Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

PubMed

Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

2015-09-01

In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electro-driven extraction of inorganic anions from water samples and water miscible organic solvents and analysis by ion chromatography.

PubMed

Nojavan, Saeed; Bidarmanesh, Tina; Memarzadeh, Farkhondeh; Chalavi, Soheila

2014-09-01

A simple electromembrane extraction (EME) procedure combined with ion chromatography (IC) was developed to quantify inorganic anions in different pure water samples and water miscible organic solvents. The parameters affecting extraction performance, such as supported liquid membrane (SLM) solvent, extraction time, pH of donor and acceptor solutions, and extraction voltage were optimized. The optimized EME conditions were as follows: 1-heptanol was used as the SLM solvent, the extraction time was 10 min, pHs of the acceptor and donor solutions were 10 and 7, respectively, and the extraction voltage was 15 V. The mobile phase used for IC was a combination of 1.8 mM sodium carbonate and 1.7 mM sodium bicarbonate. Under these optimized conditions, all anions had enrichment factors ranging from 67 to 117 with RSDs between 7.3 and 13.5% (n = 5). Good linearity values ranging from 2 to 1200 ng/mL with coefficients of determination (R(2) ) between 0.987 and 0.999 were obtained. The LODs of the EME-IC method ranged from 0.6 to 7.5 ng/mL. The developed method was applied to different samples to evaluate the feasibility of the method for real applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Deep eutectic solvent based gas-assisted dispersive liquid-phase microextraction combined with gas chromatography and flame ionization detection for the determination of some pesticide residues in fruit and vegetable samples.

PubMed

Farajzadeh, Mir Ali; Sattari Dabbagh, Masoumeh; Yadeghari, Adeleh

2017-05-01

In this study, a gas-assisted dispersive liquid-phase microextraction method using a deep eutectic solvent as the extraction solvent combined with gas chromatography and flame ionization detection was developed for the extraction and determination of some pesticide residues in vegetable and fruit juice samples. In this method, choline chloride and 4-chlorophenol at a molar ratio of 1:2 were mixed. By heating and vortexing, a clear, water-immiscible, and homogeneous liquid was formed. The obtained deep eutectic solvent was added to an aqueous solution of the analytes in a conical test tube. Air was bubbled into the aqueous solution and a cloudy solution was obtained. During this step, the analytes were extracted into the fine droplets of the extraction solvent. After centrifugation, an aliquot of the settled phase was injected into the separation system. Under the optimum extraction conditions, enrichment factors, and extraction recoveries were obtained in the ranges of 247-355 and 49-71%, respectively. The obtained values for the limits of detection and quantification were in the ranges of 0.24-1.4 and 0.71-4.2 μg/L, respectively. The proposed method is simple, fast, efficient, and inexpensive. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A RAPID AND SIMPLE PHOSPHOLIPASE A ASSAY,

DTIC Science & Technology

A simple and rapid method for the assay of phospholipase A was developed. As a substrate fresh egg yolk is used which is hydrolyzed by snake venom...phospholipase A at a 10-20 x faster rate than pure lecithin . The released fatty acids, after extraction with appropriate solvents are titrated

Lipid Extraction and Cholesterol Quantification: A Simple Protocol

ERIC Educational Resources Information Center

Barreto, M. Carmo

2005-01-01

Enzymatic methods are used to measure cholesterol levels but a simple and inexpensive method is described, which is particularly important when one has repeated lab sessions during the week. It can be carried out on the organic phase containing the lipids, without evaporating the solvent, yielding quick results.

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.

Application of solvent floatation to separation and determination of triazine herbicides in honey by high-performance liquid chromatography.

PubMed

Wang, Kun; Jiang, Jia; Lv, Xinping; Zang, Shuang; Tian, Sizhu; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei; Yu, Yong

2018-03-01

Based on the foaming property of the honey, a rapid, simple, and effective method solvent floatation (SF) was developed and firstly applied to the extraction and separation of triazine herbicides in honey. The analytes were determined by high-performance liquid chromatography. Some parameters affecting the extraction efficiencies, such as the type and volume of extraction solvent, type of salt, amount of (NH 4 ) 2 SO 4 , pH value of sample solution, gas flow rate, and floatation time, were investigated and optimized. The limits of detection for analytes are in the range of 0.16-0.56 μg kg -1 . The recoveries and relative standard deviations for determining triazines in five real honey samples are in the range of 78.2-112.9 and 0.2-9.2%, respectively.

Normal and Reversed-Phase Thin Layer Chromatography of Green Leaf Extracts

ERIC Educational Resources Information Center

Sjursnes, Birte Johanne; Kvittingen, Lise; Schmid, Rudolf

2015-01-01

Introductory experiments of chromatography are often conducted by separating colored samples, such as inks, dyes, and plant extracts, using filter paper, chalk, or thin layer chromatography (TLC) plates with various solvent systems. Many simple experiments have been reported. The relationship between normal chromatography and reversed-phase…

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.

[Extraction of 10-Deacetyl Baccatin by Supercritical CO2 from Taxus yunnanensis Branches and Leaves].

PubMed

Tang, Yang-qin; Li, Hai-chi; Huang, Wen-jie; Xiong, Yan; Ge, Fa-huan

2015-04-01

To study the supercritical CO2 fluids extraction (SFE) method to extract the components from Taxus yunnanensis. Medicinal meterials were extracted by supercritical CO2, and then purified by industrial chromatography. Using the extraction yield of 10-DAB as the index,single factor test was carried out to investigate the effect of co-solvent, extraction time, extraction pressure, extraction temperature, pressure and temperature of separation kettle I. Then orthogonal experiment was used to optimize the best extraction condition. The suitable extraction condition was as follows: the ratio of co-solvent (80% ethanol) amount and the madicinal materials was 3: 1, Separation kettle I pressure was 14 MPa, separation kettle I temperature was 40 °C, extraction pressure was 25 MPa, extraction temperature was 60 T and extraction time was 90 min. The extract was separated by industrial chromatographic and then crystallized. The supercritical CO2 extraction and purification process of 10-DAB were simple and feasible.

A Novel Selective Deep Eutectic Solvent Extraction Method for Versatile Determination of Copper in Sediment Samples by ICP-OES.

PubMed

Bağda, Esra; Altundağ, Huseyin; Tüzen, Mustafa; Soylak, Mustafa

2017-08-01

In the present study, a simple, mono step deep eutectic solvent (DES) extraction was developed for selective extraction of copper from sediment samples. The optimization of all experimental parameters, e.g. DES type, sample/DES ratio, contact time and temperature were performed with using BCR-280 R (lake sediment certified reference material). The limit of detection (LOD) and the limit of quantification (LOQ) were found as 1.2 and 3.97 µg L -1 , respectively. The RSD of the procedure was 7.5%. The proposed extraction method was applied to river and lake sediments sampled from Serpincik, Çeltek, Kızılırmak (Fadl and Tecer region of the river), Sivas-Turkey.

Direct quantification of lipopeptide biosurfactants in biological samples via HPLC and UPLC-MS requires sample modification with an organic solvent.

PubMed

Biniarz, Piotr; Łukaszewicz, Marcin

2017-06-01

The rapid and accurate quantification of biosurfactants in biological samples is challenging. In contrast to the orcinol method for rhamnolipids, no simple biochemical method is available for the rapid quantification of lipopeptides. Various liquid chromatography (LC) methods are promising tools for relatively fast and exact quantification of lipopeptides. Here, we report strategies for the quantification of the lipopeptides pseudofactin and surfactin in bacterial cultures using different high- (HPLC) and ultra-performance liquid chromatography (UPLC) systems. We tested three strategies for sample pretreatment prior to LC analysis. In direct analysis (DA), bacterial cultures were injected directly and analyzed via LC. As a modification, we diluted the samples with methanol and detected an increase in lipopeptide recovery in the presence of methanol. Therefore, we suggest this simple modification as a tool for increasing the accuracy of LC methods. We also tested freeze-drying followed by solvent extraction (FDSE) as an alternative for the analysis of "heavy" samples. In FDSE, the bacterial cultures were freeze-dried, and the resulting powder was extracted with different solvents. Then, the organic extracts were analyzed via LC. Here, we determined the influence of the extracting solvent on lipopeptide recovery. HPLC methods allowed us to quantify pseudofactin and surfactin with run times of 15 and 20 min per sample, respectively, whereas UPLC quantification was as fast as 4 and 5.5 min per sample, respectively. Our methods provide highly accurate measurements and high recovery levels for lipopeptides. At the same time, UPLC-MS provides the possibility to identify lipopeptides and their structural isoforms.

Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography.

PubMed

Tejada-Casado, Carmen; Del Olmo-Iruela, Monsalud; García-Campaña, Ana M; Lara, Francisco J

2018-08-01

A green and simple multiresidue method using capillary liquid chromatography (CLC) with UV-diode array detection (DAD) has been developed for the determination of sixteen benzimidazoles (BZs) and its metabolites in milk samples. The separation was achieved in <32 min, using a Zorbax XDB-C18 column (150 mm × 0.5 mm I.D, 5 μm), with a mobile phase consisting of 50 mM ammonium acetate (solvent A) and a mixture of acetonitrile/methanol (1:1 v/v) (solvent B), at a flow rate of 9 μL min -1 . The temperature of the column was 20 °C and 6 μL of sample were injected. In spite of the complexity of milk samples, an effective, simple and fast sample preparation method called salting out-assisted liquid-liquid extraction (SALLE) was developed for the analysis of these compounds in cow milk samples. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt. Good linearity was obtained (R 2  > 0.9985 for all BZs) with limits of detection (LOD) between 1.0 and 2.8 μg kg -1 . Relative standard deviations of repeatability and intermediate precision were below 1.6 and 14.2%, respectively. Satisfactory recoveries between 79.1 and 99.6% were also obtained for three types of milk samples (cow, sheep and goat). The advantages of a miniaturized technique such as CLC in terms of better efficiencies and reduced solvent consumption, combined with the simplicity of the SALLE procedure, make this method a useful alternative for the monitoring of these residues at trace level. Copyright © 2018 Elsevier B.V. All rights reserved.

Solvent extraction employing a static micromixer: a simple, robust and versatile technology for the microencapsulation of proteins.

PubMed

Freitas, S; Walz, A; Merkle, H P; Gander, B

2003-01-01

The potential of a static micromixer for the production of protein-loaded biodegradable polymeric microspheres by a modified solvent extraction process was examined. The mixer consists of an array of microchannels and features a simple set-up, consumes only very small space, lacks moving parts and offers simple control of the microsphere size. Scale-up from lab bench to industrial production is easily feasible through parallel installation of a sufficient number of micromixers ('number-up'). Poly(lactic-co-glycolic acid) microspheres loaded with a model protein, bovine serum albumin (BSA), were prepared. The influence of various process and formulation parameters on the characteristics of the microspheres was examined with special focus on particle size distribution. Microspheres with monomodal size distributions having mean diameters of 5-30 micro m were produced with excellent reproducibility. Particle size distributions were largely unaffected by polymer solution concentration, polymer type and nominal BSA load, but depended on the polymer solvent. Moreover, particle mean diameters could be varied in a considerable range by modulating the flow rates of the mixed fluids. BSA encapsulation efficiencies were mostly in the region of 75-85% and product yields ranged from 90-100%. Because of its simple set-up and its suitability for continuous production, static micromixing is suggested for the automated and aseptic production of protein-loaded microspheres.

Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

PubMed Central

Çabuk, Hasan; Köktürk, Mustafa

2013-01-01

A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

Novel approaches mediated by tailor-made green solvents for the extraction of phenolic compounds from agro-food industrial by-products.

PubMed

Fernández, María de Los Ángeles; Espino, Magdalena; Gomez, Federico J V; Silva, María Fernanda

2018-01-15

An environmentally friendly method for the phenolic compound extraction from agro-food industrial by-products was developed in order to contribute with their sustainable valorization. A Natural Deep Eutectic Solvent was chemometrically-designed for the first time and compared with traditional solvents in terms of analyte stabilization. The combination of lactic acid, glucose and 15% water (LGH-15) was selected as optimal. A high-efficiency ultrasound-assisted extraction mediated by LGH-15 prior to HPLC-DAD allows the determination of 14 phenols in onion, olive, tomato and pear industrial by-products. NADES synthesis as well as the extraction procedures were optimized by Response Surface Methodology. Thus, phenolic determination in these complex samples was achieved by a simple, non-expensive, eco-friendly and robust system. The application to different matrices demonstrated the versatility of the proposed method. NADES opens interesting perspectives for their potential use as vehicles of bioactive compounds as food additives or pharmaceuticals. Copyright © 2017 Elsevier Ltd. All rights reserved.

Revisiting History: Encountering Iodine Then and Now--A General Chemistry Laboratory to Observe Iodine from Seaweed

ERIC Educational Resources Information Center

Wahab, M. Farooq

2009-01-01

The history of the discovery of iodine is retold using brown-colored seaweed found commonly along the ocean shore. The seaweed is ashed at a low temperature and the iodides are extracted into boiling water. The iodides are oxidized in acidic medium. Solvent extraction of iodine by oxidation of iodides as well as simple aqueous extraction of iodide…

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.

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.

The loss of essential oil components induced by the Purge Time in the Pressurized Liquid Extraction (PLE) procedure of Cupressus sempervirens.

PubMed

Dawidowicz, Andrzej L; Czapczyńska, Natalia B; Wianowska, Dorota

2012-05-30

The influence of different Purge Times on the effectiveness of Pressurized Liquid Extraction (PLE) of volatile oil components from cypress plant matrix (Cupressus sempervirens) was investigated, applying solvents of diverse extraction efficiencies. The obtained results show the decrease of the mass yields of essential oil components as a result of increased Purge Time. The loss of extracted components depends on the extrahent type - the greatest mass yield loss occurred in the case of non-polar solvents, whereas the smallest was found in polar extracts. Comparisons of the PLE method with Sea Sand Disruption Method (SSDM), Matrix Solid-Phase Dispersion Method (MSPD) and Steam Distillation (SD) were performed to assess the method's accuracy. Independent of the solvent and Purge Time applied in the PLE process, the total mass yield was lower than the one obtained for simple, short and relatively cheap low-temperature matrix disruption procedures - MSPD and SSDM. Thus, in the case of volatile oils analysis, the application of these methods is advisable. Copyright © 2012 Elsevier B.V. All rights reserved.

Graphene-sensitized microporous membrane/solvent microextraction for the preconcentration of cinnamic acid derivatives in Rhizoma Typhonii.

PubMed

Xing, Rongrong; Hu, Shuang; Chen, Xuan; Bai, Xiaohong

2014-09-01

A novel graphene-sensitized microporous membrane/solvent microextraction method named microporous membrane/graphene/solvent synergistic microextraction, coupled with high-performance liquid chromatography and UV detection, was developed and introduced for the extraction and determination of three cinnamic acid derivatives in Rhizoma Typhonii. Several factors affecting performance were investigated and optimized, including the types of graphene and extraction solvent, concentration of graphene dispersed in octanol, sample phase pH, ionic strength, stirring rate, extraction time, extraction temperature, and sample volume. Under optimized conditions, the enrichment factors of cinnamic acid derivatives ranged from 75 to 269. Good linearities were obtained from 0.01 to 10 μg/mL for all analytes with regression coefficients between 0.9927 and 0.9994. The limits of quantification were <1 ng/mL, and satisfactory recoveries (99-104%) and precision (1.1-10.8%) were also achieved. The synergistic microextraction mechanism based on graphene sensitization was analyzed and described. The experimental results showed that the method was simple, sensitive, practical, and effective for the preconcentration and determination of cinnamic acid derivatives in Rhizoma Typhonii. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Principles of Stagewise Separation Process Calculations: A Simple Algebraic Approach Using Solvent Extraction.

ERIC Educational Resources Information Center

Crittenden, Barry D.

1991-01-01

A simple liquid-liquid equilibrium (LLE) system involving a constant partition coefficient based on solute ratios is used to develop an algebraic understanding of multistage contacting in a first-year separation processes course. This algebraic approach to the LLE system is shown to be operable for the introduction of graphical techniques…

Multiclass mycotoxin analysis in edible oils using a simple solvent extraction method and liquid chromatography with tandem mass spectrometry.

PubMed

Eom, Taeyong; Cho, Hyun-Deok; Kim, Junghyun; Park, Mihee; An, Jinyoung; Kim, Moosung; Kim, Sheen-Hee; Han, Sang Beom

2017-11-01

A simple and rapid method for the simultaneous determination of 11 mycotoxins - aflatoxins B 1 , B 2 , G 1 and G 2 ; fumonisins B 1 , B 2 and B 3 ; ochratoxin A; zearalenone; deoxynivalenol; and T-2 toxin - in edible oils was established using liquid chromatography tandem mass spectrometry (LC-MS/MS). In this study, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), QuEChERS with dispersive liquid-liquid microextraction, and solvent extraction were examined for sample preparation. Among these methods, solvent extraction with a mixture of formic acid/acetonitrile (5/95, v/v) successfully extracted all target mycotoxins. Subsequently, a defatting process using n-hexane was employed to remove the fats present in the edible oil samples. Mass spectrometry was carried out using electrospray ionisation in polarity switching mode with multiple reaction monitoring. The developed LC-MS/MS method was validated by assessing the specificity, linearity, recovery, limit of quantification (LOQ), accuracy and precision with reference to Commission Regulation (EC) 401/2006. Mycotoxin recoveries of 51.6-82.8% were achieved in addition to LOQs ranging from 0.025 ng/g to 1 ng/g. The edible oils proved to be relatively uncomplicated matrices and the developed method was applied to 9 edible oil samples, including soybean oil, corn oil and rice bran oil, to evaluate potential mycotoxin contamination. The levels of detection were significantly lower than the international regulatory standards. Therefore, we expect that our developed method, based on simple, two-step sample preparation process, will be suitable for the large-scale screening of mycotoxin contamination in edible oils.

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.

Bio-based extraction and stabilization of anthocyanins.

PubMed

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

2016-05-01

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

Direct ultrasonic agitation for rapid extraction of organic matter from airborne particulate.

PubMed

Lee, S C; Zou, S C; Ho, K F; Chan, L Y

2001-01-02

Direct ultrasonic extraction (DUE) is proposed as simple and rapid sample pretreatment method. This new approach is applied to the extraction of particulate organic matter (POM) from airborne particulate by using dichloromethane (DCM) or DCM/methanol (90/10, v/v) as extractant. The analytical determination was carried out by weighing the extractable POM on an electrobalance. Total recovery for POM could be obtained when the sample was extracted three times with 25-50 mL extractant each for about 5 min at 50 W ultrasonic power. In comparison with conventional Soxhlet extraction, less extraction time (total 15 min only) and solvent consumption (100 mL) were required by DUE. The efficiency of the DUE was similar or even higher than the routine Soxhlet method. Additionally, the new extractor is very simple and easy to use and can accelerate the extraction procedures of organic components from various solid samples.

Extraction of chemical warfare agents from water with hydrophilic-lipophilic balance and C18 cartridges: comparative study.

PubMed

Kanaujia, Pankaj K; Pardasani, Deepak; Gupta, A K; Dubey, D K

2007-01-19

Efficient extraction of chemical warfare agents (CWAs) from water is essential before subjecting them to gas chromatographic and spectral analysis aiming towards verification of the Chemical Weapons Convention (CWC). It requires development of fast, reliable, simple and reproducible sample preparation of CWAs from water which is likely to be contaminated during deliberate or inadvertent spread of CWAs. This work describes development of a solid-phase extraction method using hydrophilic-lipophilic balance (HLB) cartridges for extraction of CWAs from water. The extraction efficiencies of HLB and C18 cartridges were compared and the results revealed that HLB sorbents performed better. Extracts were analyzed by gas chromatography-mass spectrometry. Extraction parameters, such as extraction solvent, its volume and rinsing solvent were optimized. Best recoveries of target analytes were obtained using 1mL methanol and limits of detection were achieved up to 0.05microg/mL with dichloromethane. Precision of the method was found to be less than 9.2% RSD.

Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

PubMed

Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-01-01

A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

Simple method for the extraction and reversed-phase high-performance liquid chromatographic analysis of carotenoid pigments from red yeasts (Basidiomycota, Fungi).

PubMed

Weber, Roland W S; Anke, Heidrun; Davoli, Paolo

2007-03-23

A simple method for the extraction of carotenoid pigments from frozen wet cells of red yeasts (Basidiomycota) and their analysis by reversed-phase HPLC using a C(18) column and a water/acetone solvent system is described. Typical red yeast carotenoids belonging to an oxidative series from the monocyclic gamma-carotene to 2-hydroxytorularhodin and from the bicyclic beta-carotene to astaxanthin were separated. Pigment identity was confirmed by LC-atmospheric pressure chemical ionisation (APCI) mass spectrometry using similar chromatographic conditions.

In-coupled syringe assisted octanol-water partition microextraction coupled with high-performance liquid chromatography for simultaneous determination of neonicotinoid insecticide residues in honey.

PubMed

Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax

2015-07-01

A simple and fast method namely in-coupled syringe assisted octanol-water partition microextraction combined with high performance liquid chromatography (HPLC) has been developed for the extraction, preconcentration and determination of neonicotinoid insecticide residues (e.g. imidacloprid, acetamiprid, clothianidin, thiacloprid, thiamethoxam, dinotefuran, and nitenpyram) in honey. The experimental parameters affected the extraction efficiency, including kind and concentration of salt, kind of disperser solvent and its volume, kind of extraction solvent and its volume, shooting times and extraction time were investigated. The extraction process was carried out by rapid shooting of two syringes. Therefore, rapid dispersion and mass transfer processes was created between phases, and thus affects the extraction efficiency of the proposed method. The optimum extraction conditions were 10.00 mL of aqueous sample, 10% (w/v) Na2SO4, 1-octanol (100µL) as an extraction solvent, shooting 4 times and extraction time 2min. No disperser solvent and centrifugation step was necessary. Linearity was obtained within the range of 0.1-3000 ngmL(-1), with the correlation coefficients greater than 0.99. The high enrichment factor of the target analytes was 100 fold and low limit of detection (0.25-0.50 ngmL(-1)) could be obtained. This proposed method has been successfully applied in the analysis of neonicotinoid residues in honey, and good recoveries in the range of 96.93-107.70% were obtained. Copyright © 2015 Elsevier B.V. All rights reserved.

Organic solvent-free air-assisted liquid-liquid microextraction for optimized extraction of illegal azo-based dyes and their main metabolite from spices, cosmetics and human bio-fluid samples in one step.

PubMed

Barfi, Behruz; Asghari, Alireza; Rajabi, Maryam; Sabzalian, Sedigheh

2015-08-15

Air-assisted liquid-liquid microextraction (AALLME) has unique capabilities to develop as an organic solvent-free and one-step microextraction method, applying ionic-liquids as extraction solvent and avoiding centrifugation step. Herein, a novel and simple eco-friendly method, termed one-step air-assisted liquid-liquid microextraction (OS-AALLME), was developed to extract some illegal azo-based dyes (including Sudan I to IV, and Orange G) from food and cosmetic products. A series of experiments were investigated to achieve the most favorable conditions (including extraction solvent: 77μL of 1-Hexyl-3-methylimidazolium hexafluorophosphate; sample pH 6.3, without salt addition; and extraction cycles: 25 during 100s of sonication) using a central composite design strategy. Under these conditions, limits of detection, linear dynamic ranges, enrichment factors and consumptive indices were in the range of 3.9-84.8ngmL(-1), 0.013-3.1μgmL(-1), 33-39, and 0.13-0.15, respectively. The results showed that -as well as its simplicity, fastness, and use of no hazardous disperser and extraction solvents- OS-AALLME is an enough sensitive and efficient method for the extraction of these dyes from complex matrices. After optimization and validation, OS-AALLME was applied to estimate the concentration of 1-amino-2-naphthol in human bio-fluids as a main reductive metabolite of selected dyes. Levels of 1-amino-2-naphthol in plasma and urinary excretion suggested that this compound may be used as a new potential biomarker of these dyes in human body. Copyright © 2015 Elsevier B.V. All rights reserved.

Novel Fluorinated Tensioactive Extractant Combined with Flotation for Decontamination of Extractant Residual during Solvent Extraction

NASA Astrophysics Data System (ADS)

Wu, Xue; Chang, Zhidong; Liu, Yao; Choe, Chol Ryong

2017-12-01

Solvent-extraction is widely used in chemical industry. Due to the amphiphilic character, a large amount of extractant remains in water phase, which causes not only loss of reagent, but also secondary contamination in water phase. Novel fluorinated extractants with ultra-low solubility in water were regarded as effective choice to reduce extractant loss in aqueous phase. However, trace amount of extractant still remained in water. Based on the high tensioactive aptitude of fluorinated solvent, flotation was applied to separate fluorinated extractant remaining in raffinate. According to the data of surface tension measurement, the surface tension of solution was obviously decreased with the addition of fluorinated extractant tris(2,2,3,3,4,4,5,5-octafluoropentyl) phosphate (FTAP). After flotation, the FTAP dissolved in water can be removed as much as 70%, which proved the feasibility of this key idea. The effects of operation time, gas velocity, pH and salinity of bulk solution on flotation performance were discussed. The optimum operating parameters were determined as gas velocity of 12ml/min, operating time of 15min, pH of 8.7, and NaCl volume concentration of 1.5%, respectively. Moreover, adsorption process of FTAP on bubble surface was simulated by ANSYS VOF model using SIMPLE algorithm. The dynamic mechanism of flotation was also theoretically investigated, which can be considered as supplement to the experimental results.

Ligandless dispersive liquid--liquid microextraction of iron in biological and foodstuff samples and its determination by Electrothermal atomic absorption spectrometry.

PubMed

Madadizadeh, Mohadeseh; Taher, Mohammad Ali; Ashkenani, Hamid

2013-01-01

A new, simple, and efficient method comprising ligandless dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry is reported for the preconcentration and determination of ultratrace amounts of Fe(III). Carbon tetrachloride and acetone were used as the extraction and disperser solvents, respectively. Some effective parameters of the microextraction such as choice of extraction and disperser solvents, their volume, extraction time and temperature, salt and surfactant effect, and pH were optimized. Under the optimum conditions, the calibration curve was linear in the range of 0.02 to 0.46 microg/L of Fe(III), with LOD and LOQ of 5.2 and 17.4 ng/L, respectively. The RSD for seven replicated determinations of Fe(IIl) ion at 0.1 microg/L concentration level was 5.2%. Operational simplicity, rapidity, low cost, good repeatability, and low consumption of extraction solvent are the main advantages of the proposed method. The method was successfully applied to the determination of iron in biological, food, and certified reference samples.

A green ultrasonic-assisted liquid-liquid microextraction based on deep eutectic solvent for the HPLC-UV determination of ferulic, caffeic and cinnamic acid from olive, almond, sesame and cinnamon oil.

PubMed

Khezeli, Tahere; Daneshfar, Ali; Sahraei, Reza

2016-04-01

A simple, inexpensive and sensitive ultrasonic-assisted liquid-liquid microextraction method based on deep eutectic solvent (UALLME-DES) was used for the extraction of three phenolic acids (ferulic, caffeic and cinnamic) from vegetable oils. In a typical experiment, deep eutectic solvent as green extraction solvent was added to n-hexane (as a typical oil medium) containing target analytes. Subsequently, the extraction was accelerated by sonication. After the extraction, phase separation (DES rich phase/n-hexane phase) was performed by centrifugation. DES rich phase (lower phase) was withdrawn by a micro-syringe and submitted to isocratic reverse-phase HPLC with UV detection. Under optimum conditions obtained by response surface methodology (RSM) and desirability function (DF), the method has good linear calibration ranges (between 1.30 and 1000 µg L(-1)), coefficients of determination (r(2)>0.9949) and low limits of detection (between 0.39 and 0.63 µg L(-1)). This procedure was successfully applied to the determination of target analytes in olive, almond, sesame and cinnamon oil samples. The relative mean recoveries ranged from 94.7% to 104.6%. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Understanding the mechanisms of lipid extraction from microalga Chlamydomonas reinhardtii after electrical field solicitations and mechanical stress within a microfluidic device.

PubMed

Bensalem, Sakina; Lopes, Filipa; Bodénès, Pierre; Pareau, Dominique; Français, Olivier; Le Pioufle, Bruno

2018-06-01

One way envisioned to overcome part of the issues biodiesel production encounters today is to develop a simple, economically viable and eco-friendly process for the extraction of lipids from microalgae. This study investigates the lipid extraction efficiency from the microalga Chlamydomonas reinhardtii as well as the underlying mechanisms. We propose a new methodology combining a pulsed electric field (PEF) application and mechanical stresses as a pretreatment to improve lipid extraction with solvents. Cells enriched in lipids are therefore submitted to electric field pulses creating pores on the cell membrane and then subjected to a mechanical stress by applying cyclic pressures on the cell wall (using a microfluidic device). Results showed an increase in lipid extraction when cells were pretreated by the combination of both methods. Microscopic observations showed that both pretreatments affect the cell structure. Finally, the dependency of solvent lipid extraction efficiency with the cell wall structure is discussed. Copyright © 2018 Elsevier Ltd. All rights reserved.

Carbon dioxide extraction of residual chloroform from biodegradable polymers.

PubMed

Koegler, Wendy S; Patrick, Carmen; Cima, Michael J; Griffith, Linda G

2002-01-01

Biodegradable polymeric devices for drug delivery and tissue engineering are often fabricated with the use of organic solvents and may still contain significant amounts of solvent (> 1 wt%) even after aggressive vacuum drying. This excess solvent can interfere with tissue response and the mechanical properties of the devices. The aim of this article is to demonstrate that liquid CO(2) extraction can be used to reduce residual solvent in dense poly(L-lactide-co-glycolide) devices to 50 ppm relatively quickly and with minimal changes in architecture under some conditions. Two liquid CO(2) extraction systems were developed to examine the removal of residual solvents from bar-shaped PLGA devices: (1) a low-pressure (1400 psi) batch system, and (2) a high-pressure (5000 psi) continuous-flow system. Eight hours of extraction in the high-pressure system reduced residual chloroform in 3 mm thick bars below the 50-ppm target. A simple Fickian diffusion model was fit to the extraction results. Diffusion coefficients ranged from 1.10 x 10(-6) cm(2)/s to 2.64 x 10(-6) cm(2)/s. The model predicts that approximately 1 h is needed to dry 1-mm bars to chloroform levels below 50 ppm, and 7 h are needed for 3 mm thick bars. The micro- and macroarchitectures of porous PLGA scaffolds created by particulate leaching were not significantly altered by CO(2) drying if the salt used to make the pores was not removed before drying. Copyright 2002 Wiley Periodicals, Inc. J Biomed Mater Res (Appl Biomater) 63: 567-576, 2002

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.

Development of continuous dispersive liquid-liquid microextraction performed in home-made device for extraction and preconcentration of aryloxyphenoxy-propionate herbicides from aqueous samples followed by gas chromatography-flame ionization detection.

PubMed

Farajzadeh, Mir Ali; Mohebbi, Ali; Feriduni, Behruz

2016-05-12

In this study, a rapid, simple, and efficient sample preparation method based on continuous dispersive liquid-liquid microextraction has been developed for the extraction and preconcentration of aryloxyphenoxy-propionate herbicides from aqueous samples prior to their analysis by gas chromatography-flame ionization detection. In this method, two parallel glass tubes with different diameters are connected with a teflon stopcock and used as an extraction device. A mixture of disperser and extraction solvents is transferred into one side (narrow tube) of the extraction device and an aqueous phase containing the analytes is filled into the other side (wide tube). Then the stopcock is opened and the mixture of disperser and extraction solvents mixes with the aqueous phase. By this action, the extraction solvent is dispersed continuously as fine droplets into the aqueous sample and the target analytes are extracted into the fine droplets of the extraction solvent. The fine droplets move up through the aqueous phase due to its low density compared to aqueous phase and collect on the surface of the aqueous phase as an organic layer. Finally an aliquot of the organic phase is removed and injected into the separation system for analysis. Several parameters that can affect extraction efficiency including type and volume of extraction and disperser solvents, sample pH, and ionic strength were investigated and optimized. Under the optimum extraction conditions, the extraction recoveries and enrichment factors ranged from 49 to 74% and 1633 to 2466, respectively. Relative standard deviations were in the ranges of 3-6% (n = 6, C = 30 μg L(-1)) for intra-day and 4-7% (n = 4, C = 30 μg L(-1)) for inter-day precisions. The limits of detection were in the range of 0.20-0.86 μg L(-1). Finally the proposed method was successfully applied to determine the target herbicides in fruit juice and vegetable samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Steam distillation/drop-by-drop extraction with gas chromatography-mass spectrometry for fast determination of volatile components in jujube (Ziziphus jujuba Mill.) extract.

PubMed

Sun, Shi-Hao; Chai, Guo-Bi; Li, Peng; Xie, Jian-Ping; Su, Yue

2017-10-13

Jujube extract is commonly used as a food additive and flavoring. The unique jujube aroma and the mild sweet aroma of the extract are critical factors that determine product quality and affect consumer acceptability. The aroma changes with changes in the extraction condition, which is typically dependent on the characteristics of volatile oils in the extract. Despite their importance, the volatile oils of jujube extract have received less attention compared with the soluble components. So, an appropriate qualitative and quantitative method for determination of the volatile oils is vitally important for quality control of the product. A method coupling steam distillation/drop-by-drop extraction with gas chromatography-mass spectrometry (S3DE/GC-MS) was developed to determine the volatile components of jujube extract. Steam distillation was coupled with solvent extraction; the resulting condensate containing volatile components from jujube extract was drop-by-drop extracted using 2 mL of methyl tertiary butyl ether. The solvent served two purposes. First, the solvent extracted the volatile components from the condensate. Second, the volatile components were pre-concentrated by drop-by-drop accumulation in the solvent. As a result, the extraction, separation, and concentration of analytes in the sample were simultaneously completed in one step. The main parameters affecting the S3DE procedure, such as the water steam bubbling rate, extraction solvent volume, sample weight and S3DE time, were optimized. The standard addition approach was essential to obtain accurate measurements by minimizing matrix effects. Good linearity (R 2  ≥ 0.9887) and good repeatability (RSDs ≤ 10.35%, n = 5) for 16 analytes in spiked standard analyte samples were achieved. With the S3DE/GC-MS method, seventy-six volatile compounds from jujube extract were identified and the content of 16 compounds was measured. The results were similar to those from simultaneous distillation extraction. The developed method was simple, fast, effective, sensitive, and provided an overall profile of the volatile components in jujube extract. Thus, this method can be used to determine the volatile components of extracts. Graphical abstract The diagram of steam distillation/drop-by-drop extraction device.

Extraction Optimization for Phenolic- and Withanolide-Rich Fractions from Withania somnifera Roots: Identification and Quantification of Withaferin A, 12-Deoxywithastromonolide, and Withanolide A in Plant Materials and Marketed Formulations Using a Reversed-Phase HPLC-Photodiode Array Detection Method.

PubMed

Kumar, Satyanshu; Singh, Raghuraj; Gajbhiye, Narendra; Dhanani, Tushar

2018-06-26

Background : Both the roots and leaves of Withania somnifera are products of commerce. They contain active compounds of therapeutic value and mostly different withanolides. Several pharmacological activities of W. somnifera have links to one or more withanolides. The presence of phenolic compounds in extracts could play a vital role in the reduction of blood glucose levels in diabetic subjects. Objective : The present study was carried out for the selection of a solvent to prepare extracts rich in phenolics, withaferin A (WA), 12-deoxywithastromonolide (12WD), and withanolide A (WDA). A simple, rapid HPLC method was also developed for the identification and quantification of WA, 12WD, and WDA. Methods : The extraction efficiency of aqueous alcoholic solvents including hexane, chloroform, ethyl acetate, and methanol were compared for three selected withanolides and total phenolic content. The contents of WA, 12WD, and WDA and total phenolics were determined in the extracts. The quality of nine formulations containing W. sominfera were also compared in terms of the content of WA, 12WD, and WDA and total phenolics. Results : The maximum extract yield and the total withanolide and phenolic content were obtained from aqueous alcoholic compositions at 50:50 (v/v), 70:30 (v/v), and 100:0 (v/v), respectively. In the case of organic solvents, chloroform and ethyl acetate yielded the highest concentrations of phenolics and three withanolides, respectively. The total phenolic content in formulations was in the range of 1.84-3.13%, and total withanolide content showed wide variability. Conclusions : The outcome of the present investigation could be utilized for the selection of extraction solvents to prepare W. somnifera -enriched extracts and their quality monitoring by using the developed and validated HPLC-Photodiode array detection method. Highlights : A process for preparation of phenolics and withanolides (withaferin A, 12-deoxywithastramonolide and withanolide A) enriched extracts of Withania somnifera . Simple and rapid HPLC method was also developed and validated as per the ICH guidelines for identification and quantification of three major withanolides. The developed HPLC method was applied to analyze the quality of extracts and marketed herbal products (mono, as well as poly constituents). Optimized extraction process could be utilized for upscaling process development in preparation of enriched extracts from Withania somnifera , crop improvement, bio-prospection studies and quality control.

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.

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

PubMed

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

2010-05-07

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

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.

Rapid determination of triclosan in personal care products using new in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction coupled with high performance liquid chromatography-ultraviolet detection.

PubMed

Chen, Ming-Jen; Liu, Ya-Ting; Lin, Chiao-Wen; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2013-03-12

This paper describes the development of a novel, simple and efficient in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction (IT-USA-SI-LLME) technique for the rapid determination of triclosan (TCS) in personal care products by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. IT-USA-SI-LLME method is based on the rapid phase separation of water-miscible organic solvent from the aqueous phase in the presence of high concentration of salt (salting-out phenomena) under ultrasonication. In the present work, an indigenously fabricated home-made glass extraction device (8-mL glass tube inbuilt with a self-scaled capillary tip) was utilized as the phase separation device for USA-SI-LLME. After the extraction, the upper extractant layer was narrowed into the self-scaled capillary tip by pushing the plunger plug; thus, the collection and measurement of the upper organic solvent layer was simple and convenient. The effects of various parameters on the extraction efficiency were thoroughly evaluated and optimized. Under optimal conditions, detection was linear in the concentration range of 0.4-100ngmL(-1) with correlation coefficient of 0.9968. The limit of detection was 0.09ngmL(-1) and the relative standard deviations ranged between 0.8 and 5.3% (n=5). The applicability of the developed method was demonstrated for the analysis of TCS in different commercial personal care products and the relative recoveries ranged from 90.4 to 98.5%. The present method was proven to be a simple, sensitive, less organic solvent consuming, inexpensive and rapid procedure for analysis of TCS in a variety of commercially available personal care products or cosmetic preparations. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Determination of polychlorinated biphenyls in fish: optimisation and validation of a method based on accelerated solvent extraction and gas chromatography-mass spectrometry.

PubMed

Ottonello, Giuliana; Ferrari, Angelo; Magi, Emanuele

2014-01-01

A simple and robust method for the determination of 18 polychlorinated biphenyls (PCBs) in fish was developed and validated. A mixture of acetone/n-hexane (1:1, v/v) was selected for accelerated solvent extraction (ASE). After the digestion of fat, the clean-up was carried out using solid phase extraction silica cartridges. Samples were analysed by GC-MS in selected ion monitoring (SIM) using three fragment ions for each congener (one quantifier and two qualifiers). PCB 155 and PCB 198 were employed as internal standards. The lowest limit of detection was observed for PCB 28 (0.4ng/g lipid weight). The accuracy of the method was verified by means of the Certified Reference Material EDF-2525 and good results in terms of linearity (R(2)>0.994) and recoveries (80-110%) were also achieved. Precision was evaluated by spiking blank samples at 4, 8 and 12ng/g. Relative standard deviation values for repeatability and reproducibility were lower than 8% and 16%, respectively. The method was applied to the determination of PCBs in 80 samples belonging to four Mediterranean fish species. The proposed procedure is particularly effective because it provides good recoveries with lowered extraction time and solvent consumption; in fact, the total time of extraction is about 12min per sample and, for the clean-up step, a total solvent volume of 13ml is required. Copyright © 2013 Elsevier Ltd. All rights reserved.

Glycerol triacetate as solvent and acyl donor in the production of isoamyl acetate with Candida antarctica lipase B.

PubMed

Wolfson, Adi; Atyya, Aviad; Dlugy, Christina; Tavor, Dorith

2010-03-01

Glycerol triacetate was successfully used as a green solvent and as the acyl donor in the transesterification of isoamyl alcohol to produce isoamyl acetate using free and immobilized Candida antarctica lipase B. Immobilized lipase was more catalytically active than free lipase and could be easily separated from the reaction mixture by filtration. In addition, it was found that increasing either the reaction temperature or the enzyme to substrate ratio increased the conversion of isoamyl alcohol. Using triacetin as the solvent also enabled the separation of product by simple extraction with petroleum ether and catalyst recycling.

Simultaneous extraction, identification and quantification of phenolic compounds in Eclipta prostrata using microwave-assisted extraction combined with HPLC-DAD-ESI-MS/MS.

PubMed

Fang, Xinsheng; Wang, Jianhua; Hao, Jifu; Li, Xueke; Guo, Ning

2015-12-01

A simple and rapid method was developed using microwave-assisted extraction (MAE) combined with HPLC-DAD-ESI-MS/MS for the simultaneous extraction, identification, and quantification of phenolic compounds in Eclipta prostrata, a common herb and vegetable in China. The optimized parameters of MAE were: employing 50% ethanol as solvent, microwave power 400 W, temperature 70 °C, ratio of liquid/solid 30 mL/g and extraction time 2 min. Compared to conventional extraction methods, the optimized MAE can avoid the degradation of the phenolic compounds and simultaneously obtained the highest yields of all components faster with less consumption of solvent and energy. Six phenolic acids, six flavonoid glycosides and one coumarin were firstly identified. The phenolic compounds were quantified by HPLC-DAD with good linearity, precision, and accuracy. The extract obtained by MAE showed significant antioxidant activity. The proposed method provides a valuable and green analytical methodology for the investigation of phenolic components in natural plants. Copyright © 2015 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.

Determination of four major saponins in the seeds of Aesculus chinensis Bunge using accelerated solvent extraction followed by high-performance liquid chromatography and electrospray-time of flight mass spectrometry.

PubMed

Chen, Junhui; Li, Wenlong; Yang, Baijuan; Guo, Xiuchun; Lee, Frank Sen-Chun; Wang, Xiaoru

2007-07-23

A new method based on accelerated solvent extraction (ASE) followed by a reliable high-performance liquid chromatography-diode array detector (HPLC-DAD) and positive ion electrospray-time of flight mass spectrometry (ESI-TOF/MS) analysis has been developed for the characterization and quantification of four major saponins in extracts of the seeds of Aesculus chinensis Bunge (semen aesculi). The saponins escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted from seeds of A. chinesis Bunge via ASE, and the operational parameters of ASE were optimized, such as extraction solvent, extraction temperature, static extraction time and extraction cycles. The optimized procedure employed 70% MeOH as extraction solvent, 120 degrees C of extraction temperature, 7 min of static extraction time, 60% flush volume and the extraction recoveries of the four compounds were nearly to 100% for two cycles. The HPLC conditions are as follows: SinoChrom ODS BP C18 (4.6 mm x 200 mm, 5 microm) column, acetonitrile and 0.10% phosphoric acid solution as mobile phase, flow rate is 1.0 mL min(-1), detection length of UV is 203 nm, injection volume is 10 microL. The results indicated that the developed HPLC method is simple, sensitive and reliable for the determination of four major saponins in seeds of A. chinesis Bunge with a good linearity (r2 > 0.9994), precision (relative standard deviation (R.S.D.) < 1.5%) and the recovery ranges of 95.2-97.3%. The limits of detection (LOD) of the four compounds were in the range of 0.40-0.75 microg mL(-1). This assay can be readily utilized as a quality control method for semen aesculi and other related medicinal plants.

Application of dispersive liquid-liquid microextraction coupled with vortex-assisted hydrophobic magnetic nanoparticles based solid-phase extraction for determination of aflatoxin M1 in milk samples by sensitive micelle enhanced spectrofluorimetry.

PubMed

Amoli-Diva, Mitra; Taherimaslak, Zohreh; Allahyari, Mehdi; Pourghazi, Kamyar; Manafi, Mohammad Hanif

2015-03-01

An efficient, simple and fast low-density solvent based dispersive liquid-liquid microextraction (LDS-DLLME) followed by vortex-assisted dispersive solid phase extraction (VA-D-SPE) has been developed as a new approach for extraction and preconcentration of aflatoxin M1 in milk samples prior to its micelle enhanced spectrofluorimetic determination. In this LDS-DLLME coupled VA-D-SPE method, milk samples were first treated with methanol/water (80:20, v/v) after removing the fat layer. This solvent was directly used as the dispersing solvent in DLLME along with using 1-heptanol (as a low-density solvent with respect to water) as the extracting solvent. In VA-D-SPE approach, hydrophobic oleic acid modified Fe3O4 nanoparticles were used to retrieve the analyte from the DLLME step. It is considerably that the target of VA-D-SPE was 1-heptanol rather than the aflatoxin M1 directly. The main parameters affecting the efficiency of LDS-DLLME and VA-D-SPE procedures and signal enhancement of aflatoxin M1 were investigated and optimized. Under the optimum conditions, the method was linear in the range from 0.02 to 200 µg L(-1) with the correlation coefficient (R(2)) of 0.9989 and detection limit of 13 ng L(-1). The intra-day precision was 2.9 and 4.3% and the inter-day precision was 2.1 and 3.3% for concentration of 2 and 50 µg L(-1) respectively. The developed method was applied for extraction and preconcentration of AFM1 in three commercially available milk samples and the results were compared with the official AOAC method. Copyright © 2014 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

Ultrasound-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet followed by gas chromatography for the determination of eight pyrethroid pesticides in tea samples.

PubMed

Hou, Xiaohong; Zheng, Xin; Zhang, Conglu; Ma, Xiaowei; Ling, Qiyuan; Zhao, Longshan

2014-10-15

A novel ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (UA-DLLME-SFO) combined with gas chromatography (GC) was developed for the determination of eight pyrethroid pesticides in tea for the first time. After ultrasound and centrifugation, 1-dodecanol and ethanol was used as the extraction and dispersive solvent, respectively. A series of parameters, including extraction solvent and volume, dispersive solvent and volume, extraction time, pH, and ultrasonic time influencing the microextraction efficiency were systematically investigated. Under the optimal conditions, the enrichment factors (EFs) were from 292 to 883 for the eight analytes. The linear ranges for the analytes were from 5 to 100μg/kg. The method recoveries ranged from 92.1% to 99.6%, with the corresponding RSDs less than 6.0%. The developed method was considered to be simple, fast, and precise to satisfy the requirements of the residual analysis of pyrethroid pesticides. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

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.

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.

Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

PubMed

Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

2015-12-24

A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative determination of 5-hydroxy-N-methylpyrrolidone in urine for biological monitoring of N-methylpyrrolidone exposure.

PubMed

Ligocka, D; Lison, D; Haufroid, V

2002-10-05

The aim of this work was to validate a sensitive method for quantitative analysis of 5-hydroxy-N-methylpyrrolidone (5-HNMP) in urine. This compound has been recommended as a marker for biological monitoring of N-methylpyrrolidone (NMP) exposure. Different solvents and alternative methods of extraction including liquid-liquid extraction (LLE) on Chem Elut and solid-phase extraction (SPE) on Oasis HLB columns were tested. The most efficient extraction of 5-HNMP in urine was LLE with Chem Elut columns and dichloromethane as a solvent (consistently 22% of recovery). The urinary extracts were derivatized by bis(trimethylsilyl)trifluoroacetamide and analysed by gas chromatography-mass spectrometry (GC-MS) with tetradeutered 5-HNMP as an internal standard. The detection limit of this method is 0.017 mg/l urine with an intraassay precision of 1.6-2.6%. The proposed method of extraction is simple and reproducible. Four different m/z signal ratios of TMS-5-HNMP and tetralabelled TMS-5-HNMP have been validated and could be indifferently used in case of unexpected impurities from urine matrix. Copyright 2002 Elsevier Science B.V.

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.

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.

Headspace Single-Drop Microextraction Gas Chromatography Mass Spectrometry for the Analysis of Volatile Compounds from Herba Asari

PubMed Central

Wang, Guan-Jie; Tian, Li; Fan, Yu-Ming; Qi, Mei-Ling

2013-01-01

A rapid headspace single-drop microextraction gas chromatography mass spectrometry (SDME-GC-MS) for the analysis of the volatile compounds in Herba Asari was developed in this study. The extraction solvent, extraction temperature and time, sample amount, and particle size were optimized. A mixed solvent of n-tridecane and butyl acetate (1 : 1) was finally used for the extraction with sample amount of 0.750 g and 100-mesh particle size at 70°C for 15 min. Under the determined conditions, the pound samples of Herba Asari were directly applied for the analysis. The result showed that SDME-GC–MS method was a simple, effective, and inexpensive way to measure the volatile compounds in Herba Asari and could be used for the analysis of volatile compounds in Chinese medicine. PMID:23607049

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

Development of a simple and valid method for the trace determination of phthalate esters in human plasma using dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry.

PubMed

Ebrahim, Karim; Poursafa, Parinaz; Amin, Mohammad Mehdi

2017-11-01

A new method was developed for the trace determination of phthalic acid esters in plasma using dispersive liquid-liquid microextraction and gas chromatography with mass spectrometry analysis. Plasma proteins were efficiently precipitated by trichloroacetic acid and then a mixture of chlorobenzene (as extraction solvent) and acetonitrile (as dispersive solvent) rapidly injected to clear supernatant using a syringe. After centrifuging, chlorobenzene sedimented at the bottom of the test tube. 1 μL of this sedimented phase was injected into the gas chromatograph for phthalic acid esters analysis. Different factors affecting the extraction performance, such as the type of extraction and dispersive solvent, their volume, extraction time, and the effects of salt addition were investigated and optimized. Under the optimum conditions, the enrichment factors and extraction recoveries were satisfactory and ranged between 820-1020 and 91-97%, respectively. The linear range was wide (50-1000 ng/mL) and limit of detection was very low (1.5-2.5 ng/mL for all analytes). The relative standard deviations for analysis of 1 μg/mL of the analytes were between 3.2-6.1%. Salt addition showed no significant effect on extraction recovery. Finally, the proposed method was successfully utilized for the extraction and determination of the phthalic acid esters in human plasma samples and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of triazine herbicides in fresh vegetables by dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction high performance liquid chromatography.

PubMed

Wu, Lijie; Hu, Mingzhu; Li, Zhanchao; Song, Ying; Yu, Cui; Zhang, Yupu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-02-01

A novel extraction method, dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction, was developed for the determination of triazine herbicides, including desmetryn, terbumeton, propazine, terbuthylazine, dimethametryn, and dipropetryn in fresh vegetable samples by high performance liquid chromatography (HPLC). In the developed method, 120 μL of 1-butyl-3-methylimidazolium tetrafluoroborate ([C4MIM][BF4]) was added to 10 mL of aqueous solution containing 0.3 g of NaCl to obtained the extraction solvent. Six triazines could be extracted completely within 4 min by the present method. Then, [NH4][PF6] was added into the extract to form a water-insoluble ionic liquid [C4MIM][PF6] via a simple metathesis reaction, and the analytes were enriched into the ionic liquid phase. After centrifugation and dilution with acetonitrile, the resulting solution was analyzed directly by HPLC. The effects of some experimental parameters, including type and volume of ionic liquid, volume of extraction solvent, amount of ion-pairing agent [NH4][PF6], salt concentration, microwave power, and flow rate of extraction solvent on the extraction efficiency were investigated and optimized. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 2.50-250.00 μg kg(-1), with the correlation coefficients ranging from 0.9989 to 0.9999. When the present method was applied to the analysis of vegetable samples, satisfactory recoveries were obtained in the range of 76.8%-106.9%, and relative standard deviations were lower than 9.8%.

Integration of whole-cell reaction and product isolation: Highly hydrophobic solvents promote in situ substrate supply and simplify extractive product isolation.

PubMed

Leis, Dorothea; Lauß, Bernhard; Macher-Ambrosch, Robert; Pfennig, Andreas; Nidetzky, Bernd; Kratzer, Regina

2017-09-10

Product isolation from aqueous-organic reaction mixtures that contain high concentrations of whole cells constitutes a challenging task in bioprocessing. Stirring of the biphasic reaction media leads to the formation of solvent droplets coated by cells and other surface active components and an emulsion forms. We used an early focus on phase separation to simplify a whole-cell bioreduction. Octanol, heptanol, hexanol, hexane and dipropylether were tested as co-solvents in the E. coli catalyzed reduction of o-chloroacetophenone. All solvents showed very similar performance in bioreductions and highest yields were obtained with low organic-to-aqueous phase ratios. Reaction mixtures were directly investigated for organic-phase recovery. Phase separation was optimized in small-scale settling experiments and confirmed by the isolation of 20.4g (S)-1-(2-chlorophenyl)ethanol from a 0.5L batch reduction containing 40g CDW /L whole-cell catalyst. Solvent consumption during product isolation could be halved by the simple addition of sodium hydroxide prior to product extraction. Basification to pH 13.5 and three extraction steps with a total of 1.2v/v hexane led to an isolated yield of 87% (97% reduction yield). A general emulsion destabilizing effect under harsh conditions, as extreme pH values and presence of toxic reactants, was observed. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Ionic-liquid-based dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the forensic determination of methamphetamine in human urine.

PubMed

Wang, Ruifeng; Qi, Xiujuan; Zhao, Lei; Liu, Shimin; Gao, Shuang; Ma, Xiangyuan; Deng, Youquan

2016-07-01

Determination of methamphetamine in forensic laboratories is a major issue due to its health and social harm. In this work, a simple, sensitive, and environmentally friendly method based on ionic liquid dispersive liquid-liquid microextraction combined with high-performance liquid chromatography was established for the analysis of methamphetamine in human urine. 1-Octyl-3-methylimidazolium hexafluorophosphate with the help of disperser solvent methanol was selected as the microextraction solvent in this process. Various parameters affecting the extraction efficiency of methamphetamine were investigated systemically, including extraction solvent and its volume, disperser solvent and its volume, sample pH, extraction temperature, and centrifugal time. Under the optimized conditions, a good linearity was obtained in the concentration range of 10-1000 ng/mL with determination coefficient >0.99. The limit of detection calculated at a signal-to-noise ratio of 3 was 1.7 ng/mL and the relative standard deviations for six replicate experiments at three different concentration levels of 100, 500, and 1000 ng/mL were 6.4, 4.5, and 4.7%, respectively. Meanwhile, up to 220-fold enrichment factor of methamphetamine and acceptable extraction recovery (>80.0%) could be achieved. Furthermore, this method has been successfully employed for the sensitive detection of a urine sample from a suspected drug abuser. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of mixtures of fatty acids and fatty alcohols in fermentation broth.

PubMed

Liu, Yilan; Chen, Ting; Yang, Maohua; Wang, Caixia; Huo, Weiyan; Yan, Daojiang; Chen, Jinjin; Zhou, Jiemin; Xing, Jianmin

2014-01-03

Microbial production of fatty acids and fatty alcohols has attracted increasing concerns because of energy crisis and environmental impact of fossil fuels. Therefore, simple and efficient methods for the extraction and quantification of these compounds become necessary. In this study, a high-performance liquid chromatography-refractive index detection (HPLC-RID) method was developed for the simultaneous quantification of fatty acids and fatty alcohols in these samples. The optimum chromatographic conditions are C18 column eluted with methanol:water:acetic acid (90:9.9:0.1, v/v/v); column temperature, 26°C; flow rate, 1.0mL/min. Calibration curves of all selected analytes showed good linearity (r(2)≥0.9989). The intra-day and inter-day relative standard deviations (RSDs) of the 10 compounds were less than 4.46% and 5.38%, respectively, which indicated that the method had good repeatability and precision. Besides, a method for simultaneous extraction of fatty acids and fatty alcohols from fermentation broth was optimized by orthogonal design. The optimal extraction conditions were as follows: solvent, ethyl acetate; solvent to sample ratio, 0.5:1; rotation speed, 2min at 260rpm; extraction temperature, 10°C. This study provides simple and fast methods to simultaneously extract and quantify fatty acids and fatty alcohols for the first time. It will be useful for the study of microbial production of these products. Copyright © 2013 Elsevier B.V. All rights reserved.

A simultaneous analysis method of polycyclic aromatic hydrocarbons, nicotine, cotinine and metals in human hair.

PubMed

Li, Zhenjiang; Wang, Bin; Ge, Shufang; Yan, Lailai; Liu, Yingying; Li, Zhiwen; Ren, Aiguo

2016-12-01

Polycyclic aromatic hydrocarbons (PAHs), nicotine, cotinine, and metals in human hair have been used as important environmental exposure markers. We aimed to develop a simple method to simultaneously analyze these pollutants using a small quantity of hair. The digestion performances of tetramethylammonium hydroxide (TMAH) and sodium hydroxide (NaOH) for human hair were compared. Various solvents or their mixtures including n-hexane (HEX), dichloromethane (DCM) and trichloromethane (TCM), HEX:DCM32 (3/2) and HEX:TCM73 (7/3) were adopted to extract organics. The recoveries of metals were determined under an optimal operation of digestion and extraction. Our results showed that TMAH performed well in dissolving human hair and even better than NaOH. Overall, the recoveries for five solutions were acceptable for PAHs, nicotine in the range of 80%-110%. Except for HEX, other four extraction solutions had acceptable extraction efficiency for cotinine from HEX:TCM73 (88 ± 4.1%) to HEX:DCM32 (100 ± 2.8%). HEX:DCM32 was chosen as the optimal solvent in consideration of its extraction efficiency and lower density than water. The recoveries of 12 typical major or trace metals were mainly in the range of 90%-110% and some of them were close to 100%. In conclusion, the simultaneous analysis of PAHs, nicotine, cotinine, and metals was feasible. Our study provided a simple and low-cost technique for environmental epidemiological studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

PubMed

Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

2013-01-01

A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

Synthesis and application of magnetic deep eutectic solvents: Novel solvents for ultrasound assisted liquid-liquid microextraction of thiophene.

PubMed

Khezeli, Tahere; Daneshfar, Ali

2017-09-01

Two novel magnetic deep eutectic solvents (MDESs), comprised of cheap and simple components named [choline chloride/phenol] [FeCl 4 ] and [choline chloride/ethylene glycol] [FeCl 4 ] were prepared and characterized by CHN elemental analysis, proton nuclear magnetic resonance ( 1 H NMR), vibrating sample magnetometery (VSM), Raman, Fourier transform-infrared (FT-IR) and UV-Vis spectrometery. The extraction efficiency of the prepared MDESs has been investigated in ultrasound assisted liquid-liquid microextraction based MDES (UALLME-MDES). Briefly, MDESs were added to n-heptan containing thiophene. Then, MDESs were dispersed in n-heptane by sonication. After that, microdroplets of MDESs were collected by a magnet and the remained concentration of thiophene in n-heptane phase was analyzed by GC-FID. The results indicated that [choline chloride/phenol] [FeCl 4 ] has higher extraction efficiency than [choline chloride/ethylene glycol] [FeCl 4 ]. This work opens a new way to the application of MDESs. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of parabens in human milk and other food samples by capillary electrophoresis after dispersive liquid-liquid microextraction with back-extraction.

PubMed

Alshana, Usama; Ertaş, Nusret; Göğer, Nilgün G

2015-08-15

Dispersive liquid-liquid microextraction (DLLME) with back-extraction was used prior to capillary electrophoresis (CE) for the extraction of four parabens. Optimum extraction conditions were: 200 μL chloroform (extraction solvent), 1.0 mL acetonitrile (disperser solvent) and 1 min extraction time. Back-extraction of parabens from chloroform into a 50mM sodium hydroxide solution within 10s facilitated their direct injection into CE. The analytes were separated at 12°C and 25 kV with a background electrolyte of 25 mM borate buffer containing 5.0% (v/v) acetonitrile. Enrichment factors were in the range of 4.3-10.7 and limits of detection ranged from 0.1 to 0.2 μg mL(-1). Calibration graphs showed good linearity with coefficients of determination (R(2)) higher than 0.9957 and relative standard deviations (%RSDs) lower than 3.5%. DLLME-CE was demonstrated to be a simple and rapid method for the determination of parabens in human milk and food with relative recoveries in the range of 86.7-103.3%. Copyright © 2015 Elsevier Ltd. All rights reserved.

Rapid extraction of Amomum tsao-ko essential oil and determination of its chemical composition, antioxidant and antimicrobial activities.

PubMed

Cui, Qi; Wang, Li-Tao; Liu, Ju-Zhao; Wang, Hui-Mei; Guo, Na; Gu, Cheng-Bo; Fu, Yu-Jie

2017-09-01

A simple, green and efficient extraction method named modified-solvent free microwave extraction (M-SFME) was employed for the extraction of essential oils (EOs) from Amomun tsao-ko. The process of M-SFME was optimized with the prominent preponderance of such higher extraction yield (1.13%) than those of solvent free microwave extraction (SFME, 0.91%) and hydrodistillation (HD, 0.84%) under the optimal parameters. Thirty-four volatile substances representing 95.4% were identified. The IC 50 values of EOs determined by DPPH radical scavenging activity and β-carotene/linoleic acid bleaching assay were 5.27 and 0.63mg/ml. Furthermore, the EOs exhibited moderate to potent broad-spectrum antimicrobial activity against all tested strains including five gram-positive and two gram-negative bacteria (MIC: 2.94-5.86mg/ml). In general, M-SFME is a potential and desirable alternative for the extraction of EOs from aromatic herbs, and the EOs obtained from A. tsao-ko can be explored as a potent natural antimicrobial and antioxidant preservative ingredient in food industry from the technological and economical points of view. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid analysis of aflatoxins B1, B2, and ochratoxin A in rice samples using dispersive liquid-liquid microextraction combined with HPLC.

PubMed

Lai, Xian-Wen; Sun, Dai-Li; Ruan, Chun-Qiang; Zhang, He; Liu, Cheng-Lan

2014-01-01

A novel, simple, and rapid method is presented for the analysis of aflatoxin B1, aflatoxin B2, and ochratoxin A in rice samples by dispersive liquid-liquid microextraction combined with LC and fluorescence detection. After extraction of the rice samples with a mixture of acetonitrile/water/acetic acid, mycotoxins were rapidly partitioned into a small volume of organic solvent (chloroform) by dispersive liquid-liquid microextraction. The three mycotoxins were simultaneously determined by LC with fluorescence detection after precolumn derivatization for aflatoxin B1 and B2. Parameters affecting both extraction and dispersive liquid-liquid microextraction procedures, including the extraction solvent, the type and volume of extractant, the volume of dispersive solvent, the addition of salt, the pH and the extraction time, were optimized. The optimized protocol provided an enrichment factor of approximately 1.25 and with detection of limits (0.06-0.5 μg/kg) below the maximum levels imposed by current regulations for aflatoxins and ochratoxin A. The mean recovery of three mycotoxins ranged from 82.9-112%, with a RSD less than 7.9% in all cases. The method was successfully applied to measure mycotoxins in commercial rice samples collected from local supermarkets in China. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

Centrifugeless dispersive liquid-liquid microextraction based on salting-out phenomenon followed by high performance liquid chromatography for determination of Sudan dyes in different species.

PubMed

Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2018-04-01

In this work, a novel method, namely centrifugeless dispersive liquid-liquid microextraction, is introduced for the efficient extraction of banned Sudan dyes from foodstuff and water samples. In this method, which is based upon the salting-out phenomenon, in order to accelerate the extraction process, the extraction solvent (1-undecanol, 75 μL) is dispersed into the sample solution. Then the mixture is passed through a small column filled with 5 g sodium chloride, used as a separating reagent. In this condition, fine droplets of the extraction solvent are floated on the mixture, and the phase separation is simply achieved. This method is environmentally friendly, simple, and very fast, so that the overall extraction time is only 7 min. Under the optimal experimental conditions, the preconcentration factors in the range of 90-121 were obtained for the analytes. Also good linearities were obtained in the range of 2.5-1200 ng mL -1 (r 2  ≥ 0.993). Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Air-assisted liquid-liquid microextraction by solidifying the floating organic droplets for the rapid determination of seven fungicide residues in juice samples.

PubMed

You, Xiangwei; Xing, Zhuokan; Liu, Fengmao; Zhang, Xu

2015-05-22

A novel air assisted liquid-liquid microextraction using the solidification of a floating organic droplet method (AALLME-SFO) was developed for the rapid and simple determination of seven fungicide residues in juice samples, using the gas chromatography with electron capture detector (GC-ECD). This method combines the advantages of AALLME and dispersive liquid-liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO) for the first time. In this method, a low-density solvent with a melting point near room temperature was used as the extraction solvent, and the emulsion was rapidly formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent for ten times repeatedly using a 10-mL glass syringe. After centrifugation, the extractant droplet could be easily collected from the top of the aqueous samples by solidifying it at a temperature lower than the melting point. Under the optimized conditions, good linearities with the correlation coefficients (γ) higher than 0.9959 were obtained and the limits of detection (LOD) varied between 0.02 and 0.25 μgL(-1). The proposed method was applied to determine the target fungicides in juice samples and acceptable recoveries ranged from 72.6% to 114.0% with the relative standard deviations (RSDs) of 2.3-13.0% were achieved. Compared with the conventional DLLME method, the newly proposed method will neither require a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Fast, simple and efficient supramolecular solvent-based microextraction of mecoprop and dichlorprop in soils prior to their enantioselective determination by liquid chromatography-tandem mass spectrometry.

PubMed

Caballo, C; Sicilia, M D; Rubio, S

2014-02-01

A simple, sensitive, rapid and economic method was developed for the quantification of enantiomers of chiral pesticides as mecoprop (MCPP) and dichlorprop (DCPP) in soil samples using supramolecular solvent-based microextraction (SUSME) combined with liquid chromatography coupled to mass spectrometry (LC-MS/MS). SUSME has been described for the extraction of chiral pesticides in water, but this is firstly applied to soil samples. MCPP and DCPP are herbicides widely used in agriculture that have two enantiomeric forms (R- and S-) differing in environmental fate and toxicity. Therefore, it is essential to have analytical methods for monitoring individual DCPP and MCPP enantiomers in environmental samples. MCPP and DCPP were extracted in a supramolecular solvent (SUPRAS) made up of dodecanoic acid aggregates, the extract was dried under a nitrogen stream, the two herbicides dissolved in acetate buffer and the aqueous extract directly injected in the LC-MS/MS system. The recoveries obtained were independent of soil composition and age of herbicide residues. The detection and quantitation limits of the developed method for the determination of R- and S-MCPP and R- and S-DCPP in soils were 0.03 and 0.1 ng g(-1), respectively, and the precision, expressed as relative standard deviation (n=6), for enantiomer concentrations of 5 and 100 ng g(-1) were in the ranges 4.1-6.1% and 2.9-4.1%. Recoveries for soil samples spiked with enantiomer concentrations within the interval 5-180 ng g(-1) and enantiomeric ratios (ERs) of 1, 3 and 9, ranged between 93 and 104% with standard deviations of the percent recovery varying between 0.3% and 6.0%. Because the SUPRAS can solubilize analytes through different type of interactions (dispersion, dipole-dipole and hydrogen bonds), it could be used to extract a great variety of pesticides (including both polar and non-polar) in soils. © 2013 Published by Elsevier B.V.

Dynamic ultrasonic nebulisation extraction coupled with headspace ionic liquid-based single-drop microextraction for the analysis of the essential oil in Forsythia suspensa.

PubMed

Yang, Jinjuan; Wei, Hongmin; Teng, Xiane; Zhang, Hanqi; Shi, Yuhua

2014-01-01

Ionic liquids have attracted much attention as an extraction solvent instead of traditional organic solvent in single-drop microextraction. However, non-volatile ionic liquids are difficult to couple with gas chromatography. Thus, the following injection system for the determination of organic compounds is described. To establish an environmentally friendly, simple, and effective extraction method for preparation and analysis of the essential oil from aromatic plants. The dynamic ultrasonic nebulisation extraction was coupled with headspace ionic liquid-based single-drop microextraction(UNE-HS/IL/SDME)for the extraction of essential oils from Forsythia suspense fruits. After 13 min of extraction for 50 mg sample, the extracts in ionic liquid were evaporated rapidly in the gas chromatography injector through a thermal desorption unit (5 s). The traditional extraction method was carried out for comparative study. The optimum conditions were: 3 μL of 1-methyl-3-octylimidazolium hexafluorophosphate was selected as the extraction solvent, the sample amount was 50 mg, the flow rate of purging gas was 200 mL/min, the extraction time was 13 min, the injection volume was 2 μL, and the thermal desorption temperature and time were 240 °C and 5 s respectively. Comparing with hydrodistillation (HD), the proposed method was environment friendly and efficient. The proposed method is environmentally friendly, time saving, with high efficiency and low consumption. It would extend the application range of the HS/SDME and would be useful especially for aromatic plants analysis. Copyright © 2013 John Wiley & Sons, Ltd.

Optimized ultrasonic assisted extraction-dispersive liquid-liquid microextraction coupled with gas chromatography for determination of essential oil of Oliveria decumbens Vent.

PubMed

Sereshti, Hassan; Izadmanesh, Yahya; Samadi, Soheila

2011-07-22

Ultrasonic assisted extraction-dispersive liquid-liquid microextraction (UAE-DLLME) coupled with gas chromatography (GC) was applied for extraction and determination of essential oil constituents of the plant Oliveria decumbens Vent. Scanning electron microscopy (SEM) was used to see the effect of ultrasonic radiation on the extraction efficiency. By comparison with hydrodistillation, UAE-DLLME is fast, low cost, simple, efficient and consuming small amount of plant materials (∼1.0 g). The effects of various parameters such as temperature, ultrasonication time, volume of disperser and extraction solvents were investigated by a full factorial design to identify significant variables and their interactions. The results demonstrated that temperature and ultrasonication time had no considerable effect on the results. In the next step, a central composite design (CCD) was performed to obtain the optimum levels of significant parameters. The obtained optimal conditions were: 0.45 mL for disperser solvent (acetonitrile) and 94.84 μL for extraction solvent (chlorobenzene). The limits of detection (LODs), linear dynamic range and determination coefficients (R(2)) were 0.2-29 ng mL(-1), 1-2100 ng mL(-1) and 0.995-0.998, respectively. The main components of the essential oil were: thymol (47.06%), carvacrol (23.31%), gamma-terpinene (18.94%), p-cymene (8.71%), limonene (0.76%) and myristicin (0.63%). Copyright © 2011 Elsevier B.V. All rights reserved.

A Simple Method for Isolation of Caffeine from Black Tea Leaves: Use of a Dichloromethane-Alkaline Water Mixture as an Extractant

NASA Astrophysics Data System (ADS)

Onami, Tetsuo; Kanazawa, Hitoshi

1996-06-01

A simple procedure for the isolation of caffeine from tea leaves has been established without using hot or boiling water. A mixture of tea leaves, dichloromethane, and 0.2 M NaOH was shaken for 7 min, and the organic layer was separated. After evaporation of the organic solvent, residual crystals were purified by recrystallization to give 20-30 mg (student yield) of pure caffeine from one tea bag (2 g).

An improved facile method for extraction and determination of steroidal saponins in Tribulus terrestris by focused microwave-assisted extraction coupled with GC-MS.

PubMed

Li, Tianlin; Zhang, Zhuomin; Zhang, Lan; Huang, Xinjian; Lin, Junwei; Chen, Guonan

2009-12-01

An improved fast method for extraction of steroidal saponins in Tribulus terrestris based on the use of focus microwave-assisted extraction (FMAE) is proposed. Under optimized conditions, four steroidal saponins were extracted from Tribulus terrestris and identified by GC-MS, which are Tigogenin (TG), Gitogenin (GG), Hecogenin (HG) and Neohecogenin (NG). One of the most important steroidal saponins, namely TG was quantified finally. The recovery of TG was in the range of 86.7-91.9% with RSD<5.2%. The convention heating reflux extraction was also conducted in order to validate the reliability of this new FMAE method. The yield of total steroidal saponins was 90.3% in a one-step FMAE, while the yield of 65.0% was achieved during heating reflux extraction, and the extraction time was reduced from 3 h to 5 min by using less solvent. The method was successfully applied to analyze the steroidal saponins of Tribulus terrestris from different areas of occurrence. The difference in chromatographic characteristics of steroidal saponins was proved to be related to the different areas of occurrence. The results showed that FMAE-GC-MS is a simple, rapid, solvent-saving method for the extraction and determination of steroidal saponins in Tribulus terrestris.

A Fast Liquid Chromatography Tandem Mass Spectrometric Analysis of PETN (Pentaerythritol Tetranitrate), RDX (3,5-Trinitro-1,3,5-triazacyclohexane) and HMX (Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) in Soil, Utilizing a Simple Ultrasonic-Assisted Extraction with Minimum Solvent.

PubMed

Anilanmert, Beril; Aydin, Muhammet; Apak, Resat; Avci, Gülfidan Yenel; Cengiz, Salih

2016-01-01

Direct analyses of explosives in soil using liquid chromatography tandem mass spectrometry (LC-MS/MS) methods are very limited in the literature and require complex procedures or relatively high amount of solvent. A simple and rapid method was developed for the determination of pentaerythritol tetranitrate (PETN), 3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), which are among the explosives used in terrorist attacks. A one-step extraction method for 1.00 g soil with 2.00 mL acetonitrile, and a 8-min LC-MS/MS method was developed. The detection limits for PETN, RDX and HMX were 5.2, 8.5 and 3.4 ng/g and quantitation limits were 10.0, 24.5, 6.0 ng/g. The intermediate precisions and Horwitz Ratio's were between 4.10 - 13.26% and 0.24 - 0.98, in order. This method was applied to a model post-blast debris collected from an artificial explosion and real samples collected after a terrorist attack in Istanbul. The method is easy and fast and requires less solvent use than other 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.

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.

Rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection.

PubMed

Yang, Xiao; Diao, Chun-Peng; Sun, Ai-Ling; Liu, Ren-Min

2014-10-01

A method for the rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection was proposed in this paper. A simple apparatus consisting of a test tube and a cut-glass dropper was designed and applied to collect the floating extraction drop in liquid-liquid microextraction when low-density organic solvent was used as the extraction solvent. Solidification and melting steps that were tedious but necessary once the low-density organic solvent used as extraction solvent could be avoided by using this apparatus. Bisphenol A was selected as model pollutant and vortex-assisted liquid-liquid microextraction was employed to investigate the usefulness of the apparatus. High-performance liquid chromatography with fluorescence detection was selected as the analytical tool for the detection of bisphenol A. The linear dynamic range was from 0.10 to 100 μg/L for bisphenol A, with good squared regression coefficient (r(2) = 0.9990). The relative standard deviation (n = 7) was 4.7% and the limit of detection was 0.02 μg/L. The proposed method had been applied to the determination of bisphenol A in natural water samples and was shown to be economical, fast, and convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Application of modified hollow fiber liquid phase microextraction in conjunction with chromatography-electron capture detection for quantification of acrylamide in waste water samples at ultra-trace levels.

PubMed

Sobhi, Hamid Reza; Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali

2017-03-03

Herein, a simple and sensitive method was successfully developed for the extraction and quantification of acrylamide in water samples. Initially, acrylamide was derivatized through a bromination process. Subsequently, a modified hollow-fiber liquid-phase microextraction was applied for the extraction of the brominated acrylamide from a 10-ml portion of an aqueous sample. Briefly, in this method, the derivatized acrylamide (2,3-dibromopropionamide) was extracted from the aqueous sample into a thin layer of an organic solvent sustained in pores of a porous hollow fiber. Then, it was back-extracted using a small volume of organic acceptor solution (acetonitril, 25μl) located inside the lumen of the hollow fiber followed by gas chromatography-electron capture detection (GC-ECD). The optimal conditions were examined for the extraction of the analyte such as: the organic solvent: dihexyl ether+10% tri-n-octyl phosphine oxide; stirring rate: 750rpm; no salt addition and 30min extraction time. These optimal extraction conditions allowed excellent enrichment factor values for the method. Enrichment factor, detection limit (S/N=3) and dynamic linear range of 60, 2ngL -1 and 50-1000ngL -1 to be determined for the analyte. The relative standard deviations (RSD%) representing precision of the method were in the range of 2.2-5.8 based on the average of three measurements. Accuracy of the method was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 108%. Finally, the method proved to be simple, rapid, and cost-effective for routine screen of acrylamide-contaminated highly-complicated untreated waste water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid-liquid microextraction of synthetic pigments in beverages using a hydrophobic deep eutectic solvent.

PubMed

Zhu, Shuqiang; Zhou, Jia; Jia, Hongfang; Zhang, Haixia

2018-03-15

A method was developed for the determination of eight synthetic pigments in beverage samples by liquid-liquid microextraction followed by high performance liquid chromatography. Using hydrophobic deep eutectic solvent (DES) as the microextraction solvent, several key parameters were optimized, including the type and volume of the hydrophobic DES, pH value, vortex time and salt content. Detection limits were in the range 0.016-1.12 ng/mL, recoveries were in the range 74.5-102.5% and relative standard deviations were <5.4%. The method is simple, green and practical, and could be applied to the extraction and determination of synthetic pigments in beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fast, sensitive and reliable multi-residue method for routine determination of 34 pesticides from various chemical groups in water samples by using dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry.

PubMed

Tankiewicz, Maciej; Biziuk, Marek

2018-02-01

A simple and efficient dispersive liquid-liquid microextraction technique (DLLME) was developed by using a mixture of two solvents: 40 μL of tetrachlorethylene (extraction solvent) and 1.0 mL of methanol (disperser solvent), which was rapidly injected with a syringe into 10 mL of water sample. Some important parameters affecting the extraction efficiency, such as type and volume of solvents, water sample volume, extraction time, temperature, pH adjustment and salt addition effect were investigated. Simultaneous determination of 34 commonly used pesticides was performed by using gas chromatography coupled with mass spectrometry (GC-MS). The procedure has been validated in order to obtain the highest efficiency at the lowest concentration levels of analytes to fulfill the requirements of regulations on maximum residue limits. Under the optimum conditions, the linearity range was within 0.0096-100 μg L -1 . The limits of detection (LODs) of the developed DLLME-GC-MS methodology for all investigated pesticides were in the range of 0.0032 (endrin)-0.0174 (diazinon) μg L -1 and limits of quantification (LOQs) from 0.0096 to 0.052 μg L -1 . At lower concentration of 1 μg L -1 for each pesticide, recoveries ranged between 84% (tebufenpyrad) and 108% (deltamethrin) with relative standard deviations (RSDs) (n = 7) from 1.1% (metconazole) to 11% (parathion-mehtyl). This methodology was successfully applied to check contamination of environmental samples. The procedure has proved to be selective, sensitive and precise for the simultaneous determination of various pesticides. The optimized analytical method is very simple and rapid (less than 5 min). Graphical abstract Analytical procedure for testing water samples consists of dispersive liquid-liquid microextraction (DLLME) and gas chromatography coupled with mass spectrometry (GC-MS).

Microwave-assisted ionic liquid homogeneous liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of anthraquinones in Rheum palmatum L.

PubMed

Wang, Zhibing; Hu, Jianxue; Du, Hongxia; He, Shuang; Li, Qing; Zhang, Hanqi

2016-06-05

The microwave-assisted ionic liquid homogeneous liquid-liquid microextraction (MA-IL-HLLME) coupled with high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones, including aloe-emodin, emodin, chrysophanol and physcion in root of Rheum palmatum L. Several experimental parameters influencing the extraction efficiency, including amount of sample, type and volume of ionic liquid, volume and pH value of extraction medium, microwave power and extraction time, concentration of NH4PF6 as well as centrifugal condition were optimized. When 140μL of ionic liquid ([C8MIM][BF4]) was used as an extraction solvent, target analytes can be extracted from sample matrix in one minute with the help of microwave irradiation. The MA-IL-HLLME is simple and quick. The calibration curves exhibited good linear relationship (r>0.9984). The limits of detection and quantification were in the range of 0.015-0.026 and 0.051-0.088μgmL(-1), respectively. The spiked recovery for each analyte was in the range of 81.13-93.07% with relative standard deviations lower than 6.89%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with ultrasonic and heat reflux extraction. The results indicated that the present method can be successfully applied to the determination of anthraquinones in medicinal plant. Copyright © 2016 Elsevier B.V. All rights reserved.

The effects of the macrotetralide actin antibiotics on the equilibrium extraction of alkali metal salts into organic solvents.

PubMed

Eisenman, G; Ciani, S; Szabo, G

1969-12-01

In order to clarify the mechanism by which neutral molecules such as the macrotetralide actin antibiotics make phospholipid bilayer membranes selectively permeable to cations, we have studied, both theoretically and experimentally, the extraction by these antibiotics of cations from aqueous solutions into organic solvents. The experiments involve merely shaking an organic solvent phase containing the antibiotic with aqueous solutions containing various cationic salts of a lipid-soluble colored anion. The intensity of color of the organic phase is then measured spectrophotometrically to indicate how much salt has been extracted. From such measurements of the equilibrium extraction of picrate and dinitrophenolate salts of Li, Na, K, Rb, Cs, and NH4 into n-hexane, dichloromethane, and hexane-dichloromethane mixtures, we have verified that the chemical reactions are as simple as previously postulated, at least for nonactin, monactin, dinactin, and trinactin. The equilibrium constant for the extraction of each cation by a given macrotetralide actin antibiotic was also found to be measurable with sufficient precision for meaningful differences among the members of this series of antibiotics to be detected. It is noteworthy that the ratios of selectivities among the various cations were discovered to be characteristic of a given antibiotic and to be completely independent of the solvent used. This finding and others reported here indicate that the size and shape of the complex formed between the macrotetralide and a given cation is the same, regardless of the species of cation bound. For such "isosteric" complexes, notable simplifications of the theory become possible which enable us to predict not only the electrical properties of a membrane made of the same solvent and having the thinness of the phospholipid bilayer but also, and more importantly, the electrical properties of the phospholipid bilayer membrane itself. These predictions will be compared with experimental data for phospholipid bilayer membranes in the accompanying paper.

Validation of green-solvent extraction combined with chromatographic chemical fingerprint to evaluate quality of Stevia rebaudiana Bertoni.

PubMed

Teo, Chin Chye; Tan, Swee Ngin; Yong, Jean Wan Hong; Hew, Choy Sin; Ong, Eng Shi

2009-02-01

An approach that combined green-solvent methods of extraction with chromatographic chemical fingerprint and pattern recognition tools such as principal component analysis (PCA) was used to evaluate the quality of medicinal plants. Pressurized hot water extraction (PHWE) and microwave-assisted extraction (MAE) were used and their extraction efficiencies to extract two bioactive compounds, namely stevioside (SV) and rebaudioside A (RA), from Stevia rebaudiana Bertoni (SB) under different cultivation conditions were compared. The proposed methods showed that SV and RA could be extracted from SB using pure water under optimized conditions. The extraction efficiency of the methods was observed to be higher or comparable to heating under reflux with water. The method precision (RSD, n = 6) was found to vary from 1.91 to 2.86% for the two different methods on different days. Compared to PHWE, MAE has higher extraction efficiency with shorter extraction time. MAE was also found to extract more chemical constituents and provide distinctive chemical fingerprints for quality control purposes. Thus, a combination of MAE with chromatographic chemical fingerprints and PCA provided a simple and rapid approach for the comparison and classification of medicinal plants from different growth conditions. Hence, the current work highlighted the importance of extraction method in chemical fingerprinting for the classification of medicinal plants from different cultivation conditions with the aid of pattern recognition tools used.

Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by flame atomic absorption spectrometry.

PubMed

Carletto, Jeferson Schneider; Luciano, Raquel Medeiros; Bedendo, Gizelle Cristina; Carasek, Eduardo

2009-04-06

A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML(2)). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5x10(-2) mol L(-1), extraction temperature 40 degrees C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 microL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 microL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 microg L(-1), relative standard deviation (RSD) 5.5% and the working linear range 2-30 microg L(-1).

Poly(ethylene oxide) functionalization

DOEpatents

Pratt, Russell Clayton

2014-04-08

A simple procedure is provided by which the hydroxyl termini of poly(ethylene oxide) can be appended with functional groups to a useful extent by reaction and precipitation. The polymer is dissolved in warmed toluene, treated with an excess of organic base and somewhat less of an excess of a reactive acylating reagent, reacted for several hours, then precipitated in isopropanol so that the product can be isolated as a solid, and salt byproducts are washed away. This procedure enables functionalization of the polymer while not requiring laborious purification steps such as solvent-solvent extraction or dialysis to remove undesirable side products.

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.

Direct immersion single drop micro-extraction method for multi-class pesticides analysis in mango using GC-MS.

PubMed

Pano-Farias, Norma S; Ceballos-Magaña, Silvia G; Muñiz-Valencia, Roberto; Jurado, Jose M; Alcázar, Ángela; Aguayo-Villarreal, Ismael A

2017-12-15

Due the negative effects of pesticides on environment and human health, more efficient and environmentally friendly methods are needed. In this sense, a simple, fast, free from memory effects and economical direct-immersion single drop micro-extraction (SDME) method and GC-MS for multi-class pesticides determination in mango samples was developed. Sample pre-treatment using ultrasound-assisted solvent extraction and factors affecting the SDME procedure (extractant solvent, drop volume, stirring rate, ionic strength, time, pH and temperature) were optimized using factorial experimental design. This method presented high sensitive (LOD: 0.14-169.20μgkg -1 ), acceptable precision (RSD: 0.7-19.1%), satisfactory recovery (69-119%) and high enrichment factors (20-722). Several obtained LOQs are below the MRLs established by the European Commission; therefore, the method could be applied for pesticides determination in routing analysis and custom laboratories. Moreover, this method has shown to be suitable for determination of some of the studied pesticides in lime, melon, papaya, banana, tomato, and lettuce. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optimization and Validation of Thermal Desorption Gas Chromatography-Mass Spectrometry for the Determination of Polycyclic Aromatic Hydrocarbons in Ambient Air

PubMed Central

Durana, Nieves; García, José Antonio; Gómez, María Carmen; Alonso, Lucio

2018-01-01

Thermal desorption (TD) coupled with gas chromatography/mass spectrometry (TD-GC/MS) is a simple alternative that overcomes the main drawbacks of the solvent extraction-based method: long extraction times, high sample manipulation, and large amounts of solvent waste. This work describes the optimization of TD-GC/MS for the measurement of airborne polycyclic aromatic hydrocarbons (PAHs) in particulate phase. The performance of the method was tested by Standard Reference Material (SRM) 1649b urban dust and compared with the conventional method (Soxhlet extraction-GC/MS), showing a better recovery (mean of 97%), precision (mean of 12%), and accuracy (±25%) for the determination of 14 EPA PAHs. Furthermore, other 15 nonpriority PAHs were identified and quantified using their relative response factors (RRFs). Finally, the proposed method was successfully applied for the quantification of PAHs in real 8 h-samples (PM10), demonstrating its capability for determination of these compounds in short-term monitoring. PMID:29854561

Cloud-point extraction and reversed-phase high-performance liquid chromatography for the determination of synthetic phenolic antioxidants in edible oils.

PubMed

Chen, Miao; Xia, Qinghai; Liu, Mousheng; Yang, Yaling

2011-01-01

A cloud-point extraction (CPE) method using Triton X-114 (TX-114) nonionic surfactant was developed for the extraction and preconcentration of propyl gallate (PG), tertiary butyl hydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) from edible oils. The optimum conditions of CPE were 2.5% (v/v) TX-114, 0.5% (w/v) NaCl and 40 min equilibration time at 50 °C. The surfactant-rich phase was then analyzed by reversed-phase high-performance liquid chromatography with ultraviolet detection at 280 nm, using a gradient mobile phase consisting of methanol and 1.5% (v/v) acetic acid. Under the studied conditions, 4 synthetic phenolic antioxidants (SPAs) were successfully separated within 24 min. The limits of detection (LOD) were 1.9 ng mL(-1) for PG, 11 ng mL(-1) for TBHQ, 2.3 ng mL(-1) for BHA, and 5.9 ng mL(-1) for BHT. Recoveries of the SPAs spiked into edible oil were in the range 81% to 88%. The CPE method was shown to be potentially useful for the preconcentration of the target analytes, with a preconcentration factor of 14. Moreover, the method is simple, has high sensitivity, consumes much less solvent than traditional methods, and is environment-friendly. Practical Application: The method established in this article uses less organic solvent to extract SPAs from edible oils; it is simple, highly sensitive and results in no pollution to the environment.

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-ultraviolet detection to determination of opium alkaloids in human plasma.

PubMed

Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba; Pirsaheb, Meghdad

2013-11-01

A novel, simple, rapid and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine opium alkaloids in human plasma. During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. Some effective parameters on extraction were studied and optimized. Under the optimum conditions (extraction solvent: 30.0 μl 1-undecanol; disperser solvent: 470 μl acetone; pH: 9; salt addition: 1%(w/v) NaCl and extraction time: 0.5 min), calibration curves are linear in the range of 1.5-1000 μgl(-1) and limit of detections (LODs) are in the range of 0.5-5 μgl(-1). The relative standard deviations (RSDs) for 100 μgl(-1) of morphine and codeine, 10.0 μgl(-1) of papaverine and 20.0 μgl(-1) of noscapine in diluted human plasma are in the range of 4.3-7.4% (n=5). Finally, the method was successfully applied in the determination of opium alkaloids in the actual human plasma samples. The relative recoveries of plasma samples spiked with alkaloids are 88-110.5%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of opium alkaloids in human plasma. Copyright © 2013 Elsevier B.V. All rights reserved.

Miniaturized hollow fibre assisted liquid-phase microextraction and gas chromatography for determination of trace concentration of sufentanil and alfentanil in biological samples.

PubMed

Fakhari, Ali Reza; Tabani, Hadi; Nojavan, Saeed

2013-07-01

A simple and highly sensitive method that involves miniaturized hollow fibre assisted liquid-phase microextraction with gas chromatography-flame ionization detector was developed for the determination of trace concentration of sufentanil and alfentanil in biological samples. These drugs were extracted from 5 ml of aqueous solution with pH 10.0 into an organic extracting solvent (1-octanol) impregnated in the pores and lumen of a hollow fibre. After extraction for a prescribed time, 2.0 µl of the extraction solvent was injected directly in to the GC injection port. Under the optimized conditions, (1-octanol as extracting solvent, stirring rate of 700 rpm, 15% (w/v) salt addition, pH 10.0 and 25 min sampling time at 50 °C) large enrichment factors of 535 and 420 were achieved for sufentanil and alfentanil, respectively. Dynamic linear ranges were in the range of 0.05 to 500 ng/ml for sufentanil and 0.1 to 500 ng/ml for alfentanil. Limits of detection 0.01 and 0.02 ng/ml were obtained for sufentanil and alfentanil, respectively. The percent relative intra-day and inter-day standard deviations were found to be less than 8.4% (n = 5). Finally, this method was successfully applied for the separation, preconcentration and determination of trace concentration of sufentanil and alfentanil in plasma and urine samples. Copyright © 2012 John Wiley & Sons, Ltd.

Using dispersive liquid-liquid microextraction and liquid chromatography for determination of guaifenesin enantiomers in human urine.

PubMed

Hatami, Mehdi; Farhadi, Khalil; Abdollahpour, Assem

2011-11-01

A simple, rapid, and efficient method, dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography-fluorescence detector, has been developed for the determination of guaifenesin (GUA) enantiomers in human urine samples after an oral dose administration of its syrup formulation. Urine samples were collected during the time intervals 0-2, 2-4, and 4-6 h and concentration and ratio of two enantiomers was determined. The ratio of R-(-) to S-(+) enantiomer concentrations in urine showed an increase with time, with R/S ratios of 0.66 at 2 h and 2.23 at 6 h. For microextraction process, a mixture of extraction solvent (dichloromethane, 100 μL) and dispersive solvent (THF, 1 mL) was rapidly injected into 5.0 mL diluted urine sample for the formation of cloudy solution and extraction of enantiomers into the fine droplets of CH(2)Cl(2). After optimization of HPLC enantioselective conditions, some important parameters, such as the kind and volume of extraction and dispersive solvents, extraction time, temperature, pH, and salt effect were optimized for dispersive liquid-liquid microextraction process. Under the optimum extraction condition, the method yields a linear calibration curve in the concentration range from 10 to 2000 ng/mL for target analytes. LOD was 3.00 ng/mL for both of the enantiomers. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tablet-effervescence-assisted dissolved carbon flotation for the extraction of four triazole fungicides in water by gas chromatography with mass spectrometry.

PubMed

Wei, Qizhen; Song, Zhiyu; Nie, Jing; Xia, Hailun; Chen, Fujiang; Li, Zuguang; Lee, Mawrong

2016-12-01

A pretreatment method named tablet-effervescence-assisted dissolved carbon flotation was introduced for the determination of four triazole fungicides in environmental water. In this method, the use of effervescent tablet composed of nontoxic sodium carbonate and sodium dihydrogen phosphate could generate CO 2 in situ to assist the dispersion of extraction solvent and to accelerate mass transfer of target analytes. In addition, the simple phase separation simply based on the rising of low-density organic solvent from the aqueous phase was applied rather than the application of apparatus, which demonstrated the potential for on-site extraction in the field. The experimental variables, including the composition of effervescent tablets, amount of effervescent tablets, types and volume of extraction solvent, were investigated. Under the optimized conditions, the method showed good linearity for myclobutanil, tebuconazole, epoxiconazole, and difenoconazole in the range of 1-100 μg/L. The limits of detection and the limits of quantification were within the range of 0.15-0.26 and 0.49-0.86 μg/L, respectively. The obtained correlation coefficients varied from 0.997 to 0.999, and suitable enrichment factors were 422-589. The recoveries were 82.5-112.9% with relative standard deviations of 4.7-13.5%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multiclass screening method based on solvent extraction and liquid chromatography-tandem mass spectrometry for the determination of antimicrobials and mycotoxins in egg.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; Piovesana, Susy; Samperi, Roberto; Laganà, Aldo

2012-12-14

A QuEChERS (Quick Easy Cheap Effective Rugged Safe)-like extraction method was developed for the simultaneous analysis of veterinary drugs and mycotoxins in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray (ESI) source. Various classes of antimicrobials (tetracyclines, ionophores, coccidiostats, penicillins, cephalosporins, fluoroquinolones, sulfonamides) and mycotoxins (enniatins, beauvericin, ochratoxins, aflatoxins) were considered for the development of this method. Particular attention was devoted to extraction optimization: different solvents (acetone, acetonitrile and methanol), different pH values and different sample to extracting volume ratios were tested and evaluated in terms of recovery, relative standard deviation (RSD) and ESI signal suppression due to matrix effect. Chromatographic and mass spectrometric conditions were optimized to obtain the best instrumental performances for most of the analytes. Quantitative analysis was performed by means of matrix-matched calibration, in a range that varied depending on the analyte and its established maximum limit, when there was one. Recoveries at 100 μg kg(-1) spiking level were >62% (3

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.

Integration of phase separation with ultrasound-assisted salt-induced liquid-liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography.

PubMed

Wang, Huili; Gao, Ming; Wang, Mei; Zhang, Rongbo; Wang, Wenwei; Dahlgren, Randy A; Wang, Xuedong

2015-03-15

Herein, we developed a novel integrated device to perform phase separation based on ultrasound-assisted salt-induced liquid-liquid microextraction for determination of five fluoroquinones (FQs) in human body fluids. The integrated device consisted of three simple HDPE components used to separate the extraction solvent from the aqueous phase prior to retrieving the extractant. A series of extraction parameters were optimized using the response surface method based on central composite design. Optimal conditions consisted of 945μL acetone extraction solvent, pH 2.1, 4.1min stir time, 5.9g Na2SO4, and 4.0min centrifugation. Under optimized conditions, the limits of detection (at S/N=3) were 0.12-0.66μgL(-1), the linear range was 0.5-500μgL(-1) and recoveries were 92.6-110.9% for the five FQs extracted from plasma and urine. The proposed method has several advantages, such as easy construction from inexpensive materials, high extraction efficiency, short extraction time, and compatibility with HPLC analysis. Thus, this method shows excellent prospects for sample pretreatment and analysis of FQs in human body fluids. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

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.

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.

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.

Optimisation for subcritical fluid extraction of 17-methyltestosterone with 1,1,1,2-tetrafluoroethane for HPLC analysis.

PubMed

Han, Yuqian; Ma, Qinchuan; Lu, Jie; Xue, Yong; Xue, Changhu

2012-12-15

A simple, rapid and sensitive method was developed for determination of 17α-methyltestosterone in aquatic products by extraction with subcritical 1,1,1,2-tetrafluoroethane (R134a) extraction and high performance liquid chromatography (HPLC). Response surface methodology (RSM) was adopted to optimise extraction pressure, temperature and co-solvent volume. The optimum extraction conditions predicted within the experimental ranges were as follows: pressure 5 MPa, temperature 31°C, and co-solvent volume 3.35ml. The analysis was carried out on XDB-C(18) column (4.6 mm × 250 mm, 5 μm) with the mobile phase acetonitrile-water (55:45, v/v), flow rate 0.8 ml/min, temperature 30°C and wavelength 245 nm. Good linearity of detection was obtained for 17α-methyltestosterone between concentrations of 50-250 ng/ml, r(2)=0.999. The method was validated using samples fortified with 17α-methyltestosterone at levels of 10, 30 and 50 ng/g, the mean recovery exceeds 90%, and the RSD values were less than 10%. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

Easy, fast and environmental friendly method for the simultaneous extraction of the 16 EPA PAHs using magnetic molecular imprinted polymers (mag-MIPs).

PubMed

Villar-Navarro, Mercedes; Martín-Valero, María Jesús; Fernández-Torres, Rut Maria; Callejón-Mochón, Manuel; Bello-López, Miguel Ángel

2017-02-15

An easy and environmental friendly method, based on the use of magnetic molecular imprinted polymers (mag-MIPs) is proposed for the simultaneous extraction of the 16 U.S. EPA polycyclic aromatic hydrocarbons (PAHs) priority pollutants. The mag-MIPs based extraction protocol is simple, more sensitive and low organic solvent consuming compared to official methods and also adequate for those PAHs more retained in the particulate matter. The new proposed extraction method followed by HPLC determination has been validated and applied to different types of water samples: tap water, river water, lake water and mineral water. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

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.

[Determination of carbendazim and thiabendazole in tomatoes by solid-phase microextraction coupled with high performance liquid chromatography and fluorescence detection].

PubMed

Hu, Yanxue; Yang, Xiumin; Wang, Zhi; Wang, Chun; Zhao, Jin

2005-11-01

A novel method for the determination of carbendazim (MBC) and thiabendazole (TBZ) in tomatoes by solid-phase microextraction (SPME) coupled with high performance liquid chromatography (HPLC) and fluorescence detection was developed. The experimental conditions of SPME, including extraction fiber, extraction time, extraction temperature, desorption time, desorption solvent, desorption mode, pH value, organic solvent and ionic strength, and HPLC conditions were optimized. The SPME for MBC and TBZ was performed on a 65 microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 50 min at room temperature with the solution being stirred at 1 100 r/min. The florescence detection was made at 315 nm with excitation wavelength at 280 nm. The method is linear for MBC and TBZ over the range assayed from 0.01 to 1.0 mg/kg tomatoes with the detection limits of 0.003 mg/kg and 0. 001 mg/kg and the correlation coefficients of 0.995 8 and 0.996 7, respectively. The average recoveries for MBC and TBZ were 83.5% and 85.6% with the relative standard deviations (RSDs) of 6.5% and 3.8%, respectively. The method is fast, simple, sensitive, solvent-free and suitable for the determination of MBC and TBZ in tomatoes.

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.

Simultaneous dispersive liquid-liquid microextraction derivatisation and gas chromatography mass spectrometry analysis of subcritical water extracts of sweet and sour cherry stems.

PubMed

Švarc-Gajić, Jaroslava; Clavijo, Sabrina; Suárez, Ruth; Cvetanović, Aleksandra; Cerdà, Víctor

2018-03-01

Cherry stems have been used in traditional medicine mostly for the treatment of urinary tract infections. Extraction with subcritical water, according to its selectivity, efficiency and other aspects, differs substantially from conventional extraction techniques. The complexity of plant subcritical water extracts is due to the ability of subcritical water to extract different chemical classes of different physico-chemical properties and polarities in a single run. In this paper, dispersive liquid-liquid microextraction (DLLME) with simultaneous derivatisation was optimised for the analysis of complex subcritical water extracts of cherry stems to allow simple and rapid preparation prior to gas chromatography-mass spectrometry (GC-MS). After defining optimal extracting and dispersive solvents, the optimised method was used for the identification of compounds belonging to different chemical classes in a single analytical run. The developed sample preparation protocol enabled simultaneous extraction and derivatisation, as well as convenient coupling with GC-MS analysis, reducing the analysis time and number of steps. The applied analytical protocol allowed simple and rapid chemical screening of subcritical water extracts and was used for the comparison of subcritical water extracts of sweet and sour cherry stems. Graphical abstract DLLME GC MS analysis of cherry stem extracts obtained by subcritical water.

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...

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.

Matrix solid-phase dispersion extraction followed by high performance liquid chromatography-diode array detection and ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometer method for the determination of the main compounds from Carthamus tinctorius L. (Hong-hua).

PubMed

Hong, Bo; Wang, Zhe; Xu, Tianjiao; Li, Chengchong; Li, Wenjing

2015-03-25

A simple and low-cost method based on matrix solid-phase dispersion (MSPD) extraction, HPLC separation, diode array detection and UPLC-Q-TOF-MS have been developed for the determination of Hydroxysafflor yellow A (HSYA), Kaempferol and other main compounds in Carthamus tinctorius. The experimental parameters that may affect the MSPD method, including dispersing sorbent, ratio of dispersing sorbent to sample, elution solvent, and volume of the elution solvent were examined and optimized. The optimized conditions were determined to be that silica gel was used as dispersing sorbent, the ratio of silica gel to sample mass was selected to be 3:1, and 10 mL of methanol: water (1:3, v:v) was used as elution solvent. The highest extraction yields of the two compounds were obtained under the optimized conditions. The method showed good linearity (r(2)≥0.999 2) and precision (RSD≤3.4%) for HSYA and Kaempferol, with the limits of detection of 35.2 and 14.5 ng mL(-1), respectively. The recoveries were in the range of 92.62-101.7% with RSD values ranging from 1.5 to 3.5%. At the meanwhile, there were 21 compounds in the extraction by MSPD method were identified by TOF-MS method to improve the quality control for safflower. Comparing to ultrasonic and soxhlet methods, the proposed MSPD procedure was more convenient and less time-consuming with reduced requirements on sample and solvent amounts. The proposed procedure was applied to analyze four real samples that were collected from different localities. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Determination of Four Major Saponins in Skin and Endosperm of Seeds of Horse Chestnut (Aesculus Hippocastanum L.) Using High Performance Liquid Chromatography with Positive Confirmation by Thin Layer Chromatography.

PubMed

Abudayeh, Zead Helmi Mahmoud; Al Azzam, Khaldun Mohammad; Naddaf, Ahmad; Karpiuk, Uliana Vladimirovna; Kislichenko, Viktoria Sergeevna

2015-11-01

To separate and quantify four major saponins in the extracts of the skin and the endosperm of seeds of horse chestnut (Aesculus hippocastanum L.) using ultrasonic solvent extraction followed by a high performance liquid chromatography-diode array detector (HPLC-DAD) with positive confirmation by thin layer chromatography (TLC). The saponins: escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted using ultrasonic extraction method. The optimized extraction conditions were: 70% methanol as extraction solvent, 80 °C as extraction temperature, and the extraction time was achieved in 4 hours. The HPLC conditions used: Zorbax SB-ODS-(150 mm × 2.1 mm, 3 μm) column, acetonitrile and 0.10% phosphoric acid solution (39:61 v/v) as mobile phase, flow rate was 0.5 mL min(-1) at 210 nm and 230 nm detection. The injection volume was 10 μL, and the separation was carried out isothermally at 30 °C in a heated chamber. The results indicated that the developed HPLC method is simple, sensitive and reliable. Moreover, the content of escins in seeds decreased by more than 30% in endosperm and by more than 40% in skin upon storage for two years. This assay can be readily utilized as a quality control method for horse chestnut and other related medicinal plants.

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.

Multi-residue determination of 115 veterinary drugs and pharmaceutical residues in milk powder, butter, fish tissue and eggs using liquid chromatography-tandem mass spectrometry.

PubMed

Dasenaki, Marilena E; Thomaidis, Nikolaos S

2015-06-23

A simple and sensitive multi-residue method for the determination of 115 veterinary drugs and pharmaceuticals, belonging in more than 20 different classes, in butter, milk powder, egg and fish tissue has been developed. The method involves a simple generic solid-liquid extraction step (solvent extraction, SE) with 0.1% formic acid in aqueous solution of EDTA 0.1% (w/v)-acetonitrile (ACN)-methanol (MeOH) (1:1:1, v/v) with additional ultrasonic-assisted extraction. Precipitation of lipids and proteins was promoted by subjecting the extracts at very low temperature (-23°C) for 12h. Further cleanup with hexane ensures fat removal from the matrix. Analysis was performed by liquid chromatography coupled with electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS). Two separate runs were performed for positive and negative ionization in multiple reaction monitoring mode (MRM). Particular attention was devoted to extraction optimization: different sample-to-extracting volume ratios, different concentrations of formic acid in the extraction solvent and different ultrasonic extraction temperatures were tested in butter, egg and milk powder samples. The method was also applied in fish tissue samples. It was validated, on the basis of international guidelines, for all four matrices. Quantitative analysis was performed by means of standard addition calibration. For over 80% of the analytes, the recoveries were between 50% and 120% in all matrices studied, with RSD values in the range of 1-18%. Limits of detection (LODs) and quantification (LOQs) ranged from 0.008 μg kg(-1) (oxfendazole in butter) to 3.15 μg kg(-1) (hydrochlorthiazide in egg). The evaluated method provides reliable screening, quantification, and identification of 115 veterinary drug and pharmaceutical residues in foods of animal origin and has been successfully applied in real samples. Copyright © 2015 Elsevier B.V. All rights reserved.

A simple method for determination of carmine in food samples based on cloud point extraction and spectrophotometric detection.

PubMed

Heydari, Rouhollah; Hosseini, Mohammad; Zarabi, Sanaz

2015-01-01

In this paper, a simple and cost effective method was developed for extraction and pre-concentration of carmine in food samples by using cloud point extraction (CPE) prior to its spectrophotometric determination. Carmine was extracted from aqueous solution using Triton X-100 as extracting solvent. The effects of main parameters such as solution pH, surfactant and salt concentrations, incubation time and temperature were investigated and optimized. Calibration graph was linear in the range of 0.04-5.0 μg mL(-1) of carmine in the initial solution with regression coefficient of 0.9995. The limit of detection (LOD) and limit of quantification were 0.012 and 0.04 μg mL(-1), respectively. Relative standard deviation (RSD) at low concentration level (0.05 μg mL(-1)) of carmine was 4.8% (n=7). Recovery values in different concentration levels were in the range of 93.7-105.8%. The obtained results demonstrate the proposed method can be applied satisfactory to determine the carmine in food samples. Copyright © 2015 Elsevier B.V. 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...

Ultrasound-assisted extraction of azadirachtin from dried entire fruits of Azadirachta indica A. Juss. (Meliaceae) and its determination by a validated HPLC-PDA method.

PubMed

de Paula, Joelma Abadia Marciano; Brito, Lucas Ferreira; Caetano, Karen Lorena Ferreira Neves; de Morais Rodrigues, Mariana Cristina; Borges, Leonardo Luiz; da Conceição, Edemilson Cardoso

2016-01-01

Azadirachta indica A. Juss., also known as neem, is a Meliaceae family tree from India. It is globally known for the insecticidal properties of its limonoid tetranortriterpenoid derivatives, such as azadirachtin. This work aimed to optimize the azadirachtin ultrasound-assisted extraction (UAE) and validate the HPLC-PDA analytical method for the measurement of this marker in neem dried fruit extracts. Box-Behnken design and response surface methodology (RSM) were used to investigate the effect of process variables on the UAE. Three independent variables, including ethanol concentration (%, w/w), temperature (°C), and material-to-solvent ratio (gmL(-1)), were studied. The azadirachtin content (µgmL(-1)), i.e., dependent variable, was quantified by the HPLC-PDA analytical method. Isocratic reversed-phase chromatography was performed using acetonitrile/water (40:60), a flow of 1.0mLmin(-1), detection at 214nm, and C18 column (250×4.6mm(2), 5µm). The primary validation parameters were determined according to ICH guidelines and Brazilian legislation. The results demonstrated that the optimal UAE condition was obtained with ethanol concentration range of 75-80% (w/w), temperature of 30°C, and material-to-solvent ratio of 0.55gmL(-1). The HPLC-PDA analytical method proved to be simple, selective, linear, precise, accurate and robust. The experimental values of azadirachtin content under optimal UAE conditions were in good agreement with the RSM predicted values and were superior to the azadirachtin content of percolated extract. Such findings suggest that UAE is a more efficient extractive process in addition to being simple, fast, and inexpensive. Copyright © 2015 Elsevier B.V. All rights reserved.

Conventional and Accelerated-Solvent Extractions of Green Tea (Camellia sinensis) for Metabolomics-based Chemometrics

PubMed Central

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

2018-01-01

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. PMID:28787673

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

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.

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 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.

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

PubMed

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

2016-04-01

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

Suitable conditions for liquid-phase microextraction using solidification of a floating drop for extraction of fat-soluble vitamins established using an orthogonal array experimental design.

PubMed

Sobhi, Hamid Reza; Yamini, Yadollah; Esrafili, Ali; Abadi, Reza Haji Hosseini Baghdad

2008-07-04

A simple, rapid and efficient microextraction method for the extraction and determination of some fat-soluble vitamins (A, D2, D3) in aqueous samples was developed. For the first time orthogonal array designs (OADs) were employed to screen the liquid-phase microextraction (LPME) method in which few microliters of 1-undecanol were delivered to the surface of the aqueous sample and it was agitated for a selected time. Then sample vial was cooled by inserting it into an ice bath for 5 min. The solidified solvent was transferred into a suitable vial and immediately melted. Then, the extract was directly injected into a high-performance liquid chromatography (HPLC) for analysis. Several factors affecting the microextraction efficiency such as sample solution temperature, stirring speed, volume of the organic solvent, ionic strength and extraction time were investigated and screened using an OA16 (4(5)) matrix. Under the best conditions (temperature, 55 degrees C; stirring speed, 1000 rpm; the volume of extracting solvent, 15.0 microL; no salt addition and extraction time, 60 min), detection limits of the method were in the range of 1.0-3.5 microgL(-1). The relative standard deviations (RSDs) to determine the vitamins at microg L(-1) levels by applying the proposed method varied in the range of 5.1-10.7%. Dynamic linear ranges of 5-500 mugL(-1) with good correlation coefficients (0.9984

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.

Simultaneous extraction and quantification of lamotrigine, phenobarbital, and phenytoin in human plasma and urine samples using solidified floating organic drop microextraction and high-performance liquid chromatography.

PubMed

Asadi, Mohammad; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Abbasi, Bijan

2015-07-01

A novel and simple method based on solidified floating organic drop microextraction followed by high-performance liquid chromatography with ultraviolet detection has been developed for simultaneous preconcentration and determination of phenobarbital, lamotrigine, and phenytoin in human plasma and urine samples. Factors affecting microextraction efficiency such as the type and volume of the extraction solvent, sample pH, extraction time, stirring rate, extraction temperature, ionic strength, and sample volume were optimized. Under the optimum conditions (i.e. extraction solvent, 1-undecanol (40 μL); sample pH, 8.0; temperature, 25°C; stirring rate, 500 rpm; sample volume, 7 mL; potassium chloride concentration, 5% and extraction time, 50 min), the limits of detection for phenobarbital, lamotrigine, and phenytoin were 1.0, 0.1, and 0.3 μg/L, respectively. Also, the calibration curves for phenobarbital, lamotrigine, and phenytoin were linear in the concentration range of 2.0-300.0, 0.3-200.0, and 1.0-200.0 μg/L, respectively. The relative standard deviations for six replicate extractions and determinations of phenobarbital, lamotrigine, and phenytoin at 50 μg/L level were less than 4.6%. The method was successfully applied to determine phenobarbital, lamotrigine, and phenytoin in plasma and urine samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

Determination of rhenium content in molybdenite by ICP-MS after separation of the major matrix by solvent extraction with N-benzoyl-N-phenylhydroxalamine.

PubMed

Li, Jie; Zhong, Li-feng; Tu, Xiang-lin; Liang, Xi-rong; Xu, Ji-feng

2010-05-15

A simple and rapid analytical method for determining the concentration of rhenium in molybdenite for Re-Os dating was developed. The method used isotope dilution-inductively coupled plasma-mass spectrometry (ID-ICP-MS) after the removal of major matrix elements (e.g., Mo, Fe, and W) from Re by solvent extraction with N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform solution. The effect on extraction efficiency of parameters such as pH (HCl concentration), BPHA concentration, and extraction time were also assessed. Under the optimal experimental conditions, the validity of the separation method was accessed by measuring (187)Re/(185)Re values for a molybdenite reference material (JDC). The obtained values were in good agreement with previously measured values of the Re standard. The proposed method was applied to replicate Re-Os dating of JDC and seven samples of molybdenite from the Yuanzhuding large Cu-Mo porphyry deposit. The results demonstrate good precision and accuracy for the proposed method. The advantages of the method (i.e., simplicity, efficiency, short analysis time, and low cost) make it suitable for routine analysis.

Preconcentration and determination of ceftazidime in real samples using dispersive liquid-liquid microextraction and high-performance liquid chromatography with the aid of experimental design.

PubMed

Razmi, Rasoul; Shahpari, Behrouz; Pourbasheer, Eslam; Boustanifar, Mohammad Hasan; Azari, Zhila; Ebadi, Amin

2016-11-01

A rapid and simple method for the extraction and preconcentration of ceftazidime in aqueous samples has been developed using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography analysis. The extraction parameters, such as the volume of extraction solvent and disperser solvent, salt effect, sample volume, centrifuge rate, centrifuge time, extraction time, and temperature in the dispersive liquid-liquid microextraction process, were studied and optimized with the experimental design methods. Firstly, for the preliminary screening of the parameters the taguchi design was used and then, the fractional factorial design was used for significant factors optimization. At the optimum conditions, the calibration curves for ceftazidime indicated good linearity over the range of 0.001-10 μg/mL with correlation coefficients higher than the 0.98, and the limits of detection were 0.13 and 0.17 ng/mL, for water and urine samples, respectively. The proposed method successfully employed to determine ceftazidime in water and urine samples and good agreement between the experimental data and predictive values has been achieved. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

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.

A novel dispersive liquid-liquid microextraction based on solidification of floating organic droplet method for determination of polycyclic aromatic hydrocarbons in aqueous samples.

PubMed

Xu, Hui; Ding, Zongqing; Lv, Lili; Song, Dandan; Feng, Yu-Qi

2009-03-16

A new dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (DLLME-SFO) was developed for the determination of five kinds of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. In this method, no specific holder, such as the needle tip of microsyringe and the hollow fiber, is required for supporting the organic microdrop due to the using of organic solvent with low density and proper melting point. Furthermore, the extractant droplet can be collected easily by solidifying it in the lower temperature. 1-Dodecanol was chosen as extraction solvent in this work. A series of parameters that influence extraction were investigated systematically. Under optimal conditions, enrichment factors (EFs) for PAHs were in the range of 88-118. The limit of detections (LODs) for naphthalene, diphenyl, acenaphthene, anthracene and fluoranthene were 0.045, 0.86, 0.071, 1.1 and 0.66ngmL(-1), respectively. Good reproducibility and recovery of the method were also obtained. Compared with the traditional liquid-phase microextraction (LPME) and dispersive liquid-liquid microextraction (DLLME) methods, the proposed method obtained about 2 times higher enrichment factor than those in LPME. Moreover, the solidification of floating organic solvent facilitated the phase transfer. And most importantly, it avoided using high-density and toxic solvent in the traditional DLLME method. The proposed method was successfully applied to determinate PAHs in the environmental water samples. The simple and low-cost method provides an alternative method for the analysis of non-polar compounds in complex environmental water.

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®.

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.

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...

Solvent-Ion Interactions in Salt Water: A Simple Experiment.

ERIC Educational Resources Information Center

Willey, Joan D.

1984-01-01

Describes a procedurally quick, simple, and inexpensive experiment which illustrates the magnitude and some effects of solvent-ion interactions in aqueous solutions. Theoretical information, procedures, and examples of temperature, volume and hydration number calculations are provided. (JN)

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.

Overcoming the challenges of conventional dispersive liquid-liquid microextraction: analysis of THMs in chlorinated swimming pools.

PubMed

Faraji, Hakim; Helalizadeh, Masoumeh; Kordi, Mohammad Reza

2018-01-01

A rapid, simple, and sensitive approach to the analysis of trihalomethanes (THMs) in swimming pool water samples has been developed. The main goal of this study was to overcome or to improve the shortcomings of conventional dispersive liquid-liquid microextraction (DLLME) and to maximize the realization of green analytical chemistry principles. The method involves a simple vortex-assisted microextraction step, in the absence of the dispersive solvent, followed by salting-out effect for the elimination of the centrifugation step. A bell-shaped device and a solidifiable solvent were used to simplify the extraction solvent collection after phase separation. Optimization of the independent variables was performed by using chemometric methods in three steps. The method was statistically validated based on authentic guidance documents. The completion time for extraction was less than 8 min, and the limits of detection were in the range between 4 and 72 ng L -1 . Using this method, good linearity and precision were achieved. The results of THMs determination in different real samples showed that in some cases the concentration of total THMs was more than threshold values of THMs determined by accredited healthcare organizations. This method indicated satisfactory analytical figures of merit. Graphical Abstract A novel green microextraction technique for overcoming the challenges of conventional DLLME. The proposed procedure complies with the principles of green/sustainable analytical chemistry, comprising decreasing the sample size, making easy automation of the process, reducing organic waste, diminishing energy consumption, replacing toxic reagents with safer reagents, and enhancing operator safety.

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 simple, fast and cheap non-SPE screening method for antibacterial residue analysis in milk and liver using liquid chromatography-tandem mass spectrometry.

PubMed

Martins, Magda Targa; Melo, Jéssica; Barreto, Fabiano; Hoff, Rodrigo Barcellos; Jank, Louise; Bittencourt, Michele Soares; Arsand, Juliana Bazzan; Schapoval, Elfrides Eva Scherman

2014-11-01

In routine laboratory work, screening methods for multiclass analysis can process a large number of samples in a short time. The main challenge is to develop a methodology to detect as many different classes of residues as possible, combined with speed and low cost. An efficient technique for the analysis of multiclass antibacterial residues (fluoroquinolones, tetracyclines, sulfonamides and trimethoprim) was developed based on simple, environment-friendly extraction for bovine milk, cattle and poultry liver. Acidified ethanol was used as an extracting solvent for milk samples. Liver samples were treated using EDTA-washed sand for cell disruption, methanol:water and acidified acetonitrile as extracting solvent. A total of 24 antibacterial residues were detected and confirmed using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS), at levels between 10, 25 and 50% of the maximum residue limit (MRL). For liver samples a metabolite (sulfaquinoxaline-OH) was also monitored. A validation procedure was conducted for screening purposes in accordance with European Union requirements (2002/657/EC). The detection capability (CCβ) false compliant rate was less than 5% at the lowest level for each residue. Specificity and ruggedness were also discussed. Incurred and routine samples were analyzed and the method was successfully applied. The results proved that this method can be an important tool in routine analysis, since it is very fast and reliable. Copyright © 2014. Published by Elsevier B.V.

Ionic Liquid Dispersive Liquid-Liquid Microextraction Method for the Determination of Irinotecan, an Anticancer Drug, in Water and Urine Samples Using UV-Vis Spectrophotometry.

PubMed

Uysal, Deniz; Karadaş, Cennet; Kara, Derya

2017-05-01

A new, simple, efficient, and environmentally friendly ionic liquid dispersive liquid-liquid microextraction method was developed for the determination of irinotecan, an anticancer drug, in water and urine samples using UV-Vis spectrophotometry. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the extraction solvent, and ethanol was used as the disperser solvent. The main parameters affecting the extraction efficiency, including sample pH, volume of the ionic liquid, choice of the dispersive solvent and its volume, concentration of NaCl, and extraction and centrifugation times, were investigated and optimized. The effect of interfering species on the recovery of irinotecan was also examined. Under optimal conditions, the LOD (3σ) was 48.7 μg/L without any preconcentration. Because the urine sample was diluted 10-fold, the LOD for urine would be 487 μg/L. However, this could be improved 16-fold if preconcentration using a 40 mL aliquot of the sample is used. The proposed method was successfully applied to the determination of irinotecan in tap water, river water, and urine samples spiked with 10.20 mg/L for the water samples and 8.32 mg/L for the urine sample. The average recovery values of irinotecan determined were 99.1% for tap water, 109.4% for river water, and 96.1% for urine.

A novel method for the rapid detection of benzo(a)pyrene in liquid milk by dimethyl sulfoxide selectively enhanced synchronous fluorescence spectrometry.

PubMed

Lin, Li-Rong; Luo, He-Dong; Li, Xiu-Ying; Li, Na; Zhou, Na; Jia, Yu-Zhu; Liu, Yi-Hong; Li, Yao-Qun

2014-01-01

Based on the high solubility efficiency and strong fluorescence response of benzo(a)pyrene (BaP) in dimethyl sulfoxide in combination with the high-performance derivative constant-energy synchronous fluorescence spectroscopic (DCESFS) technique, a simple, sensitive and economic method was developed for the determination of BaP in liquid milk. This method comprises ultrasound-assisted solvent extraction, solvent replacement and DCESFS detection. No saponification or other tedious clean-up procedures were needed. The recoveries of BaP in different milk samples were greater than 82%. Detection limits in full- and low-fat milk were 0.03 and 0.04 μg kg(-1), respectively.

Organic-Solvent-Free Phase-Transfer Oxidation of Alcohols Using Hydrogen Peroxide

NASA Astrophysics Data System (ADS)

Hulce, Martin; Marks, David W.

2001-01-01

Organic-solvent-free oxidations of alcohols using aqueous hydrogen peroxide in the presence of sodium tungstate and phase-transfer catalysts provide a general, safe, simple, and cost-effective means to prepare ketones. Six representative alcohols, 1-phenylethanol, 1-phenylpropanol, benzhydrol, 4-methylbenzhydrol, cis,trans-4-tert-butylcyclohexanol, and benzyl alcohol are oxidized to the corresponding aldehyde or ketone over 1-3 hours in 81-99% yields. Purities are very high, with only small to trace amounts of starting alcohol remaining. Experiments can be readily designed for one or two 3-hour laboratory periods, integrating the various techniques of extraction, drying, filtration, column chromatography, gas chromatography, NMR and IR spectroscopy, and reaction kinetics.

[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.

Determination of Four Major Saponins in Skin and Endosperm of Seeds of Horse Chestnut (Aesculus Hippocastanum L.) Using High Performance Liquid Chromatography with Positive Confirmation by Thin Layer Chromatography

PubMed Central

Abudayeh, Zead Helmi Mahmoud; Al Azzam, Khaldun Mohammad; Naddaf, Ahmad; Karpiuk, Uliana Vladimirovna; Kislichenko, Viktoria Sergeevna

2015-01-01

Purpose: To separate and quantify four major saponins in the extracts of the skin and the endosperm of seeds of horse chestnut (Aesculus hippocastanum L.) using ultrasonic solvent extraction followed by a high performance liquid chromatography-diode array detector (HPLC-DAD) with positive confirmation by thin layer chromatography (TLC). Methods: The saponins: escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted using ultrasonic extraction method. The optimized extraction conditions were: 70% methanol as extraction solvent, 80 °C as extraction temperature, and the extraction time was achieved in 4 hours. The HPLC conditions used: Zorbax SB-ODS-(150 mm × 2.1 mm, 3 μm) column, acetonitrile and 0.10% phosphoric acid solution (39:61 v/v) as mobile phase, flow rate was 0.5 mL min−1 at 210 nm and 230 nm detection. The injection volume was 10 μL, and the separation was carried out isothermally at 30 °C in a heated chamber. Results: The results indicated that the developed HPLC method is simple, sensitive and reliable. Moreover, the content of escins in seeds decreased by more than 30% in endosperm and by more than 40% in skin upon storage for two years. Conclusion: This assay can be readily utilized as a quality control method for horse chestnut and other related medicinal plants. PMID:26819933

Highly selective solid-phase extraction and large volume injection for the robust gas chromatography-mass spectrometric analysis of TCA and TBA in wines.

PubMed

Insa, S; Anticó, E; Ferreira, V

2005-09-30

A reliable solid-phase extraction (SPE) method for the simultaneous determination of 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA) in wines has been developed. In the proposed procedure 50 mL of wine are extracted in a 1 mL cartridge filled with 50 mg of LiChrolut EN resins. Most wine volatiles are washed up with 12.5 mL of a water:methanol solution (70%, v/v) containing 1% of NaHCO3. Analytes are further eluted with 0.6 mL of dichloromethane. A 40 microL aliquot of this extract is directly injected into a PTV injector operated in the solvent split mode, and analysed by gas chromatography (GC)-ion trap mass spectrometry using the selected ion storage mode. The solid-phase extraction, including sample volume and rinsing and elution solvents, and the large volume GC injection have been carefully evaluated and optimized. The resulting method is precise (RSD (%) < 6% at 100 ng L(-1)), sensitive (LOD were 0.2 and 0.4 ng/L for TCA and TBA, respectively), robust (the absolute recoveries of both analytes are higher than 80% and consistent wine to wine) and friendly to the GC-MS system (the extract is clean, simple and free from non-volatiles).

A Novel Liquid-Liquid Extraction for the Determination of Sertraline in Tap Water and Waste Water at Trace Levels by GC-MS.

PubMed

Koçoğlu, Elif Seda; Bakırdere, Sezgin; Keyf, Seyfullah

2017-09-01

A simple, green and fast analytical method was developed for the determination of sertraline in tap and waste water samples at trace levels by using supportive liquid-liquid extraction with gas chromatography-mass spectrometry. Different parameters affecting extraction efficiency such as types and volumes of extraction and supporter solvents, extraction period, salt type and amount were optimized to get lower detection limits. Ethyl acetate was selected as optimum extraction solvent. In order to improve the precision, anthracene-D10 was used as an internal standard. The calibration plot of sertraline was linear from 1.0 to 1000 ng/mL with a correlation coefficient of 0.999. The limit of detection value under the optimum conditions was found to be 0.43 ng/mL. In real sample measurements, spiking experiments were performed to check the reliability of the method for these matrices. The spiking experiments yielded satisfactory recoveries of 91.19 ± 2.48%, 90.48 ± 5.19% and 95.46 ± 6.56% for 100, 250 and 500 ng/mL sertraline for tap water, and 85.80 ± 2.15% and 92.43 ± 4.02% for 250 and 500 ng/mL sertraline for waste water.

[Isolation and purification of seven catechin compounds from fresh tea leaves by semi-preparative liquid chromatography].

PubMed

Gong, Zhihong; Chen, Si; Gao, Jiangtao; Li, Meihong; Wang, Xiaxia; Lin, Jun; Yu, Xiaomin

2017-11-08

An effective and simple method was established to simultaneously purify seven tea catechins (gallocatechin (GC), epigallocatechin (EGC), catechin (C), epigallocatechin-3- O -gallate (EGCG), epicatechin (EC), epigallocatechin-3- O -(3- O -methyl)-gallate (EGCG3"Me) and epicatechin-3- O -gallate (ECG)) from fresh tea leaves by semi-preparative high performance liquid chromatography (HPLC). Fresh leaves of Tieguanyin tea were successively extracted with methanol and chloroform. Then crude catechins were precipitated from the aqueous fraction of chloroform extraction by adding lead subacetate. Crude catechins were used for the isolation of the seven target catechin compounds by semi-preparative HPLC. Methanol-water and acetonitrile-water were sequentially used as mobile phases. After two rounds of semi-preparative HPLC, all target compounds were achieved with high purities (>90%). The proposed method was tested on two additional tea cultivars and showed similar results. This method demonstrated a simple and efficient strategy based on solvent extraction, ion precipitation and semi-preparative HPLC for the preparation of multiple catechins from tea leaves.

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.

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

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.

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

Effect of Organic Solvents on Microalgae Growth, Metabolism and Industrial Bioproduct Extraction: A Review.

PubMed

Miazek, Krystian; Kratky, Lukas; Sulc, Radek; Jirout, Tomas; Aguedo, Mario; Richel, Aurore; Goffin, Dorothee

2017-07-04

In this review, the effect of organic solvents on microalgae cultures from molecular to industrial scale is presented. Traditional organic solvents and solvents of new generation-ionic liquids (ILs), are considered. Alterations in microalgal cell metabolism and synthesis of target products (pigments, proteins, lipids), as a result of exposure to organic solvents, are summarized. Applications of organic solvents as a carbon source for microalgal growth and production of target molecules are discussed. Possible implementation of various industrial effluents containing organic solvents into microalgal cultivation media, is evaluated. The effect of organic solvents on extraction of target compounds from microalgae is also considered. Techniques for lipid and carotenoid extraction from viable microalgal biomass (milking methods) and dead microalgal biomass (classical methods) are depicted. Moreover, the economic survey of lipid and carotenoid extraction from microalgae biomass, by means of different techniques and solvents, is conducted.

Effect of Organic Solvents on Microalgae Growth, Metabolism and Industrial Bioproduct Extraction: A Review

PubMed Central

Miazek, Krystian; Sulc, Radek; Jirout, Tomas; Aguedo, Mario; Goffin, Dorothee

2017-01-01

In this review, the effect of organic solvents on microalgae cultures from molecular to industrial scale is presented. Traditional organic solvents and solvents of new generation-ionic liquids (ILs), are considered. Alterations in microalgal cell metabolism and synthesis of target products (pigments, proteins, lipids), as a result of exposure to organic solvents, are summarized. Applications of organic solvents as a carbon source for microalgal growth and production of target molecules are discussed. Possible implementation of various industrial effluents containing organic solvents into microalgal cultivation media, is evaluated. The effect of organic solvents on extraction of target compounds from microalgae is also considered. Techniques for lipid and carotenoid extraction from viable microalgal biomass (milking methods) and dead microalgal biomass (classical methods) are depicted. Moreover, the economic survey of lipid and carotenoid extraction from microalgae biomass, by means of different techniques and solvents, is conducted. PMID:28677659

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.

Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of synthetic musk fragrances in aqueous matrices by gas chromatography-mass spectrometry.

PubMed

Homem, Vera; Alves, Alice; Alves, Arminda; Santos, Lúcia

2016-01-01

A rapid and simple method for the simultaneous determination of twelve synthetic musks in water samples, using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was successfully developed. The influence of seven factors (volume of the extraction solvent and disperser solvent, sample volume, extraction time, ionic strength, type of extraction and disperser solvent) affecting the UA-DLLME extraction efficiency was investigated using a screening design. The significant factors were selected and optimised employing a central composite design: 80 μL of chloroform, 880 μL of acetonitrile, 6 mL of sample volume, 3.5% (wt) of NaCl and 2 min of extraction time. Under the optimised conditions, this methodology was successfully validated for the analysis of 12 synthetic musk compounds in different aqueous samples (tap, sea and river water, effluent and influent wastewater). The proposed method showed enrichment factors between 101 and 115 depending on the analyte, limits of detection in the range of 0.004-54 ng L(-1) and good repeatability (most relative standard deviation values below 10%). No significant matrix effects were found, since recoveries ranged between 71% and 118%. Finally, the method was satisfactorily applied to the analysis of five different aqueous samples. Results demonstrated the existence of a larger amount of synthetic musks in wastewaters than in other water samples (average concentrations of 2800 ng L(-1) in influent and 850 ng L(-1) in effluent). Galaxolide, tonalide and exaltolide were the compounds most detected. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

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...

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.

Cytotoxic Deoxypodophyllotoxin Can Be Extracted in High Purity from Anthriscus sylvestris Roots by Supercritical Carbon Dioxide.

PubMed

Seegers, Christel L C; Tepper, Pieter G; Setroikromo, Rita; Quax, Wim J

2018-05-01

Deoxypodophyllotoxin is present in the roots of Anthriscus sylvestris . This compound is cytotoxic on its own, but it can also be converted into podophyllotoxin, which is in high demand as a precursor for the important anticancer drugs etoposide and teniposide. In this study, deoxypodophyllotoxin is extracted from A. sylvestris roots by supercritical carbon dioxide extraction. The process is simple and scalable. The supercritical carbon dioxide method extracts 75 - 80% of the total deoxypodophyllotoxin content, which is comparable to a single extraction by traditional Soxhlet. However, less polar components are extracted. The activity of the supercritical carbon dioxide extract containing deoxypodophyllotoxin was assessed by demonstrating that the extract arrests A549 and HeLa cells in the G 2 /M phase of the cell cycle. We conclude that biologically active deoxypodophyllotoxin can be extracted from A. sylvestris by supercritical carbon dioxide extraction. The method is solvent free and more sustainable compared to traditional methods. Georg Thieme Verlag KG Stuttgart · New York.

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.

Cloud point extraction and determination of trace trichlorfon by high performance liquid chromatography with ultraviolet-detection based on its catalytic effect on benzidine oxidizing.

PubMed

Zhu, Hai-Zhen; Liu, Wei; Mao, Jian-Wei; Yang, Ming-Min

2008-04-28

4-Amino-4'-nitrobiphenyl, which is formed by catalytic effect of trichlorfon on sodium perborate oxidizing benzidine, is extracted with a cloud point extraction method and then detected using a high performance liquid chromatography with ultraviolet detection (HPLC-UV). Under the optimum experimental conditions, there was a linear relationship between trichlorfon in the concentration range of 0.01-0.2 mgL(-1) and the peak areas of 4-amino-4'-nitrobiphenyl (r=0.996). Limit of detection was 2.0 microgL(-1), recoveries of spiked water and cabbage samples ranged between 95.4-103 and 85.2-91.2%, respectively. It was proved that the cloud point extraction (CPE) method was simple, cheap, and environment friendly than extraction with organic solvents and had more effective extraction yield.

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

PubMed

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

2014-01-01

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

Matrix precipitation: a general strategy to eliminate matrix interference for pharmaceutical toxic impurities analysis.

PubMed

Yang, Xiaojing; Xiong, Xuewu; Cao, Ji; Luan, Baolei; Liu, Yongjun; Liu, Guozhu; Zhang, Lei

2015-01-30

Matrix interference, which can lead to false positive/negative results, contamination of injector or separation column, incompatibility between sample solution and the selected analytical instrument, and response inhibition or even quenching, is commonly suffered for the analysis of trace level toxic impurities in drug substance. In this study, a simple matrix precipitation strategy is proposed to eliminate or minimize the above stated matrix interference problems. Generally, a sample of active pharmaceutical ingredients (APIs) is dissolved in an appropriate solvent to achieve the desired high concentration and then an anti-solvent is added to precipitate the matrix substance. As a result, the target analyte is extracted into the mixed solution with very less residual of APIs. This strategy has the characteristics of simple manipulation, high recovery and excellent anti-interference capability. It was found that the precipitation ratio (R, representing the ability to remove matrix substance) and the proportion of solvent (the one used to dissolve APIs) in final solution (P, affecting R and also affecting the method sensitivity) are two important factors of the precipitation process. The correlation between R and P was investigated by performing precipitation with various APIs in different solvent/anti-solvent systems. After a detailed mathematical reasoning process, P=20% was proved to be an effective and robust condition to perform the precipitation strategy. The precipitation method with P=20% can be used as a general strategy for toxic impurity analysis in APIs. Finally, several typical examples are described in this article, where the challenging matrix interference issues have been resolved successfully. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Comparison of extraction techniques and modeling of accelerated solvent extraction for the authentication of natural vanilla flavors.

PubMed

Cicchetti, Esmeralda; Chaintreau, Alain

2009-06-01

Accelerated solvent extraction (ASE) of vanilla beans has been optimized using ethanol as a solvent. A theoretical model is proposed to account for this multistep extraction. This allows the determination, for the first time, of the total amount of analytes initially present in the beans and thus the calculation of recoveries using ASE or any other extraction technique. As a result, ASE and Soxhlet extractions have been determined to be efficient methods, whereas recoveries are modest for maceration techniques and depend on the solvent used. Because industrial extracts are obtained by many different procedures, including maceration in various solvents, authenticating vanilla extracts using quantitative ratios between the amounts of vanilla flavor constituents appears to be unreliable. When authentication techniques based on isotopic ratios are used, ASE is a valid sample preparation technique because it does not induce isotopic fractionation.

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.

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.

Analysis of malachite green in aquatic products by carbon nanotube-based molecularly imprinted - matrix solid phase dispersion.

PubMed

Wang, Yu; Chen, Ligang

2015-10-01

A simple method based on matrix solid phase dispersion (MSPD) using molecularly imprinted polymers (MIPs) as sorbents for selective extraction of malachite green (MG) from aquatic products was developed. The MIPs were prepared by using carbon nanotube as support, MG as template, methacrylic acid as functional monomer, ethyleneglycol dimethacrylate as crosslinker and methylene chloride as solvent. The MIPs were characterized by Fourier transform infrared spectrometry and transmission electron microscopy. The isothermal adsorption, kinetics absorption and selective adsorption experiments were carried out. We optimized the extraction conditions as follows: the ratio of MIPs to sample was 2:3, the dispersion time was 15min, washing solvent was 4mL 50% aqueous methanol and elution solvent was 3mL methanol-acetic acid (98: 2, v/v). Once the MSPD process was completed, the MG extracted from aquatic products was determined by high performance liquid chromatography. The detection limit of MG was 0.7μgkg(-1). The relative standard deviations of intra-day and inter-day were obtained in the range of 0.9%-4.7% and 3.4%-9.8%, respectively. In order to evaluate the applicability and reliability of the proposed method, it was applied to determine MG in different aquatic products samples including fish, shrimp, squid and crabs. The satisfied recoveries were in the range of 89.2%-104.6%. The results showed that this method is faster, simpler and makes extraction and purification in the same system. Copyright © 2015 Elsevier B.V. All rights reserved.

Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid-liquid extraction for the analysis of benzimidazole residues in farm fish samples.

PubMed

Tejada-Casado, Carmen; Lara, Francisco J; García-Campaña, Ana M; Del Olmo-Iruela, Monsalud

2018-03-30

Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C 18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R 2  ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04-29.9 μg kg -1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method. Copyright © 2018 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...

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.

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

[Studies on the industrial styrene poisoning (Part X). Determination of styrene in biological materials by gas chromatography (author's transl)].

PubMed

Teramoto, K; Horiguchi, S

1980-09-01

For monitoring solvents exposure, it is useful to determine not only metabolites of the solvents in urine but also the solvents themselves in blood and tissues. In a series of studies on the industrial styrene poisoning, we have been determining styrene in blood and other tissues as occasion calls. Our examination of the method is presented in this report. The outline on the method is as follows: Aliquots of 0.5g of tissues being added 5 ml of n-hexane are homogenized by a high-speed homogenizer (Polytoron) for 10 to 30 seconds and the filtrates containing extracts are analyzed for styrene by gas chromatography. The linearity was ascertained from the calibration curve obtained by adding the known quantities of styrene (4, 10, 20, 40, 100 ppm) to the blood, liver and adipose tissues of rats. Rates of recoveries of styrene from the above tissues were 92 to 101 per cent. Reproducibility of this method was examined by repeating determinations of styrene in the blood, liver and adipose tissues of rats exposed to 500 ppm styrene for 4 hours, the coefficients of variation being 2.8 to 14.0 per cent. There was an approximately linear relationship between the styrene concentration (0 to 1,000 ppm) of the exposed air and those in the blood of exposed rats. We conclude that our simple and rapid method is applicable to determination of solvents other than styrene in organs and tissues by combining suitable solvents for extraction and packings of gas chromatography.

Extraction of aucubin from seeds of Eucommia ulmoides Oliv. using supercritical carbon dioxide.

PubMed

Li, Hui; Hu, Jiangyu; Ouyang, Hui; Li, Yanan; Shi, Hui; Ma, Chengjin; Zhang, Yongkang

2009-01-01

Supercritical CO2 was used as solvent for the extraction of aucubin from the seeds of Eucommia ulmoides Oliv. The co-solvent composition was tested and extraction conditions were optimized. Results showed that the best co-solvent was a water-ethanol mixture (1 + 3, v/v), and the highest yield was obtained when the extraction was performed under 26 MPa at extraction and separation temperatures of 55 and 30 degrees C for 120 min, using 6 mL co-solvent/g material at a CO2 flow rate of 20 L/h. In a comparison of the supercritical CO2 and Soxhlet extraction methods, the Soxhlet method needed 3 h to extract 10 g material, whereas the supercritical CO2 extraction technique needed only 2 h to extract 100 g material, thus showing a high extraction capability. The supercritical CO2 extraction produced a higher yield, with a lower cost for the extraction. Owing to the advantages of low extraction temperature, high yield, and ease of separating the product from the solvent, supercritical CO2 extraction is likely to be developed into an ideal technique for the extraction of aucubin, a compound with thermal instability, from the seeds of this plant.

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.

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.

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

PubMed Central

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85%) and oleic acid (1.64%–18.97%). Thymoquinone (0.72%–21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. PMID:28814830

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

PubMed

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P <0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

Dispersive liquid-liquid microextraction of copper ions as neocuproine complex in environmental aqueous samples.

PubMed

Shariati, Shahab; Golshekan, Mostafa

2011-06-01

In the present study, a simple and efficient extraction method based on dispersive liquid-liquid microextraction prior to UV-Vis spectrophotometry was developed for the preconcentration and determination of copper ions in environmental samples. Briefly, cupric ions (Cu II) were reduced to cuprous (Cu I) with addition of hydroxyl amine hydrochloride and formed hydrophobic chelates with neocuproine. Then, a proper mixture of acetonitrile (as dispersive solvent) and choloroform (as extraction solvent) was rapidly injected into the solution and a cloudy solution was formed. After centrifuging, choloroform was sedimented at the bottom of a conical tube and diluted with 100 µL of methanol for further UV-Vis spectrophotometry measurement. An orthogonal array design (OAD) was employed to study the effects of different parameters on the extraction efficiency. Under the optimum experimental conditions, a preconcentration factor up to 63.6 was achieved for extraction from 5.0 mL of sample solution. The limit of detection (LOD) based on S/N = 3 was 0.33 µg L-1 and the calibration curve was linear in the range of 1-200 µg L-1 with reasonable linearity (r2 > 0.997). Finally, the accuracy of the proposed method was successfully evaluated by determination of trace amounts of copper ions in different water samples and satisfactory results were obtained.

Determination of volatile organic acids in oriental tobacco by needle-based derivatization headspace liquid-phase microextraction coupled to gas chromatography/mass spectrometry.

PubMed

Sun, Shi-Hao; Xie, Jian-Ping; Xie, Fu-Wei; Zong, Yong-Li

2008-02-01

A method coupling needle-based derivatization headspace liquid-phase microextraction with gas chromatography-mass spectrometry (HS-LPME/GC-MS) was developed to determine volatile organic acids in tobacco. The mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and decane was utilized as the solvent for HS-LPME, resulting that extraction and derivatization were simultaneously completed in one step. The solvent served two purposes. First, it pre-concentrated volatile organic acids in the headspace of tobacco sample. Second, the volatile organic acids extracted were derivatized to form silyl derivatives in the drop. The main parameters affecting needle-based derivatization HS-LPME procedure such as extraction and derivatization reagent, microdrop volume, extraction and derivatization time, and preheating temperature and preheating time were optimized. The standard addition approach was essential to obtain accurate measurements by minimizing matrix effects. Good linearity (R(2)> or =0.9804) and good repeatability (RSDs< or =15.3%, n=5) for 16 analytes in spiked standard analytes sample were achieved. The method has the additional advantages that at the same time it is simple, fast, effective, sensitive, selective, and provides an overall profile of volatile organic acids in the oriental tobacco. This paper does offer an alternative approach to determine volatile organic acids in tobacco.

Rapid determination of polycyclic aromatic hydrocarbons in rainwater by liquid-liquid microextraction and LC with core-shell particles column and fluorescence detection.

PubMed

Vinci, Giuliana; Antonelli, Marta L; Preti, Raffaella

2013-02-01

Liquid-liquid microextraction coupled to LC with fluorescence detection for the determination of Environmental Protection Agency's 16 priority pollutant polycyclic aromatic hydrocarbons in rainwater has been developed. The optimization of the extraction method has involved several parameters, including the comparison between an ultrasonic bath and a magnetic stirrer as extractant apparatus, the choice of the extractant solvent, and the optimization of the extraction time. Liquid-liquid microextraction gave good results in terms of recoveries (from 73.6 to 102.8% in rainwater) and repeatability, with a very simple procedure and low solvent consumption. The reported chromatographic method uses a Core-Shell technology column, with particle size <3 μm instead of classical 5-μm particles column. The resulting backpressure was below 300 bar, allowing the use of a conventional HPLC system rather than the more expensive ultrahigh performance LC (UHPLC). An average decrease of 59% in run time and 75% in eluent consumption has been obtained, compared to classical HPLC methods, keeping good separation, sensitivity, and repeatability. The proposed conditions were successfully applied to the determinations of polycyclic aromatic hydrocarbons in genuine rainwater samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Glyoxal and methylglyoxal as urinary markers of diabetes. Determination using a dispersive liquid-liquid microextraction procedure combined with gas chromatography-mass spectrometry.

PubMed

Pastor-Belda, M; Fernández-García, A J; Campillo, N; Pérez-Cárceles, M D; Motas, M; Hernández-Córdoba, M; Viñas, P

2017-08-04

Glyoxal (GO) and methylglyoxal (MGO) are α-oxoaldehydes that can be used as urinary diabetes markers. In this study, their levels were measured using a sample preparation procedure based on salting-out assisted liquid-liquid extraction (SALLE) and dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography-mass spectrometry (GC-MS). The effect of the derivatization reaction with 2,3-diaminonaphthalene, the addition of acetonitrile and sodium chloride to urine, and the DLLME step using the acetonitrile extract as dispersant solvent and carbon tetrachloride as extractant solvent were carefully optimized. Quantification was performed by the internal standard method, using 5-bromo-2-chloroanisole. The intraday and interday precisions were lower than 6%. Limits of detection were 0.12 and 0.06ngmL -1 , and enrichment factors 140 and 130 for GO and MGO, respectively. The concentrations of these α-oxoaldehydes in urine were between 0.9 and 35.8ngg -1 levels (creatinine adjusted). A statistical comparison of the analyte contents of urine samples from non-diabetic and diabetic patients pointed to significant differences (P=0.046, 24 subjects investigated), particularly regarding MGO, which was higher in diabetic patients. The novelty of this study compared with previous procedures lies in the treatment of the urine sample by SALLE based on the addition of acetonitrile and sodium chloride to the urine. The DLLME procedure is performed with a sedimented drop of the extractant solvent, without a surfactant reagent, and using acetonitrile as dispersant solvent. Separation of the analytes was performed using GC-MS detection, being the analytes unequivocal identified. The proposed procedure is the first microextraction method applied to the analysis of urine samples from diabetic and non-diabetic patients that allows a clear differentiation between both groups using a simple analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

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/.

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

Computational screening of biomolecular adsorption and self-assembly on nanoscale surfaces.

PubMed

Heinz, Hendrik

2010-05-01

The quantification of binding properties of ions, surfactants, biopolymers, and other macromolecules to nanometer-scale surfaces is often difficult experimentally and a recurring challenge in molecular simulation. A simple and computationally efficient method is introduced to compute quantitatively the energy of adsorption of solute molecules on a given surface. Highly accurate summation of Coulomb energies as well as precise control of temperature and pressure is required to extract the small energy differences in complex environments characterized by a large total energy. The method involves the simulation of four systems, the surface-solute-solvent system, the solute-solvent system, the solvent system, and the surface-solvent system under consideration of equal molecular volumes of each component under NVT conditions using standard molecular dynamics or Monte Carlo algorithms. Particularly in chemically detailed systems including thousands of explicit solvent molecules and specific concentrations of ions and organic solutes, the method takes into account the effect of complex nonbond interactions and rotational isomeric states on the adsorption behavior on surfaces. As a numerical example, the adsorption of a dodecapeptide on the Au {111} and mica {001} surfaces is described in aqueous solution. Copyright 2009 Wiley Periodicals, Inc.

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.

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

PubMed

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

2018-06-15

Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE-D-HPLC method is a simple, rapid, sensitive and eco-friendly analytical method for the determination of EACA and amino acids in cosmetics. Copyright © 2018 Elsevier B.V. All rights reserved.

[Determination of estrogen residues in drinking water by on-line solid phase extraction based on sol-gel technique coupled with high performance liquid chromatography].

PubMed

Li, Longfei; Su, Min; Shi, Xiaolei; Wang, Yana; Wang, Minmin; He, Jinxing

2014-02-01

A method for the determination of diethylstilbestrol (DES), hexestrol (HEX) and dienestrol (DS) residues in drinking water was established by on-line solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). The material synthesized on the base of sol-gel technology was employed as adsorbent. This material was prepared using 3-aminopropyltriethoxysilane (APTES) as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and acetic acid as the initiator. The synthesized adsorbent showed outstanding property for the estrogen extraction. The estrogen can be caught effectively from water samples and the extraction can be achieved rapidly. Some important parameters, such as pH of sample solution, eluent solvents, loading flow rate, which might influence extraction efficiency, were optimized. The results indicated that the limit of detection (S/N = 3) of the developed method could reach 0.07-0.13 microg/L under the conditions of pH 7.0 of sample solution, methanol and 1% (v/v) acetic acid aqueous solution as the eluent solvent and the loading flow rate of 2 mL/min. The recoveries of the three estrogens from the water samples at three spiked levels ranged from 82.31% to 99.43% with RSD of 1.61%-7.15%. The method was simple, rapid, and suitable to detect the trace residues of estrogens in drinking water.

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

PubMed

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values < or =3-25% (n=5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were > or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

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.

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.

The BUME method: a new rapid and simple chloroform-free method for total lipid extraction of animal tissue

NASA Astrophysics Data System (ADS)

Löfgren, Lars; Forsberg, Gun-Britt; Ståhlman, Marcus

2016-06-01

In this study we present a simple and rapid method for tissue lipid extraction. Snap-frozen tissue (15-150 mg) is collected in 2 ml homogenization tubes. 500 μl BUME mixture (butanol:methanol [3:1]) is added and automated homogenization of up to 24 frozen samples at a time in less than 60 seconds is performed, followed by a 5-minute single-phase extraction. After the addition of 500 μl heptane:ethyl acetate (3:1) and 500 μl 1% acetic acid a 5-minute two-phase extraction is performed. Lipids are recovered from the upper phase by automated liquid handling using a standard 96-tip robot. A second two-phase extraction is performed using 500 μl heptane:ethyl acetate (3:1). Validation of the method showed that the extraction recoveries for the investigated lipids, which included sterols, glycerolipids, glycerophospholipids and sphingolipids were similar or better than for the Folch method. We also applied the method for lipid extraction of liver and heart and compared the lipid species profiles with profiles generated after Folch and MTBE extraction. We conclude that the BUME method is superior to the Folch method in terms of simplicity, through-put, automation, solvent consumption, economy, health and environment yet delivering lipid recoveries fully comparable to or better than the Folch method.

Analysis of carbendazim, benomyl, thiophanate methyl and 2,4-dichlorophenoxyacetic acid in fruits and vegetables after supercritical fluid extraction.

PubMed

Anastassiades, M; Schwack, W

1998-10-30

Simple methods for the analysis of carbendazim, benomyl and thiophanate methyl in fruits and vegetables and of 2,4-D in citrus fruits are presented. Sample preparation involves supercritical fluid extraction with carbon dioxide and further analysis is performed without any additional clean-up by GC-MS after derivatisation or directly by HPLC-diode array detection. The SFE methods presented are clearly faster and more cost effective than traditional solvent based approaches. The recoveries, detection limits and repeatabilities achieved, meet the needs of tolerance level monitoring of these compounds in fruits and vegetables.

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.

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.

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.

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)

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.

Accelerated solvent extraction by using an 'in-line' clean-up approach for multiresidue analysis of pesticides in organic honey.

PubMed

Chiesa, Luca Maria; Labella, Giuseppe Federico; Panseri, Sara; Britti, Domenico; Galbiati, Fabrizio; Villa, Roberto; Arioli, Francesco

2017-05-01

The worldwide loss of honeybee colonies may be due to their exposure to several contaminants (i.e., pesticides); such contamination may also have impacts on consumers' health. Therefore, it is essential to develop quick and new methods to detect several pesticide residues in honey samples. In this study, the effectiveness of accelerated solvent extraction (ASE) was compared with QuEChERS methods for the analysis of 53 pesticides in organic honey by gas chromatography-triple quadrupole mass spectrometry. Two simple and rapid ASE methods with 'in-line' clean-up were optimised and then compared with QuEChERS. Hexane-ethyl acetate (Hex:EtAc) and Florisil were chosen as extraction solvent and retainer for the first ASE method respectively; acetonitrile and a primary-secondary amine phase (ACN-PSA) were selected for the second ASE method. The methods were validated according to the European Union SANTE/11945/2015 guidelines. The validation parameters showed that QuEChERS and ASE with PSA as retainer had better repeatability than ASE with Hex:EtAc and Florisil. In particular, QuEChERS and ASE (ACN-PSA) showed good recovery, according to the SANTE criteria, for the majority of investigated pesticides. Conversely, when ASE with Hex:EtAc and Florisil was used as the retainer, several compounds showed recoveries lower than the acceptable value of 70%. The ASE in-line method was finally applied to evaluate pesticide concentration in organic honey samples.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for preconcentration and determination of trace amounts of copper by flame atomic absorption spectrometry.

PubMed

Karadaş, Cennet; Kara, Derya

2017-04-01

A novel, simple, rapid, sensitive, inexpensive and environmentally friendly dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO) was developed for the determination of copper by flame atomic absorption spectrometry (FAAS). N-o-Vanillidine-2-amino-p-cresol was used as a chelating ligand and 1-undecanol was selected as an extraction solvent. The main parameters affecting the performance of DLLME-SFO, such as sample pH, volume of extraction solvent, extraction time, concentration of the chelating ligand, salt effect, centrifugation time and sample volume were investigated and optimized. The effect of interfering ions on the recovery of copper was also examined. Under the optimum conditions, the detection limit (3σ) was 0.93μgL -1 for Cu using a sample volume of 20mL, yielding a preconcentration factor of 20. The proposed method was successfully applied to the determination of Cu in tap, river and seawater, rice flour and black tea samples as well as certified reference materials. Copyright © 2016. Published by Elsevier Ltd.

High-performance liquid chromatography with fluorescence detection for the rapid analysis of pheophytins and pyropheophytins in virgin olive oil.

PubMed

Li, Xueqi; Woodman, Michael; Wang, Selina C

2015-08-01

Pheophytins and pyropheophytin are degradation products of chlorophyll pigments, and their ratios can be used as a sensitive indicator of stress during the manufacturing and storage of olive oil. They increase over time depending on the storage condition and if the oil is exposed to heat treatments during the refining process. The traditional analysis method includes solvent- and time-consuming steps of solid-phase extraction followed by analysis by high-performance liquid chromatography with ultraviolet detection. We developed an improved dilute/fluorescence method where multi-step sample preparation was replaced by a simple isopropanol dilution before the high-performance liquid chromatography injection. A quaternary solvent gradient method was used to include a fourth strong solvent wash on a quaternary gradient pump, which avoided the need to premix any solvents and greatly reduced the oil residues on the column from previous analysis. This new method not only reduces analysis cost and time but shows reliability, repeatability, and improved sensitivity, especially important for low-level samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Simultaneous determination of brazilin and protosappanin B in Caesalpinia sappan by ionic-liquid dispersive liquid-phase microextraction method combined with HPLC.

PubMed

Xia, Zhaoyang; Li, Dongdong; Li, Qing; Zhang, Yan; Kang, Wenyi

2017-11-13

The conditions of heating, ionic liquid-based ultrasonic-assisted extraction combined with reverse-phase high performance liquid chromatography were optimized to simultaneously isolate and determinate brazilin and protosappanin B in Caesalpinia sappan. Ionic liquids, including [BMIM]Br, [BMIM]BF 4 , [BMIM]PF 6 and [HMIM]PF 6 , were selected as extraction solvents while methanol, acetone, acetonitrile, ethanol and water were selected as dispersants. The chromatographic column was Purospher star RP-C 18 (250 mm × 4.6 mm, 5 μm), a mixture of methanol and 0.2% phosphoric acid-water was used as mobile phase at a flow rate 0.65 mL/min. The result displayed that the extraction yields of brazilin and protosappanin B were highest when the concentration of [BMIM]Br methanol solution as extraction solvent was 0.5 mol/L and the solid-liquid ratio was 1:50 (g/mL). Under the optimal extraction conditions, the contents of brazilin showed a good linearity (r = 1.0000) within the range of 1.25-7.50 μg with the average recovery of 99.33%, the contents of protosappanin B also showed a good linearity (r = 0.9999) within the range of 0.50-3.00 μg with the average recovery of 98.31%. This experiment, which adopted environmentally friendly reagent as extraction solvent, not only improved the extraction efficiency, but also avoided the environmental pollution caused by organic solvent. Moreover, it was simple and reliable, and can be of important significance in the study of Traditional Chinese Medicine active ingredient extraction methods. The antibacterial activities of the ionic liquids and methanol extracts were determined using the paper disc diffusion method. The ionic liquid extract was found to possess antibacterial activity against Staphylococcus aureus and methicillin-resistant S. aureus (MIC value of 37.5 mg crude drug/mL), β-Lactamase producing S. aureus (MIC values of 18.8 mg crude drug/mL), but not against E. coli, Extended spectrum β-Lactamases E. coli and P. aeruginosa. Compared with the ionic liquid extract, the methanol extract was found to have antibacterial activity against S. aureus and methicillin-resistant S. aureus (MIC value of 75.0 mg crude drug/mL), β-Lactamase producing S. aureus (MIC values of 150.0 mg crude drug/mL). However, the same, the methanol extract did not have antibacterial activity against E. coli, Extended spectrum β-Lactamases E. coli and P. aeruginosa.

Extraction Techniques for Polycyclic Aromatic Hydrocarbons in Soils

PubMed Central

Lau, E. V.; Gan, S.; Ng, H. K.

2010-01-01

This paper aims to provide a review of the analytical extraction techniques for polycyclic aromatic hydrocarbons (PAHs) in soils. The extraction technologies described here include Soxhlet extraction, ultrasonic and mechanical agitation, accelerated solvent extraction, supercritical and subcritical fluid extraction, microwave-assisted extraction, solid phase extraction and microextraction, thermal desorption and flash pyrolysis, as well as fluidised-bed extraction. The influencing factors in the extraction of PAHs from soil such as temperature, type of solvent, soil moisture, and other soil characteristics are also discussed. The paper concludes with a review of the models used to describe the kinetics of PAH desorption from soils during solvent extraction. PMID:20396670

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.

Fundamental Chemical Kinetic And Thermodynamic Data For Purex Process Models

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

Taylor, R.J.; Fox, O.D.; Sarsfield, M.J.

2007-07-01

To support either the continued operations of current reprocessing plants or the development of future fuel processing using hydrometallurgical processes, such as Advanced Purex or UREX type flowsheets, the accurate simulation of Purex solvent extraction is required. In recent years we have developed advanced process modeling capabilities that utilize modern software platforms such as Aspen Custom Modeler and can be run in steady state and dynamic simulations. However, such advanced models of the Purex process require a wide range of fundamental data including all relevant basic chemical kinetic and thermodynamic data for the major species present in the process. Thismore » paper will summarize some of these recent process chemistry studies that underpin our simulation, design and testing of Purex solvent extraction flowsheets. Whilst much kinetic data for actinide redox reactions in nitric acid exists in the literature, the data on reactions in the diluted TBP solvent phase is much rarer. This inhibits the accurate modelization of the Purex process particularly when species show a significant extractability in to the solvent phase or when cycling between solvent and aqueous phases occurs, for example in the reductive stripping of Pu(IV) by ferrous sulfamate in the Magnox reprocessing plant. To support current oxide reprocessing, we have investigated a range of solvent phase reactions: - U(IV)+HNO{sub 3}; - U(IV)+HNO{sub 2}; - U(IV)+HNO{sub 3} (Pu catalysis); - U(IV)+HNO{sub 3} (Tc catalysis); - U(IV)+ Np(VI); - U(IV)+Np(V); - Np(IV)+HNO{sub 3}; - Np(V)+Np(V); Rate equations have been determined for all these reactions and kinetic rate constants and activation energies are now available. Specific features of these reactions in the TBP phase include the roles of water and hydrolyzed intermediates in the reaction mechanisms. In reactions involving Np(V), cation-cation complex formation, which is much more favourable in TBP than in HNO{sub 3}, also occurs and complicates the redox chemistry. Whilst some features of the redox chemistry in TBP appear similar to the corresponding reactions in aqueous HNO{sub 3}, there are notable differences in rates, the forms of the rate equations and mechanisms. Secondly, to underpin the development of advanced single cycle flowsheets using the complexant aceto-hydroxamic acid, we have also characterised in some detail its redox chemistry and solvent extraction behaviour with both Np and Pu ions. We find that simple hydroxamic acids are remarkably rapid reducing agents for Np(VI). They also reduce Pu(VI) and cause a much slower reduction of Pu(IV) through a complex mechanism involving acid hydrolysis of the ligand. AHA is a strong hydrophilic and selective complexant for the tetravalent actinide ions as evidenced by stability constant and solvent extraction data for An(IV), M(III) and U(VI) ions. This has allowed the successful design of U/Pu+Np separation flowsheets suitable for advanced fuel cycles. (authors)« less

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.

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.

Coupling solid-phase extraction and enzyme-linked immunosorbent assay for ultratrace determination of herbicides in pristine water

USGS Publications Warehouse

Aga, D.S.; Thurman, E.M.

1993-01-01

Solid-phase extraction (SPE) and enzyme-linked immunosorbent assay (ELISA) were coupled for automated trace analysis of pristine water samples containing 2-chloro-4-ethylamino-6-isopropylamine-s-triazine (atrazine) and 2-chloro-2???,6???-diethyl-N-(methoxymethyl)acetanilide (alachlor). The isolation of the two herbicides on a C18-resin involved the selection of an elution solvent that both removes interfering substances and is compatible with ELISA. Ethyl acetate was selected as the elution solvent followed by a solvent exchange with methanol/water (20/80, % v/v). The SPE-ELISA method has a detection limit of 5.0 ng/L (5 ppt), >90% recovery, and a relative standard deviation of ??10%. The performance of a microtiter plate-based ELISA and a magnetic particle-based ELISA coupled to SPE was also evaluated. Although the sensitivity of the two ELISA methods was comparable, the precision using magnetic particles was improved considerably (??10% versus ??20%) because of the faster reaction kinetics provided by the magnetic particles. Finally, SPE-ELISA and isotope dilution gas chromatography/ mass spectrometry correlated well (correlation coefficient of 0.96) for lake-water samples. The SPE-ELISA method is simple and may have broader applications for the inexpensive automated analysis of other contaminants in water at trace levels.

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.

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.

Pipette-tip solid-phase extraction using poly(1-vinylimidazole-co-trimethylolpropane trimethacrylate) as a new molecularly imprinted polymer in the determination of avermectins and milbemycins in fruit juice and water samples.

PubMed

Teixeira, Roseane Andrade; Flores, Diego Hernando Ângulo; da Silva, Ricky Cássio Santos; Dutra, Flávia Viana Avelar; Borges, Keyller Bastos

2018-10-01

A simple HPLC method was developed for the determination of abamectin (ABA), eprinomectin (EPR), and moxidectin (MOX). Pipette-tip molecularly imprinted polymer solid-phase extraction (PT-MIP-SPE) using poly(1-vinylimidazole-co-trimethylolpropane trimethacrylate) as a selective adsorbent material was studied in detail, including the washing solvent, type and volume of eluent, pH, quantity of adsorbent material and sample volume. The performance criteria for linearity, sensitivity, precision, accuracy, recovery, robustness and stability have been assessed and were within the recommended guidelines. The mean extraction recoveries/relative standard deviation for ABA 1b, EPR, ABA 1a and MOX were 98.77 ± 3.82%, 88.19 ± 2.57%, 110.54 ± 1.52% and 100.42 ± 0.59%, respectively. Finally, the results proved that PT-MIP-SPE coupled to HPLC-UV is an economical, simple and easy-to-perform technique, and presented a high potential for extraction of macrocyclic lactones in mineral water and grape and juice samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

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.

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.

Salting-out assisted liquid-liquid extraction with the aid of experimental design for determination of benzimidazole fungicides in high salinity samples by high-performance liquid chromatography.

PubMed

Wen, Yingying; Li, Jinhua; Yang, Fangfang; Zhang, Weiwei; Li, Weiran; Liao, Chunyang; Chen, Lingxin

2013-03-15

A novel method for the simultaneous separation and determination of four benzimidazole fungicides (i.e., carbendazim, fuberidazole, thiophanate-methyl and thiophanate) in high salinity samples was developed by using salting-out assisted liquid-liquid extraction (SALLE) via water-miscible acetonitrile as the extractant coupled with high-performance liquid chromatography. Box-Behnken design and response surface were employed to assist the optimization of SALLE conditions, including volume of salting-out solvent, the pH of sample solution and salting-out solvent as variable factors. The optimal salting-out parameters were obtained as follows: 2 mL of acetonitrile was added to 2 mL of sample solution with pH=4 and then 2 mL salting-out solvent containing 5 mol L(-1) sodium chloride at a pH of 7 was added to the solution for extraction. This procedure afforded a convenient and cost-saving operation with good cleanup ability for the benzimidazole fungicides, such as good linear relationships (R>0.996) between peak area and concentration from 2.5 ng mL(-1) to 500 ng mL(-1), low limits of detection between 0.14 ng mL(-1) and 0.38 ng mL(-1) and the intra-day precisions of retention time below 1.0%. The method recoveries obtained at fortified three concentrations for three seawater samples ranged from 60.4% to 99.1%. The simple, rapid and eco-benign SALLE based method proved potentially applicable for trace benzimidazole fungicides analysis in high salinity samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of octylphenol and nonylphenol in aqueous sample using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry.

PubMed

Luo, Shusheng; Fang, Ling; Wang, Xiaowei; Liu, Hongtao; Ouyang, Gangfeng; Lan, Chongyu; Luan, Tiangang

2010-10-22

A simple and fast sample preparation method for the determination of nonylphenol (NP) and octylphenol (OP) in aqueous samples by simultaneous derivatization and dispersive liquid-liquid microextraction (DLLME) was investigated using gas chromatography-mass spectrometry (GC/MS). In this method, a combined dispersant/derivatization catalyst (methanol/pyridine mixture) was firstly added to an aqueous sample, following which a derivatization reagent/extraction solvent (methyl chloroformate/chloroform) was rapidly injected to combine in situ derivatization and extraction in a single step. After centrifuging, the sedimented phase containing the analytes was injected into the GC port by autosampler for analysis. Several parameters, such as extraction solvent, dispersant solvent, amount of derivatization reagent, derivatization and extraction time, pH, and ionic strength were optimized to obtain higher sensitivity for the detection of NP and OP. Under the optimized conditions, good linearity was observed in the range of 0.1-1000 μg L⁻¹ and 0.01-100 μg L⁻¹ with the limits of detection (LOD) of 0.03 μg L⁻¹ and 0.002 μg L⁻¹ for NP and OP, respectively. Water samples collected from the Pearl River were analyzed with the proposed method, the concentrations of NP and OP were found to be 2.40 ± 0.16 μg L⁻¹ and 0.037 ± 0.001 μg L⁻¹, respectively. The relative recoveries of the water samples spiked with different concentrations of NP and OP were in the range of 88.3-106.7%. Compared with SPME and SPE, the proposed method can be successfully applied to the rapid and convenient determination of NP and OP in aqueous samples. Copyright © 2010 Elsevier B.V. All rights reserved.

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.

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.

A simple, rapid and novel method based on salting-out assisted liquid-liquid extraction for ochratoxin A determination in beer samples prior to ultra-high performance liquid chromatography coupled to tandem mass spectrometry.

PubMed

Mariño-Repizo, Leonardo; Goicoechea, Hector; Raba, Julio; Cerutti, Soledad

2018-06-07

A novel, simple, easy and cheap sample treatment strategy based on salting-out assisted liquid-liquid extraction (SALLE) for ochratoxin A (OTA) ultra-trace analysis in beer samples using ultra-high performance liquid chromatography-tandem mass spectrometry determination was developed. The factors involved in the efficiency of pretreatment were studied employing factorial design in the screening phase and the optimal conditions of the significant variables on the analytical response were evaluated using a central composite face-centred design (CCF). Consequently, the amount of salt ((NH 4 ) 2 SO 4 ), together with the volumes of sample, hydrophilic (acetone) and nonpolar (toluene) solvents, and times of vortexing and centrifugation were optimized. Under optimized conditions, the limits of detection (LOD) and quantification (LOQ) were 0.02 µg l -1 and 0.08 µg l -1 respectively. OTA extraction recovery by SALLE was approximately 90% (0.2 µg l -1 ). Furthermore, the methodology was in agreement with EU Directive requirements and was successfully applied for analysis of beer samples.

Determination of sudan dyes in red wine and fruit juice using ionic liquid-based liquid-liquid microextraction and high-performance liquid chromatography.

PubMed

Sun, Shuo; Wang, Ying; Yu, Wenzhi; Zhao, Tianqi; Gao, Shiqian; Kang, Mingqin; Zhang, Yupu; Zhang, Hanqi; Yu, Yong

2011-07-01

The liquid-liquid microextraction (LLME) was developed for extracting sudan dyes from red wine and fruit juice. Room temperature ionic liquid was used as the extraction solvent. The target analytes were determined by high-performance liquid chromatography. The extraction parameters were optimized. The optimal conditions are as follows: volume of [C(6)MIM][PF(6)] 50 μL; the extraction time 10 min; pH value of the sample solution 7.0; NaCl concentration in sample solution 5%. The extraction recoveries for the analytes in red wine and fruit samples are 86.79-108.28 and 68.54-85.66%, whereas RSDs are 1.42-5.12 and 1.43-6.19%, respectively. The limits of detection and quantification were 0.428 and 1.426 ng/mL for sudan I, 0.938 and 3.127 ng/mL for sudan II, 1.334 and 4.445 ng/mL for sudan III, 1.454 and 4.846 ng/mL for sudan IV, respectively. Compared with conventional liquid-liquid extraction (CLLE) and ultrasonic extraction (UE), when LLME was applied, the sample amount was less (LLME: 4 mL; CLLE: 10 mL; UE: 10 mL), the extraction time was shorter (LLME: 15 min; CLLE: 110 min; UE: 50 min) and the extraction solvent amount was less (LLME: 0.05 mL IL; CLLE: 15 mL hexane; UE: 20 mL hexane). The proposed method offers a simple, rapid and efficient sample preparation for determining sudan dyes in red wine and fruit juice samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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

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.

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.

A Simple Sonication Improves Protein Signal in Matrix-Assisted Laser Desorption Ionization Imaging

NASA Astrophysics Data System (ADS)

Lin, Li-En; Su, Pin-Rui; Wu, Hsin-Yi; Hsu, Cheng-Chih

2018-02-01

Proper matrix application is crucial in obtaining high quality matrix-assisted laser desorption ionization (MALDI) mass spectrometry imaging (MSI). Solvent-free sublimation was essentially introduced as an approach of homogeneous coating that gives small crystal size of the organic matrix. However, sublimation has lower extraction efficiency of analytes. Here, we present that a simple sonication step after the hydration in standard sublimation protocol significantly enhances the sensitivity of MALDI MSI. This modified procedure uses a common laboratory ultrasonicator to immobilize the analytes from tissue sections without noticeable delocalization. Improved imaging quality with additional peaks above 10 kDa in the spectra was thus obtained upon sonication treatment. [Figure not available: see fulltext.

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.

Comparison of single-ion molecular dynamics in common solvents

NASA Astrophysics Data System (ADS)

Muralidharan, A.; Pratt, L. R.; Chaudhari, M. I.; Rempe, S. B.

2018-06-01

Laying a basis for molecularly specific theory for the mobilities of ions in solutions of practical interest, we report a broad survey of velocity autocorrelation functions (VACFs) of Li+ and PF6- ions in water, ethylene carbonate, propylene carbonate, and acetonitrile solutions. We extract the memory function, γ(t), which characterizes the random forces governing the mobilities of ions. We provide comparisons controlling for the effects of electrolyte concentration and ion-pairing, van der Waals attractive interactions, and solvent molecular characteristics. For the heavier ion (PF6-), velocity relaxations are all similar: negative tail relaxations for the VACF and a clear second relaxation for γ (t ), observed previously also for other molecular ions and with n-pentanol as the solvent. For the light Li+ ion, short time-scale oscillatory behavior masks simple, longer time-scale relaxation of γ (t ). But the corresponding analysis of the solventberg Li+(H2O)4 does conform to the standard picture set by all the PF6- results.

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.

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.

Actinide and lanthanide separation process (ALSEP)

DOEpatents

Guelis, Artem V.

2013-01-15

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

Alternative and Efficient Extraction Methods for Marine-Derived Compounds

PubMed Central

Grosso, Clara; Valentão, Patrícia; Ferreres, Federico; Andrade, Paula B.

2015-01-01

Marine ecosystems cover more than 70% of the globe’s surface. These habitats are occupied by a great diversity of marine organisms that produce highly structural diverse metabolites as a defense mechanism. In the last decades, these metabolites have been extracted and isolated in order to test them in different bioassays and assess their potential to fight human diseases. Since traditional extraction techniques are both solvent- and time-consuming, this review emphasizes alternative extraction techniques, such as supercritical fluid extraction, pressurized solvent extraction, microwave-assisted extraction, ultrasound-assisted extraction, pulsed electric field-assisted extraction, enzyme-assisted extraction, and extraction with switchable solvents and ionic liquids, applied in the search for marine compounds. Only studies published in the 21st century are considered. PMID:26006714

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.

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.

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 Simplified Method for Sampling and Analysis of High Volume Surface Water for Organic Contaminants Using XAD-2

USGS Publications Warehouse

Datta, S.; Do, L.V.; Young, T.M.

2004-01-01

A simple compressed-gas driven system for field processing and extracting water for subsequent analyses of hydrophobic organic compounds is presented. The pumping device is a pneumatically driven pump and filtration system that can easily clarify at 4L/min. The extraction device uses compressed gas to drive filtered water through two parallel XAD-2 resin columns, at about 200 mL/min. No batteries or inverters are required for water collection or processing. Solvent extractions were performed directly in the XAD-2 glass columns. Final extracts are cleaned-up on Florisil cartridges without fractionation and contaminants analyzed by GC-MS. Method detection limits (MDLs) and recoveries for dissolved organic contaminants, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and pesticides are reported along with results of surface water analysis for the San Francisco Bay, CA.

A simple method to separate red wine nonpolymeric and polymeric phenols by solid-phase extraction.

PubMed

Pinelo, Manuel; Laurie, V Felipe; Waterhouse, Andrew L

2006-04-19

Simple polyphenols and tannins differ in the way that they contribute to the organoleptic profile of wine and their effects on human health. Very few straightforward techniques to separate red wine nonpolymeric phenols from the polymeric fraction are available in the literature. In general, they are complex, time-consuming, and generate large amounts of waste. In this procedure, the separation of these compounds was achieved using C18 cartridges, three solvents with different elution strengths, and pH adjustments of the experimental matrices. Two full factorial 2(3) experimental designs were performed to find the optimal critical variables and their values, allowing for the maximization of tannin recovery and separation efficiency (SE). Nonpolymeric phenols such as phenolic acids, monomers, and oligomers of flavonol and flavan-3-ols and anthocyanins were removed from the column by means of an aqueous solvent followed by ethyl acetate. The polymeric fraction was then eluted with a combination of methanol/acetone/water. The best results were attained with 1 mL of wine sample, a 10% methanol/water solution (first eluant), ethyl acetate (second eluant), and 66% acetone/water as the polymeric phenols-eluting solution (third eluant), obtaining a SE of ca. 90%. Trials with this method on fruit juices also showed high separation efficiency. Hence, this solid-phase extraction method has been shown to be a simple and efficient alternative for the separation of nonpolymeric phenolic fractions and the polymeric ones, and this method could have important applications to sample purification prior to biological testing due to the nonspecific binding of polymeric phenolics to nearly all enzymes and receptor sites.

Towards metals analysis using corona discharge ionization ion mobility spectrometry.

PubMed

Jafari, Mohammad T; Saraji, Mohammad; Sherafatmand, Hossein

2016-02-25

For the first time, the capability of corona discharge ionization ion mobility spectrometry (CD-IMS) in the determination of metal complex was evaluated. The extreme simplicity of dispersive liquid-liquid microextraction (DLLME) coupled to the high sensitivity of CD-IMS measurement could make this combination really useful for simple, rapid, and sensitive determination of metals in different samples. In this regard, mercury, as a model metal, was complexed with diethyldithiocarbamate (DEDTC), and then extracted into the carbon tetrachloride using DLLME. Some parameters affecting the extraction efficiency, including the type and volume of the extraction solvent, the type and volume of the disperser solvent, the concentration of the chelating agent, salt addition and, pH were exhaustively investigated. Under the optimized condition, the enrichment factor was obtained to be 142. The linear range of 0.035-10.0 μg mL(-1) with r(2) = 0.997 and the detection limit of 0.010 μg mL(-1) were obtained. The relative standard deviation values were calculated to be lower than 4% and 8% for intra-day and inter-day, respectively. Finally, the developed method was successfully applied for the extraction and determination of mercury in various real samples. The satisfactory results revealed the capability of the proposed method in trace analysis without tedious derivatization or hydride generation. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of parabens in beverage samples by dispersive liquid-liquid microextraction based on solidification of floating organic droplet.

PubMed

Hou, Fang; Deng, Xiaoying; Jiang, Xinyu; Yu, Jingang

2014-01-01

A simple and efficient method for dispersive liquid-liquid microextraction of methylparaben, ethylparaben, propylparaben and butylparaben in real beverage samples was developed. It is making use of solidified floating organic droplets of 1-dodecanol which has low density and a proper melting point. Parameters influencing the extraction efficiency, such as the type of extraction and dispersive solvent, the volume of extraction and dispersive solvent, salt effect, pH, extraction time, were optimized and resulted in enrichment factors (EFs) of 84 for methylparaben, 103 for ethylparaben, 115 for propylparaben and 126 for butylparaben. The limits of detection for parabens were 1.52, 1.06, 0.32 and 0.17 ng/mL, respectively. Excellent linearity with coefficients of correlation from 0.9970 to 0.9997 was observed in the concentration range of 5-1,000 ng/mL. The repeatability of the proposed method expressed as relative standard deviations (RSDs) ranged from 2.54 to 3.89% (n = 5). The relative recoveries for parabens in beverage samples were good and in the ranges of 89.8-109.9, 90.2-107.3, 90.9-101.7 and 92.3-118.1%, respectively. Thus, the proposed method has excellent potential for the determination of parabens in beverage samples. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Preparative separation and purification of steroidal saponins in Paris polyphylla var. yunnanensis by macroporous adsorption resins.

PubMed

Liu, Zhen; Wang, Jieyin; Gao, Wenyuan; Man, Shuli; Wang, Ying; Liu, Changxiao

2013-07-01

Saponins are active compounds in natural products. Many researchers have tried to find the method for knowing their concentration in herbs. Some methods, such as solid-liquid extraction and solvent extraction, have been developed. However, the extraction methods of the steroidal saponins from Paris polyphylla Smith var. yunnanensis (Liliaceae) are not fully researched. To establish a simple extraction method for the separation of steroidal saponins from the rhizomes of P. polyphylla Smith var. yunnanensis. Macroporous adsorption resins were used for the separation of steroidal saponins. To select the most suitable resins, seven kinds of macroporous resins were selected in this study. The static adsorption and desorption tests on macroporous resins were determined. Also, we optimized the temperature and the ethanol concentration in the extraction method by the contents of five kinds of saponins. Then, we compared the extraction method with two other methods. D101 resin demonstrated the best adsorption and desorption properties for steroidal saponins. Its adsorption data fits best to the Freundlich adsorption model. The contents of steroidal saponins in the product were 4.83-fold increased with recovery yields of 85.47%. The process achieved simple and effective enrichment and separation for steroidal saponins. The method provides a scientific basis for large-scale preparation of steroidal saponins from the Rhizoma Paridis and other plants.

Use of an online extraction liquid chromatography quadrupole time-of-flight tandem mass spectrometry method for the characterization of polyphenols in Citrus paradisi cv. Changshanhuyu peel.

PubMed

Tong, Chaoying; Peng, Mijun; Tong, Runna; Ma, Ruyi; Guo, Keke; Shi, Shuyun

2018-01-19

Chemical profiling of natural products by high performance liquid chromatography (HPLC) was critical for understanding of their clinical bioactivities, and sample pretreatment steps have been considered as a bottleneck for analysis. Currently, concerted efforts have been made to develop sample pretreatment methods with high efficiency, low solvent and time consumptions. Here, a simple and efficient online extraction (OLE) strategy coupled with HPLC-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS) was developed for rapid chemical profiling. For OLE strategy, guard column inserted with ground sample (2 mg) instead of sample loop was connected with manual injection valve, in which components were directly extracted and transferred to HPLC-DAD-QTOF-MS/MS system only by mobile phase without any extra time, solvent, instrument and operation. By comparison with offline heat-reflux extraction of Citrus paradisi cv. Changshanhuyu (Changshanhuyu) peel, OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of twenty-two secondary metabolites were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and nine of them were discovered in Changshanhuyu peel for the first time to our knowledge. It is concluded that the developed OLE-HPLC-DAD-QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products. Copyright © 2017 Elsevier B.V. All rights reserved.

Online extraction-high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry for rapid flavonoid profiling of Fructus aurantii immaturus.

PubMed

Tong, Runna; Peng, Mijun; Tong, Chaoying; Guo, Keke; Shi, Shuyun

2018-03-01

Chemical profiling of natural products by high performance liquid chromatography (HPLC) was critical for understanding of their clinical bioactivities, and sample pretreatment steps have been considered as a bottleneck for analysis. Currently, concerted efforts have been made to develop sample pretreatment methods with high efficiency, low solvent and time consumptions. Here, a simple and efficient online extraction (OLE) strategy coupled with HPLC-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS) was developed for rapid chemical profiling. For OLE strategy, guard column inserted with ground sample (2 mg) instead of sample loop was connected with manual injection valve, in which components were directly extracted and transferred to HPLC-DAD-QTOF-MS/MS system only by mobile phase without any extra time, solvent, instrument and operation. By comparison with offline heat-reflux extraction for Fructus aurantii immaturus (Zhishi), OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of eighteen flavonoids were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and compound 9, natsudaidain-3-O-glucoside, was discovered in Zhishi for the first time. It is concluded that the developed OLE-HPLC-DAD-QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products. Copyright © 2018. Published by Elsevier B.V.

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.

Modifier mass transfer kinetic effect in the performance of solvent gradient simulated moving bed (SG-SMB) process

NASA Astrophysics Data System (ADS)

Câmara, L. D. T.

2015-09-01

The solvent-gradient simulated moving bed process (SG-SMB) is the new tendency in the performance improvement if compared to the traditional isocratic solvent conditions. In such SG-SMB separation process the modulation of the solvent strength leads to significant increase in the purities and productivity followed by reduction in the solvent consumption. A stepwise modelling approach was utilized in the representation of the interconnected chromatographic columns of the system combined with lumped mass transfer models between the solid and liquid phase. The influence of the solvent modifier was considered applying the Abel model which takes into account the effect of modifier volume fraction over the partition coefficient. The modelling and simulations were carried out and compared to the experimental SG-SMB separation of the amino acids phenylalanine and tryptophan. A lumped mass transfer kinetic model was applied for both the modifier (ethanol) as well as the solutes. The simulation results showed that such simple and global mass transfer models are enough to represent all the mass transfer effect between the solid adsorbent and the liquid phase. The separation performance can be improved reducing the interaction or the mass transfer kinetic effect between the solid adsorbent phase and the modifier. The simulations showed great agreement fitting the experimental data of the amino acids concentrations both at the extract as well as at the raffinate.

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.

Determination of supplemental feeding needs for astaxanthin and canthaxanthin in salmonids by supramolecular solvent-based microextraction and liquid chromatography-UV/VIS spectroscopy.

PubMed

Caballo, Carmen; Costi, Esther María; Sicilia, María Dolores; Rubio, Soledad

2012-09-15

Development of simple and rapid analytical methods for predicting supplemental feeding requirements in aquaculture is a need to reduce production costs. In this article, a supramolecular solvent (SUPRAS) made up of decanoic acid (DeA) assemblies was proposed to simplify sample treatment in the total and individual determination of carotenoids (red-pink pigments) in farmed salmonids. The analytes were quantitatively extracted in a single step that spends a few minutes using a small volume of SUPRAS (i.e. 800 μL) and directly determined in extracts without the interference from fats or other matrix components. The methods based on the combination of microextraction with SUPRAS and photometry or HPLC-UV/VIS spectroscopy were developed for the determination of total and individual carotenoids, respectively. The applicability of the methods was demonstrated by analysing non-fortified and fortified samples of farmed Atlantic salmons and rainbow trouts. Recoveries obtained by photometry and HPLC-UV/VIS spectroscopy were within the intervals 98-104% and 94-106%, respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Determination of Lead in Urine by Atomic Absorption Spectrophotometry1

PubMed Central

Selander, Stig; Cramé, Kim

1968-01-01

A method for the determination of lead in urine by means of atomic absorption spectrophotometry (AAS) is described. A combination of wet ashing and extraction with ammonium pyrrolidine dithiocarbamate into isobutylmethylketone was used. The sensitivity was about 0·02 μg./ml. for 1% absorption, and the detection limit was about 0·02 μg./ml. with an instrumental setting convenient for routine analyses of urines. Using the scale expansion technique, the detection limit was below 0·01 μg./ml., but it was found easier to determine urinary lead concentrations below 0·05 μg./ml. by concentrating the lead in the organic solvent by increasing the volume of urine or decreasing that of the solvent. The method was applied to fresh urines, stored urines, and to urines, obtained during treatment with chelating agents, of patients with lead poisoning. Urines with added inorganic lead were not used. The results agreed well with those obtained with a colorimetric dithizone extraction method (r = 0·989). The AAS method is somewhat more simple and allows the determination of smaller lead concentrations. PMID:5647975

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.

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).

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.

A simple dual online ultra-high pressure liquid chromatography system (sDO-UHPLC) for high throughput proteome analysis.

PubMed

Lee, Hangyeore; Mun, Dong-Gi; Bae, Jingi; Kim, Hokeun; Oh, Se Yeon; Park, Young Soo; Lee, Jae-Hyuk; Lee, Sang-Won

2015-08-21

We report a new and simple design of a fully automated dual-online ultra-high pressure liquid chromatography system. The system employs only two nano-volume switching valves (a two-position four port valve and a two-position ten port valve) that direct solvent flows from two binary nano-pumps for parallel operation of two analytical columns and two solid phase extraction (SPE) columns. Despite the simple design, the sDO-UHPLC offers many advantageous features that include high duty cycle, back flushing sample injection for fast and narrow zone sample injection, online desalting, high separation resolution and high intra/inter-column reproducibility. This system was applied to analyze proteome samples not only in high throughput deep proteome profiling experiments but also in high throughput MRM experiments.

Water-contained surfactant-based vortex-assisted microextraction method combined with liquid chromatography for determination of synthetic antioxidants from edible oil.

PubMed

Amlashi, Nadiya Ekbatani; Hadjmohammadi, Mohammad Reza; Nazari, Seyed Saman Seyed Jafar

2014-09-26

For the first time, a novel water-contained surfactant-based vortex-assisted microextraction method (WSVAME) was developed for the extraction of two synthetic antioxidants (t-butyl hydroquinone (TBHQ) and butylated hydroxyanisole (BHA)) from edible oil samples. The novel microextraction method is based on the injection of an aqueous solution of non-ionic surfactant, Brij-35, into the oil sample in a conical bottom glass tube to form a cloudy solution. Vortex mixing was applied to accelerate the dispersion process. After extraction and phase separation by centrifugation, the lower sediment phase was directly analyzed by HPLC. The effects of the four experimental parameters including volume and concentration of extraction solvent (aqueous solution of Brij-35), percentage of acetic acid added to the oil sample and vortex time on the extraction efficiency were studied with a full factorial design. The central composite design and multiple linear regression method were applied for the construction of the best polynomial model based on experimental recoveries. The proposed method showed good linearity within the range of 0.200-200 μg mL(-1), the square of correlation coefficient higher than 0.999 and appropriate limit of detection (0.026 and 0.020 μg mL(-1) for TBHQ and BHA, respectively), while the precision for inner-day was ≤ 3.0 (n=5) and it was ≤ 3.80 (n=5) for inter-day assay. Under the optimal condition (30 μL of 0.10 mol L(-1) Brij-35 solution as extraction solvent and vortex time 1 min), the method was successfully applied for determination of TBHQ and BHA in different commercial edible oil samples. The recoveries in all cases were above 95%, with relative standard deviations below 5%. This approach is considered as a simple, sensitive and environmentally friendly method because of biodegradability of the extraction phase and no use of organic solvent in the extraction procedure. Copyright © 2014 Elsevier B.V. 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.

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.

Molecularly imprinted phloroglucinol-formaldehyde-melamine resin prepared in a deep eutectic solvent for selective recognition of clorprenaline and bambuterol in urine.

PubMed

Liang, Shiru; Yan, Hongyuan; Cao, Jiankun; Han, Yehong; Shen, Shigang; Bai, Ligai

2017-01-25

A new molecularly imprinted phloroglucinol-formaldehyde-melamine resin (MIPFMR) was synthesized in a deep eutectic solvent (DES) using phenylephrine as a dummy template. The MIPFMR was used as a solid phase extraction (SPE) sorbent for the selective isolation and recognition of clorprenaline (CLP) and bambuterol (BAM) in urine. Phloroglucinol and melamine were used as double functional monomers that introduced abundant hydrophilic groups (such as hydroxyl groups, imino groups, and ether linkages) into the MIPFMR, making it compatible with aqueous solvents. In addition, the formation of DES by combining the quaternary ammonium salt of choline chloride with ethylene glycol as a hydrogen bond donor was an environmentally safe alternative to toxic organic solvents such as chloroform and dimethylsulfoxide that are typically used in the preparation of most molecularly imprinted polymers (MIPs). Moreover, MIPFMR-based SPE of CLP and BAM in urine resulted in higher recoveries and purer extracts than those obtained by using other SPE materials (e.g., SCX, C 18 , HLB, and non-imprinted phloroglucinol-formaldehyde-melamine resin (NIPFMR)). The optimized MIPFMR-SPE-HPLC-UV method had good linearity (r 2  ≥ 0.9996) ranging from 15.0 to 3000.0 ng mL -1 for CLP and BAM, and the recoveries at three spiked levels ranged from 91.7% to 100.1% with RSDs ≤7.6%. The novel MIPFMR-SPE-HPLC-UV method is simple, selective, and accurate, and can be used for the determination of CLP and BAM in urine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

[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.

Application of dispersion-solidification liquid-liquid microextraction for the determination of triazole fungicides in environmental water samples by high-performance liquid chromatography.

PubMed

Wang, Chun; Wu, Qiuhua; Wu, Chunxia; Wang, Zhi

2011-01-15

A simple, rapid and environmentally friendly method has been developed for the determination of four triazole fungicides (myclobutanil, tebuconazole, triadimenol, hexaconazole) in water samples by dispersion-solidification liquid-liquid microextraction coupled with high performance liquid chromatography-diode array detection. Several variables that affect the extraction efficiencies, including the type and volume of the extraction solvent and dispersive solvent, extraction time, effect of pH and salt addition, were investigated and optimized. Under the optimum conditions, the proposed method is sensitive and shows a good linearity within a range of 0.5-200 ng mL(-1), with the correlation coefficients (r) varying from 0.9992 to 0.9998. High enrichment factors were achieved ranging from 190 to 450. The recoveries of the target analytes from water samples at spiking levels of 1.0, 5.0 and 50.0 ng mL(-1) were between 84.8% and 110.2%. The limits of detection (LODs) for the analytes were ranged in 0.06-0.1 ng mL(-1), and the relative standard deviations (RSD) varied from 3.9% to 5.7%. The proposed method has been successfully applied for the determination of the triazole fungicides in real water samples. Copyright © 2010 Elsevier B.V. All rights reserved.

Measuring and predicting the emission rate of phthalate plasticizer from vinyl flooring in a specially-designed chamber.

PubMed

Xu, Ying; Liu, Zhe; Park, Jinsoo; Clausen, Per A; Benning, Jennifer L; Little, John C

2012-11-20

The emission of di-2-ethylhexyl phthalate (DEHP) from vinyl flooring (VF) was measured in specially designed stainless steel chambers. In duplicate chamber studies, the gas-phase concentration in the chamber increased slowly and reached a steady state level of 0.8-0.9 μg/m(3) after about 20 days. By increasing the area of vinyl flooring and decreasing that of the stainless steel surface within the chamber, the time to reach steady state was significantly reduced, compared to a previous study (1 month versus 5 months). The adsorption isotherm of DEHP on the stainless steel chamber surfaces was explicitly measured using solvent extraction and thermal desorption. The strong partitioning of DEHP onto the stainless steel surface was found to follow a simple linear relationship. Thermal desorption resulted in higher recovery than solvent extraction. Investigation of sorption kinetics showed that it takes several weeks for the sorption of DEHP onto the stainless steel surface to reach equilibrium. The content of DEHP in VF was measured at about 15% (w/w) using pressurized liquid extraction. The independently measured or calculated parameters were used to validate an SVOC emission model, with excellent agreement between model prediction and the observed gas-phase DEHP chamber concentrations.

Eco-friendly sonoluminescent determination of free glycerol in biodiesel samples.

PubMed

Diniz, Paulo Henrique Gonçalves Dias; Pistonesi, Marcelo Fabián; de Araújo, Mário César Ugulino; Band, Beatriz Susana Fernández

2013-09-30

This paper proposes a flow-batch methodology for the determination of free glycerol in biodiesel that is notably eco-friendly, since non-chemical reagents are used. Deionized water (the solvent) was used alone for glycerol (sample) extractions from the biodiesel. The same water was used to generate water-cavitation sonoluminescence signals, which were modulated by the quenching effect associated with the amount of extracted glycerol. The necessarily reproducible signal generation was achieved by using a simple and inexpensive piezoelectric device. A linear response was observed for glycerol within the 0.001-100 mg/L range, equivalent to 0.004-400 mg/kg free glycerol in biodiesel. The lowest measurable concentration of free glycerol was estimated at 1.0 µg/L. The selectivity of the proposed method was confirmed by comparing the shape and retention of both real and calibration samples to standard solution chromatograms, presenting no peaks other than glycerol. All samples (after extraction) are greatly diluted; this minimizes (toward non-detectability) potential interference effects. The methodology was successfully applied to biodiesel analysis at a high sampling rate, with neither reagent nor solvent (other than water), and with minimum waste generation. The results agreed with the reference method (ASTM D6584-07), at a 95% confidence level. Copyright © 2013 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 ...

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...

A simple method for the enrichment of bisphenols using boron nitride.

PubMed

Fischnaller, Martin; Bakry, Rania; Bonn, Günther K

2016-03-01

A simple solid-phase extraction method for the enrichment of 5 bisphenol derivatives using hexagonal boron nitride (BN) was developed. BN was applied to concentrate bisphenol derivatives in spiked water samples and the compounds were analyzed using HPLC coupled to fluorescence detection. The effect of pH and organic solvents on the extraction efficiency was investigated. An enrichment factor up to 100 was achieved without evaporation and reconstitution. The developed method was applied for the determination of bisphenol A migrated from some polycarbonate plastic products. Furthermore, bisphenol derivatives were analyzed in spiked and non-spiked canned food and beverages. None of the analyzed samples exceeded the migration limit set by the European Union of 0.6mg/kg food. The method showed good recovery rates ranging from 80% to 110%. Validation of the method was performed in terms of accuracy and precision. The applied method is robust, fast, efficient and easily adaptable to different analytical problems. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

Development of an ionic-liquid-based dispersive liquid-liquid microextraction method for the determination of antichagasic drugs in human breast milk: Optimization by central composite design.

PubMed

Padró, Juan M; Pellegrino Vidal, Rocío B; Echevarria, Romina N; Califano, Alicia N; Reta, Mario R

2015-05-01

Chagas disease constitutes a major public health problem in Latin America. Human breast milk is a biological sample of great importance for the analysis of therapeutic drugs, as unwanted exposure through breast milk could result in pharmacological effects in the nursing infant. Thus, the goal of breast milk drug analysis is to inquire to which extent a neonate may be exposed to a drug during lactation. In this work, we developed an analytical technique to quantify benznidazole and nifurtimox (the two antichagasic drugs currently available for medical treatment) in human breast milk, with a simple sample pretreatment followed by an ionic-liquid-based dispersive liquid-liquid microextraction combined with high-performance liquid chromatography and UV detection. For this technique, the ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate has been used as the "extraction solvent." A central composite design was used to find the optimum values for the significant variables affecting the extraction process: volume of ionic liquid, volume of dispersant solvent, ionic strength, and pH. At the optimum working conditions, the average recoveries were 77.5 and 89.7%, the limits of detection were 0.06 and 0.09 μg/mL and the interday reproducibilities were 6.25 and 5.77% for benznidazole and nifurtimox, respectively. The proposed methodology can be considered sensitive, simple, robust, accurate, and green. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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

PubMed Central

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

2014-01-01

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

Determination of Low Level Alpha and Beta Emitters Using Liquid-Liquid Extraction and a Liquid Scintillation Spectrometer

NASA Astrophysics Data System (ADS)

Yu, Yu-Fu; BjØRnstad, H. E.; Salbu, B.

Two radiochemical procedures for determination of low level strontium-90 and plutonium-239+240 in environmental and biological materials using combined selective solvent extraction with low level liquid scintillation counting have been presented. Y-90, the daughter nuclide of Sr-90, and Pu-239+240 are selectively extracted from nitric acid solution into 5% di(-2ethylhexyl)phosphoric acid (HDEHP) in toluene and the radionuclides of interest in organic phase are counted with an ultra low level scintillation counter "Quantulus". The lower detection limits for Sr-90 and Pu-239+240 are estimated to be 20 mBq and 0.3 mBq respectively. The developed procedures have been tested for soma environmental and biological samples and the preminarly results show that they are more simple and time-saving than traditional methods.

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.

Dynamic pH junction high-speed counter-current chromatography coupled with microwave-assisted extraction for online separation and purification of alkaloids from Stephania cepharantha.

PubMed

Yuan, Zhiquan; Xiao, Xiaohua; Li, Gongke

2013-11-22

A simple and efficient dynamic pH junction high-speed counter-current chromatography method was developed and further applied to the online extraction, separation and purification of alkaloids from Stephania cepharantha by coupling with microwave-assisted extraction. Mineral acid and organic base were added into the mobile phase and the sample solution, respectively, leading to the formation of a dynamic pH junction in the column and causing focus of alkaloids. Selective focus of analytes can be achieved on the basis of velocity changes of the pH junction through appropriate selection of solvent systems and optimization of additive concentrations. The extract can be directly introduced into the HSCCC for the online extraction, separation and purification of alkaloids from S. cepharantha. Continuous separation can be easily achieved with the same solvent system. Under the optimum conditions, 6.0 g original sample was extracted with 60 mL of the upper phase of hexane-ethyl acetate-methanol-water (1:1:1:1, v/v/v/v) containing 10% triethylamine under 50 °C and 400 W irradiation power for 10 min, the extracts were directly separated and purified by high-speed counter-current chromatography. A total of 5.7 mg sinomenine, 8.3mg 6,7-di-O-acetylsinococuline, 17.9 mg berbamine, 12.7 mg isotetrandrine and 14.6 mg cepharanthine were obtained with purities of 96.7%, 93.7%, 98.7%, 97.3% and 99.3%, respectively. The online method provides good selectivity to ionizable compounds and improves the separation and purification efficiency of the high-speed counter-current chromatography technique. It has good potential for separation and purification of effective compounds from natural products. Copyright © 2013 Elsevier B.V. All rights reserved.

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

EPA Science Inventory

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

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

Extraction of three bioactive diterpenoids from Andrographis paniculata: effect of the extraction techniques on extract composition and quantification of three andrographolides using high-performance liquid chromatography.

PubMed

Kumar, Satyanshu; Dhanani, Tushar; Shah, Sonal

2014-10-01

Andrographis paniculata (Burm.f.) wall.ex Nees (Acanthaceae) or Kalmegh is an important medicinal plant finding uses in many Ayurvedic formulations. Diterpenoid compounds andrographolides (APs) are the main bioactive phytochemicals present in leaves and herbage of A. paniculata. The efficiency of supercritical fluid extraction (SFE) using carbon dioxide was compared with the solid-liquid extraction techniques such as solvent extraction, ultrasound-assisted solvent extraction and microwave-assisted solvent extraction with methanol, water and methanol-water as solvents. Also a rapid and validated reverse-phase high-performance liquid chromatography-diode array detection method was developed for the simultaneous determination of the three biologically active compounds, AP, neoandrographolide and andrograpanin, in the extracts of A. paniculata. Under the best SFE conditions tested for diterpenoids, which involved extraction at 60°C and 100 bar, the extractive efficiencies were 132 and 22 µg/g for AP and neoandrographolide, respectively. The modifier percentage significantly affected the extraction efficiency. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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.

Complex investigation of extraction techniques applied for cyclitols and sugars isolation from different species of Solidago genus.

PubMed

Ratiu, Ileana-Andreea; Al-Suod, Hossam; Ligor, Magdalena; Ligor, Tomasz; Railean-Plugaru, Viorica; Buszewski, Bogusław

2018-03-15

Cyclitols are phytochemicals naturally occurring in plant material, which attracted an increasing interest due to multiple medicinal attributes, among which the most important are the antidiabetic, antioxidant, and anticancer properties. Due to their valuable properties, sugars are used in the food industry as sweeteners, preservatives, texture modifiers, fermentation substrates, and flavoring and coloring agents. In this study, we report for the first time the quantitative analysis of sugars and cyclitols isolated from Solidago virgaurea L., which was used for the selection of the optimal solvent and extraction technique that can provide the best possible yield. Moreover, the quantities of sugars and cyclitols extracted from two other species, Solidago canadensis and Solidago gigantea, were investigated using the best extraction method and the most appropriate solvent. Comparative analysis of natural plant extracts obtained using five different techniques-maceration, Soxhlet extraction, pressurized liquid extraction, ultrasound-assisted extraction, and supercritical fluid extraction-was performed in order to decide the most suitable, efficient, and economically convenient extraction method. Three different solvents were used. Analysis of samples has been performed by solid-phase extraction for purification and pre-concentration, followed by derivation and GC-MS analysis. Highest efficiency for the total amount of obtained compounds has been reached by PLE, when water was used as a solvent. d-pinitol amount was almost similar for every solvent and for all the extraction techniques involved. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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

Ferrell, Jack R; Ware, Anne E

Two catalytic fast pyrolysis (CFP) oils (bottom/heavy fraction) were analyzed in various solvents that are used in common analytical methods (nuclear magnetic resonance - NMR, gas chromatography - GC, gel permeation chromatography - GPC, thermogravimetric analysis - TGA) for oil characterization and speciation. A more accurate analysis of the CFP oils can be obtained by identification and exploitation of solvent miscibility characteristics. Acetone and tetrahydrofuran can be used to completely solubilize CFP oils for analysis by GC and tetrahydrofuran can be used for traditional organic GPC analysis of the oils. DMSO-d6 can be used to solubilize CFP oils for analysismore » by 13C NMR. The fractionation of oils into solvents that did not completely solubilize the whole oils showed that miscibility can be related to the oil properties. This allows for solvent selection based on physico-chemical properties of the oils. However, based on semi-quantitative comparisons of the GC chromatograms, the organic solvent fractionation schemes did not speciate the oils based on specific analyte type. On the other hand, chlorinated solvents did fractionate the oils based on analyte size to a certain degree. Unfortunately, like raw pyrolysis oil, the matrix of the CFP oils is complicated and is not amenable to simple liquid-liquid extraction (LLE) or solvent fractionation to separate the oils based on the chemical and/or physical properties of individual components. For reliable analyses, for each analytical method used, it is critical that the bio-oil sample is both completely soluble and also not likely to react with the chosen solvent. The adoption of the standardized solvent selection protocols presented here will allow for greater reproducibility of analysis across different users and facilities.« less

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.

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.

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.

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.

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.

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.

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.

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.

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

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.

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 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.

Development of a carbon-nanoparticle-coated stirrer for stir bar sorptive extraction by a simple carbon deposition in flame.

PubMed

Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

2016-03-01

Stir bar sorptive extraction is an environmentally friendly microextraction technique based on a stir bar with various sorbents. A commercial stirrer is a good support, but it has not been used in stir bar sorptive extraction due to difficult modification. A stirrer was modified with carbon nanoparticles by a simple carbon deposition process in flame and characterized by scanning electron microscopy and energy-dispersive X-ray spectrometry. A three-dimensional porous coating was formed with carbon nanoparticles. In combination with high-performance liquid chromatography, the stir bar was evaluated using five polycyclic aromatic hydrocarbons as model analytes. Conditions including extraction time and temperature, ionic strength, and desorption solvent were investigated by a factor-by-factor optimization method. The established method exhibited good linearity (0.01-10 μg/L) and low limits of quantification (0.01 μg/L). It was applied to detect model analytes in environmental water samples. No analyte was detected in river water, and five analytes were quantified in rain water. The recoveries of five analytes in two samples with spiked at 2 μg/L were in the range of 92.2-106% and 93.4-108%, respectively. The results indicated that the carbon nanoparticle-coated stirrer was an efficient stir bar for extraction analysis of some polycyclic aromatic hydrocarbons. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

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.

Antifungal activity of extracts from Piper aduncum leaves prepared by different solvents and extraction techniques against dermatophytes Trichophyton rubrum and Trichophyton interdigitale.

PubMed

Santos, Maximillan Leite; Magalhães, Chaiana Froés; da Rosa, Marcelo Barcellos; de Assis Santos, Daniel; Brasileiro, Beatriz Gonçalves; de Carvalho, Leandro Machado; da Silva, Marcelo Barreto; Zani, Carlos Leomar; de Siqueira, Ezequias Pessoa; Peres, Rodrigo Loreto; Andrade, Anderson Assunção

2013-12-01

The effects of different solvents and extraction techniques upon the phytochemical profile and anti-Trichophyton activity of extracts from Piper aduncum leaves were evaluated. Extract done by maceration method with ethanol has higher content of sesquiterpenes and antifungal activity. This extract may be useful as an alternative treatment for dermatophytosis.

Antifungal activity of extracts from Piper aduncum leaves prepared by different solvents and extraction techniques against dermatophytes Trichophyton rubrum and Trichophyton interdigitale

PubMed Central

Santos, Maximillan Leite; Magalhães, Chaiana Froés; da Rosa, Marcelo Barcellos; de Assis Santos, Daniel; Brasileiro, Beatriz Gonçalves; de Carvalho, Leandro Machado; da Silva, Marcelo Barreto; Zani, Carlos Leomar; de Siqueira, Ezequias Pessoa; Peres, Rodrigo Loreto; Andrade, Anderson Assunção

2013-01-01

The effects of different solvents and extraction techniques upon the phytochemical profile and anti-Trichophyton activity of extracts from Piper aduncum leaves were evaluated. Extract done by maceration method with ethanol has higher content of sesquiterpenes and antifungal activity. This extract may be useful as an alternative treatment for dermatophytosis. PMID:24688522

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...

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.

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

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.

Enhancing concentration and mass sensitivities for liquid chromatography trace analysis of clopyralid in drinking water.

PubMed

Gu, Binghe; Meldrum, Brian; McCabe, Terry; Phillips, Scott

2012-01-01

A theoretical treatment was developed and validated that relates analyte concentration and mass sensitivities to injection volume, retention factor, particle diameter, column length, column inner diameter and detection wavelength in liquid chromatography, and sample volume and extracted volume in solid-phase extraction (SPE). The principles were applied to improve sensitivity for trace analysis of clopyralid in drinking water. It was demonstrated that a concentration limit of detection of 0.02 ppb (μg/L) for clopyralid could be achieved with the use of simple UV detection and 100 mL of a spiked drinking water sample. This enabled reliable quantitation of clopyralid at the targeted 0.1 ppb level. Using a buffered solution as the elution solvent (potassium acetate buffer, pH 4.5, containing 10% of methanol) in the SPE procedures was found superior to using 100% methanol, as it provided better extraction recovery (70-90%) and precision (5% for a concentration at 0.1 ppb level). In addition, the eluted sample was in a weaker solvent than the mobile phase, permitting the direct injection of the extracted sample, which enabled a faster cycle time of the overall analysis. Excluding the preparation of calibration standards, the analysis of a single sample, including acidification, extraction, elution and LC run, could be completed in 1 h. The method was used successfully for the determination of clopyralid in over 200 clopyralid monoethanolamine-fortified drinking water samples, which were treated with various water treatment resins. Copyright © 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

SOLVENT EXTRACTION PROCESS FOR THE RECOVERY OF METALS FROM PHOSPHORIC ACID

DOEpatents

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

1958-11-01

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

Multiresidue analysis of endocrine-disrupting compounds and perfluorinated sulfates and carboxylic acids in sediments by ultra-high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Cavaliere, Chiara; Capriotti, Anna Laura; Ferraris, Francesca; Foglia, Patrizia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

2016-03-18

A multiresidue analytical method for the determination of 11 perfluorinated compounds and 22 endocrine-disrupting compounds (ECDs) including 13 natural and synthetic estrogens (free and conjugated forms), 2 alkylphenols, 1 plasticiser, 2 UV-filters, 1 antimicrobial, and 2 organophosphorus compounds in sediments has been developed. Ultrasound-assisted extraction followed by solid phase extraction (SPE) with graphitized carbon black (GCB) cartridge as clean-up step were used. The extraction process yield was optimized in terms of solvent composition. Then, a 3(2) experimental design was used to optimize solvent volume and sonication time by response surface methodology, which simplifies the optimization procedure. The final extract was analyzed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry. The optimized sample preparation method is simple and robust, and allows recovery of ECDs belonging to different classes in a complex matrix such as sediment. The use of GCB for SPE allowed to obtain with a single clean-up procedure excellent recoveries ranging between 75 and 110% (relative standard deviation <16%). The developed methodology has been successfully applied to the analysis of ECDs in sediments from different rivers and lakes of the Lazio Region (Italy). These analyses have shown the ubiquitous presence of chloro-substituted organophosphorus flame retardants and bisphenol A, while other analyzed compounds were occasionally found at concentration between the limit of detection and quantification. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Determination of residual nonsteroidal anti-inflammatory drugs in aqueous sample using magnetic nanoparticles modified with cetyltrimethylammonium bromide by high performance liquid chromatography.

PubMed

Khoeini Sharifabadi, Malihe; Saber-Tehrani, Mohammad; Waqif Husain, Syed; Mehdinia, Ali; Aberoomand-Azar, Parviz

2014-01-01

A simple and sensitive solid-phase extraction method for separation and preconcentration of trace amount of four nonsteroidal anti-inflammatory drugs (naproxen, indomethacin, diclofenac, and ibuprofen) using Fe3O4 magnetic nanoparticles modified with cetyltrimethylammonium bromide has been developed. For this purpose, the surface of MNPs was modified with cetyltrimethylammonium bromide (CTAB) as a cationic surfactant. Effects of different parameters influencing the extraction efficiency of drugs including the pH, amount of salt, shaking time, eluent type, the volume of solvent, amount of adsorbent, sample volume, and the time of desorption were investigated and optimized. Methanol has been used as desorption solvent and the extracts were analysed on a reversed-phase octadecyl silica column using 0.02 M phosphate-buffer (pH = 6.02) acetonitrile (65 : 35 v/v) as the mobile phase and the effluents were measured at 202 nm with ultraviolet detector. The relative standard deviation (RSD%) of the method was investigated at three concentrations (25, 50, and 200 ng/mL) and was in the range of 3.98-9.83% (n = 6) for 50 ng/mL. The calibration curves obtained for studied drugs show reasonable linearity (R (2) > 0.99) and the limit of detection (LODs) ranged between 2 and 7 ng/mL. Finally, the proposed method has been effectively employed in extraction and determination of the drugs in biological and environmental samples.

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 ...

Combination of magnetic dispersive micro solid-phase extraction and supramolecular solvent-based microextraction followed by high-performance liquid chromatography for determination of trace amounts of cholesterol-lowering drugs in complicated matrices.

PubMed

Arghavani-Beydokhti, Somayeh; Rajabi, Maryam; Asghari, Alireza

2017-07-01

A novel, efficient, rapid, simple, sensitive, selective, and environmentally friendly method termed magnetic dispersive micro solid-phase extraction combined with supramolecular solvent-based microextraction (Mdμ-SPE-SSME) followed by high-performance liquid chromatography (HPLC) with UV detection is introduced for the simultaneous microextraction of cholesterol-lowering drugs in complicated matrices. In the first microextraction procedure, using layered double hydroxide (LDH)-coated Fe 3 O 4 magnetic nanoparticles, an efficient sample cleanup is simply and rapidly provided without the need for time-consuming centrifugation and elution steps. In the first step, desorption of the target analytes is easily performed through dissolution of the LDH-coated magnetic nanoparticles containing the target analytes in an acidic solution. In the next step, an emulsification microextraction method based on a supramolecular solvent is used for excellent preconcentration, ultimately resulting in an appropriate determination of the target analytes in real samples. Under the optimal experimental conditions, the Mdμ-SPE-SSME-HPLC-UV detection procedure provides good linearity in the ranges of 1.0-1500 ng mL -1 , 1.5-2000 ng mL -1 , and 2.0-2000 ng mL -1 with coefficients of determination of 0.995 or less, low limits of detection (0.3, 0.5, and 0.5 ng mL -1 ), and good extraction repeatabilities (relative standard deviations below 7.8%, n = 5) in deionized water for rosuvastatin, atorvastatin, and gemfibrozil, respectively. Finally, the proposed method is successfully applied for the determination of the target analytes in complicated matrices. Graphical Abstract Mdμ-SPE-SSME procedure.

Ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction for the simultaneous determination of 12 new antidepressants and 2 antipsychotics in whole blood by gas chromatography-mass spectrometry.

PubMed

Chen, Xiujuan; Zheng, Shuiqing; Le, Jian; Qian, Zheyuan; Zhang, Runsheng; Hong, Zhanying; Chai, Yifeng

2017-08-05

Antidepressant drugs are widely used in the treatment of different psychiatric disorders, as well as in conjunction with antipsychotics for the treatment of major depressive disorder. In this study, a simple and rapid ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) method was developed for the simultaneous determination of 12 new antidepressants (norfluoxetine, fluoxetine, fluvoxamine, agomelatine, mirtazapine, moclobemide, melitracen, N-desmethylmirtazapine, maprotiline, sertraline, citalopram, paroxetine) and 2 antipsychotics (clozapine and haloperidol) in human whole blood by gas chromatography-mass spectrometry (GC-MS). Different parameters affecting the UA-LDS-DLLME were optimized and the optimal conditions were as follows: 100μL of toluene as extraction solvent, extraction pH 12 and 3min of ultrasound stirring. Good linearity (R 2 ≥0.991) was obtained at the concentration range of 15-1500ng/mL for norfluoxetine, fluoxetine, fluvoxamine, melitracen, maprotiline and citalopram, and 5-500ng/mL for agomelatine, mirtazapine, moclobemide, N-desmethylmirtazapine, sertraline, paroxetine, clozapine and haloperidol. The intra-day and inter-day precision were all less than 10%, and accuracy of intra-day and inter-day were in the range of -12.7% to 7.9% and -13.9 to 11.8%, respectively. The extraction recoveries of most analytes were more than 60%. The UA-LDS-DLLME/GC-MS method was demonstrated with acceptable precision, accuracy and good specificity for the simultaneous determination of 12 antidepressants and 2 antipsychotics, and has been successfully applied in a real case. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

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

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

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.

Dispersive liquid-liquid microextraction of phenolic compounds from vegetable oils using a magnetic ionic liquid.

PubMed

Zhu, Shuqiang; Wang, Lijun; Su, Along; Zhang, Haixia

2017-08-01

A novel method was developed for the determination of two endocrine-disrupting chemicals, bisphenol A and 4-nonylphenol, in vegetable oil by dispersive liquid-liquid microextraction followed by ultra high performance liquid chromatography with tandem mass spectrometry. Using a magnetic liquid as the microextraction solvent, several key parameters were optimized, including the type and volume of the magnetic liquid, extraction time, amount of dispersant, and the type of reverse extractant. The detection limits for bisphenol A and 4-nonylphenol were 0.1 and 0.06 μg/kg, respectively. The recoveries were 70.4-112.3%, and the relative standard deviations were less than 4.2%. The method is simple for the extraction of bisphenol A and 4-nonylphenol from vegetable oil and suitable for routine analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The influence of extractable organic matter on vitrinite reflectance suppression: A survey of kerogen and coal types

USGS Publications Warehouse

Barker, C.E.; Lewan, M.D.; Pawlewicz, M.J.

2007-01-01

The vitrinite reflectance suppression literature shows that while bitumen impregnation of the vitrinite group is often invoked as a significant contributor to suppression, its existence is not often supported by petrological evidence. This study examines bitumen impregnation as a factor in vitrinite suppression by comparing the vitrinite reflectance of source rock and coal samples before and after solvent-extraction. Bitumen, often defined as organic matter soluble or extractable in certain organic solvents, should be removed by Soxhlet method solvent extraction using chloroform. Removing the extractable bitumen should restore the suppressed reflectance to its true higher value. However, the solvent extracted samples averaged 0.014% Rv less than that of the unextracted samples. We conclude from these results and from other published data that reflectance suppression by bitumen impregnation in the vitrinite maceral group, above the huminite stage of gelification, is seemingly a rare phenomenon and whose effect on suppressing vitrinite reflectance is typically negligible. ?? 2006.

Oil extraction from sheanut (Vitellaria paradoxa Gaertn C.F.) kernels assisted by microwaves.

PubMed

Nde, Divine B; Boldor, Dorin; Astete, Carlos; Muley, Pranjali; Xu, Zhimin

2016-03-01

Shea butter, is highly solicited in cosmetics, pharmaceuticals, chocolates and biodiesel formulations. Microwave assisted extraction (MAE) of butter from sheanut kernels was carried using the Doehlert's experimental design. Factors studied were microwave heating time, temperature and solvent/solute ratio while the responses were the quantity of oil extracted and the acid number. Second order models were established to describe the influence of experimental parameters on the responses studied. Under optimum MAE conditions of heating time 23 min, temperature 75 °C and solvent/solute ratio 4:1 more than 88 % of the oil with a free fatty acid (FFA) value less than 2, was extracted compared to the 10 h and solvent/solute ratio of 10:1 required for soxhlet extraction. Scanning electron microscopy was used to elucidate the effect of microwave heating on the kernels' microstructure. Substantial reduction in extraction time and volumes of solvent used and oil of suitable quality are the main benefits derived from the MAE process.

ALKYL PYROPHOSPHATE METAL SOLVENT EXTRACTANTS AND PROCESS

DOEpatents

Long, R.L.

1958-09-30

A process is presented for the recovery of uranium from aqueous mineral acidic solutions by solvent extraction. The extractant is a synmmetrical dialkyl pyrophosphate in which the alkyl substituents have a chain length of from 4 to 17 carbon atoms. Mentioned as a preferred extractant is dioctyl pyrophosphate. The uranium is precipitated irom the organic extractant phase with an agent such as HF, fluoride salts. alcohol, or ammonia.

Stable Isotope-Assisted Evaluation of Different Extraction Solvents for Untargeted Metabolomics of Plants

PubMed Central

Doppler, Maria; Kluger, Bernhard; Bueschl, Christoph; Schneider, Christina; Krska, Rudolf; Delcambre, Sylvie; Hiller, Karsten; Lemmens, Marc; Schuhmacher, Rainer

2016-01-01

The evaluation of extraction protocols for untargeted metabolomics approaches is still difficult. We have applied a novel stable isotope-assisted workflow for untargeted LC-HRMS-based plant metabolomics , which allows for the first time every detected feature to be considered for method evaluation. The efficiency and complementarity of commonly used extraction solvents, namely 1 + 3 (v/v) mixtures of water and selected organic solvents (methanol, acetonitrile or methanol/acetonitrile 1 + 1 (v/v)), with and without the addition of 0.1% (v/v) formic acid were compared. Four different wheat organs were sampled, extracted and analysed by LC-HRMS. Data evaluation was performed with the in-house-developed MetExtract II software and R. With all tested solvents a total of 871 metabolites were extracted in ear, 785 in stem, 733 in leaf and 517 in root samples, respectively. Between 48% (stem) and 57% (ear) of the metabolites detected in a particular organ were found with all extraction mixtures, and 127 of 996 metabolites were consistently shared between all extraction agent/organ combinations. In aqueous methanol, acidification with formic acid led to pronounced pH dependency regarding the precision of metabolite abundance and the number of detectable metabolites, whereas extracts of acetonitrile-containing mixtures were less affected. Moreover, methanol and acetonitrile have been found to be complementary with respect to extraction efficiency. Interestingly, the beneficial properties of both solvents can be combined by the use of a water-methanol-acetonitrile mixture for global metabolite extraction instead of aqueous methanol or aqueous acetonitrile alone. PMID:27367667

Streamlined structure elucidation of an unknown compound in a pigment formulation.

PubMed

Yüce, Imanuel; Morlock, Gertrud E

2016-10-21

A fast and reliable quality control is important for ink manufacturers to ensure a constant production grade of mixtures and chemical formulations, and unknown components attract their attention. Structure elucidating techniques seem time-consuming in combination with column-based methods, but especially the low solubility of pigment formulations is challenging the analysis. In contrast, layer chromatography is more tolerant with regard to pigment particles. One PLC plate for NMR and FTIR analyses and one HPTLC plate for recording of high resolution mass spectra, MS/MS spectra and for gathering information on polarity and spectral properties were needed to characterize a structure, exemplarily shown for an unknown component in pigment Red 57:1 to be 3-hydroxy-2-naphtoic acid. A preparative layer chromatography (PLC) workflow was developed that used an Automated Multiple Development 2 (AMD 2) system. The 0.5-mm PLC plate could still be operated in the AMD 2 system and allowed a smooth switch from the analytical to the preparative gradient separation. Through automated gradient development and the resulting focusing of bands, the sharpness of the PLC bands was improved. For NMR, the necessary high load of the target compound on the PLC plate was achieved via a selective solvent extraction that discriminated the polar sample matrix and thus increased the application volume of the extract that could maximally be applied without overloading. By doing so, the yield for NMR analysis was improved by a factor of 9. The effectivity gain through a simple, but thoroughly chosen extraction solvent is often overlooked, and for educational purpose, it was clearly illustrated and demonstrated by an extended solvent screening. Thus, PLC using an automated gradient development after a selective extraction was proven to be a new powerful combination for structural elucidation by NMR. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of residual 1,4-dioxane in surfactants and cleaning agents using headspace single-drop microextraction followed by gas chromatography-flame ionization detection.

PubMed

Saraji, M; Shirvani, N

2017-02-01

Polyethoxylated surfactants are widely used in the formulation of different cleaning agents such as shampoo, dish washing and hand washing products and lotion formulation. During the production of polyethoxylated surfactants, 1,4-dioxane as a toxic and carcinogenic by-product is formed. A simple low-cost method based on headspace single-drop microextraction combined with gas chromatography-flame ionization detection was developed for the determination of 1,4-dioxane in surfactants and cleaning agents. In this method, 1,4-dioxane was extracted from 8.0 mL sample solution into a microdrop of an organic solvent, and then, it was injected to gas chromatography. The effects of such parameters as the solvent type, salt addition, microdrop volume, stirring rate, equilibrium time, extraction time and the temperature of sample solution on the extraction performance were studied and optimized. An ethoxylated surfactant containing 1,4-dioxane was used as the sample for the optimization of the extraction parameters. The linear range, determination coefficient, limit of detection and relative standard deviation of the method were 0.5-100 μg g -1 , 0.9977, 0.4 μg g -1 and 7.2% (n = 5), respectively. Different real samples including sodium lauryl ether sulphate, sodium lauryl sulphate (SLS), four brands of shampoo, and hand washing and dish washing liquids were analysed by the method. 1,4-Dioxane was detected at the concentration range of 2.4-201 μg g -1 in the samples, except dish washing liquid and SLS. A new method with the merits of simplicity, low cost, low organic solvent consumption, short analysis time, good repeatability and suitable detection limit was developed for the analysis of 1,4-dioxane in surfactants and cleaning agents. © 2016 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Unique reversibility in extraction mechanism of U compared to solvent extraction for sorption of U(VI) and Pu(IV) by a novel solvent impregnated resin containing trialkyl phosphine oxide functionalized ionic liquid.

PubMed

Paramanik, M; Panja, S; Dhami, P S; Yadav, J S; Kaushik, C P; Ghosh, S K

2018-07-15

Novel Solvent Impregnated Resin (SIR) material was prepared by impregnating a trialkyl phosphine oxide functionalized ionic liquid (IL) into an inert polymeric material XAD-7. A series of SIR materials were prepared by varying the IL quantity. Sorption of both U(VI) and Pu(IV) were found to increase with increasing IL concentration in SIR up to an optimum IL concentration of 435 mg g -1 of SIR beyond which no effect of IL concentration was observed. A change of mechanism of sorption for U(VI) by SIR was observed in comparison to solvent extraction. The dependency of U(VI) sorption with nitric acid concentration showed a reverse trend compared to solvent extraction studies while for Pu(IV) the trend remained same as observed with solvent extraction. Sorption of both the radionuclides was found to follow pseudo second order mechanism and Langmuir adsorption isotherm. Distribution co-efficient measurements on IL impregnated SIR showed highly selective sorption of U(VI) and Pu(IV) over other trivalent f-elements and fission products from nitric acid medium. Copyright © 2018 Elsevier B.V. All rights reserved.

Fluid extraction

DOEpatents

Wai, Chien M.; Laintz, Kenneth E.

1999-01-01

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

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.

REMOVAL OF PCBS FROM A CONTAMINATED SOIL USING CF-SYSTEMS SOLVENT EXTRACTION PROCESS

EPA Science Inventory

The US EPA's START team in cooperation with EPA's SITE program evaluated a pilot scale solvent extraction process developed by CF-Systems. This process uses liquified propane to extract organic contaminants from soils, sludges, and sediments. A pilot-scale evaluation was conducte...

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...

Spent NiMH batteries-The role of selective precipitation in the recovery of valuable metals

NASA Astrophysics Data System (ADS)

Bertuol, Daniel Assumpção; Bernardes, Andréa Moura; Tenório, Jorge Alberto Soares

The production of electronic equipment, such as computers and cell phones, and, consequently, batteries, has increased dramatically. One of the types of batteries whose production and consumption has increased in recent times is the nickel metal hydride (NiMH) battery. This study evaluated a hydrometallurgical method of recovery of rare earths and a simple method to obtain a solution rich in Ni-Co from spent NiMH batteries. The active materials from both electrodes were manually removed from the accumulators and leached. Several acid and basic solutions for the recovery of rare earths were evaluated. Results showed that more than 98 wt.% of the rare earths were recovered as sulfate salts by dissolution with sulfuric acid, followed by selective precipitation at pH 1.2 using sodium hydroxide. The complete process, precipitation at pH 1.2 followed by precipitation at pH 7, removed about 100 wt.% of iron and 70 wt.% of zinc from the leaching solution. Results were similar to those found in studies that used solvent extraction. This method is easy, economic, and does not pose environmental threats of solvent extraction.

Alternative solvent-based methyl benzoate vortex-assisted dispersive liquid-liquid microextraction for the high-performance liquid chromatographic determination of benzimidazole fungicides in environmental water samples.

PubMed

Santaladchaiyakit, Yanawath; Srijaranai, Supalax

2014-11-01

Vortex-assisted dispersive liquid-liquid microextraction using methyl benzoate as an alternative extraction solvent for extracting and preconcentrating three benzimidazole fungicides (i.e., carbendazim, thiabendazole, and fluberidazole) in environmental water samples before high-performance liquid chromatographic analysis has been developed. The selected microextraction conditions were 250 μL of methyl benzoate containing 300 μL of ethanol, 1.0% w/v sodium acetate, and vortex agitation speed of 2100 rpm for 30 s. Under optimum conditions, preconcentration factors were 14.5-39.0 for the target fungicides. Limits of detection were obtained in the range of 0.01-0.05 μg/L. The proposed method was then applied to surface water samples and the recovery evaluations at three spiked concentration levels of 5, 30, and 50 μg/L were obtained in the range of 77.4-110.9% with the relative standard deviation <7.4%. The present method was simple, rapid, low cost, sensitive, environmentally friendly, and suitable for the trace analysis of the studied fungicides in environmental water samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Study on extracting and separating curcuminoids from Curcuma longa rhizome using ultrasound strengthen by microemulsion].

PubMed

Yue, Chun-Hua; Zheng, Li-Tao; Guo, Qi-Ming; Li, Kun-Ping

2014-05-01

To establish a new method for the extraction and separation of curcuminoids from Curcuma longa rhizome by cloud-point preconcentration using microemulsions as solvent. The spectrophotometry was used to detect the solubility of curcumin in different oil phase, emulsifier and auxiliary emulsifier, and the microemulsion prescription was used for false three-phase figure optimization. The extraction process was optimized by uniform experiment design. The curcuminoids were separated from microemulsion extract by cloud-point preconcentration. Oil phase was oleic acid ethyl ester; Emulsifier was OP emulsifier; Auxiliary emulsifier was polyethylene glycol(peg) 400; The quantity of emulsifier to auxiliary emulsifier was the ratio of 5: 1; Microemulsion prescription was water-oleic acid ethyl ester-mixed emulsifier (0.45:0.1:0.45). The optimum extraction process was: time for 12.5 min, temperature of 52 degrees C, power of 360 W, frequency of 400 kHz, and the liquid-solid ratio of 40:1. The extraction rate of curcuminoids was 92.17% and 86.85% in microemulsion and oil phase, respectively. Curcuminoids is soluble in this microemulsion prescription with good extraction rate. This method is simple and suitable for curcuminoids extraction from Curcuma longa rhizome.

Ionic liquid-based microwave-assisted extraction of flavonoids from Bauhinia championii (Benth.) Benth.

PubMed

Xu, Wei; Chu, Kedan; Li, Huang; Zhang, Yuqin; Zheng, Haiyin; Chen, Ruilan; Chen, Lidian

2012-12-03

An ionic liquids (IL)-based microwave-assisted approach for extraction and determination of flavonoids from Bauhinia championii (Benth.) Benth. was proposed for the first time. Several ILs with different cations and anions and the microwave-assisted extraction (MAE) conditions, including sample particle size, extraction time and liquid-solid ratio, were investigated. Two M 1-butyl-3-methylimidazolium bromide ([bmim] Br) solution with 0.80 M HCl was selected as the optimal solvent. Meanwhile the optimized conditions a ratio of liquid to material of 30:1, and the extraction for 10 min at 70 °C. Compared with conventional heat-reflux extraction (CHRE) and the regular MAE, IL-MAE exhibited a higher extraction yield and shorter extraction time (from 1.5 h to 10 min). The optimized extraction samples were analysed by LC-MS/MS. IL extracts of Bauhinia championii (Benth.)Benth consisted mainly of flavonoids, among which myricetin, quercetin and kaempferol, β-sitosterol, triacontane and hexacontane were identified. The study indicated that IL-MAE was an efficient and rapid method with simple sample preparation. LC-MS/MS was also used to determine the chemical composition of the ethyl acetate/MAE extract of Bauhinia championii (Benth.) Benth, and it maybe become a rapid method to determine the composition of new plant extracts.

Auto-Tandem Catalysis in Ionic Liquids: Synthesis of 2-Oxazolidinones by Palladium-Catalyzed Oxidative Carbonylation of Propargylic Amines in EmimEtSO₄.

PubMed

Mancuso, Raffaella; Maner, Asif; Ziccarelli, Ida; Pomelli, Christian; Chiappe, Cinzia; Della Ca', Nicola; Veltri, Lucia; Gabriele, Bartolo

2016-07-08

A convenient carbonylative approach to 2-oxazolidinone derivatives carried out using an ionic liquid (1-ethyl-3-methylimidazolium ethyl sulfate, EmimEtSO₄) as the solvent is presented. It is based on the sequential concatenation of two catalytic cycles, both catalyzed by the same metal species (auto-tandem catalysis): the first cycle corresponds to the oxidative monoaminocarbonylation of the triple bond of propargylic amines to give the corresponding 2-ynamide intermediates, while the second one involves the cyclocarbonylation of the latter to yield 2-(2-oxooxazolidin-5-ylidene)-acetamides. Reactions are carried out using a simple catalytic system consisting of PdI₂ in conjunction with an excess of KI, and the catalyst/solvent system could be recycled several times without appreciable loss of activity after extraction of the organic product with Et₂O.

Investigation of the pharmaceutical and pharmacological equivalence of different Hawthorn extracts.

PubMed

Vierling, W; Brand, N; Gaedcke, F; Sensch, K H; Schneider, E; Scholz, M

2003-01-01

Seven Hawthorn extracts were tested in isolated guinea pig aorta rings. The effect on noradrenaline- (10 microM) induced contraction was investigated. The extracts were prepared using ethanol (40 to 70% v/v), methanol (40 to 70% v/v), and water as the extraction solvents. The aqueous-alcoholic extracts displayed similar spectra of constituents. They were characterised by similar procyanidin, flavonoid, total vitexin and total phenols content and by similar TLC fingerprint chromatograms. The aqueous extract, however, showed a different fingerprint and a noticeably lower concentration of procyanidins, flavonoids and total phenols but a similar total vitexin content. All 7 extracts had a relaxant effect on the aorta precontracted by noradrenaline and led to relaxations to 44 until 29% of the initial values. The EC50 values of the aqueous-alcoholic extracts varied between 4.16 and 9.8 mg/l. The aqueous extract produced a similarly strong maximal relaxation as the other extracts, but the EC50, at 22.39 mg/l, was markedly higher. The results show that Hawthorn extracts with comparable quality profiles were obtained by using aqueous-alcoholic extraction solvents (40 to 70% ethanol or methanol). The extracts exerted comparable pharmacological effects. When using water as the extraction solvent, both, the spectrum of constituents and the pharmacological effect, deviated remarkably. It is thus possible to obtain bioequivalent extracts with comparable effect profiles by using 40 to 70% ethanol or methanol as the extraction solvent.

Solvent Selection for Extraction of Neodymium Concentrates of Monazite Sand Processed Product

NASA Astrophysics Data System (ADS)

Setyadji, Moch; Purwani, MV

2018-02-01

The extraction of neodymium concentrates of monazite sand processed product has been done. The objective of this investigation was to determine the best solvent to separate Nd from Nd concentrate. As an aqueous phase was Nd(OH)3 concentrated in HNO3 and as solvent or the organic phase was trioctylamine (TOA). tryibuthyl phosphate (TBP). trioctylphosphine oxyde (TOPO) and di-ethyl hexyl phosphoric acid (D2EHPA) in kerosene. The investigated variables were HNO3 concentration. feed concentration. solvent concentration or solvent in kerosene. time and stirring speeds. From the investigation on the selection of solvent for the extraction of Nd(OH)3 concentrate with various solvents. it was concluded that the extraction of Nd could be carried out by using TBP or TOA. Extraction of Nd using TOA at the optimum HNO3 concentration of 2M. feed concentration of 5 gram/10 mL. TOA in kerosene concentration of 6 %. stirring time of 15 minutes. stirring speed of 200 rpm was chosen if the Y concentration in Nd concentrate is small. In these condition DNd obtained was 0.65; extraction efficiency of Nd (ENd)=37.10%. the concentrations of Nd2(C2O4)3 = 67.14%. Ce2(C2O4)3 = 1.79%. La2(C2O4)3 = 1.37% and Y2(C2O4)3 = 24.70%. Extraction of Nd using TBP at the optimum HNO3 concentration of 1M. feed concentration of 5 gram/10 m. the TBP concentration in kerosene of 15%. stirring time of 15 minutes and stirring speed of 200 rpm was chosen if the Ce concentration in Nd concentrate is small. In these condition DNd obtained was 0.20. extraction efficiency of Nd (ENd)=17%. concentration of Nd2(C2O4)3 = 70.84%. Ce2(C2O4)3=15.53%. La2(C2O4)3 = 0.00% and Y2(C2O4)3 = 8.63%.

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

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

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

This report summarizes the results of the extraction, scrub, and strip testing for the September 2013 sampling of the Next Generation Solvent (NGS) Blended solvent from the Modular Caustic Side-Solvent Extraction Unit (MCU) Solvent Hold Tank. MCU is in the process of transitioning from the BOBCalixC6 solvent to the NGS Blend solvent. As part of that transition, MCU has intentionally created a blended solvent to be processed using the Salt Batch program. This sample represents the first sample received from that blended solvent. There were two ESS tests performed where NGS blended solvent performance was assessed using either the Tankmore » 21 material utilized in the Salt Batch 7 analyses or a simulant waste material used in the V-5/V-10 contactor testing. This report tabulates the temperature corrected cesium distribution, or D Cs values, step recovery percentage, and actual temperatures recorded during the experiment. This report also identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. The calculated extraction D Cs values using the Tank 21H material and simulant are 59.4 and 53.8, respectively. The DCs values for two scrub and three strip processes for the Tank 21 material are 4.58, 2.91, 0.00184, 0.0252, and 0.00575, respectively. The D-values for two scrub and three strip processes for the simulant are 3.47, 2.18, 0.00468, 0.00057, and 0.00572, respectively. These values are similar to previous measurements of Salt Batch 7 feed with lab-prepared blended solvent. These numbers are considered compatible to allow simulant testing to be completed in place of actual waste due to the limited availability of feed material.« less

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.

Effective and sensitive determination of eleven disinfection byproducts in drinking water by DLLME and GC-MS.

PubMed

On, Jiwon; Pyo, Heesoo; Myung, Seung-Woon

2018-10-15

The aim of this study was to optimize the dispersive liquid-liquid microextraction (DLLME) parameters for simultaneous analysis through DLLME-gas chromatography-mass spectrometry (GC-MS) of six iodo-trihalomethanes, four haloacetonitriles, and one halonitromethane, which are residual disinfection products found in drinking water. Eleven disinfection by-product (DBPs) remaining in aqueous samples were extracted and concentrated using a simple, rapid, and environmentally friendly DLLME method, and then analyzed simultaneously by GC-MS. The optimized DLLME parameters were a sample volume of 5 mL, 100 μL of dichloromethane as the extraction solvent, 1 mL of methanol as the dispersion solvent, an extraction time of 60 s, and 1.5 g of sodium chloride for the salting out effect. The enrichment factor values obtained using the established DLLME-GC-MS method were 19.8-141.5, and the limit of detection and limit of quantification were 0.22-1.19 μg/L and 0.75-3.98 μg/L, respectively. The calibration curves had correlation coefficients (r 2 ) of 0.9958-0.9992 in the concentration range of 0.5-40 μg/L, and they exhibited good linearity in quantitative analysis. This new method could be useful for analyzing eleven DBPs that remain in drinking water. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid-liquid microextraction followed by gas chromatographic analysis.

PubMed

Jain, Rajeev; Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Ch, Ratnasekhar; Murthy, R C; Khan, Haider A

2013-11-01

A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid-liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC-FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC-PCI-MS). Method was found to be linear over the range of 0.1-10 μg mL(-1) with square of correlation coefficient (R(2)) in the range of 0.9913-0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029-0.102 μg mL(-1) and 0.095-0.336 μg mL(-1) with a signal to noise ratio of 3:1 and 10:1, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Effective Method of Purification of Betulin from Birch Bark: The Importance of Its Purity for Scientific and Medicinal Use

PubMed Central

Šiman, Pavel; Filipová, Alžběta; Tichá, Alena; Niang, Mohamed; Bezrouk, Aleš; Havelek, Radim

2016-01-01

A new and relatively simple method for purification of betulin from birch bark extract was developed in this study. Its five purification steps are based on the differential solubility of extract components in various solvents and their crystallization and/or precipitation, on their affinity for Ca(OH)2 in ethanol, and on the affinity of some impurities for silica gel in chloroform. In addition, all used solvents can be simply recycled. Betulin of more than 99% purity can be prepared by this method with minimal costs. Various observations including crystallization of betulin, changes in crystals during heating, and attempt of localization of betulin in outer birch bark are also described in this work. The original extract, fraction without betulinic acid and lupeol, amorphous fraction of pure betulin, final crystalline fraction of pure betulin and commercial betulin as a standard were employed to determine the antiproliferative/cytotoxic effect. We used WST-1 tetrazolium-based assays with triple negative breast cancer cell line BT-549. The decrease in cell survival showed clear relationship with the purity of the samples, being most pronounced using our final product of pure crystalline betulin. WST-1 proliferation/cytotoxicity test using triple negative breast cancer cell line BT-549 clearly showed the importance of purity of betulin for biological experiments and, apparently, for its medicinal use. PMID:27152419

Analysis of PBDEs in soil, dust, spiked lake water, and human serum samples by hollow fiber-liquid phase microextraction combined with GC-ICP-MS.

PubMed

Xiao, Qin; Hu, Bin; Duan, Jiankun; He, Man; Zu, Wanqing

2007-10-01

A novel method for the analysis of four polybrominated diphenyl ethers (PBDEs) in environmental and human serum samples based on hollow fiber-liquid phase microextraction (HF-LPME) followed by gas chromatography-inductively coupled plasma mass spectrometric (GC-ICP-MS) detection has been developed. The organic solvent in the porous hollow fiber was first dipped into the sample for extraction at a given time, and the retracted organic phase was introduced into the GC-ICP-MS for analysis. The addition of methanol has a strong effect on the HF-LPME extraction efficiency. Other significant parameters affecting the extraction efficiency of HF-LPME were also studied. HF-LPME was effective to isolate the analytes from the complex matrix. Under the optimized conditions, the detection limits of the proposed method varied from 15.2 to 40.5 ng/L. In general, the relative standard deviations (RSDs) were less than 10%. Good linearity was obtained with the correlation coefficients all better than 0.999. The proposed method is simple, quick, few microliters of organic solvent required, and is especially suitable for the analysis of the real sample with small amount available. The overall process of HF-LPME with GC-ICP-MS was applied successfully for the determination of polybrominated diphenyl ethers (PBDEs) in environmental and spiked human serum samples, and the results were satisfactory.

Optimization of extraction conditions of some polyphenolic compounds from parsley leaves (Petroselinum crispum).

PubMed

Kuźma, Paula; Drużyńska, Beata; Obiedziński, Mieczysław

2014-01-01

Parsley leaf is a rich source of natural antioxidants, which serve a lot of functions in human body and prevent food from oxidation processes. The aim of the study was to investigate the influence of different extraction solvents and times of extraction on natural antioxidants content. Owing to the knowledge of the properties of extracted components and solvents, as well as their interactions, it is possible to achieve a high effectiveness of active compounds recovery. Three different extraction solvents (acetone 70% in water, methanol 80% in water and distilled water) and different times of extraction (30 and 60 minutes) were used to determine the efficiency of extraction of polyphenols and catechins, antioxidant activity against free radicals DPPH and ABTS and the ability to chelate ion Fe(2+) in dried parsley leaves. Other natural antioxidants contents in parsley leaves were also determined. In this study the best extraction solvent for polyphenols was acetone 70% and for catechins was distilled water. All extracts examined displayed the antioxidative activity, but water was the best solvent in the method of assaying the activity against ABTS(•+) and Fe(2+) ions chelating capability, whereas methanol turned out to be the least effective in this respect. Opposite results were observed in the case of determining the activity against DPPH(•). The prolongation of the extraction time enhanced or decreased antiradical activity in some cases. Additionally, important biologically active compounds in parsley leaves, such as vitamin C (248.31 mg/100 g dry matter), carotenoids (31.28 mg/100 g dry matter), chlorophyll (0.185 mg/g dry matter) were also analysed.

Effect of different solvents extracts and mode of action of Loktanella spp. Gb03 on toxic dinoflagellate

NASA Astrophysics Data System (ADS)

Hameed, Anmar; Usup, Gires; Ahmad, Asmat

2016-11-01

This study was aimed to evaluate the algicidal activity of Loktanella sp. Gb-03 bacterial extracts against toxic dinoflagellate, using various polar and non-polar solvents. For this purpose, six different solvent extracts were prepared (i.e. methanol, ethyl acetate, hexane, chloroform, acetonitrile and water). Ratio of 1:100 (v:v) (extract to dinoflagellate culture) of each extract was used for preliminary algicidal activity screening against toxic dinoflagellate Coolia malaynesis. Dinoflagellate cells at the stationary phase (1.0 × 103 cells/ mL) were treated with 1% (v/v) of each extract by using 24-well microplate. The plates were then incubated for 24 hours at dinoflagellate culture condition (under a light intensity of 140 µmol m-2s-1 and 12:12 hours light:dark photoperiod). The result of algicidal activity screening showed that all 6 extracts from Loktanella sp. Gb-03 had different ranges of algicidal activity against the toxic dinoflagellates. Ethyl acetate extract showed the highest activity against C. malaynesis and also other harmful dinoflagellate (Alexandrium sp. Alexandrium leei, Alexandrium affine, Alexandrium tamiyavanichi, Alexandrium tamarense, Gambierdiscus belizeanus, and Ostreopsis). This study was the first to explore the algicidal activity of Loktanella sp. Gb-03 extracts against toxic dinoflagellate with ethyl acetate as the best solvent to extract algicidal active compounds.

Feasibility of Surfactant-Free Supported Emulsion Liquid Membrane Extraction

NASA Technical Reports Server (NTRS)

Hu, Shih-Yao B.; Li, Jin; Wiencek, John M.

2001-01-01

Supported emulsion liquid membrane (SELM) is an effective means to conduct liquid-liquid extraction. SELM extraction is particularly attractive for separation tasks in the microgravity environment where density difference between the solvent and the internal phase of the emulsion is inconsequential and a stable dispersion can be maintained without surfactant. In this research, dispersed two-phase flow in SELM extraction is modeled using the Lagrangian method. The results show that SELM extraction process in the microgravity environment can be simulated on earth by matching the density of the solvent and the stripping phase. Feasibility of surfactant-free SELM (SFSELM) extraction is assessed by studying the coalescence behavior of the internal phase in the absence of the surfactant. Although the contacting area between the solvent and the internal phase in SFSELM extraction is significantly less than the area provided by regular emulsion due to drop coalescence, it is comparable to the area provided by a typical hollow-fiber membrane. Thus, the stripping process is highly unlikely to become the rate-limiting step in SFSELM extraction. SFSELM remains an effective way to achieve simultaneous extraction and stripping and is able to eliminate the equilibrium limitation in the typical solvent extraction processes. The SFSELM design is similar to the supported liquid membrane design in some aspects.

Interlaboratory comparison of mutagenesis testing of coal fly ash derived from differenct coal conversion technologies

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

Chrisp, C.; Hobbs, C.; Clark, R.

1979-01-01

This experiment showed that mutagenicity of fly ash derived from different coal conversion technologies, as determined by the Ames plate incorporation test, was similar in all three laboratories. The differences in mutagenic activity of each fly ash between laboratories with different solvent extraction methods were no greater than one order of magnitude. In addition, there were much smaller, but still significant differences in mutagenic activity between laboratories when the same solvent extract of a particular fly ash was tested in each laboratory. There were also significant differences in mutagenicity of the positive control mutagen (maximum of fivefold) between laboratories. Becausemore » of this difference in Ames test sensitivity between laboratories, the influence of the solvent extraction methods on differences in mutagenicity was not clear. However, the data suggested that either there were significant differences in the degree of sensitivity of Ames tests for different complex mixtures within each laboratory, or else there were differences in mutagen extraction efficiency between different solvent extraction methods. Both Ames test sensitivity and solvent extraction may be important. Further work would be necessary to separate the contribution of these two factors. An important aspect of further work would be to separate the contribution of the innate sensitivity of substrains of Ames tester strains in each laboratory from the possible effects of differences in Ames testing methodology. This could be done by testing the same extracts of fly ash and positive control mutagens with substrains of tester strains exchanged between laboratories. This work also implies that caution should be exercised in assuming that the same solvent would have the same efficiency for extraction of mutagens from different fly ashes even within the same laboratory.« less

Reutilization of mango byproducts: study of the effect of extraction solvent and temperature on their antioxidant properties.

PubMed

Dorta, Eva; Lobo, M Gloria; Gonzalez, Monica

2012-01-01

Mango biowastes, obtained after processing, contain large amounts of compounds with antioxidant activity that can be reused to reduce their environmental impact. The present study evaluates the effect of solvent (methanol, ethanol, acetone, water, methanol:water [1:1], ethanol:water [1:1], and acetone:water [1:1]), and temperature (25, 50, and 75 °C) on the efficiency of the extraction of antioxidants from mango peel and seed. Among the factors optimized, extraction solvent was the most important. The solvents that best obtained extracts with high antioxidant capacity were methanol, methanol:water, ethanol:water, and acetone:water (β-carotene test, antioxidant activity coefficient 173 to 926; thiobarbituric acid reactive substances test, inhibition ratio 15% to 89%; 2,2'-azino-bis-(3-ethylbenzothiazoline)-6-sulfonic acid ABTS(·+); and 2,2-diphenyl-1-picrylhydrazyl DPPH· scavenging, 7 to 22 and 8 to 28 g trolox equivalent antioxidant capacity [TE] per 100 g mango biowaste on a dry matter basis [DW]). Similarly, the flavonoid (0.21 to 1.4 g (+)-catechin equivalents per 100 g DW), tannin (3.8 to 14 g tannic acid equivalents per 100 g DW), and proanthocyanidin (0.23 to 7.8 g leucoanthocyanidin equivalents per 100 g DW) content was highest in the peel extracts obtained with methanol, ethanol:water, or acetone:water and in the seed extracts obtained with methanol or acetone:water. From the perspective of food security, it is advisable to choose ethanol (which also has a notable antioxidant content), ethanol:water, or acetone:water, as they are all solvents that can be used in compliance with good manufacturing practice. In general, increasing temperature improves the capacity of the extracts obtained from mango peel and seed to inhibit lipid peroxidation; however, its effect on the extraction of phytochemical compounds or on the capacity of the extracts to scavenge free radicals was negligible in comparison to that of the solvent. There are many antioxidant compounds in mango peel and seed, and they could be used as a natural and very inexpensive alternative to synthetic food additives. However, the conditions in which the antioxidants are extracted must be optimized. This work proves that conditions such as extraction solvent or temperature have a crucial impact on obtaining extracts rich in antioxidants from mango biowastes. © 2011 Institute of Food Technologists®

Multi-response optimisation of ultrasound-assisted extraction for recovery of flavonoids from red grape skins using response surface methodology.

PubMed

Tomaz, Ivana; Maslov, Luna; Stupić, Domagoj; Preiner, Darko; Ašperger, Danijela; Karoglan Kontić, Jasminka

2016-01-01

For the characterisation of grape cultivars, the profile and content of flavonoids are important because these compounds impact grape and wine quality. To determine the correct profile and content of flavonoids, the use of robust, sensitive and reliable methods is necessary. The object of this research is to develop a new ultrasound-assisted extraction (UAE) method for the recovery of flavonoids from grape skins using response surface methodology. Optimisation of UAE was performed using a complementary study combining a Box-Behnken experimental design with qualitative analysis by high-performance liquid chromatography. Optimal extraction conditions were obtained using the extraction solvent composed of acetonitrile:water:formic acid (26:73:1, v/v/v) at an extraction temperature of 50 °C, an extraction time of 15 min in a single-extraction step and with a solid-to-solvent ratio of 1:80 g/mL. The calculated relative standard deviations for the optimal extraction method were very low, measuring less than 5%. This study demonstrates that numerous factors have strong effects on the extraction efficiency, including the type of organic modifier and its percentage in the extraction solvent, the number of extraction steps, the solid-to-solvent ratio, the extraction time and temperature and, finally, the particular nature of analyte and their position within the grape skin cell. Copyright © 2015 John Wiley & Sons, Ltd.

Optimization of extraction of polysaccharides from fruiting body of Cordyceps militaris (L.) link using response surface methodology

NASA Astrophysics Data System (ADS)

Nguyen, Hoang Chinh; Thi, Dinh Huynh Mong; Pham, Dinh Chuong

2018-04-01

Polysaccharides from fruiting body of Cordyceps militaris (L.) Link possess various pharmaceutical activities. In this study, polysaccharides from the fruiting body of C. militaris were extracted with different solvents. Of those solvents tested, distilled water was identified as the most efficient solvent for the extraction, resulting in a significant increase in polysaccharides yield. Response surface methodology was then used to optimize the extraction conditions and establish a reliable mathematical model for prediction. A maximum polysaccharides yield of 11.07% was reached at a ratio of water to raw material of 23.2:1 mL/g, an extraction time of 76 min, and a temperature of 93.6°C. This study indicates that the obtained optimal extraction conditions are an efficient method for extraction of polysaccharides from the fruiting body of C. militaris.

Evaluation of different solvent mixtures in esterifiable lipids extraction from microalgae Botryococcus braunii for biodiesel production.

PubMed

Hidalgo, Pamela; Ciudad, Gustavo; Navia, Rodrigo

2016-02-01

Non-polar and polar solvents as well as their mixtures were tested for the extraction of microalgae lipids and thus, to evaluate their effect on total and esterifiable lipids extraction yields with potential to be converted to biodiesel. The obtained results show an increase in lipids and esterifiable lipids extraction yields when non-polar and polar solvent mixtures were used. The higher esterifiable lipids extraction yield was 19.2%wt (based on dry biomass) using a chloroform-methanol mixture (75%v/v of methanol), corresponding to a 98.9%wt esterifiable lipids extraction. In addition, esterifiable lipids extraction yield of 18.9%wt (based on dry biomass) was obtained when a petroleum ether-methanol mixture (75%v/v of methanol) was used, corresponding to a 96.9%wt esterifiable lipids extraction. Copyright © 2015 Elsevier Ltd. All rights reserved.

Comparison of ambient solvent extraction methods for the analysis of fatty acids in non-starch lipids of flour and starch

PubMed Central

Bahrami, Niloufar; Yonekura, Lina; Linforth, Robert; Carvalho da Silva, Margarida; Hill, Sandra; Penson, Simon; Chope, Gemma; Fisk, Ian Denis

2014-01-01

BACKGROUND Lipids are minor components of flours, but are major determinants of baking properties and end-product quality. To the best of our knowledge, there is no single solvent system currently known that efficiently extracts all non-starch lipids from all flours without the risk of chemical, mechanical or thermal damage. This paper compares nine ambient solvent systems (monophasic and biphasic) with varying polarities: Bligh and Dyer (BD); modified Bligh and Dyer using HCl (BDHCL); modified BD using NaCl (BDNaCl); methanol–chloroform–hexane (3:2:1, v/v); Hara and Radin (hexane–isopropanol, 3:2, v/v); water-saturated n-butanol; chloroform; methanol and hexane for their ability to extract total non-starch lipids (separated by lipid classes) from wheat flour (Triticum aestivum L.). Seven ambient extraction protocols were further compared for their ability to extract total non-starch lipids from three alternative samples: barley flour (Hordeum vulgare L.), maize starch (Zea mays L.) and tapioca starch (Manihot esculenta Crantz). RESULTS For wheat flour the original BD method and those containing HCl or NaCl tended to extract the maximum lipid and a significant correlation between lipid extraction yield (especially the glycolipids and phospholipids) and the polarity of the solvent was observed. For the wider range of samples BD and BD HCl repeatedly offered the maximum extraction yield and using pooled standardized (by sample) data from all flours, total non-starch lipid extraction yield was positively correlated with solvent polarity (r = 0.5682, P < 0.05) and water ratio in the solvent mixture (r = 0.5299, P < 0.05). CONCLUSION In general, BD-based methods showed better extraction yields compared to methods without the addition of water and, most interestingly, there was much greater method dependence of lipid yields in the starches when compared to the flour samples, which is due to the differences in lipid profiles between the two sample types (flours and starches). PMID:24132804

Fluoro-alcohol phase modifiers and process for cesium solvent extraction

DOEpatents

Bonnesen, Peter V.; Moyer, Bruce A.; Sachleben, Richard A.

2003-05-20

The invention relates to a class of phenoxy fluoro-alcohols, their preparation, and their use as phase modifiers and solvating agents in a solvent composition for the extraction of cesium from alkaline solutions. These phenoxy fluoro-alcohols comply with the formula: ##STR1## in which n=2 to 4; X represents a hydrogen or a fluorine atom, and R.sup.2 -R.sup.6 are hydrogen or alkyl substituents. These phenoxy fluoro-alcohol phase modifiers are a necessary component to a robust solvent composition and process useful for the removal of radioactive cesium from alkaline nuclear waste streams. The fluoro-alcohols can also be used in solvents designed to extract other cesium from acidic or neutral solutions.

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.

Isocratic non-aqueous reversed-phase high-performance liquid chromatographic separation of capsanthin and capsorubin in red peppers (Capsicum annuum L.), paprika and oleoresin.

PubMed

Weissenberg, M; Schaeffler, I; Menagem, E; Barzilai, M; Levy, A

1997-01-03

A simple, rapid high-performance liquid chromatography method has been devised in order to separate and quantify the xanthophylls capsorubin and capasanthin present in red pepper (Capsicum annuum L.) fruits and preparations made from them (paprika and oleoresin). A reversed-phase isocratic non-aqueous system allows the separation of xanthophylls within a few minutes, with detection at 450 nm, using methyl red as internal standard to locate the various carotenoids and xanthophylls found in plant extracts. The selection of extraction solvents, mild saponification conditions, and chromatographic features is evaluated and discussed. The method is proposed for rapid screening of large plant populations, plant selection, as well as for paprika products and oleoresin, and also for nutrition and quality control studies.

Pipette tip solid-phase extraction and high-performance liquid chromatography for the determination of flavonoids from Epimedii herba in rat serum and application of the technique to pharmacokinetic studies.

PubMed

Wang, Nani; Huang, Xiaowen; Wang, Xuping; Zhang, Yang; Wu, Renjie; Shou, Dan

2015-05-15

Epimedii herba is a traditional Chinese medicine for the treatment of osteoporosis. Epimedin A, B and C and icariin are the primary effective ingredients of this medicine. In this study, a simple and low-cost method based on pipette tip solid-phase extraction, high-performance liquid chromatography separation, and diode array detection has been developed for the simultaneous analysis of four flavonoids (epimedin A, B and C and icariin) from Epimedii herba in rat serum samples. In this novel extraction configuration, the sorbents were placed between a filter (hollow fiber) and the pipette tip. Pipette tip solid-phase extraction has several advantages compared to conventional extraction methods: faster extraction time (6.0min); lower sample volume (100μL); lower solvent volume (100μL); and less solvent waste. Under the optimum extraction conditions, the method showed good linearity (0.05-10.0μgmL(-1)), acceptable intra- and inter precision (RSD<6%), low limits of quantification (0.027-0.045μgmL(-1)) and satisfactory relative recoveries (98.63-103.18%). This method was successfully applied to investigate the pharmacokinetics of the major flavonoids in Epimedii herba extract after oral administration to rats (10gkg(-1) body weight). The primary pharmacokinetic parameters for rats were determined as follows: Cmax, 0.45-4.11μgmL(-1); Tmax, 0.21-0.26h; t1/2α, 0.06-0.12h; t1/2β, 2.02-3.48h; AUC0-∞: 0.50-2.58μghmL(-1); CL, 19.53-44.72Lkg(-1)h(-1); and MRT0-∞, 2.25-3.77h. The developed method has the potential to promulgate the pharmacokinetics and provide more information for clinical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Alcohol based-deep eutectic solvent (DES) as an alternative green additive to increase rotenone yield

NASA Astrophysics Data System (ADS)

Othman, Zetty Shafiqa; Hassan, Nur Hasyareeda; Zubairi, Saiful Irwan

2015-09-01

Deep eutectic solvents (DESs) are basically molten salts that interact by forming hydrogen bonds between two added components at a ratio where eutectic point reaches a melting point lower than that of each individual component. Their remarkable physicochemical properties (similar to ionic liquids) with remarkable green properties, low cost and easy handling make them a growing interest in many fields of research. Therefore, the objective of pursuing this study is to analyze the potential of alcohol-based DES as an extraction medium for rotenone extraction from Derris elliptica roots. DES was prepared by a combination of choline chloride, ChCl and 1, 4-butanediol at a ratio of 1/5. The structure of elucidation of DES was analyzed using FTIR, 1H-NMR and 13C-NMR. Normal soaking extraction (NSE) method was carried out for 14 hours using seven different types of solvent systems of (1) acetone; (2) methanol; (3) acetonitrile; (4) DES; (5) DES + methanol; (6) DES + acetonitrile; and (7) [BMIM] OTf + acetone. Next, the yield of rotenone, % (w/w), and its concentration (mg/ml) in dried roots were quantitatively determined by means of RP-HPLC. The results showed that a binary solvent system of [BMIM] OTf + acetone and DES + acetonitrile was the best solvent system combination as compared to other solvent systems. It contributed to the highest rotenone content of 0.84 ± 0.05% (w/w) (1.09 ± 0.06 mg/ml) and 0.84 ± 0.02% (w/w) (1.03 ± 0.01 mg/ml) after 14 hours of exhaustive extraction time. In conclusion, a combination of the DES with a selective organic solvent has been proven to have a similar potential and efficiency as of ILs in extracting bioactive constituents in the phytochemical extraction process.

METHOD FOR DISSOLVING ZIRCONIUM-URANIUM COMPOSITIONS

DOEpatents

Gens, T.A.

1961-07-18

A method is descrioed for treating a zirconium-- uranium composition to form a stable solution from which uranium and other values may be extracted by contacting the composition with at least a 4 molar aqueous solution of ammonium fluoride at a temperature of about 100 deg C, adding a peroxide, in incremental amounts, to the heated solution throughout the period of dissolution until all of the uranium is converted to soluble uranyl salt, adding nitric acid to the resultant solution to form a solvent extraction feed solution to convert the uranyl salt to a solvent extractable state, and thereafter recovering the uranium and other desired values from the feed solution by solvent extraction.

Fast and effective low-temperature freezing extraction technique to determine organotin compounds in edible vegetable oil.

PubMed

Liu, Yingxia; Ma, Yaqian; Wan, Yiqun; Guo, Lan; Wan, Xiaofen

2016-06-01

Most organotin compounds that have been widely used in food packaging materials and production process show serious toxicity effects to human health. In this study, a simple and low-cost method based on high-performance liquid chromatography with inductively coupled plasma mass spectrometry for the simultaneous determination of four organotins in edible vegetable oil samples was developed. Four organotins including dibutyltin dichloride, tributyltin chloride, diphenyltin dichloride, and triphenyltin chloride were simultaneously extracted with methanol using the low-temperature precipitation process. After being concentrated, the extracts were purified by matrix solid-phase dispersion using graphitized carbon black. The experimental parameters such as extraction solvent and clean-up material were optimized. To evaluate the accuracy of the new method, the recoveries were investigated. In addition, a liquid chromatography with tandem mass spectrometry method was also proposed for comparison. The procedures of extracting and purifying samples for the analysis were simple and easy to perform batch operations, also showed good efficiency with lower relative standard deviation. The limits of detection of the four organotins were 0.28-0.59 μg/L, and the limits of quantification of the four organotins were 0.93-1.8 μg/L, respectively. The proposed method was successfully applied to the simultaneous analysis of the four organotins in edible vegetable oil. Some analytes were detected at the level of 2.5-28.8 μg/kg. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fabric phase sorptive extraction of selected penicillin antibiotic residues from intact milk followed by high performance liquid chromatography with diode array detection.

PubMed

Samanidou, Victoria; Michaelidou, Katia; Kabir, Abuzar; Furton, Kenneth G

2017-06-01

Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows' milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10μg/kg for benzylpenicillin, 20μg/kg for cloxacillin, 25μg/kg dicloxacillin and 30μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Vegetable Oils as Alternative Solvents for Green Oleo-Extraction, Purification and Formulation of Food and Natural Products.

PubMed

Yara-Varón, Edinson; Li, Ying; Balcells, Mercè; Canela-Garayoa, Ramon; Fabiano-Tixier, Anne-Sylvie; Chemat, Farid

2017-09-05

Since solvents of petroleum origin are now strictly regulated worldwide, there is a growing demand for using greener, bio-based and renewable solvents for extraction, purification and formulation of natural and food products. The ideal alternative solvents are non-volatile organic compounds (VOCs) that have high dissolving power and flash point, together with low toxicity and less environmental impact. They should be obtained from renewable resources at a reasonable price and be easy to recycle. Based on the principles of Green Chemistry and Green Engineering, vegetable oils could become an ideal alternative solvent to extract compounds for purification, enrichment, or even pollution remediation. This review presents an overview of vegetable oils as solvents enriched with various bioactive compounds from natural resources, as well as the relationship between dissolving power of non-polar and polar bioactive components with the function of fatty acids and/or lipid classes in vegetable oils, and other minor components. A focus on simulation of solvent-solute interactions and a discussion of polar paradox theory propose a mechanism explaining the phenomena of dissolving polar and non-polar bioactive components in vegetable oils as green solvents with variable polarity.

Microwave-assisted micellar extraction of organic and inorganic iodines using zwitterionic surfactants.

PubMed

Wang, Shu-Ling; Yi, Ling; Ye, Li-Hong; Cao, Jun; Du, Li-Jing; Peng, Li-Qing; Xu, Jing-Jing; Zhang, Qi-Dong

2017-08-04

Zwitterionic surfactant, used as extractant in microwave-assisted extraction (MAE) was investigated for the first time to extract organic and inorganic iodines from kelp samples. Optimized conditions for the MAE were 200W of microwave irradiation power, 100°C of extraction temperature, 10min of microwave irradiation time, 1g of sample, and 20mL of solvent volume. Ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS) was used for the quantitative and qualitative analyses of the iodines. Under the optimum experimental conditions, KI, MIT and DIT were identified in kelp samples, the limits of detection of these analytes were ranged between 3.39 and 6.31ng/mL. The recoveries for spiked samples obtained from different areas were all higher than 92.48%. Compared with the ultrasound-assisted extraction, the proposed method is faster and more effective. Thus, the combination of zwitterionic surfactant-MAE and UHPLC-Q-TOF/MS made up a simple, rapid and effective approach for extraction and determination of iodine compounds in complex seaweed materials. Copyright © 2017 Elsevier B.V. All rights reserved.

Theory of hydrophobicity: transient cavities in molecular liquids

NASA Technical Reports Server (NTRS)

Pratt, L. R.; Pohorille, A.

1992-01-01

Observation of the size distribution of transient cavities in computer simulations of water, n-hexane, and n-dodecane under benchtop conditions shows that the sizes of cavities are more sharply defined in liquid water but the most-probable-size cavities are about the same size in each of these liquids. The calculated solvent atomic density in contact with these cavities shows that water applies more force per unit area of cavity surface than do the hydrocarbon liquids. This contact density, or "squeezing" force, reaches a maximum near cavity diameters of 2.4 angstroms. The results for liquid water are compared to the predictions of simple theories and, in addition, to results for a reference simple liquid. The numerical data for water at a range of temperatures are analyzed to extract a surface free energy contribution to the work of formation of atomic-size cavities. Comparison with the liquid-vapor interfacial tensions of the model liquids studied here indicates that the surface free energies extracted for atomic-size cavities cannot be accurately identified with the macroscopic surface tensions of the systems.

Theory of hydrophobicity: Transient cavities in molecular liquids

PubMed Central

Pratt, Lawrence R.; Pohorille, Andrew

1992-01-01

Observation of the size distribution of transient cavities in computer simulations of water, n-hexane, and n-dodecane under benchtop conditions shows that the sizes of cavities are more sharply defined in liquid water but the most-probable-size cavities are about the same size in each of these liquids. The calculated solvent atomic density in contact with these cavities shows that water applies more force per unit area of cavity surface than do the hydrocarbon liquids. This contact density, or “squeezing” force, reaches a maximum near cavity diameters of 2.4 Å. The results for liquid water are compared to the predictions of simple theories and, in addition, to results for a reference simple liquid. The numerical data for water at a range of temperatures are analyzed to extract a surface free energy contribution to the work of formation of atomic-size cavities. Comparison with the liquid-vapor interfacial tensions of the model liquids studies here indicates that the surface free energies extracted for atomic-size cavities cannot be accurately identified with the macroscopic surface tensions of the systems. PMID:11537863

Investigating the effect of various extracting solvents on the potential use of red-apple skin (Malus domestica) as natural sensitizer for dye-sensitized solar cell

NASA Astrophysics Data System (ADS)

Saputro, Aldhi; Mizan, Adlan; Sofyan, Nofrijon; Yuwono, Akhmad Herman

2017-03-01

In the current investigation, the natural dye extracted from red-apple (Malus domestica) skin was used as natural sensitizer for dye sensitized solar cell (DSSC) application. The present study was specifically aimed at observing the effect of different solvents, i.e. deionized water, ethanol, and acidified ethanol, on the performance of the natural dye and thus the DSSC. For synthesis purposes, red-apple skin was peeled off, dried, crushed and furthermore extracted with ratio red-apple skin powder to solvent 1:20 w/v for 2 hours at 50°C under mechanical stirring. Subsequently, the resulting natural dyes with different solvents were examined by Fourier transform infrared (FTIR) to analyze their functional groups, UV-Vis spectroscopy to observe their absorption spectra for a wide range of wavelength, while TiO2 nanoparticle used as the semiconductor oxide layer in the device was characterized by field emission scanning electron microscope (FESEM). The FTIR results showed that the red-apple skin has anthocyanin group which functions as the sensitizer agent for photon energy absorption from the sunlight. The UV-Vis spectroscopy results showed that ethanol solvent has higher absorption of sunlight wavelength as compared to those of deionized water and acidified ethanol solvents. The performance test of the fabricated DSSC showed the prototype made of the red apple skin dye extracted by ethanol solvent can provide the highest open circuit voltage (Voc) up to 324 mV and efficiency around 0.046%. On the basis of investigation, it has been found that ethanol was the best solvent to extract anthocyanin from the red-apple skin.

U-EXTRACTION--IMPROVEMENTS IN ELIMINATION OF Mo BY USE OF FERRIC ION

DOEpatents

Clark, H.M.; Duffey, D.

1958-06-10

An improved solvent extraction process is described whereby U may be extracted by a water immiscible organic solvent from an aqueous solution of uranyl nitrate. It has been found that Mo in the presence of phosphate ions appears to form a complex with the phosphate which extracts along with the U. This extraction of Mo may be suppressed by providing ferric ion in the solution prior to the extraction step. The ferric ion is preferably provided in the form of ferric nitrate.

Immunomodulatory activities of different solvent extracts from Tricholoma matsutake (S. Ito et S. Imai) singer (higher basidiomycetes) on normal mice.

PubMed

Yin, Xiulian; You, Qinghong; Jiang, Zhonghai

2012-01-01

The immunomodulatory activities of different solvent extracts from the culinary-medicinal mushroom Tricholoma matsutake were studied in vivo in normal mice. The extracts were prepared using different solvents in an order of increasing polarity. The immunomodulatory activities were investigated by measuring the thymus and spleen index, phagocytic rate of macrophage phagocytosis, delayed-type hypersensitivity, plaque-forming cell, and proliferation of splenocytes. Results demonstrated that water extract (WE) and n-butyl alcohol extract (BAE) of T. matsutake could enhance the immunity of mice significantly compared with the control group. Main components of WE and BAE were polysaccharides, proteins, and flavonoids; we presume that these may be the main immunomodulating and immuno-enhancing agents in T. matsutake.

Fundamental studies on the feasibility of deep eutectic solvents for the selective partition of glaucarubinone present in the roots of Simarouba glauca.

PubMed

Kholiya, Faisal; Bhatt, Nidhi; Rathod, Meena R; Meena, Ramavatar; Prasad, Kamalesh

2015-07-14

Several deep eutectic solvents prepared by the complexation of choline chloride as the hydrogen bond acceptor and hydrogen bond donors such as urea, thiourea, ethylene glycol, and glycerol were employed to partition glaucarubinone, an antimalarial compound present in roots of the plant, Simarouba glauca. Among all the solvents, the deep eutectic solvent consisting of the mixture of choline chloride and urea the most suitable to partition the antimalarial compound from the extract selectively. Analytical tools such as high-performance liquid chromatography and electrospray ionization mass spectrometry were used for characterizations, and glaucarubinone extracted from the roots of the plant by conventional solvent extraction method was used as a reference for comparison. The hydrogen and noncovalent bonds formed between glaucarubinone and the deep eutectic solvents could be responsible for the selective partition of the drug molecule. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of HEH[EHP] impurities on the ALSEP solvent extraction process

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

Holfeltz, Vanessa E.; Campbell, Emily L.; Peterman, Dean R.

In solvent extraction processes, organic phase impurities can negatively impact separation factors, hydrolytic performance, and overall system robustness. This affects the process-level viability of a separation concept and necessitates knowledge of the behavior and mechanisms to control impurities in the solvent. The most widespread way through which impurities are introduced into a system is through impure extractants and/or diluents used to prepare the solvent, and often development of new purification schemes to achieve the desired level of purity is needed. In this work, the acidic extractant, 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (HEH[EHP])—proposed for application in extractive processes aimed at separating trivalentmore » minor actinides from lanthanides and other fission products—is characterized with respect to its common impurities and their impact on Am(III) stripping in the Actinide Lanthanide SEParation (ALSEP) system. To control impurities in HEH[EHP], existing purification technologies commonly applied for the acidic organophosphorus reagents are reviewed, and a new method specific to HEH[EHP] purification is presented.« less

Supercritical-Fluid Extraction of Oil From Tar Sands

NASA Technical Reports Server (NTRS)

Compton, L. E.

1982-01-01

New supercritical solvent mixtures have been laboratory-tested for extraction of oil from tar sands. Mixture is circulated through sand at high pressure and at a temperature above critical point, dissolving organic matter into the compressed gas. Extract is recovered from sand residues. Low-temperature super-critical solvents reduce energy consumption and waste-disposal problems.

Spectroscopic, calorimetric and structural analyses of the effects of hydrothermal treatment of rice beans and the extraction solvent on starch characteristics.

PubMed

González-Cruz, Leopoldo; Montañez-Soto, José Luis; Conde-Barajas, Eloy; Negrete-Rodríguez, María de la Luz Xochilt; Flores-Morales, Areli; Bernardino-Nicanor, Aurea

2018-02-01

The modification of the starches extracted from rice beans both with and without hydrothermal treatment was evaluated via scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and Fourier transform infrared (FT-IR) and Raman spectroscopy. SEM indicated that the starch granules of rice beans exhibit wide variation in granule shape, showing the greatest size and modification of the surface when extracted with ethanol. It was found that the extraction solvent had no significant effect on the onset (T o ) and peak (T p ) temperatures of the starch, whereas hydrothermal treatment of rice beans decreased the T o , T p and ΔH of the starch. The modification of FT-IR spectra showed that hydrothermal treatment of rice beans and the solvent used in the extraction of starch affected starch crystallinity, mainly when ethanol was used. Raman spectroscopy revealed that the smaller changes in the starch bonds were due to the solvent used for starch extraction but that hydrothermal treatment disturbed all bonds in the starch. Copyright © 2017 Elsevier B.V. All rights reserved.

Dispersive liquid-liquid microextraction based on the solidification of floating organic droplet for the determination of polychlorinated biphenyls in aqueous samples.

PubMed

Dai, Liping; Cheng, Jing; Matsadiq, Guzalnur; Liu, Lu; Li, Jun-Kai

2010-08-03

In the proposed method, an extraction solvent with a lower toxicity and density than the solvents typically used in dispersive liquid-liquid microextraction was used to extract seven polychlorinated biphenyls (PCBs) from aqueous samples. Due to the density and melting point of the extraction solvent, the extract which forms a layer on top of aqueous sample can be collected by solidifying it at low temperatures, which form a layer on top of the aqueous sample. Furthermore, the solidified phase can be easily removed from the aqueous phase. Based on preliminary studies, 1-undecanol was selected as the extraction solvent, and a series of parameters that affect the extraction efficiency were systematically investigated. Under the optimized conditions, enrichment factors for PCBs ranged between 494 and 606. Based on a signal-to-noise ratio of 3, the limit of detection for the method ranged between 3.3 and 5.4 ng L(-1). Good linearity, reproducibility and recovery were also obtained. 2010 Elsevier B.V. All rights reserved.

Comparison of magnesium sulfate and sodium sulfate for removal of water from pesticide extracts of foods.

PubMed

Schenck, Frank J; Callery, Patrick; Gannett, Peter M; Daft, Jonathan R; Lehotay, Steven J

2002-01-01

Water-miscible solvents, such as acetone and acetonitrile, effectively extract both polar and nonpolar pesticide residues from nonfatty foods. The addition of sodium chloride to the resulting acetonitrile-water or acetone-water extract (salting out) results in the separation of the water from the organic solvent. However, the organic solvent layer (pesticide extract) still contains some residual water, which can adversely affect separation procedures that follow, such as solid-phase extraction and/or gas chromatography. Drying agents, such as sodium sulfate or magnesium sulfate, are used to remove the water from the organic extracts. In the present study, we used nuclear magnetic resonance spectroscopy to study the composition of the phases resulting from salting out and to compare the effectiveness of sodium sulfate and magnesium sulfate as drying agents. The study showed that considerable amounts of water remained in the organic phase after phase separation. Sodium sulfate was a relatively ineffective drying agent, removing little or no residual water from the organic solvent. Magnesium sulfate proved to be a much more effective drying agent.

Deterred drug abuse using superabsorbent polymers.

PubMed

Mastropietro, David J; Muppalaneni, Srinath; Omidian, Hossein

2016-11-01

This study aimed to determine whether selected superabsorbent polymers (SAPs) could be used as a suitable alternative to thwart extraction, filtration, and syringeability attempts for abuse. Many abuse-deterrent formulations (ADFs) rely on high molecular weight polymers such as poly(ethylene oxide) to provide crush and extraction resistance. However, these polymers suffer from slow dissolution kinetics, and are susceptible to a variety of abuse conditions. Several commercially available SAPs were evaluated for swelling behavior in extraction solvents, and tableting properties. Post-compaction abuse properties were evaluated by recoverable volume and syringeability after solvent extraction. Drug release and percent drug extraction were conducted using tramadol HCl as a model drug. Certain SAPs had the ability to rapidly imbibe solvent and effectively stop extraction processes in a variety of solvents, including water and water/alcohol mixtures. Tablets containing SAP and drug showed no effect on drug release in vitro. SAPs possess adequate properties for tableting, and maintain their high and fast swelling properties after compaction. The fast and extensive interactions of SAPs with aqueous medium are a major advantage over non-crosslinked high molecular weight viscosifying agents such as poly(ethylene oxide).

Gradient x Isocratic Elution CCC on the Isolation of Verbascoside and Other Phenylethanoids: Influence of the Complexity of the Matrix.

PubMed

Leitão, Gilda Guimarães; Pinto, Shaft Correa; de Oliveira, Danilo Ribeiro; Timoteo, Patrícia; Guimarães, Michelle Guedes; Cordova, Wilmer H Perera; Leitão, Suzana Guimarães

2015-11-01

Verbascoside is a phenylethanoid glycoside widely distributed in nature, especially among the order Lamiales, occurring in numerous plants that are constituents of folk medicine preparations. This natural compound, previously isolated by our group from the ethyl acetate extract of Lantana trifolia using the gradient approach in countercurrent chromatography, was now isolated from the butanol extract of the same plant and from Lippia alba f. intermedia (Verbenaceae) using countercurrent chromatography in either gradient or isocratic elution modes. The ethyl acetate extract of L. alba, rich in phenylethanoids and flavonoids, was fractionated using countercurrent chromatography in the step-gradient elution approach. The four-step solvent system was composed of n-hexane-ethyl acetate-n-butanol-water (4 : 10 : X : 10), where X = 1 (solvent system A), 3 (solvent system B), 5 (solvent system C), and 7 (solvent system D), and allowed for the isolation of verbascoside along with other phenylethanoids and flavonoids from both plants. Verbascoside and 2'-O-β-apiosylverbascoside were further isolated from the n-butanol extract of L. trifolia using the solvent system ethyl acetate-n-butanol-water 10 : 2 : 10 on an isocratic run. The difference in the complexity of the two plant extracts demanded different purification steps, which included a second high-speed countercurrent chromatography purification using the isocratic elution mode. Georg Thieme Verlag KG Stuttgart · New York.

Metabolite fingerprinting of Punica granatum L. (pomegranate) polyphenols by means of high-performance liquid chromatography with diode array and electrospray ionization-mass spectrometry detection.

PubMed

Brighenti, Virginia; Groothuis, Sebastiaan Frearick; Prencipe, Francesco Pio; Amir, Rachel; Benvenuti, Stefania; Pellati, Federica

2017-01-13

The present study was aimed at the development of a new analytical method for the comprehensive multi-component analysis of polyphenols in Punica granatum L. (pomegranate) juice and peel. While pomegranate juice was directly analysed after simple centrifugation, different extraction techniques, including maceration, heat reflux extraction, ultrasound-assisted extraction and microwave-assisted extraction, were compared in order to obtain a high yield of the target analytes from pomegranate peel. Dynamic maceration with a mixture of water and ethanol 80:20 (v/v) with 0.1% of hydrochloric acid as the extraction solvent provided the best result in terms of recovery of pomegranate secondary metabolites. The quali- and quantitative analysis of pomegranate polyphenols was performed by high-performance liquid chromatography with diode array and electrospray ionization-mass spectrometry detection. The application of fused-core column technology allowed us to obtain an improvement of the chromatographic performance in comparison with that of conventional particulate stationary phases, thus enabling a good separation of all constituents in a shorter time and with low solvent usage. The analytical method was completely validated to show compliance with the International Conference on Harmonization of Technical Requirements for the Registration of Pharmaceuticals for Human Use guidelines and successfully applied to the characterisation of commercial and experimental pomegranate samples, thus demonstrating its efficiency as a tool for the fingerprinting of this plant material. The quantitative data collected were submitted to principal component analysis, in order to highlight the possible presence of pomegranate samples with high content of secondary metabolites. From the statistical analysis, four experimental samples showed a notable content of bioactive compounds in the peels, while commercial ones still represent the best source of healthy juice. Copyright © 2016 Elsevier B.V. All rights reserved.

Single-step preparation of selected biological fluids for the high performance liquid chromatographic analysis of fat-soluble vitamins and antioxidants.

PubMed

Lazzarino, Giacomo; Longo, Salvatore; Amorini, Angela Maria; Di Pietro, Valentina; D'Urso, Serafina; Lazzarino, Giuseppe; Belli, Antonio; Tavazzi, Barbara

2017-12-08

Fat-soluble vitamins and antioxidants are of relevance in health and disease. Current methods to extract these compounds from biological fluids mainly need use of multi-steps and multi organic solvents. They are time-consuming and difficult to apply to treat simultaneously large sample number. We here describe a single-step, one solvent extraction of fat-soluble vitamins and antioxidants from biological fluids, and the chromatographic separation of all-trans-retinoic acid, 25-hydroxycholecalciferol, all-trans-retinol, astaxanthin, lutein, zeaxanthin, trans-β-apo-8'-carotenal, γ-tocopherol, β-cryptoxanthin, α-tocopherol, phylloquinone, lycopene, α-carotene, β-carotene and coenzyme Q 10 . Extraction is obtained by adding one volume of biological fluid to two acetonitrile volumes, vortexing for 60s and incubating for 60min at 37°C under agitation. HPLC separation occurs in 30min using Hypersil C18, 100×4.6mm, 5μm particle size column, gradient from 70% methanol+30% H 2 O to 100% acetonitrile, flow rate of 1.0ml/min and 37°C column temperature. Compounds are revealed using highly sensitive UV-VIS diode array detector. The HPLC method suitability was assessed in terms of sensitivity, reproducibility and recovery. Using the present extraction and chromatographic conditions we obtained values of the fat-soluble vitamins and antioxidants in serum from 50 healthy controls similar to those found in literature. Additionally, the profile of these compounds was also measured in seminal plasma from 20 healthy fertile donors. Results indicate that this simple, rapid and low cost sample processing is suitable to extract fat-soluble vitamins and antioxidants from biological fluids and can be applied in clinical and nutritional studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Acetic acid removal from corn stover hydrolysate using ethyl acetate and the impact on Saccharomyces cerevisiae bioethanol fermentation.

PubMed

Aghazadeh, Mahdieh; Ladisch, Michael R; Engelberth, Abigail S

2016-07-08

Acetic acid is introduced into cellulose conversion processes as a consequence of composition of lignocellulose feedstocks, causing significant inhibition of adapted, genetically modified and wild-type S. cerevisiae in bioethanol fermentation. While adaptation or modification of yeast may reduce inhibition, the most effective approach is to remove the acetic acid prior to fermentation. This work addresses liquid-liquid extraction of acetic acid from biomass hydrolysate through a pathway that mitigates acetic acid inhibition while avoiding the negative effects of the extractant, which itself may exhibit inhibition. Candidate solvents were selected using simulation results from Aspen Plus™, based on their ability to extract acetic acid which was confirmed by experimentation. All solvents showed varying degrees of toxicity toward yeast, but the relative volatility of ethyl acetate enabled its use as simple vacuum evaporation could reduce small concentrations of aqueous ethyl acetate to minimally inhibitory levels. The toxicity threshold of ethyl acetate, in the presence of acetic acid, was found to be 10 g L(-1) . The fermentation was enhanced by extracting 90% of the acetic acid using ethyl acetate, followed by vacuum evaporation to remove 88% removal of residual ethyl acetate along with 10% of the broth. NRRL Y-1546 yeast was used to demonstrate a 13% increase in concentration, 14% in ethanol specific production rate, and 11% ethanol yield. This study demonstrated that extraction of acetic acid with ethyl acetate followed by evaporative removal of ethyl acetate from the raffinate phase has potential to significantly enhance ethanol fermentation in a corn stover bioethanol facility. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:929-937, 2016. © 2016 American Institute of Chemical Engineers.

A novel reverse phase high-performance liquid chromatography method for standardization of Orthosiphon stamineus leaf extracts.

PubMed

Saidan, Noor Hafizoh; Aisha, Abdalrahim F A; Hamil, Mohd Shahrul Ridzuan; Majid, Amin Malik Shah Abdul; Ismail, Zhari

2015-01-01

Orthosiphon stamineus Benth. (Lamiaceae) is a traditional medicinal plant which has been used in treating various ailments such as kidney diseases, bladder inflammation, arthritis and diabetes. The leaves contain high concentration of phenolic compounds, thus, rosmarinic acid (RA), 3'-hydroxy-5, 6, 7, 4'-tetramethoxyflavone (TMF), sinensetin (SIN) and eupatorin (EUP) were chosen as a marker compounds for standardization of various O. stamineus leaf extracts. The aim was to develop and validate a new high-performance liquid chromatography (HPLC) method for quantification of 4 marker compounds (RA, TMF, SIN, EUP) in various O. stamineus leaf extracts. The method was developed and validated using RP-HPLC-diode-array detection at 320 nm for accuracy, precision and limits of detection and was applied for quantification of it markers in five different extracts prepared in solvents with increasing polarity, using a gradient mobile phase 0.1% formic acid: Acetonitrile at a flow rate of 1 ml/min on reverse phase acclaim polar advantage II C18 column (3 μm, 3 × 150 mm) with 18 min separation time. The developed method provided satisfactory precision, and the accuracy of this method was in the range of 90.2% to 105.5%. All of 4 compounds showed good linearity at R2 > 0.999. The developed method is a simple, cost effective with shorter run time (18 min) in comparison to previous methods (30 min) and utilization of environmental-friendly solvents system. Therefore, this method has the potential to replace currently used methods in the routine standardization work of O. stamineus extracts, raw materials and its commercial products.

A novel reverse phase high-performance liquid chromatography method for standardization of Orthosiphon stamineus leaf extracts

PubMed Central

Saidan, Noor Hafizoh; Aisha, Abdalrahim F.A.; Hamil, Mohd Shahrul Ridzuan; Majid, Amin Malik Shah Abdul; Ismail, Zhari

2015-01-01

Background: Orthosiphon stamineus Benth. (Lamiaceae) is a traditional medicinal plant which has been used in treating various ailments such as kidney diseases, bladder inflammation, arthritis and diabetes. The leaves contain high concentration of phenolic compounds, thus, rosmarinic acid (RA), 3’-hydroxy-5, 6, 7, 4’-tetramethoxyflavone (TMF), sinensetin (SIN) and eupatorin (EUP) were chosen as a marker compounds for standardization of various O. stamineus leaf extracts. Objective: The aim was to develop and validate a new high-performance liquid chromatography (HPLC) method for quantification of 4 marker compounds (RA, TMF, SIN, EUP) in various O. stamineus leaf extracts. Materials and Methods: The method was developed and validated using RP-HPLC-diode-array detection at 320 nm for accuracy, precision and limits of detection and was applied for quantification of it markers in five different extracts prepared in solvents with increasing polarity, using a gradient mobile phase 0.1% formic acid: Acetonitrile at a flow rate of 1 ml/min on reverse phase acclaim polar advantage II C18 column (3 μm, 3 × 150 mm) with 18 min separation time. Results: The developed method provided satisfactory precision, and the accuracy of this method was in the range of 90.2% to 105.5%. All of 4 compounds showed good linearity at R2 > 0.999. Conclusion: The developed method is a simple, cost effective with shorter run time (18 min) in comparison to previous methods (30 min) and utilization of environmental-friendly solvents system. Therefore, this method has the potential to replace currently used methods in the routine standardization work of O. stamineus extracts, raw materials and its commercial products. PMID:25598631

[Extraction of lambda-cyhalothrin from aqueous dioxan solutions].

PubMed

Shormanov, V K; Chigareva, E N; Belousova, O V

2011-01-01

The results of extraction of lambda-cigalotrin from dioxan aqueous solutions by hydrophobic organic solvents are presented. It is shown that the degree of extraction depends on the nature of the extractant, the water to dioxan ratio, and saturation of the water-dioxan layer with the electrolyte. The highest efficiency of lambda-cigalotrin extraction was achieved using chlorophorm as a solvent under desalination conditions. The extraction factor was calculated necessary to obtain the desired amount of lambda-cigalotrin from the water-dioxan solution (4:1) with the help of the extractants being used.

A simple graphene-based pipette tip solid-phase extraction of malondialdehyde from human plasma and its determination by spectrofluorometry.

PubMed

Kaykhaii, Massoud; Yahyavi, Hossain; Hashemi, Mohammad; Khoshroo, Mohammad Reza

2016-07-01

Determination of malondialdehyde (MDA) in human blood plasma is important because of its role as a biomarker of lipid peroxidation in biological and medical sciences. In this work, a miniaturized graphene-based pipette tip solid-phase extraction technique was developed for very efficient extraction of MDA as its dithiobarbituric acid (TBA) adduct from human plasma. Two milligrams of graphene as sorbent were placed into a pipette tip and MDA-TBA compound was extracted and preconcentrated by it, after 4 repeated aspirating/dispensing cycles, then the column was eluted with 80 μL of dimethyl sulfoxide by 4 repeated aspirating/dispensing cycles and elusion was measured spectrofluorimetrically. Various effective parameters such as type and volume of eluent solvent, temperature, sample volume, number of cycles of extraction and desorption, derivatization reaction time, and pH of the sample solution were investigated and optimized. Under optimum conditions, a linear calibration curve was obtained in the range of 0.5-90 μg L(-1) (r (2) = 0.991) with a detection limit of 0.3 μg L(-1). The relative standard deviations for 8 replicate measurements of 10 and 40 μg L(-1) of MDA were found to be 4.51 and 3.78 % respectively. The developed protocol was successfully applied to the determination of MDA in a human blood plasma sample. Graphical Abstract A simple graphene-based pipette tip solid-phase extraction of malondialdehyde from human plasma and its determination by spectrofluorometry.