized for quantification of each explosive from the substrate extracts.« less

Integrated Stable Isotope - Reactive Transport Model Approach for Assessment of Chlorinated Solvent Degradation

DTIC Science & Technology

2016-05-01

Certification Program ETH Ethene GC Gas Chromatography GC-IRMS Gas Chromatography Isotope Ratio Mass Spectroscopy H Hydrogen IRMS Isotope...tool for attenuation of chlorinated solvents. The Demonstration Site was Operable Unit 10 at Hill AFB, Utah , a site where groundwater is impacted...techniques. The method involves extraction of the target compounds from environmental sample matrix, followed by separation of the compounds using gas

Distribution and uptake dynamics of mercury in leaves of common deciduous tree species in Minnesota, U.S.A.

Treesearch

Aicam Laacouri; Edward A. Nater; Randall K. Kolka

2013-01-01

A sequential extraction technique for compartmentalizing mercury (Hg) in leaves was developed based on a water extraction of Hg from the leaf surface followed by a solvent extraction of the cuticle. The bulk of leaf Hg was found in the tissue compartment (90-96%) with lesser amounts in the surface and cuticle compartments. Total leaf concentrations of Hg varied among...

Sensing cocaine in saliva with attenuated total reflection infrared (ATR-IR) spectroscopy combined with a one-step extraction method

NASA Astrophysics Data System (ADS)

Hans, Kerstin M.-C.; Gianella, Michele; Sigrist, Markus W.

2012-03-01

On-site drug tests have gained importance, e.g., for protecting the society from impaired drivers. Since today's drug tests are majorly only positive/negative, there is a great need for a reliable, portable and preferentially quantitative drug test. In the project IrSens we aim to bridge this gap with the development of an optical sensor platform based on infrared spectroscopy and focus on cocaine detection in saliva. We combine a one-step extraction method, a sample drying technique and infrared attenuated total reflection (ATR) spectroscopy. As a first step we have developed an extraction technique that allows us to extract cocaine from saliva to an almost infrared-transparent solvent and to record ATR spectra with a commercially available Fourier Transform-infrared spectrometer. To the best of our knowledge this is the first time that such a simple and easy-to-use one-step extraction method is used to transfer cocaine from saliva into an organic solvent and detect it quantitatively. With this new method we are able to reach a current limit of detection around 10 μg/ml. This new extraction method could also be applied to waste water monitoring and controlling caffeine content in beverages.

Process for removing halogenated aliphatic and aromatic compounds from petroleum products

DOEpatents

Googin, J.M.; Napier, J.M.; Travaglini, M.A.

1983-09-20

A process is described for removing halogenated aliphatic and aromatic compounds, e.g., polychlorinated biphenyls, from petroleum products by solvent extraction. The halogenated aliphatic and aromatic compounds are extracted from a petroleum product into a polar solvent by contacting the petroleum product with the polar solvent. The polar solvent is characterized by a high solubility for the extracted halogenated aliphatic and aromatic compounds, a low solubility for the petroleum product and considerable solvent power for polyhydroxy compound. The preferred polar solvent is dimethylformamide. A miscible compound, such as, water or a polyhydroxy compound, is added to the polar extraction solvent to increase the polarity of the polar extraction solvent. The halogenated aliphatic and aromatic compounds are extracted from the highly-polarized mixture of water or polyhydroxy compound and polar extraction solvent into a low polar or nonpolar solvent by contacting the water or polyhydroxy compound-polar solvent mixture with the low polar or nonpolar solvent. The halogenated aliphatic and aromatic compounds and the low polar or nonpolar solvent are separated by physical means, e.g., vacuum evaporation. The polar and nonpolar solvents are recovered from recycling. The process can easily be designed for continuous operation. Advantages of the process include that the polar solvent and a major portion of the nonpolar solvent can be recycled, the petroleum products are reclaimable and the cost for disposing of waste containing polychlorinated biphenyls is significantly reduced. 1 fig.

Process for removing halogenated aliphatic and aromatic compounds from petroleum products

DOEpatents

Googin, John M.; Napier, John M.; Travaglini, Michael A.

1983-01-01

A process for removing halogenated aliphatic and aromatic compounds, e.g., polychlorinated biphenyls, from petroleum products by solvent extraction. The halogenated aliphatic and aromatic compounds are extracted from a petroleum product into a polar solvent by contacting the petroleum product with the polar solvent. The polar solvent is characterized by a high solubility for the extracted halogenated aliphatic and aromatic compounds, a low solubility for the petroleum product and considerable solvent power for polyhydroxy compound. The preferred polar solvent is dimethylformamide. A miscible compound, such as, water or a polyhydroxy compound, is added to the polar extraction solvent to increase the polarity of the polar extraction solvent. The halogenated aliphatic and aromatic compounds are extracted from the highly-polarized mixture of water or polyhydroxy compound and polar extraction solvent into a low polar or nonpolar solvent by contacting the water or polyhydroxy compound-polar solvent mixture with the low polar or nonpolar solvent. The halogenated aliphatic and aromatic compounds and the low polar or nonpolar solvent are separated by physical means, e.g., vacuum evaporation. The polar and nonpolar solvents are recovered from recycling. The process can easily be designed for continuous operation. Advantages of the process include that the polar solvent and a major portion of the nonpolar solvent can be recycled, the petroleum products are reclaimable and the cost for disposing of waste containing polychlorinated biphenyls is significantly reduced.

Process for removing halogenated aliphatic and aromatic compounds from petroleum products. [Polychlorinated biphenyls; methylene chloride; perchloroethylene; trichlorofluoroethane; trichloroethylene; chlorobenzene

DOEpatents

Googin, J.M.; Napier, J.M.; Travaglini, M.A.

1982-03-31

A process for removing halogenated aliphatic and aromatic compounds, e.g., polychlorinated biphenyls, from petroleum products by solvent extraction. The halogenated aliphatic and aromatic compounds are extracted from a petroleum product into a polar solvent by contracting the petroleum product with the polar solvent. The polar solvent is characterized by a high solubility for the extracted halogenated aliphatic and aromatic compounds, a low solubility for the petroleum product and considerable solvent power for polyhydroxy compound. The preferred polar solvent is dimethylformamide. A miscible polyhydroxy compound, such as, water, is added to the polar extraction solvent to increase the polarity of the polar extraction solvent. The halogenated aliphatic and aromatic compounds are extracted from the highly-polarized mixture of polyhydroxy compound and polar extraction solvent into a low polar or nonpolar solvent by contacting the polyhydroxy compound-polar solvent mixture with the low polar or nonpolar solvent. The halogenated aliphatic and aromatic compounds in the low polar or nonpolar solvent by physical means, e.g., vacuum evaporation. The polar and nonpolar solvents are recovered for recycling. The process can easily be designed for continuous operation. Advantages of the process include that the polar solvent and a major portion of the nonpolar solvent can be recycled, the petroleum products are reclaimable and the cost for disposing of waste containing polychlorinated biphenyls is significantly reduced. 2 tables.

Development of a novel ultrasound-assisted headspace liquid-phase microextraction and its application to the analysis of chlorophenols in real aqueous samples.

PubMed

Xu, Hui; Liao, Ying; Yao, Jinrong

2007-10-05

A new sample pretreatment technique, ultrasound-assisted headspace liquid-phase microextraction was developed as mentioned in this paper. In the technique, the volatile analytes were headspace extracted into a small drop of solvent, which suspended on the bottom of a cone-shaped PCR tube instead of the needle tip of a microsyringe. More solvent could be suspended in the PCR tube than microsyringe due to the larger interfacial tension, thus the analysis sensitivity was significantly improved with the increase of the extractant volume. Moreover, ultrasound-assisted extraction and independent controlling temperature of the extractant and the sample were performed to enhance the extraction efficiency. Following the extraction, the solvent-loaded sample was analyzed by high-performance liquid chromatography. Chlorophenols (2-chlorophenol, 2,4-dichlorophenol and 2,6-dichlorophenol) were chosen as model analytes to investigate the feasibility of the method. The experimental conditions related to the extraction efficiency were systematically studied. Under the optimum experimental conditions, the detection limit (S/N=3), intra- and inter-day RSD were 6 ng mL(-1), 4.6%, 3.9% for 2-chlorophenol, 12 ng mL(-1), 2.4%, 8.8% for 2,4-dichlorophenol and 23 ng mL(-1), 3.3%, 5.3% for 2,6-dichlorophenol, respectively. The proposed method was successfully applied to determine chlorophenols in real aqueous samples. Good recoveries ranging from 84.6% to 100.7% were obtained. In addition, the extraction efficiency of our method and the conventional headspace liquid-phase microextraction were compared; the extraction efficiency of the former was about 21 times higher than that of the latter. The results demonstrated that the proposed method is a promising sample pretreatment approach, its advantages over the conventional headspace liquid-phase microextraction include simple setup, ease of operation, rapidness, sensitivity, precision and no cross-contamination. The method is very suitable for the analysis of trace volatile and semivolatile pollutants in real aqueous sample.

Supercritical fluid processing: opportunities for new resist materials and processes

NASA Astrophysics Data System (ADS)

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

1996-05-01

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

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

PubMed

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

2014-04-01

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

Solvent wash solution

DOEpatents

Neace, J.C.

1984-03-13

A process is claimed for removing diluent degradation products from a solvent extraction solution, which has been used to recover uranium and plutonium from spent nuclear fuel. A wash solution and the solvent extraction solution are combined. The wash solution contains (a) water and (b) up to about, and including, 50 vol % of at least one-polar water-miscible organic solvent based on the total volume of the water and the highly-polar organic solvent. The wash solution also preferably contains at least one inorganic salt. The diluent degradation products dissolve in the highly-polar organic solvent and the organic solvent extraction solvent do not dissolve in the highly-polar organic solvent. The highly-polar organic solvent and the extraction solvent are separated.

Solvent wash solution

DOEpatents

Neace, James C.

1986-01-01

Process for removing diluent degradation products from a solvent extraction solution, which has been used to recover uranium and plutonium from spent nuclear fuel. A wash solution and the solvent extraction solution are combined. The wash solution contains (a) water and (b) up to about, and including, 50 volume percent of at least one-polar water-miscible organic solvent based on the total volume of the water and the highly-polar organic solvent. The wash solution also preferably contains at least one inorganic salt. The diluent degradation products dissolve in the highly-polar organic solvent and the organic solvent extraction solvent do not dissolve in the highly-polar organic solvent. The highly-polar organic solvent and the extraction solvent are separated.

Histological techniques for study of photoreceptor orientation.

PubMed

Laties, A M

1969-01-01

An histological method for the study of photoreceptor orientation in primate eyes is described. To preserve photoreceptor orientation it is necessary to protect the fragile rod and cone outer segments to the maximum extent possible from mechanical deformation and from injury by solvent extraction. To prevent mechanical deformation the eyes are freeze-dried and embedded in plastic with or without prior vapor fixation. Solvent extraction from the lipid-rich outer segment is limited by avoidance or restriction of organic solvents. When large segments of primate eyes are so treated, it is possible to section the plastic blocks along the visual axis, polish the block surface, and view photoreceptor orientation by epi-illumination microscopy. In such specimens a differential orientation of photoreceptors exists with the long axis of photoreceptor inner and outer segments in line with incoming light rays.

Novel micronisation β-carotene using rapid expansion supercritical solution with co-solvent

NASA Astrophysics Data System (ADS)

Kien, Le Anh

2017-09-01

Rapid expansion of supercritical solution (RESS) is the most common approach of pharmaceutical pacticle forming methods using supercritical fluids. The RESS method is a technology producing a small solid product with a very narrow particle size distribution, organic solvent-free particles. This process is also simple and easy to control the operating parameters in comparision with other ways based on supercritical techniques. In this study, β-carotene, a strongly colored red-orange pigment abundant in plants and fruits, has been forming by RESS. In addition, the size and morphology effect of four different RESS parameters including co-solvent, extraction temperature, and extraction pressure and expansion nozzle temperature has surveyed. The particle size distribution has been determined by using laser diffraction experiment. SEM has conducted to analyze the surface structure, DSC and FTIR for thermal and chemical structure analysis.

Green analytical chemistry--theory and practice.

PubMed

Tobiszewski, Marek; Mechlińska, Agata; Namieśnik, Jacek

2010-08-01

This tutorial review summarises the current state of green analytical chemistry with special emphasis on environmentally friendly sample preparation techniques. Green analytical chemistry is a part of the sustainable development concept; its history and origins are described. Miniaturisation of analytical devices and shortening the time elapsing between performing analysis and obtaining reliable analytical results are important aspects of green analytical chemistry. Solventless extraction techniques, the application of alternative solvents and assisted extractions are considered to be the main approaches complying with green analytical chemistry principles.

NEPTUNIUM SOLVENT EXTRACTION PROCESS

DOEpatents

Dawson, L.R.; Fields, P.R.

1959-10-01

The separation of neptunium from an aqueous solution by solvent extraction and the extraction of neptunium from the solvent solution are described. Neptunium is separated from an aqueous solution containing tetravalent or hexavalent neptunium nitrate, nitric acid, and a nitrate salting out agent, such as sodium nitrate, by contacting the solution with an organic solvent such as diethyl ether. Subsequently, the neptunium nitrate is extracted from the organic solvent extract phase with water.

Measurement of dielectric constant of organic solvents by indigenously developed dielectric probe

NASA Astrophysics Data System (ADS)

Keshari, Ajay Kumar; Rao, J. Prabhakar; Rao, C. V. S. Brahmmananda; Ramakrishnan, R.; Ramanarayanan, R. R.

2018-04-01

The extraction, separation and purification of actinides (uranium and plutonium) from various matrices are an important step in nuclear fuel cycle. One of the separation process adopted in an industrial scale is the liquid-liquid extraction or solvent extraction. Liquid-liquid extraction uses a specific ligand/extractant in conjunction with suitable diluent. Solvent extraction or liquid-liquid extraction, involves the partitioning of the solute between two immiscible phases. In most cases, one of the phases is aqueous, and the other one is an organic solvent. The solvent used in solvent extraction should be selective for the metal of interest, it should have optimum distribution ratio, and the loaded metal from the organic phase should be easily stripped under suitable experimental conditions. Some of the important physical properties which are important for the solvent are density, viscosity, phase separation time, interfacial surface tension and the polarity of the extractant.

Extraction, stability, and separation of betalains from Opuntia joconostle cv. using response surface methodology.

PubMed

Sanchez-Gonzalez, Noe; Jaime-Fonseca, Monica R; San Martin-Martinez, Eduardo; Zepeda, L Gerardo

2013-12-11

Betalains were extracted and analyzed from Opuntia joconostle (the prickly pear known as xoconostle in Mexico). For the extraction, two solvent systems were used, methanol/water and ethanol/water. A three-variable Box-Behnken statistical design was used for extraction: solvent concentration (0-80%, v/v), temperature (5-30 °C), and treatment time (10-30 min). The extraction and stability of betalains from xoconostle were studied using response surface methodology (RSM). Techniques such as UV-vis, column chromatography, and HPLC were employed for the separation and analysis of the main pigments present in the extracts. Maximum pigment concentration (92 mg/100 g of fruit) was obtained at a temperature of 15 °C and a time of 10 min for methanol/water (20:80), whereas maximum stability of the pigment was observed at pH 5 and a temperature of 25 °C. HPLC chromatograms showed the main betalains of the xoconostle characterized were betalain, betanidin, and isobetalain.

A Review on the Pharmacological Activities and Phytochemicals of Alpinia officinarum (Galangal) Extracts Derived from Bioassay-Guided Fractionation and Isolation

PubMed Central

Basri, Aida Maryam; Taha, Hussein; Ahmad, Norhayati

2017-01-01

The rhizomes of Alpinia officinarum Hance have been used conventionally for the treatment of various ailments, triggering a wide interest from the scientific research community on this ethnomedicinal plant. This review summarizes the phytochemical and pharmacological properties of the extracts and fractions from A. officinarum, a plant species of the Zingiberaceae family. Different parts of the plant – leaves, roots, rhizomes, and aerial parts – have been extracted in various solvents – methanol, ethanol, ethyl acetate, hexane, dichloromethane, aqueous, chloroform, and petroleum ether, using various techniques – Soxhlet extraction, maceration, ultrasonication, and soaking, whereas fractionation of the plant extracts involves the solvent–solvent partition method. The extracts, fractions, and isolated compounds have been studied for their biological activities – antioxidant, antibacterial, anti-inflammatory, anticancer, antiproliferative, inhibition of enzymes, as well as the inhibition of nitric oxide production. More findings on A. officinarum are certainly important to further develop potential bioactive drug compounds. PMID:28503054

Extraction of fullerenes from environmental matrices as affected by solvent characteristics and analyte concentration.

PubMed

Place, Benjamin J; Kleber, Markus; Field, Jennifer A

2013-03-01

Fullerenes possess unique chemical properties that make the isolation of these compounds from heterogeneous environmental matrices difficult. For example, previous reports indicate that toluene-based extraction techniques vary in their ability to extract C60, especially from highly carbonaceous solid matrices. Here, we examined the effects of (i) solvent type (toluene alone versus an 80:20 v/v mixture of toluene and 1-methylnaphthalene) and (ii) analyte concentration on the extraction efficiency of an isotopically labeled surrogate compound, (13)C60. The toluene/1-methylnaphthalene mixture increased fullerene extraction efficiency from carbon lampblack by a factor of five, but was not significantly different from 100% toluene when applied to wood stove soot or montmorillonite. Recovery of the (13)C60 surrogate declined with decreasing analyte concentration. The usefulness of isotopically labeled surrogate is demonstrated and the study provides a quantitative assessment regarding the dependence of fullerene extraction efficiencies on the geochemical characteristics of solid matrices. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical fluid extraction of plant flavors and fragrances.

PubMed

Capuzzo, Andrea; Maffei, Massimo E; Occhipinti, Andrea

2013-06-19

Supercritical fluid extraction (SFE) of plant material with solvents like CO₂, propane, butane, or ethylene is a topic of growing interest. SFE allows the processing of plant material at low temperatures, hence limiting thermal degradation, and avoids the use of toxic solvents. Although today SFE is mainly used for decaffeination of coffee and tea as well as production of hop extracts on a large scale, there is also a growing interest in this extraction method for other industrial applications operating at different scales. In this review we update the literature data on SFE technology, with particular reference to flavors and fragrance, by comparing traditional extraction techniques of some industrial medicinal and aromatic crops with SFE. Moreover, we describe the biological activity of SFE extracts by describing their insecticidal, acaricidal, antimycotic, antimicrobial, cytotoxic and antioxidant properties. Finally, we discuss the process modelling, mass-transfer mechanisms, kinetics parameters and thermodynamic by giving an overview of SFE potential in the flavors and fragrances arena.

Ultrasonication followed by single-drop microextraction combined with GC/MS for rapid determination of organochlorine pesticides from fish.

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2008-02-01

A novel, rapid and simple sample pretreatment technique termed ultrasonication followed by single-drop micro-extraction (U-SDME) has been developed and combined with GC/MS for the determination of organochlorine pesticides (OCPs) in fish. In the present work, the lengthy procedures generally used in the conventional methods like, Soxhlet extraction, supercritical fluid extraction, pressurized liquid extraction and microwave assisted solvent extraction for extraction of OCPs from fish tissues are minimized by the use of two simple extraction procedures. Firstly, OCPs from fish were extracted in organic solvent with ultrasonication and then subsequently preconcentrated by single-drop micro-extraction (SDME). Extraction parameters of ultrasonication and SDME were optimized in spiked sample solution in order to obtain efficient extraction of OCPs from fish tissues. The calibration curves for OCPs were found to be linear between 10-1000 ng/g with correlation of estimations in the range 0.990-0.994. The recoveries obtained in blank fish tissues were ranged from 82.1 to 95.3%. The LOD and RSD for determination of OCPs in fish were 0.5 ng/g and 9.4-10.0%, respectively. The proposed method was applied for the determination of bioconcentration factor in fish after exposure to different concentrations of OCPs in cultured water. The present method avoids the co-extraction of lipids, long extraction steps (>12 h) and large amount of organic solvent for the separation of OCPs. The main advantages of the present method are rapid, selective, sensitive and low cost for the determination of OCPs in fish.

Compressed air-assisted solvent extraction (CASX) for metal removal.

PubMed

Li, Chi-Wang; Chen, Yi-Ming; Hsiao, Shin-Tien

2008-03-01

A novel process, compressed air-assisted solvent extraction (CASX), was developed to generate micro-sized solvent-coated air bubbles (MSAB) for metal extraction. Through pressurization of solvent with compressed air followed by releasing air-oversaturated solvent into metal-containing wastewater, MSAB were generated instantaneously. The enormous surface area of MSAB makes extraction process extremely fast and achieves very high aqueous/solvent weight ratio (A/S ratio). CASX process completely removed Cr(VI) from acidic electroplating wastewater under A/S ratio of 115 and extraction time of less than 10s. When synthetic wastewater containing Cd(II) of 50mgl(-1) was treated, A/S ratios of higher than 714 and 1190 could be achieved using solvent with extractant/diluent weight ratio of 1:1 and 5:1, respectively. Also, MSAB have very different physical properties, such as size and density, compared to the emulsified solvent droplets, making separation and recovery of solvent from treated effluent very easy.

SOLVENT EXTRACTION PROCESS

DOEpatents

Jonke, A.A.

1957-10-01

In improved solvent extraction process is described for the extraction of metal values from highly dilute aqueous solutions. The process comprises contacting an aqueous solution with an organic substantially water-immiscible solvent, whereby metal values are taken up by a solvent extract phase; scrubbing the solvent extract phase with an aqueous scrubbing solution; separating an aqueous solution from the scrubbed solvent extract phase; and contacting the scrubbed solvent phase with an aqueous medium whereby the extracted metal values are removed from the solvent phase and taken up by said medium to form a strip solution containing said metal values, the aqueous scrubbing solution being a mixture of strip solution and an aqueous solution which contains mineral acids anions and is free of the metal values. The process is particularly effective for purifying uranium, where one starts with impure aqueous uranyl nitrate, extracts with tributyl phosphate dissolved in carbon tetrachloride, scrubs with aqueous nitric acid and employs water to strip the uranium from the scrubbed organic phase.

Analysis of Compounds Dissolved in Nonpolar Solvents by Electrospray Ionization on Conductive Nanomaterials

NASA Astrophysics Data System (ADS)

Xia, Bing; Gao, Yuanji; Ji, Baocheng; Ma, Fengwei; Ding, Lisheng; Zhou, Yan

2018-03-01

Electrospray ionization mass spectrometry (ESI-MS) technique has limitations in analysis of compounds that are dissolved in nonpolar solvents. In this study, ambient ionization of compounds in solvents that are not "friendly" to electrospray ionization, such as n-hexane, is achieved by conductive nanomaterials spray ionization (CNMSI) on nanomaterial emitters, including carbon nanotubes paper and mesodendritic silver covered metal, which applies high voltages to emitters made of these materials without the assistance of polar solvents. Although the time intensity curves (TIC) commonly vary from 4.5% to 23.7% over analyses, protonated molecular ions were found to be the most abundant species, demonstrating good reproducibility of the technique in terms of ionized species. Higher mass spectrometric responses are observed in analyzing nonpolar systems than polar systems. 2-Methoxyacetophenone, 4-methylacetophenone, benzothiazole, quinolone, and cycloheptanone as low as 2 pg in n-hexane can be directly detected using the developed method. The developed technique expands the analysis capability of ESI-MS for direct, online analysis of nonpolar systems, such as low polarity extracts, normal phase liquid chromatography eluates, and synthetic mixtures. [Figure not available: see fulltext.

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

PubMed

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

2017-03-01

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

Accelerated solvent extraction (ASE) for purification and extraction of silicone passive samplers used for the monitoring of organic pollutants.

PubMed

Brockmeyer, Berit; Kraus, Uta R; Theobald, Norbert

2015-12-01

Silicone passive samplers have gained an increasing attention as single-phased, practical and robust samplers for monitoring of organic contaminants in the aquatic environment in recent years. However, analytical challenges arise in routine application during the extraction of analytes as silicone oligomers are co-extracted and interfere severely during chemical analyses (e.g. gas chromatographic techniques). In this study, we present a fast, practical pre-cleaning method for silicone passive samplers applying accelerated solvent extraction (ASE) for the removal of silicone oligomers prior to the water deployment (hexane/dichloromethane, 100 °C, 70 min). ASE was also shown to be a very fast (10 min) and efficient extraction method for non-polar contaminants (non-exposed PRC recoveries 66-101 %) sampled by the silicone membrane. For both applications, temperature, extraction time and the solvent used for ASE have been optimized. Purification of the ASE extract was carried out by silica gel and high-pressure liquid size exclusion chromatography (HPLC-SEC). The silicone oligomer content was checked by total reflection X-ray fluorescence spectroscopy (TXRF) in order to confirm the absence of the silicone oligomers prior to analysis of passive sampler extracts. The established method was applied on real silicone samplers from the North- and Baltic Sea and showed no matrix effects during analysis of organic pollutants. Internal laboratory standard recoveries were in the same range for laboratory, transport and exposed samplers (85-126 %).

Mass transfer coefficient in ginger oil extraction by microwave hydrotropic solution

NASA Astrophysics Data System (ADS)

Handayani, Dwi; Ikhsan, Diyono; Yulianto, Mohamad Endy; Dwisukma, Mandy Ayulia

2015-12-01

This research aims to obtain mass transfer coefficient data on the extraction of ginger oil using microwave hydrotropic solvent as an alternative to increase zingiberene. The innovation of this study is extraction with microwave heater and hydrotropic solvent,which able to shift the phase equilibrium, and the increasing rate of the extraction process and to improve the content of ginger oil zingiberene. The experiment was conducted at the Laboratory of Separation Techniques at Chemical Engineering Department of Diponegoro University. The research activities carried out in two stages, namely experimental and modeling work. Preparation of the model postulated, then lowered to obtain equations that were tested and validated using data obtained from experimental. Measurement of experimental data was performed using microwave power (300 W), extraction temperature of 90 ° C and the independent variable, i.e.: type of hydrotropic, the volume of solvent and concentration in order, to obtain zingiberen levels as a function of time. Measured data was used as a tool to validate the postulation, in order to obtain validation of models and empirical equations. The results showed that the mass transfer coefficient (Kla) on zingiberene mass transfer models ginger oil extraction at various hydrotropic solution attained more 14 ± 2 Kla value than its reported on the extraction with electric heating. The larger value of Kla, the faster rate of mass transfer on the extraction process. To obtain the same yields, the microwave-assisted extraction required one twelfth time shorter.

Optimization of microwave-assisted extraction for the characterization of olive leaf phenolic compounds by using HPLC-ESI-TOF-MS/IT-MS(2).

PubMed

Taamalli, Amani; Arráez-Román, David; Ibañez, Elena; Zarrouk, Mokhtar; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto

2012-01-25

In the present work, a simple and rapid method for the extraction of phenolic compounds from olive leaves, using microwave-assisted extraction (MAE) technique, has been developed. The experimental variables that affect the MAE process, such as the solvent type and composition, microwave temperature, and extraction time, were optimized using a univariate method. The obtained extracts were analyzed by using high-performance liquid chromatography (HPLC) coupled to electrospray time-of-flight mass spectrometry (ESI-TOF-MS) and electrospray ion trap tandem mass spectrometry (ESI-IT-MS(2)) to prove the MAE extraction efficiency. The optimal MAE conditions were methanol:water (80:20, v/v) as extracting solvent, at a temperature equal to 80 °C for 6 min. Under these conditions, several phenolic compounds could be characterized by HPLC-ESI-MS/MS(2). As compared to the conventional method, MAE can be used as an alternative extraction method for the characterization of phenolic compounds from olive leaves due to its efficiency and speed.

Design and optimization of a semicontinuous hot-cold extraction of polyphenols from grape pomace.

PubMed

Monrad, Jeana K; Srinivas, Keerthi; Howard, Luke R; King, Jerry W

2012-06-06

Grape pomace contains appreciable amounts of polyphenolic compounds such as anthocyanins and procyanidins which can be recovered for use as food supplements. The extraction of these polyphenols from the pomace is usually accomplished at slightly elevated temperatures, frequently employing hydroethanolic solvents. Due to governmental regulations and the cost involved in using ethanol as a solvent, as well as the loss in polyphenolics due to thermal degradation, improved extraction techniques are required. In this study, a semicontinuous extraction apparatus employing only water was developed to maximize the recovery of anthocyanins and procyanidins from red grape pomace (Vitis vinifera). Water is preheated prior to its entry to the extraction cell containing the grape pomace sample, where it is allowed to then flow continuously through the unheated extraction vessel prior to its collection at ambient conditions. Extraction variables that impacted the polyphenolic recovery included pomace moisture content (crude or dried), sample mass, water flow rate, and extraction temperature. A response surface method was used to analyze the results from the extraction, and the optimal conditions were found to be 140 °C and 9 mL/min water flow rate. These conditions can produce an extract containing 130 mg/100 g DW of anthocyanins and 2077 mg/100 g DW of procyanidins. Higher yields of polyphenolics were observed using crude (wet) rather than dried pomace, hence avoiding the need to dry the pomace prior to extraction. The described semicontinuous extraction method using only water as the extraction solvent under subcritical conditions allowed the efficient extraction of polyphenols from red grape pomace without the attendant loss of polyphenolic content due to having to heat the extraction vessel prior to commencement of extraction.

Comparison of different methods for extraction from Tetraclinis articulata: yield, chemical composition and antioxidant activity.

PubMed

Herzi, Nejia; Bouajila, Jalloul; Camy, Séverine; Romdhane, Mehrez; Condoret, Jean-Stéphane

2013-12-15

In the present study, three techniques of extraction: hydrodistillation (HD), solvent extraction (conventional 'Soxhlet' technique) and an innovative technique, i.e., the supercritical fluid extraction (SFE), were applied to ground Tetraclinis articulata leaves and compared for extraction duration, extraction yield, and chemical composition of the extracts as well as their antioxidant activities. The extracts were analyzed by GC-FID and GC-MS. The antioxidant activity was measured using two methods: ABTS(•+) and DPPH(•). The yield obtained using HD, SFE, hexane and ethanol Soxhlet extractions were found to be 0.6, 1.6, 40.4 and 21.2-27.4 g/kg respectively. An original result of this study is that the best antioxidant activity was obtained with an SFE extract (41 mg/L). The SFE method offers some noteworthy advantages over traditional alternatives, such as shorter extraction times, low environmental impact, and a clean, non-thermally-degraded final product. Also, a good correlation between the phenolic contents and the antioxidant activity was observed with extracts obtained by SFE at 9 MPa. Copyright © 2013 Elsevier Ltd. All rights reserved.

Optimization of deep eutectic solvent-based ultrasound-assisted extraction of polysaccharides from Dioscorea opposita Thunb.

PubMed

Zhang, Lijin; Wang, Maoshan

2017-02-01

In this study, deep eutectic solvents were proposed for the ultrasound-assisted extraction of polysaccharides from Dioscorea opposita Thunb. Several deep eutectic solvents were prepared for the extraction of polysaccharides, among which the deep eutectic solvent composed of choline chloride and 1,4-butanediol was proved to be suitable for the extraction. Based on the screening of single-factor experiment design and orthogonal experiment design, three experimental factors were optimized for the Box-Behnken experimental design combined with response surface methodology, which gave the optimal extraction conditions: water content of 32.89%(v/v), extraction temperature of 94.00°C, and the extraction time of 44.74min. The optimal extraction conditions could supply higher extraction yield than those of hot water extraction and water-based ultrasound-assisted extraction. Therefore, deep eutectic solvents were an excellent extraction solvent alternative to the extraction of polysaccharides from sample matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

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...

Rapid analysis of chlorinated anilines in environmental water samples using ultrasound assisted emulsification microextraction with solidification of floating organic droplet followed by HPLC-UV detection.

PubMed

Ramkumar, Abilasha; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2012-08-15

The present study demonstrates a simple, rapid and efficient method for the determination of chlorinated anilines (CAs) in environmental water samples using ultrasonication assisted emulsification microextraction technique based on solidification of floating organic droplet (USAEME-SFO) coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection. In this extraction method, 1-dodecanol was used as extraction solvent which is of lower density than water, low toxicity, low volatility, and low melting point (24 °C). After the USAEME, extraction solvent could be collected easily by keeping the extraction tube in ice bath for 2 min and the solidified organic droplet was scooped out using a spatula and transferred to another glass vial and allowed to thaw. Then, 10 μL of extraction solvent was diluted with mobile phase (1:1) and taken for HPLC-UV analysis. Parameters influencing the extraction efficiency, such as the kind and volume of extraction solvent, volume of sample, ultrasonication time, pH and salt concentration were thoroughly examined and optimized. Under the optimal conditions, the method showed good linearity in the concentration range of 0.05-500 ng mL(-1) with correlation coefficients ranging from 0.9948 to 0.9957 for the three target CAs. The limit of detection based on signal to noise ratio of 3 ranged from 0.01 to 0.1 ng mL(-1). The relative standard deviations (RSDs) varied from 2.1 to 6.1% (n=3) and the enrichment factors ranged from 44 to 124. The proposed method has also been successfully applied to analyze real water samples and the relative recoveries of environmental water samples ranged from 81.1 to 116.9%. Copyright © 2012 Elsevier B.V. All rights reserved.

Process and apparatus for solvent extraction of oil from oil-containing diatomite ore

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

Karnofsky, G. B.

1980-12-16

A process for solvent extraction of oil from oil bearing diatomite ore and an apparatus for use therewith, wherein the ore is extracted by countercurrent decantation with a hydrocarbon solvent, solvent is recovered from the extract by multiple effect evaporation followed by stripping, and the spent diatomite is contacted with water to displace a major portion of the solvent therefrom, and solvent is recovered from the aqueous slurry of the spent diatomite by stripping with steam at superatmospheric pressure.

Sample preparation techniques for the determination of trace residues and contaminants in foods.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2007-06-15

The determination of trace residues and contaminants in complex matrices, such as food, often requires extensive sample extraction and preparation prior to instrumental analysis. Sample preparation is often the bottleneck in analysis and there is a need to minimise the number of steps to reduce both time and sources of error. There is also a move towards more environmentally friendly techniques, which use less solvent and smaller sample sizes. Smaller sample size becomes important when dealing with real life problems, such as consumer complaints and alleged chemical contamination. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This review considers all aspects of sample preparation, covering general extraction techniques, such as Soxhlet and pressurised liquid extraction, microextraction techniques such as liquid phase microextraction (LPME) and more selective techniques, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The applicability of each technique in food analysis, particularly for the determination of trace organic contaminants in foods is discussed.

Development of a rapid method for the sequential extraction and subsequent quantification of fatty acids and sugars from avocado mesocarp tissue.

PubMed

Meyer, Marjolaine D; Terry, Leon A

2008-08-27

Methods devised for oil extraction from avocado (Persea americana Mill.) mesocarp (e.g., Soxhlet) are usually lengthy and require operation at high temperature. Moreover, methods for extracting sugars from avocado tissue (e.g., 80% ethanol, v/v) do not allow for lipids to be easily measured from the same sample. This study describes a new simple method that enabled sequential extraction and subsequent quantification of both fatty acids and sugars from the same avocado mesocarp tissue sample. Freeze-dried mesocarp samples of avocado cv. Hass fruit of different ripening stages were extracted by homogenization with hexane and the oil extracts quantified for fatty acid composition by GC. The resulting filter residues were readily usable for sugar extraction with methanol (62.5%, v/v). For comparison, oil was also extracted using the standard Soxhlet technique and the resulting thimble residue extracted for sugars as before. An additional experiment was carried out whereby filter residues were also extracted using ethanol. Average oil yield using the Soxhlet technique was significantly (P < 0.05) higher than that obtained by homogenization with hexane, although the difference remained very slight, and fatty acid profiles of the oil extracts following both methods were very similar. Oil recovery improved with increasing ripeness of the fruit with minor differences observed in the fatty acid composition during postharvest ripening. After lipid removal, methanolic extraction was superior in recovering sucrose and perseitol as compared to 80% ethanol (v/v), whereas mannoheptulose recovery was not affected by solvent used. The method presented has the benefits of shorter extraction time, lower extraction temperature, and reduced amount of solvent and can be used for sequential extraction of fatty acids and sugars from the same sample.

Modern extraction techniques and their impact on the pharmacological profile of Serenoa repens extracts for the treatment of lower urinary tract symptoms

PubMed Central

2014-01-01

Background Bioactive compounds from plants (i.e., Serenoa repens) are often used in medicine in the treatment of several pathologies, among which benign prostatic hyperplasia (BPH) associated to lower urinary tract symptoms (LUTS). Discussion There are different techniques of extraction, also used in combination, with the aim of enhancing the amount of the target molecules, gaining time and reducing waste of solvents. However, the qualitative and quantitative composition of the bioactives depends on the extractive process, and so the brands of the recovered products from the same plant are different in terms of clinical efficacy (no product interchangeability among different commercial brands). Summary In this review, we report on several and recent extraction techniques and their impact on the composition/biological activity of S. repens-based available products. PMID:25112532

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.

Remediating pesticide contaminated soils using solvent extraction

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

Sahle-Demessie, E.; Meckes, M.C.; Richardson, T.L.

Bench-scale solvent extraction studies were performed on soil samples obtained from a Superfund site contaminated with high levels of p,p{prime}-DDT, p,p{prime}-DDE and toxaphene. The effectiveness of the solvent extraction process was assessed using methanol and 2-propanol as solvents over a wide range of operating conditions. It was demonstrated that a six-stage methanol extraction using a solvent-to-soil ratio of 1.6 can decrease pesticide levels in the soil by more than 99% and reduce the volume of material requiring further treatment by 25 times or more. The high solubility of the pesticides in methanol resulted in rapid extraction rates, with the systemmore » reaching quasi-equilibrium state in 30 minutes. The extraction efficiency was influenced by the number of extraction stages, the solvent-to-soil ratio, and the soil moisture content. Various methods were investigated to regenerate and recycle the solvent. Evaporation and solvent stripping are low cost and reliable methods for removing high pesticide concentrations from the solvent. For low concentrations, GAC adsorption may be used. Precipitating and filtering pesticides by adding water to the methanol/pesticide solution was not successful when tested with soil extracts. 26 refs., 10 figs., 6 tabs.« less

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.

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...

Supercritical Fluid Extraction and Separation of Uranium from Other Actinides

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

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

2014-06-01

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

Innovative Alternative Technologies to Extract Carotenoids from Microalgae and Seaweeds

PubMed Central

Poojary, Mahesha M.; Barba, Francisco J.; Aliakbarian, Bahar; Donsì, Francesco; Pataro, Gianpiero; Dias, Daniel A.; Juliano, Pablo

2016-01-01

Marine microalgae and seaweeds (microalgae) represent a sustainable source of various bioactive natural carotenoids, including β-carotene, lutein, astaxanthin, zeaxanthin, violaxanthin and fucoxanthin. Recently, the large-scale production of carotenoids from algal sources has gained significant interest with respect to commercial and industrial applications for health, nutrition, and cosmetic applications. Although conventional processing technologies, based on solvent extraction, offer a simple approach to isolating carotenoids, they suffer several, inherent limitations, including low efficiency (extraction yield), selectivity (purity), high solvent consumption, and long treatment times, which have led to advancements in the search for innovative extraction technologies. This comprehensive review summarizes the recent trends in the extraction of carotenoids from microalgae and seaweeds through the assistance of different innovative techniques, such as pulsed electric fields, liquid pressurization, supercritical fluids, subcritical fluids, microwaves, ultrasounds, and high-pressure homogenization. In particular, the review critically analyzes technologies, characteristics, advantages, and shortcomings of the different innovative processes, highlighting the differences in terms of yield, selectivity, and economic and environmental sustainability. PMID:27879659

Innovative Alternative Technologies to Extract Carotenoids from Microalgae and Seaweeds.

PubMed

Poojary, Mahesha M; Barba, Francisco J; Aliakbarian, Bahar; Donsì, Francesco; Pataro, Gianpiero; Dias, Daniel A; Juliano, Pablo

2016-11-22

Marine microalgae and seaweeds (microalgae) represent a sustainable source of various bioactive natural carotenoids, including β-carotene, lutein, astaxanthin, zeaxanthin, violaxanthin and fucoxanthin. Recently, the large-scale production of carotenoids from algal sources has gained significant interest with respect to commercial and industrial applications for health, nutrition, and cosmetic applications. Although conventional processing technologies, based on solvent extraction, offer a simple approach to isolating carotenoids, they suffer several, inherent limitations, including low efficiency (extraction yield), selectivity (purity), high solvent consumption, and long treatment times, which have led to advancements in the search for innovative extraction technologies. This comprehensive review summarizes the recent trends in the extraction of carotenoids from microalgae and seaweeds through the assistance of different innovative techniques, such as pulsed electric fields, liquid pressurization, supercritical fluids, subcritical fluids, microwaves, ultrasounds, and high-pressure homogenization. In particular, the review critically analyzes technologies, characteristics, advantages, and shortcomings of the different innovative processes, highlighting the differences in terms of yield, selectivity, and economic and environmental sustainability.

[The progress in speciation analysis of trace elements by atomic spectrometry].

PubMed

Wang, Zeng-Huan; Wang, Xu-Nuo; Ke, Chang-Liang; Lin, Qin

2013-12-01

The main purpose of the present work is to review the different non-chromatographic methods for the speciation analysis of trace elements in geological, environmental, biological and medical areas. In this paper, the sample processing methods in speciation analysis were summarized, and the main strategies for non-chromatographic technique were evaluated. The basic principles of the liquid extractions proposed in the published literatures recently and their advantages and disadvantages were discussed, such as conventional solvent extraction, cloud point extraction, single droplet microextraction, and dispersive liquid-liquid microextraction. Solid phase extraction, as a non-chromatographic technique for speciation analysis, can be used in batch or in flow detection, and especially suitable for the online connection to atomic spectrometric detector. The developments and applications of sorbent materials filled in the columns of solid phase extraction were reviewed. The sorbents include chelating resins, nanometer materials, molecular and ion imprinted materials, and bio-sorbents. Other techniques, e. g. hydride generation technique and coprecipitation, were also reviewed together with their main applications.

A modified approach for isolation of essential oil from fruit of Amorpha fruticosa Linn using microwave-assisted hydrodistillation concatenated liquid-liquid extraction.

PubMed

Chen, Fengli; Jia, Jia; Zhang, Qiang; Gu, Huiyan; Yang, Lei

2017-11-17

In this work, a modified technique was developed to separate essential oil from the fruit of Amorpha fruticosa using microwave-assisted hydrodistillation concatenated liquid-liquid extraction (MHD-LLE). The new apparatus consists of two series-wound separation columns for separating essential oil, one is the conventional oil-water separation column, and the other is the extraction column of components from hydrosol using an organic solvent. Therefore, the apparatus can simultaneously collect the essential oil separated on the top of hydrosol and the components extracted from hydrosol using an organic solvent. Based on the yield of essential oil in the first and second separation columns, the effects of parameters were investigated by single factor experiments and Box-Behnken design. Under the optimum conditions (2mL ethyl ether as the extraction solvent in the second separation column, 12mL/g liquid-solid ratio, 4.0min homogenate time, 35min microwave irradiation time and 540W microwave irradiation power), satisfactory yields for the essential oil in the first separation column (10.31±0.33g/kg) and second separation column (0.82±0.03g/kg) were obtained. Compared with traditional methods, the developed method gave a higher yield of essential oil in a shorter time. In addition, GC-MS analysis of the essential oil indicated significant differences of the relative contents of individual volatile components in the essential oils obtained in the two separation columns. Therefore, the MHD-LLE technique developed here is a good alternative for the isolation of essential oil from A. fruticosa fruit as well as other herbs. Copyright © 2017 Elsevier B.V. All rights reserved.

Extraction of bioactive carbohydrates from artichoke (Cynara scolymus L.) external bracts using microwave assisted extraction and pressurized liquid extraction.

PubMed

Ruiz-Aceituno, Laura; García-Sarrió, M Jesús; Alonso-Rodriguez, Belén; Ramos, Lourdes; Sanz, M Luz

2016-04-01

Microwave assisted extraction (MAE) and pressurized liquid extraction (PLE) methods using water as solvent have been optimized by means of a Box-Behnken and 3(2) composite experimental designs, respectively, for the effective extraction of bioactive carbohydrates (inositols and inulin) from artichoke (Cynara scolymus L.) external bracts. MAE at 60 °C for 3 min of 0.3 g of sample allowed the extraction of slightly higher concentrations of inositol than PLE at 75 °C for 26.7 min (11.6 mg/g dry sample vs. 7.6 mg/g dry sample). On the contrary, under these conditions, higher concentrations of inulin were extracted with the latter technique (185.4 mg/g vs. 96.4 mg/g dry sample), considering two successive extraction cycles for both techniques. Both methodologies can be considered appropriate for the simultaneous extraction of these bioactive carbohydrates from this particular industrial by-product. To the best of our knowledge this is the first time that these techniques are applied for this purpose. Copyright © 2015 Elsevier Ltd. All rights reserved.

Infrared Database for Process Support Materials

NASA Technical Reports Server (NTRS)

Bennett, K. E.; Boothe, R. E.; Burns, H. D.

2003-01-01

Process support materials' compatibility with cleaning processes is critical to ensure final hardware cleanliness and that performance requirements are met. Previous discovery of potential contaminants in process materials shows the need for incoming materials testing and establishment of a process materials database. The Contamination Control Team of the Materials, Processes, and Manufacturing (MP&M) Department at Marshall Space Flight Center (MSFC) has initiated the development of such an infrared (IR) database, called the MSFC Process Materials IR database, of the common process support materials used at MSFC. These process support materials include solvents, wiper cloths, gloves, bagging materials, etc. Testing includes evaluation of the potential of gloves, wiper cloths, and other items to transfer contamination to handled articles in the absence of solvent exposure, and the potential for solvent exposure to induce material degradation. This Technical Memorandum (TM) summarizes the initial testing completed through December 2002. It is anticipated that additional testing will be conducted with updates provided in future TMs.Materials were analyzed using two different IR techniques: (1) Dry transference and (2) liquid extraction testing. The first of these techniques utilized the Nicolet Magna 750 IR spectrometer outfitted with a horizontal attenuated total reflectance (HATR) crystal accessory. The region from 650 to 4,000 wave numbers was analyzed, and 50 scans were performed per IR spectrum. A dry transference test was conducted by applying each sample with hand pressure to the HATR crystal to first obtain a spectrum of the parent material. The material was then removed from the HATR crystal and analyzed to determine the presence of any residues. If volatile, liquid samples were examined both prior to and following evaporation.The second technique was to perform an extraction test with each sample in five different solvents.Once the scans were complete for both the dry transference and the extraction tests, the residue from each scan was interpreted.

Extraction, scrub, and strip test results for the salt waste processing facility caustic side solvent extraction solvent example

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

Peters, T. B.

An Extraction, Scrub, and Strip (ESS) test was performed on a sample of Salt Waste Processing Facility (SWPF) Caustic-Side Solvent Extraction (CSSX) solvent and salt simulant to determine cesium distribution ratios (D(Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams; this data will be used by Parsons to help determine if the solvent is qualified for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations. The extraction D(Cs) measured 12.9, exceeding the required value of 8. This value is consistent with results from previousmore » ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges.« less

Thermal degradation of the solvent employed in the next-generation caustic-side solvent extraction process and its effect on the extraction, scrubbing, and stripping of cesium

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

Roach, Benjamin D.; Williams, Neil J.; Moyer, Bruce A.

As part of the ongoing development of the Next-Generation Caustic-Side Solvent Extraction (NGS) process, the thermal stability of the process solvent was investigated and shown to be adequate for industrial application. The solvent was thermally treated at 35 C over a period of 13 months whilst in dynamic contact with each of the aqueous phases of the current NGS process, namely SRS 15 (a highly caustic waste simulant), sodium hydroxide scrub solution (0.025 M), and boric acid strip solution (0.01 M). The effect of thermal treatment was evaluated by assessing batch extract/scrub/strip performance as a function of time, by monitoringmore » the sodium extraction capacity of the solvent, and by analysis of the solvent using electrospray mass spectrometry. Current studies indicate that the NGS solvent should be thermally robust for a period of XXX months at the Modular Caustic-Side Solvent Extraction Unit (MCU) pilot plant located at Savannah River Site. Furthermore, the guanidine suppressor appears to be the solvent component most significantly impacted by thermal treatment of the solvent, showing significant degradation over time.« less

Thermal degradation of the solvent employed in the next-generation caustic-side solvent extraction process and its effect on the extraction, scrubbing, and stripping of cesium

DOE PAGES

Roach, Benjamin D.; Williams, Neil J.; Moyer, Bruce A.

2015-09-02

As part of the ongoing development of the Next-Generation Caustic-Side Solvent Extraction (NGS) process, the thermal stability of the process solvent was investigated and shown to be adequate for industrial application. The solvent was thermally treated at 35 C over a period of 13 months whilst in dynamic contact with each of the aqueous phases of the current NGS process, namely SRS 15 (a highly caustic waste simulant), sodium hydroxide scrub solution (0.025 M), and boric acid strip solution (0.01 M). The effect of thermal treatment was evaluated by assessing batch extract/scrub/strip performance as a function of time, by monitoringmore » the sodium extraction capacity of the solvent, and by analysis of the solvent using electrospray mass spectrometry. Current studies indicate that the NGS solvent should be thermally robust for a period of XXX months at the Modular Caustic-Side Solvent Extraction Unit (MCU) pilot plant located at Savannah River Site. Furthermore, the guanidine suppressor appears to be the solvent component most significantly impacted by thermal treatment of the solvent, showing significant degradation over time.« less

Preparation of non-porous microspheres with high entrapment efficiency of proteins by a (water-in-oil)-in-oil emulsion technique.

PubMed

Viswanathan, N B; Thomas, P A; Pandit, J K; Kulkarni, M G; Mashelkar, R A

1999-03-08

Emulsification-solvent removal methods have been widely used for encapsulating bioactive macromolecules like proteins and polypeptides in biodegradable polymers. We report, a (water-in-oil)-in-oil emulsion technique wherein proteins and polypeptides differing in molecular weight and shape were encapsulated in polymers of current biomedical interest. When an oil was used as the processing medium in combination with a carefully selected mixed solvent system such that a stable (w/o1/o2 emulsion is formed and solvents are removed by a combination of extraction and evaporation, the entrapment efficiency was high and the product nonporous. The entrapment efficiency of globular proteins exceeded 90% while that of fibrous proteins was around 70%. Fracture studies revealed that the polymer matrix was dense. The mechanism of entrapment involved solvent-induced precipitation of the protein as the microspheres were being formed. The principle of the method will find use in preparation of non-porous polymer microparticles with reduced burst effect.

Process and apparatus for solvent extraction of oil from oil-containing diatomite ore

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

Karnofsky, G.B.

1979-09-11

A process is described for solvent extraction of oil-bearing diatomite ore. An apparatus is provided for use therewith, wherein the ore is extracted by countercurrent decantation with a hydrocarbon solvent. The solvent is recovered from the extract by multiple effect evaporation followed by stripping, and the spent diatomite is contacted with water to displace a major portion of the solvent therefrom. The solvent is recovered from the aqueous slurry of the spent diatomite by stripping with steam at superatmospheric pressure. 17 claims.

Alkaline-side extraction of technetium from tank waste using crown ethers and other extractants

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

Bonnesen, P.V.; Moyer, B.A.; Presley, D.J.

The chemical development of a new crown-ether-based solvent-extraction process for the separation of (Tc) from alkaline tank-waste supernate is ready for counter-current testing. The process addresses a priority need in the proposed cleanup of Hanford and other tank wastes. This need has arisen from concerns due to the volatility of Tc during vitrification, as well as {sup 99}Tc`s long half-life and environmental mobility. The new process offers several key advantages that direct treatability--no adjustment of the waste composition is needed; economical stripping with water; high efficiency--few stages needed; non-RCRA chemicals--no generation of hazardous or mixed wastes; co-extraction of {sup 90}Sr;more » and optional concentration on a resin. A key concept advanced in this work entails the use of tandem techniques: solvent extraction offers high selectivity, while a subsequent column sorption process on the aqueous stripping solution serves to greatly concentrate the Tc. Optionally, the stripping solution can be evaporated to a small volume. Batch tests of the solvent-extraction and stripping components of the process have been conducted on actual melton Valley Storage Tank (MVST) waste as well as simulants of MVST and Hanford waste. The tandem process was demonstrated on MVST waste simulants using the three solvents that were selected the final candidates for the process. The solvents are 0.04 M bis-4,4{prime}(5{prime})[(tert-butyl)cyclohexano]-18-crown-6 (abbreviated di-t-BuCH18C6) in a 1:1 vol/vol blend of tributyl phosphate and Isopar{reg_sign} M (an isoparaffinic kerosene); 0.02 M di-t-BuCH18C6 in 2:1 vol/vol TBP/Isopar M and pure TBP. The process is now ready for counter-current testing on actual Hanford tank supernates.« less

Optimization of soy isoflavone extraction with different solvents using the simplex-centroid mixture design.

PubMed

Yoshiara, Luciane Yuri; Madeira, Tiago Bervelieri; Delaroza, Fernanda; da Silva, Josemeyre Bonifácio; Ida, Elza Iouko

2012-12-01

The objective of this study was to optimize the extraction of different isoflavone forms (glycosidic, malonyl-glycosidic, aglycone and total) from defatted cotyledon soy flour using the simplex-centroid experimental design with four solvents of varying polarity (water, acetone, ethanol and acetonitrile). The obtained extracts were then analysed by high-performance liquid chromatography. The profile of the different soy isoflavones forms varied with different extractions solvents. Varying the solvent or mixture used, the extraction of different isoflavones was optimized using the centroid-simplex mixture design. The special cubic model best fitted to the four solvents and its combination for soy isoflavones extraction. For glycosidic isoflavones extraction, the polar ternary mixture (water, acetone and acetonitrile) achieved the best extraction; malonyl-glycosidic forms were better extracted with mixtures of water, acetone and ethanol. Aglycone isoflavones, water and acetone mixture were best extracted and total isoflavones, the best solvents were ternary mixture of water, acetone and ethanol.

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

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

Michael F. Gray; Peter Zalupski; Mikael Nilsson

2013-08-01

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

The optimization of phthalate analysis from plastic matrices by using GC/MS related techniques

NASA Astrophysics Data System (ADS)

Pusfitasari, Eka Dian; Hendarsyah, Hendris; Athaillah, Zatil Afrah

2017-11-01

Indication of malicious acts conducted by food vendors has been reported in many places in Indonesia and has been worrying the population. One of the issues is the indication that frying oil used by the vendors has been added with food packaging plastic to impart more crispy texture of the fried foods. One of the challenges for the monitoring process is to find suitable analytical method to identify this type of food adulteration. Because some food packaging, particularly from polyethylene group, contains plasticizer diethylhexylphthalate (DEHP), we intended to investigate the adulteration by detecting the phthalate compound. In this preliminary study, we focused on the optimization of GC equipment as well as the optimization of plastic extraction process with various types of solvents (hexane, dichloromethane, and acetonitrile) and extraction time (24, 48, and 72 hours). For 72-hour duration, treatment with solvent refreshment was also conducted to minimize solvent saturation effect. Our findings suggested that LOD and LOQ of the GC/MS instrument used for the DEHP analysis were 19.6 ng and 65.5 ng, respectively. In addition, it could be concluded that the process of plastic extraction through sonication for five minutes with n-hexane as a solvent resulted in the optimal value.

Enhancement of ionization efficiency of mass spectrometric analysis from non-electrospray ionization friendly solvents with conventional and novel ionization techniques.

PubMed

Jiang, Ping; Lucy, Charles A

2015-10-15

Electrospray ionization mass spectrometry (ESI-MS) has significantly impacted the analysis of complex biological and petroleum samples. However ESI-MS has limited ionization efficiency for samples in low dielectric and low polarity solvents. Addition of a make-up solvent through a T union or electrospray solvent through continuous flow extractive desorption electrospray ionization (CF-EDESI) enable ionization of analytes in non-ESI friendly solvents. A conventional make-up solvent addition setup was used and a CF-EDESI source was built for ionization of nitrogen-containing standards in hexane or hexane/isopropanol. Factors affecting the performance of both sources have been investigated and optimized. Both the make-up solvent addition and CF-EDESI improve the ionization efficiency for heteroatom compounds in non-ESI friendly solvents. Make-up solvent addition provides higher ionization efficiency than CF-EDESI. Neither the make-up solvent addition nor the CF-EDESI eliminates ionization suppression of nitrogen-containing compounds caused by compounds of the same chemical class. Copyright © 2015 Elsevier B.V. All rights reserved.

Recent patents on the extraction of carotenoids.

PubMed

Riggi, Ezio

2010-01-01

This article reviews the patents that have been presented during the last decade related to the extraction of carotenoids from various forms of organic matter (fruit, vegetables, animals), with an emphasis on the methods and mechanisms exploited by these technologies, and on technical solutions for the practical problems related to these technologies. I present and classify 29 methods related to the extraction processes (physical, mechanical, chemical, and enzymatic). The large number of processes for extraction by means of supercritical fluids and the growing number of large-scale industrial plants suggest a positive trend towards using this technique that is currently slowed by its cost. This trend should be reinforced by growing restrictions imposed on the use of most organic solvents for extraction of food products and by increasingly strict waste management regulations that are indirectly promoting the use of extraction processes that leave the residual (post-extraction) matrix substantially free from solvents and compounds that must subsequently be removed or treated. None of the reviewed approaches is the best answer for every extractable compound and source, so each should be considered as one of several alternatives, including the use of a combination of extraction approaches.

Ultrasound-assisted leaching-dispersive solid-phase extraction followed by liquid-liquid microextraction for the determination of polybrominated diphenyl ethers in sediment samples by gas chromatography-tandem mass spectrometry.

PubMed

Fontana, Ariel R; Lana, Nerina B; Martinez, Luis D; Altamirano, Jorgelina C

2010-06-30

Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 microL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates were <9.8%. The calibration graphs were linear within the concentration range of 0.07-1000 ng g(-1) for BDE-47, 0.09-1000 ng g(-1) for BDE-100, 0.10-1000 ng g(-1) for BDE-99 and 0.19-1000 ng g(-1) for BDE-153 and the coefficients of estimation were > or =0.9991. Validation of the methodology was carried out by standard addition method at two concentration levels (0.25 and 1 ng g(-1)) and by comparing with a reference Soxhlet technique. Recovery values were > or =80%, which showed a satisfactory robustness of the analytical methodology for determination of low PBDEs concentration in sediment samples. Copyright 2010 Elsevier B.V. All rights reserved.

Development of deep eutectic solvents applied in extraction and separation.

PubMed

Li, Xiaoxia; Row, Kyung Ho

2016-09-01

Deep eutectic solvents, as an alternative to ionic liquids, have greener credentials than ionic liquids, and have attracted considerable attention in related chemical research. Deep eutectic solvents have attracted increasing attention in chemistry for the extraction and separation of various target compounds from natural products. This review highlights the preparation of deep eutectic solvents, unique properties of deep eutectic solvents, and synthesis of deep-eutectic-solvent-based materials. On the other hand, application in the extraction and separation of deep eutectic solvents is also included in this report. In this paper, the available data and references in this field are reviewed to summarize the applications and developments of deep eutectic solvents. Based on the development of deep eutectic solvents, an exploitation of new deep eutectic solvents and deep eutectic solvents-based materials is expected to diversify into extraction and separation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In vitro screening of organotin compounds and sediment extracts for cytotoxicity to fish cells.

PubMed

Giltrap, Michelle; Macken, Ailbhe; McHugh, Brendan; McGovern, Evin; Foley, Barry; Davoren, Maria

2011-01-01

The present study reports an in vitro screening method for contaminants in sediment samples utilizing an RTG-2 cell line. This technique integrates cytotoxicity testing with analytical chemistry with the aim of achieving a toxicity evaluation of the sediment sample. The toxic effect of individual organotin (OT) compounds and their presence in the sediment sample is the focus of the present study; however, other contaminants are also discussed. The following OT compounds: tributyltin (TBT), dibutyltin (DBT), monobutyltin (MBT), triphenyltin (TPT), diphenyltin (DPT), and a sediment solvent extract are exposed to the RTG-2 fish cell line. Both the alamar blue (AB) and neutral red (NR) assays are used to assess cytotoxicity after 24-h and 96-h exposure. Methodology for preparation of a sediment solvent extract suitable for biological testing and analytical determination is also described. With the RTG-2 cells, the AB and NR assays had comparable sensitivity for each individual OT compound exposure after 24 h, with TPT being the most toxic compound tested. The individual OT compound concentrations required to induce a 50% toxic effect on the cells (369 ng ml⁻¹ TBT, 1,905 ng ml⁻¹ DBT) did not equate to the concentrations of these contaminants present in the sediment extract that induced a 50% effect on the cells (294 ng ml⁻¹ TBT, 109 ng ml⁻¹ DBT). The solvent extract therefore exhibited a greater toxicity, and this suggests that the toxic effects observed were not due to OT compounds alone. The presence of other contaminants in the solvent extract is confirmed with chemical analysis, warranting further toxicity testing of contaminant mixtures and exposure to the cell line to further elucidate a complete toxicity evaluation. © 2010 SETAC.

Separation of Trivalent Actinides from Lanthanides Using a Capillary Electrophoresis

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

Mori, Tomotaka; Ishii, Yasuo; Hayashi, Kazunori

2007-07-01

A separation of {sup 241}Am(III) from {sup 152,154}Eu(III) was carried out using a capillary electrophoresis technique in a mixed solvent (CH{sub 3}OH/H{sub 2}O) system containing thiocyanate ion. First, the formation constants ({beta}{sub n}) between thiocyanate ion and Eu(III) or Am(III) were investigated in the mixed solvent solutions by a back-extraction technique using bis (2-ethylhexyl) hydrogen phosphate-toluene. The mean charges calculated on the basis of the data of {beta}{sub n} for Eu(III) were comparatively higher than those for Am(III). Based on the differences between the mean charges of Eu(III) and Am(III), separations for Am(III)/Eu(III) by means of capillary electrophoresis technique weremore » tried in the (H{sup +}, Na{sup +})(SCN{sup -}, ClO{sub 4}{sup -}) mixed solvent solutions. It was proved that Am(III) was completely separated from Eu(III). (authors)« less

Substitution of carcinogenic solvent dichloromethane for the extraction of volatile compounds in a fat-free model food system.

PubMed

Cayot, Nathalie; Lafarge, Céline; Bou-Maroun, Elias; Cayot, Philippe

2016-07-22

Dichloromethane is known as a very efficient solvent, but, as other halogenated solvents, is recognized as a hazardous product (CMR substance). The objective of the present work is to propose substitution solvent for the extraction of volatile compounds. The most important physico-chemical parameters in the choice of an appropriate extraction solvent of volatile compounds are reviewed. Various solvents are selected on this basis and on their hazard characteristics. The selected solvents, safer than dichloromethane, are compared using the extraction efficiency of volatile compounds from a model food product able to interact with volatile compounds. Volatile compounds with different hydrophobicity are used. High extraction yields were positively correlated with high boiling points and high Log Kow values of volatile compounds. Mixtures of solvents such as azeotrope propan-2-one/cyclopentane, azeotrope ethyl acetate/ethanol, and mixture ethyl acetate/ethanol (3:1, v/v) gave higher extraction yields than those obtained with dichloromethane. Copyright © 2016 Elsevier B.V. All rights reserved.

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

DOEpatents

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

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.

Evaluation of solvent effect on the extraction of phenolic compounds and antioxidant capacities from the berries: application of principal component analysis.

PubMed

Boeing, Joana Schuelter; Barizão, Erica Oliveira; E Silva, Beatriz Costa; Montanher, Paula Fernandes; de Cinque Almeida, Vitor; Visentainer, Jesuí Vergilio

2014-01-01

This study evaluated the effect of the solvent on the extraction of antioxidant compounds from black mulberry (Morus nigra), blackberry (Rubus ulmifolius) and strawberry (Fragaria x ananassa). Different extracts of each berry were evaluated from the determination of total phenolic content, anthocyanin content and antioxidant capacity, and data were applied to the principal component analysis (PCA) to gain an overview of the effect of the solvent in extraction method. For all the berries analyzed, acetone/water (70/30, v/v) solvent mixture was more efficient solvent in the extracting of phenolic compounds, and methanol/water/acetic acid (70/29.5/0.5, v/v/v) showed the best values for anthocyanin content. Mixtures of ethanol/water (50/50, v/v), acetone water/acetic acid (70/29.5/0.5, v/v/v) and acetone/water (50/50, v/v) presented the highest antioxidant capacities for black mulberries, blackberries and strawberries, respectively. Antioxidants extractions are extremely affected by the solvent combination used. In addition, the obtained extracts with the organic solvent-water mixtures were distinguished from the extracts obtained with pure organic solvents, through the PCA analysis.

Effect of extraction method on the yield of furanocoumarins from fruits of Archangelica officinalis Hoffm.

PubMed

Waksmundzka-Hajnos, M; Petruczynik, A; Dragan, A; Wianowska, D; Dawidowicz, A L

2004-01-01

Optimal conditions for the extraction and analysis of furanocoumarins from fruits of Archangelica officinalis Hoffm. have been determined. The following extraction methods were used: exhaustive extraction in a Soxhlet apparatus, ultrasonication at 25 and 60 degrees C, microwave-assisted solvent extraction in open and closed systems, and accelerated solvent extraction (ASE). In most cases the yields of furanocoumarins were highest using the ASE method. The effects of extracting solvent, temperature and time of extraction using this method were investigated. The highest yield of furanocoumarins by ASE was obtained with methanol at 100-130 degrees C for 10 min. The extraction yields of furanocoumarins from plant material by ultrasonication at 60 degrees C and microwave-assisted solvent extraction in an open system were comparable to the extraction yields obtained in the time- and solvent-consuming exhaustive process involving the Soxhlet apparatus.

Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

PubMed

You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

2018-01-15

A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

Ionic liquids: solvents and sorbents in sample preparation.

PubMed

Clark, Kevin D; Emaus, Miranda N; Varona, Marcelino; Bowers, Ashley N; Anderson, Jared L

2018-01-01

The applications of ionic liquids (ILs) and IL-derived sorbents are rapidly expanding. By careful selection of the cation and anion components, the physicochemical properties of ILs can be altered to meet the requirements of specific applications. Reports of IL solvents possessing high selectivity for specific analytes are numerous and continue to motivate the development of new IL-based sample preparation methods that are faster, more selective, and environmentally benign compared to conventional organic solvents. The advantages of ILs have also been exploited in solid/polymer formats in which ordinarily nonspecific sorbents are functionalized with IL moieties in order to impart selectivity for an analyte or analyte class. Furthermore, new ILs that incorporate a paramagnetic component into the IL structure, known as magnetic ionic liquids (MILs), have emerged as useful solvents for bioanalytical applications. In this rapidly changing field, this Review focuses on the applications of ILs and IL-based sorbents in sample preparation with a special emphasis on liquid phase extraction techniques using ILs and MILs, IL-based solid-phase extraction, ILs in mass spectrometry, and biological applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous multicomponent spectrophotometric monitoring of methyl and propyl parabens using multivariate statistical methods after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction.

PubMed

Khani, Rouhollah; Ghasemi, Jahan B; Shemirani, Farzaneh

2014-03-25

A powerful and efficient signal-preprocessing technique that combines local and multiscale properties of the wavelet prism with the global filtering capability of orthogonal signal correction (OSC) is applied for pretreatment of spectroscopic data of parabens as model compounds after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction method (IL-DLLME). In the proposed technique, a mixture of a water-immiscible ionic liquid (as extraction solvent) [Hmim][PF6] and disperser solvent is injected into an aqueous sample solution containing one of the IL's ions, NaPF6, as extraction solvent and common ion source. After preconcentration, the absorbance of the extracted compounds was measured in the wavelength range of 200-700 nm. The wavelet orthogonal signal correction with partial least squares (WOSC-PLS) method was then applied for simultaneous determination of each individual compound. Effective parameters, such as amount of IL, volume of the disperser solvent and amount of NaPF6, were inspected by central composite design to identify the most important parameters and their interactions. The effect of pH on the sensitivity and selectivity was studied according to the net analyte signal (NAS) for each component. Under optimum conditions, enrichment factors of the studied compounds were 75 for methyl paraben (MP) and 71 for propyl paraben (PP). Limits of detection for MP and PP were 4.2 and 4.8 ng mL(-)(1), respectively. The root mean square errors of prediction for MP and PP were 0.1046 and 0.1275 μg mL(-)(1), respectively. The practical applicability of the developed method was examined using hygienic, cosmetic, pharmaceutical and natural water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Supercritical fluid technology: concepts and pharmaceutical applications.

PubMed

Deshpande, Praful Balavant; Kumar, G Aravind; Kumar, Averineni Ranjith; Shavi, Gopal Venkatesh; Karthik, Arumugam; Reddy, Meka Sreenivasa; Udupa, Nayanabhirama

2011-01-01

In light of environmental apprehension, supercritical fluid technology (SFT) exhibits excellent opportunities to accomplish key objectives in the drug delivery sector. Supercritical fluid extraction using carbon dioxide (CO(2)) has been recognized as a green technology. It is a clean and versatile solvent with gas-like diffusivity and liquid-like density in the supercritical phase, which has provided an excellent alternative to the use of chemical solvents. The present commentary provides an overview of different techniques using supercritical fluids and their future opportunity for the drug delivery industry. Some of the emerging applications of SFT in pharmaceuticals, such as particle design, drug solubilization, inclusion complex, polymer impregnation, polymorphism, drug extraction process, and analysis, are also covered in this review. The data collection methods are based on the recent literature related to drug delivery systems using SFT platforms. SFT has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This cutting-edge technology is growing predominantly to surrogate conventional unit operations in relevance to the pharmaceutical production process. Supercritical fluid technology has recently drawn attention in the field of pharmaceuticals. It is a distinct conception that utilizes the solvent properties of supercritical fluids above their critical temperature and pressure, where they exhibit both liquid-like and gas-like properties, which can enable many pharmaceutical applications. For example, the liquid-like properties provide benefits in extraction processes of organic solvents or impurities, drug solubilization, and polymer plasticization, and the gas-like features facilitate mass transfer processes. It has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This review is focused on different techniques that use supercritical fluids and their opportunities for the pharmaceutical sector.

Comparative study between extraction techniques and column separation for the quantification of sinigrin and total isothiocyanates in mustard seed.

PubMed

Cools, Katherine; Terry, Leon A

2012-07-15

Glucosinolates are β-thioglycosides which are found naturally in Cruciferae including the genus Brassica. When enzymatically hydrolysed, glucosinolates yield isothiocyanates and give a pungent taste. Both glucosinolates and isothiocyanates have been linked with anticancer activity as well as antifungal and antibacterial properties and therefore the quantification of these compounds is scientifically important. A wide range of literature exists on glucosinolates, however the extraction and quantification procedures differ greatly resulting in discrepancies between studies. The aim of this study was therefore to compare the most popular extraction procedures to identify the most efficacious method and whether each extraction can also be used for the quantification of total isothiocyanates. Four extraction techniques were compared for the quantification of sinigrin from mustard cv. Centennial (Brassica juncea L.) seed; boiling water, boiling 50% (v/v) aqueous acetonitrile, boiling 100% methanol and 70% (v/v) aqueous methanol at 70 °C. Prior to injection into the HPLC, the extractions which involved solvents (acetonitrile or methanol) were freeze-dried and resuspended in water. To identify whether the same extract could be used to measure total isothiocyanates, a dichloromethane extraction was carried out on the sinigrin extracts. For the quantification of sinigrin alone, boiling 50% (v/v) acetonitrile was found to be the most efficacious extraction solvent of the four tested yielding 15% more sinigrin than the water extraction. However, the removal of the acetonitrile by freeze-drying had a negative impact on the isothiocyanate content. Quantification of both sinigrin and total isothiocyanates was possible when the sinigrin was extracted using boiling water. Two columns were compared for the quantification of sinigrin revealing the Zorbax Eclipse to be the best column using this particular method. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of Different Solvents on the Measurement of Phenolics and the Antioxidant Activity of Mulberry (Morus atropurpurea Roxb.) with Accelerated Solvent Extraction.

PubMed

Yang, Jiufang; Ou, XiaoQun; Zhang, Xiaoxu; Zhou, ZiYing; Ma, LiYan

2017-03-01

The effects of 9 different solvents on the measurement of the total phenolics and antioxidant activities of mulberry fruits were studied using accelerated solvent extraction (ASE). Sixteen to 22 types of phenolics (flavonols, flavan-3-ols, flavanol, hydroxycinnamic acids, hydroxybenzoic acids, and stilbenes) from different mulberry extracts were characterized and quantified using HPLC-MS/MS. The principal component analysis (PCA) was used to determine the suitable solvents to distinguish between different classes of phenolics. Additionally, the phenolic extraction abilities of ASE and ultrasound-assisted extraction (UAE) were compared. The highest extraction efficiency could be achieved by using 50% acidified methanol (50MA) as ASE solvents with 15.14 mg/gallic acid equivalents g dry weight of mulberry fruit. The PCA results revealed that the 50MA followed by 50% acidified acetone (50AA) was the most efficient solvent for the extraction of phenolics, particularly flavonols (627.12 and 510.31 μg/g dry weight, respectively), while water (W) was not beneficial to the extraction of all categories of phenolics. Besides, the results of 3 antioxidant capability assays (DPPH, ABTS free radical-scavenging assay, and ferric-reducing antioxidant power assay) showed that water-based organic solvents increased the antioxidant capabilities of the extracts compared with water or pure organic solvents. ASE was more suitable for the extraction of phenolics than UAE. © 2017 Institute of Food Technologists®.

Determination of 129I in environmental samples by AMS and NAA using an anion exchange resin disk

NASA Astrophysics Data System (ADS)

Suzuki, Takashi; Banba, Shigeru; Kitamura, Toshikatsu; Kabuto, Shoji; Isogai, Keisuke; Amano, Hikaru

2007-06-01

We have developed a new extraction method for the measurement of 129I by accelerator mass spectrometry (AMS) utilizing an anion exchange resin disk. In comparison to traditional methods such as solvent extraction and ion exchange, this method provides for simple and quick sample handling. This extraction method was tested on soil, seaweed and milk samples, but because of disk clogging, the milk samples and some of the seaweed could not be applied successfully. Using this new extraction method to prepare samples for AMS analysis produced isotope ratios of iodine in good agreement with neutron activation analysis (NAA). The disk extraction method which take half an hour is faster than previous techniques, such as solvent extraction or ion exchange which take a few hours. The combination of the disk method and the AMS measurement is a powerful tool for the determination of 129I. Furthermore, these data will be available for the environmental monitoring before and during the operation of a new nuclear fuel reprocessing plant in Japan.

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

PubMed

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

2014-04-01

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

A cell extraction method for oily sediments

NASA Astrophysics Data System (ADS)

Lappé, M.; Kallmeyer, J.

2012-04-01

Hydrocarbons can be found in many different habitats and represent an important carbon source for microbes. As fossil fuels, they are an important economical resource and, through natural seepage or accidental release, they can be major pollutants. Oil sands from Alberta, Canada, and samples from the seafloor of the Gulf of Mexico represent typical examples of either natural or anthropogenically affected oily sediments. DNA-specific stains and molecular probes bind to hydrocarbons, causing massive background fluorescence and thereby massively hampering cell enumeration. The cell extraction procedure of Kallmeyer et al. (2008) separates the cells from the sediment matrix, producing a sediment free cell extract that can then be used for subsequent staining and cell enumeration under a fluorescence microscope. In principle, this technique can also be used to separate cells from oily sediments, but it was not originally optimized for this application and does not provide satisfactory results. Here we present a modified extraction method in which the hydrocarbons are removed prior to cell extraction by a solvent treatment. Due to the reduced background fluorescence the microscopic image becomes clearer, making cell identification and enumeration much easier. Consequently, the resulting cell counts from oily samples treated according to our new protocol were significantly higher than those treated according to Kallmeyer et al. (2008). We tested different amounts of a variety of solvents for their ability to remove hydrocarbons and found that n-hexane and - in samples containing more biodegraded oils - methanol, delivered the best results. Because solvents also tend to lyse cells, it was important to find the optimum solvent to sample ratio, at which the positive effect of hydrocarbon extraction overcomes the negative effect of cell lysis. A volumetric ratio of 1:2 to 1:5 between a formalin-fixed sediment slurry and solvent delivered highest cell counts. Extraction efficiency was around 30 to 50% and was checked on both oily samples spiked with known amounts of E.coli cells and oil-free samples amended with non-biodegraded and biodegraded oil. The method provided reproducible results on samples containing very different kinds of oils with regard to their degree of biodegradation. For strongly biodegraded oils, like those from the Alberta oil sands, methanol turned out to be the most appropriate solvent. For less biodegraded oils, like those from sediments from the Gulf of Mexico, n-hexane delivered best results. The relative amount of polar groups increases with an increasing level of biodegradation. Therefore polar solvents like methanol are better suited to dissolve biodegraded oils than less polar solvents like n-hexane. Our new method only provides a minimum estimate of cell abundance, as some cells are either lysed by the solvent treatment or remain attached to mineral grains and therefore do not end up in the cell extract but remain in the sediment pellet which will not be used for further microbiological analysis.

Switchable hydrophilicity solvents for lipid extraction from microalgae for biofuel production.

PubMed

Boyd, Alaina R; Champagne, Pascale; McGinn, Patrick J; MacDougall, Karen M; Melanson, Jeremy E; Jessop, Philip G

2012-08-01

A switchable hydrophilicity solvent (SHS) was studied for its effectiveness at extracting lipids from freeze-dried samples of Botryococcus braunii microalgae. The SHS N,N-dimethylcyclohexylamine extracted up to 22 wt.% crude lipid relative to the freeze-dried cell weight. The solvent was removed from the extract with water saturated with carbon dioxide at atmospheric pressure and recovered from the water upon de-carbonation of the mixture. Liquid chromatography-mass spectrometry (LC-MS) showed that the extracted lipids contained high concentrations of long chain tri-, di- and mono-acylglycerols, no phospholipids, and only 4-8% of residual solvent. Unlike extractions with conventional organic solvents, this new method requires neither distillation nor the use of volatile, flammable or chlorinated organic solvents. Copyright © 2012 Elsevier Ltd. All rights reserved.

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

PubMed

Kaykhaii, Massoud; Sargazi, Mona

2014-01-01

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

Analytical validation applied to simultaneous determination of solvents dichloromethane (DCM), methyl isobutyl ketone (MIBK), tetrahydrofuran (THF) and toluene (TOL) in urine by headspace extraction and injection on chromatographic system with a flame ionization detector

NASA Astrophysics Data System (ADS)

Muna, E. D. M.; Pereira, R. P.

2016-07-01

The determination of the volatile organic solvents dichloromethane (DCM), methyl isobutyl ketone (MIBK), tetrahydrofuran (THF) and toluene (TOL) is applied on toxicological monitoring of employees in various industrial activities. The gas chromatography technique with flame ionization detector and headspace injection system has been applied. The analytical procedure developed allows the simultaneous determination of the above-mentioned solvents and the accuracy of the method was tested following the INMETRO guidelines through the DOQ-CGRE 008 Rev.04-July/2011.

Measurement of residual solvents in a drug substance by a purge-and-trap method.

PubMed

Lakatos, Miklós

2008-08-05

The purge-and-trap (P&T) gas extraction method combined with gas chromatography was studied for its suitability for quantitative residual solvents determination in a water-soluble active pharmaceutical ingredient (API). Some analytical method performance characteristics were investigated, namely, the repeatability, the accuracy and the detection limit of determination. The results show that the P&T technique is--as expected--more sensitive than the static headspace, thus it can be used for the determination of residual solvents pertaining to the ICH Class 1 group. It was found that it could be an alternative sample preparation method besides the static headspace (HS) method.

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

EPA Science Inventory

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

Supercritical CO₂assisted extraction and LC-MS identification of picroside I and picroside II from Picrorhiza kurroa.

PubMed

Patil, Ajit A; Sachin, Bhusari S; Shinde, Devanand B; Wakte, Pravin S

2013-02-01

Picroside I and picroside II have been studied intensively because of their pharmacological actions and clinical applications. Numerous methods have been reported for extracting picroside I and picroside II from Picrorrhiza. kurroa rhizomes. This is the first report of picroside I and picroside II extraction using the supercritical carbon dioxide assisted extraction technique. To develop supercritical carbon dioxide assisted extraction and LC-MS identification of picroside I and picroside II from the Picrorrhiza kurroa Royle rhizomes. Surface response methodology based on 3³ fractional factorial design was used to extract picroside I and picroside II from P. kurroa rhizomes. The effects of various process factors, namely temperature (40-80°C), pressure (25-35 MPa) and co-solvent (methanol) concentration (0-10% v/v) on extraction yield of the two compounds were evaluated. The picroside I and picroside II contents were determined using validated LC-MS methodology. The maximum yield of picroside I (32.502 ± 1.131 mg/g) and picroside II (9.717 ± 0.382 mg/g) was obtained at the 10% v/v co-solvent concentration, 40°C temperature and 30 MPa pressure. The conventional Soxhlet assisted methanol extract of P. kurroa powder resulted in 36.743 ± 1.75 and 11.251 ± 0.54 mg/g yield of picroside I and picroside II, respectively. Variation of concentration and extraction time showed a significant effect on the picroside I and picroside II yield. Supercritical carbon dioxide assisted extraction using methanol as a co-solvent is an efficient and environmentally sustainable method for extracting picroside I and picroside II from P. kurroa rhizomes. Copyright © 2012 John Wiley & Sons, Ltd.

Modeling and prediction of extraction profile for microwave-assisted extraction based on absorbed microwave energy.

PubMed

Chan, Chung-Hung; Yusoff, Rozita; Ngoh, Gek-Cheng

2013-09-01

A modeling technique based on absorbed microwave energy was proposed to model microwave-assisted extraction (MAE) of antioxidant compounds from cocoa (Theobroma cacao L.) leaves. By adapting suitable extraction model at the basis of microwave energy absorbed during extraction, the model can be developed to predict extraction profile of MAE at various microwave irradiation power (100-600 W) and solvent loading (100-300 ml). Verification with experimental data confirmed that the prediction was accurate in capturing the extraction profile of MAE (R-square value greater than 0.87). Besides, the predicted yields from the model showed good agreement with the experimental results with less than 10% deviation observed. Furthermore, suitable extraction times to ensure high extraction yield at various MAE conditions can be estimated based on absorbed microwave energy. The estimation is feasible as more than 85% of active compounds can be extracted when compared with the conventional extraction technique. Copyright © 2013 Elsevier Ltd. All rights reserved.

Solvent vapour monitoring in work space by solid phase micro extraction.

PubMed

Li, K; Santilli, A; Goldthorp, M; Whiticar, S; Lambert, P; Fingas, M

2001-05-07

Solid phase micro extraction (SPME) is a fast, solvent-less alternative to conventional charcoal tube sampling/carbon disulfide extraction for volatile organic compounds (VOC). In this work, SPME was compared to the active sampling technique in a typical lab atmosphere. Two different types of fibre coatings were evaluated for solvent vapour at ambient concentration. A general purpose 100 microm film polydimethylsiloxane (PDMS) fibre was found to be unsuitable for VOC work, despite the thick coating. The mixed-phase carboxen/PDMS fibre was found to be suitable. Sensitivity of the SPME was far greater than charcoal sorbent tube method. Calibration studies using typical solvent such as dichloromethane (DCM), benzene (B) and toluene (T) showed an optimal exposure time of 5 min, with a repeatability of less than 20% for a broad spectrum of organic vapour. Minimum detectable amount for DCM is in the range of 0.01 microg/l (0.003 ppmv). Variation among different fibres was generally within 30% at a vapour concentration of 1 microg DCM/l, which was more than adequate for field monitoring purpose. Adsorption characteristics and calibration procedures were studied. An actual application of SPME was carried out to measure background level of solvent vapour at a bench where DCM was used extensively. Agreement between the SPME and the charcoal sampling method was generally within a factor of two. No DCM concentration was found to be above the regulatory limit of 50 ppmv.

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

PubMed

Shen, Jinchao; Shao, Xueguang

2005-11-01

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

A comparative analysis of modified binders : original asphalts and materials extracted from existing pavements.

DOT National Transportation Integrated Search

2010-01-18

This research demonstrated the application of gel permeation chromatography (GPC) as an analytical tool to : ascertain the amounts of polymer modifiers in polymer modified asphalt cements, which are soluble in eluting GPC : solvents. The technique wa...

A Comparative Analysis of Modified Binders : Original Asphalt and Material Extracted from Existing Pavement

DOT National Transportation Integrated Search

2010-01-18

This research demonstrated the application of gel permeation chromatography (GPC) as an analytical tool to ascertain the amounts of polymer modifiers in polymer modified asphalt cements, which are soluble in eluting GPC solvents. The technique was ap...

Binary Solvents Dispersive Liquid-Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography.

PubMed

Kiarostami, Vahid; Rouini, Mohamad-Reza; Mohammadian, Razieh; Lavasani, Hoda; Ghazaghi, Mehri

2014-02-03

Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 - 99.6%. Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

Binary Solvents Dispersive Liquid—Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography

PubMed Central

2014-01-01

Background Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Results Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 – 99.6%. Conclusions Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories. PMID:24495475

[Advances in studies on multi-stage countercurrent extraction technology in traditional Chinese medicine].

PubMed

Xie, Zhi-Peng; Liu, Xue-Song; Chen, Yong; Cai, Ming; Qu, Hai-Bin; Cheng, Yi-Yu

2007-05-01

Multi-stage countercurrent extraction technology, integrating solvent extraction, repercolation with dynamic and countercurrent extraction, is a novel extraction technology for the traditional Chinese medicine. This solvent-saving, energy-saving and high-extraction-efficiency technology can at the most drive active compounds to diffuse from the herbal materials into the solvent stage by stage by creating concentration differences between the herbal materials and the solvents. This paper reviewed the basic principle, the influence factors and the research progress and trends of the equipments and the application of the multi-stage countercurrent extraction.

Optimization of microwave-assisted extraction of hydrocarbons in marine sediments: comparison with the Soxhlet extraction method.

PubMed

Vázquez Blanco, E; López Mahía, P; Muniategui Lorenzo, S; Prada Rodríguez, D; Fernández Fernández, E

2000-02-01

Microwave energy was applied to extract polycyclic aromatic hydrocarbons (PAHs) and linear aliphatic hydrocarbons (LAHs) from marine sediments. The influence of experimental conditions, such as different extracting solvents and mixtures, microwave power, irradiation time and number of samples extracted per run has been tested using real marine sediment samples; volume of the solvent, sample quantity and matrix effects were also evaluated. The yield of extracted compounds obtained by microwave irradiation was compared with that obtained using the traditional Soxhlet extraction. The best results were achieved with a mixture of acetone and hexane (1:1), and recoveries ranged from 92 to 106%. The extraction time is dependent on the irradiation power and the number of samples extracted per run, so when the irradiation power was set to 500 W, the extraction times varied from 6 min for 1 sample to 18 min for 8 samples. Analytical determinations were carried out by high-performance liquid chromatography (HPLC) with an ultraviolet-visible photodiode-array detector for PAHs and gas chromatography (GC) using a FID detector for LAHs. To test the accuracy of the microwave-assisted extraction (MAE) technique, optimized methodology was applied to the analysis of standard reference material (SRM 1941), obtaining acceptable results.

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

PubMed

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

2018-05-02

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

A comparative study: the impact of different lipid extraction methods on current microalgal lipid research

PubMed Central

2014-01-01

Microalgae cells have the potential to rapidly accumulate lipids, such as triacylglycerides that contain fatty acids important for high value fatty acids (e.g., EPA and DHA) and/or biodiesel production. However, lipid extraction methods for microalgae cells are not well established, and there is currently no standard extraction method for the determination of the fatty acid content of microalgae. This has caused a few problems in microlagal biofuel research due to the bias derived from different extraction methods. Therefore, this study used several extraction methods for fatty acid analysis on marine microalga Tetraselmis sp. M8, aiming to assess the potential impact of different extractions on current microalgal lipid research. These methods included classical Bligh & Dyer lipid extraction, two other chemical extractions using different solvents and sonication, direct saponification and supercritical CO2 extraction. Soxhlet-based extraction was used to weigh out the importance of solvent polarity in the algal oil extraction. Coupled with GC/MS, a Thermogravimetric Analyser was used to improve the quantification of microalgal lipid extractions. Among these extractions, significant differences were observed in both, extract yield and fatty acid composition. The supercritical extraction technique stood out most for effective extraction of microalgal lipids, especially for long chain unsaturated fatty acids. The results highlight the necessity for comparative analyses of microalgae fatty acids and careful choice and validation of analytical methodology in microalgal lipid research. PMID:24456581

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

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

PubMed

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

2007-07-01

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

Separation of major catechins from green tea by ultrahigh pressure extraction.

PubMed

Jun, Xi; Shuo, Zhao; Bingbing, Lu; Rui, Zhang; Ye, Li; Deji, Shen; Guofeng, Zhou

2010-02-15

This study presents a novel extraction technique, ultrahigh pressure extraction, to obtain major catechins from green tea leaves. The effects of various high pressure level (100, 200, 300, 400, 500, 600 MPa) on the extract are examined. HPLC chromatographic analyses determine the concentration of four major catechins and caffeine. The extraction yields of active ingredients with ultrahigh pressure extraction (400 MPa pressure) for only 15 min were given the same as those of organic solvent extraction for 2h. These excellent results for the ultrahigh pressure extraction are promising for the future separation of active ingredients from traditional Chinese herbal medicine. Copyright 2009 Elsevier B.V. All rights reserved.

Metabolomic analysis-Addressing NMR and LC-MS related problems in human feces sample preparation.

PubMed

Moosmang, Simon; Pitscheider, Maria; Sturm, Sonja; Seger, Christoph; Tilg, Herbert; Halabalaki, Maria; Stuppner, Hermann

2017-10-31

Metabolomics is a well-established field in fundamental clinical research with applications in different human body fluids. However, metabolomic investigations in feces are currently an emerging field. Fecal sample preparation is a demanding task due to high complexity and heterogeneity of the matrix. To gain access to the information enclosed in human feces it is necessary to extract the metabolites and make them accessible to analytical platforms like NMR or LC-MS. In this study different pre-analytical parameters and factors were investigated i.e. water content, different extraction solvents, influence of freeze-drying and homogenization, ratios of sample weight to extraction solvent, and their respective impact on metabolite profiles acquired by NMR and LC-MS. The results indicate that profiles are strongly biased by selection of extraction solvent or drying of samples, which causes different metabolites to be lost, under- or overstated. Additionally signal intensity and reproducibility of the measurement were found to be strongly dependent on sample pre-treatment steps: freeze-drying and homogenization lead to improved release of metabolites and thus increased signals, but at the same time induced variations and thus deteriorated reproducibility. We established the first protocol for extraction of human fecal samples and subsequent measurement with both complementary techniques NMR and LC-MS. Copyright © 2017 Elsevier B.V. All rights reserved.

Phenolic Extracts from Wild Olive Leaves and Their Potential as Edible Oils Antioxidants

PubMed Central

Lafka, Theodora-Ioanna; Lazou, Andriana E.; Sinanoglou, Vassilia J.; Lazos, Evangelos S.

2013-01-01

The kinetics solid-liquid extraction of phenolics from wild olive leaves was elaborated using different mathematical models (Peleg, second order, Elovich, and power law model). As solvents, methanol, ethanol, ethanol:water 1:1, n-propanol, isopropanol and ethyl acetate were used. The second order model best described the solvent extraction process, followed by the Elovich model. The most effective solvent was ethanol with optimum phenol extraction conditions 180 min, solvent to sample ratio 5:1 v/w and pH 2. Ethanol extract exhibited the highest antiradical activity among solvent and supercritical fluid extraction (SFE) extracts, which in addition showed the highest antioxidant capacity compared to synthetic and natural food antioxidants such as BHT, ascorbyl palmitate and vitamin E. Antioxidant potential of SFE extract was quite high, although its phenolic potential was not. Leaf extracts were proven to be good protectors for olive and sunflower oils at levels of 150 ppm. PMID:28239093

Extraction optimization and UHPLC method development for determination of the 20-hydroxyecdysone in Sida tuberculata leaves.

PubMed

da Rosa, Hemerson S; Koetz, Mariana; Santos, Marí Castro; Jandrey, Elisa Helena Farias; Folmer, Vanderlei; Henriques, Amélia Teresinha; Mendez, Andreas Sebastian Loureiro

2018-04-01

Sida tuberculata (ST) is a Malvaceae species widely distributed in Southern Brazil. In traditional medicine, ST has been employed as hypoglycemic, hypocholesterolemic, anti-inflammatory and antimicrobial. Additionally, this species is chemically characterized by flavonoids, alkaloids and phytoecdysteroids mainly. The present work aimed to optimize the extractive technique and to validate an UHPLC method for the determination of 20-hydroxyecdsone (20HE) in the ST leaves. Box-Behnken Design (BBD) was used in method optimization. The extractive methods tested were: static and dynamic maceration, ultrasound, ultra-turrax and reflux. In the Box-Behnken three parameters were evaluated in three levels (-1, 0, +1), particle size, time and plant:solvent ratio. In validation method, the parameters of selectivity, specificity, linearity, limits of detection and quantification (LOD, LOQ), precision, accuracy and robustness were evaluated. The results indicate static maceration as better technique to obtain 20HE peak area in ST extract. The optimal extraction from surface response methodology was achieved with the parameters granulometry of 710 nm, 9 days of maceration and plant:solvent ratio 1:54 (w/v). The UHPLC-PDA analytical developed method showed full viability of performance, proving to be selective, linear, precise, accurate and robust for 20HE detection in ST leaves. The average content of 20HE was 0.56% per dry extract. Thus, the optimization of extractive method in ST leaves increased the concentration of 20HE in crude extract, and a reliable method was successfully developed according to validation requirements and in agreement with current legislation. Copyright © 2018 Elsevier Inc. All rights reserved.

A highly selective dispersive liquid-liquid microextraction approach based on the unique fluorous affinity for the extraction and detection of per- and polyfluoroalkyl substances coupled with high performance liquid chromatography tandem-mass spectrometry.

PubMed

Wang, Juan; Shi, Yali; Cai, Yaqi

2018-04-06

In the present study, a highly selective fluorous affinity-based dispersive liquid-liquid microextraction (DLLME) technique was developed for the extraction and analysis of per- and polyfluoroalkyl substances (PFASs) followed by high performance liquid chromatography tandem-mass spectrometry. Perfluoro-tert-butanol with multiple C-F bonds was chosen as the extraction solvent, which was injected into the aqueous samples with a dispersive solvent (acetonitrile) in a 120:800 (μL, v/v) mixture for PFASs enrichment. The fluorous affinity-based extraction mechanism was confirmed by the significantly higher extraction recoveries for PFASs containing multiple fluorine atoms than those for compounds with fewer or no fluorine atoms. The extraction recoveries of medium and long-chain PFASs (CF 2  > 5) exceeded 70%, except perfluoroheptanoic acid, while those of short-chain PFASs were lower than 50%, implying that the proposed DLLME may not be suitable for their extraction due to weak fluorous affinity. This highly fluoroselective DLLME technique can greatly decrease the matrix effect that occurs in mass spectrometry detection when applied to the analysis of urine samples. Under the optimum conditions, the relative recoveries of PFASs with CF 2  > 5 ranged from 80.6-121.4% for tap water, river water and urine samples spiked with concentrations of 10, 50 and 100 ng/L. The method limits of quantification for PFASs in water and urine samples were in the range of 0.6-8.7 ng/L. Furthermore, comparable concentrations of PFASs were obtained via DLLME and solid-phase extraction, confirming that the developed DLLME technique is a promising method for the extraction of PFASs in real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Comprehensive identification of bioactive compounds of avocado peel by liquid chromatography coupled to ultra-high-definition accurate-mass Q-TOF.

PubMed

Figueroa, Jorge G; Borrás-Linares, Isabel; Lozano-Sánchez, Jesús; Segura-Carretero, Antonio

2018-04-15

Industrially the avocado pulp is exploited principally as oil and paste, generating a huge quantity of peel and seed as by-products. Avocado peel is a promising inexpensive candidate for recovery phenolic compounds. The aim of this work was to identify the bioactive compounds present in an extract of avocado peel obtained by a green extraction technique. Accelerated solvent extraction was performed using water and ethanol as extraction solvents. Liquid chromatography coupled to ultra-high-definition accurate-mass spectrometry was used in order to identify the bioactive compounds. A total of sixty-one compounds belonging to eleven families were identified. Procyanidins, flavonols, hydroxybenzoic and hydroxycinnamic acids were the most common compounds. A sum of thirty-five compounds has been identified here for the first time in avocado peel. These results confirm the potential of avocado peel as a source of bioactive ingredients for its use in the food, cosmetic or pharmaceutical sector. Copyright © 2017 Elsevier Ltd. All rights reserved.

Recovery of bioactive molecules from chestnut (Castanea sativa Mill.) by-products through extraction by different solvents.

PubMed

Vella, Filomena Monica; Laratta, Bruna; La Cara, Francesco; Morana, Alessandra

2018-05-01

The underutilised forest and industrial biomass of Castanea sativa (Mill.) is generally discarded during post-harvest and food processing, with high impact on environmental quality. The searching on alternative sources of natural antioxidants from low-cost supplies, by methods involving environment-friendly techniques, has become a major goal of numerous researches in recent times. The aim of the present study was the set-up of a biomolecules extraction procedure from chestnut leaves, burs and shells and the assessing of their potential antioxidant activity. Boiling water was the best extraction solvent referring to polyphenols from chestnut shells and burs, whereas the most efficient for leaves resulted 60% ethanol at room temperature. Greatest polyphenol contents were 90.35, 60.01 and 17.68 mg gallic acid equivalents g -1 in leaves, burs and shells, respectively. Moreover, flavonoids, tannins and antioxidant activity were assessed on the best extract obtained from each chestnut by-product.

Step-wise supercritical extraction of carbonaceous residua

DOEpatents

Warzinski, Robert P.

1987-01-01

A method of fractionating a mixture containing high boiling carbonaceous material and normally solid mineral matter includes processing with a plurality of different supercritical solvents. The mixture is treated with a first solvent of high critical temperature and solvent capacity to extract a large fraction as solute. The solute is released as liquid from solvent and successively treated with other supercritical solvents of different critical values to extract fractions of differing properties. Fractionation can be supplemented by solute reflux over a temperature gradient, pressure let down in steps and extractions at varying temperature and pressure values.

Comparison of extraction methods for quantifying vitamin E from animal tissues.

PubMed

Xu, Zhimin

2008-12-01

Four extraction methods: (1) solvent (SOL), (2) ultrasound assisted solvent (UA), (3) saponification and solvent (SP), and (4) saponification and ultrasound assisted solvent (SP-UA), were used in sample preparation for quantifying vitamin E (tocopherols) in chicken liver and plasma samples. The extraction yields of SOL, UA, SP, and SP-UA methods obtained by adding delta-tocopherol as internal reference were 95%, 104%, 65%, and 62% for liver and 98%, 103%, 97%, and 94% for plasma, respectively. The methods with saponification significantly affected the stabilities of tocopherols in liver samples. The measured values of alpha- and gamma-tocopherols using the solvent only extraction (SOL) method were much lower than that using any of the other extraction methods. This indicated that less of the tocopherols in those samples were in a form that could be extracted directly by solvent. The measured value of alpha-tocopherol in the liver sample using the ultrasound assisted solvent (UA) method was 1.5-2.5 times of that obtained from the saponification and solvent (SP) method. The differences in measured values of tocopherols in the plasma samples by using the two methods were not significant. However, the measured value of the saponification and ultrasound assisted solvent (SP-UA) method was lower than either the saponification and solvent (SP) or the ultrasound assisted solvent (UA) method. Also, the reproducibility of the ultrasound assisted solvent (UA) method was greater than any of the saponification methods. Compared with the traditional saponification method, the ultrasound assisted solvent method could effectively extract tocopherols from sample matrix without any chemical degradation reactions, especially for complex animal tissue such as liver.

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

PubMed

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

2015-12-11

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

Extraction, Scrub, and Strip Test Results for the Salt Waste Processing Facility Caustic Side Solvent Extraction Solvent Sample

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

Peters, T. B.

An Extraction, Scrub, and Strip (ESS) test was performed on a sample of Salt Waste Processing Facility (SWPF) Caustic-Side Solvent Extraction (CSSX) solvent and salt simulant to determine cesium distribution ratios (D( Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams; this data will be used by Parsons to help determine if the solvent is qualified for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations. The extraction D( Cs) measured 12.5, exceeding the required value of 8. This value is consistent with resultsmore » from previous ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges. This revision was created to correct an error. The previous revision used an incorrect set of temperature correction coefficients which resulted in slight deviations from the correct D( Cs) results.« less

Crystallography of ordered colloids using optical microscopy. 2. Divergent-beam technique.

PubMed

Rogers, Richard B; Lagerlöf, K Peter D

2008-04-10

A technique has been developed to extract quantitative crystallographic data from randomly oriented colloidal crystals using a divergent-beam approach. This technique was tested on a series of diverse experimental images of colloidal crystals formed from monodisperse suspensions of sterically stabilized poly-(methyl methacrylate) spheres suspended in organic index-matching solvents. Complete sets of reciprocal lattice basis vectors were extracted in all but one case. When data extraction was successful, results appeared to be accurate to about 1% for lattice parameters and to within approximately 2 degrees for orientation. This approach is easier to implement than a previously developed parallel-beam approach with the drawback that the divergent-beam approach is not as robust in certain situations with random hexagonal close-packed crystals. The two techniques are therefore complimentary to each other, and between them it should be possible to extract quantitative crystallographic data with a conventional optical microscope from any closely index-matched colloidal crystal whose lattice parameters are compatible with visible wavelengths.

Alternative Solvents through Green Chemistry Project

NASA Technical Reports Server (NTRS)

Hintze, Paul E.; Quinn, Jacqueline

2014-01-01

Components in the aerospace industry must perform with accuracy and precision under extreme conditions, and surface contamination can be detrimental to the desired performance, especially in cases when the components come into contact with strong oxidizers such as liquid oxygen. Therefore, precision cleaning is an important part of a components preparation prior to utilization in aerospace applications. Current cleaning technologies employ a variety of cleaning agents, many of which are halogenated solvents that are either toxic or cause environmental damage. Thus, this project seeks to identify alternative precision cleaning solvents and technologies, including use of less harmful cleaning solvents, ultrasonic and megasonic agitation, low-pressure plasma cleaning techniques, and supercritical carbon dioxide extraction. Please review all data content found in the Public Data tab located at: https:techport.nasa.govview11697public

Solid-phase microextraction of methadone in urine samples by electrochemically co-deposited sol-gel/Cu nanocomposite fiber.

PubMed

Mohammadiazar, Sirwan; Hasanli, Fateme; Maham, Mehdi; Payami Samarin, Somayeh

2017-08-01

Electrochemically co-deposited sol-gel/Cu nanocomposites have been introduced as a novel, simple and single-step technique for preparation of solid-phase microextraction (SPME) coating to extract methadone (MDN) (a synthetic opioid) in urine samples. The porous surface structure of the sol-gel/Cu nanocomposite coating was revealed by scanning electron microscopy. Direct immersion SPME followed by HPLC-UV determination was employed. The factors influencing the SPME procedure, such as the salt content, desorption solvent type, pH and equilibration time, were optimized. The best conditions were obtained with no salt content, acetonitrile as desorption solvent type, pH 9 and 10 min equilibration time. The calibration graphs for urine samples showed good linearity. The detection limit was about 0.2 ng mL -1 . Also, the novel method for preparation of nanocomposite fiber was compared with previously reported techniques for MDN determination. The results show that the novel nanocomposite fiber has relatively high extraction efficiency. Copyright © 2016 John Wiley & Sons, Ltd.

Extraction, scrub, and strip test results for the solvent transfer to salt waste processing facility

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

Peters, T.

The Savannah River National Laboratory (SRNL) prepared approximately 240 gallons of Caustic-Side Solvent Extraction (CSSX) solvent for use at the Salt Waste Processing Facility (SWPF). An Extraction, Scrub, and Strip (ESS) test was performed on a sample of the prepared solvent using a salt solution prepared by Parsons to determine cesium distribution ratios (D(Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams. This data will be used by Parsons to help qualify the solvent for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations.more » The extraction D(Cs) measured 15.5, exceeding the required value of 8. This value is consistent with results from previous ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges.« less

Extracting organic matter on Mars: A comparison of methods involving subcritical water, surfactant solutions and organic solvents

NASA Astrophysics Data System (ADS)

Luong, Duy; Court, Richard W.; Sims, Mark R.; Cullen, David C.; Sephton, Mark A.

2014-09-01

The first step in many life detection protocols on Mars involves attempts to extract or isolate organic matter from its mineral matrix. A number of extraction options are available and include heat and solvent assisted methods. Recent operations on Mars indicate that heating samples can cause the loss or obfuscation of organic signals from target materials, raising the importance of solvent-based systems for future missions. Several solvent types are available (e.g. organic solvents, surfactant based solvents and subcritical water extraction) but a comparison of their efficiencies in Mars relevant materials is missing. We have spiked the well characterised Mars analogue material JSC Mars-1 with a number of representative organic standards. Extraction of the spiked JSC Mars-1 with the three solvent methods provides insights into the relative efficiency of these methods and indicates how they may be used on future Mars missions.

Evaluation of various solvent systems for lipid extraction from wet microalgal biomass and its effects on primary metabolites of lipid-extracted biomass.

PubMed

Ansari, Faiz Ahmad; Gupta, Sanjay Kumar; Shriwastav, Amritanshu; Guldhe, Abhishek; Rawat, Ismail; Bux, Faizal

2017-06-01

Microalgae have tremendous potential to grow rapidly, synthesize, and accumulate lipids, proteins, and carbohydrates. The effects of solvent extraction of lipids on other metabolites such as proteins and carbohydrates in lipid-extracted algal (LEA) biomass are crucial aspects of algal biorefinery approach. An effective and economically feasible algae-based oil industry will depend on the selection of suitable solvent/s for lipid extraction, which has minimal effect on metabolites in lipid-extracted algae. In current study, six solvent systems were employed to extract lipids from dry and wet biomass of Scenedesmus obliquus. To explore the biorefinery concept, dichloromethane/methanol (2:1 v/v) was a suitable solvent for dry biomass; it gave 18.75% lipids (dry cell weight) in whole algal biomass, 32.79% proteins, and 24.73% carbohydrates in LEA biomass. In the case of wet biomass, in order to exploit all three metabolites, isopropanol/hexane (2:1 v/v) is an appropriate solvent system which gave 7.8% lipids (dry cell weight) in whole algal biomass, 20.97% proteins, and 22.87% carbohydrates in LEA biomass. Graphical abstract: Lipid extraction from wet microalgal biomass and biorefianry approach.

Comparative analysis of volatiles in traditionally cured Bourbon and Ugandan vanilla bean ( Vanilla planifolia ) extracts.

PubMed

Zhang, Suying; Mueller, Christoph

2012-10-24

Traditionally cured vanilla beans ( Vanilla planifolia ) from Madagascar and Uganda were extracted with organic solvents, and the volatiles were separated from the nonvolatile fraction using the solvent assisted flavor evaporation (SAFE) technique. Concentrated vanilla bean extracts were analyzed using GC-MS and GC-O. Two hundred and forty-six volatile compounds were identified using the Automated Mass Spectral Deconvolution and Identification System (AMDIS) software, of which 13 were confirmed with authentic compounds from commercial sources and the others were tentatively identified on the basis of calibrated linear retention indices and the comparison of deconvoluted mass spectra with the in-house and/or NIST spectra databases. Vanillin was the most abundant constituent followed by guaiacol. The total concentration of the volatile compounds, excluding vanillin, was 301 mg/kg for Bourbon and 398 mg/kg for Ugandan vanilla bean extracts. Analytical comparison between the two vanilla bean extracts was discussed. Seventy-eight compounds were identified as odor-active compounds in the vanilla bean extracts with 10 confirmed with authentic references. It was found that there were substantial analytical differences in the odor-active compounds of the two extracts.

Highly efficient extraction of anthocyanins from grape skin using deep eutectic solvents as green and tunable media.

PubMed

Jeong, Kyung Min; Zhao, Jing; Jin, Yan; Heo, Seong Rok; Han, Se Young; Yoo, Da Eun; Lee, Jeongmi

2015-12-01

Deep eutectic solvents (DESs) were investigated as tunable, environmentally benign, yet superior extraction media to enhance the extraction of anthocyanins from grape skin, which is usually discarded as waste. Ten DESs containing choline chloride as hydrogen bond acceptor combined with different hydrogen bond donors were screened for high extraction efficiencies based on the anthocyanin extraction yields. As a result, citric acid, D-(+)-maltose, and fructose were selected as the effective DES components, and the newly designed DES, CM-6 that is composed of citric acid and D-(+)-maltose at 4:1 molar ratio, exhibited significantly higher levels of anthocyanin extraction yields than conventional extraction solvents such as 80% aqueous methanol. The final extraction method was established based on the ultrasound-assisted extraction under conditions optimized using response surface methodology. Its extraction yields were double or even higher than those of conventional methods that are time-consuming and use volatile organic solvents. Our method is truly a green method for anthocyanin extraction with great extraction efficiency using a minimal amount of time and solvent. Moreover, this study suggested that grape skin, the by-products of grape juice processing, could serve as a valuable source for safe, natural colorants or antioxidants by use of the eco-friendly extraction solvent, CM-6.

EXTRACTION AND DETECTION OF ARSENICALS IN SEAWEED VIA ACCELERATED SOLVENT EXTRACTION WITH ION CHROMATOGRAPHIC SEPARATION AND ICP-MS DETECTION

EPA Science Inventory

An accelerated solvent extraction (ASE) device was evaluated as a semi-automated means of extracting arsenicals from ribbon kelp. Objective was to investigate effect of experimentally controllable ASE parameters (pressure, temperature, static time and solvent composition) on extr...

Application of Ionic Liquids in the Microwave-Assisted Extraction of Proanthocyanidins from Larix gmelini Bark

PubMed Central

Yang, Lei; Sun, Xiaowei; Yang, Fengjian; Zhao, Chunjian; Zhang, Lin; Zu, Yuangang

2012-01-01

Ionic liquid based, microwave-assisted extraction (ILMAE) was successfully applied to the extraction of proanthocyanidins from Larix gmelini bark. In this work, in order to evaluate the performance of ionic liquids in the microwave-assisted extraction process, a series of 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were evaluated for extraction yield, and 1-butyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the ILMAE procedure for the proanthocyanidins was optimized and compared with other conventional extraction techniques. Under the optimized conditions, satisfactory extraction yield of the proanthocyanidins was obtained. Relative to other methods, the proposed approach provided higher extraction yield and lower energy consumption. The Larix gmelini bark samples before and after extraction were analyzed by Thermal gravimetric analysis, Fourier-transform infrared spectroscopy and characterized by scanning electron microscopy. The results showed that the ILMAE method is a simple and efficient technique for sample preparation. PMID:22606036

Supercritical solvent extraction of oil sand bitumen

NASA Astrophysics Data System (ADS)

Imanbayev, Ye. I.; Ongarbayev, Ye. K.; Tileuberdi, Ye.; Mansurov, Z. A.; Golovko, A. K.; Rudyk, S.

2017-08-01

The supercritical solvent extraction of bitumen from oil sand studied with organic solvents. The experiments were performed in autoclave reactor at temperature above 255 °C and pressure 29 atm with stirring for 6 h. The reaction resulted in the formation of coke products with mineral part of oil sands. The remaining products separated into SARA fractions. The properties of the obtained products were studied. The supercritical solvent extraction significantly upgraded extracted natural bitumen.

Solvent selection in ultrasonic-assisted emulsification microextraction: Comparison between high- and low-density solvents by means of novel type of extraction vessel.

PubMed

Nojavan, Saeed; Gorji, Tayebeh; Davarani, Saied Saeed Hosseiny; Morteza-Najarian, Amin

2014-08-01

There are numerous published reports about dispersive liquid phase microextraction of the wide range of substances, however, till now no broadly accepted systematic and purpose oriented selection of extraction solvent has been proposed. Most works deal with the optimization of available solvents without adequate pre-consideration of properness. In this study, it is tried to compare the performances of low- and high-density solvents at the same conditions by means of novel type of extraction vessel with head and bottom conical shape. Extraction efficiencies of seven basic pharmaceutical compounds using eighteen common organic solvents were studied in this work. It was much easier to work with high-density solvents and they mostly showed better performances. This work shows that although exact predicting the performance of the solvents is multifaceted case but the pre-consideration of initial selection of solvents with attention to the physiochemical properties of the desired analytes is feasible and promising. Finally, the practicality of the method for extraction from urine and plasma samples was investigated. Copyright © 2014 Elsevier B.V. All rights reserved.

Re-refining of waste petroleum by competing solubility characteristics

NASA Astrophysics Data System (ADS)

Byars, Michael Steven

1998-11-01

The United States produces over 1.3 billion gallons of used oil per year. Of the 1.3 billion gallons about 60% is used as fuel, nearly 20% is dumped into the environment, 13% is placed in landfills, 2% is re-refined into lube oil, and the remaining is either used for other purposes or incinerated. This is a great potential source of lubricating oil. The work presented here is a solvent extraction process using a solvent (highly miscible with the oil) and a co-solvent (slightly miscible with the oil). Extractions using isopropanol, ethanol, methyl tert-butylether and methanol are presented. The criteria used for evaluation of the extraction processes are yield, product viscosity index, and ash percent. The solvent/co-solvent combinations of MTBE and ethanol performed best and had the advantage of a common solvent/co-solvent in all extraction steps. The extraction process that provided the best results was a two step process using a combination solvent of MTBE and ethanol. The used oil was first extracted using MTBE/ethanol. The extracted oil was then contacted with a solvent combination composed of 80% ethanol. This solvent combination extracted the remaining additives from the oil. The recovered oil was nearly 60% by weight with a high viscosity index and no ash content. A preliminary battery limits design and economic analysis of the process was performed. A 500 bbl/day plant would have a capital cost of 1.9 million and an annual operation cost of 310,000. The plant as designed would produce 300 bbl/day of lube feedstock and have an ROI of 19%.

Separation of Gadolinium (Gd) using Synergic Solvent Mixed Topo-D2EHPA with Extraction Method.

NASA Astrophysics Data System (ADS)

Effendy, N.; Basuki, K. T.; Biyantoro, D.; Perwira, N. K.

2018-04-01

The main problem to obtain Gd with high purity is the similarity of chemical properties and physical properties with the other rare earth elements (REE) such as Y and Dy, it is necessary to do separation by the extraction process. The purpose of this research to determine the best solvent type, amount of solvent, feed and solvent ratio in the Gd extraction process, to determine the rate order and the value of the rate constant of Gd concentration based on experimental data of aqueous phase concentration as a function of time and to know the effect of temperature on the reaction speed constant. This research was conducted on variation of solvent, amount of solvent, feed and solvent ratio in the extraction process of Gd separation, extraction time to determine the order value and the rate constant of Gd concentration in extraction process based on the aqueous phase concentration data as a function of time, to the rate constant of decreasing concentration of Gd. Based on the calculation results, the solvent composition was obtained with the best feed to separate the rare earth elements Gd in the extraction process is 1 : 4 with 15% concentration of TOPO and 10% concentration of D2EHPA. The separation process of Gd using extraction method by solvent TOPO-D2EHPA 2 : 1 comparison is better than single solvent D2EHPA / TOPO because of the synergistic effect. The rate order of separation process of Gd follows order 1. The Arrhenius Gd equation becomes k = 1.46 x 10-7 exp (-6.96 kcal / mol / RT).

Terpenes as green solvents for extraction of oil from microalgae.

PubMed

Dejoye Tanzi, Celine; Abert Vian, Maryline; Ginies, Christian; Elmaataoui, Mohamed; Chemat, Farid

2012-07-09

Herein is described a green and original alternative procedure for the extraction of oil from microalgae. Extractions were carried out using terpenes obtained from renewable feedstocks as alternative solvents instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using Soxhlet extraction followed by the elimination of the solvent from the medium using Clevenger distillation in the second step. Oils extracted from microalgae were compared in terms of qualitative and quantitative determination. No significant difference was obtained between each extract, allowing us to conclude that the proposed method is green, clean and efficient.

The optimization of essential oils supercritical CO2 extraction from Lavandula hybrida through static-dynamic steps procedure and semi-continuous technique using response surface method

PubMed Central

Kamali, Hossein; Aminimoghadamfarouj, Noushin; Golmakani, Ebrahim; Nematollahi, Alireza

2015-01-01

Aim: The aim of this study was to examine and evaluate crucial variables in essential oils extraction process from Lavandula hybrida through static-dynamic and semi-continuous techniques using response surface method. Materials and Methods: Essential oil components were extracted from Lavandula hybrida (Lavandin) flowers using supercritical carbon dioxide via static-dynamic steps (SDS) procedure, and semi-continuous (SC) technique. Results: Using response surface method the optimum extraction yield (4.768%) was obtained via SDS at 108.7 bar, 48.5°C, 120 min (static: 8×15), 24 min (dynamic: 8×3 min) in contrast to the 4.620% extraction yield for the SC at 111.6 bar, 49.2°C, 14 min (static), 121.1 min (dynamic). Conclusion: The results indicated that a substantial reduction (81.56%) solvent usage (kg CO2/g oil) is observed in the SDS method versus the conventional SC method. PMID:25598636

Surface nanodroplets for highly efficient liquid-liquid microextraction

NASA Astrophysics Data System (ADS)

Li, Miaosi; Lu, Ziyang; Yu, Haitao; Zhang, Xuehua

2016-11-01

Nanoscale droplets on a substrate are an essential element for a wide range of applications, such as laboratory-on-chip devices, simple and highly efficient miniaturized reactors for concentrating products, high-throughput single-bacteria or single-biomolecular analysis, encapsulation, and high-resolution imaging techniques. The solvent exchange process is a simple bottom-up approach for producing droplets at solid-liquid interfaces that are only several tens to hundreds of nanometers in height, or a few femtoliters in volume Oil nanodroplets can be produced on a substrate by solvent exchange in which a good solvent of oil is displaced by a poor solvent. Our previous work has significantly advanced understanding of the principle of solvent exchange, and the droplet size can be well-controlled by several parameters, including flow rates, flow geometry, gravitational effect and composition of solutions. In this work, we studied the microextraction effect of surface nanodroplets. Oil nanodroplets have been demonstrated to provide highly-efficient liquid-liquid microextraction of hydrophobic solute in a highly diluted solution. This effect proved the feasibility of nanodroplets as a platform for preconcentrating compounds for in situ highly sensitive microanalysis without further separation. Also the long lifetime and temporal stability of surface nanodroplets allow for some long-term extraction process and extraction without addition of stabilisers.

Deep Eutectic Solvents as Efficient Media for the Extraction and Recovery of Cynaropicrin from Cynara cardunculus L. Leaves.

PubMed

de Faria, Emanuelle L P; do Carmo, Rafael S; Cláudio, Ana Filipa M; Freire, Carmen S R; Freire, Mara G; Silvestre, Armando J D

2017-10-30

In recent years a high demand for natural ingredients with nutraceutical properties has been witnessed, for which the development of more environmentally-friendly and cost-efficient extraction solvents and methods play a primary role. In this perspective, in this work, the application of deep eutectic solvents (DES), composed of quaternary ammonium salts and organic acids, as alternative solvents for the extraction of cynaropicrin from Cynara cardunculus L. leaves was studied. After selecting the most promising DES, their aqueous solutions were investigated, allowing to obtain a maximum cynaropicrin extraction yield of 6.20 wt %, using 70 wt % of water. The sustainability of the extraction process was further optimized by carrying out several extraction cycles, reusing either the biomass or the aqueous solutions of DES. A maximum cynaropicrin extraction yield of 7.76 wt % by reusing the solvent, and of 8.96 wt % by reusing the biomass, have been obtained. Taking advantage of the cynaropicrin solubility limit in aqueous solutions, water was added as an anti-solvent, allowing to recover 73.6 wt % of the extracted cynaropicrin. This work demonstrates the potential of aqueous solutions of DES for the extraction of value-added compounds from biomass and the possible recovery of both the target compounds and solvents.

Ultrasonic-assisted extraction of essential oil from Botryophora geniculate using different extracting solvents

NASA Astrophysics Data System (ADS)

Habibullah, Wilfred, Cecilia Devi

2016-11-01

This study compares the performance of ionic liquids to substitute conventional solvents (hexane, dichloromethane and methanol) to extract essential oil from Botryophora geniculate plant. Two different Ionic liquids ([C3MIM][Ac], [C4MIM][Ac]) with co-solvent diethyl ether were used in the ultrasonic-assisted extraction. The effect of various experimental conditions such as time, temperature and solvent were studied. Gas chromatography-mass spectroscopy (GC-MS) was used to analyze essential oils. The results showed that in ultrasonic-assisted extraction using ionic liquids as a solvent gave highest yield (9.5%) in 30 min at temperature 70°C. When using ultrasonic bath with hexane, dichloromethane and methanol, yields was (3.34%), (3.6%) and (3.81%) at 90 min, respectively were obtained. The ultrasonic-assisted extraction under optimal extraction conditions (time 30 min, temperature of 70°C) gave the best yield for the essential oil extraction.

Extraction and Determination of Quercetin from Ginkgo biloba by DESs-Based Polymer Monolithic Cartridge.

PubMed

Wang, Xiaoqin; Li, Guizhen; Ho Row, Kyung

2017-09-01

Deep eutectic solvents (DES) were formed from choline chloride (ChCl). DES-modified polymer monolithic (DES-M), template molecular polymer monolithic and non-DES-M without a molecular template were synthesized in identical process. These polymer materials were characterized by field emission scanning electron microscopy and Fourier transform infrared spectroscopy. The significant selective adsorption properties of the polymers were assessed by an absorption capacity experiment and solid-phase extraction (SPE). The optimized extraction procedure was as follows: ultrasonic time (30 min), optimal solvent (ethanol) and liquid to material ratio (20 mL g-1). Under this condition, the amount of quercetin extracted from Ginkgo biloba was 290.8 mg g-1. The purification of G. biloba was achieved by the SPE process. Based on the results, DESs-based monolithic cartridges can be used for simple and efficient extraction and as a pre-concentration technique for the purification of bioactive compounds or drugs in aqueous environments with high affinity and selectivity. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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.

Effect of dye extracting solvents and sensitization time on photovoltaic performance of natural dye sensitized solar cells

NASA Astrophysics Data System (ADS)

Hossain, Md. Khalid; Pervez, M. Firoz; Mia, M. N. H.; Mortuza, A. A.; Rahaman, M. S.; Karim, M. R.; Islam, Jahid M. M.; Ahmed, Farid; Khan, Mubarak A.

In this study, natural dye sensitizer based solar cells were successfully fabricated and photovoltaic performance was measured. Sensitizer (turmeric) sources, dye extraction process, and photoanode sensitization time of the fabricated cells were analyzed and optimized. Dry turmeric, verdant turmeric, and powder turmeric were used as dye sources. Five distinct types of solvents were used for extraction of natural dye from turmeric. Dyes were characterized by UV-Vis spectrophotometric analysis. The extracted turmeric dye was used as a sensitizer in the dye sensitized solar cell's (DSSC) photoanode assembly. Nano-crystalline TiO2 was used as a film coating semiconductor material of the photoanode. TiO2 films on ITO glass substrate were prepared by simple doctor blade technique. The influence of the different parameters VOC, JSC, power density, FF, and η% on the photovoltaic characteristics of DSSCs was analyzed. The best energy conversion performance was obtained for 2 h adsorption time of dye on TiO2 nano-porous surface with ethanol extracted dye from dry turmeric.

In Situ Miniaturised Solid Phase Extraction (m-SPE) for Organic Pollutants in Seawater Samples

PubMed Central

Abaroa-Pérez, B.; Sánchez-Almeida, G.; Hernández-Brito, J. J.

2018-01-01

Solid phase extraction (SPE) is a consolidated technique for determining pollutants in seawater samples. The current tendency is to miniaturise systems that extract and determine pollutants in the environment, reducing the use of organic solvents, while maintaining the quality in the extraction and preconcentration. On the other hand, there is a need to develop new extraction systems that can be fitted to in situ continual monitoring buoys, especially for the marine environment. This work has developed a first model of a low-pressure micro-SPE (m-SPE) for persistent organic pollutants (POPs) that can be simply applied to in situ monitoring in the marine environment. This system reduces the volumes of sample and solvents required in the laboratory in comparison with conventional SPE. In the future, it could be used in automated or robotic systems in marine technologies such as marine gliders and oceanographic buoys. This system has been optimised and validated to determine polycyclic aromatic hydrocarbons (PAH) in seawater samples, but it could also be applied to other kinds of persistent organic pollutants (POPs) and emerging pollutants. PMID:29805837

A green deep eutectic solvent dispersive liquid-liquid micro-extraction (DES-DLLME) for the UHPLC-PDA determination of oxyprenylated phenylpropanoids in olive, soy, peanuts, corn, and sunflower oil.

PubMed

Ferrone, Vincenzo; Genovese, Salvatore; Carlucci, Maura; Tiecco, Matteo; Germani, Raimondo; Preziuso, Francesca; Epifano, Francesco; Carlucci, Giuseppe; Taddeo, Vito Alessandro

2018-04-15

A green dispersive liquid-liquid microextraction (DLLME) using deep eutectic solvent (DES) as the extracting solvent has been developed and applied for the simultaneous quantification of ferulic acid, umbelliferone, boropinic acid, 7-isopentenyloxycoumarin, 4'-geranyloxyferulic acid (GOFA), and auraptene in some vegetable oils using ultra high performance liquid chromatography (UHPLC) with photodiode array detection (PDA). All parameters in the extraction step, including selection and loading of both extracting and dispersing solvents, amount of both extractant and disperser solvent were investigated and optimized. PhAA/TMG DES achieved higher recovery and enrichment factor compared to other DESs. The validated method showed good linearity with correlation coefficients, r 2 >0.9990 for all the analytes. Furthermore, this is the first time that eco-friendly solvents are used for the extraction of oxyprenylated phenylpropanoids and the corresponding extract analyzed with ultra high performance liquid chromatography with photodiode array detection. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

PubMed

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

2010-06-01

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

Rapid analysis of the essential oil components of dried Zanthoxylum bungeanum Maxim by Fe2O3-magnetic-microsphere-assisted microwave distillation and simultaneous headspace single-drop microextraction followed by GC-MS.

PubMed

Ye, Qing

2013-06-01

In this work, microwave distillation assisted by Fe2 O3 magnetic microspheres (FMMS) and headspace single-drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent-free technique for the determination of volatile compounds in Chinese herbs. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Use of advanced techniques for the extraction of phenolic compounds from Tunisian olive leaves: phenolic composition and cytotoxicity against human breast cancer cells.

PubMed

Taamalli, Amani; Arráez-Román, David; Barrajón-Catalán, Enrique; Ruiz-Torres, Verónica; Pérez-Sánchez, Almudena; Herrero, Miguel; Ibañez, Elena; Micol, Vicente; Zarrouk, Mokhtar; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto

2012-06-01

A comparison among different advanced extraction techniques such as microwave-assisted extraction (MAE), supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE), together with traditional solid-liquid extraction, was performed to test their efficiency towards the extraction of phenolic compounds from leaves of six Tunisian olive varieties. Extractions were carried out at the best selected conditions for each technique; the obtained extracts were chemically characterized using high-performance liquid chromatography (HPLC) coupled to electrospray time-of-flight mass spectrometry (ESI-TOF-MS) and electrospray ion trap tandem mass spectrometry (ESI-IT-MS(2)). As expected, higher extraction yields were obtained for PLE while phenolic profiles were mainly influenced by the solvent used as optimum in the different extraction methods. A larger number of phenolic compounds, mostly of a polar character, were found in the extracts obtained by using MAE. Best extraction yields do not correlate with highest cytotoxic activity against breast cancer cells, indicating that cytotoxicity is highly dependent on the presence of certain compounds in the extracts, although not exclusively on a single compound. Therefore, a multifactorial behavior is proposed for the anticancer activity of olive leaf compounds. Copyright © 2012 Elsevier Ltd. All rights reserved.

Exploration of the wound healing potential of Helichrysum graveolens (Bieb.) Sweet: isolation of apigenin as an active component.

PubMed

Süntar, Ipek; Küpeli Akkol, Esra; Keles, Hikmet; Yesilada, Erdem; Sarker, Satyajit D

2013-08-26

In Turkish traditional medicine, the flowers of Helichrysum graveolens (Bieb.) Sweet (Asteraceae) have been used for the treatment of jaundice, for wound-healing and as a diuretic. In order to find scientific evidence for the traditional utilization of this plant in wound-healing, the effect of the plant extract was investigated by using in vivo and in vitro experimental models. Then through bioassay-guided fractionation procedures active wound-healing component(s) was isolated and its possible role in the wound-healing process was also determined. The linear incision and the circular excision wound models were applied in order to evaluate in vivo wound-healing potential of Helichrysum graveolens. Anti-inflammatory and antioxidant activities, which are known to involve in wound-healing process, were also assessed by the Whittle method and the DPPH (2,2-diphenyl-1-picrylhydrazyl) radical-scavenging assay, respectively. The total phenolic content of the crude extract and solvent fractions was estimated to find correlation between the phenolic content and the antioxidant activity. Combined application of the chromatographic separation techniques on sephadex and silica gel columns, and bioassay techniques have yielded the active wound-healing principle of Helichrysum graveolens. Moreover, in vitro inhibitory effect of active principle on hyaluronidase, collagenase and elastase enzymes were investigated to explore the activity pathways. The 85% methanol (MeOH) extract of Helichrysum graveolens flowers displayed significant wound-healing, anti-inflammatory and antioxidant activities. Then the crude extract was partitioned by successive solvent extractions, in increasing polarity, to give five solvent fractions. Among the solvent fractions, the ethyl acetate (EtOAc) fraction exerted the highest activity. The EtOAc fraction was further subjected to chromatographic separations to yield active constituent and its structure was elucidated to be apigenin by spectrometric methods. Further in vivo and in vitro assays revealed that apigenin was one of the components responsible for the wound-healing effect of the plant remedy and also found to possess significant anti-inflammatory, antioxidant, anti-hyaluronidase and anti-collagenase activities. Present study supported the traditional use of Helichrysum graveolens flowers for wound-healing and through bioassay-guided fractionation procedures from the crude extract apigenin was isolated as one of the active components. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

An approach of ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergistic extraction for two coumarins preparation from Cortex fraxini.

PubMed

Liu, Zaizhi; Gu, Huiyan; Yang, Lei

2015-10-23

Ionic liquids/lithium salts solvent system was successfully introduced into the separation technique for the preparation of two coumarins (aesculin and aesculetin) from Cortex fraxini. Ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergy extraction (ILSMP-UMSE) procedure was developed and optimized for the sufficient extraction of these two analytes. Several variables which can potentially influence the extraction yields, including pretreatment time and temperature, [C4mim]Br concentration, LiAc content, ultrasound-microwave synergy extraction (UMSE) time, liquid-solid ratio, and UMSE power were optimized by Plackett-Burman design. Among seven variables, UMSE time, liquid-solid ratio, and UMSE power were the statistically significant variables and these three factors were further optimized by Box-Behnken design to predict optimal extraction conditions and find out operability ranges with maximum extraction yields. Under optimum operating conditions, ILSMP-UMSE showed higher extraction yields of two target compounds than those obtained by reference extraction solvents. Method validation studies also evidenced that ILSMP-UMSE is credible for the preparation of two coumarins from Cortex fraxini. This study is indicative of the proposed procedure that has huge application prospects for the preparation of natural products from plant materials. Copyright © 2015 Elsevier B.V. All rights reserved.

Solvent and process for recovery of hydroxide from aqueous mixtures

DOEpatents

Moyer, Bruce A.; Chambliss, C. Kevin; Bonnesen, Peter V.; Keever, Tamara J.

2001-01-01

Hydroxide values and associated alkali metal may be recovered from alkaline aqueous solutions using classes of fluorinated alcohols in a water immiscible solvent. The alcohols are characterized by fluorine substituents which are proximal to the acidic alcohol protons and are located to adjust the acidity of the extractant and the solubility of the extractant in the solvent. A method for stripping the extractant and solvent to regenerate the extractant and purified aqueous hydroxide solution is described.

Solvent extraction of diatomite

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

Williams, W.

1984-07-24

There is provided a method of extracting hydrocarbons from a diatomite ore. The particle size of the ore is first reduced to form a processed ore. The processed ore is then mixed with a substantially irregular granular material to form an unstratified ore mixture having increased permeability to an extracting solvent. The unstratified ore mixture is then permeated with an extracting solvent to obtain a hydrocarbon-solvent stream from which hydrocarbons are subsequently separated. The irregular granular material may be sand.

Improved Supercritical-Solvent Extraction of Coal

NASA Technical Reports Server (NTRS)

Compton, L.

1982-01-01

Raw coal upgraded by supercritical-solvent extraction system that uses two materials instead of one. System achieved extraction yields of 20 to 49 weight percent. Single-solvent yields are about 25 weight percent. Experimental results show extraction yields may be timedependent. Observed decreases in weight of coal agreed well with increases in ash content of residue.

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 solvent refining of coal using a denitrogenated and dephenolated solvent

DOEpatents

Garg, Diwakar; Givens, Edwin N.; Schweighardt, Frank K.

1984-01-01

A process is disclosed for the solvent refining of non-anthracitic coal at elevated temperatures and pressure in a hydrogen atmosphere using a hydrocarbon solvent which before being recycled in the solvent refining process is subjected to chemical treatment to extract substantially all nitrogenous and phenolic constituents from the solvent so as to improve the conversion of coal and the production of oil in the solvent refining process. The solvent refining process can be either thermal or catalytic. The extraction of nitrogenous compounds can be performed by acid contact such as hydrogen chloride or fluoride treatment, while phenolic extraction can be performed by caustic contact or contact with a mixture of silica and alumina.

Understanding the potential benefits of thyme and its derived products for food industry and consumer health: From extraction of value-added compounds to the evaluation of bioaccessibility, bioavailability, anti-inflammatory, and antimicrobial activities.

PubMed

Lorenzo, Jose M; Mousavi Khaneghah, Amin; Gavahian, Mohsen; Marszałek, Krystian; Eş, Ismail; Munekata, Paulo E S; Ferreira, Isabel C F R; Barba, Francisco J

2018-05-17

Natural bioactive compounds isolated from several aromatic plants have been studied for centuries due to their unique characteristics that carry great importance in food, and pharmaceutical, and cosmetic industries. For instance, several beneficial activities have been attributed to some specific compounds found in Thymus such as anti-inflammatory, antioxidant, antimicrobial, and antiseptic properties. Moreover, these compounds are classified as Generally Recognized as Safe (GRAS) which means they can be used as an ingrident of may food producs. Conventional extraction processes of these compounds and their derived forms from thyme leaves are well established. Hoewever, they present some important drawbacks such as long extraction time, low yield, high solvent consumption and degradation thermolabile compounds. Therefore, innovative extraction techniques such as ultrasound, microwave, enzyme, ohmic and heat-assisted methods can be useful strategies to enhance the exytraction yield and to reduce processing temperature, extraction time, and energy and solvent consumption. Furthermore, bioaccessibility and bioavailability aspects of these bioactive compounds as well as their metabolic fates are crucial for developing novel functional foods. Additionally, immobilization methods to improve stability, solubility, and the overall bioavailability of these valuable compounds are necessary for their commercial applications. This review aims to give an overall perspective of innovative extraction techniques to extract the targeted compounds with anti-inflammatory and antimicrobial activities. Moreover, the bioaccessi-bility and bioavailability of these compounds before and after processing discussed. In addition, some of the most important characteristics of thyme and their derived products discussed in this paper.

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

PubMed

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

2016-01-01

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

Use of normal propyl bromide solvents for extraction and recovery of asphalt cements

DOT National Transportation Integrated Search

2000-11-01

Four normal propyl bromide (nPB) solvents were evaluated for use as chlorinated solvent replacements in typical hot mix asphalt (HMA) extraction and recovery processes. The experimental design included one method of extraction (centrifuge), one metho...

Semiautomated solid-phase extraction manifold with a solvent-level sensor.

PubMed

Orlando, R M; Rath, S; Rohwedder, J J R

2013-11-15

A semiautomated solid-phase extraction manifold for multiple extractions is presented. The manifold utilizes commercial solid-phase syringe cartridges and automatically introduces and elutes all the solvents during the extraction, reducing the typical workload and stress of the analyst. The manifold consists of a peristaltic pump with solenoid valves in a flow circuit that contains transmissive photomicrosensors. The photomicrosensors were used to control the solvent dispenser and the solvent level inside the cartridge. As solvent-level sensors, the photomicrosensors determined the exact time the solvent reached the top frit to avoid sorbent drying and accurately perform the solvent exchange. The repeatability of the manifold to introduce a particular volume of solvent into the cartridges was measured, and the precisions were between 0.05 and 2.89% (RSD). To evaluate the manifold, the amount of two fluoroquinolones in a fortified blank milk sample was determined. The results of the intra- and inter-day precision of multiple extractions from the fortified milk samples resulted in precisions better than 9.0% (RSD) and confirmed that the arrangement of the semiautomated manifold could adequately be used in solid-phase extraction with commercial cartridges. Copyright © 2013 Elsevier B.V. All rights reserved.

Solvent Extraction of Chemical Attribution Signature Compounds from Painted Wall Board: Final Report

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

Wahl, Jon H.; Colburn, Heather A.

2009-10-29

This report summarizes work that developed a robust solvent extraction procedure for recovery of chemical attribution signature (CAS) compound dimethyl methyl phosphonate (DMMP) (as well as diethyl methyl phosphonate (DEMP), diethyl methyl phosphonothioate (DEMPT), and diisopropyl methyl phosphonate (DIMP)) from painted wall board (PWB), which was selected previously as the exposed media by the chemical attribution scientific working group (CASWG). An accelerated solvent extraction approach was examined to determine the most effective method of extraction from PWB. Three different solvent systems were examined, which varied in solvent strength and polarity (i.e., 1:1 dichloromethane : acetone,100% methanol, and 1% isopropanol inmore » pentane) with a 1:1 methylene chloride : acetone mixture having the most robust and consistent extraction for four original target organophosphorus compounds. The optimum extraction solvent was determined based on the extraction efficiency of the target analytes from spiked painted wallboard as determined by gas chromatography x gas chromatography mass spectrometry (GCxGC-MS) analysis of the extract. An average extraction efficiency of approximately 60% was obtained for these four compounds. The extraction approach was further demonstrated by extracting and detecting the chemical impurities present in neat DMMP that was vapor-deposited onto painted wallboard tickets.« less

Effect of solvent polarity on the extraction of components of pharmaceutical plastic containers.

PubMed

Ahmad, Iqbal; Sabah, Arif; Anwar, Zubair; Arif, Aysha; Arsalan, Adeel; Qadeer, Kiran

2017-01-01

A study of the extraction of polymeric material and dyes from the pharmaceutical plastic containers using various organic solvents was conducted to evaluate the effect of polarity on the extraction process. The plastic containers used included semi-opaque, opaque, transparent and amber colored and the solvent used were acetonitrile, methanol, ethanol, acetone, dichloroethane, chloroform and water. The determination of extractable material was carried out by gravimetric and spectrometric methods. The yield of extractable materials from containers in 60 h was 0.10-1.29% (w/w) and the first-order rate constant (kobs) for the extraction of polymeric material ranged from 0.52-1.50 × 10-3 min -1 and for the dyes 6.43- 6.74 x10-3min-1. The values of (k obs ) were found to be an inverse function of solvent dielectric constant and decreased linearly with the solvent acceptor number. The extractable polymeric materials exhibited absorption in the 200-400 nm region and the dyes in the 300-500nm region. The rates of extraction of polymeric material and dyes from plastic containers were dependent on the solvent dielectric constant. The solvents of low polarity were more effective in the extraction of material indicating that the extracted material were of low polarity or have non-polar character. The dyes were soluble in acetone and chloroform. No plastic material was found to be extracted from the containers in aqueous solution.

Focused microwave-assisted solvent extraction and HPLC determination of effective constituents in Eucommia ulmodies Oliv. (E. ulmodies).

PubMed

Li, Hui; Chen, Bo; Zhang, Zhaohui; Yao, Shouzhuo

2004-06-17

A new focused microwave-assisted solvent extraction method using water as solvent has been developed for leaching geniposidic and chlorogenic acids from Eucommia ulmodies Oliv. The extraction procedures were optimized using a two indexes orthogonal experimental design and graphical analysis, by varying irradiation time, solvent volume, solvent composition and microwave power. The optimum extraction conditions were obtained: for geniposidic acid, 50% micorwave power, 40s irradiation, and 80% (v/v) aqueous methanol as extraction solvent (20mlg(-1) sample); and for chlorogenic acid, 50% micorwave power, 30s irradiation, and 20% aqueous methanol (20mlg(-1) sample). The composition of the extraction solvent was optimized and can be directly used as the mobile phase in the HPLC separation. Quantification of organic acids was done by HPLC at room temperature using Spherigel C(18) chromatographic column (250 mm x4.6 mm , i.d. 5mum), the methanol:water:acetic acid (20:80:1.0, v/v) mobile phase and UV detection at 240nm. The R.S.D. of the extraction process for geniposidic and chlorogenic acid were 3.8 and 4.1%, respectively.

Water-based gas purge microsyringe extraction coupled with liquid chromatography for determination of alkylphenols from sea food Laminaria japonica Aresh.

PubMed

Yang, Cui; Zhao, Jinhua; Wang, Juan; Yu, Hongling; Piao, Xiangfan; Li, Donghao

2013-07-26

A novel organic solvent-free mode of gas purge microsyringe extraction, termed water-based gas purge microsyringe extraction, was developed. This technique can directly extract target compounds in wet samples without any drying process. Parameters affecting the extraction efficiency were investigated. Under optimal extraction conditions, the recoveries of alkylphenols were between 87.6 and 105.8%, and reproducibility was between 5.2 and 12.1%. The technique was also used to determine six kinds of alkylphenols (APs) from samples of Laminaria japonica Aresh. The OP and NP were detected in all the samples, and concentrations ranged from 26.0 to 54.5ngg(-1) and 45.0-180.4ngg(-1), respectively. The 4-n-butylphenol was detected in only one sample and its concentration was very low. Other APs were not detected in L. japonica Aresh samples. The experimental results demonstrated that the technique is fast, simple, non-polluting, allows for quantitative extraction, and a drying process was not required for wet samples. Since only aqueous solution and a conventional microsyringe were used, this technique proved affordable, efficient, and convenient for the extraction of volatile and semivolatile ionizable compounds. Copyright © 2013 Elsevier B.V. All rights reserved.

Unusual seeding mechanism for enhanced performance in solid-phase magnetic extraction of Rare Earth Elements

PubMed Central

Polido Legaria, Elizabeth; Rocha, Joao; Tai, Cheuk-Wai; Kessler, Vadim G.; Seisenbaeva, Gulaim A.

2017-01-01

Due to the increasing demand of Rare Earth Elements (REE or RE), new and more efficient techniques for their extraction are necessary, suitable for both mining and recycling processes. Current techniques such as solvent extraction or solid adsorbents entail drawbacks such as using big volumes of harmful solvents or limited capacity. Hybrid nanoadsorbents based on SiO2 and highly stable γ-Fe2O3-SiO2 nanoparticles, proved recently to be very attractive for adsorption of REE, yet not being the absolute key to solve the problem. In the present work, we introduce a highly appealing new approach in which the nanoparticles, rather than behaving as adsorbent materials, perform as inducers of crystallization for the REE in the form of hydroxides, allowing their facile and practically total removal from solution. This induced crystallization is achieved by tuning the pH, offering an uptake efficiency more than 20 times higher than previously reported (up to 900 mg RE3+/g vs. 40 mg RE3+/g). The obtained phases were characterized by SEM-EDS, TEM, STEM and EFTEM and 13C and 29Si solid state NMR. Magnetic studies showed that the materials possessed enough magnetic properties to be easily removed by a magnet, opening ways for an efficient and industrially applicable separation technique. PMID:28266566

Unusual seeding mechanism for enhanced performance in solid-phase magnetic extraction of Rare Earth Elements

NASA Astrophysics Data System (ADS)

Polido Legaria, Elizabeth; Rocha, Joao; Tai, Cheuk-Wai; Kessler, Vadim G.; Seisenbaeva, Gulaim A.

2017-03-01

Due to the increasing demand of Rare Earth Elements (REE or RE), new and more efficient techniques for their extraction are necessary, suitable for both mining and recycling processes. Current techniques such as solvent extraction or solid adsorbents entail drawbacks such as using big volumes of harmful solvents or limited capacity. Hybrid nanoadsorbents based on SiO2 and highly stable γ-Fe2O3-SiO2 nanoparticles, proved recently to be very attractive for adsorption of REE, yet not being the absolute key to solve the problem. In the present work, we introduce a highly appealing new approach in which the nanoparticles, rather than behaving as adsorbent materials, perform as inducers of crystallization for the REE in the form of hydroxides, allowing their facile and practically total removal from solution. This induced crystallization is achieved by tuning the pH, offering an uptake efficiency more than 20 times higher than previously reported (up to 900 mg RE3+/g vs. 40 mg RE3+/g). The obtained phases were characterized by SEM-EDS, TEM, STEM and EFTEM and 13C and 29Si solid state NMR. Magnetic studies showed that the materials possessed enough magnetic properties to be easily removed by a magnet, opening ways for an efficient and industrially applicable separation technique.

SOLVENT EXTRACTION OF URANIUM VALUES

DOEpatents

Feder, H.M.; Ader, M.; Ross, L.E.

1959-02-01

A process is presented for extracting uranium salt from aqueous acidic solutions by organic solvent extraction. It consists in contacting the uranium bearing solution with a water immiscible dialkylacetamide having at least 8 carbon atoms in the molecule. Mentioned as a preferred extractant is dibutylacetamide. The organic solvent is usually used with a diluent such as kerosene or CCl/sub 4/.

Solvent Effects of Model Polymeric Corrosion Control Coatings on Water Transport and Corrosion Rate

NASA Astrophysics Data System (ADS)

Konecki, Christina

Industrial coating formulations are often made for volatile organic content compliance and ease of application, with little regard for the solvent impact on resultant performance characteristics. Our research objective was to understand the effect of both solvent retention and chemical structure on water transport through polymer films and resultant corrosion area growth of coated steel substrates. A clear, unpigmented Phenoxy(TM) thermoplastic polymer (PKHH) was formulated into resin solutions with three separate solvent blends selected by Hansen solubility parameter (HSP), boiling point, and ability to solubilize PKHH. Polymer films cast from MEK/PGME (methyl ethyl ketone/ propylene glycol methyl ether), dried under ambient conditions (AMB, > 6wt.% residual solvent) produced a porous morphology, which resulted in a corrosion area greater than 50%. We attributed this to the water-soluble solvent used in film preparation, which enabled residual PGME to be extracted by water. The resin solution prepared with CYCOH/DXL (Cyclohexanol/ 1,3 dioxolane) was selected because CYCOH is a solid at room temperature which acts as a pigment in the final film. Therefore, increasing the tortuosity of water transport, as well as a high hydrogen bonding character, which caused more interactions with water, slowing diffusion, producing a nodular morphology, and 37% less corrosion area than MEK/PGME AMB. The HSP of PKHH and EEP (ethyl 3-ethoxypropionate) are within 5% of each other, which produced a homogeneous morphology and resulted in comparable corrosion rates regardless of residual solvent content. We utilized electrochemical techniques and attenuated total reflectance- Fourier transform infrared spectroscopy to elucidate dynamic water absorption and solvent extraction in the exposed model formulations. We found that water absorption resulted in a loss of barrier properties, and increased corrosion due to the voids formed by solvent extraction. The polymer films were rejuvenated (removal of water) as an attempt to decrease the number of water transport pathways during exposure. Results found that samples rejuvenated at temperatures above the glass transition temperature of the samples achieved lower moisture content and consequently, lower corrosion growth rates. In commercial systems, rejuvenation lowered the corrosion rate up to 60% indicating better coating formulations and maintenance cycles would control the corrosion rate.

Solidification of floating organic droplet in dispersive liquid-liquid microextraction as a green analytical tool.

PubMed

Mansour, Fotouh R; Danielson, Neil D

2017-08-01

Dispersive liquid-liquid microextraction (DLLME) is a special type of microextraction in which a mixture of two solvents (an extracting solvent and a disperser) is injected into the sample. The extraction solvent is then dispersed as fine droplets in the cloudy sample through manual or mechanical agitation. Hence, the sample is centrifuged to break the formed emulsion and the extracting solvent is manually separated. The organic solvents commonly used in DLLME are halogenated hydrocarbons that are highly toxic. These solvents are heavier than water, so they sink to the bottom of the centrifugation tube which makes the separation step difficult. By using solvents of low density, the organic extractant floats on the sample surface. If the selected solvent such as undecanol has a freezing point in the range 10-25°C, the floating droplet can be solidified using a simple ice-bath, and then transferred out of the sample matrix; this step is known as solidification of floating organic droplet (SFOD). Coupling DLLME to SFOD combines the advantages of both approaches together. The DLLME-SFOD process is controlled by the same variables of conventional liquid-liquid extraction. The organic solvents used as extractants in DLLME-SFOD must be immiscible with water, of lower density, low volatility, high partition coefficient and low melting and freezing points. The extraction efficiency of DLLME-SFOD is affected by types and volumes of organic extractant and disperser, salt addition, pH, temperature, stirring rate and extraction time. This review discusses the principle, optimization variables, advantages and disadvantages and some selected applications of DLLME-SFOD in water, food and biomedical analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Next Generation Solvent Performance in the Modular Caustic Side Solvent Extraction Process - 15495

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

Smith, Tara E.; Scherman, Carl; Martin, David

Changes to the Modular Caustic Side Solvent Extraction Unit (MCU) flow-sheet were implemented in the facility. Implementation included changing the scrub and strip chemicals and concentrations, modifying the O/A ratios for the strip, scrub, and extraction contactor banks, and blending the current BoBCalixC6 extractant-based solvent in MCU with clean MaxCalix extractant-based solvent. During the successful demonstration period, the MCU process was subject to rigorous oversight to ensure hydraulic stability and chemical/radionuclide analysis of the key process tanks (caustic wash tank, solvent hold tank, strip effluent hold tank, and decontaminated salt solution hold tank) to evaluate solvent carryover to downstream facilitiesmore » and the effectiveness of cesium removal from the liquid salt waste. Results indicated the extraction of cesium was significantly more effective with an average Decontamination Factor (DF) of 1,129 (range was 107 to 1,824) and that stripping was effective. The contactor hydraulic performance was stable and satisfactory, as indicated by contactor vibration, contactor rotational speed, and flow stability; all of which remained at or near target values. Furthermore, the Solvent Hold Tank (SHT) level and specific gravity was as expected, indicating that solvent integrity and organic hydraulic stability were maintained. The coalescer performances were in the range of processing results under the BOBCalixC6 flow sheet, indicating negligible adverse impact of NGS deployment. After the Demonstration period, MCU began processing via routine operations. Results to date reiterate the enhanced cesium extraction and stripping capability of the Next Generation Solvent (NGS) flow sheet. This paper presents process performance results of the NGS Demonstration and continued operations of MCU utilizing the blended BobCalixC6-MaxCalix solvent under the NGS flowsheet.« less

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

NASA Astrophysics Data System (ADS)

Inayati, Puspita, Rifka Intan; Fajrin, Vika Latifiana

2018-02-01

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

Lipase biofilm deposited by Matrix Assisted Pulsed Laser Evaporation technique

NASA Astrophysics Data System (ADS)

Aronne, Antonio; Bloisi, Francesco; Calabria, Raffaela; Califano, Valeria; Depero, Laura E.; Fanelli, Esther; Federici, Stefania; Massoli, Patrizio; Vicari, Luciano R. M.

2015-05-01

Lipase is an enzyme that finds application in biodiesel production and for detection of esters and triglycerides in biosensors. Matrix Assisted Pulsed Laser Evaporation (MAPLE), a technique derived from Pulsed Laser Deposition (PLD) for deposition of undamaged biomolecules or polymers, is characterized by the use of a frozen target obtained from a solution/suspension of the guest material (to be deposited) in a volatile matrix (solvent). The presence of the solvent avoids or at least reduces the potential damage of guest molecules by laser radiation but only the guest material reaches the substrate in an essentially solvent-free deposition. MAPLE can be used for enzymes immobilization, essential for industrial application, allowing the development of continuous processes, an easier separation of products, the reuse of the catalyst and, in some cases, enhancing enzyme properties (pH, temperature stability, etc.) and catalytic activity in non-aqueous media. Here we show that MAPLE technique can be used to deposit undamaged lipase and that the complex structure (due to droplets generated during extraction from target) of the deposited material can be controlled by changing the laser beam fluence.

Higher Americium Oxidation State Research Roadmap

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

Mincher, Bruce J.; Law, Jack D.; Goff, George S.

2015-12-18

The partitioning of hexavalent Am from dissolved nuclear fuel requires the ability to efficiently oxidize Am(III) to Am(VI) and to maintain that oxidation state for a length of time sufficient to perform the separation. Several oxidants have been, or are being developed. Chemical oxidants include Ag-catalyzed ozone, Ag-catalyzed peroxydisulfate, Cu(III) periodate, and sodium bismuthate. Hexavalent americium has also now successfully been prepared by electrolysis, using functionalized electrodes. So-called auto-reduction rates of Am(VI) are sufficiently slow to allow for separations. However, for separations based on solvent extraction or ion exchange using organic resins, the high valence state must be maintained undermore » the reducing conditions of the organic phase contact, and a holding oxidant is probably necessary. Until now, only Cu(III) periodate and sodium bismuthate oxidation have been successfully combined with solvent extraction separations. Bismuthate oxidation provided the higher DAm, since it acts as its own holding oxidant, and a successful hot test using centrifugal contactors was performed. For the other oxidants, Ag-catalyzed peroxydisulfate will not oxidize americium in nitric acid concentrations above 0.3 M, and it is not being further investigated. Peroxydisulfate in the absence of Ag catalysis is being used to prepare Am(V) in ion exchange work, discussed below. Preliminary work with Ag-catalyzed ozone has been unsuccessful for extractions of Am(VI) from 6.5 M HNO3, and only one attempt at extraction, also from 6.5 M HNO3, using the electrolytic oxidation has been attempted. However, this high acid concentration was based on the highest Am extraction efficiency using the bismuthate oxidant; which is only sparingly soluble, and thus the oxidation yield is based on bismuthate solubility. Lower acid concentrations may be sufficient with alternative oxidants and work with Ag-ozone, Cu(III) and electrolysis is on-going. Two non-solvent-extraction separations are also under investigation. The first would separate Am(VI) by co-crystallization with uranium and the other oxidizable actinides as their nitrate salts. This novel idea has been successful in lab scale testing, and merits further investigation. Similarly, success has been achieved in separations using inorganic or hybrid ion exchange materials to sorb the lanthanides and actinides, while allowing pentavalent americium to elute. This is the only technique currently investigating Am(V), despite the advantages of this oxidation state with regard to its higher stability. The ultimate destination for this roadmap is to develop an americium separation that can be applied under process conditions, preferably affording a co-separation of the actinyl (VI) ions. Toward that end, emphasis is given here to selection of a solvent extraction flowsheet for testing in the INL centrifugal contactor hot test bed during FY16. A solvent extraction process will be tested mainly because solvent extraction separations of Am(VI) are relatively mature and the test bed currently exists in a configuration to support them. Thus, a major goal of FY16 is to select the oxidant/ligand combination to run such a test using the contactors. The only ligands under consideration are DAAP and DEHBA. This is not to say that ion exchange and co-crystallization techniques are unimportant. They merit continued investigation, but are not mature enough for hot test bed testing at this time.« less

Extraction of vitexin from binahong (Anredera cordifolia (Ten.) Steenis) leaves using betaine - 1,4 butanediol natural deep eutectic solvent (NADES)

NASA Astrophysics Data System (ADS)

Mulia, Kamarza; Muhammad, Fajri; Krisanti, Elsa

2017-03-01

The leaves of binahong (Anredera cordifolia (Ten) Steenis) contain flavonoids as bioactive substances that have efficacy to treat wounds and diseases caused by bacteria. One of the flavonoids contained in the leaves is 8-glucopyranosyl-4'5'7-trihydroxyflavone or vitexin. Conventional extraction of flavonoids from leaves of binahong has been developed and usually using non-friendly organic solvent. To overcome these problems, a Natural Deep Eutectic Solvent (NADES) is used to replace the conventional organic solvents, as it is an environmentally friendly, non-toxic and high boiling point solvent. In this study, a betaine-based NADES combined with 1,4-butanediol in 1:3 mole ratio was used as the extraction solvent. Vitexin in the extract was analyzed qualitatively and quantitatively using an HPLC. The extraction of vitexin from binahong leaves at room temperature (27 °C) for four hours give yield of 46 ppm, much lower than 200 ppm yield obtained after extraction at 55 °C for 90 minutes. This results showed that (a) NADES consisting of betaine and 1,4 butanediol is a promising green solvent for extraction of vitexin from binahong leaves, and, (b) the extraction can be performed above ambient temperature, as long as it does not exceed the degradation temperature of the bioactive compound extracted.

Determination of flavonoids in Triticum aestivum L. treated with ampicillin

NASA Astrophysics Data System (ADS)

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

2012-02-01

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

PROCESS OF SEPARATING URANIUM FROM AQUEOUS SOLUTION BY SOLVENT EXTRACTION

DOEpatents

Warf, J.C.

1958-08-19

A process is described for separating uranium values from aqueous uranyl nitrate solutions. The process consists in contacting the uramium bearing solution with an organic solvent, tributyl phosphate, preferably diluted with a less viscous organic liquida whereby the uranyl nitrate is extracted into the organic solvent phase. The uranvl nitrate may be recovered from the solvent phase bv back extracting with an aqueous mediuin.

An Efficient Extraction Method for Fragrant Volatiles from Jasminum sambac (L.) Ait.

PubMed

Ye, Qiuping; Jin, Xinyi; Zhu, Xinliang; Lin, Tongxiang; Hao, Zhilong; Yang, Qian

2015-01-01

The sweet smell of aroma of Jasminum sambac (L.) Ait. is releasing while the flowers are blooming. Although components of volatile oil have been extensively studied, there are problematic issues, such as low efficiency of yield, flavour distortion. Here, the subcritical fluid extraction (SFE) was performed to extract fragrant volatiles from activated carbon that had absorbed the aroma of jasmine flowers. This novel method could effectively obtain main aromatic compounds with quality significantly better than solvent extraction (SE). Based on the analysis data with response surface methodology (RSM), we optimized the extraction conditions which consisted of a temperature of 44°C, a solvent-to-material ratio of 3.5:1, and an extraction time of 53 min. Under these conditions, the extraction yield was 4.91%. Furthermore, the key jasmine essence oil components, benzyl acetate and linalool, increase 7 fold and 2 fold respectively which lead to strong typical smell of the jasmine oil. The new method can reduce spicy components which lead to the essential oils smelling sweeter. Thus, the quality of the jasmine essence oil was dramatically improved and yields based on the key component increased dramatically. Our results provide a new effective technique for extracting fragrant volatiles from jasmine flowers.

Analysis of N-Nitrosodimethylamine and N-Nitrodimethylamine in Groundwater

NASA Technical Reports Server (NTRS)

Greene, Ben; Mast, Dion; Baker, David L.

2006-01-01

A method for the analytical determination of N-nitrosodimethylamine (NDMA) and N-nitrodimethylamine (DMN) at parts-per-trillion (ppt) concentrations in groundwater is reported. The method uses a solid phase extraction (SPE) cartridge containing 2 g of activated coconut charcoal to extract a 500-mL water sample. NDMA and DMN are eluted from the SPE cartridge using acetone. The acetone is concentrated and brought to a final volume of 1.0 mL, which results in a theoretical 500-fold concentration of the analytes. The extracts are analyzed by gas chromatography (GC) with a nitrogenphosphorous detector (NPD), which is a highly sensitive and relatively inexpensive technique. The measured extraction efficiencies averaged 61 percent for NDMA and 74 percent for DMN. Extraction efficiencies were independent of NDMA and DMN concentrations from 40 to 2000 ppt. Several samples could be extracted then analyzed in a single day with the use of an extraction manifold and GC autosampler. A reporting limit of 10 ppt for NDMA and DMN was achieved. The MDLs for NDMA and DMN were 6.4 and 5.8 ppt, respectively. A typical turn-around time from beginning of extraction to reporting was 4 h. The method avoids the use of halogenated solvents, such as dichloromethane, and subsequent solvent exchange procedures necessary for use of the NPD detector.

PREPARATION OF ALKYL PYROPHOSPHATE EXTRACTANTS

DOEpatents

Levine, C.A.; Skiens, W.E.; Moore, G.R.

1960-08-01

A process for providing superior solvent extractants for metal recovery processes is given wherein the extractant comprises an alkyl pyrophosphoric acid ester dissolved in an organic solvent diluent. Finely divided solid P/sub 2/O/ sub 5/ is slurried in an organic solvent-diluent selected from organic solvents such as kerosene, benzene, chlorobenzene, toluene, etc. An alcohol selected from the higher alcohols having 4 to 17 carbon atoms. e.g.. hexanol-1. heptanol-3, octanol-1. 2.6-dimethyl-heptanol-4, and decanol-1, is rapidly added to the P/sub 2/O/sub 5/ slurry in the amount of about 2 moles of alcohol to 1 mole of P/sub 2/ O/sub 5/. The temperature is maintained below about 110 deg C during the course of the P/sub 2/O/sub 5/-alcohol reaction. An alkyl pyrophosphate extractant compound is formed as a consequence of the reaction process. The alkyl pyrophosphate solvent-diluent extractant phase is useful in solvent extraction metal recovery processes.

Process for the removal of impurities from combustion fullerenes

DOEpatents

Alford, J. Michael; Bolskar, Robert

2005-08-02

The invention generally relates to purification of carbon nanomaterials, particularly fullerenes, by removal of PAHs and other hydrocarbon impurities. The inventive process involves extracting a sample containing carbon nanomaterials with a solvent in which the PAHs are substantially soluble but in which the carbon nanomaterials are not substantially soluble. The sample can be repeatedly or continuously extracted with one or more solvents to remove a greater amount of impurities. Preferred solvents include ethanol, diethyl ether, and acetone. The invention also provides a process for efficiently separating solvent extractable fullerenes from samples containing fullerenes and PAHs wherein the sample is extracted with a solvent in which both fullerenes and PAHs are substantially soluble and the sample extract then undergoes selective extraction to remove PAHs. Suitable solvents in which both fullerenes and PAHs are soluble include o-xylene, toluene, and o-dichlorobenzene. The purification process is capable of treating quantities of combustion soot in excess of one kilogram and can produce fullerenes or fullerenic soot of suitable purity for many applications.

Extraction of Illegal Dyes from Red Chili Peppers with Cholinium-Based Deep Eutectic Solvents

PubMed Central

Zhu, Shuqiang; Zhu, Xinyue; Su, Along

2017-01-01

Deep eutectic solvents (DESs) as a new kind of green solvents have been used to extract bioactive compounds but there are few applications in extracting chrysoidine dyes. In this study, we developed an ultrasonic-assisted extraction method with choline chloride/hydrogen bond donor (ChCl/HBD) DES for the extraction of chrysoidine G (COG), astrazon orange G (AOG), and astrazon orange R (AOR) in food samples. Some experimental parameters, such as extraction time, raw material/solvent ratio, and temperature, were evaluated and optimized as follows: the ratio of ChCl/HBD, 1 : 2 (v/v); the ratio of sample/DES, 1 : 10 (g/mL); extraction time, 20 min; extraction temperature, 50°C. Under the optimized conditions, the limits of detection (μg/mL) were 0.10 for COG and 0.06 for AOG and AOR. The relative standard deviations were in the range of 1.2–2.1%. The recoveries of the three dyes were in the range of 80.2–105.0%. By comparing with other commonly used solvents for extracting chrysoidine dyes, the advantages of DESs proved them to be potential extraction solvents for chrysoidine G, astrazon orange G, and astrazon orange R in foods. PMID:28831327

Study to find the best extraction solvent for use with guava leaves (Psidium guajava L.) for high antioxidant efficacy.

PubMed

Seo, Jongkwon; Lee, Soojung; Elam, Marcus L; Johnson, Sarah A; Kang, Jonghoon; Arjmandi, Bahram H

2014-03-01

The effects of guava leaves extracted using solvents of water, ethanol, methanol, and different concentrations of hydroethanolic solvents on phenolic compounds and flavonoids, and antioxidant properties have been investigated. The antioxidant capability was assessed based on 2,2-diphenyl-1-picrylhydrazyl radical and 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) radical-scavenging abilities, reducing power, and nitric oxide-and nitrate-scavenging activities. The results demonstrated that the antioxidant ability of guava leaf extracts has a strong relationship with phenolic compound content rather than flavonoid content. Phenolic compound content of water extracted guava leaves was higher compared to pure ethanol and methanol extracts. However, phenolic compound content extracted using hydroethanolic solvent was higher than water, whereas 50% hydroethanolic was observed to be the most effective solvent showing high antioxidant ability.

Deep eutectic solvents as efficient solvent system for the extraction of κ-carrageenan from Kappaphycus alvarezii.

PubMed

Das, Arun Kumar; Sharma, Mukesh; Mondal, Dibyendu; Prasad, Kamalesh

2016-01-20

Three different deep eutectic solvents (DESs) prepared by the complexation of choline chloride with urea, ethylene glycol and glycerol along with their hydrated counterparts were used for the selective extraction of κ-carrageenan from Kappaphycus alvarezii. Upon comparison of the quality of the polysaccharide with the one obtained using water as extraction media as well as the one extracted using widely practiced conventional method, it was found that, the physicochemical as well as rheological properties of κ-carrageenan obtained using DESs as solvents was at par to the one obtained using conventional method and was superior in quality when compared to κ-carrageenan obtained using water as solvent. Considering the tedious nature of the extraction method employed in conventional extraction process, the DESs can be considered as suitable alternative solvents for the facile extraction of the polysaccharide directly from the seaweed. However, among the hydrated and non-hydrated DESs, the hydrated ones were found to be more effective in comparison to their non-hydrated counterparts. Copyright © 2015 Elsevier Ltd. All rights reserved.

High-temperature solid-phase microextraction procedure for the detection of drugs by gas chromatography-mass spectrometry.

PubMed

Staerk, U; Külpmann, W R

2000-08-18

High-temperature headspace solid-phase microextraction (SPME) with simultaneous ("in situ") derivatisation (acetylation or silylation) is a new sample preparation technique for the screening of illicit drugs in urine and for the confirmation analysis in serum by GC-MS. After extraction of urine with a small portion of an organic solvent mixture (e.g., 2 ml of hexane-ethyl acetate) at pH 9, the organic layer is separated and evaporated to dryness in a small headspace vial. A SPME-fiber (e.g., polyacrylate) doped with acetic anhydride-pyridine (for acetylation) is exposed to the vapour phase for 10 min at 200 degrees C in a blockheater. The SPME fiber is then injected into the GC-MS for thermal desorption and analysis. After addition of perchloric acid and extraction with n-hexane to remove lipids, the serum can be analysed after adjusting to pH 9 as described for urine. Very clean extracts are obtained. The various drugs investigated could be detected and identified in urine by the total ion current technique at the following concentrations: amphetamines (200 microg/l), barbiturates (500 microg/l), benzodiazepines (100 microg/l), benzoylecgonine (150 microg/l), methadone (100 microg/l) and opiates (200 microg/l). In serum all drugs could be detected by the selected ion monitoring technique within their therapeutic range. As compared to liquid-liquid extraction only small amounts of organic solvent are needed and larger amounts of the pertinent analytes could be transferred to the GC column. In contrast to solid-phase extraction (SPE), the SPME-fiber is reusable several times (as there is no contamination by endogenous compounds). The method is time-saving and can be mechanised by the use of a dedicated autosampler.

Green ultrasound-assisted extraction of carotenoids from pomegranate wastes using vegetable oils.

PubMed

Goula, Athanasia M; Ververi, Maria; Adamopoulou, Anna; Kaderides, Kyriakos

2017-01-01

The objective of this work was to develop a new process for pomegranate peels application in food industries based on ultrasound-assisted extraction of carotenoids using different vegetable oils as solvents. In this way, an oil enriched with antioxidants is produced. Sunflower oil and soy oil were used as alternative solvents and the effects of various parameters on extraction yield were studied. Extraction temperature, solid/oil ratio, amplitude level, and extraction time were the factors investigated with respect to extraction yield. Comparative studies between ultrasound-assisted and conventional solvent extraction were carried out in terms of processing procedure and total carotenoids content. The efficient extraction period for achieving maximum yield of pomegranate peel carotenoids was about 30min. The optimum operating conditions were found to be: extraction temperature, 51.5°C; peels/solvent ratio, 0.10; amplitude level, 58.8%; solvent, sunflower oil. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound extraction under different processing parameters. Copyright © 2016 Elsevier B.V. All rights reserved.

A novel procedure for the extraction of protein deposits from soft hydrophilic contact lenses for analysis.

PubMed

Keith, D; Hong, B; Christensen, M

1997-05-01

A quick, simple, and efficient extraction technique was developed for the removal of protein from soft hydrophilic contact lenses. An extraction solvent consisting of a 50:50 mix of 0.2% trifluoroacetic acid and acetonitrile was used to remove protein from in vitro laboratory-deposited and human-worn contact lenses. The protein removed was analyzed using HPLC, bicinchoninic acid (BCA) analysis, and SDS-PAGE gel electreophoresis. Extraction efficiency for lysozyme from laboratory-deposited Group IV lenses was determined to be approximately 100%. Group IV human-worn contact lenses were extracted and analyzed for lysozyme by HPLC and total protein by bicinchoninic acid (BCA) analysis. Groups I, II, III, and IV contact lenses deposited with an artificial tear protein solution and human-worn lenses were extracted and analyzed by SDS-PAGE gel electreophoresis and micro-BCA. The ACN/TFA procedure offers a simple, quick, and efficient extraction technique for removal of protein from contact lenses for subsequent analysis.

Characteristics and antioxidant of Ulva intestinalis sulphated polysaccharides extracted with different solvents.

PubMed

Peasura, Napassorn; Laohakunjit, Natta; Kerdchoechuen, Orapin; Wanlapa, Sorada

2015-11-01

Ulva intestinalis, a tubular green seaweed, is a rich source of nutrient, especially sulphated polysaccharides. Sulphated polysaccharides from U. intestinalis were extracted with distilled water, 0.1N HCl, and 0.1N NaOH at 80°C for 1, 3, 6, 12, and 24h to study the effect of the extraction solvent and time on their chemical composition and antioxidant activity. Different types of solvents and extraction time had a significant influence on the chemical characteristics and antioxidant activity (p<0.05). Monosaccharide composition and FT-IR spectra analyses revealed that sulphated polysaccharides from all solvent extractions have a typical sugar backbone (glucose, rhamnose, and sulphate attached at C-2 or C-3 of rhamnose). Sulphated polysaccharides extracted with acid exhibited greater antioxidant activity than did those extracted with distilled water and alkali. The results indicated that solvent extraction could be an efficacious method for enhancing antioxidant activity by distinct molecular weight and chemical characteristic of sulphated polysaccharides. Copyright © 2015 Elsevier B.V. All rights reserved.

SOLVENT EXTRACTION PROCESS FOR THE SEPARATION OF URANIUM AND THORIUM FROM PROTACTINIUM AND FISSION PRODUCTS

DOEpatents

Rainey, R.H.; Moore, J.G.

1962-08-14

A liquid-liquid extraction process was developed for recovering thorium and uranium values from a neutron irradiated thorium composition. They are separated from a solvent extraction system comprising a first end extraction stage for introducing an aqueous feed containing thorium and uranium into the system consisting of a plurality of intermediate extractiorr stages and a second end extractron stage for introducing an aqueous immiscible selective organic solvent for thorium and uranium in countercurrent contact therein with the aqueous feed. A nitrate iondeficient aqueous feed solution containing thorium and uranium was introduced into the first end extraction stage in countercurrent contact with the organic solvent entering the system from the second end extraction stage while intro ducing an aqueous solution of salting nitric acid into any one of the intermediate extraction stages of the system. The resultant thorium and uranium-laden organic solvent was removed at a point preceding the first end extraction stage of the system. (AEC)

Selective mixed-bed solid phase extraction of atrazine herbicide from environmental water samples using molecularly imprinted polymer.

PubMed

Zarejousheghani, Mashaalah; Fiedler, Petra; Möder, Monika; Borsdorf, Helko

2014-11-01

A novel approach for the selective extraction of organic target compounds from water samples has been developed using a mixed-bed solid phase extraction (mixed-bed SPE) technique. The molecularly imprinted polymer (MIP) particles are embedded in a network of silica gel to form a stable uniform porous bed. The capabilities of this method are demonstrated using atrazine as a model compound. In comparison to conventional molecularly imprinted-solid phase extraction (MISPE), the proposed mixed-bed MISPE method in combination with gas chromatography-mass spectrometry (GC-MS) analysis enables more reproducible and efficient extraction performance. After optimization of operational parameters (polymerization conditions, bed matrix ingredients, polymer to silica gel ratio, pH of the sample solution, breakthrough volume plus washing and elution conditions), improved LODs (1.34 µg L(-1) in comparison to 2.25 µg L(-1) obtained using MISPE) and limits of quantification (4.5 µg L(-1) for mixed-bed MISPE and 7.5 µg L(-1) for MISPE) were observed for the analysis of atrazine. Furthermore, the relative standard deviations (RSDs) for atrazine at concentrations between 5 and 200 µg L(-1) ranged between 1.8% and 6.3% compared to MISPE (3.5-12.1%). Additionally, the column-to-column reproducibility for the mixed-bed MISPE was significantly improved to 16.1%, compared with 53% that was observed for MISPE. Due to the reduced bed-mass sorbent and at optimized conditions, the total amount of organic solvents required for conditioning, washing and elution steps reduced from more than 25 mL for conventional MISPE to less than 2 mL for mixed-bed MISPE. Besides reduced organic solvent consumption, total sample preparation time of the mixed-bed MISPE method relative to the conventional MISPE was reduced from more than 20 min to less than 10 min. The amount of organic solvent required for complete elution diminished from 3 mL (conventional MISPE) to less than 0.4 mL with the mixed-bed technique shows its inherent potential for online operation with an analytical instrument. In order to evaluate the selectivity and matrix effects of the developed mixed-bed MISPE method, it was applied as an extraction technique for atrazine from environmental wastewater and river water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-06-26

Counter-current chromatography (CCC) is an efficient liquid-liquid chromatography technique for separation and purification of complex mixtures like natural products extracts and synthetic chemicals. However, CCC is still a challenging process requiring some special technical knowledge especially in the selection of appropriated solvent systems. In this work, we introduced a new 9 × 9 map-based solvent selection strategy for CCC isolation of targets, which permit more than 60 hexane-ethyl acetate-methanol-water (HEMWat) solvent systems as the start candidates for the selection of solvent systems. Among these solvent systems, there are clear linear correlations between partition coefficient (K) and the system numbers. Thus, an appropriate CCC solvent system (i.e., sweet spot for K = 1) may be hit by measurement of k values of the target only in two random solvent systems. Besides this, surprisingly, we found that through two sweet spots, we could get a line ("Sweet line") where there are infinite sweet solvent systems being suitable for CCC separation. In these sweet solvent systems, the target has the same partition coefficient (K) but different solubilities. Thus, the better sweet solvent system with higher sample solubility can be obtained for high capacity CCC preparation. Furthermore, we found that there is a zone ("Sweet zone") where all solvent systems have their own sweet partition coefficients values for the target in range of 0.4 < K< 2.5 or extended range of 0.25 < K < 16. All results were validated by using 14 pure GUESSmix mimic natural products as standards and further confirmed by isolation of several targets including honokiol and magnolol from the extracts of Magnolia officinalis Rehd. Et Wils and tanshinone IIA from Salvia miltiorrhiza Bunge. In practice, it is much easier to get a suitable solvent system only by making a simple screening two to four HEMWat two-phase solvent systems to obtain the sweet line or sweet zone without special knowledge or comprehensive standards as references. This is an important advancement for solvent system selection and also will be very useful for isolation of current natural products including Traditional Chinese Medicines. Copyright © 2015 Elsevier B.V. All rights reserved.

REMEDIATING PESTICIDE CONTAMINATED SOILS USING SOLVENT EXTRACTION

EPA Science Inventory

Bench-scale solvent extraction studies were performed on soil samples obtained from a Superfund site contaminated with high levels of p,p'-DDT, p,p'-DDD,, p,p'-DDE and toxaphene. The effectiveness of the solvent extraction process was assessed using methanol and 2-propanol as sol...

Solvent Extraction of Furfural From Biomass

NASA Technical Reports Server (NTRS)

Humphrey, M. F.

1984-01-01

Solvent-extraction method reduces energy required to remove furfural produced during acid hydrolysis of biomass. Acid hydrolysis performed in vessel containing both solvents and reacting ingredients. With intimate contact between solvents and aqueous hydrolyis liqour, furfural removed form liquor almost as fast as it forms.

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

Brown, Nigel; Lodge, Mike; Hilton, Linda

The nuclear industry is not a provider of oils and solvents but uses them in motors, equipment and even in chemical processes to extract valuable products. Currently, for old and contaminated oils and solvents, techniques still exist, such as incineration, but not all the oils and solvents are compatible with this technique because the activities of some components inside the oils are too high to be accepted at the incineration facility. For these oils, an alternative technique needs to be found for treatment. A process developed for water treatment using a technique of adsorption coupled with electrochemical regeneration has beenmore » investigated to assess its capability to treat these organic wastes. One of the strengths of the process is its flexibility and adaptation to different compositions of oils. This point is important because, in the AREVA case, there are a lot of small volumes of old oils which need to be re-characterized. It takes time and money to do it especially when oils are contaminated; this is one reason why the technique is interesting to investigate. Tests have been performed with different oils coming from different sites to test the feasibility. Results demonstrate the destruction of a range of organics with regeneration energy requirements of 13.4 - 68.7 kWh/l and offer confidence for the future potential of the process. (authors)« less

Comparison of solvent extraction and solid-phase extraction for the determination of polychlorinated biphenyls in transformer oil.

PubMed

Mahindrakar, A N; Chandra, S; Shinde, L P

2014-01-01

Solid-phase extraction (SPE) of nine polychlorinated biphenyls (PCBs) from transformer oil samples was evaluated using octadecyl (CI8)-bonded porous silica. The efficiency of SPE of these PCBs was compared with those obtained by solvent extraction with DMSO and hexane. Average recoveries exceeding 95% for these PCBs were obtained via the SPE method using small cartridges containing 100mg of 40 pm CI8-bonded porous silica. The average recovery by solvent extraction with DMSO and hexane exceeded 83%. It was concluded that the recoveries and precision for the solvent extraction of PCBs were poorer than those for the SPE. Copyright © 2013 Elsevier Ltd. All rights reserved.

An alternative method for analysis of food taints using stir bar sorptive extraction.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2010-09-10

The determination of taints in food products currently can involve the use of several sample extraction techniques, including direct headspace (DHS), steam distillation extraction (SDE) and more recently solid phase microextraction (SPME). Each of these techniques has disadvantages, such as the use of large volumes of solvents (SDE), or limitations in sensitivity (DHS), or have only been applied to date for determination of individual or specific groups of tainting compounds (SPME). The use of stir bar sorptive extraction (SBSE) has been evaluated as a quantitative screening method for unknown tainting compounds in foods. A range of commonly investigated problem compounds, with a range of physical and chemical properties, were examined. The method was optimised to give the best response for the majority of compounds and the performance was evaluated by examining the accuracy, precision, linearity, limits of detection and quantitation and uncertainties for each analyte. For most compounds SBSE gave the lowest limits of detection compared to steam distillation extraction or direct headspace analysis and in general was better than these established techniques. However, for methyl methacrylate and hexanal no response was observed following stir bar extraction under the optimised conditions. The assays were carried out using a single quadrupole GC-MS in scan mode. A comparison of acquisition modes and instrumentation was performed using standards to illustrate the increase in sensitivity possible using more targeted ion monitoring or a more sensitive high resolution mass spectrometer. This comparison illustrated the usefulness of this approach as an alternative to specialised glassware or expensive instrumentation. SBSE in particular offers a 'greener' extraction method by a large reduction in the use of organic solvents and also minimises the potential for contamination from external laboratory sources, which is of particular concern for taint analysis. Copyright © 2010 Elsevier B.V. All rights reserved.

Method of infusion extraction

NASA Technical Reports Server (NTRS)

Chang-Diaz, Franklin R. (Inventor)

1989-01-01

Apparatus and method of removing desirable constituents from an infusible material by infusion extraction, where a piston operating in a first chamber draws a solvent into the first chamber where it may be heated, and then moves the heated solvent into a second chamber containing the infusible material, and where infusion extraction takes place. The piston then moves the solvent containing the extract through a filter into the first chamber, leaving the extraction residue in the second chamber.

Emerging Trends in Microwave Processing of Spices and Herbs.

PubMed

Rahath Kubra, Ismail; Kumar, Devender; Jagan Mohan Rao, Lingamallu

2016-10-02

Today, spices are integral part of our food as they provide sensory attributes such as aroma, color, flavour and taste to food. Further their antimicrobial, antioxidant, pharmaceutical and nutritional properties are also well known. Since spices are seasonal so their availability can be extended year round by adopting different preservation techniques. Drying and extraction are most important methods for preservation and value addition to spices. There are different techniques for drying of spices with their own advantages and limitations. A novel, non-conventional technique for drying of spices is use of microwave radiation. This technique proved to be very rapid, and also provide a good quality product. Similarly, there are a number of non-conventional extraction methods in use that are all, in principle, solid-liquid extractions but which introduce some form of additional energy to the process in order to facilitate the transfer of analytes from sample to solvent. This paper reviews latest advances in the use of microwave energy for drying of spices and herbs. Also, the review describes the potential application of microwave energy for extraction of essential oil/bioactive components from spices and herbs and the advantages of microwave-assisted process over the other extraction processes generally employed for extraction. It also showcases some recent research results on microwave drying/extraction from spices and herbs.

Continuous extraction of organic materials from water

USGS Publications Warehouse

Goldberg, M.C.; DeLong, L.; Kahn, L.

1971-01-01

A continuous liquid solvent extractor, designed to utilize organic solvents that are heavier than water, is described. The extractor is capable of handling input rates up to 2 liters per hour and has a 500-ml. extractant capacity. Extraction efficiency is dependent upon the p-value, the two solvent ratios, rate of flow of the aqueous phase, and rate of reflux of the organic phase. Extractors can be serially coupled to increase extraction efficiency and, when coupled with a lighter-than-water extractor, the system will allow the use of any immiscible solvent.

Process for producing fuel grade ethanol by continuous fermentation, solvent extraction and alcohol separation

DOEpatents

Tedder, Daniel W.

1985-05-14

Alcohol substantially free of water is prepared by continuously fermenting a fermentable biomass feedstock in a fermentation unit, thereby forming an aqueous fermentation liquor containing alcohol and microorganisms. Continuously extracting a portion of alcohol from said fermentation liquor with an organic solvent system containing an extractant for said alcohol, thereby forming an alcohol-organic solvent extract phase and an aqueous raffinate. Said alcohol is separated from said alcohol-organic solvent phase. A raffinate comprising microorganisms and unextracted alcohol is returned to the fermentation unit.

Microwave-assisted extraction (MAE) of bioactive saponin from mahogany seed (Swietenia mahogany Jacq)

NASA Astrophysics Data System (ADS)

Waziiroh, E.; Harijono; Kamilia, K.

2018-03-01

Mahogany is frequently used for medicines for cancer, tumor, and diabetes, as it contains saponin and flavonoid. Saponin is a complex glycosydic compound consisted of triterpenoids or steroids. Saponin can be extracted from a plant by using a solvent extraction. Microwave Assisted Extraction (MAE) is a non-conventional extraction method that use micro waves in the process. This research was conducted by a Complete Random Design with two factors which were extraction time (120, 150, and 180 seconds) and solvent ratio (10:1, 15:1, and 20:1 v/w). The best treatment of MAE were the solvent ratio 15:1 (v/w) for 180 seconds. The best treatment resulting crude saponin extract yield of 41.46%, containing 11.53% total saponins, and 49.17% of antioxidant activity. Meanwhile, the treatment of maceration method were the solvent ratio 20:1 (v/w) for 48 hours resulting 39.86% yield of saponin crude extract, 9.26% total saponins and 56.23% of antioxidant activity. The results showed MAE was more efficient (less time of extraction and solvent amount) than maceration method.

Environmental life cycle assessment on the separation of rare earth oxides through solvent extraction.

PubMed

Vahidi, Ehsan; Zhao, Fu

2017-12-01

Over the past decade, Rare Earth Elements (REEs) have gained special interests due to their significance in many industrial applications, especially those related to clean energy. While REEs production is known to cause damage to the ecosystem, only a handful of Life Cycle Assessment (LCA) investigations have been conducted in recent years, mainly due to lack of data and information. This is especially true for the solvent extraction separation of REEs from aqueous solution which is a challenging step in the REEs production route. In the current investigation, an LCA is carried out on a typical REE solvent extraction process using P204/kerosene and the energy/material flows and emissions data were collected from two different solvent extraction facilities in Inner Mongolia and Fujian provinces in China. In order to develop life cycle inventories, Ecoinvent 3 and SimaPro 8 software together with energy/mass stoichiometry and balance were utilized. TRACI and ILCD were applied as impact assessment tools and LCA outcomes were employed to examine and determine ecological burdens of the REEs solvent extraction operation. Based on the results, in comparison with the production of generic organic solvent in the Ecoinvent dataset, P204 production has greater burdens on all TRACI impact categories. However, due to the small amount of consumption, the contribution of P204 remains minimal. Additionally, sodium hydroxide and hydrochloric acid are the two impactful chemicals on most environmental categories used in the solvent extraction operation. On average, the solvent extraction step accounts for 30% of the total environmental impacts associated with individual REOs. Finally, opportunities and challenges for an enhanced environmental performance of the REEs solvent extraction operation were investigated. Copyright © 2017 Elsevier Ltd. All rights reserved.

Study to find the best extraction solvent for use with guava leaves (Psidium guajava L.) for high antioxidant efficacy

PubMed Central

Seo, Jongkwon; Lee, Soojung; Elam, Marcus L; Johnson, Sarah A; Kang, Jonghoon; Arjmandi, Bahram H

2014-01-01

The effects of guava leaves extracted using solvents of water, ethanol, methanol, and different concentrations of hydroethanolic solvents on phenolic compounds and flavonoids, and antioxidant properties have been investigated. The antioxidant capability was assessed based on 2,2-diphenyl-1-picrylhydrazyl radical and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) radical-scavenging abilities, reducing power, and nitric oxide-and nitrate-scavenging activities. The results demonstrated that the antioxidant ability of guava leaf extracts has a strong relationship with phenolic compound content rather than flavonoid content. Phenolic compound content of water extracted guava leaves was higher compared to pure ethanol and methanol extracts. However, phenolic compound content extracted using hydroethanolic solvent was higher than water, whereas 50% hydroethanolic was observed to be the most effective solvent showing high antioxidant ability. PMID:24804076

A combination of solvent extraction and freeze thaw for oil recovery from petroleum refinery wastewater treatment pond sludge.

PubMed

Hu, Guangji; Li, Jianbing; Hou, Haobo

2015-01-01

A combination of solvent extraction and freeze thaw was examined for recovering oil from the high-moisture petroleum refinery wastewater treatment pond sludge. Five solvents including cyclohexane (CHX), dichloromethane (DCM), methyl ethyl ketone (MEK), ethyl acetate (EA), and 2-propanol (2-Pro) were examined. It was found that these solvents except 2-Pro showed a promising oil recovery rate of about 40%, but the recycling of DCM solvent after oil extraction was quite low. Three solvents (CHX, MEK and EA) were then selected for examining the effect of freeze/thaw treatment on improving the quality of recovered oil. This treatment increased the total petroleum hydrocarbon (TPH) content in recovered oil from about 40% to 60% for both MEK and EA extractions, but little effect was observed for CHX extraction. Although the solid residue after oil recovery had a significantly decreased TPH content, a high concentration of heavy metals was observed, indicating that this residue may require proper management. In general, the combination of solvent extraction with freeze/thaw is effective for high-moisture oily hazardous waste treatment. Copyright © 2014 Elsevier B.V. All rights reserved.

Optimisation of Microwave-Assisted Extraction of Pomegranate (Punica granatum L.) Seed Oil and Evaluation 
of Its Physicochemical and Bioactive Properties.

PubMed

Çavdar, Hasene Keskin; Yanık, Derya Koçak; Gök, Uğur; Göğüş, Fahrettin

2017-03-01

Pomegranate seed oil was extracted in a closed-vessel high-pressure microwave system. The characteristics of the obtained oil, such as fatty acid composition, free fatty acidity, total phenolic content, antioxidant activity and colour, were compared to those of the oil obtained by cold solvent extraction. Response surface methodology was applied to optimise extraction conditions: power (176-300 W), time (5-20 min), particle size ( d =0.125-0.800 mm) and solvent to sample ratio (2:1, 6:1 and 10:1, by mass). The predicted highest extraction yield (35.19%) was obtained using microwave power of 220 W, particle size in the range of d =0.125-0.450 mm and solvent-to-sample ratio of 10:1 (by mass) in 5 min extraction time. Microwave-assisted solvent extraction (MASE) resulted in higher extraction yield than that of Soxhlet (34.70% in 8 h) or cold (17.50% in 8 h) extraction. The dominant fatty acid of pomegranate seed oil was punicic acid (86%) irrespective of the extraction method. Oil obtained by MASE had better physicochemical properties, total phenolic content and antioxidant activity than the oil obtained by cold solvent extraction.

Control of human filarial vector, Culex quinquefasciatus Say 1823 (Diptera: Culicidae) through bioactive fraction of Cayratia trifolia leaf.

PubMed

Chakraborty, Sumanta; Singha, Someshwar; Bhattacharya, Kuntal; Chandra, Goutam

2013-12-01

To investigate the mosquito larvicidal activity of Cayratia trifolia (L.) Domin (Vitaceae: Vitales) (C. trifolia) which is distributed in many parts of India with medicinal properties as vector control is facing threat due to the emergence of resistance to synthetic insecticides. Young and mature leaves of C. trifolia were investigated for larvicidal activity against 3rd instars larvae of Culex quinquefasciatus in different seasons throughout the year. The active fractions were extracted using six different solvents in a non-polar to polar fashion viz petroleum-ether, benzene, chloroform: methanol (1:1 v/v), acetone, absolute alcohol and distilled water. Dose dependent mortality was recorded against each solvent extract. Determination of LD50 and LD90 were executed through log-probit analysis using the most bioactive fraction. The fluctuations in mortality were statistically co-related through ANOVA analyses concerning different seasons and types of leaves as random variables. Justification of larvicidal activity was established through student's t-test. Costing effects were evaluated on the non-target water fauna under laboratory conditions. Thin layer chromatographic techniques were performed for phytochemical analysis and categorization of chemical personality of the active fractions using the most effective solvent extract following standard methods. Significant variations in mortality rate were noted with respect to the type of leaves (mature and senescence), concentration of leaf extract and between seasons. The water extract among all the solvent extracts was found to induce cent percent mortality at 50 mg/L in test mosquito species within 24 h with a LD50 and LD90 value of 10.70 mg/L and 27.64 mg/L respectively. No significant mortality was recorded in non-target water population. Chromatographic analyses of the water extract revealed the presence of steroids, triterpene glycosides, essential oil, phenolics and diterpenes as secondary phytochemicals. Water extract of C. trifolia leaf promised as a cost effective and potent larvicidal agent against Culex quinquefasciatus. Copyright © 2013 Asian Pacific Tropical Biomedical Magazine. Published by Elsevier B.V. All rights reserved.

ASE extraction method for simultaneous carbon and nitrogen stable isotope analysis in soft tissues of aquatic organisms.

PubMed

Bodin, Nathalie; Budzinski, Hélène; Le Ménach, Karyn; Tapie, Nathalie

2009-06-08

Since lipids are depleted in 13C relative to proteins and carbohydrates, variations in lipid composition among species and within individuals significantly influence delta13C and may result in misleading ecological interpretations. Whereas lipid extraction before IRMS analysis constitutes a way of stable isotope result lipid-normalisation, such a procedure was given up because of the un-controlled effects of the methods used (i.e., "Bligh & Dyer", Soxhlet, etc.) on delta15N. The aim of this work was to develop a simple, rapid and efficient lipid extraction method allowing for simultaneous C and N stable isotope analysis in the biological soft tissues of aquatic organisms. The goal was to be free from the lipid influence on delta13C values without interfering with delta15N values. For that purpose, the modern automated pressurized liquid extraction technique ASE (accelerated solvent extraction) was selected. Eel muscles representative of a broad range of fat contents were extracted via ASE by using different semi-polar solvents (100% dichloromethane and 80% n-hexane/20% acetone) and by operating at different temperature (ambient temperature and 100 degrees C) and pressure (750 and 1900 psi) conditions. The results were discussed in terms of lipid extraction efficiency as well as delta13C and delta15N variability.

Instrument for Analysis of Organic Compounds on Other Planets

NASA Technical Reports Server (NTRS)

Daulton, Riley M.; Hintze, Paul E.

2016-01-01

The goal of this project is to develop the Instrument for Solvent Extraction and Analysis of Extraterrestrial Bodies using In Situ Resources (ISEE). Specifically, ISEE will extract and characterize organic compounds from regolith which is found on the surface of other planets or asteroids. The techniques this instrument will use are supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC). ISEE aligns with NASA's goal to expand the frontiers of knowledge, capability, and opportunities in space in addition to supporting NASA's aim to search for life elsewhere by characterizing organic compounds. The outcome of this project will be conceptual designs of 2 components of the ISEE instrument as well as the completion of proof-of-concept extraction experiments to demonstrate the capabilities of SFE. The first conceptual design is a pressure vessel to be used for the extraction of the organic compounds from the regolith. This includes a comparison of different materials, geometry's, and a proposition of how to insert the regolith into the vessel. The second conceptual design identifies commercially available fluid pumps based on the requirements needed to generate supercritical CO2. The proof-of-concept extraction results show the percent mass lost during standard solvent extractions of regolith with organic compounds. This data will be compared to SFE results to demonstrate the capabilities of ISEE's approach.

Process development for recovery of vanadium and nickel from an industrial solid waste by a leaching-solvent extraction technique.

PubMed

Barik, S P; Park, K H; Nam, C W

2014-12-15

A process for recovering V(V) and Ni(II) from an industrial solid waste using sulfuric acid leaching, solvent extraction, precipitation and crystallization has been developed. The leaching parameters investigated were time, temperature and H2SO4 concentration. To quantify the linear and interaction coefficients a 2(3) full factorial experimental design was used. Regression equations for the extraction of V(V) and Ni(II) were determined and the adequacy of these equations was tested by Student's t-Test. More than 98% of both V(V) and Ni(II) were extracted in 90 min using 1.35 M H2SO4 at 40 °C. In addition, solvent extraction of V(V) with LIX 84-I in kerosene from the acidic leach liquor bearing 10.922 g/L V(V) and 18.871 g/L of Ni(II) was investigated. V(V) was extracted selectively using 40% LIX 84-I followed by stripping with NH4OH solution. McCabe-Thiele plots at O:A = 2:3 with 40% LIX 84-I and O:A = 3:1 with 15% (v/v) NH4OH showed two and three theoretical stages are needed for quantitative extraction and stripping of V(V), respectively. Ni(II) was selectively recovered from the V(V) free raffinate by adding ammonium oxalate at 60 °C. The purity of different products such as ammonium vanadate, nickel oxalate and nickel oxide obtained during the processes were analyzed and confirmed from the XRD studies. Copyright © 2014 Elsevier Ltd. All rights reserved.

FY10 Report on Multi-scale Simulation of Solvent Extraction Processes: Molecular-scale and Continuum-scale Studies

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

Wardle, Kent E.; Frey, Kurt; Pereira, Candido

2014-02-02

This task is aimed at predictive modeling of solvent extraction processes in typical extraction equipment through multiple simulation methods at various scales of resolution. We have conducted detailed continuum fluid dynamics simulation on the process unit level as well as simulations of the molecular-level physical interactions which govern extraction chemistry. Through combination of information gained through simulations at each of these two tiers along with advanced techniques such as the Lattice Boltzmann Method (LBM) which can bridge these two scales, we can develop the tools to work towards predictive simulation for solvent extraction on the equipment scale (Figure 1). Themore » goal of such a tool-along with enabling optimized design and operation of extraction units-would be to allow prediction of stage extraction effrciency under specified conditions. Simulation efforts on each of the two scales will be described below. As the initial application of FELBM in the work performed during FYl0 has been on annular mixing it will be discussed in context of the continuum-scale. In the future, however, it is anticipated that the real value of FELBM will be in its use as a tool for sub-grid model development through highly refined DNS-like multiphase simulations facilitating exploration and development of droplet models including breakup and coalescence which will be needed for the large-scale simulations where droplet level physics cannot be resolved. In this area, it can have a significant advantage over traditional CFD methods as its high computational efficiency allows exploration of significantly greater physical detail especially as computational resources increase in the future.« less

Group extraction of organic compounds present in liquid samples

NASA Technical Reports Server (NTRS)

Jahnsen, Vilhelm J. (Inventor)

1976-01-01

An extraction device is disclosed comprising a tube containing a substantially inert, chemically non-reactive packing material with a large surface area to volume ratio. A sample which consists of organic compounds dissolved in a liquid, is introduced into the tube. As the sample passes through the packing material it spreads over the material's large surface area to form a thin liquid film which is held on the packing material in a stationary state. A particular group or family of compounds is extractable from the sample by passing a particular solvent system consisting of a solvent and selected reagents through the packing material. The reagents cause optimum conditions to exist for the compounds of the particular family to pass through the phase boundary between the sample liquid and the solvent of the solvent system. Thus, the compounds of the particular family are separated from the sample liquid and become dissolved in the solvent of the solvent system. The particular family of compounds dissolved in the solvent, representing an extract, exits the tube together with the solvent through the tube's nozzle, while the rest of the sample remains on the packing material in a stationary state. Subsequently, a different solvent system may be passed through the packing material to extract another family of compounds from the remaining sample on the packing material.

EXTRACTION OF SEDIMENT-BOUND CHLORINATED ORGANIC COMPOUNDS: IMPLICATIONS ON FATE AND HAZARD ASSESSMENT. (R825513C007)

EPA Science Inventory

Five methods were used for the extraction of hexachlorobutadiene and chlorobenzenes from a contaminated estuarine sediment. The following extraction methods were used: Soxhlet extraction, sonication and solvent extraction, sequential solvent extraction, saponification and solv...

Phenolic content and antioxidant activity of Hibiscus cannabinus L. seed extracts after sequential solvent extraction.

PubMed

Yusri, Noordin Mohd; Chan, Kim Wei; Iqbal, Shahid; Ismail, Maznah

2012-10-25

A sequential solvent extraction scheme was employed for the extraction of antioxidant compounds from kenaf (Hibiscus cannabinus L.) seeds. Yield of extracts varied widely among the solvents and was the highest for hexane extract (16.6% based on dry weight basis), while water extract exhibited the highest total phenolic content (18.78 mg GAE/g extract), total flavonoid content (2.49 mg RE/g extract), and antioxidant activities (p < 0.05). DPPH and hydroxyl radical scavenging, β-carotene bleaching, metal chelating activity, ferric thiocyanate and thiobarbituric acid reactive substances assays were employed to comprehensively assess the antioxidant potential of different solvent extracts prepared sequentially. Besides water, methanolic extract also exhibited high retardation towards the formation of hydroperoxides and thiobarbituric acid reactive substances in the total antioxidant activity tests (p < 0.05). As conclusion, water and methanol extracts of kenaf seed may potentially serve as new sources of antioxidants for food and nutraceutical applications.

Method for testing earth samples for contamination by organic contaminants

DOEpatents

Schabron, John F.

1996-01-01

Provided is a method for testing earth samples for contamination by organic contaminants, and particularly for aromatic compounds such as those found in diesel fuel and other heavy fuel oils, kerosene, creosote, coal oil, tars and asphalts. A drying step is provided in which a drying agent is contacted with either the earth sample or a liquid extract phase to reduce to possibility of false indications of contamination that could occur when humic material is present in the earth sample. This is particularly a problem when using relatively safe, non-toxic and inexpensive polar solvents such as isopropyl alcohol since the humic material tends to be very soluble in those solvents when water is present. Also provided is an ultraviolet spectroscopic measuring technique for obtaining an indication as to whether a liquid extract phase contains aromatic organic contaminants. In one embodiment, the liquid extract phase is subjected to a narrow and discrete band of radiation including a desired wave length and the ability of the liquid extract phase to absorb that wavelength of ultraviolet radiation is measured to provide an indication of the presence of aromatic organic contaminants.

Free radical scavenging of grape pomace extracts from Cabernet sauvingnon (Vitis vinifera).

PubMed

de Campos, Luanda M A S; Leimann, Fernanda V; Pedrosa, Rozangela Curi; Ferreira, Sandra R S

2008-11-01

Pressed grape pomace obtained from the wine production of Cabernet sauvignon (Vitis vinifera) vintage was dried until 9.8% moisture content, ground and submitted to extraction of soluble components from different extraction techniques. Low pressure extractions were performed with ethanol maceration followed by fractionation with n-hexane, dichloromethane, butanol and ethyl acetate. These solvents were furthermore applied for soxhlet extraction. Supercritical fluid extraction (SFE) was also performed to obtain grape pomace extracts by using pure CO2 and CO2 with ethanol as co-solvent in concentrations of 10, 15 and 20%w/w. The operating condition used in high pressure extractions was 150bar and 40 degrees C. The antioxidant activity of the grape pomace extracts was determined considering the free radical scavenging assay using 1,1-Diphenyl-2-picrylhydrazyl (DPPH) and was correlated with the total phenol content determined according to the Folin-Ciocalteu method. The results obtained in DPPH tests indicate the highest antioxidant activity of 96.6+/-0.3%AA, with an IC50 value of 13+/-1, for the extracts obtained with ethyl acetate in solid-liquid extraction. The highest yield values were achieved in soxhlet extraction with ethanol (13.2%w/w) and with butanol (12.2%w/w), and also by SFE with 15% ethanol (9.2%w/w). The lipophilic composition of grape pomace extracts was evaluated by gas chromatography-mass spectrometry with the identification of components like linoleic acid and ethyl linoleate, with important therapeutic activities.

Effects of pH changes in water-based solvents to isolate antibacterial activated extracts of natural products

NASA Astrophysics Data System (ADS)

Buang, Yohanes; Suwari, Ola, Antonius R. B.

2017-12-01

Effects of pH changes in solvents on isolation of antibacterial activities of natural product extracts were conducted in the present study. Sarang semut (M. pendens) tubers as the model material for the study was considered to be the strategic resource of natural products based on its biochemical and therapeutical effects. The water with pH 5, 7, 9, and 13 was used as the solvents. The antibacterial activities of the resulted extracts indicated that higher the working pH, higher activities of the resulted extracts. The extent activities of the resulted extracts followed the increasing pH of the maceration system. The study also found that higher pH of the working solvent, higher the amounts of the antibacterial extracts isolated from the sample matrix of the natural product. The higher pH of the water solvents plays essential roles to promote the antibacterial activities of the natural product extracts from M. pendens tubers.

Immobilized aptamer paper spray ionization source for ion mobility spectrometry.

PubMed

Zargar, Tahereh; Khayamian, Taghi; Jafari, Mohammad T

2017-01-05

A selective thin-film microextraction based on aptamer immobilized on cellulose paper was used as a paper spray ionization source for ion mobility spectrometry (PSI-IMS), for the first time. In this method, the paper is not only used as an ionization source but also it is utilized for the selective extraction of analyte, based on immobilized aptamer. This combination integrates both sample preparation and analyte ionization in a Whatman paper. To that end, an appropriate sample introduction system with a novel design was constructed for the paper spray ionization source. Using this system, a continuous solvent flow works as an elution and spray solvent simultaneously. In this method, analyte is adsorbed on a triangular paper with immobilized aptamer and then it is desorbed and ionized by elution solvent and applied high voltage on paper, respectively. The effects of different experimental parameters such as applied voltage, angle of paper tip, distance between paper tip and counter electrode, elution solvent type, and solvent flow rate were optimized. The proposed method was exhaustively validated in terms of sensitivity and reproducibility by analyzing the standard solutions of codeine and acetamiprid. The analytical results obtained are promising enough to ensure the use of immobilized aptamer paper-spray as both the extraction and ionization techniques in IMS for direct analysis of biomedicine. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

PubMed Central

2016-01-01

Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient's plasma sample using less than 550 μL of organic solvent. PMID:27830105

Organosolv extraction of lignin from hydrolyzed almond shells and application of the delta-value theory.

PubMed

Quesada-Medina, Joaquín; López-Cremades, Francisco Javier; Olivares-Carrillo, Pilar

2010-11-01

The solubility of lignin from hydrolyzed almond (Prunus amygdalus) shells in different acetone, ethanol and dioxane-water mixtures and conditions (extraction time and temperature) was studied. The concept of the solubility parameter (delta-value) was applied to explain the effect of organic solvent concentration on lignin solubility. The organic solvent-water mixture that led to the highest lignin extraction was composed of a 75% vol. of organic solvent for all the solvent series investigated (acetone, ethanol and dioxane). Moreover, the best lignin extraction conditions were a temperature of 210 degrees C and an extraction time of 40 min for the acetone and ethanol series, and 25 min for the dioxane series. The delta-value of the hydrolyzed almond shell lignin [14.60 (cal/cm(3))(1/2)] and that of the organic solvent-water mixtures was calculated. The experimental delignification capacity of the aqueous organic solvents clearly reflected the proximity of their delta-value to that of lignin. The hydrogen-bonding capacity of the solvent-water mixtures was also taken into account. Copyright 2010 Elsevier Ltd. All rights reserved.

Supercritical multicomponent solvent coal extraction

NASA Technical Reports Server (NTRS)

Corcoran, W. H.; Fong, W. S.; Pichaichanarong, P.; Chan, P. C. F.; Lawson, D. D. (Inventor)

1983-01-01

The yield of organic extract from the supercritical extraction of coal with larger diameter organic solvents such as toluene is increased by use of a minor amount of from 0.1 to 10% by weight of a second solvent such as methanol having a molecular diameter significantly smaller than the average pore diameter of the coal.

Oil recovery from petroleum sludge through ultrasonic assisted solvent extraction.

PubMed

Hu, Guangji; Li, Jianbing; Huang, Shuhui; Li, Yubao

2016-09-18

The effect of ultrasonic assisted extraction (UAE) process on oil recovery from refinery oily sludge was examined in this study. Two types of UAE treatment including UAE probe (UAEP) system and UAE bath (UAEB) system were investigated. Their oil recovery efficiencies were compared to that of mechanical shaking extraction (MSE). Three solvents including cyclohexane (CHX), ethyl acetate (EA), and methyl ethyl ketone (MEK) were examined as the extraction solvents. The influence of experimental factors on oil and solvent recovery was investigated using an orthogonal experimental design. Results indicated that solvent type, solvent-to-sludge (S/S) ratio, and treatment duration could have significant effects on oil recovery in UAE treatment. Under the optimum conditions, UAEP treatment can obtain an oil recovery of 68.8% within 20 s, which was higher than that (i.e., 62.0%) by MSE treatment after 60 min' extraction. UAEB treatment can also obtain a promising oil recovery within shorter extraction duration (i.e., 15 min) than MSE. UAE was thus illustrated as an effective and improved approach for oily sludge recycling.

Extending metabolome coverage for untargeted metabolite profiling of adherent cultured hepatic cells.

PubMed

García-Cañaveras, Juan Carlos; López, Silvia; Castell, José Vicente; Donato, M Teresa; Lahoz, Agustín

2016-02-01

MS-based metabolite profiling of adherent mammalian cells comprises several challenging steps such as metabolism quenching, cell detachment, cell disruption, metabolome extraction, and metabolite measurement. In LC-MS, the final metabolome coverage is strongly determined by the separation technique and the MS conditions used. Human liver-derived cell line HepG2 was chosen as adherent mammalian cell model to evaluate the performance of several commonly used procedures in both sample processing and LC-MS analysis. In a first phase, metabolite extraction and sample analysis were optimized in a combined manner. To this end, the extraction abilities of five different solvents (or combinations) were assessed by comparing the number and the levels of the metabolites comprised in each extract. Three different chromatographic methods were selected for metabolites separation. A HILIC-based method which was set to specifically separate polar metabolites and two RP-based methods focused on lipidome and wide-ranging metabolite detection, respectively. With regard to metabolite measurement, a Q-ToF instrument operating in both ESI (+) and ESI (-) was used for unbiased extract analysis. Once metabolite extraction and analysis conditions were set up, the influence of cell harvesting on metabolome coverage was also evaluated. Therefore, different protocols for cell detachment (trypsinization or scraping) and metabolism quenching were compared. This study confirmed the inconvenience of trypsinization as a harvesting technique, and the importance of using complementary extraction solvents to extend metabolome coverage, minimizing interferences and maximizing detection, thanks to the use of dedicated analytical conditions through the combination of HILIC and RP separations. The proposed workflow allowed the detection of over 300 identified metabolites from highly polar compounds to a wide range of lipids.

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.

Alternatives for Benzene in the Extraction of Bitumen Fume from Exposure Sample Media.

PubMed

Sutter, Benjamin; Ravera, Christel; Hussard, Caroline; Langlois, Eddy

2016-01-01

Benzene is frequently used to extract collected bitumen fumes from personal sampler substrates. However, this solvent is particularly dangerous because of its carcinogenicity (group 1 of the International Agency for Research on Cancer classification). Therefore, to prevent the exposure of laboratory technicians to benzene during the fume extraction step from samplers, a compromise had to be found to identify a less toxic solvent with the same extraction capacity. To compare the extraction capacities of selected solvents, bitumen fumes were generated in the laboratory from three different batches of road surfacing bitumen collected on dedicated bitumen fume samplers. The samplers were then extracted by benzene and the solvents tested. Of 11 selected solvents less toxic than benzene and used in studies on bitumen and bitumen fume analyses, n-hexane and n-heptane were identified as alternatives to benzene. In particular, the results demonstrated that n-heptane was the best candidate solvent for benzene replacement, due to its extraction efficiency comparable to benzene for the three bitumen fumes tested and its low toxicity, which is highly compatible with benzene replacement. © The Author 2015. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.

Direct analyte-probed nanoextraction coupled to nanospray ionization-mass spectrometry of drug residues from latent fingerprints.

PubMed

Clemons, Kristina; Wiley, Rachel; Waverka, Kristin; Fox, James; Dziekonski, Eric; Verbeck, Guido F

2013-07-01

Here, we present a method of extracting drug residues from fingerprints via Direct Analyte-Probed Nanoextraction coupled to nanospray ionization-mass spectrometry (DAPNe-NSI-MS). This instrumental technique provides higher selectivity and lower detection limits over current methods, greatly reducing sample preparation, and does not compromise the integrity of latent fingerprints. This coupled to Raman microscopy is an advantageous supplement for location and identification of trace particles. DAPNe uses a nanomanipulator for extraction and differing microscopies for localization of chemicals of interest. A capillary tip with solvent of choice is placed in a nanopositioner. The surface to be analyzed is placed under a microscope, and a particle of interest is located. Using a pressure injector, the solvent is injected onto the surface where it dissolves the analyte, and then extracted back into the capillary tip. The solution is then directly analyzed via NSI-MS. Analyses of caffeine, cocaine, crystal methamphetamine, and ecstasy have been performed successfully. © 2013 American Academy of Forensic Sciences.

Optimisation and validation of the microwave-assisted extraction of phenolic compounds from rice grains.

PubMed

Setyaningsih, W; Saputro, I E; Palma, M; Barroso, C G

2015-02-15

A new microwave-assisted extraction (MAE) method has been investigated for the extraction of phenolic compounds from rice grains. The experimental conditions studied included temperature (125-175°C), microwave power (500-1000W), time (5-15min), solvent (10-90% EtOAc in MeOH) and solvent-to-sample ratio (10:1 to 20:1). The extraction variables were optimised by the response surface methodology. Extraction temperature and solvent were found to have a highly significant effect on the response value (p<0.0005) and the extraction time also had a significant effect (p<0.05). The optimised MAE conditions were as follows: extraction temperature 185°C, microwave power 1000W, extraction time 20min, solvent 100% MeOH, and solvent-to-sample ratio 10:1. The developed method had a high precision (in terms of CV: 5.3% for repeatability and 5.5% for intermediate precision). Finally, the new method was applied to real samples in order to investigate the presence of phenolic compounds in a wide variety of rice grains. Copyright © 2014 Elsevier Ltd. All rights reserved.

Estimating body fat by using bioelectrical-impedance measurements: a preliminary assessment.

Treesearch

M.G. Raphael; H.J. Harlow; S.W. Buskirk

1991-01-01

We evaluated a technique for measuring body fat content of marten (Martes americana) by using a noninvasive bioelectrical-impedance device with four electrodes to introduce a current into the body. Instantaneous readings of resistance were significantly correlated with fat-free mass (determined from solvent extraction) of carcasses of 17 skinned (r...

Influence of extraction methodologies on the analysis of five major volatile aromatic compounds of citronella grass (Cymbopogon nardus) and lemongrass (Cymbopogon citratus) grown in Thailand.

PubMed

Chanthai, Saksit; Prachakoll, Sujitra; Ruangviriyachai, Chalerm; Luthria, Devanand L

2012-01-01

This paper deals with the systematic comparison of extraction of major volatile aromatic compounds (VACs) of citronella grass and lemongrass by classical microhydrodistillation (MHD), as well as modern accelerated solvent extraction (ASE). Sixteen VACs were identified by GC/MS. GC-flame ionization detection was used for the quantification of five VACs (citronellal, citronellol, geraniol, citral, and eugenol) to compare the extraction efficiency of the two different methods. Linear range, LOD, and LOQ were calculated for the five VACs. Intraday and interday precisions for the analysis of VACs were determined for each sample. The extraction recovery, as calculated by a spiking experiment with known standards of VACs, by ASE and MHD ranged from 64.9 to 91.2% and 74.3 to 95.2%, respectively. The extraction efficiency of the VACs was compared for three solvents of varying polarities (hexane, dichloromethane, and methanol), seven different temperatures (ranging from 40 to 160 degrees C, with a gradual increment of 20 degrees C), five time periods (from 1 to 10 min), and three cycles (1, 2, and 3 repeated extractions). Optimum extraction yields of VACs were obtained when extractions were carried out for 7 min with dichloromethane and two extraction cycles at 120 degrees C. The results showed that the ASE technique is more efficient than MHD, as it results in improved yields and significant reduction in extraction time with automated extraction capabilities.

Alternative Bio-Based Solvents for Extraction of Fat and Oils: Solubility Prediction, Global Yield, Extraction Kinetics, Chemical Composition and Cost of Manufacturing

PubMed Central

Sicaire, Anne-Gaëlle; Vian, Maryline; Fine, Frédéric; Joffre, Florent; Carré, Patrick; Tostain, Sylvain; Chemat, Farid

2015-01-01

The present study was designed to evaluate the performance of alternative bio-based solvents, more especially 2-methyltetrahydrofuran, obtained from crop’s byproducts for the substitution of petroleum solvents such as hexane in the extraction of fat and oils for food (edible oil) and non-food (bio fuel) applications. First a solvent selection as well as an evaluation of the performance was made with Hansen Solubility Parameters and the COnductor-like Screening MOdel for Realistic Solvation (COSMO-RS) simulations. Experiments were performed on rapeseed oil extraction at laboratory and pilot plant scale for the determination of lipid yields, extraction kinetics, diffusion modeling, and complete lipid composition in term of fatty acids and micronutrients (sterols, tocopherols and tocotrienols). Finally, economic and energetic evaluations of the process were conducted to estimate the cost of manufacturing using 2-methyltetrahydrofuran (MeTHF) as alternative solvent compared to hexane as petroleum solvent. PMID:25884332

Development of a rapid screening technique for organochlorine pesticides using solvent microextraction (SME) and fast gas chromatography (GC).

PubMed

de Jager, L S; Andrews, A R

2000-11-01

A novel, fast screening method for organochlorine pesticides (OCPs) in water samples has been developed. Total analysis time was less than 9 min, allowing 11 samples to be screened per hour. The relatively new technique of solvent microextraction (SME) was used to extract and preconcentrate the pesticides into a single drop of hexane. The use of a conventional carbon dioxide cryotrap was investigated for introduction of the extract onto a micro-bore (0.1 mm) capillary column for fast GC analysis. A pulsed-discharge electron capture detector was used which yielded selective and sensitive measurement of the pesticide peaks. Fast GC conditions were optimised and tested with the previously developed SME procedure. Calibration curves yielded good linearity and concentrations down to 0.25 ng mL-1 were detectable with RSD values ranging from 12.0 to 28% and LOD for most OCPs at 0.25 ng mL-1. Spiked river water samples were tested and using the developed screen we were able to differentiate between spiked samples and samples containing no OCPs.

Supercritical solvent coal extraction

NASA Technical Reports Server (NTRS)

Compton, L. E. (Inventor)

1984-01-01

Yields of soluble organic extract are increased up to about 50% by the supercritical extraction of particulate coal at a temperature below the polymerization temperature for coal extract fragments (450 C.) and a pressure from 500 psig to 5,000 psig by the conjoint use of a solvent mixture containing a low volatility, high critical temperature coal dissolution catalyst such as phenanthrene and a high volatility, low critical temperature solvent such as toluene.

Total milk fat extraction and quantification of polar and neutral lipids of cow, goat, and ewe milk by using a pressurized liquid system and chromatographic techniques.

PubMed

Castro-Gómez, M P; Rodriguez-Alcalá, L M; Calvo, M V; Romero, J; Mendiola, J A; Ibañez, E; Fontecha, J

2014-11-01

Although milk polar lipids such as phospholipids and sphingolipids located in the milk fat globule membrane constitute 0.1 to 1% of the total milk fat, those lipid fractions are gaining increasing interest because of their potential beneficial effects on human health and technological properties. In this context, the accurate quantification of the milk polar lipids is crucial for comparison of different milk species, products, or dairy treatments. Although the official International Organization for Standardization-International Dairy Federation method for milk lipid extraction gives satisfactory results for neutral lipids, it has important disadvantages in terms of polar lipid losses. Other methods using mixtures of solvents such as chloroform:methanol are highly efficient for extracting polar lipids but are also associated with low sample throughput, long time, and large solvent consumption. As an alternative, we have optimized the milk fat extraction yield by using a pressurized liquid extraction (PLE) method at different temperatures and times in comparison with those traditional lipid extraction procedures using 2:1 chloroform:methanol as a mixture of solvents. Comparison of classical extraction methods with the developed PLE procedure were carried out using raw whole milk from different species (cows, ewes, and goats) and considering fat yield, fatty acid methyl ester composition, triacylglyceride species, cholesterol content, and lipid class compositions, with special attention to polar lipids such as phospholipids and sphingolipids. The developed PLE procedure was validated for milk fat extraction and the results show that this method performs a complete or close to complete extraction of all lipid classes and in less time than the official and Folch methods. In conclusion, the PLE method optimized in this study could be an alternative to carry out milk fat extraction as a routine method. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Spiral computed tomography assessment of the efficacy of different rotary versus hand retreatment system.

PubMed

Mittal, Neelam; Jain, Jyoti

2014-01-01

The purpose of this study was to evaluate the efficacy of nickel-titanium rotary retreatment systems versus stainless steel hand retreatment system with or without solvent for gutta-percha removal during retreatment. Sixty extracted human mandibular molar teeth with single canal in a distal root was prepared with ProTaper rotary nickel-titanium files and obturated with gutta-percha and sealer. The teeth were randomly divided into six groups of 10 specimens in each groups. The volume of filling material before and after retreatment were evaluated in cm(3) using the computed tomography (CT) scanner proprietary software. Maximum amount of filling material removed during retreatment with ProTaper retreatment system with solvent and minimum with hand retreatment system with solvent. None of the technique was 100% effective in removing the filling materials, but the ProTaper retreatment system with solvent was better.

Ionic Liquids as Extraction Media for Metal Ions

NASA Astrophysics Data System (ADS)

Hirayama, Naoki

In solvent extraction separation of metal ions, recently, many researchers have investigated possible use of hydrophobic ionic liquids as extraction media instead of organic solvents. Ionic liquids are salts of liquid state around room temperature and can act not only as solvents but also as ion-exchangers. Therefore, the extraction mechanism of metal ions into ionic liquids is complicated. This review presents current overview and perspective on evaluation of nature of hydrophobic ionic liquids as extraction media for metal ions.

In vitro cytotoxicity of nonpolar constituents from different parts of kava plant (Piper methysticum).

PubMed

Jhoo, Jin-Woo; Freeman, James P; Heinze, Thomas M; Moody, Joanna D; Schnackenberg, Laura K; Beger, Richard D; Dragull, Klaus; Tang, Chung-Shih; Ang, Catharina Y W

2006-04-19

Kava (Piper methysticum), a perennial shrub native to the South Pacific islands, has been used to relieve anxiety. Recently, several cases of severe hepatotoxicity have been reported from the consumption of dietary supplements containing kava. It is unclear whether the kava constituents, kavalactones, are responsible for the associated hepatotoxicity. To investigate the key components responsible for the liver toxicity, bioassay-guided fractionation was carried out in this study. Kava roots, leaves, and stem peelings were extracted with methanol, and the resulting residues were subjected to partition with a different polarity of solvents (hexane, ethyl acetate, n-butanol, and water) for evaluation of their cytotoxicity on HepG2 cells based on the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay and lactate dehydrogenase and aspartate aminotransferase enzyme leakage assays. Organic solvent fractions displayed a much stronger cytotoxicity than water fractions for all parts of kava. The hexane fraction of the root exhibited stronger cytotoxic effects than fractions of root extracted with other solvents or extracts from the other parts of kava. Further investigations using bioassay-directed isolation and analysis of the hexane fraction indicated that the compound responsible for the cytotoxicity was flavokavain B. The identity of the compound was confirmed by (1)H and (13) C NMR and MS techniques.

Improved performance of mesoscopic perovskite solar cell using an accelerated crystalline formation method

NASA Astrophysics Data System (ADS)

Sidhik, Siraj; Esparza, Diego; Martínez-Benítez, Alejandro; López-Luke, Tzarara; Carriles, Ramón; De la Rosa, Elder

2017-10-01

Highly smooth organo-lead halide perovskite (OHP) films with less intra-granular defects are necessary to minimize the non-radiative carrier recombination in photovoltaic devices. Herein, a simple air-extraction anti-solvent deposition (AAD) technique is proposed to improve the quality of perovskite films. An air extraction process accompanied by anti-solvent washing helps to improve the morphology of perovskite, leading to smooth, homogeneous, compact, pin-hole free and densely packed films. Perovskite films with an average roughness of 5.01 nm, which is the smoothest morphology in mesoscopic-perovskite solar cell to the extent of our knowledge, high crystallinity, and a crystallite size in the range of ∼500 nm to 1 μm have been achieved. Average power conversion efficiency (PCE) of 16.99% for 15 cells and a best PCE of 17.70% with a high open circuit voltage of 1.075 and fill factor of 74.22% were achieved using the AAD approach without a glove box. The cells exhibit virtually no hysteresis. These efficiency values are approximately 37.68% higher than the cells fabricated using anti-solvent process without air-extraction, where an average efficiency of 12.34% was measured. This method demonstrates high reproducibility and can be employed for the large scale production of PSC at reduced cost.

Determination of amantadine in biological fluids using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection.

PubMed

Farajzadeh, Mir Ali; Nouri, Nina; Alizadeh Nabil, Ali Akbar

2013-12-01

A one-step derivatization and microextraction technique for the determination of amantadine in the human plasma and urine samples is presented. An appropriate mixture of methanol (disperser solvent), 1,2-dibromoethane (extraction solvent), and butylchloroformate (derivatization agent) is rapidly injected into samples. After centrifuging, the sedimented phase is analyzed by gas chromatography-flame ionization detection (GC-FID). The kind of extraction and disperser solvents and their volumes, amount of derivatization agent and reaction/extraction time which are effective in derivatization/dispersive liquid-liquid microextraction (DLLME) procedure are optimized. Under the optimal conditions, the enrichment factor (EF) of the target analyte was obtained to be 408 and 420, and limit of detection (LOD) 4.2 and 2.7ngmL(-1), in plasma and urine respectively. The linear range is 14-5000 and 8.7-5000ng/mL for plasma and urine, respectively (squared correlation coefficient≥0.990). The relative recoveries obtained for the spiked plasma and urine samples are between 72% and 93%. Moreover, the inter- and intra-day precisions are acceptable at all spiked concentrations (relative standard deviation <7%). Finally the method was successfully applied to determine amantadine in biological samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Optimization, validation and comparison of various extraction techniques for the trace determination of polycyclic aromatic hydrocarbons in sewage sludges by liquid chromatography coupled to diode-array and fluorescence detection.

PubMed

Miège, C; Dugay, J; Hennion, M C

2003-05-02

There is a need for a better characterization of sludges from wastewater treatment plants which are destined to be spread on agricultural lands. Inorganic pollutants are regularly controlled but organic pollutants have received few attention up to now. On this paper, we have been interested on the analysis of the 16 polycyclic aromatic hydrocarbons (PAHs) listed in the US Environmental Protection Agency (US EPA) priority list and more particularly of the six PAHs listed in the European community list (fluoranthene, benzo[b and k]fluoranthene, benzo[a]pyrene, benzo[ghi]perylene, indeno[1,2,3-cd]pyrene). The analysis step consists on liquid chromatography with both fluorescence and UV detections as described in the EPA Method 8310. As for the extraction step, several techniques such as supercritical fluid extraction, pressurized liquid extraction, focused microwave extraction in open vessels, Soxhlet and ultrasonic extractions are compared after optimization of the experimental conditions (solvent nature and quantity, temperature, pressure, duration, ... ) and validation with certified sludges. When optimized, these five extraction techniques are as much efficient with similar relative standard deviation. Whatever the extraction techniques used, the whole analysis protocol permits to quantify PAHs in the range of 0.09 to 0.9 mg/kg of dried sludges.

Analysis of biogenic carbonyl compounds in rainwater by stir bar sorptive extraction technique with chemical derivatization and gas chromatography‐mass spectrometry

PubMed Central

Lewis, Alastair C.; Shaw, Marvin D.

2016-01-01

Stir bar sorptive extraction is a powerful technique for the extraction and analysis of organic compounds in aqueous matrices. Carbonyl compounds are ubiquitous components in rainwater, however, it is a major challenge to accurately identify and sensitively quantify carbonyls from rainwater due to the complex matrix. A stir bar sorptive extraction technique was developed to efficiently extract carbonyls from aqueous samples following chemical derivatization by O‐(2,3,4,5,6‐pentafluorobenzyl) hydroxylamine hydrochloride. Several commercial stir bars in two sizes were used to simultaneously measure 29 carbonyls in aqueous samples with detection by gas chromatography with mass spectrometry. A 100 mL aqueous sample was extracted by stir bars and the analytes on stir bars were desorbed into a 2 mL solvent solution in an ultrasonic bath. The preconcentration Coefficient for different carbonyls varied between 30 and 45 times. The limits of detection of stir bar sorptive extraction with gas chromatography mass spectrometry for carbonyls (10–30 ng/L) were improved by ten times compared with other methods such as gas chromatography with electron capture detection and stir bar sorptive extraction with high‐performance liquid chromatography and mass spectrometry. The technique was used to determine carbonyls in rainwater samples collected in York, UK, and 20 carbonyl species were quantified including glyoxal, methylglyoxal, isobutenal, 2‐hydroxy ethanal. PMID:27928898

Effect of Piper betle L. and its extracts on the growth and aflatoxin production by Aspergillus parasiticus.

PubMed

Chou, C C; Yu, R C

1984-01-01

Ground powder of the leaf and fruit of Piper betle L., a tropical spice plant grown in Southeast Asia, was prepared and extracted by chloroform, ethanol and water with one solvent only or with 3 solvents in sequence. The betel powder and various extracts were added to YES broth to determine their effects on the growth and aflatoxin production by Aspergillus parasiticus. Results showed that betel leaf powder exhibited higher antimycotic activity than fruit. One half percent of ground leaf powder completely inhibited the growth and aflatoxin production by A. parasiticus. Among the solvent extracts, chloroform and ethanol extracts of betel leaf prepared from a single solvent extraction showed more antimycotic activity. The ethanol extract of betel leaf at the level of 450 micrograms/ml would eliminate A. parasiticus growth and aflatoxin production. The antimycotic activity of this ethanol extract was most pronounced at pH 4.

Comparative Analysis of Chemical Composition, Antioxidant Activity and Quantitative Characterization of Some Phenolic Compounds in Selected Herbs and Spices in Different Solvent Extraction Systems.

PubMed

Sepahpour, Shabnam; Selamat, Jinap; Abdul Manap, Mohd Yazid; Khatib, Alfi; Abdull Razis, Ahmad Faizal

2018-02-13

This study evaluated the efficacy of various organic solvents (80% acetone, 80% ethanol, 80% methanol) and distilled water for extracting antioxidant phenolic compounds from turmeric, curry leaf, torch ginger and lemon grass extracts. They were analyzed regarding the total phenol and flavonoid contents, antioxidant activity and concentration of some phenolic compounds. Antioxidant activity was determined by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging assay and the ferric reducing antioxidant power (FRAP) assay. Quantification of phenolic compounds was carried out using high-performance liquid chromatography (HPLC). All the extracts possessed antioxidant activity, however, the different solvents showed different efficiencies in the extraction of phenolic compounds. Turmeric showed the highest DPPH values (67.83-13.78%) and FRAP (84.9-2.3 mg quercetin/g freeze-dried crude extract), followed by curry leaf, torch ginger and lemon grass. While 80% acetone was shown to be the most efficient solvent for the extraction of total phenolic compounds from turmeric, torch ginger and lemon grass (221.68, 98.10 and 28.19 mg GA/g freeze dried crude extract, respectively), for the recovery of phenolic compounds from curry leaf (92.23 mg GA/g freeze-dried crude extract), 80% ethanol was the most appropriate solvent. Results of HPLC revealed that the amount of phenolic compounds varied depending on the types of solvents used.

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

Chunshan Song; Hatcher, P.G.; Saini, A.K.

It has been indicated by DOE COLIRN panel that low-temperature catalytic pretreatment is a promising approach to the development of an improved liquefaction process. This work is a fundamental study on effects of pretreatments on coal structure and reactivity in liquefaction. The main objectives of this project are to study the coal structural changes induced by low-temperature catalytic and thermal pretreatments by using spectroscopic techniques; and to clarify the pretreatment-induced changes in reactivity or convertibility of coals. As the second volume of the final report, here we summarize our work on spectroscopic characterization of four raw coals including two subbituminousmore » coals and two bituminous coals, tetrahydrofuran (THF)-extracted but unreacted coals, the coals (THF-insoluble parts) that have been thermally pretreated. in the absence of any solvents and in the presence of either a hydrogen-donor solvent or a non-donor solvent, and the coals (THF-insoluble parts) that have been catalytically pretreated in the presence of a dispersed Mo sulfide catalyst in the absence of any solvents and in the presence of either a hydrogen-donor solvent or a non-donor solvent.« less

Optimisation of Microwave-Assisted Extraction of Pomegranate (Punica granatum L.) Seed Oil and Evaluation 
of Its Physicochemical and Bioactive Properties

PubMed Central

Çavdar, Hasene Keskin; Gök, Uğur; Göğüş, Fahrettin

2017-01-01

Summary Pomegranate seed oil was extracted in a closed-vessel high-pressure microwave system. The characteristics of the obtained oil, such as fatty acid composition, free fatty acidity, total phenolic content, antioxidant activity and colour, were compared to those of the oil obtained by cold solvent extraction. Response surface methodology was applied to optimise extraction conditions: power (176–300 W), time (5–20 min), particle size (d=0.125–0.800 mm) and solvent to sample ratio (2:1, 6:1 and 10:1, by mass). The predicted highest extraction yield (35.19%) was obtained using microwave power of 220 W, particle size in the range of d=0.125–0.450 mm and solvent-to-sample ratio of 10:1 (by mass) in 5 min extraction time. Microwave-assisted solvent extraction (MASE) resulted in higher extraction yield than that of Soxhlet (34.70% in 8 h) or cold (17.50% in 8 h) extraction. The dominant fatty acid of pomegranate seed oil was punicic acid (86%) irrespective of the extraction method. Oil obtained by MASE had better physicochemical properties, total phenolic content and antioxidant activity than the oil obtained by cold solvent extraction. PMID:28559737

Cesium and strontium extraction using a mixed extractant solvent including crown ether and calixarene extractants

DOEpatents

Meikrantz, David H.; Todd, Terry A.; Riddle, Catherine L.; Law, Jack D.; Peterman, Dean R.; Mincher, Bruce J.; McGrath, Christopher A.; Baker, John D.

2007-11-06

A mixed extractant solvent including calix[4]arene-bis-(tert-octylbenzo)-crown-6 ("BOBCalixC6"), 4',4',(5')-di-(t-butyldicyclo-hexano)-18-crown-6 ("DtBu18C6"), and at least one modifier dissolved in a diluent. The mixed extractant solvent may be used to remove cesium and strontium from an acidic solution. The DtBu18C6 may be present from approximately 0.01 M to approximately 0.4M, such as from approximately 0.086 M to approximately 0.108 M. The modifier may be 1-(2,2,3,3-tetrafluoropropoxy)-3-(4-sec-butylphenoxy)-2-propanol ("Cs-7SB") and may be present from approximately 0.01M to approximately 0.8M. In one embodiment, the mixed extractant solvent includes approximately 0.15M DtBu18C6, approximately 0.007M BOBCalixC6, and approximately 0.75M Cs-7SB modifier dissolved in an isoparaffinic hydrocarbon diluent. The mixed extractant solvent may form an organic phase in an extraction system that also includes an aqueous phase. Methods of extracting cesium and strontium as well as strontium alone are also disclosed.

Effect of various solvent on the specific amino acids of black soybean (Glycine soja) sprout

NASA Astrophysics Data System (ADS)

Kanetro, B.; Slamet, A.; Wazyka, A.

2018-01-01

The objective of this research was to study the effect of various solvent extractions on the specific amino acids as small peptide or free amino acids that was contained in the extract after removal of the macromolecule protein of black soybean sprouts. The experimental design of this research was randomized complete design with one factor, which was the three various solvent, i.e. hexane, ethanol and water. The black soybean seed was germinated for 36 h. The small peptide and free amino acids of black soybean sprout were isolated at 3 various of solvents extraction, and then the macromolecule proteins in the extracts were precipitated at the pH 4. The extracts of black soybean sprout after removal of the macromolecule protein were analysed by HPLC to determine the profile of amino acids for stimulation of insulin secretion. The result of this research showed that the extracts contained the small peptide and free amino acid for stimulation of insulin secretion. The best solvent extraction was water that was due to the content of Leu, Arg, Ala, Phe, Ile, and Lys of water extract was higher than hexane and ethanol extracts.

Extraction of phenolic compounds from extra virgin olive oil by a natural deep eutectic solvent: Data on UV absorption of the extracts.

PubMed

Paradiso, Vito Michele; Clemente, Antonia; Summo, Carmine; Pasqualone, Antonella; Caponio, Francesco

2016-09-01

This data article refers to the paper "Towards green analysis of virgin olive oil phenolic compounds: extraction by a natural deep eutectic solvent and direct spectrophotometric detection" [1]. A deep eutectic solvent (DES) based on lactic acid and glucose was used as green solvent for phenolic compounds. Eight standard phenolic compounds were solubilized in the DES. Then, a set of extra virgin olive oil (EVOO) samples (n=65) were submitted to liquid-liquid extraction by the DES. The standard solutions and the extracts were analyzed by UV spectrophotometry. This article reports the spectral data of both the standard solutions and the 65 extracts, as well as the total phenolic content of the corresponding oils, assessed by the Folin-Ciocalteu assay.

Infusion Extractor

NASA Technical Reports Server (NTRS)

Chang-Diaz, Franklin R.

1988-01-01

Apparatus and method of removing desirable constituents from an infusible material by infusion extraction, where a piston operating in a first chamber draws a solvent into the first chamber where it may be heated, and then moves the heated solvent into a second chamber containing the infusible material, and where infusion extraction takes place. The piston then moves the solvent containing the extract through a filter into the first chamber, leaving the extraction residue in the second chamber.

An interesting two-phase solvent system and its use in preparative isolation of aconitines from aconite roots by counter-current chromatography.

PubMed

Han, Quan-Bin; Tang, Wai-Lun; Dong, Cai-Xia; Xu, Hong-Xi; Jiang, Zhi-Hong

2013-04-01

Two-phase solvent system plays crucial role in successful separation of organic compounds using counter-current chromatography (CCC). An interesting two-phase solvent system, composed of chloroform/ethyl acetate/methanol/water, is reported here, in which both phases contain sufficient organic solvents to balance their dissolving capacities. Adjusting the solvent system to get satisfactory partition coefficients (K values) for target compounds becomes relatively simple. This solvent system succeeded in sample preparation of aconitine (8.07 mg, 93.69%), hypaconitine (7.74 mg, 93.17%), mesaconitine (1.95 mg, 94.52%) from raw aconite roots (102.24 mg, crude extract), benzoylmesaconine (34.79 mg, 98.67%) from processed aconite roots (400.01 mg, crude extract), and yunaconitine (253.59 mg, 98.65%) from a crude extract of Aconitum forrestii (326.69 mg, crude extract). © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of microwave-assisted extraction of analgesic and anti-inflammatory drugs from human plasma and urine using response surface experimental designs.

PubMed

Fernández, Purificación; Fernández, Ana M; Bermejo, Ana M; Lorenzo, Rosa A; Carro, Antonia M

2013-04-01

The performance of microwave-assisted extraction and HPLC with photodiode array detection method for determination of six analgesic and anti-inflammatory drugs from plasma and urine, is described, optimized, and validated. Several parameters affecting the extraction technique were optimized using experimental designs. A four-factor (temperature, phosphate buffer pH 4.0 volume, extraction solvent volume, and time) hybrid experimental design was used for extraction optimization in plasma, and three-factor (temperature, extraction solvent volume, and time) Doehlert design was chosen to extraction optimization in urine. The use of desirability functions revealed the optimal extraction conditions as follows: 67°C, 4 mL phosphate buffer pH 4.0, 12 mL of ethyl acetate and 9 min, for plasma and the same volume of buffer and ethyl acetate, 115°C and 4 min for urine. Limits of detection ranged from 4 to 45 ng/mL in plasma and from 8 to 85 ng/mL in urine. The reproducibility evaluated at two concentration levels was less than 6.5% for both specimens. The recoveries were from 89 to 99% for plasma and from 83 to 99% for urine. The proposed method was successfully applied in plasma and urine samples obtained from analgesic users. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrasound assisted dialysis of semi-permeable membrane devices for the simultaneous analysis of a wide number of persistent organic pollutants.

PubMed

Bustamante, Julen; Navarro, Patricia; Arana, Gorka; de Diego, Alberto; Madariaga, Juan Manuel

2013-09-30

A new procedure based on ultrasound assisted dialysis (UAD) for the simultaneous and quantitative extraction of a wide number of persistent organic pollutants (POPs) such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) or some other organochlorinated pesticides (OCPs) contained in semi-permeable membrane devices (SPMDs) has been developed. This extraction technique combines the advantages of the organic solvent dialysis (OSD) and the speed of the ultrasound assisted extraction. The extraction was performed in an ultrasound bath for 32 min placing the SPMD in a glass flask covered with 80 mL of hexane. This set-up is able to extract simultaneously up to 8 samples. The proposed method entails good repeatabilities (RSD 2-13%) and recoveries (around 100% for almost every analyte). Limits of detection were at ng SPMD(-1) level and enough for the determination of the target analytes in a slightly polluted aquatic environment, as it was tested by successfully comparing the OSD to the proposed methodology. Therefore, the results obtained show that the UAD can be a good alternative for the extraction of POPs in SPMDs as it requires short extraction times and solvent volumes, and provides a cleaner extract for the subsequent clean-up step. Moreover, it fits better than the OSD to the general requirements of Green Chemistry. Copyright © 2013 Elsevier B.V. All rights reserved.

Optimization of flavanones extraction by modulating differential solvent densities and centrifuge temperatures.

PubMed

Chebrolu, Kranthi K; Jayaprakasha, G K; Jifon, J; Patil, Bhimanagouda S

2011-07-15

Understanding the factors influencing flavonone extraction is critical for the knowledge in sample preparation. The present study was focused on the extraction parameters such as solvent, heat, centrifugal speed, centrifuge temperature, sample to solvent ratio, extraction cycles, sonication time, microwave time and their interactions on sample preparation. Flavanones were analyzed in a high performance liquid chromatography (HPLC) and later identified by liquid chromatography and mass spectrometry (LC-MS). The five flavanones were eluted by a binary mobile phase with 0.03% phosphoric acid and acetonitrile in 20 min and detected at 280 nm, and later identified by mass spectral analysis. Dimethylsulfoxide (DMSO) and dimethyl formamide (DMF) had optimum extraction levels of narirutin, naringin, neohesperidin, didymin and poncirin compared to methanol (MeOH), ethanol (EtOH) and acetonitrile (ACN). Centrifuge temperature had a significant effect on flavanone distribution in the extracts. The DMSO and DMF extracts had homogeneous distribution of flavanones compared to MeOH, EtOH and ACN after centrifugation. Furthermore, ACN showed clear phase separation due to differential densities in the extracts after centrifugation. The number of extraction cycles significantly increased the flavanone levels during extraction. Modulating the sample to solvent ratio increased naringin quantity in the extracts. Current research provides critical information on the role of centrifuge temperature, extraction solvent and their interactions on flavanone distribution in extracts. Published by Elsevier B.V.

Fabric phase sorptive extraction: Two practical sample pretreatment techniques for brominated flame retardants in water.

PubMed

Huang, Guiqi; Dong, Sheying; Zhang, Mengfei; Zhang, Haihan; Huang, Tinglin

2016-09-15

Sample pretreatment is the critical section for residue monitoring of hazardous pollutants. In this paper, using the cellulose fabric as host matrix, three extraction sorbents such as poly (tetrahydrofuran) (PTHF), poly (ethylene glycol) (PEG) and poly (dimethyldiphenylsiloxane) (PDMDPS), were prepared on the surface of the cellulose fabric. Two practical extraction techniques including stir bar fabric phase sorptive extraction (stir bar-FPSE) and magnetic stir fabric phase sorptive extraction (magnetic stir-FPSE) have been designed, which allow stirring of fabric phase sorbent during the whole extraction process. In the meantime, three brominated flame retardants (BFRs) [tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bisallylether (TBBPA-BAE), tetrabromobisphenol A bis(2,3-dibromopropyl)ether (TBBPA-BDBPE)] in the water sample were selected as model analytes for the practical evaluation of the proposed two techniques using high-performance liquid chromatography (HPLC). Moreover, various experimental conditions affecting extraction process such as the type of fabric phase, extraction time, the amount of salt and elution conditions were also investigated. Due to the large sorbent loading capacity and unique stirring performance, both techniques possessed high extraction capability and fast extraction equilibrium. Under the optimized conditions, high recoveries (90-99%) and low limits of detection (LODs) (0.01-0.05 μg L(-1)) were achieved. In addition, the reproducibility was obtained by evaluating the intraday and interday precisions with relative standard deviations (RSDs) less than 5.1% and 6.8%, respectively. The results indicated that two pretreatment techniques were promising and practical for monitoring of hazardous pollutants in the water sample. Due to low solvent consumption and high repeated use performance, proposed techniques also could meet green analytical criteria. Copyright © 2016 Elsevier Ltd. All rights reserved.

Critical assessment of various techniques for the extraction of carotenoids and co-enzyme Q10 from the Thraustochytrid strain ONC-T18.

PubMed

Armenta, Roberto E; Burja, Adam; Radianingtyas, Helia; Barrow, Colin J

2006-12-27

A variety of techniques for extracting carotenoids from the marine Thraustochytrium sp. ONC-T18 was compared. Specifically, the organic solvents acetone, ethyl acetate, and petroleum ether were tested, along with direct and indirect ultrasonic assisted extraction (probe vs bath) methods. Techniques that used petroleum ether/acetone/water (15:75:10, v/v/v) with 3 h of agitation, or 5 min in an ultrasonic bath, produced the highest extraction yields of total carotenoids (29-30.5 microg g-1). Concentrations up to 11.5 microg g-1 of canthaxanthin and 17.5 microg g-1 of beta;-carotene were detected in extracts stored for 6 weeks. Astaxanthin and echinenone were also detected as minor compounds. Extracts with and without antioxidants showed similar carotenoid concentration profiles. However, total carotenoid concentrations were approximately 8% higher when antioxidants were used. Finally, an easy-to-perform and inexpensive method to detect co-enzymes in ONC-T18 was also developed using silica gel TLC plates. Five percent methanol in toluene as a mobile phase consistently eluted co-enzyme Q10 standards and could separate the co-enzyme fractions present in ONC-T18.

Enhancing Phenolic Contents and Antioxidant Potentials of Antidesma thwaitesianum by Supercritical Carbon Dioxide Extraction

PubMed Central

Poontawee, Warut; Natakankitkul, Surapol; Wongmekiat, Orawan

2015-01-01

Supercritical fluid extraction (SFE) has increasingly gained attention as an alternative technique for extraction of natural products without leaving toxic residues in extracts. Antidesma thwaitesianum Muell. Arg. (Phyllanthaceae), or ma mao, has been reported to exhibit antioxidant health benefits due to its phenolic constituents. To determine whether SFE technique could impact on phenolic contents and associated antioxidant potentials, ripe fruits of Antidesma thwaitesianum (Phyllanthaceae) were extracted using supercritical carbon dioxide (SC-CO2) and conventional solvents (ethanol, water). The results showed that the SC-CO2 extract contained significantly higher yield, total phenolic, flavonoid, and proanthocyanidin contents than those obtained from ethanol and water. It also demonstrated the greatest antioxidant activities as assessed by ABTS radical cation decolorization, DPPH radical scavenging, and ferric reducing antioxidant power (FRAP) assays. Further analysis using high-performance liquid chromatography with diode array and mass spectrometry detectors (HPLC-DAD/MSD) revealed the presence of catechin as a major phenolic compound of Antidesma thwaitesianum (Phyllanthaceae), with the maximum amount detected in the SC-CO2 extract. These data indicate that SFE technology improves both quantity and quality of Antidesma thwaitesianum fruit extract. The findings added more reliability of using this technique to produce high added value products from this medicinal plant. PMID:25977832

Solvent-assisted dispersive micro-SPE by using aminopropyl-functionalized magnetite nanoparticle followed by GC-PID for quantification of parabens in aqueous matrices.

PubMed

Abbasghorbani, Maryam; Attaran, Abdolmohammad; Payehghadr, Mahmood

2013-01-01

In this research, solvent-assisted dispersive micro-SPE was introduced as a simple modified technique for the determination of parabens in water and cosmetic samples. Aminopropyl-functionalized magnetite nanoparticles (MNPs) were successfully synthesized and applied. GC with photoionization detector was used for the separation and detection of parabens. In this method, hexylacetate (15 μL) as a solvent and aminopropyl-functionalized MNPs (5 μg) as a sorbent were added to an aqueous sample (10 mL) and then the sample was sonicated. Dispersed magnetite was collected in the bottom of the conical tube by using a strong magnet and then ACN was added as a desorption solvent. Forty microliters of this solvent was transferred into a microvial and then acetic anhydride and pyridine were added, thus derivatization was performed by acetic anhydride. After evaporation, 1 μL of derivatized sample was injected into a gas chromatograph for analysis. Several important parameters, such as kind of organic solvent, desorption solvent and volume, amount of aminopropyl-functionalized MNPs and effect of salt addition were investigated. Under optimum conditions, the limits of detection achieved were between 50 and 300 ng/L, with RSDs (n = 5) lower than 8%. Under the optimum conditions, the enrichment factors ranged from 217 to 1253 and the extraction recoveries ranged from 10 to 62%. The recoveries were obtained for the analytes in river water and mouthwash solution and hand cream in the range of 87-103%. The advantages of proposed method are simplicity of operation, rapidity, high extraction yields, and environmental friendly character. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Process for enhancing the value of hydrocabonaceous natural recources

DOEpatents

Bunger, James W.; Cogswell, Donald E.

2005-04-05

A process for upgrading hydrocarbonaceous oil containing heteroatom-containing compounds where the hydrocarbonaceous oil is contacted with a solvent system that is a mixture of a major portion of a polar solvent having a dipole moment greater than about 1 debye and a minor portion of water to selectively separate the constituents of the carbonaceous oil into a heteroatom-depleted raffinate fraction and heteroatom-enriched extract fraction. The polar solvent and the water-in-solvent system are formulated at a ratio where the water is an antisolvent in an amount to inhibit solubility of heteroatom-containing compounds and the polar solvent in the raffinate, and to inhibit solubility of non-heteroatom-containing compounds in the extract. The ratio of the hydrocarbonaceous oil to the solvent system is such that a coefficient of separation is at least 50%. The coefficient of separation is the mole percent of heteroatom-containing compounds from the carbonaceous oil that are recovered in the extract fraction minus the mole percent of non-heteroatom-containing compounds from the carbonaceous oil that are recovered in the extract fraction. The solvent-free extract and the raffinate concentrates may be used directly or processed to make valuable petroleum, chemical or industrial products.

Optimisation of the recovery of carotenoids from tomato processing wastes: application on textile dyeing and assessment of its antioxidant activity.

PubMed

Baaka, Noureddine; El Ksibi, Imen; Mhenni, Mohamed Farouk

2017-01-01

The present study has been focused on the extraction of natural pigments from tomato industry waste. At first, different solvents and solvents mixture were compared to determine which one is the best for extracting carotenoids compounds from tomato by-products. A mixture of hexane and acetone gave the highest carotenoids extraction yield among the others examined. The extraction conditions were optimised using a five-level-five-factor central composite design. Under optimal conditions, solvent solid ratio 90, hexane percentage in the solvent mixture 60, extraction duration 50, number of extractions 4 and extraction temperature 35 °C, the yield of carotenoids was 80.7 μg/g. The coloured extract of tomato by-products was applied on textile fabrics to investigate the dyeing characteristics and antioxidant activities. The results indicate that extract can be applied on textile fabrics (wool, silk and polyamide) to produce coloured clothing with acceptable antioxidant properties.

MICROWAVE-ASSISTED EXTRACTION OF PHENOLIC COMPOUNDS FROM POLYGONUM MULTIFLORUM THUNB. ROOTS.

PubMed

Quoc, Le Pham Tan; Muoi, Nguyen Van

2016-01-01

The aim of this study was to determine the best extraction conditions for total phenolic content (TPC) and antioxidant capacity (AC) of Polygonum multiflorum Thunb. root using microwave-assisted extraction (MAE). The raw material used was Polygonum multiflorum Thunb. root powder. Five factors such as solvent type, solvent concentrations, solvent/material ratio, extraction time and microwave power were studied; TPC and AC values were determined by the Folin-Ciocalteu method and DPPH free radical scavenging activity measurement, respectively. In addition, studies involved assaying the HPLC test of extracts and SEM of samples. Optimal results pointed to acetone as the solvent, acetone concentration of 60%, solvent/material ratio of 40/1 (v/w), extraction time of 5 mins and microwave power of 127 W. TPC and AC obtained were approximates 44.3 ±0.13 mg GAE/g DW and 341.26 ±1.54 μmol TE/g DW, respectively. The effect of microwaving on the cell destruction of Polygonum multiflorum Thunb. root was observed by scanning electron microscopy (SEM). Some phenolic compounds were determined by the HPLC method, for instance, gallic acid, catechin and resveratrol. These factors significantly affected TPC and AC. We can use acetone as a solvent with microwave-assisted extraction to achieve the best result.

Ultrasonically assisted extraction of total phenols and flavonoids from Rhodiola rosea.

PubMed

Staneva, Jordanka; Todorova, Milka; Neykov, Neyko; Evstatieva, Ljuba

2009-07-01

This work deals with ultrasonically assisted extraction (UAE) of biologically active compounds from rhizomes of Rhodiola rosea, a popular medicinal plant. The influence of temperature, type of solvent and solid/solvent ratio on the yield of total extracts, total phenols and flavonoids was established. The best extraction of total phenols and flavonoids was achieved by using 50% aqueous EtOH and MeOH, respectively. Five times increase of solid/solvent ratio (from 1:20 to 1:100 (w/v)) leads to slow increase of the yield of total phenols and flavonoids. The extraction effectiveness of conventional maceration with 50% EtOH and UAE performed for 1 h at 25 degrees C using the same solvent with respect of total phenols was comparable.

Green ultrasound-assisted extraction of carotenoids based on the bio-refinery concept using sunflower oil as an alternative solvent.

PubMed

Li, Ying; Fabiano-Tixier, Anne Sylvie; Tomao, Valérie; Cravotto, Giancarlo; Chemat, Farid

2013-01-01

A green, inexpensive and easy-to-use method for carotenoids extraction from fresh carrots assisted by ultrasound was designed in this work. Sunflower oil was applied as a substitute to organic solvents in this green ultrasound-assisted extraction (UAE): a process which is in line with green extraction and bio-refinery concepts. The processing procedure of this original UAE was first compared with conventional solvent extraction (CSE) using hexane as solvent. Moreover, the UAE optimal conditions for the subsequent comparison were optimized using response surface methodology (RSM) and ultra performance liquid chromatography--diode array detector--mass spectroscopy (UPLC-DAD-MS). The results showed that the UAE using sunflower as solvent has obtained its highest β-carotene yield (334.75 mg/l) in 20 min only, while CSE using hexane as solvent obtained a similar yield (321.35 mg/l) in 60 min. The green UAE performed under optimal extraction conditions (carrot to oil ratio of 2:10, ultrasonic intensity of 22.5 W cm(-2), temperature of 40 °C and sonication time of 20 min) gave the best yield of β-carotene. Copyright © 2012 Elsevier B.V. All rights reserved.

High-throughput screening for new psychoactive substances (NPS) in whole blood by DLLME extraction and UHPLC-MS/MS analysis.

PubMed

Odoardi, Sara; Fisichella, Marco; Romolo, Francesco Saverio; Strano-Rossi, Sabina

2015-09-01

The increasing number of new psychoactive substances (NPS) present in the illicit market render their identification in biological fluids/tissues of great concern for clinical and forensic toxicology. Analytical methods able to detect the huge number of substances that can be used are sought, considering also that many NPS are not detected by the standard immunoassays generally used for routine drug screening. The aim of this work was to develop a method for the screening of different classes of NPS (a total of 78 analytes including cathinones, synthetic cannabinoids, phenethylamines, piperazines, ketamine and analogues, benzofurans, tryptamines) from blood samples. The simultaneous extraction of analytes was performed by Dispersive Liquid/Liquid Microextraction DLLME, a very rapid, cheap and efficient extraction technique that employs microliters amounts of organic solvents. Analyses were performed by a target Ultrahigh Performance Liquid Chromatography tandem Mass Spectrometry (UHPLC-MS/MS) method in multiple reaction monitoring (MRM). The method allowed the detection of the studied analytes with limits of detection (LODs) ranging from 0.2 to 2ng/mL. The proposed DLLME method can be used as an alternative to classical liquid/liquid or solid-phase extraction techniques due to its rapidity, necessity to use only microliters amounts of organic solvents, cheapness, and to its ability to extract simultaneously a huge number of analytes also from different chemical classes. The method was then applied to 60 authentic real samples from forensic cases, demonstrating its suitability for the screening of a wide number of NPS. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of polycyclic aromatic hydrocarbons in water and beverages using membrane-assisted solvent extraction in combination with large volume injection-gas chromatography-mass spectrometric detection.

PubMed

Rodil, Rosario; Schellin, Manuela; Popp, Peter

2007-09-07

Membrane-assisted solvent extraction (MASE) in combination with large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) was applied for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. The MASE conditions were optimized for achieving high enrichment of the analytes from aqueous samples, in terms of extraction conditions (shaking speed, extraction temperature and time), extraction solvent and composition (ionic strength, sample pH and presence of organic solvent). Parameters like linearity and reproducibility of the procedure were determined. The extraction efficiency was above 65% for all the analytes and the relative standard deviation (RSD) for five consecutive extractions ranged from 6 to 18%. At optimized conditions detection limits at the ng/L level were achieved. The effectiveness of the method was tested by analyzing real samples, such as river water, apple juice, red wine and milk.

Reactive extraction at liquid-liquid systems

NASA Astrophysics Data System (ADS)

Wieszczycka, Karolina

2018-01-01

The chapter summarizes the state of knowledge about a metal transport in two-phase system. The first part of this review focuses on the distribution law and main factors determination in classical solvent extraction (solubility and polarity of the solute, as well as inter- and intramolecules interaction. Next part of the chapter is devoted to the reactive solvent extraction and the molecular modeling requiring knowledge on type of extractants, complexation mechanisms, metals ions speciation and oxidation during complexes forming, and other parameters that enable to understand the extraction process. Also the kinetic data that is needed for proper modeling, simulation and design of processes needed for critical separations are discussed. Extraction at liquid-solid system using solvent impregnated resins is partially identical as in the case of the corresponding solvent extraction, therefore this subject was also presented in all aspects of separation process (equilibrium, mechanism, kinetics).

Phytochemical and antimicrobial activities of Himalayan Cordyceps sinensis (Berk.) Sacc.

PubMed

Mamta; Mehrotra, Shubhi; Amitabh; Kirar, Vandana; Vats, Praveen; Nandi, Shoma Paul; Negi, P S; Misra, Kshipra

2015-01-01

This study evaluated the phytochemical and antimicrobial activities and also quantified bioactive nucleoside using high performance thin layer chromatography (HPTLC) of five extracts of Indian Himalayan Cordyceps sinensis prepared with different solvents employing accelerated solvent extraction (ASE) technique. The phytochemical potential of these extracts was quantified in terms of total phenolic and total flavonoid content while antioxidant activities were determined by 1,1-diphenyl-2-pycryl-hydrazyl (DPPH) and 2,2 -azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) and ferric-reducing antioxidant power (FRAP) assays. Total reducing power (TRP) was determined by converting iron (III) into iron (II) reduction assay. CS(50%Alc) (15.1 ± 0.67mg/g of dry extract) and CS(100%Alc) (19.3 ± 0.33 mg/g of dry extract) showed highest phenolic and flavonoid content, respectively while CS(Aq) extract showed maximum antioxidant activity and the highest concentration of the three nucleosides (adenine 12.8 ± 0.49 mg/g, adenosine 0.36 ± 0.28 mg/g and uracil 0.14 ± 0.36 mg/g of dry extract) determined by HPTLC. The evaluation of extracts for antimicrobial activity against gram-negative and gram-positive bacterial strains showed CS(25%Alc), CS(75%Alc) and CS(100%Alc) extract to be more effective against E. coli, P. aerugenosa and B. subtilis giving 9, 7 and 6.5 mm of zone of inhibition (ZOI) in 93.75, 93.75 and 45 μg concentration, respectively, whereas CS(Aq) extract showed minimal inhibition against these.

A survey of extraction solvents in the forensic analysis of textile dyes.

PubMed

Groves, Ethan; Palenik, Christopher S; Palenik, Skip

2016-11-01

The characterization and identification of dyes in fibers can be used to provide investigative leads and strengthen associations between known and questioned items of evidence. The isolation of a dye from its matrix (e.g., a textile fiber) permits detailed characterization, comparison and, in some cases, identification using methods such as thin layer chromatography in conjunction with infrared and Raman spectroscopy. A survey of dye extraction publications reveals that pyridine:water (4:3) is among the most commonly cited extraction solvent across a range of fiber and dye chemistries. Here, the efficacy of this solvent system has been evaluated for the extraction of dyes from 172 commercially prevalent North American textile dyes. The evaluated population represents seven dye application classes, 18 chemical classes, and spans nine types of commercial textile fibers. The results of this survey indicate that ∼82% of the dyestuffs studied are extractable using this solvent system. The results presented here summarize the extraction efficacy by class and fiber type and illustrate that this solvent system is applicable to a wider variety of classes and fibers than previously indicated in the literature. While there is no universal solvent for fiber extraction, these results demonstrate that pyridine:water represents an excellent first step for extracting unknown dyes from questioned fibers in forensic casework. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Effect of the type and level of hydration of alcoholic solvents on the simultaneous extraction of oil and chlorogenic acids from sunflower seed press cake.

PubMed

Scharlack, Nayara K; Aracava, Keila K; Rodrigues, Christianne Ec

2017-10-01

The present study aimed to evaluate the replacement of hexane by alcoholic solvents in oil extraction from sunflower seed press cake. The use of ethanol and isopropanol has important advantages, including low toxicity and good operational safety. Thus, in the present study, solid-liquid extractions were performed in a single stage from 60 to 90 °C and in consecutive extractions in three stages at 90 °C. Solvent hydration negatively affected the extraction of oil but favored the extraction of chlorogenic acids (CAs), especially when ethanol was used. Regarding oxidative stability, the oils extracted using ethanol presented long induction times, which could be related to the high levels of not only CAs and tocopherols, but also phospholipids. Alcoholic solvents can be used for extraction to produce sunflower seed oil containing minor compounds that give it greater oxidative stability. In addition, the results obtained using hydrous ethanol showed that this solvent can yield defatted sunflower seed meal with a low content of CAs, enabling future use of the protein fraction. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Optimization of an accelerated solvent extraction dispersive liquid-liquid microextraction method for the separation and determination of essential oil from Ligusticum chuanxiong Hort by gas chromatography with mass spectrometry.

PubMed

Yang, Guang; Sun, Qiushi; Hu, Zhiyan; Liu, Hua; Zhou, Tingting; Fan, Guorong

2015-10-01

In this study, an accelerated solvent extraction dispersive liquid-liquid microextraction coupled with gas chromatography and mass spectrometry was established and employed for the extraction, concentration and analysis of essential oil constituents from Ligusticum chuanxiong Hort. Response surface methodology was performed to optimize the key parameters in accelerated solvent extraction on the extraction efficiency, and key parameters in dispersive liquid-liquid microextraction were discussed as well. Two representative constituents in Ligusticum chuanxiong Hort, (Z)-ligustilide and n-butylphthalide, were quantitatively analyzed. It was shown that the qualitative result of the accelerated solvent extraction dispersive liquid-liquid microextraction approach was in good agreement with that of hydro-distillation, whereas the proposed approach took far less extraction time (30 min), consumed less plant material (usually <1 g, 0.01 g for this study) and solvent (<20 mL) than the conventional system. To sum up, the proposed method could be recommended as a new approach in the extraction and analysis of essential oil. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reducing Time and Increasing Sensitivity in Sample Preparation for Adherent Mammalian Cell Metabolomics

PubMed Central

Lorenz, Matthew A.; Burant, Charles F.; Kennedy, Robert T.

2011-01-01

A simple, fast, and reproducible sample preparation procedure was developed for relative quantification of metabolites in adherent mammalian cells using the clonal β-cell line INS-1 as a model sample. The method was developed by evaluating the effect of different sample preparation procedures on high performance liquid chromatography- mass spectrometry quantification of 27 metabolites involved in glycolysis and the tricarboxylic acid cycle on a directed basis as well as for all detectable chromatographic features on an undirected basis. We demonstrate that a rapid water rinse step prior to quenching of metabolism reduces components that suppress electrospray ionization thereby increasing signal for 26 of 27 targeted metabolites and increasing total number of detected features from 237 to 452 with no detectable change of metabolite content. A novel quenching technique is employed which involves addition of liquid nitrogen directly to the culture dish and allows for samples to be stored at −80 °C for at least 7 d before extraction. Separation of quenching and extraction steps provides the benefit of increased experimental convenience and sample stability while maintaining metabolite content similar to techniques that employ simultaneous quenching and extraction with cold organic solvent. The extraction solvent 9:1 methanol: chloroform was found to provide superior performance over acetonitrile, ethanol, and methanol with respect to metabolite recovery and extract stability. Maximal recovery was achieved using a single rapid (~1 min) extraction step. The utility of this rapid preparation method (~5 min) was demonstrated through precise metabolite measurements (11% average relative standard deviation without internal standards) associated with step changes in glucose concentration that evoke insulin secretion in the clonal β-cell line INS-1. PMID:21456517

In vitro Antioxidant Potentials of Cyperus rotundus L. Rhizome Extracts and Their Phytochemical Analysis.

PubMed

Kamala, Arunagiri; Middha, Sushil Kumar; Gopinath, Chitra; Sindhura, H S; Karigar, Chandrakant S

2018-01-01

Cyperus rotundus L. (family Cyperaceae), native to India, is a multivalent medicinal plant widely used in conventional medicine. The research reports on bioactive components from C. rotundus L. are scanty. The objective of the study was to optimize the best solvent system and bioprospect the possible phytochemicals in C. rotundus L. rhizome (CRR). The phytochemicals were extracted from the rhizomes of C. rotundus L. by successive Soxhlet technique with solvents of increasing polarity. The resultant extracts were analyzed for their total flavonoid content (TFC), total phenolic content (TPC), total proanthocyanidin content (TPAC), in vitro antioxidant potential, and inhibition of lipid peroxidation. The 70% acetone extract of CRR was analyzed using gas chromatography-mass spectrometry (GC-MS) for probable phytochemicals. The TPC, TFC, and TPAC estimates ranged from 0.036 ± 0.002 to 118.924 ± 5.946 μg/mg extract, 7.196 ± 0.359 to 200.654 ± 10.032 μg/mg extract, and 13.115 ± 0.656 to 45.901 ± 2.295 μg/mg extract, respectively. The quantities of TPC, TFC, and TPAC were found to be the highest in 70% acetone extract. The 70% acetone and 70% methanol extracts revealed best radical scavenging effect. GC-MS analysis of CRR extract revealed the presence of a novel compound 1 (2)-acetyl-3 (5)-styryl-5 (3)-methylthiopyrazole. The study indicated that 70% acetone and 70% methanol extracts of CRRs can be a potential source of antioxidants. The studies suggest 70% methanol and acetone as the suitable solvents for the extraction of phytochemicalsNovel compound 1(2)-Acetyl-3(5)-styryl-5(3)-methylthiopyrazole was detected in 70% acetone extract. Abbreviations used: ACRE: Acetone C. rotundus L. rhizome extract; AlCl 3 : Aluminum chloride; AQRE: Aqueous C. rotundus L. rhizome extract; CE: Catechin Equivalent; CHRE: Chloroform C. rotundus L. rhizome extract; CRR: C. rotundus L. rhizome; DPPH: 2,2 diphenyl-1-picrylhydrazyl; ETRE: Ethanolic C. rotundus L. rhizome extract; EARE: Ethyl acetate C. rotundus L. rhizome extract; FRP: Ferric reducing power; GAE: Gallic acid equivalent; GC-MS: Gas chromatography-mass spectrometry; HERE: Hexane C. rotundus L. rhizome extract; MERE: Methanolic C. rotundus L. rhizome extract; PERE: Petroleum ether C. rotundus L. rhizome extract; QE: Quercetin equivalent; RNS: Reactive nitrogen species; ROS: Reactive oxygen species; TFC: Total flavonoid content; TPC: Total phenolic content; TPAC: Total proanthocyanidin content.

Supercritical-Multiple-Solvent Extraction From Coal

NASA Technical Reports Server (NTRS)

Corcoran, W.; Fong, W.; Pichaichanarong, P.; Chan, P.; Lawson, D.

1983-01-01

Large and small molecules dissolve different constituents. Experimental apparatus used to test supercritical extraction of hydrogen rich compounds from coal in various organic solvents. In decreasing order of importance, relevant process parameters were found to be temperature, solvent type, pressure, and residence time.

Use of gas chromatography-mass spectrometry for the assessment of the contamination caused by small concentrations of nitrophenols in soils and sediments

NASA Astrophysics Data System (ADS)

Cacho, Juan-Ignacio; Campillo, Natalia; Viñas, Pilar; Hernandez-Cordoba, Manuel

2015-04-01

Nitrophenols (NPs) are widely distributed environmental contaminants that can be present in soils and sediments due to the degradation of some pesticides (parathion and fenitrothion) or by accidental spilling in ammunition plants or storage places. This communication reports a rapid and sensitive procedure for the determination of the most common NPs in soils by using gas chromatography coupled to mass spectrometry (GC-MS) as the analytical technique. Ultrasound assisted extraction (UAE) was employed for the extraction of the NPs from the soil samples to an organic solvent. Next, the resulting UAE extracts were submitted to dispersive liquid-liquid microextraction (DLLME) for achieving an effective preconcentration. DLLME is an easy-to-carry out, environmentally friendly separation technique involving minimal amounts of organic solvents. Since the volatility of NPs is low, as a previous stage to the GC-MS measurement the compounds were derivatized using a simple "in-situ" acetylation procedure. The main parameters affecting the UAE stage, as well as the DLLME and derivatization steps, were investigated looking for maximum analytical signals. The optimized procedure provided extraction recoveries in the 72-86% range, with precision values (expressed as relative standard deviation, RSD) ≤ 12%, and detection limits ranging from 1.3 and 3.3 ng g-1, depending on the compound. 20 soil and sediment samples, from military, industrial and agricultural areas were analyzed by the studied procedure in order to check its applicability.

[Study on ultrafine vibration extraction technology of Rhizoma Chuanxiong].

PubMed

Dai, Long

2009-04-01

To explore the best ultrafine vibration extraction technology of Rhizoma Chuanxiong. Using the content of ligustrazine hydrochloride and ferulic acid as determination indexes, quadrature test was used to choose extraction times, time, solvent amount and to compare with the result of conventional extraction technology. The best condition of the Rhizoma chuanxiong was with 90% ethanol of 4 times volume, extracting 2 times in 25 degrees C, 15 minutes each time. Comparing with conventional extraction technology, extraction time of UVET was 1/6, solvent amount was 4/7, the extraction rate of marker components was 1.19 and 1.09 times, respectivley. UVET can improve the extracting rate of effective constituents, reduce the time and solvent amount and be used in industrialization.

High-efficient extraction of principal medicinal components from fresh Phellodendron bark (cortex phellodendri).

PubMed

Xu, Keqin; He, Gongxiu; Qin, Jieming; Cheng, Xuexiang; He, Hanjie; Zhang, Dangquan; Peng, Wanxi

2018-05-01

There are three key medicinal components (phellodendrine, berberine and palmatine) in the extracts of Phellodendron bark, as one of the fundamental herbs of traditional Chinese medicine. Different extraction methods and solvent combinations were investigated to obtain the optimal technologies for high-efficient extraction of these medicinal components. The results showed that combined solvents have higher extracting effect of phellodendrine, berberine and palmatine than single solvent, and the effect of ultrasonic extraction is distinctly better than those of distillation and soxhlet extraction. The hydrochloric acid/methanol-ultrasonic extraction has the best effect for three medicinal components of fresh Phellodendron bark, providing an extraction yield of 103.12 mg/g berberine, 24.41 mg/g phellodendrine, 1.25 mg/g palmatine.

Evaluation of new natural deep eutectic solvents for the extraction of isoflavones from soy products.

PubMed

Bajkacz, Sylwia; Adamek, Jakub

2017-06-01

Natural deep eutectic solvents (NADESs) are considered to be new, safe solvents in green chemistry that can be widely used in many chemical processes such as extraction or synthesis. In this study, a simple extraction method based on NADES was used for the isolation of isoflavones (daidzin, genistin, genistein, daidzein) from soy products. Seventeen different NADES systems each including two or three components were tested. Multivariate data analysis revealed that NADES based on a 30% solution of choline chloride: citric acid (molar ratio of 1:1) are the most effective systems for the extraction of isoflavones from soy products. After extraction, the analytes were detected and quantified using ultra-high performance liquid chromatography with ultraviolet detection (UHPLC-UV). The proposed NADES extraction procedure achieved enrichment factors up to 598 for isoflavones and the recoveries of the analytes were in the range 64.7-99.2%. The developed NADES extraction procedure and UHPLC-UV determination method was successfully applied for the analysis of isoflavones in soy-containing food samples. The obtained results indicated that new natural deep eutectic solvents could be an alternative to traditional solvents for the extraction of isoflavones and can be used as sustainable and safe extraction media for another applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Infusion extractor

NASA Technical Reports Server (NTRS)

Chang-Diaz, Franklin R. (Inventor)

1986-01-01

This invention relates to an apparatus and method of removing desirable constituents from an infusible material by infusion extraction. A piston operating in a first chamber draws a solvent into the first chamber where it may be heated, and then moves the heated solvent into a second chamber containing the infusible material, where infusion extraction takes place. The piston then moves the solvent containing the extract through a filter into the first chamber, leaving the extraction residue in the second chamber. The method is applicable to operation in low or micro-gravity environments.

Ultrasound-assisted extraction of three bufadienolides from Chinese medicine ChanSu.

PubMed

Sun, Yinshi; Bi, Jianjie; Zhang, Li; Ye, Baoxing

2012-11-01

In this study, the application of ultrasound-assisted extraction (UAE) method was shown to be more efficient in extracting anti-tumor bufadienolides (bufalin, cinobufagin and resibufogenin) from important animal medicine of ChanSu than the maceration extraction (ME) and soxhlet extraction (SE) method. The effects of ultrasonic variables including extraction solvent, solvent concentration, solvent to solid ratio, ultrasound power, temperature, extraction time and particle size on the yields of three bufadienolides were investigated. The optimum extraction conditions found were: 70% (v/v) methanol solution, solvent to solid ratio of 10ml/g, ultrasound power of 125W, temperature of 20°C, extraction time of 20min and particle size of 60-80 mesh. The extraction yields of bufalin, cinobufagin and resibufogenin were 43.17±0.85, 52.58±1.12, 137.70±2.65mg/g, respectively. In order to achieve a similar yield as UAE, soxhlet extraction required 6h and maceration extraction required much longer time of 18h. The results indicated that UAE is an alternative method for extracting bufadienolides from ChanSu. Copyright © 2012 Elsevier B.V. All rights reserved.

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

EPA Science Inventory

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

Water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction for the determination of fungicides in wine.

PubMed

Tseng, Wan-Chi; Chu, Shang-Ping; Kong, Po-Hsin; Huang, Chun-Kai; Chen, Jung-Hsuan; Chen, Pai-Shan; Huang, Shang-Da

2014-09-17

A sample preparation method, dispersive liquid-liquid microextraction assisted by an emulsion with low concentration of a surfactant in water and dispersed solvent coupled with gas chromatography-mass spectrometry, was developed for the analysis of the fungicides cyprodinil, procymidone, fludioxonil, flusilazole, benalaxyl, and tebuconazole in wine. A microsyringe was used to withdraw and discharge a mixture of extraction solvent and 240 μL of an aqueous solution of Triton X-100 (the dispersed agent) four times within 10 s to form a cloudy emulsion in the syringe. This emulsion was then injected into a 5 mL wine sample spiked with all of the above fungicides. The total extraction time was approximately 0.5 min. Under optimum conditions using 1-octanol (12 μL) as extraction solvent, the linear range of the method in analysis of all six fungicides was 0.05-100 μg L(-1), and the limit of detection ranged from 0.013 to 0.155 μg L(-1). The absolute recoveries (n = 3) and relative recoveries (n = 3) were 30-83 and 81-108% for white wine at 0.5, 5, and 5 μg L(-1), and 30-92 and 81-110% for red wine, respectively. The intraday (n = 7) and interday (n = 6) relative standard deviations ranged from 4.4 to 8.8% and from 4.3 to 11.2% at 0.5 μg L(-1), respectively. The method achieved high enrichment factors. It is an alternative sample preparation technique with good performance.

Supercritical fluid extraction. Principles and practice

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

McHugh, M.A.; Krukonis, V.J.

This book is a presentation of the fundamentals and application of super-critical fluid solvents (SCF). The authors cover virtually every facet of SCF technology: the history of SCF extraction, its underlying thermodynamic principles, process principles, industrial applications, and analysis of SCF research and development efforts. The thermodynamic principles governing SCF extraction are covered in depth. The often complex three-dimensional pressure-temperature composition (PTx) phase diagrams for SCF-solute mixtures are constructed in a coherent step-by-step manner using the more familiar two-dimensional Px diagrams. The experimental techniques used to obtain high pressure phase behavior information are described in detail and the advantages andmore » disadvantages of each technique are explained. Finally, the equations used to model SCF-solute mixtures are developed, and modeling results are presented to highlight the correlational strengths of a cubic equation of state.« less

Research News: Emulsion Liquid Membrane Extraction in a Hollow-Fiber Contactor

NASA Technical Reports Server (NTRS)

Wiencek, John M.; Hu, Shih-Yao

2000-01-01

This article describes how ELMs (emulsion liquid membranes) can be used for extraction. The article addresses the disadvantages of ELM extraction in a stirred contactor, and the advantages of SELMs (supported emulsion liquid membranes). The introduction of the article provides background information on liquid-liquid solvent extraction and dispersion-free solvent extraction.

AN EVALUATION OF SAMPLE DISPERSION MEDIAS USED WITH ACCELERATED SOLVENT EXTRACTION FOR THE EXTRACTION AND RECOVERY OF ARSENICALS FROM LFB AND DORM-2

EPA Science Inventory

An accelerated solvent extraction (ASE) device was evaluated as a semi-automated means for extracting arsenicals from quality control (QC) samples and DORM-2 [standard reference material (SRM)]. Unlike conventional extraction procedures, the ASE requires that the sample be dispe...

Extraction and purification of high added value compounds from by-products of the winemaking chain using alternative/nonconventional processes/technologies.

PubMed

Yammine, Sami; Brianceau, Sylène; Manteau, Sébastien; Turk, Mohammad; Ghidossi, Rémy; Vorobiev, Eugène; Mietton-Peuchot, Martine

2018-05-24

Grape byproducts are today considered as a cheap source of valuable compounds since existent technologies allow the recovery of target compounds and their recycling. The goal of the current article is to explore the different recovery stages used by both conventional and alternative techniques and processes. Alternative pre-treatments techniques reviewed are: ultrasounds, pulsed electric fields and high voltage discharges. In addition, nonconventional solvent extraction under high pressure, specifically, supercritical fluid extraction and subcritical water extraction are discussed. Finally alternative purification technologies, for example membrane processing were also examined. The intent is to describe the mechanisms involved by these alternative technologies and to summarize the work done on the improvement of the extraction process of phenolic compounds from winery by-products. With a focus on the developmental stage of each technology, highlighting the research need and challenges to be overcome for an industrial implementation of these unitary operations in the overall extraction process. A critical comparison of conventional and alternative techniques will be reviewed for ethe pre-treatment of raw material, the diffusion of polyphenols and the purification of these high added value compounds. This review intends to give the reader some key answers (costs, advantages, drawbacks) to help in the choice of alternative technologies for extraction purposes.

Evaluation of antibacterial, antioxidant and nootropic activities of Tiliacora racemosa Colebr. leaves: In vitro and in vivo approach.

PubMed

T, Vivek Kumar; M, Vishalakshi; M, Gangaraju; Das, Parijat; Roy, Pratiti; Banerjee, Anindita; Dutta Gupta, Sayan

2017-02-01

The antibacterial and antioxidant potential of Tiliacora racemosa leaf extracts in various solvents (methanolic, hexane, chloroform and ethyl acetate) was determined. Additionally, the presence of bisbenzylisoquinoline alkaloids in the plant prompted us to evaluate the nootropic activity of the methanolic extract in mice. Further, we seek to verify the nootropic effect by examining the anticholinesterase inhibition potential of the methanolic extract. The leaf extracts in various solvents were evaluated for their antibacterial and antioxidant activity by agar diffusion technique and α, α-diphenyl-β-picrylhydrazyl (DPPH) free radical scavenging method, respectively. The ex vivo acetylcholine esterase inhibitory activity of the methanolic extract was carried out by Ellman's method in male Wistar rats. The nootropic capacity of the methanolic extract was examined in Swiss albino mice by utilizing the diazepam induced acute amnesic model. The chloroform/n-hexane and ethyl acetate fraction showed promising antioxidant and antibacterial (Gram positive and Gram negative bacteria) property, respectively. The methanolic extract was able to diminish the amnesic effect induced by diazepam (1mg/kg i.p.) in mice. The extract also showed significant acetyl cholinesterase inhibition in rats. The findings prove that the memory enhancing capability is due to increased acetyl choline level at the nerve endings. The strong antioxidant nature and potential nootropic activity shown by the extract suggests its future usage in the treatment of neurodegenerative disorders such as dementia and Alzheimer. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

A comparison of certain extracting agents for extraction of adenosine triphosphate (ATP) from microorganisms for use in the firefly luciferase ATP assay

NASA Technical Reports Server (NTRS)

Knust, E. A.; Chappelle, E. W.; Picciolo, G. L.

1975-01-01

Firefly luciferase ATP assay is used in clinical and industrial applications, such as determination of urinary infection levels, microbial susceptibility testing, and monitoring of yeast levels in beverages. Three categories of extractants were investigated for their extracting efficiency. They were ionizing organic solvents, nonionizing organic solvents, and inorganic acids. Dimethylsulfoxide and formamide represented the ionizing organic solvents, while n-butanol, chloroform, ethanol, acetone, and methylene chloride were used for the nonionizing organic solvents. Nitric acid and perchloric acid were chosen for the inorganic acids category. Pathogens were tested with each solvent. They included: Saccharomyces carlsbergensis, E. coli, Staphylococcus aureus, Klebsiella pneumoniae, Enterobacter species, Proteus mirabilis, Proteus vulgaris, Staphylococcus epidermidis, Streptococcus faecalis, Pseudomonas aeruginosa, and Candida albicans. These results are shown in graphic representations.

AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

DOEpatents

Van Berkel, Gary J.

2015-06-23

An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

Optimisation of Croton gratissimus Oil Extraction by n-Hexane and Ethyl Acetate Using Response Surface Methodology.

PubMed

Jiyane, Phiwe Charles; Tumba, Kaniki; Musonge, Paul

2018-04-01

The extraction of oil from Croton gratissimus seeds was studied using the three-factor five-level full-factorial central composite rotatable design (CCRD) of the response surface methodology (RSM). The effect of the three factors selected, viz., extraction time, extraction temperature and solvent-to-feed ratio on the extraction oil yield was investigated when n-hexane and ethyl acetate were used as extraction solvents. The coefficients of determination (R 2 ) of the models developed were 0.98 for n-hexane extraction and 0.97 for ethyl acetate extraction. These results demonstrated that the models developed adequately represented the processes they described. From the optimized model, maximum extraction yield obtained from n-hexane and ethyl acetate extraction were 23.88% and 23.25%, respectively. In both cases the extraction temperature and solvent-to-feed ratio were 35°C and 5 mL/g, respectively. In n-hexane extraction the maximum conditions were reached only after 6 min whereas in ethyl acetate extraction it took 20 min to get the maximum extraction oil yield. Oil extraction of Croton gratissimus seeds, in this work, favoured the use of n-hexane as an extraction solvent as it offered higher oil yields at low temperatures and reduced residence times.

Solvent extraction: the coordination chemistry behind extractive metallurgy.

PubMed

Wilson, A Matthew; Bailey, Phillip J; Tasker, Peter A; Turkington, Jennifer R; Grant, Richard A; Love, Jason B

2014-01-07

The modes of action of the commercial solvent extractants used in extractive hydrometallurgy are classified according to whether the recovery process involves the transport of metal cations, M(n+), metalate anions, MXx(n-), or metal salts, MXx into a water-immiscible solvent. Well-established principles of coordination chemistry provide an explanation for the remarkable strengths and selectivities shown by most of these extractants. Reagents which achieve high selectivity when transporting metal cations or metal salts into a water-immiscible solvent usually operate in the inner coordination sphere of the metal and provide donor atom types or dispositions which favour the formation of particularly stable neutral complexes that have high solubility in the hydrocarbons commonly used in recovery processes. In the extraction of metalates, the structures of the neutral assemblies formed in the water-immiscible phase are usually not well defined and the cationic reagents can be assumed to operate in the outer coordination spheres. The formation of secondary bonds in the outer sphere using, for example, electrostatic or H-bonding interactions are favoured by the low polarity of the water-immiscible solvents.

Extraction of basil leaves (ocimum canum) oleoresin with ethyl acetate solvent by using soxhletation method

NASA Astrophysics Data System (ADS)

Tambun, R.; Purba, R. R. H.; Ginting, H. K.

2017-09-01

The goal of this research is to produce oleoresin from basil leaves (Ocimum canum) by using soxhletation method and ethyl acetate as solvent. Basil commonly used in culinary as fresh vegetables. Basil contains essential oils and oleoresin that are used as flavouring agent in food, in cosmetic and ingredient in traditional medicine. The extraction method commonly used to obtain oleoresin is maceration. The problem of this method is many solvents necessary and need time to extract the raw material. To resolve the problem and to produce more oleoresin, we use soxhletation method with a combination of extraction time and ratio from the material with a solvent. The analysis consists of yield, density, refractive index, and essential oil content. The best treatment of basil leaves oleoresin extraction is at ratio of material and solvent 1:6 (w / v) for 6 hours extraction time. In this condition, the yield of basil oleoresin is 20.152%, 0.9688 g/cm3 of density, 1.502 of refractive index, 15.77% of essential oil content, and the colour of oleoresin product is dark-green.

RECOVERY OF METAL VALUES FROM AQUEOUS SOLUTIONS BY SOLVENT EXTRACTION

DOEpatents

Moore, R.L.

1959-09-01

An organic solvent mixure is described for extracting actinides from aqueous solutions; the solvent mixture consists of from 10 to 25% by volume of tributyl phosphate and the remainder a chlorine-fluorine-substituted saturated hydrocarbon having two carbon atoms in the molecule.

Thermal stability study of a new guanidine suppressor for the next-generation caustic-side solvent extraction process

DOE PAGES

Hill, Talon G.; Ensor, Dale D.; Delmau, Lætitia Helene; ...

2016-02-06

Cesium stripping performance of thermally stressed solvent degrades slowly over time in batch tests of the Next Generation Caustic-Side Solvent Extraction (NGS) process. NGS is currently used at pilot scale at the Savannah River Site for the selective removal of cesium from high-level salt waste. Recently a new guanidine, N,N',N" -tris(3,7-dimethyloctyl)guanidine (TiDG), was chosen for use as the suppressor, a lipophilic organic base needed for stripping, and the present study was undertaken to address the question of its stability. The NGS process solvent was evaluated for a period of three months under a variety of temperature and storage conditions. Themore » performance of the solvent was tested at 30-day increments using a standard extraction, scrub, strip, and extraction (ES 2S 3E) sequence. Lastly, the results provide insight on the effects of storage and process conditions, the stripping behavior of TiDG, and the stability of the new solvent composition.« less

Thermal stability study of a new guanidine suppressor for the next-generation caustic-side solvent extraction process

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

Hill, Talon G.; Ensor, Dale D.; Delmau, Lætitia Helene

Cesium stripping performance of thermally stressed solvent degrades slowly over time in batch tests of the Next Generation Caustic-Side Solvent Extraction (NGS) process. NGS is currently used at pilot scale at the Savannah River Site for the selective removal of cesium from high-level salt waste. Recently a new guanidine, N,N',N" -tris(3,7-dimethyloctyl)guanidine (TiDG), was chosen for use as the suppressor, a lipophilic organic base needed for stripping, and the present study was undertaken to address the question of its stability. The NGS process solvent was evaluated for a period of three months under a variety of temperature and storage conditions. Themore » performance of the solvent was tested at 30-day increments using a standard extraction, scrub, strip, and extraction (ES 2S 3E) sequence. Lastly, the results provide insight on the effects of storage and process conditions, the stripping behavior of TiDG, and the stability of the new solvent composition.« less

An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides.

PubMed

Wang, Ziming; Zhao, Xin; Xu, Xu; Wu, Lijie; Su, Rui; Zhao, Yajing; Jiang, Chengfei; Zhang, Hanqi; Ma, Qiang; Lu, Chunmei; Dong, Deming

2013-01-14

A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%. Copyright © 2012 Elsevier B.V. All rights reserved.

Two-Stage Separation of V(IV) and Al(III) by Crystallization and Solvent Extraction from Aluminum-Rich Sulfuric Acid Leaching Solution of Stone Coal

NASA Astrophysics Data System (ADS)

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

2017-10-01

To improve separation of V(IV) and Al(III) from aluminum-rich sulfuric acid leaching solution of stone coal, the two-stage separation by crystallization and solvent extraction methods have been developed. A co-extraction coefficient ( k) was put forward to evaluate comprehensively co-extraction extent in different solutions. In the crystallization stage, 68.2% of aluminum can be removed from the solution. In the solvent extraction stage, vanadium was selectively extracted using di-2-ethylhexyl phosphoric acid/tri-n-butyl phosphate from the crystalline mother solution, followed by H2SO4 stripped efficiently. A V2O5 product with purity of 98.39% and only 0.10% Al was obtained after oxidation, precipitation, and calcination. Compared with vanadium extraction from solution without crystallization, the counter-current extraction stage of vanadium can be decreased from 6 to 3 and co-extraction coefficient ( k) decreased from 2.51 to 0.58 with two-stage separation. It is suggested that the aluminum removal by crystallization can evidently weaken the influence of aluminum co-extraction on vanadium extraction and improve the selectivity of solvent extraction for vanadium.

LC-MS determination of steroidal glycosides from Dioscorea deltoidea Wall cell suspension culture: Optimization of pre-LC-MS procedure parameters by Latin Square design.

PubMed

Sarvin, Boris; Fedorova, Elizaveta; Shpigun, Oleg; Titova, Maria; Nikitin, Mikhail; Kochkin, Dmitry; Rodin, Igor; Stavrianidi, Andrey

2018-03-30

In this paper, the ultrasound assisted extraction method for isolation of steroidal glycosides from D. deltoidea plant cell suspension culture with a subsequent HPLC-MS determination was developed. After the organic solvent was selected via a two-factor experiment the optimization via Latin Square 4 × 4 experimental design was carried out for the following parameters: extraction time, organic solvent concentration in extraction solution and the ratio of solvent to sample. It was also shown that the ultrasound assisted extraction method is not suitable for isolation of steroidal glycosides from the D. deltoidea plant material. The results were double-checked using the multiple successive extraction method and refluxing extraction. Optimal conditions for the extraction of steroidal glycosides by the ultrasound assisted extraction method were: extraction time, 60 min; acetonitrile (water) concentration in extraction solution, 50%; the ratio of solvent to sample, 400 mL/g. Also, the developed method was tested on D. deltoidea cell suspension cultures of different terms and conditions of cultivation. The completeness of the extraction was confirmed using the multiple successive extraction method. Copyright © 2018 Elsevier B.V. All rights reserved.

Elucidation of key aroma compounds in traditional dry fermented sausages using different extraction techniques.

PubMed

Corral, Sara; Salvador, Ana; Flores, Mónica

2015-04-01

The use of different extraction techniques - solid phase microextraction (SPME) and solvent assisted flavour evaporation (SAFE) - can deliver different aroma profiles and it is essential to determine which is most suitable to extract the aroma compounds from dry fermented sausages. Forty-five aroma-active compounds were detected by SPME and SAFE, with 11 of them reported for the first time as aroma compounds in dry fermented sausages: ethyl 3-hydroxy butanoate, trimethyl pyrazine, D-pantolactone, isobutyl hexanoate, ethyl benzoate, α-terpineol, ethyl 3-pyridinecarboxylate, benzothiazole, 2,3-dihydrothiophene, methyl eugenol, γ-nonalactone. The aroma concentration and odour activity values (OAVs) were calculated. Flavour reconstitution analyses were performed using 20 odorants with OAVs above 1 obtained from the SAFE and SPME extracts to prepare the aroma model. SPME and SAFE techniques were complementary and necessary to reproduce the overall dry fermented sausage aroma. The final aroma model included the odorants from both extraction techniques (SPME and SAFE) but it was necessary to incorporate the compounds 2,4-decadienal (E,E), benzothiazole, methyl eugenol, α-terpineol, and eugenol to the final aroma model to evoked the fresh sausage aroma although a lowest cured meat aroma note was perceived. © 2014 Society of Chemical Industry.

Enhanced and green extraction polyphenols and furanocoumarins from Fig (Ficus carica L.) leaves using deep eutectic solvents.

PubMed

Wang, Tong; Jiao, Jiao; Gai, Qing-Yan; Wang, Peng; Guo, Na; Niu, Li-Li; Fu, Yu-Jie

2017-10-25

Nowadays, green extraction of bioactive compounds from medicinal plants has gained increasing attention. As green solvent, deep eutectic solvent (DES) have been highly rated to replace toxic organic solvents in extraction process. In present study, to simultaneous extraction five main bioactive compounds from fig leaves, DES was tailor-made. The tailor-made DES composed of a 3:3:3 molar ratio of glycerol, xylitol and D-(-)-Fructose showed enhanced extraction yields for five target compounds simultaneously compared with traditional methanol and non-tailor DESs. Then, the tailor-made DES based extraction methods have compared and microwave-assisted extraction was selected and optimized due to its high extraction yields with lower time consumption. The influencing parameters including extraction temperature, liquid-solid ratio, and extraction time were optimized using response surface methodology (RSM). Under optimal conditions the extraction yield of caffeoylmalic acid, psoralic acid-glucoside, rutin, psoralen and bergapten was 6.482mg/g, 16.34mg/g, 5.207mg/g, 15.22mg/g and 2.475mg/g, respectively. Macroporous resin D101 has been used to recovery target compounds with recovery yields of 79.2%, 83.4%, 85.5%, 81.2% and 75.3% for caffeoylmalic acid, psoralic acid-glucoside, rutin, psoralen and bergapten, respectively. The present study suggests that DESs are truly designer and efficient solvents and the method we developed was efficient and sustainable for extraction main compounds from Fig leaves.mg/g. Copyright © 2017 Elsevier B.V. All rights reserved.

Green procedure with a green solvent for fats and oils' determination. Microwave-integrated Soxhlet using limonene followed by microwave Clevenger distillation.

PubMed

Virot, Matthieu; Tomao, Valérie; Ginies, Christian; Visinoni, Franco; Chemat, Farid

2008-07-04

Here is described a green and original alternative procedure for fats and oils' determination in oleaginous seeds. Extractions were carried out using a by-product of the citrus industry as extraction solvent, namely d-limonene, instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using microwave energy: at first, extractions are attained using microwave-integrated Soxhlet, followed by the elimination of the solvent from the medium using a microwave Clevenger distillation in the second step. Oils extracted from olive seeds were compared with both conventional Soxhlet and microwave-integrated Soxhlet extraction procedures performed with n-hexane in terms of qualitative and quantitative determination. No significant difference was obtained between each extract allowing us to conclude that the proposed method is effective and valuable.

Process analysis and modeling of a single-step lutein extraction method for wet microalgae.

PubMed

Gong, Mengyue; Wang, Yuruihan; Bassi, Amarjeet

2017-11-01

Lutein is a commercial carotenoid with potential health benefits. Microalgae are alternative sources for the lutein production in comparison to conventional approaches using marigold flowers. In this study, a process analysis of a single-step simultaneous extraction, saponification, and primary purification process for free lutein production from wet microalgae biomass was carried out. The feasibility of binary solvent mixtures for wet biomass extraction was successfully demonstrated, and the extraction kinetics of lutein from chloroplast in microalgae were first evaluated. The effects of types of organic solvent, solvent polarity, cell disruption method, and alkali and solvent usage on lutein yields were examined. A mathematical model based on Fick's second law of diffusion was applied to model the experimental data. The mass transfer coefficients were used to estimate the extraction rates. The extraction rate was found more significantly related with alkali ratio to solvent than to biomass. The best conditions for extraction efficiency were found to be pre-treatment with ultrasonication at 0.5 s working cycle per second, react 0.5 h in 0.27 L/g solvent to biomass ratio, and 1:3 ether/ethanol (v/v) with 1.25 g KOH/L. The entire process can be controlled within 1 h and yield over 8 mg/g lutein, which is more economical for scale-up.

Application of natural deep eutectic solvents to the extraction of anthocyanins from Catharanthus roseus with high extractability and stability replacing conventional organic solvents.

PubMed

Dai, Yuntao; Rozema, Evelien; Verpoorte, Robert; Choi, Young Hae

2016-02-19

Natural deep eutectic solvents (NADES) have attracted a great deal of attention in recent times as promising green media. They are generally composed of neutral, acidic or basic compounds that form liquids of high viscosity when mixed in certain molar ratio. Despite their potential, viscosity and acid or basic nature of some ingredients may affect the extraction capacity and stabilizing ability of the target compounds. To investigate these effects, extraction with a series of NADES was employed for the analysis of anthocyanins in flower petals of Catharanthus roseus in combination with HPLC-DAD-based metabolic profiling. Along with the extraction yields of anthocyanins their stability in NADES was also studied. Multivariate data analysis indicates that the lactic acid-glucose (LGH), and 1,2-propanediol-choline chloride (PCH) NADES present a similar extraction power for anthocyanins as conventional organic solvents. Furthermore, among the NADES employed, LGH exhibits an at least three times higher stabilizing capacity for cyanidins than acidified ethanol, which facilitates their extraction and analysis process. Comparing NADES to the conventional organic solvents, in addition to their reduced environmental impact, they proved to provide higher stability for anthocyanins, and therefore have a great potential as possible alternatives to those organic solvents in health related areas such as food, pharmaceuticals and cosmetics. Copyright © 2016 Elsevier B.V. All rights reserved.

Flotation/ultrasound-assisted microextraction followed by HPLC for determination of fat-soluble vitamins in multivitamin pharmaceutical preparations.

PubMed

Shahdousti, Parvin; Aghamohammadi, Mohammad

2018-04-01

Dissolved carbon dioxide flotation-emulsification microextraction technique coupled with high-performance liquid chromatography was developed for separation and determination of fat-soluble vitamins (A, D 3 , E, and K 3 ) in multivitamin pharmaceutical preparations. Dissolved carbon dioxide flotation was used to break up the emulsion of extraction solvent in water and to collect the extraction solvent on the surface of aqueous sample in narrowed capillary part of extraction cell. Carbon dioxide bubbles were generated in situ through the addition of 300 μL of concentrated hydrochloric acid into the alkaline sample solution at pH = 11.5 (1% w/v sodium carbonate), which was sonicated to intensify the carbon dioxide bubble generation. Several factors affecting the extraction process were optimized. Under the optimal conditions, the limits of detection were 0.11, 0.47, 0.20 and 0.35 μg/L for A, E, D 3 , and K 3 vitamins in water samples, respectively. The inter-day and intra-day precision of the proposed method were evaluated in terms of the relative standard deviation and were <10.5%. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Method for testing earth samples for contamination by organic contaminants

DOEpatents

Schabron, J.F.

1996-10-01

Provided is a method for testing earth samples for contamination by organic contaminants, and particularly for aromatic compounds such as those found in diesel fuel and other heavy fuel oils, kerosene, creosote, coal oil, tars and asphalts. A drying step is provided in which a drying agent is contacted with either the earth sample or a liquid extract phase to reduce to possibility of false indications of contamination that could occur when humic material is present in the earth sample. This is particularly a problem when using relatively safe, non-toxic and inexpensive polar solvents such as isopropyl alcohol since the humic material tends to be very soluble in those solvents when water is present. Also provided is an ultraviolet spectroscopic measuring technique for obtaining an indication as to whether a liquid extract phase contains aromatic organic contaminants. In one embodiment, the liquid extract phase is subjected to a narrow and discrete band of radiation including a desired wave length and the ability of the liquid extract phase to absorb that wavelength of ultraviolet radiation is measured to provide an indication of the presence of aromatic organic contaminants. 2 figs.

Investigation of aggregation in solvent extraction of lanthanides by acidic extractants (organophosphorus and naphthenic acid)

USGS Publications Warehouse

Zhou, N.; Wu, J.; Yu, Z.; Neuman, R.D.; Wang, D.; Xu, G.

1997-01-01

Three acidic extractants (I) di(2-ethylhexyl) phosphoric acid (HDEHP), (II) 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (HEHPEHE) and (III) naphthenic acid were employed in preparing the samples for the characterization of the coordination structure of lanthanide-extractant complexes and the physicochemical nature of aggregates formed in the organic diluent of the solvent extraction systems. Photo correlation spectroscopy (PCS) results on the aggregates formed by the partially saponified HDEHP in n-heptane showed that the hydrodynamic radius of the aggregates was comparable to the molecular dimensions of HDEHP. The addition of 2-octanol into the diluent, by which the mixed solvent was formed, increased the dimensions of the corresponding aggregates. Aggregates formed from the lanthanide ions and HDEHP in the organic phase of the extraction systems were found very unstable. In the case of naphthenic acid, PCS data showed the formation of w/o microemulsion from the saponified naphthenic acid in the mixed solvent. The extraction of lanthanides by the saponified naphthenic acid in the mixed solvent under the given experimental conditions was a process of destruction of the w/o microemulsion. A possible mechanism of the breakdown of the w/o microemulsion droplets is discussed.

High-pressure processing as emergent technology for the extraction of bioactive ingredients from plant materials.

PubMed

Jun, Xi

2013-01-01

High-pressure processing is a food processing technique that has shown great potentials in the food industry. Recently, it was developed to extract bioactive ingredients from plant materials, known as ultrahigh pressure extraction (UPE), taking advantages of time saving, higher extraction yields, fewer impurities in the extraction solution, minimal heat and can avoid thermal degradation on the activity and structure of bioactive components, and so on. This review provides an overview of the developments in the UPE of bioactive ingredients from plant material. Apart from a brief presentation of the theories of UPE and extraction equipment systems, the principal parameters that influence the extraction efficiency to be optimized in the UPE (e.g., solvent, pressure, temperature, extraction time, and the number of cycle) were discussed in detail, and finally the more recent applications of UPE for the extraction of active compounds from plant materials were summarized.

Modified extraction procedure for gas-liquid chromatography applied to the identification of anaerobic bacteria.

PubMed Central

Thomann, W R; Hill, G B

1986-01-01

Chloroform and ether commonly are used as solvents to extract metabolic organic acids for analysis by gas-liquid chromatography in the identification of anaerobic bacteria. Because these solvents are potentially hazardous to personnel, modified extraction procedures involving the use of a safer solvent, methyl tert-butyl ether were developed which remained both simple to perform and effective for organism identification. PMID:3700623

SOLVENT EXTRACTION OF RUTHENIUM

DOEpatents

Hyman, H.H.; Leader, G.R.

1959-07-14

The separation of rathenium from aqueous solutions by solvent extraction is described. According to the invention, a nitrite selected from the group consisting of alkali nitrite and alkaline earth nitrite in an equimolecular quantity with regard to the quantity of rathenium present is added to an aqueous solution containing ruthenium tetrantrate to form a ruthenium complex. Adding an organic solvent such as ethyl ether to the resulting mixture selectively extracts the rathenium complex.

Pressurised solvent extraction for organotin speciation in vegetable matrices.

PubMed

Marcic, Christophe; Lespes, Gaëtane; Potin-Gautier, Martine

2005-08-01

Because organotin compounds (OTC) are widely used in many fields of activity, they have become an ubiquitous environmental presence. The presence of organotins in the environment impacts upon food safety, making it important to monitor the levels of organotin pesticides in fruits and vegetables. Nevertheless, only a few studies have been published on organotin speciation in plants. The objective of the present study was to evaluate and optimise a specific procedure based on pressurised solvent extraction (PSE) that is suitable for monitoring organotin content in vegetables. In ASE, solvents are used at elevated temperatures and pressures to increase the rate and efficiency of the extraction process. The results from this procedure were compared to those from the technique usually employed, solid/liquid extraction (SLE) performed in an acidic solvent by mechanical shaking. Three extracting solutions were tested-methanol, ethyl acetate and a mixture of methanol and ethyl acetate-and the mixture was found to give the most quantitative results while preserving the speciation. French bean and lettuce leaves as well as potato tubers were used as the plant materials. These vegetables were considered because they are the vegetables consumed in the most quantities in Europe. The study focuses on trisubstituted OTCs, which are the most toxic tin species. The samples were spiked with four trisubstituted organotins: tributyltin (TBT), triphenyltin (TPhT), tricyclohexyltin (TcHexT) and trioctyltin (TOcT). The influence of the pressure and the temperature of the PSE on the quantitativity of the process and on species preservation was evaluated using the experimental design methodology. The optimised PSE allowed detection limits down to 1-2 ng (Sn) g(-1) to be reached. These are higher than those obtained by SLE (0.1-1 ng (Sn) g(-1)). Although the repeatability is similar for both PSE and SLE (2-12% for triorganotin compounds), this appears to be highly time-dependent in the case of SLE. Comparison with SLE confirms that PSE is an interesting tool for vegetable analysis considering the satisfactory OTC preservation and repeatability obtained for a relatively short extraction duration (only 15 min against 2-12 h for SLE).

The influence of purge times on the yields of essential oil components extracted from plants by pressurized liquid extraction.

PubMed

Wianowska, Dorota

2014-01-01

The influence of different purge times on the yield of the main essential oil constituents of rosemary (Rosmarinus officinalis L.), thyme (Thymus vulgaris L.), and chamomile (Chamomilla recutita L.) was investigated. The pressurized liquid extraction process was performed by applying different extraction temperatures and solvents. The results presented in the paper show that the estimated yield of essential oil components extracted from the plants in the pressurized liquid extraction process is purge time-dependent. The differences in the estimated yields are mainly connected with the evaporation of individual essential oil components and the applied solvent during the purge; the more volatile an essential oil constituent is, the greater is its loss during purge time, and the faster the evaporation of the solvent during the purge process is, the higher the concentration of less volatile essential oil components in the pressurized liquid extraction receptacle. The effect of purge time on the estimated yield of individual essential oil constituents is additionally differentiated by the extraction temperature and the extraction ability of the applied solvent.

Interdisciplinary Chemistry Experiment: An Environmentally Friendly Extraction of Lycopene

ERIC Educational Resources Information Center

Zhu, Jie; Zhang, Mingjie; Liu, Qingwei

2008-01-01

A novel experiment for the extraction of lycopene from tomato paste without the use of an organic solvent is described. The experiment employs polymer, green, and analytical chemistry. This environmentally friendly extraction is more efficient and requires less time than the traditional approach using an organic solvent. The extraction is…

Multiple Solvent Extraction System with Flow Injection Technology.

DTIC Science & Technology

1981-09-30

encounters a back extraction step where the direction of the extraction is from organic to aqueous solvent. Thus it is advantageous to incorporate both...stainless steel ( Alltech Associates, Arlington Heights, IQ) and prepared from a single section of 180 cmn in length. The Section 2 mixing and extraction

Recovery of 1,3-, 2,3-dichloropropenes, 1,2-dibromo-3-chloropropane, and o-, p-dichlorobenzenes from fatty and non-fat foodstuffs by liquid extraction technique.

PubMed

Daft, J L

1990-01-01

Food samples including fatty, non-fatty, grain-based, and nongrain-based types were fortified with the following five nematocides and fumigants: 1,3-dichloropropene, 2,3-dichloropropene, 1,2-dibromo-3-chloropropane, o-dichlorobenzene, and p-dichlorobenzene. Then, depending on sample consistency and type, the samples were diluted in, or extracted with organic solvent such as isooctane. A few of the high-fat extracts were passed through Florisil to remove excess fat or endogenous interferences. Analysis of the initial or cleaned up extracts was done by gas chromatography (GC) at 90 degrees C. The dichloropropenes were determined on 20% OV-101 columns with electron-capture and Hall electroconductivity detectors. The dichlorobenzenes and 1,2-dibromo-3-chloropropane, which elute beyond 30 min on the above columns, were determined on 5%-loaded columns using the same detectors. All five analytes were recovered from these techniques. Mean analyte recovery following a direct dilution or extraction was 83%, and following the Florisil cleanup step, was 52%. In 1986, a fumigant survey of about 200 foodstuffs by using this overall technique gave no findings of the five compounds studied here.

Systematic assessment of different solvents for the extraction of drugs of abuse and pharmaceuticals from an authentic hair pool.

PubMed

Madry, Milena M; Kraemer, Thomas; Baumgartner, Markus R

2018-01-01

Hair analysis has been established as a prevalent tool for retrospective drug monitoring. In this study, different extraction solvents for the determination of drugs of abuse and pharmaceuticals in hair were evaluated for their efficiency. A pool of authentic hair from drug users was used for extraction experiments. Hair was pulverized and extracted in triplicate with seven different solvents in a one- or two-step extraction. Three one- (methanol, acetonitrile, and acetonitrile/water) and four two-step extractions (methanol two-fold, methanol and methanol/acetonitrile/formate buffer, methanol and methanol/formate buffer, and methanol and methanol/hydrochloric acid) were tested under accurately equal experimental conditions. The extracts were directly analyzed by liquid chromatography-tandem mass spectrometry for opiates/opioids, stimulants, ketamine, selected benzodiazepines, antidepressants, antipsychotics, and antihistamines using deuterated internal standards. For most analytes, a two-step extraction with methanol did not significantly improve the yield compared to a one-step extraction with methanol. Extraction with acetonitrile alone was least efficient for most analytes. Extraction yields of acetonitrile/water, methanol and methanol/acetonitrile/formate buffer, and methanol and methanol/formate buffer were significantly higher compared to methanol. Highest efficiencies were obtained by a two-step extraction with methanol and methanol/hydrochloric acid, particularly for morphine, 6-monoacetylmorphine, codeine, 6-acetylcodeine, MDMA, zopiclone, zolpidem, amitriptyline, nortriptyline, citalopram, and doxylamine. For some analytes (e.g., tramadol, fluoxetine, sertraline), all extraction solvents, except for acetonitrile, were comparably efficient. There was no significant correlation between extraction efficiency with an acidic solvent and the pka or log P of the analyte. However, there was a significant trend for the extraction efficiency with acetonitrile to the log P of the analyte. The study demonstrates that the choice of extraction solvent has a strong impact on hair analysis outcomes. Therefore, validation protocols should include the evaluation of extraction efficiency of drugs by using authentic rather than spiked hair. Different extraction procedures may contribute to the scatter of quantitative results in inter-laboratory comparisons. Harmonization of extraction protocols is recommended, when interpretation is based on same cut-off levels. Copyright © 2017 Elsevier B.V. All rights reserved.

A molecular method to assess bioburden embedded within silicon-based resins used on modern spacecraft materials

NASA Astrophysics Data System (ADS)

Stam, Christina N.; Bruckner, James; Spry, J. Andy; Venkateswaran, Kasthuri; La Duc, Myron T.

2012-07-01

Current assessments of bioburden embedded in spacecraft materials are based on work performed in the Viking era (1970s), and the ability to culture organisms extracted from such materials. To circumvent the limitations of such approaches, DNA-based techniques were evaluated alongside established culturing techniques to determine the recovery and survival of bacterial spores encapsulated in spacecraft-qualified polymer materials. Varying concentrations of Bacillus pumilus SAFR-032 spores were completely embedded in silicone epoxy. An organic dimethylacetamide-based solvent was used to digest the epoxy and spore recovery was evaluated via gyrB-targeted qPCR, direct agar plating, most probably number analysis, and microscopy. Although full-strength solvent was shown to inhibit the germination and/or outgrowth of spores, dilution in excess of 100-fold allowed recovery with no significant decrease in cultivability. Similarly, qPCR (quantitative PCR) detection sensitivities as low as ~103 CFU ml-1 were achieved upon removal of inhibitory substances associated with the epoxy and/or solvent. These detection and enumeration methods show promise for use in assessing the embedded bioburden of spacecraft hardware.

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

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

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

1986-01-01

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

Pressurized liquid extraction of ginger (Zingiber officinale Roscoe) with bioethanol: an efficient and sustainable approach.

PubMed

Hu, Jiajin; Guo, Zheng; Glasius, Marianne; Kristensen, Kasper; Xiao, Langtao; Xu, Xuebing

2011-08-26

To develop an efficient green extraction approach for recovery of bioactive compounds from natural plants, we examined the potential of pressurized liquid extraction (PLE) of ginger (Zingiber officinale Roscoe) with bioethanol/water as solvents. The advantages of PLE over other extraction approaches, in addition to reduced time/solvent cost, the extract of PLE showed a distinct constituent profile from that of Soxhlet extraction, with significantly improved recovery of diarylheptanoids, etc. Among the pure solvents tested for PLE, bioethanol yield the highest efficiency for recovering most constituents of gingerol-related compounds; while for a broad concentration spectrum of ethanol aqueous solutions, 70% ethanol gave the best performance in terms of yield of total extract, complete constituent profile and recovery of most gingerol-related components. PLE with 70% bioethanol operated at 1500 psi and 100 °C for 20 min (static extraction time: 5 min) is recommended as optimized extraction conditions, achieving 106.8%, 109.3% and 108.0% yield of [6]-, [8]- and [10]-gingerol relative to the yield of corresponding constituent obtained by 8h Soxhlet extraction (absolute ethanol as extraction solvent). Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of Three Organochlorine Pesticides in Aqueous Samples by Solid-Phase Extraction Based on Natural Nano Diatomite in Packed Syringe Coupled to Gas Chromatography-Mass Spectrometry.

PubMed

Taghani, Abdollah; Goudarzi, Nasser; Bagherian, Ghadamali; Chamjangali, Mansour Arab

2017-01-01

A rapid, simple, and sensitive technique is proposed based on a miniaturized solid-phase extraction method named mictroextraction in a packed syringe coupled with gas chromatography-mass spectrometry for the preconcentration and determination of three organochlorine pesticides. These include hexachlorobenzene, heptachlor and aldrine in aqueous samples. For the first time, the natural nano diatomite is used a sorbent. Based on this technique, 6.0 mg of the nano sorbent is inserted in a syringe between two polypropylene frits. The analytes would be adsorbed on the solid phase, and would subsequently be eluted using organic solvents. The influence of some important parameters, such as the solution pH, type and volume of the organic desorption solvent, and amount of sorbent on the extraction efficiency of the selected pesticides, is investigated. The proposed method shows good linearity in the range of 0.1 - 40.0 μg L -1 , and at low limits of detection in the range of 0.02 - 0.13 μg L -1 using the selected ion-monitoring mode. The reproducibility of this method was found to be in the range of 3.5 - 11.1% for the understudied pesticides. In order to evaluate the matrix effect, the developed method is also applied to the preconcentration and determination of the selected pesticides in different water samples.

LC-UV-solid-phase extraction-NMR-MS combined with a cryogenic flow probe and its application to the identification of compounds present in Greek oregano.

PubMed

Exarchou, Vassiliki; Godejohann, Markus; van Beek, Teris A; Gerothanassis, Ioannis P; Vervoort, Jacques

2003-11-15

Structure elucidation of natural products usually relies on a combination of NMR spectroscopy with mass spectrometry whereby NMR trails MS in terms of the minimum sample amount required. In the present study, the usefulness of on-line solid-phase extraction (SPE) in LC-NMR for peak storage after the LC separation prior to NMR analysis is demonstrated. The SPE unit allows the use of normal protonated solvents for the LC separation and fully deuterated solvents for flushing the trapped compounds to the NMR probe. Thus, solvent suppression is no longer necessary. Multiple trapping of the same analyte from repeated LC injections was utilized to solve the problem of low concentration and to obtain 2D heteronuclear NMR spectra. In addition, a combination of the SPE unit with a recently developed cryoflow NMR probe and an MS was evaluated. This on-line LC-UV-SPE-NMR-MS system was used for the automated analysis of a Greek oregano extract. Combining the data provided by the UV, MS, and NMR spectra, the flavonoids taxifolin, aromadendrin, eriodictyol, naringenin, and apigenin, the phenolic acid rosmarinic acid, and the monoterpene carvacrol were identified. This automated technique is very useful for natural product analysis, and the large sensitivity improvement leads to significantly reduced NMR acquisition times.

Extraction of Trivalent Actinides and Lanthanides from Californium Campaign Rework Solution Using TODGA-based Solvent Extraction System

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

Benker, Dennis; Delmau, Laetitia Helene; Dryman, Joshua Cory

This report presents the studies carried out to demonstrate the possibility of quantitatively extracting trivalent actinides and lanthanides from highly acidic solutions using a neutral ligand-based solvent extraction system. These studies stemmed from the perceived advantage of such systems over cationexchange- based solvent extraction systems that require an extensive feed adjustment to make a low-acid feed. The targeted feed solutions are highly acidic aqueous phases obtained after the dissolution of curium targets during a californium (Cf) campaign. Results obtained with actual Cf campaign solutions, but highly diluted to be manageable in a glove box, are presented, followed by results ofmore » tests run in the hot cells with Cf campaign rework solutions. It was demonstrated that a solvent extraction system based on the tetraoctyl diglycolamide molecule is capable of quantitatively extracting trivalent actinides from highly acidic solutions. This system was validated using actual feeds from a Cf campaign.« less

Optimization by response surface methodology of lutein recovery from paprika leaves using accelerated solvent extraction.

PubMed

Kang, Jae-Hyun; Kim, Suna; Moon, BoKyung

2016-08-15

In this study, we used response surface methodology (RSM) to optimize the extraction conditions for recovering lutein from paprika leaves using accelerated solvent extraction (ASE). The lutein content was quantitatively analyzed using a UPLC equipped with a BEH C18 column. A central composite design (CCD) was employed for experimental design to obtain the optimized combination of extraction temperature (°C), static time (min), and solvent (EtOH, %). The experimental data obtained from a twenty sample set were fitted to a second-order polynomial equation using multiple regression analysis. The adjusted coefficient of determination (R(2)) for the lutein extraction model was 0.9518, and the probability value (p=0.0000) demonstrated a high significance for the regression model. The optimum extraction conditions for lutein were temperature: 93.26°C, static time: 5 min, and solvent: 79.63% EtOH. Under these conditions, the predicted extraction yield of lutein was 232.60 μg/g. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ultrasound-Assisted Extraction of Stilbenes from Grape Canes.

PubMed

Piñeiro, Zulema; Marrufo-Curtido, Almudena; Serrano, Maria Jose; Palma, Miguel

2016-06-16

An analytical ultrasound-assisted extraction (UAE) method has been optimized and validated for the rapid extraction of stilbenes from grape canes. The influence of sample pre-treatment (oven or freeze-drying) and several extraction variables (solvent, sample-solvent ratio and extraction time between others) on the extraction process were analyzed. The new method allowed the main stilbenes in grape canes to be extracted in just 10 min, with an extraction temperature of 75 °C and 60% ethanol in water as the extraction solvent. Validation of the extraction method was based on analytical properties. The resulting RSDs (n = 5) for interday/intraday precision were less than 10%. Furthermore, the method was successfully applied in the analysis of 20 different grape cane samples. The result showed that grape cane byproducts are potentially sources of bioactive compounds of interest for pharmaceutical and food industries.

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

DOEpatents

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

1982-01-01

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

Experiment on the treatment of waste extraction solvent from the molybdenum-99 process

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

Hsien-Ming Hsiao; Chang-Liang Hu; Kuang-Li Chien

2013-07-01

In the Mo-99 (Molybdenum-99) isotope extraction test process for radiopharmaceutical applications, organic solvent is used to extract Mo-99 from an irradiated UO{sub 2} dissolution. The extraction solvent was stored when the test work was stopped. A total of about 120 liters of waste solvent was stored at INER (Institute of Nuclear Energy Research, Taiwan). The extraction solvent consisted of 5% di-(2-ethylhexyl)-phosphoric acid (D2EHPA) and kerosene. The radionuclides found in the waste solvent include Cs-137, Am-241, Tc-99, and Sr-90, which give off gross alpha and beta radioactivity of 1898 and 471 Bq/ml, respectively. This study aims to remove radionuclides from themore » waste solvent using sodium carbonate and sodium hydroxide solutions in different concentrations. After mixing the waste solvent with the alkaline solution followed by settling, a third phase other than organic and aqueous phase appeared which is expected due to the saponification reaction. The experimental results showed that increasing the number of washing and the alkaline solution concentration could enhance the radionuclides removal rate. An optimal removal method was proposed using 2 M Na{sub 2}CO{sub 3} solution twice followed by 1 M NaOH solution one time for the third phase generated early in the mixing stages. The remaining gross alpha and beta radioactivity of the treated organic solvent was 2 and 3 Bq/ml, respectively. The treated solvent could be stabilized by ashing at 500 deg. C and then immobilized. The alkaline solution would be neutralized by hydrochloric or nitric acid and then treated using a variety of adsorbents or bone char via adsorption to remove nuclides to meet the wastewater discharge limitation. (authors)« less

Changes in total phenol, flavonoid contents and anti-Lactobacillus activity of Callisia fragrans due to extraction solvent

NASA Astrophysics Data System (ADS)

Le, Thom; Cao, Diem Kieu; Pham, Thanh Vy; Huynh, Tan Dat; Ta, Nhat Thuy Anh; Nguyen, Ngoc Thao Linh; Nguyen, Huu Thanh; Le, Hue Huong; Bui, Anh Vo; Truong, Dieu-Hien

2018-04-01

Callisia fragrans is a wonder herb with many medicinal properties such as burn, dental diseases, cancer diseases and arthritis in folk medicine. It is noted that the phytochemical constituents and antimicrobial activity of traditional plants depend on not only the extracting method but also the solvent used for extraction. In this study, the effect of five extraction solvents (i.e., distilled water, 80% methanol, 80% ethanol, 80% ethyl acetate, and 80% chloroform) on yield, total phenolic content (TPC) and total flavonoid content (TFC) of Callisia leaves was determined. Besides, changes in anti-Lactobacillus fermentum activity of C. fragrans freeze-dried extract was also evaluated using disk-diffusion method. The recovery percentage of extractable yield of fresh leaves are ranged from 11.93% w/w for distilled water extract to 16.60% w/w for aqueous ethanol extracts. The yield of 80% aqueous methanol extract (16.27% w/w) is only slightly less than that of the ethanol extract. Significant differences were observed among TPC and TFC obtaining by 80% methanol (0.0522% and 0.0335% w/w, respectively) compared to other solvents (p < 0.05). TPC and TFC of C. fragrans extracts increase in the following order: distilled water < 80% chloroform < 80% ethyl acetate < 80% ethanol < 80% methanol. The results revealed that 80% aqueous methanol Calissia extracts has moderate inhibition (9.0 mm of inhibition zone for 1.5 mg/mL of extracts) of L. fermentum compared to standard antibacterial agent. Based on the study results, it can be concluded that the yield, TPC and TFC of C. frgrans extract varied with the extracting solvent. It also showed that Callisia extracts can prevent dental caries by inhibiting the growth of L. fermentum, towards new insights for treatment of dental caries.

Assessment of Multiple Solvents for Extraction and Direct GC-MS Determination of the Phytochemical Inventory of Sansevieria Extrafoliar Nectar Droplets.

PubMed

Gaylor, Michael O; Juntunen, Hope L; Hazelwood, Donna; Videau, Patrick

2018-04-01

Considerable effort has been devoted to analytical determinations of sugar and amino acid constituents of plant nectars, with the primary aim of understanding their ecological roles, yet few studies have reported more exhaustive organic compound inventories of plant nectars or extrafoliar nectars. This work evaluated the efficacy of four solvents (ethyl acetate, dichloromethane, toluene and hexane) to extract the greatest number of organic compound classes and unique compounds from extrafoliar nectar drops produced by Sansevieria spp. Aggregation of the results from each solvent revealed that 240 unique compounds were extracted in total, with 42.5% of those detected in multiple extracts. Aliphatic hydrocarbons dominated in all but the ethyl acetate extracts, with 44 unique aliphatic hydrocarbons detected in dichloromethane (DCM) extracts, followed by 41, 19 and 8 in hexane, toluene and ethyl acetate extracts, respectively. Hexane extracted the most unique compounds (79), followed by DCM (73), ethyl acetate (56) and toluene (32). Integrated total ion chromatographic peak areas of extracted compound classes were positively correlated with numbers of unique compounds detected within those classes. In addition to demonstrating that multi-solvent extraction with direct GC-MS detection is a suitable analytical approach for determining secondary nectar constituents, to the best of our knowledge, this study also represents: (i) the first attempt to inventory the secondary phytochemical constituents of Sansevieria spp. extrafoliar nectar secretions and (ii) the largest organic solvent extractable compound inventory reported for any plant matrix to date.

Optimization of solvent extraction of shea butter (Vitellaria paradoxa) using response surface methodology and its characterization.

PubMed

Ajala, E O; Aberuagba, F; Olaniyan, A M; Onifade, K R

2016-01-01

Shea butter (SB) was extracted from its kernel by using n-hexane as solvent in an optimization study. This was to determine the optima operating variables that would give optimum yield of SB and to study the effect of solvent on the physico-chemical properties and chemical composition of SB extracted using n-hexane. A Box-behnken response surface methodology (RSM) was used for the optimization study while statistical analysis using ANOVA was used to test the significance of the variables for the process. The variables considered for this study were: sample weight (g), solvent volume (ml) and extraction time (min). The physico-chemical properties of SB extracted were determined using standard methods and Fourier Transform Infrared Spectroscopy (FTIR) for the chemical composition. The results of RSM analysis showed that the three variables investigated have significant effect (p < 0.05) on the %yield of SB, with R(2) - 0.8989 which showed good fitness of a second-order model. Based on this model, optima operating variables for the extraction process were established as: sample weight of 30.04 g, solvent volume of 346.04 ml and extraction time of 40 min, which gave 66.90 % yield of SB. Furthermore, the result of the physico-chemical properties obtained for the shea butter extracted using traditional method (SBT) showed that it is a more suitable raw material for food, biodiesel production, cosmetics, medicinal and pharmaceutical purposes than shea butter extracted using solvent extraction method (SBS). Fourier Transform Infrared Spectroscopy (FTIR) results obtained for the two samples were similar to what was obtainable from other vegetable oil.

Solvent for the simultaneous recovery of radionuclides from liquid radioactive wastes

DOEpatents

Romanovskiy, Valeriy Nicholiavich; Smirnov, Igor V.; Babain, Vasiliy A.; Todd, Terry A.; Brewer, Ken N.

2002-01-01

The present invention relates to solvents, and methods, for selectively extracting and recovering radionuclides, especially cesium and strontium, rare earths and actinides from liquid radioactive wastes. More specifically, the invention relates to extracting agent solvent compositions comprising complex organoboron compounds, substituted polyethylene glycols, and neutral organophosphorus compounds in a diluent. The preferred solvent comprises a chlorinated cobalt dicarbollide, diphenyl-dibutylmethylenecarbamoylphosphine oxide, PEG-400, and a diluent of phenylpolyfluoroalkyl sulfone. The invention also provides a method of using the invention extracting agents to recover cesium, strontium, rare earths and actinides from liquid radioactive waste.

Method for the simultaneous recovery of radionuclides from liquid radioactive wastes using a solvent

DOEpatents

Romanovskiy, Valeriy Nicholiavich; Smirnov, Igor V.; Babain, Vasiliy A.; Todd, Terry A.; Brewer, Ken N.

2001-01-01

The present invention relates to solvents, and methods, for selectively extracting and recovering radionuclides, especially cesium and strontium, rare earths and actinides from liquid radioactive wastes. More specifically, the invention relates to extracting agent solvent compositions comprising complex organoboron compounds, substituted polyethylene glycols, and neutral organophosphorus compounds in a diluent. The preferred solvent comprises a chlorinated cobalt dicarbollide, diphenyl-dibutylmethylenecarbamoylphosphine oxide, PEG-400, and a diluent of phenylpolyfluoroalkyl sulfone. The invention also provides a method of using the invention extracting agents to recover cesium, strontium, rare earths and actinides from liquid radioactive waste.

Application of an automatic thermal desorption-gas chromatography-mass spectrometry system for the analysis of polycyclic aromatic hydrocarbons in airborne particulate matter.

PubMed

Gil-Moltó, J; Varea, M; Galindo, N; Crespo, J

2009-02-27

The application of the thermal desorption (TD) method coupled with gas chromatography-mass spectrometry (GC-MS) to the analysis of aerosol organics has been the focus of many studies in recent years. This technique overcomes the main drawbacks of the solvent extraction approach such as the use of large amounts of toxic organic solvents and long and laborious extraction processes. In this work, the application of an automatic TD-GC-MS instrument for the determination of particle-bound polycyclic aromatic hydrocarbons (PAHs) is evaluated. This device offers the advantage of allowing the analysis of either gaseous or particulate organics without any modification. Once the thermal desorption conditions for PAH extraction were optimised, the method was verified on NIST standard reference material (SRM) 1649a urban dust, showing good linearity, reproducibility and accuracy for all target PAHs. The method has been applied to PM10 and PM2.5 samples collected on quartz fibre filters with low volume samplers, demonstrating its capability to quantify PAHs when only a small amount of sample is available.

Gold in natural water: A method of determination by solvent extraction and electrothermal atomization

USGS Publications Warehouse

McHugh, J.B.

1984-01-01

A method has been developed using electrothermal atomization to effectively determine the amount of gold in natural water within the nanogram range. The method has four basic steps: (1) evaporating a 1-L sample; (2) putting it in hydrobromic acid-bromine solution; (3) extracting the sample with methyl-isobutyl-ketone; and (4) determining the amount of gold using an atomic absorption spectrophotometer. The limit of detection is 0.001 ??g gold per liter. Results from three studies indicate, respectively, that the method is precise, effective, and free of interference. Specifically, a precision study indicates that the method has a relative standard deviation of 16-18%; a recovery study indicates that the method recovers gold at an average of 93%; and an interference study indicates that the interference effects are eliminated with solvent extraction and background correction techniques. Application of the method to water samples collected from 41 sites throughout the Western United States and Alaska shows a gold concentration range of < 0.001 to 0.036 ??g gold per liter, with an average of 0.005 ??g/L. ?? 1984.

Microwave-assisted extraction of polycyclic aromatic compounds from coal.

PubMed

Kerst, M; Andersson, J T

2001-08-01

Microwave-assisted extraction (MAE) of polycyclic aromatic compounds (PACs) from coal is shown to give the same pattern of compounds as Soxhlet extraction. MAE requires only 10 mL solvent and 10 min extraction time whereas Soxhlet uses 200 mL and takes 24 h. Although the yields were lower, dichloromethane (DCM) was preferred to pyridine, N-methyl-2-pyrrolidone (NMP), and NMP with CS2 because the pattern of the PACs is shown to be independent of solvent and DCM is a much more convenient solvent to work with.

CHLORINATED SOLVENT CONTAMINATED SOILS AND GROUNDWATER: FIELD APPLICATION OF THE SOLVENT EXTRACTION RESIDUAL BIOTREATMENT TECHNOLOGY

EPA Science Inventory

A pilot scale demonstration of the Solvent Extraction Residual Biotreatment (SERB) technology was conducted at the former Sage's Dry Cleaner site in Jacksonville, FL. The SERB technology is a treatment train approach to complete site restoration, which combines an active in situ...

Extraction and identification of cyclobutanones from irradiated cheese employing a rapid direct solvent extraction method.

PubMed

Tewfik, Ihab

2008-01-01

2-Alkylcyclobutanones (cyclobutanones) are accepted as chemical markers for irradiated foods containing lipid. However, current extraction procedures (Soxhlet-florisil chromatography) for the isolation of these markers involve a long and tedious clean-up regime prior to gas chromatography-mass spectrophotometry identification. This paper outlines an alternative isolation and clean-up method for the extraction of cyclobutanones in irradiated Camembert cheese. The newly developed direct solvent extraction method enables the efficient screening of large numbers of food samples and is not as resource intensive as the BS EN 1785:1997 method. Direct solvent extraction appears to be a simple, robust method and has the added advantage of a considerably shorter extraction time for the analysis of foods containing lipid.

A review on green trend for oil extraction using subcritical water technology and biodiesel production.

PubMed

Abdelmoez, Weal; Ashour, Eman; Naguib, Shahenaz M

2015-01-01

It became a global agenda to develop clean alternative fuels which were domestically available, environmentally acceptable and technically feasible. Thus, biodiesel was destined to make a substantial contribution to the future energy demands of the domestic and industrial economies. Utilization of the non edible vegetable oils as raw materials for biodiesel production had been handled frequently for the past few years. The oil content of these seeds could be extracted by different oil extraction methods, such as mechanical extraction, solvent extraction and by subcritical water extraction technology SWT. Among them, SWT represents a new promising green extraction method. Therefore this review covered the current used non edible oil seeds for biodiesel production as well as giving a sharp focus on the efficiency of using the SWT as a promising extraction method. In addition the advantages and the disadvantages of the different biodiesel production techniques would be covered.

Extraction of rapamycin (sirolimus) from Streptomyces rapamycinicus using ultrasound.

PubMed

More, Amol S; Gadalkar, Sagar; Rathod, Virendra K

2017-07-03

The study was designed to investigate the use of ultrasound-assisted extraction (UAE) of rapamycin (sirolimus) from bacterial strain of Streptomyces rapamycinicus NRRL 5491. To achieve the maximum extraction yield, various parameters were optimized which include S. rapamycinicus (10 g) of biomass in toluene (50 mL), temperature (20°C), acoustic intensity (35.67 W/cm 2 ), and duty cycle (40%) for 4 min extraction time with probe tip length of 0.5 cm dipped into extraction solvent from the surface. The maximum extraction yield 60.15 ± 0.01 mg/L was attained under the mentioned optimum parameters. The use of ultrasound for the extraction of rapamycin shows about twofold increase in the yield as compared to the conventional solid-liquid extraction (29.7 ± 0.2 mg/L). The study provides the effective UAE technique to produce potential value-added products.

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

PubMed

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

2012-06-01

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

Recovery of catechin compounds from Korean tea by solvent extraction.

PubMed

Row, Kyung Ho; Jin, Yinzhe

2006-03-01

Catechin compounds from Korean green tea as potential sources of anticancer and antioxidant components were target materials in this work. The methodologies of solvent extraction and partition were utilized to recover catechin compounds from green tea. The optimum experimental condition was obtained by optimizing operating factors, such as, the extraction solvent, extraction time and operating temperature. After extracting the green tea with water at 80 degrees C for 40 min, the extract was partitioned with water/chloroform, which was best suited to remove caffeine impurity from the extract. Further, the resulting extract was partitioned water/ethyl acetate to deeply purify the catechin compounds of EGC, EC, EGCG and ECG. The experimental result in this work could be extended to preparative HPLC to obtain EGCG on commercial scale.

Rapid determination of eight bioactive alkaloids in Portulaca oleracea L. by the optimal microwave extraction combined with positive-negative conversion multiple reaction monitor (+/-MRM) technology.

PubMed

Liang, Xiao; Tian, Jinlong; Li, Lingzhi; Gao, Jun; Zhang, Qingyi; Gao, Pinyi; Song, Shaojiang

2014-03-01

A rapid and reliable microwave extraction and the triple quadrupole-linear ion trap mass spectrometry method was developed and validated for the determination of eight alkaloids in Portulaca oleracea L. The optimal microwave extraction (MWE) condition was performed at 60 °C for 12 min with ethanol-water (70:30, v/v) as the extracting solvent, and the solvent to solid ratio was 30:1. The alkaloids were first detected simultaneously by electrospray ionization tandem mass spectrometry under positive-negative conversion multiple reaction monitor ((+/-)MRM) technique. With investigating three different columns, samples were separated in only 8 min on a Waters ACQUITY UPLC HSS T3 (50 × 2.1 mm(2), 1.8 μm) column using acetonitrile and formic acid-water solution as a mobile phase with a flow rate at 0.2 mL/min. All calibration curves showed good linearity (r>0.999) within the test ranges. The method developed was validated with acceptable sensitivity, intra- and inter-day precision, reproducibility, and extraction recoveries. It was successfully applied to the determination of eight alkaloids in Portulaca oleracea L. from different sources and different harvest periods. The method also provide a reference for extraction and determination of alkaloids in other complex systems. © 2013 Elsevier B.V. All rights reserved.

Prevalence of pesticides in postconsumer agrochemical polymeric packaging.

PubMed

Eras, J; Costa, J; Vilaró, F; Pelacho, A M; Canela-Garayoa, R; Martin-Closas, L

2017-02-15

Pesticide remains contained in agrochemical packaging waste are a source of uncontrolled risk for human health; they are also a quality feedstock for the plastic recycling industry. Many governments have recently started to establish laws and regulations to develop systems for recovering and recycling the polymeric packages used for pesticides. There is also a demand in having a procedure to control the suitability of the pesticide packages to be reused. We have developed a two-step operation process to assess the pesticide residues in agricultural containers made of a variety of polymeric matrices. The procedure is based on an extraction with a solvent mixture followed by UPLC-MS/MS determination. Solvents for neutral pesticides were selected considering the Hildebrand solubility (δ) of solvents and polymers together with those estimated for the pesticides. The proposed technique is effective in recovering imbibed pesticides in polymeric matrices. Also, a simplified extraction procedure has been tested to become a routine method for these wastes. We have found that in many cases a significant amount of pesticides remain into the polymeric matrix, even after a standardized cleaning; the impact of releasing these hazardous compounds into the environment is to be of further consideration. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2017-03-25

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

Bio-Oil Separation and Stabilization by Near-Critical Propane Fractionation

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

Ginosar, Daniel M.; Petkovic, Lucia M.; Agblevor, Foster A.

Bio-oils produced by thermal process are promising sources of sustainable, low greenhouse gas alternative fuels. These thermal processes are also well suited to decentralized energy production due to low capital and operating costs. Algae feedstocks for bio-oil production are of particular interest, due in part to their high-energy growth yields. Further, algae can be grown in non-arable areas in fresh, brackish, salt water, or even waste water. Unfortunately, bio-oils produced by thermal processes present significant stability challenges. These oils have complex chemical compositions, are viscous, reactive, and thermally unstable. Further, the components within the oils are difficult to separate bymore » fractional distillation. By far, the most effective separation and stabilization method has been solvent extraction. However, liquid phase extraction processes pose two main obstacles to commercialization; they require a significant amount of energy to remove and recover the solvent from the product, and they have a propensity for the solvent to become contaminated with minerals from the char and ash present in the original bio-oil. Separation and fractionation of thermally produced bio-oils using supercritical fluids (SCF) offers the advantages of liquid solvent extraction while drastically reducing energy demands and the predisposition to carry over solids into the extracted phase. SCFs are dense fluids with liquid-like solvent properties and gas-like transport properties. Further, SCF density and solvent strength can be tuned with minor adjustments in pressure, co-solvent addition, or gas anti-solvent addition. Catalytic pyrolysis oils were produced from Scenedesmus dimorphus algae using a fluid catalytic cracking catalyst. Bio-oil produced from catalytic fast pyrolysis (CFP) was separated using critical fluids. Propane extraction was performed at 65 °C at a fluid reduced pressure of 2.0 (85 bar) using an eight to one solvent to feed ratio by weight. Extraction of catalytic fast pyrolysis oil with near critical propane produced an oil extract that was physically and chemically different from and more stable than the original oil. The propane extract displayed lower viscosity and lower average molecular weight. The species present in the propane extract were likely the less polar that would be expected from using a non-polar solvent (propane). Carbonyl containing species in the extract were likely ketones and esters. The raffinate contained a higher amnount of OH bonded species along with the more polar more polar acids, amides, and alcohols. The higher concentration of nitrogen in the raffinate may confirm the presence of amides. Viscosity of the propane extract increased only half as much as that of the CFP bio-oil. Further, In situ NMR aging studies showed that the propane extract was more stable than the raw oil. In conclusion, propane extraction is a promising method to decrease the nitrogen content of bio-oils and to improve the stability of bio-oils obtained by the catalytic pyrolysis of algae based biomass.« less

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

PubMed

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

2011-11-01

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

Determination of terpenoid content in pine by organic solvent extraction and fast-GC analysis

DOE PAGES

Harman-Ware, Anne E.; Sykes, Robert; Peter, Gary F.; ...

2016-01-25

Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts frommore » the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. In conclusion, diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.« less

Fast automated dual-syringe based dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

PubMed

Guo, Liang; Tan, Shufang; Li, Xiao; Lee, Hian Kee

2016-03-18

An automated procedure, combining low density solvent based solvent demulsification dispersive liquid-liquid microextraction (DLLME) with gas chromatography-mass spectrometry analysis, was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Capitalizing on a two-rail commercial autosampler, fast solvent transfer using a large volume syringe dedicated to the DLLME process, and convenient extract collection using a small volume microsyringe for better GC performance were enabled. Extraction parameters including the type and volume of extraction solvent, the type and volume of dispersive solvent and demulsification solvent, extraction and demulsification time, and the speed of solvent injection were investigated and optimized. Under the optimized conditions, the linearity ranged from 0.1 to 50 μg/L, 0.2 to 50 μg/L, and 0.5 to 50 μg/L, depending on the analytes. Limits of detection were determined to be between 0.023 and 0.058 μg/L. The method was applied to determine PAHs in environmental water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Automation of static and dynamic non-dispersive liquid phase microextraction. Part 2: Approaches based on impregnated membranes and porous supports.

PubMed

Alexovič, Michal; Horstkotte, Burkhard; Solich, Petr; Sabo, Ján

2016-02-11

A critical overview on automation of modern liquid phase microextraction (LPME) approaches based on the liquid impregnation of porous sorbents and membranes is presented. It is the continuation of part 1, in which non-dispersive LPME techniques based on the use of the extraction phase (EP) in the form of drop, plug, film, or microflow have been surveyed. Compared to the approaches described in part 1, porous materials provide an improved support for the EP. Simultaneously they allow to enlarge its contact surface and to reduce the risk of loss by incident flow or by components of surrounding matrix. Solvent-impregnated membranes or hollow fibres are further ideally suited for analyte extraction with simultaneous or subsequent back-extraction. Their use can therefore improve the procedure robustness and reproducibility as well as it "opens the door" to the new operation modes and fields of application. However, additional work and time are required for membrane replacement and renewed impregnation. Automation of porous support-based and membrane-based approaches plays an important role in the achievement of better reliability, rapidness, and reproducibility compared to manual assays. Automated renewal of the extraction solvent and coupling of sample pretreatment with the detection instrumentation can be named as examples. The different LPME methodologies using impregnated membranes and porous supports for the extraction phase and the different strategies of their automation, and their analytical applications are comprehensively described and discussed in this part. Finally, an outlook on future demands and perspectives of LPME techniques from both parts as a promising area in the field of sample pretreatment is given. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Intensification of marrubiin concentration by optimization of microwave-assisted (low CO2 yielding) extraction process for Marrubium vulgare using central composite design and antioxidant evaluation.

PubMed

Mittal, Vineet; Nanda, Arun

2017-12-01

Marrubium vulgare Linn (Lamiaceae) was generally extracted by conventional methods with low yield of marrubiin; these processes were not considered environment friendly. This study extracts the whole plant of M. vulgare by microwave assisted extraction (MAE) and optimizes the effect of various extraction parameters on the marrubiin yield by using Central Composite Design (CCD). The selected medicinal plant was extracted using ethanol: water (1:1) as solvent by MAE. The plant material was also extracted using a Soxhlet and the various extracts were analyzed by HPTLC to quantify the marrubiin concentration. The optimized conditions for the microwave-assisted extraction of selected medicinal plant was microwave power of 539 W, irradiation time of 373 s and solvent to drug ratio, 32 mL per g of the drug. The marrubiin concentration in MAE almost doubled relative to the traditional method (0.69 ± 0.08 to 1.35 ± 0.04%). The IC 50 for DPPH was reduced to 66.28 ± 0.6 μg/mL as compared to conventional extract (84.14 ± 0.7 μg/mL). The scanning electron micrographs of the treated and untreated drug samples further support the results. The CCD can be successfully applied to optimize the extraction parameters (MAE) for M. vulgare. Moreover, in terms of environmental impact, the MAE technique could be assumed as a 'Green approach' because the MAE approach for extraction of plant released only 92.3 g of CO 2 as compared to 3207.6 g CO 2 using the Soxhlet method of extraction.

SOLVENT EXTRACTION PROCESSES: A SURVEY OF SYSTEMS IN THE SITE PROGRAM

EPA Science Inventory

Solvent extraction of contaminated soils, sludges and sediments has been successfully completed at a number ofSuperfund sites. Each commercialized process uses a unique operating system to extract organic contaminants from solids. These operating systems may be classified by the ...

Effective recovery of poly-β-hydroxybutyrate (PHB) biopolymer from Cupriavidus necator using a novel and environmentally friendly solvent system.

PubMed

Fei, Tao; Cazeneuve, Stacy; Wen, Zhiyou; Wu, Lei; Wang, Tong

2016-05-01

This work demonstrates a significant advance in bioprocessing for a high-melting lipid polymer. A novel and environmental friendly solvent mixture, acetone/ethanol/propylene carbonate (A/E/P, 1:1:1 v/v/v) was identified for extracting poly-hydroxybutyrate (PHB), a high-value biopolymer, from Cupriavidus necator. A set of solubility curves of PHB in various solvents was established. PHB recovery of 85% and purity of 92% were obtained from defatted dry biomass (DDB) using A/E/P. This solvent mixture is compatible with water, and from non-defatted wet biomass, PHB recovery of 83% and purity of 90% were achieved. Water and hexane were evaluated as anti-solvents to assist PHB precipitation, and hexane improved recovery of PHB from biomass to 92% and the purity to 93%. A scale-up extraction and separation reactor was designed, built and successfully tested. Properties of PHB recovered were not significantly affected by the extraction solvent and conditions, as shown by average molecular weight (1.4 × 10(6) ) and melting point (175.2°C) not being different from PHB extracted using chloroform. Therefore, this biorenewable solvent system was effective and versatile for extracting PHB biopolymers. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:678-685, 2016. © 2016 American Institute of Chemical Engineers.

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

PubMed

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

2017-09-01

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

Comparative Analysis of the Properties of Acid-Base Indicator of Rose (Rosa setigera), Allamanda (Allamanda cathartica), and Hibiscus (Hibiscus rosa-sinensis) Flowers

PubMed Central

Okoduwa, Stanley I. R.; Mbora, Lovina O.; Adu, Matthew E.; Adeyi, Ameh A.

2015-01-01

The need to develop effective alternative for synthetic indicators is the demand of present-day chemistry. The acid-base indicator properties of Rose (Rosa setigera), Allamanda (Allamanda cathartica), and Hibiscus (Hibiscus rosa-sinensis) flowers were examined. Colour pigments were extracted from the flowers via cold and solvent extraction using soxhlet extractor. The pH value of the extracts with wavelengths of absorption was determined using ultraviolet spectrophotometer. From the results obtained, all the extracts exhibited sharp contrast between their colours in acid and base. Their pH was found to be 5.5 for cold extract of Rose and 5.6 for solvent extraction, 5.24 for cold extract of a Hibiscus and 6.52 for solvent extraction, 5.35 for cold extract of Allamanda, and 5.45 for solvent extraction. The maximum wavelengths of absorption obtained for all the extract fall within the visible region of electromagnetic spectrum. These values are almost similar to that obtained from synthetic indicators. It is on these bases that we concluded that natural indicators could be an excellent replacement for synthetic indicators since they are cheap, readily available, simple to extract, not toxic, user and environmentally friendly. PMID:26819757

Microemulsion-based lycopene extraction: Effect of surfactants, co-surfactants and pretreatments.

PubMed

Amiri-Rigi, Atefeh; Abbasi, Soleiman

2016-04-15

Lycopene is a potent antioxidant that has received extensive attention recently. Due to the challenges encountered with current methods of lycopene extraction using hazardous solvents, industry calls for a greener, safer and more efficient process. The main purpose of present study was application of microemulsion technique to extract lycopene from tomato pomace. In this respect, the effect of eight different surfactants, four different co-surfactants, and ultrasound and enzyme pretreatments on lycopene extraction efficiency was examined. Experimental results revealed that application of combined ultrasound and enzyme pretreatments, saponin as a natural surfactant, and glycerol as a co-surfactant, in the bicontinuous region of microemulsion was the optimal experimental conditions resulting in a microemulsion containing 409.68±0.68 μg/glycopene. The high lycopene concentration achieved, indicates that microemulsion technique, using a low-cost natural surfactant could be promising for a simple and safe separation of lycopene from tomato pomace and possibly from tomato industrial wastes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Determination of Organophosphorus Pesticides in Soil by Dispersive Liquid–Liquid Microextraction and Gas Chromatography

PubMed Central

Yang, Zhonghua; Liu, Yu; Liu, Donghui; Zhou, Zhiqiang

2012-01-01

In this article, a rapid and sensitive sample pretreatment technique for the determination of organophosphorus pesticides (OPPs) in soil samples is developed by using dispersive liquid–liquid microextraction (DLLME) combined with gas chromatography–flame photometric detection. Experimental conditions, including the kind of extraction and disperser solvent and their volumes, the extraction time, and the salt addition, are investigated, and the following experiment factors are used: 20 µL chlorobenzene as the extraction solvent; 1.0 mL acetonitrile as the disperser solvent; no addition of salt; and an extraction time of 1 min. Under the optimum conditions, the linearities for the three target OPPs (ethoprophos, chlorpyriphos, and profenofos) are obtained by five points in the concentration range of 2.5–1500 µg/kg, and three replicates are used for each point. Correlation coefficients vary from 0.9987 to 0.9997. The repeatability is tested by spiking soil samples at a concentration level of 5.0 µg/kg. The relative standard deviation (n = 3) varied between 2.0% and 6.6%. The limits of detection, based on a signal-to-noise ratio (S/N) of 3, range from 200 to 500 pg/g. This method is applied to the analysis of the spiked samples S1, S2, and S3, which are collected from the China Agriculture University's orchard, lawn, and garden, respectively. The recoveries for each target analyte are in the range between 87.9% and 108.0%, 87.4% and 108.0%, and 86.7% and 107.2%, respectively. PMID:22291051

Maximizing Lipid Yield in Neochloris oleoabundans Algae Extraction by Stressing and Using Multiple Extraction Stages with N-Ethylbutylamine as Switchable Solvent

PubMed Central

2017-01-01

The extraction yield of lipids from nonbroken Neochloris oleoabundans was maximized by using multiple extraction stages and using stressed algae. Experimental parameters that affect the extraction were investigated. The study showed that with wet algae (at least) 18 h extraction time was required for maximum yield at room temperature and a solvent/feed ratio of 1:1 (w/w). For fresh water (FW), nonstressed, nonbroken Neochloris oleoabundans, 13.1 wt % of lipid extraction yield (based on dry algae mass) was achieved, which could be improved to 61.3 wt % for FW stressed algae after four extractions, illustrating that a combination of stressing the algae and applying the solvent N-ethylbutylamine in multiple stages of extraction results in almost 5 times higher yield and is very promising for further development of energy-efficient lipid extraction technology targeting nonbroken wet microalgae. PMID:28781427

LPS-induced NO inhibition and antioxidant activities of ethanol extracts and their solvent partitioned fractions from four brown seaweeds

NASA Astrophysics Data System (ADS)

Cho, Myoung Lae; Lee, Dong-Jin; Lee, Hyi-Seung; Lee, Yeon-Ju; You, Sang Guan

2013-12-01

The nitric oxide inhibitory (NOI) and antioxidant (ABTS and DPPH radical scavenging effects with reducing power) activities of the ethanol (EtOH) extracts and solvent partitioned fractions from Scytosiphon lomentaria, Chorda filum, Agarum cribrosum, and Desmarestia viridis were investigated, and the correlation between biological activity and total phenolic (TP) and phlorotannin (TPT) content was determined by PCA analysis. The yield of EtOH extracts from four brown seaweeds ranged from 2.6 to 6.6% with the highest yield from D. viridis, and the predominant compounds in their solvent partitioned fractions had medium and/or less polarity. The TP and TPT content of the EtOH extracts were in the ranges of 25.0-44.1 mg GAE/g sample and 0.2-4.6 mg PG/g sample, respectively, which were mostly included in the organic solvent partitioned fractions. Strong NOI activity was observed in the EtOH extracts and their solvent partitioned fractions from D. viridis and C. filum. In addition, the EtOH extract and its solvent partitioned fractions of D. viridis exhibited little cytotoxicity to Raw 264.7 cells. The most potent ABTS and DPPH radical scavenging capacity was shown in the EtOH extracts and their solvent partitioned fractions from S. lomentaria and C. filum, and both also exhibited strong reducing ability. In the PCA analysis the content of TPT had a good correlation with DPPH ( r = 0.62), ABTS ( r = 0.69) and reducing power ( r = 0.65), however, an unfair correlation was observed between the contents of TP and TPT and NOI, suggesting that the phlorotannins might be responsible for the DPPH and ABTS radical scavenging activities.

Use of solvent mixtures for total lipid extraction of Chlorella vulgaris and gas chromatography FAME analysis.

PubMed

Moradi-Kheibari, Narges; Ahmadzadeh, Hossein; Hosseini, Majid

2017-09-01

Lipid extraction is the bottleneck step for algae-based biodiesel production. Herein, 12 solvent mixture systems (mixtures of three non-polar and two polar organic solvents) were examined to evaluate their effects on the total lipid yield from Chlorella vulgaris (C. vulgaris). Moreover, the extraction yields of three solvent systems with maximum extraction efficiency of esterifiable lipids were determined by acidic transesterification and GC-FID analysis. Three solvent systems, which resulted in a higher extraction yield, were further subjected to fatty acid methyl ester (FAME) analysis. The total lipid extraction yields (based on dry biomass) were (38.57 ± 1.51), (25.33 ± 0.58), and (25.17 ± 1.14) %, for chloroform-methanol (1:2) (C1M2), hexane-methanol (1:2) (H1M2), and chloroform-methanol (2:1) (C2M1), respectively. The extraction efficiency of C1M2 was approximately 1.5 times higher than H1M2 and C2M1, whereas the FAME profile of extracted lipids by H1M2 and C1M2 were almost identical. Moreover, the esterifiable lipid extraction yields of (18.14 ± 2.60), (16.66 ± 0.35), and (13.22 ± 0.31) % (based on dry biomass) were obtained for C1M2, H1M2, and C2M1 solvent mixture systems, respectively. The biodiesel fuel properties produced from C. vulgaris were empirically predicted and compared to that of the EN 14214 and ASTM 6751 standard specifications.

A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

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

Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani

Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

DOE PAGES

Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani; ...

2017-07-11

Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

Impact of quality parameters on the recovery of putrescine and cadaverine in fish using methanol-hydrochloric acid solvent extraction.

PubMed

Richard, Nicole L; Pivarnik, Lori F; Ellis, P Christopher; Lee, Chong M

2011-01-01

Methanol (MeOH) extraction by AOAC Official Method 996.07 has resulted in low amine recoveries in fresh fish tissue. Addition of 25% 0.4 M HCl to the 75% methanol-water extraction solvent resulted in higher recoveries of putrescine and cadaverine. Average putrescine recovery increased from 55 to 92% in flounder, scup, bluefish, and salmon; from 92 to 98% in mackerel; and from 83 to 107% in processed mackerel. Average cadaverine recovery increased from 57 to 95% in flounder, scup, bluefish, and salmon; from 91 to 97% in mackerel; and from 92 to 108% in processed mackerel. Fish stored on ice for 12 days also showed differences between background concentrations determined with the two solvents. However, the values decreased with storage time, indicating that degradation of the protein matrix may cause more comparable measurements between the two solvents. However, consistently higher putrescine and cadaverine measurements were determined using MeOH-HCl. Although significant differences in the extraction of amines from the high-fat fish tissue were not seen between MeOH and MeOH-HCl, it would be ideal to have one solvent for biogenic amine extraction. This study confirms that MeOH-HCl is a better solvent for complete extraction and recovery of putrescine and cadaverine in fresh and processed fish tissues.

Trace elements retained in washed nuclear fuel reprocessing solvents

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

Gray, L.W.; MacMurdo, K.W.

1979-09-01

Analysis of purified TBP extractant from solvent extraction processes at Savannah River Plant showed several stable elements and several long-lived radioisotopes. Stable elements Al, Na, Br, Ce, Hg, and Sm are found in trace quantities in the solvent. The only stable metallic element consistently found in the solvent was Al, with a concentration which varies from about 30 ppM to about 10 ppM. The halogens Br and Cl appear to be found in the solvent systems as organo halides. Radionuclides found were principally /sup 106/Ru, /sup 129/I, /sup 3/H, /sup 235/U, and /sup 239/Pu. The /sup 129/I concentration was aboutmore » 1 ppM in the first solvent extraction cycle of each facility. In the other cycles, /sup 129/I concentration varied from about 0.1 to 0.5 ppM. Both /sup 129/I and /sup 3/H appear to be in the organic solvent as a result of exchange with hydrogen.« less

Deep Eutectic Solvent-Based Microwave-Assisted Method for Extraction of Hydrophilic and Hydrophobic Components from Radix Salviae miltiorrhizae.

PubMed

Chen, Jue; Liu, Mengjun; Wang, Qi; Du, Huizhi; Zhang, Liwei

2016-10-17

Deep eutectic solvents (DESs) have attracted significant attention as a promising green media. In this work, twenty-five kinds of benign choline chloride-based DESs with microwave-assisted methods were applied to quickly extract active components from Radix Salviae miltiorrhizae . The extraction factors, including temperature, time, power of microwave, and solid/liquid ratio, were investigated systematically by response surface methodology. The hydrophilic and hydrophobic ingredients were extracted simultaneously under the optimized conditions: 20 vol% of water in choline chloride/1,2-propanediol (1:1, molar ratio) as solvent, microwave power of 800 W, temperature at 70 °C, time at 11.11 min, and solid/liquid ratio of 0.007 g·mL -1 . The extraction yield was comparable to, or even better than, conventional methods with organic solvents. The microstructure alteration of samples before and after extraction was also investigated. The method validation was tested as the linearity of analytes ( r ² > 0.9997 over two orders of magnitude), precision (intra-day relative standard deviation (RSD) < 2.49 and inter-day RSD < 2.96), and accuracy (recoveries ranging from 95.04% to 99.93%). The proposed DESs combined with the microwave-assisted method provided a prominent advantage for fast and efficient extraction of active components, and DESs could be extended as solvents to extract and analyze complex environmental and pharmaceutical samples.

Application of enzyme-linked immunosorbent assay for measurement of polychlorinated biphenyls from hydrophobic solutions: Extracts of fish and dialysates of semipermeable membrane devices: Chapter 26

USGS Publications Warehouse

Zajicek, James L.; Tillitt, Donald E.; Huckins, James N.; Petty, Jimmie D.; Potts, Michael E.; Nardone, David A.

1996-01-01

Determination of PCBs in biological tissue extracts by enzyme-linked immunosorbent assays (ELISAs) can be problematic, since the hydrophobic solvents used for their extraction and isolation from interfering biochemicals have limited compatibility with the polar solvents (e.g. methanol/water) and the immunochemical reagents used in ELISA. Our studies of these solvent effects indicate that significant errors can occur when microliter volumes of PCB containing extracts, in hydrophobic solvents, are diluted directly into methanol/water diluents. Errors include low recovery and excess variability among sub-samples taken from the same sample dilution. These errors are associated with inhomogeneity of the dilution, which is readily visualized by the use of a hydrophobic dye, Solvent Blue 35. Solvent Blue 35 is also used to visualize the evaporative removal of hydrophobic solvent and the dissolution of the resulting PCB/dye residue by pure methanol and 50% (v/v) methanol/water, typical ELISA diluents. Evaporative removal of isooctane by an ambient temperature nitrogen purge with subsequent dissolution in 100% methanol gives near quantitative recovery of model PCB congeners. We also compare concentrations of total PCBs from ELISA (ePCB) to their corresponding concentrations determined from capillary gas chromatography (GC) in selected fish sample extracts and dialysates of semipermeable membrane device (SPMD) passive samplers using an optimized solvent exchange procedure. Based on Aroclor 1254 calibrations, ePCBs (ng/mL) determined in fish extracts are positively correlated with total PCB concentrations (ng/mL) determined by GC: ePCB = 1.16 * total-cPCB - 5.92. Measured ePCBs (ng/3 SPMDs) were also positively correlated (r2 = 0.999) with PCB totals (ng/3 SPMDs) measured by GC for dialysates of SPMDs: ePCB = 1.52 * total PCB - 212. Therefore, this ELISA system for PCBs can be a rapid alternative to traditional GC analyses for determination of PCBs in extracts of biota or in SPMD dialysates.