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

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

NASA Astrophysics Data System (ADS)

Nishimura, Mitsugu; Baker, Earl W.

1987-06-01

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

Bioavailability of butachlor and myclobutanil residues in soil to earthworms.

PubMed

Yu, Y L; Wu, X M; Li, S N; Fang, H; Tan, Y J; Yu, J Q

2005-05-01

To establish chemical extraction procedures for predicting bioavailability of butachlor and myclobutanil in soil, several solvent systems, including methanol, methanol-water (9:1), methanol-water (1:1), acetone-water (5:3), petroleum ether and water, were assessed for their feasibility in determining extractability of the target compounds from soil samples. Experimental data showed that the extractability of butachlor and myclobutanil by the solvents was well linearly correlated with their bioavailability to Eisenia foetida and Allolobophora caliginosa, indicating that these extraction procedures may be efficient for predicting bioavailability of the two pesticides. The concentrations of the pesticides accumulated in E. foetida and A. caliginosa varied with species, suggesting that the availability of the soil-sequestered pesticide is a species-dependent process.

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.

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.

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.

Procedure for the determination of retinol and alpha-tocopherol in poultry tissues using capillary gas chromatography with solvent venting injection.

PubMed

Maraschiello, C; García Regueiro, J A

1998-08-28

A procedure designed for the determination of retinol (vitamin A) and alpha-tocopherol (vitamin E) in poultry tissues has been developed. The procedure involves lipid extraction, saponification, solid-phase clean-up and capillary gas chromatography (cGC). Retinol and alpha-tocopherol were determined separately by cGC-flame ionisation detection using a fused-silica open tubular capillary column, 30 m x 0.25 mm I.D. coated with 5% phenylmethylsilicone and with a film thickness of 0.25 micron. Solvent extraction followed by saponification were sufficient to provide a purified extract which was directly analyzed for retinol by cGC in the solvent venting mode. However, in order to accurately determine alpha-tocopherol by cGC, further purification of the extract by solid-phase extraction was necessary. A silica SPE column was used to remove interfering cholesterol from the extract. alpha-Tocopherol was analyzed in its derivatized form. Absolute and relative recoveries for both vitamins from spiked samples were evaluated. Absolute and relative recoveries ranging from 80 to 95% were obtained for both compounds. 5 alpha-Cholestane and alpha-tocopheryl acetate were used as internal standards. Poultry muscle meat and liver tissue were analyzed for their retinol and alpha-tocopherol content and the peaks detected by cGC were confirmed by cGC-mass spectrometry.

Ultrasound extraction and thin layer chromatography-flame ionization detection analysis of the lipid fraction in marine mucilage samples.

PubMed

Mecozzi, M; Amici, M; Romanelli, G; Pietrantonio, E; Deluca, A

2002-07-19

This paper reports an analytical procedure based on ultrasound to extract lipids in marine mucilage samples. The experimental conditions of the ultrasound procedure (solvent and time) were identified by a FT-IR study performed on different standard samples of lipids and of a standard humic sample, before and after the sonication treatment. This study showed that diethyl ether was a more suitable solvent than methanol for the ultrasonic extraction of lipids from environmental samples because it allowed to minimize the possible oxidative modifications of lipids due to the acoustic cavitation phenomena. The optimized conditions were applied to the extraction of total lipid amount in marine mucilage samples and TLC-flame ionization detection analysis was used to identify the relevant lipid sub-fractions present in samples.

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.

Multivessel supercritical fluid extraction of food items in Total Diet Study.

PubMed

Hopper, M L; King, J W; Johnson, J H; Serino, A A; Butler, R J

1995-01-01

An off-line, large capacity, multivessel supercritical fluid extractor (SFE) was designed and constructed for extraction of large samples. The extractor can simultaneously process 1-6 samples (15-25 g) by using supercritical carbon dioxide (SC-CO2), which is relatively nontoxic and nonflammable, as the solvent extraction medium. Lipid recoveries for the SFE system were comparable to those obtained by blending or Soxhlet extraction procedures. Extractions at 10,000 psi, 80 degrees C, expanded gaseous CO2 flow rates of 4-5 L/min (35 degrees C), and 1-3 h extraction times gave reproducible lipid recoveries for pork sausage (relative standard deviation [RSD], 1.32%), corn chips (RSD, 0.46%), cheddar cheese (RSD, 1.14%), and peanut butter (RSD, 0.44%). In addition, this SFE system gave reproducible recoveries (> 93%) for butter fortified with cis-chlordane and malathion at the 100 ppm and 0.1 ppm levels. Six portions each of cheddar cheese, saltine crackers, sandwich cookies, and ground hamburger also were simultaneously extracted with SC-CO2 and analyzed for incurred pesticide residues. Results obtained with this SFE system were reproducible and comparable with results from organic-solvent extraction procedures currently used in the Total Diet Study; therefore, use and disposal of large quantities of organic solvents can be eliminated.

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

PubMed

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

2013-04-01

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

Combination pulsed electric field with ethanol solvent for Nannochloropsis sp. extraction

NASA Astrophysics Data System (ADS)

Nafis, Ghazy Ammar; Mumpuni, Perwitasari Yekti; Indarto, Budiman, Arief

2015-12-01

Nowadays, energy is one of human basic needs. As the human population increased, energy consumption also increased. This condition causes energy depletion. In case of the situation, alternative energy is needed to replace existing energy. Microalgae is chosen to become one of renewable energy resource, especially biodiesel, because it contains high amount of lipid instead of other feedstock which usually used. Fortunately, Indonesia has large area of water and high intensity of sunlight so microalgae cultivation becomes easier. Nannochloropsis sp., one of microalgae species, becomes the main focus because of its high lipid content. Many ways to break the cell wall of microalgae so the lipid content inside the microalgae will be released, for example conventional extraction, ultrasonic wave extraction, pressing, and electrical method. The most effective way for extraction is electrical method such as pulsed electric field method (PEF). The principal work of this method is by draining the electrical current into parallel plate. Parallel plate will generate the electrical field to break microalgae cell wall and the lipid will be released. The aim of this work is to evaluate two-stage procedure for extraction of useful components from microalgae Nannochloropsis sp. The first stage of this procedure includes pre-treatment of microalgae by ethanol solvent extraction and the second stage applies the PEF extraction using a binary mixture of water and ethanol solvent. Ethanol is chosen as solvent because it's safer to be used and easier to be handled than other solvent. Some variables that used to study the most effective operation conditions are frequency and duty cycle for microalgae. The optimum condition based on this research are at frequency 1 Hz and duty cycle 13%.

Self-immobilization of poly(methyloctylsiloxane) on high-performance liquid chromatographic silica.

PubMed

Collins, Kenneth E; Bottoli, Carla B G; Vigna, Camila R M; Bachmann, Stefan; Albert, Klaus; Collins, Carol H

2004-03-12

Poly(methyloctylsiloxane) (PMOS) was deposited on HPLC silica by a solvent evaporation procedure and this material was then extracted, using a good solvent for the PMOS, after different time periods, to remove unretained liquid polymer. Solvent extraction data reveal changes which occur at ambient temperature as a function of the time interval between particle loading and extraction. The quantity of PMOS remaining on the silica after extraction, as determined by elemental analysis for carbon, is attributed to strongly adsorbed polymer. This phenomenon is termed self-immobilization. Solid-state 29Si NMR spectra indicate the formation of a silicon species with a different chemical shift than the original PMOS. These new signals are attributed to a combination of different adsorbed and chemically bonded groups.

Preparation, isolation, and characterization of cutin monomers and oligomers from tomato peels.

PubMed

Osman, S F; Irwin, P; Fett, W F; O'Connor, J V; Parris, N

1999-02-01

Cutin in tomato peels was depolymerized in methanolic base to yield cutin monomers or a mixture of cutin oligomers. These products were isolated by typical solvent extraction methods or by precipitation, and the isolates were characterized by chromatographic and spectroscopic analyses. It was determined that the compositions of the isolates from both isolation procedures were similar, although solvent extraction gave higher yields. However, the precipitation method, which is easy to carry out and avoids the use of undesirable organic solvents, may be preferable in commercial processes for recovering these compounds.

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

PubMed

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

2014-02-03

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

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

PubMed Central

2014-01-01

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

Multiple functional ionic liquids based dispersive liquid-liquid microextraction combined with high performance chromatography for the determination of phenolic compounds in water samples.

PubMed

Sun, Jian-Nan; Chen, Juan; Shi, Yan-Ping

2014-07-01

A new mode of ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) is developed. In this work, [C6MIm][PF6] was chosen as the extraction solvent, and two kinds of hydrophilic ionic liquids, [EMIm][BF4] and [BSO3HMIm][OTf], functioned as the dispersive solvent. So in the whole extraction procedure, no organic solvent was used. With the aid of SO3H group, the acidic compound was extracted from the sample solution without pH adjustment. Two phenolic compounds, namely, 2-naphthol and 4-nitrophenol were chosen as the target analytes. Important parameters affecting the extraction efficiency, such as the type of hydrophilic ionic liquids, the volume ratio of [EMIm][BF4] to [BSO3HMIm][OTf], type and volume of extraction solvent, pH value of sample solution, sonication time, extraction time and centrifugation time were investigated and optimized. Under the optimized extraction conditions, the method exhibited good sensitivity with the limits of detection (LODs) at 5.5 μg L(-1)and 10.0 μg L(-1) for 4-nitrophenol and 2-naphthol, respectively. Good linearity over the concentration ranges of 24-384 μg L(-1) for 4-nitrophenol and 28-336 μg L(-1) for 2-naphthol was obtained with correlation coefficients of 0.9998 and 0.9961, respectively. The proposed method can directly extract acidic compound from environmental sample or even more complex sample matrix without any pH adjustment procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Separation and characterization of antioxidants from Spirulina platensis microalga combining pressurized liquid extraction, TLC, and HPLC-DAD.

PubMed

Jaime, Laura; Mendiola, José A; Herrero, Miguel; Soler-Rivas, Cristina; Santoyo, Susana; Señorans, F Javier; Cifuentes, Alejandro; Ibáñez, Elena

2005-11-01

A new procedure has been developed to separate and characterize antioxidant compounds from Spirulina platensis microalga based on the combination of pressurized liquid extraction (PLE) and different chromatographic procedures, such as TLC, at preparative scale, and HPLC with a diode array detector (DAD). Different solvents were tested for PLE extraction of antioxidants from S. platensis microalga. An optimized PLE process using ethanol (generally recognized as safe, GRAS) as extraction solvent has been obtained that provides natural extracts with high yields and good antioxidant properties. TLC analysis of this ethanolic extract obtained at 115 degrees C for 15 min was carried out and the silica layer was stained with a DPPH (diphenyl-pycril-hydrazyl) radical solution to determine the antioxidant activity of different chromatographic bands. Next, these colored bands were collected for their subsequent analysis by HPLC-DAD, revealing that the compounds with the most important antioxidant activity present in Spirulina extracts were carotenoids, as well as phenolic compounds and degradation products of chlorophylls.

SW-846 Test Method 3200: Mercury Species Fractionation and Quantification by Microwave Assisted Extraction, Selective Solvent Extraction and/or Solid Phase Extraction

EPA Pesticide Factsheets

a sequential extraction and separation procedure that maybe used in conjunction with a determinative method to differentiate mercury species that arepresent in soils and sediments. provides information on both total mercury andvarious mercury species.

QUANTITATIVE RADIO-CHEMICAL ANALYSIS-SOLVENT EXTRACTION OF MOLYBDENUM-99

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

Wish, L.

1961-09-12

A method was developed for the rapid quantitative separation of Mo/sup 99/ from fission product mixtures. It is based on the extraction of Mo into a solution of alpha -benzoin oxime in chloroform. The main contaminants are Zr, Nb, and 1. The first two are eliminated by couple with fluoride and the third by volatilization or solvent extraction. About 5% of the Te/sup 99/ daughter is extracted with its parent, and it is necessary to wait 48 hrs for equilibrium of fission product mixtures by this method and a standard radiochemical gravimetric procedure showed agreement within 1 to 2%. (auth)

Solvent effects on quantitative analysis of brominated flame retardants with Soxhlet extraction.

PubMed

Zhong, Yin; Li, Dan; Zhu, Xifen; Huang, Weilin; Peng, Ping'an

2017-05-18

Reliable quantifications of brominated flame retardants (BFRs) not only ensure compliance with laws and regulations on the use of BFRs in commercial products, but also is key for accurate risk assessments of BFRs. Acetone is a common solvent widely used in the analytical procedure of BFRs, but our recent study found that acetone can react with some BFRs. It is highly likely that such reactions can negatively affect the quantifications of BFRs in environmental samples. In this study, the effects of acetone on the extraction yields of three representative BFRs [i.e., decabrominated diphenyl ether (decaBDE), hexabromocyclododecane (HBCD) and tetrabromobisphenol A (TBBPA)] were evaluated in the Soxhlet extraction (SE) system. The results showed that acetone-based SE procedure had no measureable effect for the recovery efficiencies of decaBDE but could substantially lower the extraction yields for both TBBPA and HBCD. After 24 h of extraction, the recovery efficiencies of TBBPA and HBCD by SE were 93 and 78% with acetone, 47 and 70% with 3:1 acetone:n-hexane, and 82 and 94% with 1:1 acetone:n-hexane, respectively. After 72 h of extraction, the extraction efficiencies of TBBPA and HBCD decreased to 68 and 55% with acetone, 0 and 5% with 3:1 acetone/n-hexane mixtures, and 0 and 13% with 1:1 acetone/n-hexane mixtures, respectively. The study suggested that the use of acetone alone or acetone-based mixtures should be restricted in the quantitative analysis of HBCD and TBBPA. We further evaluated nine alternative solvents for the extraction of the three BFRs. The result showed that diethyl ether might be reactive with HBCD and may not be considered as the alternative to acetone used solvents for the extraction of HBCD.

Ionic liquid based dispersive liquid-liquid microextraction for the extraction of pesticides from bananas.

PubMed

Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Asensio-Ramos, María; Rodríguez-Delgado, Miguel Angel

2009-10-23

This paper describes a dispersive liquid-liquid microextraction (DLLME) procedure using room temperature ionic liquids (RTILs) coupled to high-performance liquid chromatography with diode array detection capable of quantifying trace amounts of eight pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox and fenazaquin) in bananas. Fruit samples were first homogenized and extracted (1g) with acetonitrile and after suitable evaporation and reconstitution of the extract in 10 mL of water, a DLLME procedure using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) as extraction solvent was used. Experimental conditions affecting the DLLME procedure (sample pH, sodium chloride percentage, ionic liquid amount and volume of disperser solvent) were optimized by means of an experimental design. In order to determine the presence of a matrix effect, calibration curves for standards and fortified banana extracts (matrix matched calibration) were studied. Mean recovery values of the extraction of the pesticides from banana samples were in the range of 69-97% (except for thiophanate-methyl and carbofuran, which were 53-63%) with a relative standard deviation lower than 8.7% in all cases. Limits of detection achieved (0.320-4.66 microg/kg) were below the harmonized maximum residue limits established by the European Union (EU). The proposed method, was also applied to the analysis of this group of pesticides in nine banana samples taken from the local markets of the Canary Islands (Spain). To the best of our knowledge, this is the first application of RTILs as extraction solvents for DLLME of pesticides from samples different than water.

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.

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.

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

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2008-02-01

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

"Solvent-free" ultrasound-assisted extraction of lipids from fresh microalgae cells: a green, clean and scalable process.

PubMed

Adam, Fanny; Abert-Vian, Maryline; Peltier, Gilles; Chemat, Farid

2012-06-01

In order to comply with criteria of green chemistry concepts and sustainability, a new procedure has been performed for solvent-free ultrasound-assisted extraction (UAE) to extract lipids from fresh Nannochloropsis oculata biomass. Through response surface methodology (RSM) parameters affecting the oil recovery were optimized. Optimum conditions for oil extraction were estimated as follows: (i) 1000 W ultrasonic power, (ii) 30 min extraction time and (iii) biomass dry weight content at 5%. Yields were calculated by the total fatty acids methyl esters amounts analyzed by GC-FID-MS. The maximum oil recovery was around 0.21%. This value was compared with the one obtained with the conventional extraction method (Bligh and Dyer). Furthermore, effect of temperature on the yield was also investigated. The overall results show an innovative and effective extraction method adapted for microalgae oil recovery, without using solvent and with an enable scaling up. Copyright © 2012 Elsevier Ltd. All rights reserved.

Extracting metalworking fluid aerosol samples in cassettes by provisional ASTM and NIOSH methods.

PubMed

Harper, Martin

2002-01-01

Recent provisional methods for the determination of metalworking fluid aerosol in workplace air involve a solvent extraction procedure to separate the nonvolatile fraction of the fluid from insoluble material such as metal turnings and dirt. The procedure calls for preweighing a filter (W1) and assembling it into a cassette and taking a sample. In the laboratory the filter is removed from the cassette, desiccated to remove any collected water or other volatile substances, and weighed again (W2). The filter is then extracted in an organic solvent blend, allowed to dry, and weighed a final time (W3). The total weight collected by the filter is given by (W2-W1), and the weight of (nonvolatile) metalworking fluid collected is given by (W2-W3). The extraction step can take place within a cassette housing if it is relatively inert to the solvent blend used. The extraction of four metalworking fluids (straight oil, soluble oil, synthetic and semisynthetic) within disposable polypropylene cassettes was investigated using the same protocol used to evaluate the original method. For all fluids the extraction efficiency was greater than 95% with a precision better than 5%. The mean blank contribution to the extraction step was 16 micrograms. Blanks were also evaluated after storage, and after transport and storage. A small additional blank contribution could be removed by desiccation. The limits of detection and quantitation of the extraction step were calculated to be 28 and 94 micrograms, respectively.

Total milk fat extraction and quantification of polar and neutral lipids of cow, goat, and ewe milk by using a pressurized liquid system and chromatographic techniques.

PubMed

Castro-Gómez, M P; Rodriguez-Alcalá, L M; Calvo, M V; Romero, J; Mendiola, J A; Ibañez, E; Fontecha, J

2014-11-01

Although milk polar lipids such as phospholipids and sphingolipids located in the milk fat globule membrane constitute 0.1 to 1% of the total milk fat, those lipid fractions are gaining increasing interest because of their potential beneficial effects on human health and technological properties. In this context, the accurate quantification of the milk polar lipids is crucial for comparison of different milk species, products, or dairy treatments. Although the official International Organization for Standardization-International Dairy Federation method for milk lipid extraction gives satisfactory results for neutral lipids, it has important disadvantages in terms of polar lipid losses. Other methods using mixtures of solvents such as chloroform:methanol are highly efficient for extracting polar lipids but are also associated with low sample throughput, long time, and large solvent consumption. As an alternative, we have optimized the milk fat extraction yield by using a pressurized liquid extraction (PLE) method at different temperatures and times in comparison with those traditional lipid extraction procedures using 2:1 chloroform:methanol as a mixture of solvents. Comparison of classical extraction methods with the developed PLE procedure were carried out using raw whole milk from different species (cows, ewes, and goats) and considering fat yield, fatty acid methyl ester composition, triacylglyceride species, cholesterol content, and lipid class compositions, with special attention to polar lipids such as phospholipids and sphingolipids. The developed PLE procedure was validated for milk fat extraction and the results show that this method performs a complete or close to complete extraction of all lipid classes and in less time than the official and Folch methods. In conclusion, the PLE method optimized in this study could be an alternative to carry out milk fat extraction as a routine method. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Comparison of extraction procedures on the immunocontraceptive activity of neem seed extracts.

PubMed

Garg, S; Talwar, G P; Upadhyay, S N

1994-10-01

Azadirachta indica (Neem) seed extracts are known to activate the local cell-mediated immune reactions after a single intrauterine administration, leading to a long term reversible block of fertility. In order to identify and characterize the active fraction responsible for this activity, neem seeds were extracted by both mechanical expression and solvent extraction using a range of polar to non-polar solvents which yielded 3 broad fractions. The mechanically expressed oil was fractionated using different approaches and studied for antifertility activity. The hexane extract and a corresponding column fraction showed potent and reproducible antifertility activity. Other fractions were less stable with regard to reproducibility of effects and composition. It is our conclusion that for subsequent fractionation to reach the last active fraction, the hexane extract is the most useful starting material.

Optimizing conditions for the extraction of pigments in cochineals (Dactylopius coccus Costa) using response surface methodology.

PubMed

González, Mónica; Méndez, Jesús; Carnero, Aurelio; Lobo, M Gloria; Afonso, Ana

2002-11-20

A simple method was developed for the extraction and determination of color pigments in cochineals (Dactylopius coccus Costa). The procedure was based on the solvent extraction of pigments in insect samples using methanol:water (65:35, v:v) as extractant. Two-level factorial design was used in order to optimize the solvent extraction parameters: temperature, time, methanol concentration in the extractant mixture, and the number of extractions. The results suggest that the number of extractions is statistically the most significant factor. The separation and determination of the pigments was carried out by high-performance liquid chromatography with UV-visible detection. Because the absorption spectra of different pigments are different in the visible region, it is convenient to use a diode array detector to obtain chromatographic profiles that allow for the characterization of the extracted pigments.

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.

Combination of QuEChERS and DLLME for GC-MS determination of pesticide residues in orange samples.

PubMed

Andraščíková, Mária; Hrouzková, Svetlana; Cunha, Sara C

2013-01-01

A new method combining QuEChERS (quick, easy, cheap, effective, rugged and safe) and DLLME (dispersive liquid-liquid microextraction) followed by gas chromatography-mass spectrometry with selected ion monitoring (SIM) was developed for the simultaneous determination of 19 pesticides from nine chemical groups exhibiting or suspected to exhibit endocrine-disrupting properties in orange samples. Acetonitrile extract obtained from QuEChERS extraction was used for DLLME as dispersive solvent and carbon tetrachloride as extractive solvent to increase the enrichment factor of the extraction procedure. The effect of several extraction parameters, such as volume extract achieved by the QuEChERS method and subsequently used for DLLME, selection of extractive solvent and its volume, was tested. Under optimum conditions, good linearity, satisfactory recoveries and repeatability were obtained. Limits of quantification (LOQs) achieved (ranging from 0.02 to 47 ng/g) were below the maximum residue limits established by the European Union. The proposed method was applied to the monitoring of pesticide residue levels in oranges commercialised in Portugal.

Development of biodegradable drug delivery system to treat addiction.

PubMed

Mandal, T K

1999-06-01

Opiate addiction is a serious problem that has now spread worldwide to all levels of society. Buprenorphine has been used for several years for the treatment of opiate addiction. The objective of this project was to develop sustained-release biodegradable microcapsules for the parenteral delivery of buprenorphine. Biodegradable microcapsules of buprenorphine/poly(lactide-co-glycolide) were prepared using two main procedures based on an in-water drying process in a complex emulsion system. These procedures differ in the way the organic solvent was eliminated: evaporation or extraction. The effect of drug loading and the effect of partial saturation of the aqueous phase with the core material during the in-water solvent evaporation were also studied. The efficiency of encapsulation increased from 11% to 34% when the drug loading was decreased from 20% to 5%. There was no significant change in the efficiency of encapsulation when the aqueous phase was partially saturated with buprenorphine. In changing the solvent removal process from evaporation to extraction, no significant change in the efficiency of encapsulation was observed. The microcapsules prepared by the solvent evaporation were smooth and spherical. However, the microcapsules prepared by the extraction of the organic solvent lost their surface smoothness and became slightly irregular and porous compared with the other batches. The average particle size of the microcapsules was between 14 and 49 microns. The cumulative drug release was between 2% and 4% within the first 24 hr. A sustained drug release continued over 45 days.

Physico-chemical separation process of nanoparticles in cosmetic formulations

NASA Astrophysics Data System (ADS)

Retamal Marín, R. R.; Babick, F.; Stintz, M.

2017-06-01

Understanding the world of nanoparticles, especially their interactions with the environment, begins with their correct detection and successive quantification. To achieve this purpose, one needs to perform correctly developed standard operating procedures (SOPs). Furthermore, the study of nanoparticles frequently requires their characterisation in complex media (e.g. in cosmetic formulations). In this study, a set of sample preparation procedures for the detection and extraction of NMs in emulsion-based formulations is proposed and their performance for model and real-life products is discussed. A separation or extraction of lipid phases is achieved by means of organic solvents. The polarity of the lipid phases is decisive for selecting an optimum solvent. The use of the Hansen Solubility Parameters (HSP) may clearly support this decision.

THE ANALYSIS OF URANIUM-ZIRCONIUM ALLOYS

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

Milner, G.W.C.; Skewies, A.F.

1953-03-01

A satisfactory procedure is described for the analysis of uranium-zirconium alloys containing up to 25% zirconium. It is based on the separation of the zirconium from the uranium by dissolving the cupferron complex of the former element into chloroform. After the evaporation of the solvent from the combined organic extracts, the residue is ignited to zirconium oxide. The latter is then re-dissolved and zirconium is separated from other elements co-extracted in the solvent extraction procedure by precipitation with mandelic acid. The zirconium mandelate is finally ignited to oxide at 960 deg C. The uranium is separated from the aqueous solutionmore » remaining from the cupferron extraction by precipitating with tannin at a pH of 8; the precipitate being removed by filtration and then ignited a t 800 deg C. The residue is dissolved in nitric acid and the uranium is finally determined by precipitating as ammonium diuranate and then igniting to U{sub 3}O{sub 8}. (auth)« less

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.

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.

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

PubMed

Liu, Zaizhi; Gu, Huiyan; Yang, Lei

2015-10-23

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

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR ANALYSIS OF VOLATILE ORGANIC COMPOUNDS COLLECTED WITH A PASSIVE SAMPLER (BCO-L-17.1)

EPA Science Inventory

The purpose of this SOP is to describe the methodology used for the analysis of the 3M OVM 3500 Organic Vapor Monitors for volatile organic compounds (VOCs), using solvent extraction and standard gas chromatography/mass spectrometry (GC/MS) analysis procedures. This procedure was...

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.

COMPARISON OF TWO DIFFERENT SOLID PHASE EXTRACTION/LARGE VOLUME INJECTION PROCEDURES FOR METHOD 8270

EPA Science Inventory

Two solid phase (SPE) and one traditional continuous liquid-liquid extraction method are compared for analysis of Method 8270 SVOCs. Productivity parameters include data quality, sample volume, analysis time and solvent waste.

One SPE system, unique in the U.S., uses aut...

EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High Performance Liquid Chromatography-Thermospray-Mass Spectrometry (HPLC-TS-MS) or Ultraviolet (UV) Detection

EPA Pesticide Factsheets

Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.

Prevalence of pesticides in postconsumer agrochemical polymeric packaging.

PubMed

Eras, J; Costa, J; Vilaró, F; Pelacho, A M; Canela-Garayoa, R; Martin-Closas, L

2017-02-15

Pesticide remains contained in agrochemical packaging waste are a source of uncontrolled risk for human health; they are also a quality feedstock for the plastic recycling industry. Many governments have recently started to establish laws and regulations to develop systems for recovering and recycling the polymeric packages used for pesticides. There is also a demand in having a procedure to control the suitability of the pesticide packages to be reused. We have developed a two-step operation process to assess the pesticide residues in agricultural containers made of a variety of polymeric matrices. The procedure is based on an extraction with a solvent mixture followed by UPLC-MS/MS determination. Solvents for neutral pesticides were selected considering the Hildebrand solubility (δ) of solvents and polymers together with those estimated for the pesticides. The proposed technique is effective in recovering imbibed pesticides in polymeric matrices. Also, a simplified extraction procedure has been tested to become a routine method for these wastes. We have found that in many cases a significant amount of pesticides remain into the polymeric matrix, even after a standardized cleaning; the impact of releasing these hazardous compounds into the environment is to be of further consideration. Copyright © 2016 Elsevier B.V. All rights reserved.

Occupational exposure to complex mixtures of volatile organic compounds in ambient air: desorption from activated charcoal using accelerated solvent extraction can replace carbon disulfide?

PubMed

Fabrizi, Giovanni; Fioretti, Marzia; Rocca, Lucia Mainero

2013-01-01

A desorption study of 57 volatile organic compounds (VOCs) has been conducted by use of accelerated solvent extraction (ASE) and gas chromatography-mass spectrometry. Different solvents were tested to extract activated charcoal tubes with the objective of replacing carbon disulfide, used in official methods, because of its highly toxic health and environmental effects. Extraction conditions, for example temperature and number of cycles, were investigated and optimized. The definitive extraction procedure selected was use of acetone at 150 °C and two consecutive extraction cycles at a pressure of 1,500 psi. Considering a sample volume of 0.005 Nm(3), corresponding to a sampling time of 8 h at a flow rate of 0.01 L min(-1), the method was validated over the concentration range 65-26,300 μg Nm(-3). The lowest limit of quantification was 6 μg Nm(-3), and recovery for the 93 % of analytes ranged from 65 to 102 %. For most of the compounds, relative standard deviations were less than 15 % for inter and intra-day precision. Uncertainty of measurement was also determined: the relative expanded uncertainty was always below 29.6 %, except for dichlorodifluoromethane. This work shows that use of friendlier solvent, for example acetone, coupled with use of ASE, can replace use of CS(2) for chemical removal of VOCs from activated charcoal. ASE has several advantages over traditional solvent-extraction methods, including shorter extraction time, minimum sample manipulation, high reproducibility, and less extraction discrimination. No loss of sensitivity occurs and there is also a salutary effect on bench workers' health and on the smell of laboratory air.

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

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

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

1986-01-01

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

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

PubMed

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

2017-02-01

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

OPTIMIZED DETERMINATION OF TRACE JET FUEL VOLATILE ORGANIC COMPOUNDS IN HUMAN BLOOD USING IN-FIELD LIQUID-LIQUID EXTRACTION WITH SUBSEQUENT LABORATORY GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS AND ON-COLUMN LARGE VOLUME INJECTION

EPA Science Inventory

A practical and sensitive method to assess volatile organic compounds (VOCs) from JP-8 jet fuel in human whole blood was developed by modifying previously established liquid-liquid extraction procedures, optimizing extraction times, solvent volume, specific sample processing te...

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

PubMed

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

2015-04-01

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

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

PubMed

Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

2000-02-11

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

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.

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry.

PubMed

Janiszewski, J; Schneider, P; Hoffmaster, K; Swyden, M; Wells, D; Fouda, H

1997-01-01

The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts.

Evaluation of radiochemical neutron activation analysis methods for determination of arsenic in biological materials.

PubMed

Paul, Rick L

2011-01-01

Radiochemical neutron activation analysis (RNAA) with retention on hydrated manganese dioxide (HMD) has played a key role in the certification of As in biological materials at NIST. Although this method provides very high and reproducible yields and detection limits at low microgram/kilogram levels, counting geometry uncertainties may arise from unequal distribution of As in the HMD, and arsenic detection limits may not be optimal due to significant retention of other elements. An alternate RNAA procedure with separation of arsenic by solvent extraction has been investigated. After digestion of samples in nitric and perchloric acids, As(III) is extracted from 2 M sulfuric acid solution into a solution of zinc diethyldithiocarbamate in chloroform. Counting of (76)As allows quantitation of arsenic. Addition of an (77)As tracer solution prior to dissolution allows correction for chemical yield and counting geometries, further improving reproducibility. The HMD and solvent extraction procedures for arsenic were compared through analysis of SRMs 1577c (bovine liver), 1547 (peach leaves), and 1575a (pine needles). Both methods gave As results in agreement with certified values with comparable reproducibility. However, the solvent extraction method yields a factor of 3 improvement in detection limits and is less time-consuming than the HMD method. The new method shows great promise for use in As certification in reference materials.

A dispersive liquid-liquid micellar microextraction for the determination of pharmaceutical compounds in wastewaters using ultra-high-performace liquid chromatography with DAD detection.

PubMed

Montesdeoca-Esponda, Sarah; Mahugo-Santana, Cristina; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

2015-03-01

A dispersive liquid-liquid micellar microextraction (DLLMME) method coupled with ultra-high-performance liquid chromatography (UHPLC) using Diode Array Detector (DAD) detector was developed for the analysis of five pharmaceutical compounds of different nature in wastewaters. A micellar solution of a surfactant, polidocanol, as extraction solvent (100 μL) and chloroform as dispersive solvent (200 μL) were used to extract and preconcentrate the target analytes. Samples were heated above critical temperature and the cloudy solution was centrifuged. After removing the chloroform, the reduced volume of surfactant was then injected in the UHPLC system. In order to obtain high extraction efficiency, the parameters affecting the liquid-phase microextraction, such as time and temperature extraction, ionic strength and surfactant and organic solvent volume, were optimized using an experimental design. Under the optimized conditions, this procedure allows enrichment factors of up to 47-fold. The detection limit of the method ranged from 0.1 to 2.0 µg/L for the different pharmaceuticals. Relative standard deviations were <26% for all compounds. The procedure was applied to samples from final effluent collected from wastewater treatment plants in Las Palmas de Gran Canaria (Spain), and two compounds were measured at 67 and 113 µg/L in one of them. Copyright © 2014 John Wiley & Sons, Ltd.

Accelerated solvent extraction combined with solid phase extraction for the determination of organophosphate esters from sewage sludge compost by UHPLC-MS/MS.

PubMed

Pang, Long; Yang, Peijie; Ge, Liming; Du, Jingjing; Zhang, Hongzhong

2017-02-01

Organophosphate esters (OPEs), widely used as flame retardants and plasticizers, are regarded as emerging pollutants. OPEs are prone to concentrate into residual activated sludge, which might cause secondary pollution if not suitably treated. Composting is an economical and effective approach to make sewage sludge stable and harmless. Therefore, it is essential to develop a novel method for analyzing OPEs in sewage sludge compost samples. However, in the composting process, large amounts of amendments are doped into the sludge to adjust the carbon-nitrogen ratio. Amendment has a strong capacity for adsorption and thus induces a decrease of extraction efficiency. This study developed a novel procedure for determining OPEs in compost samples. Accelerated solvent extraction (ASE) and solid phase extraction (SPE) were used for extracting and concentrating the OPEs from sewage sludge compost samples, and then analyzed by UHPLC-MS/MS. Some parameters were optimized in this study, mainly including the extraction solvent type, extraction temperature, static extraction time, extraction cycles, and flush volume. Under the optimal conditions, the proposed method showed good linearity between 0.50 and 100 μg kg -1 with regression coefficients in the range of 0.9984-0.9998. Detection limits were in the range of 0.02-3 μg kg -1 with standard deviations ranging from 2 to 6%. Acceptable recoveries between 56 and 119% for samples spiked at different concentration levels were achieved. In contrast, the recoveries merely ranged from 24 to 58% by using ultrasonic-assisted extraction. Graphical abstract A comparison of recoveries between ultrasonic-assisted extraction (UAS) and accelerated solvent extraction (ASE) for organophosphate esters from sewage sludge compost samples.

Saffron Samples of Different Origin: An NMR Study of Microwave-Assisted Extracts

PubMed Central

Sobolev, Anatoly P.; Carradori, Simone; Capitani, Donatella; Vista, Silvia; Trella, Agata; Marini, Federico; Mannina, Luisa

2014-01-01

An NMR analytical protocol is proposed to characterize saffron samples of different geographical origin (Greece, Spain, Hungary, Turkey and Italy). A microwave-assisted extraction procedure was developed to obtain a comparable recovery of metabolites with respect to the ISO specifications, reducing the solvent volume and the extraction time needed. Metabolite profiles of geographically different saffron extracts were compared showing significant differences in the content of some metabolites. PMID:28234327

Preparation of hydrophobic organic aeorgels

DOEpatents

Baumann, Theodore F.; Satcher, Jr., Joe H.; Gash, Alexander E.

2007-11-06

Synthetic methods for the preparation of hydrophobic organics aerogels. One method involves the sol-gel polymerization of 1,3-dimethoxybenzene or 1,3,5-trimethoxybenzene with formaldehyde in non-aqueous solvents. Using a procedure analogous to the preparation of resorcinol-formaldehyde (RF) aerogels, this approach generates wet gels that can be dried using either supercritical solvent extraction to generate the new organic aerogels or air dried to produce an xerogel. Other methods involve the sol-gel polymerization of 1,3,5 trihydroxy benzene (phloroglucinol) or 1,3 dihydroxy benzene (resorcinol) and various aldehydes in non-aqueous solvents. These methods use a procedure analogous to the one-step base and two-step base/acid catalyzed polycondensation of phloroglucinol and formaldehyde, but the base catalyst used is triethylamine. These methods can be applied to a variety of other sol-gel precursors and solvent systems. These hydrophobic organics aerogels have numerous application potentials in the field of material absorbers and water-proof insulation.

Preparation of hydrophobic organic aeorgels

DOEpatents

Baumann, Theodore F.; Satcher, Jr., Joe H.; Gash, Alexander E.

2004-10-19

Synthetic methods for the preparation of hydrophobic organics aerogels. One method involves the sol-gel polymerization of 1,3-dimethoxybenzene or 1,3,5-trimethoxybenzene with formaldehyde in non-aqueous solvents. Using a procedure analogous to the preparation of resorcinol-formaldehyde (RF) aerogels, this approach generates wet gels that can be dried using either supercritical solvent extraction to generate the new organic aerogels or air dried to produce an xerogel. Other methods involve the sol-gel polymerization of 1,3,5 trihydroxy benzene (phloroglucinol) or 1,3 dihydroxy benzene (resorcinol) and various aldehydes in non-aqueous solvents. These methods use a procedure analogous to the one-step base and two-step base/acid catalyzed polycondensation of phloroglucinol and formaldehyde, but the base catalyst used is triethylamine. These methods can be applied to a variety of other sol-gel precursors and solvent systems. These hydrophobic organics aerogels have numerous application potentials in the field of material absorbers and water-proof insulation.

Composition of sulla (Hedysarum coronarium L.) honey solvent extractives determined by GC/MS: norisoprenoids and other volatile organic compounds.

PubMed

Jerković, Igor; Tuberoso, Carlo I G; Tuberso, Carlo I G; Gugić, Mirko; Bubalo, Dragan

2010-09-09

Samples of unifloral sulla (Hedysarum coronarum L.) honey from Sardinia (Italy) were analysed. To investigate the chemical composition of the honey volatiles two solvent systems were used for ultrasonic solvent extraction (USE): 1) a 1:2 (v/v) pentane and diethyl ether mixture and 2) dichloromethane. All the extracts were analysed by GC and GC/MS. These procedures have permitted the identification of 56 compounds that include norisoprenoids, benzene derivatives, aliphatic compounds and Maillard reaction products. Norisoprenoids were the major compounds in both extracts, dominated by vomifoliol (5.3-11.2%; 9.6-14.0%) followed by minor percentages of other norisoprenoids such as α-isophorone, 4-ketoisophorone, 3-oxo-α-ionol or 3-oxo-α-ionone. Other abundant single compounds in the extracts were 3-hydroxy-4-phenylbutan-2-one (0.8-5.4%; 0.6-5.7%) and methyl syringate (3.0-5.7%; 2.2-4.1%). The composition of the volatiles and semi-volatiles in the obtained extracts suggests that sulla honey is quite distinctive relative to the other honeys that have been chemically studied by GC/MS, but no specific markers of the honey botanical origin were found.

Dispersive liquid-liquid microextraction of quinolones in porcine blood: Optimization of extraction procedure and CE separation using experimental design.

PubMed

Vera-Candioti, Luciana; Teglia, Carla M; Cámara, María S

2016-10-01

A dispersive liquid-liquid microextraction procedure was developed to extract nine fluoroquinolones in porcine blood, six of which were quantified using a univariate calibration method. Extraction parameters including type and volume of extraction and dispersive solvent and pH, were optimized using a full factorial and a central composite designs. The optimum extraction parameters were a mixture of 250 μL dichloromethane (extract solvent) and 1250 μL ACN (dispersive solvent) in 500 μL of porcine blood reached to pH 6.80. After shaking and centrifugation, the upper phase was transferred in a glass tube and evaporated under N 2 steam. The residue was resuspended into 50 μL of water-ACN (70:30, v/v) and determined by CE method with DAD, under optimum separation conditions. Consequently, a tenfold enrichment factor can potentially be reached with the pretreatment, taking into account the relationship between initial sample volume and final extract volume. Optimum separation conditions were as follows: BGE solution containing equal amounts of sodium borate (Na 2 B 4 O 7 ) and di-sodium hydrogen phosphate (Na 2 HPO 4 ) with a final concentration of 23 mmol/L containing 0.2% of poly (diallyldimethylammonium chloride) and adjusted to pH 7.80. Separation was performed applying a negative potential of 25 kV, the cartridge was maintained at 25.0°C and the electropherograms were recorded at 275 nm during 4 min. The hydrodynamic injection was performed in the cathode by applying a pressure of 50 mbar for 10 s. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of solvents extraction on total phenolics and antioxidant activity of extracts from flaxseed (Linum usitatissimum L.).

PubMed

Anwar, Farooq; Przybylski, Roman

2012-01-01

Plant origin food ingredients are the main source of very potent antioxidants. Tocopherols, the main oilseeds natural antioxidants are very potent and when implemented into cell membranes are able to scavenge large number of free radicals. Among plant antioxidants are mainly phenolics, large and diversified group of chemical compounds with different radical scavenging potential. Defatted flaxseed meals were extracted with pure alcohols and its mixture with water. Acquired extracts were analysed for the content of phenolics and flavonoids using colorimetric procedures. Antioxidative capacity was assessed by utilizing: DPPH stable free radicals; inhibition of linoleic acid oxidation and reducing power of components. Investigation was conducted on two different batches of flaxseed, assessing antioxidant capacity of compounds extracted with different polarity solvents and extracts were tested for antioxidant activity with different methods. The highest yield of extraction was achieved with 80% methanol but the extract did not contain the highest amount of phenolics and flavonoids. When 80% ethanol was used for extraction the highest amount of flavonoids was detected and also the best antioxidant capacity. The results clearly showed that utilization of polar solvent enable extraction of significant amounts of phenolics and flavonoids. Those components were the most potent antioxidants present in those extracts. Content of these compounds correlated well with results from applied methods for antioxidant assessment.

Techno-economic assessment of hybrid extraction and distillation processes for furfural production from lignocellulosic biomass.

PubMed

Nhien, Le Cao; Long, Nguyen Van Duc; Kim, Sangyong; Lee, Moonyong

2017-01-01

Lignocellulosic biomass is one of the most promising alternatives for replacing mineral resources to overcome global warming, which has become the most important environmental issue in recent years. Furfural was listed by the National Renewable Energy Laboratory as one of the top 30 potential chemicals arising from biomass. However, the current production of furfural is energy intensive and uses inefficient technology. Thus, a hybrid purification process that combines extraction and distillation to produce furfural from lignocellulosic biomass was considered and investigated in detail to improve the process efficiency. This effective hybrid process depends on the extracting solvent, which was selected based on a comprehensive procedure that ranged from solvent screening to complete process design. Various solvents were first evaluated in terms of their extraction ability. Then, the most promising solvents were selected to study the separation feasibility. Eventually, processes that used the three best solvents (toluene, benzene, and butyl chloride) were designed and optimized in detail using Aspen Plus. Sustainability analysis was performed to evaluate these processes in terms of their energy requirements, total annual costs (TAC), and carbon dioxide (CO 2 ) emissions. The results showed that butyl chloride was the most suitable solvent for the hybrid furfural process because it could save 44.7% of the TAC while reducing the CO 2 emissions by 45.5% compared to the toluene process. In comparison with the traditional purification process using distillation, this suggested hybrid extraction/distillation process can save up to 19.2% of the TAC and reduce 58.3% total annual CO 2 emissions. Furthermore, a sensitivity analysis of the feed composition and its effect on the performance of the proposed hybrid system was conducted. Butyl chloride was found to be the most suitable solvent for the hybrid extraction/distillation process of furfural production. The proposed hybrid sequence was more favorable than the traditional distillation process when the methanol fraction of the feed stream was <3% and more benefit could be obtained when that fraction decreased.

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.

Efficient extraction and preparative separation of four main isoflavonoids from Dalbergia odorifera T. Chen leaves by deep eutectic solvents-based negative pressure cavitation extraction followed by macroporous resin column chromatography.

PubMed

Li, Lu; Liu, Ju-Zhao; Luo, Meng; Wang, Wei; Huang, Yu-Yan; Efferth, Thomas; Wang, Hui-Mei; Fu, Yu-Jie

2016-10-15

In this study, green and efficient deep eutectic solvent-based negative pressure cavitation-assisted extraction (DES-NPCE) followed by macroporous resin column chromatography was developed to extract and separate four main isoflavonoids, i.e. prunetin, tectorigenin, genistein and biochanin A from Dalbergia odorifera T. Chen leaves. The extraction procedure was optimized systematically by single-factor experiments and a Box-Behnken experimental design combined with response surface methodology. The maximum extraction yields of prunetin, tectorigenin, genistein and biochanin A reached 1.204, 1.057, 0.911 and 2.448mg/g dry weight, respectively. Moreover, the direct enrichment and separation of four isoflavonoids in DES extraction solution was successfully achieved by macroporous resin AB-8 with recovery yields of more than 80%. The present study provides a convenient and efficient method for the green extraction and preparative separation of active compounds from plants. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of an analytical procedure to study linear alkylbenzenesulphonate (LAS) degradation in sewage sludge-amended soils.

PubMed

Comellas, L; Portillo, J L; Vaquero, M T

1993-12-24

A procedure for determining linear alkylbenzenesulphonates (LASs) in sewage sludge and amended soils has been developed. Extraction by sample treatment with 0.5 M potassium hydroxide in methanol and reflux was compared with a previously described extraction procedure in Soxhlet with methanol and solid sodium hydroxide in the sample. Repeatability results were similar with savings in extraction time, solvents and evaporation time. A clean-up method involving a C18 cartridge has been developed. Analytes were quantified by a reversed-phase HPLC method with UV and fluorescence detectors. Recoveries obtained were higher than 84%. The standing procedure was applied to high doses of sewage sludge-amended soils (15%) with increasing quantities of added LASs. Degradation data for a 116-day period are presented.

Subcritical water extraction of organic matter from sedimentary rocks.

PubMed

Luong, Duy; Sephton, Mark A; Watson, Jonathan S

2015-06-16

Subcritical water extraction of organic matter containing sedimentary rocks at 300°C and 1500 psi produces extracts comparable to conventional solvent extraction. Subcritical water extraction of previously solvent extracted samples confirms that high molecular weight organic matter (kerogen) degradation is not occurring and that only low molecular weight organic matter (free compounds) are being accessed in analogy to solvent extraction procedures. The sedimentary rocks chosen for extraction span the classic geochemical organic matter types. A type I organic matter-containing sedimentary rock produces n-alkanes and isoprenoidal hydrocarbons at 300°C and 1500 psi that indicate an algal source for the organic matter. Extraction of a rock containing type II organic matter at the same temperature and pressure produces aliphatic hydrocarbons but also aromatic compounds reflecting the increased contributions from terrestrial organic matter in this sample. A type III organic matter-containing sample produces a range of non-polar and polar compounds including polycyclic aromatic hydrocarbons and oxygenated aromatic compounds at 300°C and 1500 psi reflecting a dominantly terrestrial origin for the organic materials. Although extraction at 300°C and 1500 psi produces extracts that are comparable to solvent extraction, lower temperature steps display differences related to organic solubility. The type I organic matter produces no products below 300°C and 1500 psi, reflecting its dominantly aliphatic character, while type II and type III organic matter contribute some polar components to the lower temperature steps, reflecting the chemical heterogeneity of their organic inventory. The separation of polar and non-polar organic compounds by using different temperatures provides the potential for selective extraction that may obviate the need for subsequent preparative chromatography steps. Our results indicate that subcritical water extraction can act as a suitable replacement for conventional solvent extraction of sedimentary rocks, but can also be used for any organic matter containing mineral matrix, including soils and recent sediments, and has the added benefit of tailored extraction for analytes of specific polarities. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

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.

Antioxidant Activity in the Extracts of Two Edible Aroids

PubMed Central

Mandal, P.; Misra, T. K.; Singh, I. D.

2010-01-01

Two neglected species of Araceae, Alocasia macrorhiza (Linn.) G. Don and Alocasia fornicata (Roxb.) Schott are important as food and ethno medicine in Asia and Africa. Their bioefficacy is documented in the Ayurveda. The solvent extracts of different edible parts of these two species like rhizomes, leaves, roots and stolons were screened for in vitro antioxidant properties using standard procedures. The successive extracts in hexane, benzene, toluene, chloroform, diethyl ether, ethyl acetate and water fraction exhibited IC50 values in the following order, roots>rhizome>leaves for Alocasia macrorhiza and leaves>stolon for Alocasia fornicate, respectively in 2,2-diphenyl-1-picryl hydrazyl antioxidant inhibition assay. Maximum antioxidant activity was observed in diethyl ether extracts for both species. The IC50 values were comparable with those of quercetine and ascorbic acid as standards. These results suggest that the two aroid species have antioxidant activity in their edible parts and should be extracted using diethyl ether solvent. PMID:20582198

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

PubMed

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

2016-09-01

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

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.

Extraction and Determination of Cyproheptadine in Human Urine by DLLME-HPLC Method.

PubMed

Maham, Mehdi; Kiarostami, Vahid; Waqif-Husain, Syed; Abroomand-Azar, Parviz; Tehrani, Mohammad Saber; Khoeini Sharifabadi, Malihe; Afrouzi, Hossein; Shapouri, Mahmoudreza; Karami-Osboo, Rouhollah

2013-01-01

Novel dispersive liquid-liquid microextraction (DLLME), coupled with high performance liquid chromatography with photodiode array detection (HPLC-DAD) has been applied for the extraction and determination of cyproheptadine (CPH), an antihistamine, in human urine samples. In this method, 0.6 mL of acetonitrile (disperser solvent) containing 30 μL of carbon tetrachloride (extraction solvent) was rapidly injected by a syringe into 5 mL urine sample. After centrifugation, the sedimented phase containing enriched analyte was dissolved in acetonitrile and an aliquot of this solution injected into the HPLC system for analysis. Development of DLLME procedure includes optimization of some important parameters such as kind and volume of extraction and disperser solvent, pH and salt addition. The proposed method has good linearity in the range of 0.02-4.5 μg mL(-1) and low detection limit (13.1 ng mL(-1)). The repeatability of the method, expressed as relative standard deviation was 4.9% (n = 3). This method has also been applied to the analysis of real urine samples with satisfactory relative recoveries in the range of 91.6-101.0%.

Microwave-Assisted Extraction of Fucoidan from Marine Algae.

PubMed

Mussatto, Solange I

2015-01-01

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

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.

Determination of Microalgal Lipid Content and Fatty Acid for Biofuel Production

PubMed Central

Chen, Zhipeng; Wang, Lingfeng

2018-01-01

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

Isolation and characterization of a Ca/sup 2 +/ carrier candidate from calf heart inner mitochondrial membrane

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

Jeng, A.Y.

1979-01-01

A protein was isolated from calf heart inner mitochondrial membrane with the aid of an electron paramagnetic resonance assay based on the relative binding properties of Ca/sup 2 +/, Mn/sup 2 +/, and Mg/sup 2 +/ to the protein. Partial delipidation of the protein was performed by using either the organic solvent extraction procedure or the silicic acid column chromatography. Control experiments indicated that the Ca/sup 2 +/ transport properties of the isolated protein were not due to the contaminating phospholipids. A complete delipidation procedure was developd by using Sephadex LH-20 column chromatography. Further characterization of the physical and chemicalmore » properties of the delipidated protein showed that delipidated protein becomes more hydrophobic in the presence of Ca/sup 2 +/ and alkaline pH in the organic solvent extraction experiments. Two possible models of calciphorin-mediated Ca/sup 2 +/ transport in mitochondria are proposed. (PCS)« less

Response surface methodology based on central composite design as a chemometric tool for optimization of dispersive-solidification liquid-liquid microextraction for speciation of inorganic arsenic in environmental water samples.

PubMed

Asadollahzadeh, Mehdi; Tavakoli, Hamed; Torab-Mostaedi, Meisam; Hosseini, Ghaffar; Hemmati, Alireza

2014-06-01

Dispersive-solidification liquid-liquid microextraction (DSLLME) coupled with electrothermal atomic absorption spectrometry (ETAAS) was developed for preconcentration and determination of inorganic arsenic (III, V) in water samples. At pH=1, As(III) formed complex with ammonium pyrrolidine dithiocarbamate (APDC) and extracted into the fine droplets of 1-dodecanol (extraction solvent) which were dispersed with ethanol (disperser solvent) into the water sample solution. After extraction, the organic phase was separated by centrifugation, and was solidified by transferring into an ice bath. The solidified solvent was transferred to a conical vial and melted quickly at room temperature. As(III) was determined in the melted organic phase while As(V) remained in the aqueous layer. Total inorganic As was determined after the reduction of the pentavalent forms of arsenic with sodium thiosulphate and potassium iodide. As(V) was calculated by difference between the concentration of total inorganic As and As(III). The variable of interest in the DSLLME method, such as the volume of extraction solvent and disperser solvent, pH, concentration of APDC (chelating agent), extraction time and salt effect, was optimized with the aid of chemometric approaches. First, in screening experiments, fractional factorial design (FFD) was used for selecting the variables which significantly affected the extraction procedure. Afterwards, the significant variables were optimized using response surface methodology (RSM) based on central composite design (CCD). In the optimum conditions, the proposed method has been successfully applied to the determination of inorganic arsenic in different environmental water samples and certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-01-01

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

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.

Analysis of swainsonine and swainsonine N-oxide as trimethylsilyl derivatives by Liquid Chromatography-Mass Spectrometry and their relative occurrence in plants toxic to livestock

USDA-ARS?s Scientific Manuscript database

A liquid chromatography-mass spectrometry method was developed for the analysis of the indolizidine alkaloid swainsonine and its N-oxide. The method is based on a one step solvent partitioning extraction procedure followed by trimethylsilylation of the dried extract and subsequent detection and qua...

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

PubMed

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

2005-12-01

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

Starch extraction process coupled to protein recovery from leguminous tuberous roots (Pachyrhizus ahipa).

PubMed

Díaz, Andrea; Dini, Cecilia; Viña, Sonia Z; García, María A

2016-11-05

The objective of this work was to fit together the starch extraction from Pachyrhizus ahipa roots and the recovery of the proteins present in these storage organs, making an improved use of this novel raw material. The replacement of water by buffer PO4(-3)/NaCl as solvent in the first extraction steps improved protein extraction without lowering the starch yield. The starches obtained from the traditional and the proposed methods exhibited some differences in appearance and technological and thermal properties, which were endorsed to the adjustment in the methodology of extraction rather than to the use of buffer as solvent. Thus, P. ahipa starch obtaining procedure could be coupled to protein extraction with a minimum change in the methodology. This innovation did not significantly shift the characteristics of the starch obtained and allowed to obtain a protein yield of 135.7mg BSA equivalent protein/100g of fresh roots. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2016-09-01

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

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

PubMed Central

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

2016-01-01

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

A new method for microwave assisted ethanolic extraction of Mentha rotundifolia bioactive terpenoids.

PubMed

García-Sarrió, María Jesús; Sanz, María Luz; Sanz, Jesús; González-Coloma, Azucena; Cristina Soria, Ana

2018-04-14

A new microwave-assisted extraction (MAE) method using ethanol as solvent has been optimized by means of a Box-Behnken experimental design for the enhanced extraction of bioactive terpenoids from Mentha rotundifolia leaves; 100°C, 5 min, 1.125 g dry sample: 10 mL solvent and a single extraction cycle were selected as optimal conditions. Improved performance of MAE method in terms of extraction yield and/or reproducibility over conventional solid-liquid extraction and ultrasound assisted extraction was also previously assessed. A comprehensive characterization of MAE extracts was carried out by GC-MS. A total of 46 compounds, mostly terpenoids, were identified; piperitenone oxide and piperitenone were the major compounds determined. Several neophytadiene isomers were also detected for the first time in MAE extracts. Different procedures (solid-phase extraction and activated charcoal (AC) treatment) were also evaluated for clean-up of MAE extracts, with AC providing the highest enrichment in bioactive terpenoids. Finally, the MAE method here developed is shown as a green, fast, efficient and reproducible liquid extraction methodology to obtain M. rotundifolia bioactive extracts for further application, among others, as food preservatives. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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).

In situ alcoholysis of triacylglycerols by application of switchable-polarity solvents. A new derivatization procedure for the gas-chromatographic analysis of vegetable oils.

PubMed

Saliu, Francesco; Orlandi, Marco

2013-10-01

We describe a new use of switchable-polarity solvents for the simultaneous derivatization and extraction of triacylglycerols from vegetable oils before gas-chromatographic analysis. Different equimolecular mixtures of the commercially available amidine 1,8-diazabicyclo[5.4.0]undec-7-ene and n-alkyl alcohols were tested. Triolein was used as a model compound. Very good results were achieved by using butanol (recovery of butyl oleate was 89 ± 4%). The procedure was applied for the characterization of the fatty acid profile of different vegetable oils. No statistically significant differences from the results obtained with the application of two traditional methods were evidenced. Moreover, the use of switchable-polarity solvents showed many advantages: owing to the basicity of the amidines, no catalyst was required; the transterification reaction was conducted under mild conditions, one step and in situ; no particular matrix interferences were evidenced; the solvent was recovered.

Ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME)-a fast new approach to measure phthalate metabolites in nails.

PubMed

Alves, Andreia; Vanermen, Guido; Covaci, Adrian; Voorspoels, Stefan

2016-09-01

A new, fast, and environmentally friendly method based on ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME) was developed and optimized for assessing the levels of seven phthalate metabolites (including the mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP), and mono-benzyl phthalate (MBzP)) in human nails by UPLC-MS/MS. The optimization of the US-DLLME method was performed using a Taguchi combinatorial design (L9 array). Several parameters such as extraction solvent, solvent volume, extraction time, acid, acid concentration, and vortex time were studied. The optimal extraction conditions achieved were 180 μL of trichloroethylene (extraction solvent), 2 mL trifluoroacetic acid in methanol (2 M), 2 h extraction and 3 min vortex time. The optimized method had a good precision (6-17 %). The accuracy ranged from 79 to 108 % and the limit of method quantification (LOQm) was below 14 ng/g for all compounds. The developed US-DLLME method was applied to determine the target metabolites in 10 Belgian individuals. Levels of the analytes measured in nails ranged between <12 and 7982 ng/g. The MEHP, MBP isomers, and MEP were the major metabolites and detected in every sample. Miniaturization (low volumes of organic solvents used), low costs, speed, and simplicity are the main advantages of this US-DLLME based method. Graphical Abstract Extraction and phase separation of the US-DLLME procedure.

Simultaneous determination of the endocrine disrupting compounds nonylphenol, nonylphenol ethoxylates, triclosan and bisphenol A in wastewater and sewage sludge by gas chromatography-mass spectrometry.

PubMed

Gatidou, Georgia; Thomaidis, Nikolaos S; Stasinakis, Athanasios S; Lekkas, Themistokles D

2007-01-05

An integrated analytical method for the simultaneous determination of 4-n-nonylphenol (4-n-NP), nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), bisphenol A (BPA) and triclosan (TCS) in wastewater (dissolved and particulate phase) and sewage sludge was developed based on gas chromatography-mass spectrometry. Chromatographic analysis was achieved after derivatization with bis(trimethylsilyl)trifluoroacetamide (BSTFA). Extraction from water samples was performed by solid-phase extraction (SPE). The optimization of SPE procedure included the type of sorbent and the type of the organic solvent used for the elution. Referred to solid samples, the target compounds were extracted by sonication. In this case the optimization of the extraction procedure included the variation of the amount of the extracted biomass, the duration and the temperature of sonication and the type of the extraction organic solvent. The developed extraction procedures resulted in good repeatability and reproducibility with relative standard deviations (RSDs) less than 13% for all the tested compounds for both types of samples. Satisfactory recoveries were obtained (>60%) for all the compounds in both liquid and solid samples, except for 4-n-NP, which gave recoveries up to 35% in wastewater samples and up to 63% in sludge samples. The limits of detection (LODs) of the target compounds varied from 0.03 (4-n-NP) to 0.41 microg l(-1) (NP2EO) and from 0.04 (4-n-NP) to 0.96 microg kg(-1) (NP2EO) for liquid and solid samples, respectively. The developed methods were successfully applied to the analysis of the target compounds in real samples.

DETERMINATION OF PESTICIDES AND PCB'S IN INDUSTRIAL AND MUNICIPAL WASTEWATERS

EPA Science Inventory

Steps in the procedure for the analysis of 25 chlorinated pesticides and polychlorinated biphenyls were studied. Two gas chromatographic columns and two detectors (electron capture and Hall electrolytic conductivity) were evaluated. Extractions were performed with two solvents (d...

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.

Pressurised solvent extraction for organotin speciation in vegetable matrices.

PubMed

Marcic, Christophe; Lespes, Gaëtane; Potin-Gautier, Martine

2005-08-01

Because organotin compounds (OTC) are widely used in many fields of activity, they have become an ubiquitous environmental presence. The presence of organotins in the environment impacts upon food safety, making it important to monitor the levels of organotin pesticides in fruits and vegetables. Nevertheless, only a few studies have been published on organotin speciation in plants. The objective of the present study was to evaluate and optimise a specific procedure based on pressurised solvent extraction (PSE) that is suitable for monitoring organotin content in vegetables. In ASE, solvents are used at elevated temperatures and pressures to increase the rate and efficiency of the extraction process. The results from this procedure were compared to those from the technique usually employed, solid/liquid extraction (SLE) performed in an acidic solvent by mechanical shaking. Three extracting solutions were tested-methanol, ethyl acetate and a mixture of methanol and ethyl acetate-and the mixture was found to give the most quantitative results while preserving the speciation. French bean and lettuce leaves as well as potato tubers were used as the plant materials. These vegetables were considered because they are the vegetables consumed in the most quantities in Europe. The study focuses on trisubstituted OTCs, which are the most toxic tin species. The samples were spiked with four trisubstituted organotins: tributyltin (TBT), triphenyltin (TPhT), tricyclohexyltin (TcHexT) and trioctyltin (TOcT). The influence of the pressure and the temperature of the PSE on the quantitativity of the process and on species preservation was evaluated using the experimental design methodology. The optimised PSE allowed detection limits down to 1-2 ng (Sn) g(-1) to be reached. These are higher than those obtained by SLE (0.1-1 ng (Sn) g(-1)). Although the repeatability is similar for both PSE and SLE (2-12% for triorganotin compounds), this appears to be highly time-dependent in the case of SLE. Comparison with SLE confirms that PSE is an interesting tool for vegetable analysis considering the satisfactory OTC preservation and repeatability obtained for a relatively short extraction duration (only 15 min against 2-12 h for SLE).

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.

Optimization of extraction methods for quantification of microcystin-LR and microcystin-RR in fish, vegetable, and soil matrices using UPLC-MS/MS.

PubMed

Manubolu, Manjunath; Lee, Jiyoung; Riedl, Kenneth M; Kua, Zi Xun; Collart, Lindsay P; Ludsin, Stuart A

2018-06-01

Human-driven environmental change has increased the occurrence of harmful cyanobacteria blooms in aquatic ecosystems. Concomitantly, exposure to microcystin (MC), a cyanobacterial toxin that can accumulate in animals, edible plants, and agricultural soils, has become a growing public health concern. For accurate estimation of health risks and timely monitoring, availability of reliable detection methods is imperative. Nonetheless, quantitative analysis of MCs in many types of biological and environmental samples has proven challenging because matrix interferences can hinder sample preparation and extraction procedures, leading to poor MC recovery. Herein, controlled experiments were conducted to enhance the use of ultra-performance liquid-chromatography tandem-mass spectrometry (UPLC-MS/MS) to recover MC-LR and MC-RR at a range of concentrations in seafood (fish), vegetables (lettuce), and environmental (soil) matrices. Although these experiments offer insight into detailed technical aspects of the MC homogenization and extraction process (i.e., sonication duration and centrifugation speed during homogenization; elution solvent to use during the final extraction), they centered on identifying the best (1) solvent system to use during homogenization (2-3 tested per matrix) and (2) single-phase extraction (SPE) column type (3 tested) to use for the final extraction. The best procedure consisted of the following, regardless of sample type: centrifugation speed = 4200 × g; elution volume = 8 mL; elution solvent = 80% methanol; and SPE column type = hydrophilic-lipophilic balance (HLB), with carbon also being satisfactory for fish. For sonication, 2 min, 5 min, and 10 min were optimal for fish, lettuce, and soil matrices, respectively. Using the recommended HLB column, the solvent systems that led to the highest recovery of MCs were methanol:water:butanol for fish, methanol:water for lettuce, and EDTA-Na 4 P 2 O 7 for soils. Given that the recommended procedures resulted in average MC-LR and MC-RR recoveries that ranged 93 to 98%, their adoption for the preparation of samples with complex matrices before UPLC-MS/MS analysis is encouraged. Copyright © 2018 Elsevier B.V. All rights reserved.

New method to enhance the extraction yield of rutin from Sophora japonica using a novel ultrasonic extraction system by determining optimum ultrasonic frequency.

PubMed

Liao, Jianqing; Qu, Baida; Liu, Da; Zheng, Naiqin

2015-11-01

A new method has been proposed for enhancing extraction yield of rutin from Sophora japonica, in which a novel ultrasonic extraction system has been developed to perform the determination of optimum ultrasonic frequency by a two-step procedure. This study has systematically investigated the influence of a continuous frequency range of 20-92 kHz on rutin yields. The effects of different operating conditions on rutin yields have also been studied in detail such as solvent concentration, solvent to solid ratio, ultrasound power, temperature and particle size. A higher extraction yield was obtained at the ultrasonic frequency of 60-62 kHz which was little affected under other extraction conditions. Comparative studies between existing methods and the present method were done to verify the effectiveness of this method. Results indicated that the new extraction method gave a higher extraction yield compared with existing ultrasound-assisted extraction (UAE) and soxhlet extraction (SE). Thus, the potential use of this method may be promising for extraction of natural materials on an industrial scale in the future. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

A rapid and effective approach for on-site assessment of total carotenoid content in wolfberry juice during processing.

PubMed

Zheng, Xiaodong; Zhu, Fengtao; Wu, Maoyu; Yan, Xinhuan; Meng, Xiaomeng; Song, Ye

2015-11-01

Carotenoid content analysis in wolfberry processed products has mainly focused on the determination of zeaxanthin or zeaxanthin dipalmitate, which cannot indicate the total carotenoid content (TCC) in wolfberries. We have exploited an effective approach for rapid extraction of carotenoid from wolfberry juice and determined TCC using UV-visible spectrophotometry. Several solvent mixtures, adsorption wavelengths of carotenoid extracts and extraction procedures were investigated. The optimal solvent mixture with broad spectrum polarity was hexane-ethanol-acetone (2:1:1) and optimal wavelength was 456 nm. There was no significant difference of TCC in wolfberry juice between direct extraction and saponification extraction. The developed method for assessment of TCC has been successfully employed in quality evaluation of wolfberry juice under different processing conditions. This measurement approach has inherent advantages (simplicity, rapidity, effectiveness) that make it appropriate for obtaining on-site information of TCC in wolfberry juice during processing. © 2014 Society of Chemical Industry.

Extraction and Determination of Cyproheptadine in Human Urine by DLLME-HPLC Method

PubMed Central

Maham, Mehdi; Kiarostami, Vahid; Waqif-Husain, Syed; Abroomand-Azar, Parviz; Tehrani, Mohammad Saber; Khoeini Sharifabadi, Malihe; Afrouzi, Hossein; Shapouri, MahmoudReza; Karami-Osboo, Rouhollah

2013-01-01

Novel dispersive liquid-liquid microextraction (DLLME), coupled with high performance liquid chromatography with photodiode array detection (HPLC-DAD) has been applied for the extraction and determination of cyproheptadine (CPH), an antihistamine, in human urine samples. In this method, 0.6 mL of acetonitrile (disperser solvent) containing 30 μL of carbon tetrachloride (extraction solvent) was rapidly injected by a syringe into 5 mL urine sample. After centrifugation, the sedimented phase containing enriched analyte was dissolved in acetonitrile and an aliquot of this solution injected into the HPLC system for analysis. Development of DLLME procedure includes optimization of some important parameters such as kind and volume of extraction and disperser solvent, pH and salt addition. The proposed method has good linearity in the range of 0.02-4.5 μg mL-1 and low detection limit (13.1 ng mL-1). The repeatability of the method, expressed as relative standard deviation was 4.9% (n = 3). This method has also been applied to the analysis of real urine samples with satisfactory relative recoveries in the range of 91.6-101.0%. PMID:24250605

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

PubMed

Cools, Katherine; Terry, Leon A

2012-07-15

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

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.

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.

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

PubMed

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

2017-07-01

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

Development of salt and pH-induced solidified floating organic droplets homogeneous liquid-liquid microextraction for extraction of ten pyrethroid insecticides in fresh fruits and fruit juices followed by gas chromatography-mass spectrometry.

PubMed

Torbati, Mohammadali; Farajzadeh, Mir Ali; Torbati, Mostafa; Nabil, Ali Akbar Alizadeh; Mohebbi, Ali; Afshar Mogaddam, Mohammad Reza

2018-01-01

A new microextraction method named salt and pH-induced homogeneous liquid-liquid microextraction has been developed in a home-made extraction device for the extraction and preconcentration of some pyrethroid insecticides from different fruit juice samples prior to gas chromatography-mass spectrometry. In the present work, an extraction device made from two parallel glass tubes with different lengths and diameters was used in the microextraction procedure. In this method, a homogeneous solution of a sample solution and an extraction solvent (pivalic acid) was broken by performing an acid-base reaction and the extraction solvent was produced in whole of the solution. The produced droplets of the extraction solvent went up through the solution and solidified using an ice-bath. They were collected without centrifugation step. Under the optimum conditions, limits of detection and quantification were obtained in the ranges of 0.006-0.038, and 0.023-0.134ngmL -1 , respectively. The enrichment factors and extraction recoveries of the selected analytes ranged from 365-460 to 73-92%, respectively. The relative standard deviations were lower than 9% for intra- (n = 6) and inter-day (n = 4) precisions at a concentration of 1ngmL -1 of each analyte. Finally, some fruit juice samples were effectively analyzed by the proposed method. Copyright © 2017 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2016-07-01

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

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.

Preparing silica aerogel monoliths via a rapid supercritical extraction method.

PubMed

Carroll, Mary K; Anderson, Ann M; Gorka, Caroline A

2014-02-28

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The procedure requires 15-20 min of preparation time, during which a liquid precursor mixture is prepared and poured into wells of a metal mold that is placed between the platens of a hydraulic hot press, followed by several hours of processing within the hot press. The precursor solution consists of a 1.0:12.0:3.6:3.5 x 10(-3) molar ratio of tetramethylorthosilicate (TMOS):methanol:water:ammonia. In each well of the mold, a porous silica sol-gel matrix forms. As the temperature of the mold and its contents is increased, the pressure within the mold rises. After the temperature/pressure conditions surpass the supercritical point for the solvent within the pores of the matrix (in this case, a methanol/water mixture), the supercritical fluid is released, and monolithic aerogel remains within the wells of the mold. With the mold used in this procedure, cylindrical monoliths of 2.2 cm diameter and 1.9 cm height are produced. Aerogels formed by this rapid method have comparable properties (low bulk and skeletal density, high surface area, mesoporous morphology) to those prepared by other methods that involve either additional reaction steps or solvent extractions (lengthier processes that generate more chemical waste).The rapid supercritical extraction method can also be applied to the fabrication of aerogels based on other precursor recipes.

Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

PubMed Central

Gorka, Caroline A.

2014-01-01

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The procedure requires 15-20 min of preparation time, during which a liquid precursor mixture is prepared and poured into wells of a metal mold that is placed between the platens of a hydraulic hot press, followed by several hours of processing within the hot press. The precursor solution consists of a 1.0:12.0:3.6:3.5 x 10-3 molar ratio of tetramethylorthosilicate (TMOS):methanol:water:ammonia. In each well of the mold, a porous silica sol-gel matrix forms. As the temperature of the mold and its contents is increased, the pressure within the mold rises. After the temperature/pressure conditions surpass the supercritical point for the solvent within the pores of the matrix (in this case, a methanol/water mixture), the supercritical fluid is released, and monolithic aerogel remains within the wells of the mold. With the mold used in this procedure, cylindrical monoliths of 2.2 cm diameter and 1.9 cm height are produced. Aerogels formed by this rapid method have comparable properties (low bulk and skeletal density, high surface area, mesoporous morphology) to those prepared by other methods that involve either additional reaction steps or solvent extractions (lengthier processes that generate more chemical waste).The rapid supercritical extraction method can also be applied to the fabrication of aerogels based on other precursor recipes. PMID:24637334

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

PubMed

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

2010-07-01

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

EXTRACTION OF PENTACHLOROPHENOL (PCP) FROM SOILS USING ENVIRONMENTALLY BENIGN ACID SOLUTIONS

EPA Science Inventory

The presence of organic contaminants like PCP in soil is a major environmental concern. Various remediation methods have been used of which soil washing is a common procedure. Many different solvents like surfactants, ionic liquids and cyclodextrins have been studied. the pres...

Solidified Floating Organic Drop Microextraction for the Detection of Trace Amount of Lead in Various Samples by Electrothermal Atomic Absorption Spectrometry.

PubMed

Aydın Urucu, Oya; Dönmez, Şeyda; Kök Yetimoğlu, Ece

2017-01-01

A novel method was developed for determination of trace amounts of lead in water and food samples. Solidified floating organic drop microextraction was used to preconcentrate the lead ion. After the analyte was complexed with 1-(2-pyridylazo)-2-naphthol, undecanol and acetonitrile were added as extraction and dispersive solvent, respectively. Variables such as pH, volumes of extraction and dispersive solvents, and concentration of chelating agent were optimized. Under the optimum conditions, the detection limit of Pb (II) was determined as 0.042  µ g L -1 with an enrichment factor of 300. The relative standard deviation is <10%. Accuracy of the developed procedure was evaluated by the analysis of certified reference material of human hair (NCS DC 73347) and wastewater (SPS-WW2) with satisfactory results. The developed procedure was then successfully applied to biscuit and water samples for detection of Pb (II) ions.

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.

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.

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

PubMed

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

2014-03-07

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

Development of pressurized subcritical water extraction combined with stir bar sorptive extraction for the analysis of organochlorine pesticides and chlorobenzenes in soils.

PubMed

Rodil, Rosario; Popp, Peter

2006-08-18

An analytical method for the determination of several organochlorine pesticides (OCPs) like hexachlorocyclohexanes (HCHs), cyclodiene derivates (dieldrin, aldrin, endrin, heptachlor, heptachlor epoxide, endrin aldehyde, endosulfan and ensodulfan sulphate) and DDX compounds (p,p'-DDE, p,p'-DDD and p,p'-DDT) as well as chlorobenzenes in soils has been developed. The procedure is based on pressurized subcritical water extraction (PSWE) followed by stir bar sorptive extraction (SBSE) and subsequent thermodesorption-gas chromatography/mass spectrometry analysis. Significant PSWE and SBSE parameters were optimized using spiked soil and water samples. For the PSWE of the organochlorine compounds, water modified with acetonitrile as the extraction solvent, at an extraction temperature of 120 degrees C, and three cycles of 10 min extraction proved to be optimal. Under optimized conditions, the figures of merit, such as precision, accuracy and detection limits were evaluated. The detection limits obtained for soil samples were in the range 0.002-4.7 ng/g. Recoveries between 4.1 and 85.2% were achieved from samples spiked at a concentration level of 25-155 ng/g. The main advantages of this method are the avoidance of clean-up and concentration procedures as well as the significant reduction of the required volume of organic solvents. The described method was applied to the determination of the pollutants in soil samples collected from a polluted area, the Bitterfeld region (Germany). The results obtained by PSWE-SBSE were in a good agreement with those obtained by a reference method, a conventional pressurized liquid extraction (PLE).

Comparison and evaluation of volatile oils from three different extraction methods for some Thai fragrant flowers.

PubMed

Paibon, W; Yimnoi, C-A; Tembab, N; Boonlue, W; Jampachaisri, K; Nuengchamnong, N; Waranuch, N; Ingkaninan, K

2011-04-01

Several tropical flowers have distinctive fragrances which are very appealing to use in perfumery, cosmetics and spa. However, to obtain a 'natural fragrance' from the flower is a challenge as the scent could change during the extraction process. The aim of the study is to find the suitable procedure for extraction of volatile oils from some Thai fragrant flowers. Three different methods: hydrodistillation, solvent extraction and enfleurage methods have been applied for the extraction of volatile oil from Jasminum sambac L. Aiton; Oleaceae (jasmine). The quantities and quality of jasmine volatile oils obtained from the different tested methods were compared. The solvent extraction method using 95% ethanol provided the greatest level of oil yield. However, sensory evaluation using preference test showed that the scents of the volatile oils from solvent extraction using diethyl ether and from enfleurage method were the closest to the fresh flowers compared with the volatile oils obtained from other methods. Their chemical constituents were analysed using gas chromatography coupled with mass spectrometer. Both volatile oils were then evaluated using a triangle discrimination test. From the triangle test, we found that 14 panellists from the total of 36 could not distinguish between the scents of jasmine oil from enfleurage and fresh jasmine flowers whereas only one panellist could not distinguish between the scent of jasmine oil from the solvent extraction and fresh jasmine flowers. These results suggest that the scent of the volatile oil obtained from the enfleurage method was the closest to fresh flowers compared with that obtained from other methods. This method was then successfully applied for extraction of volatile oils from three other Thai fragrant flowers, Michelia alba DC.; Magnoliaceae, Millingtonia hortensis L.; Bignoniaceae and Hedychium coronarium J. Konig; Zingiberaceae. © 2010 The Authors. Journal compilation © 2010 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Determination of rutin and quercetin in Chinese herbal medicine by ionic liquid-based pressurized liquid extraction-liquid chromatography-chemiluminescence detection.

PubMed

Wu, Hongwei; Chen, Meilan; Fan, Yunchang; Elsebaei, Fawzi; Zhu, Yan

2012-01-15

A novel ionic liquid-based pressurized liquid extraction (IL-PLE) procedure coupled with high performance liquid chromatography (HPLC) tandem chemiluminescence (CL) detection capable of quantifying trace amounts of rutin and quercetin in four Chinese medicine plants including Flos sophorae Immaturus, Crateagus pinnatifida Bunge, Hypericum japonicum Thunb and Folium Mori was described in this paper. To avoid environmental pollution and toxicity to the operators, ionic liquids (ILs), 1-alkyl-3-methylimidazolium chloride ([C(n)mim][Cl]) aqueous solutions were used in the PLE procedure as extractants replacing traditional organic solvents. In addition, chemiluminescence detection was utilized for its minimal interference from endogenous components of complex matrix. Parameters affecting extraction and analysis were carefully optimized. Compared with the conventional ultrasonic-assisted extraction (UAE) and heat-reflux extraction (HRE), the optimized method achieved the highest extraction efficiency in the shortest extraction time with the least solvent consumption. The applicability of the proposed method to real sample was confirmed. Under the optimized conditions, good reproducibility of extraction performance was obtained and good linearity was observed with correlation coefficients (r) between 0.9997 and 0.9999. The detection limits of rutin and quercetin (LOD, S/N=3) were 1.1×10(-2)mg/L and 3.8×10(-3)mg/L, respectively. The average recoveries of rutin and quercetin for real samples were 93.7-105% with relative standard deviation (RSD) lower than 5.7%. To the best of our knowledge, this paper is the first contribution to utilize a combination of IL-PLE with chemiluminescence detection. And the experimental results indicated that the proposed method shows a promising prospect in extraction and determination of rutin and quercetin in medicinal plants. Copyright © 2011 Elsevier B.V. All rights reserved.

Using a Microscale Approach to Rapidly Separate and Characterize Three Photosynthetic Pigment Species from Fern

ERIC Educational Resources Information Center

Ayudhya, Theppawut Israsena Na; Posey, Frederick T.; Tyus, Jessica C.; Dingra, Nin N.

2015-01-01

A rapid separation of three photosynthetic pigments (chlorophyll "a" and "b" and xanthophyll) from fern ("Polystichum acrostichoides") is described using microscale solvent extraction and traditional thin layer chromatography that minimizes use of harmful chemicals and lengthy procedures. The experiment introduces…

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

DOT National Transportation Integrated Search

2010-01-01

The initial objective of this research was to develop procedures and standards for applying GPC as an analytical tool to define the percentage amounts of polymer modifiers in polymer modified asphalt cements soluble in eluting GPC solvents. Quantific...

Kerosene/Water/2,4-Dinitrophenol.

ERIC Educational Resources Information Center

Whyman, Derek

1986-01-01

Background information/theory, procedures used, and typical results obtained are discussed for a system in which kerosene, water, and 2,4-dinitrophenol (DNP) are used to demonstrate the principles of liquid-liquid extraction in a Graesser rotary contractor. The DNP is almost equal between the two disimilar solvents. (JN)

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.

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

PubMed

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

2001-05-07

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

Solid-phase extraction sorbent consisting of alkyltrimethylammonium surfactants immobilized onto strong cation-exchange polystyrene resin.

PubMed

Reid, Kendra R; Kennedy, Lonnie J; Crick, Eric W; Conte, Eric D

2002-10-25

Presented is a solid-phase extraction sorbent material composed of cationic alkyltrimethylammonium surfactants attached to a strong cation-exchange resin via ion-exchange. The original hydrophilic cation-exchange resin is made hydrophobic by covering the surface with alkyl chains from the hydrophobic portion of the surfactant. The sorbent material now has a better ability to extract hydrophobic molecules from aqueous samples. The entire stationary phase (alkyltrimethylammonium surfactant) is removed along with the analyte during the elution step. The elution step requires a mild elution solvent consisting of 0.25 M Mg2+ in a 50% 2-propanol solution. The main advantage of using a removable stationary phase is that traditionally utilized toxic elution solvents such as methylene chloride, which are necessary to efficiently release strongly hydrophobic species from SPE stationary phases, may now be avoided. Also, the final extract is directly compatible with reversed-phase liquid chromatography. The performance of this procedure is presented using pyrene as a test molecule.

On-matrix derivatization extraction of chemical weapons convention relevant alcohols from soil.

PubMed

Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Dubey, D K; Pardasani, Deepak

2013-10-11

Present study deals with the on-matrix derivatization-extraction of aminoalcohols and thiodiglycols, which are important precursors and/or degradation products of VX analogues and vesicants class of chemical warfare agents (CWAs). The method involved hexamethyldisilazane (HMDS) mediated in situ silylation of analytes on the soil. Subsequent extraction and gas chromatography-mass spectrometry analysis of derivatized analytes offered better recoveries in comparison to the procedure recommended by the Organization for the Prohibition of Chemical Weapons (OPCW). Various experimental conditions such as extraction solvent, reagent and catalyst amount, reaction time and temperature were optimized. Best recoveries of analytes ranging from 45% to 103% were obtained with DCM solvent containing 5%, v/v HMDS and 0.01%, w/v iodine as catalyst. The limits of detection (LOD) and limit of quantification (LOQ) with selected analytes ranged from 8 to 277 and 21 to 665ngmL(-1), respectively, in selected ion monitoring mode. Copyright © 2013 Elsevier B.V. All rights reserved.

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

PubMed

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

2018-05-01

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

Supercritical Carbon Dioxide Extraction of Carotenoids from Pumpkin (Cucurbita spp.): A Review

PubMed Central

Durante, Miriana; Lenucci, Marcello Salvatore; Mita, Giovanni

2014-01-01

Carotenoids are well known for their nutritional properties and health promoting effects representing attractive ingredients to develop innovative functional foods, nutraceutical and pharmaceutical preparations. Pumpkin (Cucurbita spp.) flesh has an intense yellow/orange color owing to the high level of carotenoids, mainly α-carotene, β-carotene, β-cryptoxanthin, lutein and zeaxanthin. There is considerable interest in extracting carotenoids and other bioactives from pumpkin flesh. Extraction procedures able to preserve nutritional and pharmacological properties of carotenoids are essential. Conventional extraction methods, such as organic solvent extraction (CSE), have been used to extract carotenoids from plant material for a long time. In recent years, supercritical carbon dioxide (SC-CO2) extraction has received a great deal of attention because it is a green technology suitable for the extraction of lipophylic molecules and is able to give extracts of high quality and totally free from potentially toxic chemical solvents. Here, we review the results obtained so far on SC-CO2 extraction efficiency and quali-quantitative composition of carotenoids from pumpkin flesh. In particular, we consider the effects of (1) dehydration pre-treatments; (2) extraction parameters (temperature and pressure); the use of water, ethanol and olive oil singularly or in combination as entrainers or pumpkin seeds as co-matrix. PMID:24756094

Supercritical carbon dioxide extraction of carotenoids from pumpkin (Cucurbita spp.): a review.

PubMed

Durante, Miriana; Lenucci, Marcello Salvatore; Mita, Giovanni

2014-04-21

Carotenoids are well known for their nutritional properties and health promoting effects representing attractive ingredients to develop innovative functional foods, nutraceutical and pharmaceutical preparations. Pumpkin (Cucurbita spp.) flesh has an intense yellow/orange color owing to the high level of carotenoids, mainly α-carotene, β-carotene, β-cryptoxanthin, lutein and zeaxanthin. There is considerable interest in extracting carotenoids and other bioactives from pumpkin flesh. Extraction procedures able to preserve nutritional and pharmacological properties of carotenoids are essential. Conventional extraction methods, such as organic solvent extraction (CSE), have been used to extract carotenoids from plant material for a long time. In recent years, supercritical carbon dioxide (SC-CO2) extraction has received a great deal of attention because it is a green technology suitable for the extraction of lipophylic molecules and is able to give extracts of high quality and totally free from potentially toxic chemical solvents. Here, we review the results obtained so far on SC-CO2 extraction efficiency and quali-quantitative composition of carotenoids from pumpkin flesh. In particular, we consider the effects of (1) dehydration pre-treatments; (2) extraction parameters (temperature and pressure); the use of water, ethanol and olive oil singularly or in combination as entrainers or pumpkin seeds as co-matrix.

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.

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.

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.

The Separatory Cylinder: A Novel Solvent Extraction System for the Study of Chemical Equilibrium in Solution.

ERIC Educational Resources Information Center

Cwikel, Dori; And Others

1986-01-01

Dicusses the use of the separatory cylinder in student laboratory experiments for investigating equilibrium distribution of a solute between immiscible phases. Describes the procedures for four sets of experiments of this nature. Lists of materials needed and quantities of reagents are provided. (TW)

EPA CRL MS014: Analysis of Aldicarb, Bromadiolone, Carbofuran, Oxamyl and Methomyl in Water by Multiple Reaction Monitoring Liquid Chromatography / Tandem Mass Spectrometry (LC/MS/MS)

EPA Pesticide Factsheets

Method MS014 describes procedures for solvent extraction of aldicarb, bromadiolone, carbofuran, oxamyl and methomyl from water samples, followed by analysis using liquid chromatography tandem mass spectrometry (LC-MS-MS).

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.

Chemical speciation and recovery of gold(I, III) from wastewater and silver by liquid-liquid extraction with the ion-pair reagent amiloride mono hydrochloride and AAS determination.

PubMed

El-Shahawi, M S; Bashammakh, A S; Bahaffi, S O

2007-06-15

A novel and low cost liquid-liquid extraction procedure for the separation of gold(III) at trace level from aqueous medium of pH 5-9 has been developed. The method has been based upon the formation of a yellow colored ternary complex ion associate of tetrachloro gold(III) complex anion, AuCl(4)(-) with the ion-pair reagent 1-(3,5-diamino-6-chloropyrazinecarboxyl) guanidine hydrochloride monohydrate, namely amiloride, DPG(+).Cl(-). The effect of various parameters, e.g. pH, organic solvent, shaking time, etc. on the preconcentration of gold(III) from the aqueous media by the DPG(+).Cl(-) reagent has been investigated. The colored gold species was quantitatively extracted into 4-methyl pentan-2-one. The chemical composition of the ion associate of DPG(+).Cl(-) with AuCl(4)(-) in the organic solvent has been determined by the Job's method. The molar absorptivity (2.19x10(4)Lmol(-1)cm(-1)) of the associate DPG(+).AuCl(4)(-) at 362nm enabled a convenient application of the developed extraction procedure for the separation and AAS determination of traces of aurate ions. Mono-valence gold ions after oxidation to gold(III) with bromine water in HCl (1.0molL(-1)) media have been also extracted quantitatively from the aqueous media by the developed procedure. The chemical speciation of mono- and/or tri-valence gold species spiked to fresh and industrial wastewater samples has been achieved. The method has been also applied successfully from the separation of gold(I) and gold(III) species from metallic ions and silver. The developed method has also the advantage of freedom from most diverse ions.

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.

Evaluation of different extraction methods from pomegranate whole fruit or peels and the antioxidant and antiproliferative activity of the polyphenolic fraction.

PubMed

Masci, Alessandra; Coccia, Andrea; Lendaro, Eugenio; Mosca, Luciana; Paolicelli, Patrizia; Cesa, Stefania

2016-07-01

Pomegranate is a functional food of great interest, due to its multiple beneficial effects on human health. This fruit is rich in anthocyanins and ellagitannins, which exert a protective role towards degenerative diseases. The aim of the present work was to optimize the extraction procedure, from different parts of the fruit, to obtain extracts enriched in selected polyphenols while retaining biological activity. Whole fruits or peels of pomegranate cultivars, with different geographic origin, were subjected to several extraction methods. The obtained extracts were analyzed for polyphenolic content, evaluated for antioxidant capacity and tested for antiproliferative activity on human bladder cancer T24 cells. Two different extraction procedures, employing ethyl acetate as a solvent, were useful in obtaining extracts enriched in ellagic acid and/or punicalagins. Antioxidative and antiproliferative assays demonstrated that the antioxidant capability is directly related to the phenolic content, whereas the antiproliferative activity is to be mainly attributed to ellagic acid. Copyright © 2016 Elsevier Ltd. All rights reserved.

Optimized ultrasound-assisted extraction procedure for the analysis of opium alkaloids in papaver plants by cyclodextrin-modified capillary electrophoresis.

PubMed

Fakhari, Ali Reza; Nojavan, Saeed; Ebrahimi, Samad Nejad; Evenhuis, Christopher John

2010-07-01

This study investigated the use of ultrasound-assisted extraction to improve the extraction efficiency of morphine, codeine and thebaine from the papaver plants. Extraction conditions such as type of solvent, temperature, duration, frequency and power level of ultrasonic were optimized and the influences of different parameters on resolution of alkaloids in CE were studied. The optimized condition for CE separation includes a sodium phosphate buffer (100 mM, pH 3.0) containing 5 mM alpha-CD. The optimized extraction conditions for ultrasound-assisted extraction was an extraction time of 1 h, an ultrasonic frequency of 60 kHz with water-methanol (80:20) at 40 degrees C as the extraction solvent. The LOD for alkaloids was found to be 0.1 microg/mL at a signal-to-noise ratio of 3:1. The RSDs for peak areas were in the range of 1.4-4.4%. The amounts of opium alkaloids (mg/100 g dried sample) in four Iranian papaver plants were found to be in the range of 7.8-8.7 (morphine), 5.5-9.5 (codeine) and 1.4-10.4 (thebaine). It should be emphasized that no cleanup of the filtered extract was required; hence, direct determination after extraction drastically simplifies the analytical process.

Optimization of Ultrasound Assisted Extraction of Functional Ingredients from Stevia Rebaudiana Bertoni Leaves

NASA Astrophysics Data System (ADS)

Šic Žlabur, Jana; Voća, Sandra; Dobričević, Nadica; Brnčić, Mladen; Dujmić, Filip; Rimac Brnčić, Suzana

2015-04-01

The aim of the present study was to reveal an effective extraction procedure for maximization of the yield of steviol glycosides and total phenolic compounds as well as antioxidant activity in stevia extracts. Ultrasound assisted extraction was compared with conventional solvent extraction. The examined solvents were water (100°C/24 h) and 70% ethanol (at 70°C for 30 min). Qualitative and quantitative analyses of steviol glycosides in the extracts obtained were performed using high performance liquid chromatography. Total phenolic compounds, flavonoids, and radical scavenging capacity by 2, 2-azino-di-3-ethylbenzothialozine- sulphonic acid) assay were also determined. The highest content of steviol glycosides, total phenolic compounds, and flavonoids in stevia extracts were obtained when ultrasound assisted extraction was used. The antioxidant activity of the extracts was correlated with the total amount of phenolic compounds. The results indicated that the examined sonication parameters represented as the probe diameter (7 and 22 mm) and treatment time (2, 4, 6, 8, and 10 min) significantly contributed to the yield of steviol glycosides, total phenolic compounds, and flavonoids. The optimum conditions for the maximum yield of steviol glycosides, total phenolic compounds, and flavonoids were as follows: extraction time 10 min, probe diameter 22 mm, and temperature 81.2°C.

Study on electrical current variations in electromembrane extraction process: Relation between extraction recovery and magnitude of electrical current.

PubMed

Rahmani, Turaj; Rahimi, Atyeh; Nojavan, Saeed

2016-01-15

This contribution presents an experimental approach to improve analytical performance of electromembrane extraction (EME) procedure, which is based on the scrutiny of current pattern under different extraction conditions such as using different organic solvents as supported liquid membrane, electrical potentials, pH values of donor and acceptor phases, variable extraction times, temperatures, stirring rates, different hollow fiber lengths and the addition of salts or organic solvents to the sample matrix. In this study, four basic drugs with different polarities were extracted under different conditions with the corresponding electrical current patterns compared against extraction recoveries. The extraction process was demonstrated in terms of EME-HPLC analyses of selected basic drugs. Comparing the obtained extraction recoveries with the electrical current patterns, most cases exhibited minimum recovery and repeatability at the highest investigated magnitude of electrical current. . It was further found that identical current patterns are associated with repeated extraction efficiencies. In other words, the pattern should be repeated for a successful extraction. The results showed completely different electrical currents under different extraction conditions, so that all variable parameters have contributions into the electrical current pattern. Finally, the current patterns of extractions from wastewater, plasma and urine samples were demonstrated. The results indicated an increase in the electrical current when extracting from complex matrices; this was seen to decrease the extraction efficiency. Copyright © 2015 Elsevier B.V. All rights reserved.

Gas-liquid chromatographic determination of 3-trifluoromethyl-4-nitrophenol residues in fish

USGS Publications Warehouse

Allen, J.L.; Sills, J.B.

1974-01-01

A procedure for the determination of 3-mftuormethyl-4-nitrophenol (TFM) in fish tissues is described. Homogenized tissues are extracted with hexane-ethyl ether; the extract is cleaned up by partitioning the TFM from the extracting solvent into O.IN NaOB, acidifying the aqueous solution, and partitioning again with hexaneethyl ether. The TFM is methylated with diazomethane and analyzed by gas-liquid chromatography, using electron capture detection. Recoveries ranged from 75 to 1000/., from fish muscles that were spiked with 0.01-2.00 JA#g TFM/g.

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.

A cell extraction method for oily sediments

NASA Astrophysics Data System (ADS)

Lappé, M.; Kallmeyer, J.

2012-04-01

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

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

PubMed

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

2013-08-26

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

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.

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

PubMed Central

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

2015-01-01

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

"Bligh and Dyer" and Folch Methods for Solid-Liquid-Liquid Extraction of Lipids from Microorganisms. Comprehension of Solvatation Mechanisms and towards Substitution with Alternative Solvents.

PubMed

Breil, Cassandra; Abert Vian, Maryline; Zemb, Thomas; Kunz, Werner; Chemat, Farid

2017-03-27

Bligh and Dyer (B & D) or Folch procedures for the extraction and separation of lipids from microorganisms and biological tissues using chloroform/methanol/water have been used tens of thousands of times and are "gold standards" for the analysis of extracted lipids. Based on the Conductor-like Screening MOdel for realistic Solvatation (COSMO-RS), we select ethanol and ethyl acetate as being potentially suitable for the substitution of methanol and chloroform. We confirm this by performing solid-liquid extraction of yeast ( Yarrowia lipolytica IFP29 ) and subsequent liquid-liquid partition-the two steps of routine extraction. For this purpose, we consider similar points in the ternary phase diagrams of water/methanol/chloroform and water/ethanol/ethyl acetate, both in the monophasic mixtures and in the liquid-liquid miscibility gap. Based on high performance thin-layer chromatography (HPTLC) to obtain the distribution of lipids classes, and gas chromatography coupled with a flame ionisation detector (GC/FID) to obtain fatty acid profiles, this greener solvents pair is found to be almost as effective as the classic methanol-chloroform couple in terms of efficiency and selectivity of lipids and non-lipid material. Moreover, using these bio-sourced solvents as an alternative system is shown to be as effective as the classical system in terms of the yield of lipids extracted from microorganism tissues, independently of their apparent hydrophilicity.

“Bligh and Dyer” and Folch Methods for Solid–Liquid–Liquid Extraction of Lipids from Microorganisms. Comprehension of Solvatation Mechanisms and towards Substitution with Alternative Solvents

PubMed Central

Breil, Cassandra; Abert Vian, Maryline; Zemb, Thomas; Kunz, Werner; Chemat, Farid

2017-01-01

Bligh and Dyer (B & D) or Folch procedures for the extraction and separation of lipids from microorganisms and biological tissues using chloroform/methanol/water have been used tens of thousands of times and are “gold standards” for the analysis of extracted lipids. Based on the Conductor-like Screening MOdel for realistic Solvatation (COSMO-RS), we select ethanol and ethyl acetate as being potentially suitable for the substitution of methanol and chloroform. We confirm this by performing solid–liquid extraction of yeast (Yarrowia lipolytica IFP29) and subsequent liquid–liquid partition—the two steps of routine extraction. For this purpose, we consider similar points in the ternary phase diagrams of water/methanol/chloroform and water/ethanol/ethyl acetate, both in the monophasic mixtures and in the liquid–liquid miscibility gap. Based on high performance thin-layer chromatography (HPTLC) to obtain the distribution of lipids classes, and gas chromatography coupled with a flame ionisation detector (GC/FID) to obtain fatty acid profiles, this greener solvents pair is found to be almost as effective as the classic methanol–chloroform couple in terms of efficiency and selectivity of lipids and non-lipid material. Moreover, using these bio-sourced solvents as an alternative system is shown to be as effective as the classical system in terms of the yield of lipids extracted from microorganism tissues, independently of their apparent hydrophilicity. PMID:28346372

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.

Microwave-assisted extraction of cyclotides from Viola ignobilis.

PubMed

Farhadpour, Mohsen; Hashempour, Hossein; Talebpour, Zahra; A-Bagheri, Nazanin; Shushtarian, Mozhgan Sadat; Gruber, Christian W; Ghassempour, Alireza

2016-03-15

Cyclotides are an interesting family of circular plant peptides. Their unique three-dimensional structure, comprising a head-to-tail circular backbone chain and three disulfide bonds, confers them stability against thermal, chemical, and enzymatic degradation. Their unique stability under extreme conditions creates an idea about the possibility of using harsh extraction methods such as microwave-assisted extraction (MAE) without affecting their structures. MAE has been introduced as a potent extraction method for extraction of natural compounds, but it is seldom used for peptide and protein extraction. In this work, microwave irradiation was applied to the extraction of cyclotides. The procedure was performed in various steps using a microwave instrument under different conditions. High-performance liquid chromatography (HPLC) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) results show stability of cyclotide structures on microwave radiation. The influential parameters, including time, temperature, and the ratio of solvents that are affecting the MAE potency, were optimized. Optimal conditions were obtained at 20 min of irradiation time, 1200 W of system power in 60 °C, and methanol/water at the ratio of 90:10 (v/v) as solvent. The comparison of MAE results with maceration extraction shows that there are similarities between cyclotide sequences and extraction yields. Copyright © 2015 Elsevier Inc. All rights reserved.

Deep Eutectic Solvent Aqueous Solutions as Efficient Media for the Solubilization of Hardwood Xylans.

PubMed

Morais, Eduarda S; Mendonça, Patrícia V; Coelho, Jorge F J; Freire, Mara G; Freire, Carmen S R; Coutinho, João A P; Silvestre, Armando J D

2018-02-22

This work contributes to the development of integrated lignocellulosic-based biorefineries by the pioneering exploitation of hardwood xylans by solubilization and extraction in deep eutectic solvents (DES). DES formed by choline chloride and urea or acetic acid were initially evaluated as solvents for commercial xylan as a model compound. The effects of temperature, molar ratio, and concentration of the DES aqueous solutions were evaluated and optimized by using a response surface methodology. The results obtained demonstrated the potential of these solvents, with 328.23 g L -1 of xylan solubilization using 66.7 wt % DES in water at 80 °C. Furthermore, xylans could be recovered by precipitation from the DES aqueous media in yields above 90 %. The detailed characterization of the xylans recovered after solubilization in aqueous DES demonstrated that 4-O-methyl groups were eliminated from the 4-O-methylglucuronic acids moieties and uronic acids (15 %) were cleaved from the xylan backbone during this process. The similar M w values of both pristine and recovered xylans confirmed the success of the reported procedure. DES recovery in four additional extraction cycles was also demonstrated. Finally, the successful extraction of xylans from Eucalyptus globulus wood by using aqueous solutions of DES was demonstrated. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Pressurized liquid extraction coupled with countercurrent chromatography for systematic isolation of chemical constituents by preprogrammed automatic control.

PubMed

Zhang, Yuchi; Guo, Liping; Liu, Chunming; Fu, Zi' ao; Cong, Lei; Qi, Yanjuan; Li, Dongping; Li, Sainan; Wang, Jing

2013-09-15

Pressurized liquid extraction (PLE) coupled with high-speed countercurrent chromatography (HSCCC) via an automated procedure was firstly developed to extract and isolate ginsenosides from Panax quinquefolium. The experiments were designed under the guidance of mathematical model. The partition coefficient (K) values of the target compounds and resolutions of peak profiles were employed as the research indicators, and exponential function and binomial formulas were used to optimizing the solvent systems and flow rates of the mobile phases in a three-stage separation. In the first stage, ethyl acetate, n-butanol, and water were simultaneously pumped into the solvent separator at the flow rates 11.0, 10.0, and 23.0mL/min, respectively. The upper phase of the solvent system in the solvent separator was used as both the PLE solvent and the HSCCC stationary phase, followed by elution with the lower phase of the corresponding solvent system to separate the common ginsenosides. In the second and third stages, rare ginsenosides were first separated by elution with ethyl acetate, n-butanol, methanol, and water (flow rates: 20.0, 3.0, 5.0, and 11.0mL/min, respectively), then with n-heptane, n-butanol, methanol, and water (flow rates: 17.5, 6.0, 5.0, and 22.5mL/min, respectively). Nine target compounds, with purities exceeding 95.0%, and three non-target compounds, with purities above 84.48%, were successfully separated at the semipreparative scale in 450min. The separation results prove that the PLE/HSCCC parameters calculated via mathematical model and formulas were accurately and scientifically. This research has opened up great prospects for industrial automation application. Copyright © 2013 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...

Simultaneous accelerated solvent extraction and hydrolysis of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide in meconium samples for gas chromatography-mass spectrometry analysis.

PubMed

Mantovani, Cinthia de Carvalho; Silva, Jefferson Pereira E; Forster, Guilherme; Almeida, Rafael Menck de; Diniz, Edna Maria de Albuquerque; Yonamine, Mauricio

2018-02-01

Cannabis misuse during pregnancy is associated with severe impacts on the mother and baby health, such as newborn low birth weight, growth restriction, pre-term birth, neurobehavioral and developmental deficits. In most of the cases, drug abuse is omitted or denied by the mothers. Thus, toxicological analyzes using maternal-fetal matrices takes place as a suitable tool to assess drug use. Herein, meconium was the chosen matrix to evaluate cannabis exposure through identification and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic (THCCOOH). Accelerated solvent extraction (ASE) was applied for sample preparation technique to simultaneously extract and hydrolyze conjugated THCCOOH from meconium, followed by a solid-phase extraction (SPE) procedure. The method was developed and validated for gas chromatography-mass spectrometry (GC-MS), reaching hydrolysis efficiency of 98%. Limits of detection (LOD) and quantification (LOQ) were, respectively, 5 and 10 ng/g. The range of linearity was LOQ to 500 ng/g. Inter and intra-batch coefficients of variation were <8.4% for all concentration levels. Accuracy was in 101.7-108.9% range. Recovery was on average 60.3%. Carryover effect was not observed. The procedure was applied in six meconium samples from babies whose mothers were drug users and showed satisfactory performance to confirm fetal cannabis exposure. Copyright © 2018 Elsevier B.V. All rights reserved.

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

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

Karnofsky, G. B.

1980-12-16

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

Salting-out assisted liquid-liquid extraction for the determination of biogenic amines in fruit juices and alcoholic beverages after derivatization with 1-naphthylisothiocyanate and high performance liquid chromatography.

PubMed

Jain, Archana; Gupta, Manju; Verma, Krishna K

2015-11-27

A new method for determining biogenic amines in fruit juices and alcoholic beverages is described involving reaction of biogenic amines with 1-naphthylisothiocyanate followed by extraction of 1-naphthylthiourea derivatives with water-miscible organic solvent acetonitrile when solvents phase separation occurred using ammonium sulphate, a process called salting-out assisted liquid-liquid extraction. The extract was analyzed by high-performance liquid chromatography with UV detection at 254nm. The new reagent avoided many of the inconveniences as observed with existing derivatizing agents, such as dansyl chloride and benzoyl chloride, in regard to their inselectivity, instability, adverse effect of excess reagent, and necessity to remove excess reagent. The procedure has been optimized with respect to reaction time and temperature, water-miscible extraction solvent, and salt for solvents phase separation. Use of reagent as dispersed phase in aqueous medium produced derivatives in high yield. A linear calibration was obtained between the amount of biogenic amines in range 1-1000μgL(-1) and peak areas of corresponding thioureas formed; the correlation coefficient was 0.9965, and the limit of detection and limit of quantification found were 1.1μgL(-1) and 3.2μgL(-1), respectively. The pre-concentration method gave an average enrichment factor of 94. The application of the method has been demonstrated in the determination of biogenic amines in commercial samples of fruit juices and alcoholic beverages. In spiking experiments to real samples, the average recovery found by the present method was 94.5% that agreed well with 95.8% obtained by established comparison methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Supramolecular solvent-based extraction of benzimidazolic fungicides from natural waters prior to their liquid chromatographic/fluorimetric determination.

PubMed

Moral, Antonia; Sicilia, María Dolores; Rubio, Soledad

2009-05-01

A supramolecular solvent made up of vesicles of decanoic acid in the nano- and microscale regimes dispersed in a continuous aqueous phase is proposed for the extraction/preconcentration of benzimidazolic fungicides (BFs) from river and underground water samples prior to their determination by liquid chromatography (LC)/fluorimetry. The solvent is produced from the coacervation of decanoic acid aqueous vesicles by the action of tetrabutylammonium (Bu(4)N(+)). Carbendazim (CB), thiabendazole (TB) and fuberidazole (FB) are extracted on the basis of hydrophobic and pi-cation interactions and the formation of hydrogen bonds. The extraction provides high preconcentration factors (160 for CB and 190 for TB and FB), requires a short time (the procedure takes less than 20 min and several samples can be simultaneously processed) and a low sample volume (20 mL), and avoids the use of toxic organic solvents. Because of the absence of matrix interferences and the low viscosity of the extracts, these can be directly injected into the chromatographic system without the need of cleaning-up or diluting them. Recoveries are not influenced by the presence of salt concentrations up to 1 M. The proposed method provides detection limits for the determination of CB, TB and FB in natural waters of 32, 4 and 0.1 ng L(-1), respectively, and a precision, expressed as relative standard deviation (n=11) of 5.5% for CB (100 ng L(-1)), 4.0% for TB (80 ng L(-1)) and 2.5% for FB (30 ng L(-1)). Recoveries obtained by applying this approach to the analysis of river and underground water samples fortified at the ng L(-1) level are in the intervals 75-83, 95-102 and 97-101% for CB, TB and FB, respectively.

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).

Salting-out-enhanced ionic liquid microextraction with a dual-role solvent for simultaneous determination of trace pollutants with a wide polarity range in aqueous samples.

PubMed

Gao, Man; Qu, Jingang; Chen, Kai; Jin, Lide; Dahlgren, Randy Alan; Wang, Huili; Tan, Chengxia; Wang, Xuedong

2017-11-01

In real aquatic environments, many occupational pollutants with a wide range of polarities coexist at nanogram to milligram per liter levels. Most reported microextraction methods focus on extracting compounds with similar properties (e.g., polarity or specific functional groups). Herein, we developed a salting-out-enhanced ionic liquid microextraction based on a dual-role solvent (SILM-DS) for simultaneous detection of tetracycline, doxycycline, bisphenol A, triclosan, and methyltriclosan, with log K ow ranging from -1.32 to 5.40 in complex milk and environmental water matrices. The disperser in the ionic-liquid-based dispersive liquid-liquid microextraction was converted to the extraction solvent in the subsequent salting-out-assisted microextraction procedures, and thus a single solvent performed a dual role as both extractant and disperser in the SILM-DS process. Acetonitrile was selected as the dual-role solvent because of its strong affinity for both ionic liquids and water, as well as the extractant in the salting-out step. Optimized experimental conditions were 115 μL [C 8 MIM][PF 6 ] as extractor, 1200 μL acetonitrile as dual-role solvent, pH 2.0, 5.0 min ultrasound extraction time, 3.0 g Na 2 SO 4 , and 3.0 min vortex extraction time. Under optimized conditions, the recoveries of the five pollutants ranged from 74.5 to 106.9%, and their LODs were 0.12-0.75 μg kg -1 in milk samples and 0.11-0.79 μg L -1 in environmental waters. Experimental precision based on relative standard deviation was 1.4-6.4% for intraday and 2.3-6.5% for interday analyses. Compared with previous methods, the prominent advantages of the newly developed method are simultaneous determination of pollutants with a wide range of polarities and a substantially reduced workload for ordinary environmental monitoring and food tests. Therefore, the new method has great application potential for simultaneous determination of trace pollutants with strongly contrasting polarities in several analytical fields. Graphical Abstract A salting-out-enhanced ionic liquid microextraction based on a dual-role solvent (SILM-DS) was developed for simultaneous detection of tetracycline, doxycycline, bisphenol A, triclosan and methyltriclosan, with log K ow ranging from -1.32 to 5.40. The novelty of SILM-DS method lies in (1) simultaneous quantification of pollutants with contrasting polarity; (2) microextraction based on a dual-role solvent (as a disperser and extractant); (3) giving high recoveries for analytes with a wide range of polarities; and (4) reducing workload for ordinary environmental monitoring and food tests.

Determination of siloxanes in silicone products and potential migration to milk, formula and liquid simulants.

PubMed

Zhang, Kai; Wong, Jon W; Begley, Timothy H; Hayward, Douglas G; Limm, William

2012-08-01

A pressurised solvent extraction procedure coupled with a gas chromatography-mass spectrometry-selective ion monitoring (GC-MS-SIM) method was developed to determine three cyclic siloxanes, octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6) and three linear siloxanes, octamethyltrisiloxane (L3), decamethyltetrasiloxane (L4), dodecamethylpentasiloxane (L5), in silicone products. Additionally, two different extraction methods were developed to measure these siloxanes migrating into milk, infant formula and liquid simulants (50 and 95% ethanol in water). The limits of quantification (LOQs) of the six siloxanes ranged from 6 ng/g (L3) to 15 ng/g (D6). Silicone nipples and silicone bakewares were extracted using pressurised solvent extraction (PSE) and analysed using the GC-MS-SIM method. No linear siloxanes were detected in the silicone nipple samples analysed. The three cyclic siloxanes (D4, D5 and D6) were detected in all silicone nipple samples with concentrations ranging from 0.5 to 269 µg/g. In the bakeware samples, except for L3, the other five siloxanes were detected with concentrations ranging from 0.2 µg/g (L4) to 7030 µg/g (D6). To investigate the potential migration of the six siloxanes from silicone nipples to milk and infant formula, a liquid extraction and dispersive clean-up procedure was developed for the two matrices. The procedure used a mix of hexane and ethyl acetate (1 : 1, v/v) as extraction solvent and C₁₈ powder as the dispersive clean-up sorbent. For the liquid simulants, extraction of the siloxanes was achieved using hexane without any salting out or clean-up procedures. The recoveries of the six siloxanes from the milk, infant formula and simulants fortified at 50, 100, 200, 500 and 1000 µg/l ranged from 70 to 120% with a relative standard derivation (RSD) of less than 15% (n = 4). Migration tests were performed by exposing milk, infant formula and the liquid simulants to silicone baking sheets with known concentrations of the six siloxanes at 40°C. No siloxanes were detected in milk or infant formula after 6 h of direct contact with the silicone baking sheet plaques, indicating insignificant migration of the siloxanes to milk or infant formula. Migration tests in the two simulants lasted up to 72 h and the three cyclic siloxanes were detected in 50% ethanol after an 8-h exposure and after 2 h in 95% ethanol. The highest detected concentrations of D4, D5 and D6 were 42, 36 and 155 ng/ml, respectively, indicating very limited migration of D4, D5 or D6 into the two simulants.

Chemical Analysis and Risk Assessment of Diethyl Phthalate in Alcoholic Beverages with Special Regard to Unrecorded Alcohol

PubMed Central

Leitz, Jenny; Kuballa, Thomas; Rehm, Jürgen; Lachenmeier, Dirk W.

2009-01-01

Background Phthalates are synthetic compounds with a widespread field of applications. For example, they are used as plasticizers in PVC plastics and food packaging, or are added to personal care products. Diethyl phthalate (DEP) may be used to denature alcohol, e.g., for cosmetic purposes. Public health concerns of phthalates include carcinogenic, teratogenic, hepatotoxic and endocrine effects. The aim of this study was to develop and validate a method for determining phthalates in alcohol samples and to provide a risk assessment for consumers of such products. Methodology/Principal Findings A liquid-liquid extraction procedure was optimized by varying the following parameters: type of extraction solvent (cyclohexane, n-hexane, 1,1,2-trichlorotrifluoroethane), the ratio extraction solvent/sample volume (1∶1 to 50∶1) and the number of extraction repetitions (1–10). The best extraction yield (99.9%) was achieved with the solvent 1,1,2-trichlorotrifluoroethane, an extraction solvent volume/sample volume ratio of 10∶1 and a double extraction. For quantification, gas chromatography/mass spectrometry with deuterated internal standards was used. The investigated samples were alcoholic beverages and unrecorded alcohol products from different countries (n = 257). Two unrecorded alcohol samples from Lithuania contained diethyl phthalate in concentrations of 608 mg/L and 210 mg/L. Conclusions/Significance The consumption of the phthalate-positive unrecorded alcohols would exceed tolerable daily intakes as derived from animal experiments. Both positive samples were labelled as cosmetic alcohol, but had clearly been offered for human consumption. DEP seems to be unsuitable as a denaturing agent as it has no effect on the organoleptic properties of ethanol. In light of our results that DEP might be consumed by humans in unrecorded alcohols, the prohibition of its use as a denaturing agent should be considered. PMID:19956573

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.

Antioxidant potential of polyphenols and tannins from burs of Castanea mollissima Blume.

PubMed

Zhao, Shan; Liu, Jie Yuan; Chen, Si Yu; Shi, Ling Ling; Liu, Yu Jun; Ma, Chao

2011-10-12

Spiny burs of Castanea mollissima Blume (Chinese chestnut) are usually discarded as industrial waste during post-harvesting processing. The objective of this study was to establish an extraction and isolation procedure for tannins from chestnut burs, and to assess their potential antioxidant activity. Aqueous ethanol solution was used as extraction solvent, and HPD 100 macroporous resin column was applied for isolation. The influence of solvent concentration in the extraction and elution process on extraction yield, tannins and polyphenols content, as well as antioxidant potential, including DPPH and ABTS radical scavenging ability, reducing power ability and cellular antioxidant ability were assessed. In both the extraction and isolation process, 50% aqueous ethanol led to superior total tannins and polyphenols content as well as significantly higher antioxidant activity. In addition, the antioxidant activity and the total tannins content in extracts and fractions had a positive linear correlation, and the predominant components responsible for antioxidant activities were characterized as hydrolysable tannins. To the best of our knowledge, this is the first report on the enrichment of tannins from burs of C. mollissim using macroporous resin chromatography, and to assess the cellular antioxidant activity of them.

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

PubMed

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

2006-06-01

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

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...

Extraction and Identification of Phlorotannins from the Brown Alga, Sargassum fusiforme (Harvey) Setchell

PubMed Central

Li, Yajing; Fu, Xiaoting; Duan, Delin; Liu, Xiaoyong; Xu, Jiachao; Gao, Xin

2017-01-01

Phlorotannins are a group of complex polymers of phloroglucinol (1,3,5-trihydroxybenzene), which are unique compounds from marine brown algae. In our present study, a procedure for extraction and enrichment of phlorotannins from S. fusiforme with highly antioxidant potentials was established. After comparison of different extraction methods, the optimal extraction conditions were established as follows. The freeze-dried seaweed powder was extracted with 30% ethanol-water solvent with a solid/liquid ratio of 1:5 at temperature of 25 °C for 30 min. After extraction, the phlorotannins were fractioned by different solvents, among which the ethyl acetate fraction exhibited both the highest total phlorotannin content (88.48 ± 0.30 mg PGE/100 mg extract) and the highest antioxidant activities. The extracts obtained from these locations were further purified and characterized using a modified UHPLC-QQQ-MS method. Compounds with 42 different molecular weights were detected and tentatively identified, among which the fuhalol-type phlorotannins were the dominant compounds, followed by phlorethols and fucophlorethols with diverse degree of polymerization. Eckol-type phlorotannins including some newly discovered carmalol derivatives were detected in Sargassum species for the first time. Our study not only described the complex phlorotannins composition in S. fusiforme, but also highlighted the challenges involved in structural elucidation of these compounds. PMID:28230766

Analysis of N-Nitrosodimethylamine and N-Nitrodimethylamine in Groundwater

NASA Technical Reports Server (NTRS)

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

2006-01-01

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

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.

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.

Metal speciation of environmental samples using SPE and SFC-AED analysis

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

Mitchell, S.C.; Burford, M.D.; Robson, M.

1995-12-31

Due to growing public concern over heavy metals in the environment, soil, water and air particulate samples azre now routinely screened for their metal content. Conventional metal analysis typically involves acid digestion extraction and results in the generation of large aqueous and organic solvent waste. This harsh extraction process is usually used to obtain the total metal content of the sample, the extract being analysed by atomic emission or absorption spectroscoply techniques. A more selective method of metal extraction has been investigated which uses a supercritical fluid modified with a complexing agent. The relatively mild extraction method enables both organometallicmore » and inorganic metal species to be recovered intact. The various components from the supercritical fluid extract can be chromatographically separated using supercritical fluid chromatography (SFC) and positive identification of the metals achieved using atomic emission detection (AED). The aim of the study is to develop an analytical extraction procedure which enables a rapid, sensitive and quantitative analysis of metals in environmental samples, using just one extraction (eg SFE) and one analysis (eg SFC-AED) procedure.« less

Development of a novel naphthoic acid ionic liquid and its application in "no-organic solvent microextraction" for determination of triclosan and methyltriclosan in human fluids and the method optimization by central composite design.

PubMed

Wang, Hui; Gao, Jiajia; Yu, Nana; Qu, Jingang; Fang, Fang; Wang, Huili; Wang, Mei; Wang, Xuedong

2016-07-01

In traditional ionic liquids (ILs)-based microextraction, the hydrophobic and hydrophilic ILs are often used as extractant and disperser, respectively. However, the functional effects of ILs are not utilized in microextraction procedures. Herein, we introduced 1-naphthoic acid into imidazolium ring to synthesize a novel ionic liquid 1-butyl-3-methylimidazolium naphthoic acid salt ([C4MIM][NPA]), and its structure was characterized by IR, (1)H NMR and MS. On the basis of its acidic property and lower solubility than common [CnMIM][BF4], it was used as a mixing dispersive solvent with [C4MIM][BF4] in "functionalized ionic liquid-based no organic solvent microextraction (FIL-NOSM)". Utilization of [C4MIM][NPA] in FIL-NOSM procedures has two obvious advantages: (1) it promoted the non-polar environment, increased volume of the sedimented phase, and thus could enhance the extraction recoveries of triclosan (TCS) and methyltriclosan (MTCS) by more than 10%; and (2) because of the acidic property, it can act as a pH modifier, avoiding extra pH adjustment step. By combining single factor optimization and central composite design, the main factors in the FIL-NOSM method were optimized. Under the optimal conditions, the relative recoveries of TCS and MTCS reached up to 98.60-106.09%, and the LODs of them were as low as 0.12-0.15µgL(-1) in plasma and urine samples. In total, this [C4MIM][NPA]-based FIL-NOSM method provided high extraction efficiency, and required less pretreatment time and unutilized any organic solvent. To the best of our knowledge, this is the first application of [C4mim][NPA]-based microextraction method for the simultaneous quantification of trace TCS and MTCS in human fluids. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2012-12-01

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

Determination of blood concentrations of main active compounds in Zi-Cao-Cheng-Qi decoction and their total plasma protein binding rates based on hollow fiber liquid phase microextraction coupled with high performance liquid chromatography.

PubMed

Li, Miaomiao; Chen, Xuan; Hu, Shuang; Wang, Runqin; Peng, Xiaoli; Bai, Xiaohong

2018-01-01

Oil-in-salt hollow fiber liquid phase microextraction coupled with high performance liquid chromatography ultraviolet detection (HPLC-UV) was developed for determination of the blood concentrations of the main active compounds, hesperidin, honokiol, shikonin, magnolol, emodin and β,β'-dimethylacrylshikonin, after oral administration of Zi-Cao-Cheng-Qi decoction (ZCCQD) and their total plasma protein binding rates. In the procedure, a hollow fiber segment was immersed in organic solvent to fill the solvent in the fiber lumen and wall pore, and then the fiber was immersed into sodium chloride solution to cover a thin salt membrane on the fiber wall pore filling organic solvent. Various factors affecting the procedure, such as extraction solvent, sample phase pH, stirring rate, extraction time, NaCl concentration and fiber immersion time in the NaCl solution, were optimized. Under the optimum conditions, good linearities (r 2 ≥0.9905), low limits of detection (0.7-2.5ng/mL) or quantitation (1.2-12ng/mL), satisfactory precision (2.6%-12.8%) and accuracy (81.0%-114.2%) of this method, were observed. The results showed that, after oral administration of a 25g/kg dose, (1) the blood concentrations (at 0.5h) of hesperidin, honokiol, shikonin, magnolol, emodin and β,β'-dimethylacrylshikonin were 0.45, 0.40, 0.48, 0.74, 0.11 and 1.11μg/mL, respectively; (2) the total plasma protein binding rates of the six active compounds were 42.0% (hesperidin), 71.8% (honokiol), 64.6% (shikonin), 77.7% (magnolol), 75.3% (emodin) and 75.7% (β,β'-dimethylacrylshikonin), respectively. The proposed procedure coupled with HPLC shows obvious advantages, such as low solvent consumption, simple operation, high sensitivity and strong purifying and can be used for the determination of both the blood concentrations and total plasma protein binding rates of active compounds in traditional Chinese medicine. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of deep eutectic solvents applied in extraction and separation.

PubMed

Li, Xiaoxia; Row, Kyung Ho

2016-09-01

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

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.

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 solvent-extraction module for cyclotron production of high-purity technetium-99m.

PubMed

Martini, Petra; Boschi, Alessandra; Cicoria, Gianfranco; Uccelli, Licia; Pasquali, Micòl; Duatti, Adriano; Pupillo, Gaia; Marengo, Mario; Loriggiola, Massimo; Esposito, Juan

2016-12-01

The design and fabrication of a fully-automated, remotely controlled module for the extraction and purification of technetium-99m (Tc-99m), produced by proton bombardment of enriched Mo-100 molybdenum metallic targets in a low-energy medical cyclotron, is here described. After dissolution of the irradiated solid target in hydrogen peroxide, Tc-99m was obtained under the chemical form of 99m TcO 4 - , in high radionuclidic and radiochemical purity, by solvent extraction with methyl ethyl ketone (MEK). The extraction process was accomplished inside a glass column-shaped vial especially designed to allow for an easy automation of the whole procedure. Recovery yields were always >90% of the loaded activity. The final pertechnetate saline solution Na 99m TcO 4 , purified using the automated module here described, is within the Pharmacopoeia quality control parameters and is therefore a valid alternative to generator-produced 99m Tc. The resulting automated module is cost-effective and easily replicable for in-house production of high-purity Tc-99m by cyclotrons. Copyright © 2016 Elsevier Ltd. All rights reserved.

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.

Extraction and characterization of polysaccharides from Semen Cassiae by microwave-assisted aqueous two-phase extraction coupled with spectroscopy and HPLC.

PubMed

Chen, Zhi; Zhang, Wei; Tang, Xunyou; Fan, Huajun; Xie, Xiujuan; Wan, Qiang; Wu, Xuehao; Tang, James Z

2016-06-25

A novel and rapid method for simultaneous extraction and separation of the different polysaccharides from Semen Cassiae (SC) was developed by microwave-assisted aqueous two-phase extraction (MAATPE) in a one-step procedure. Using ethanol/ammonium sulfate system as a multiphase solvent, the effects of MAATPE on the extraction of polysaccharides from SC such as the composition of the ATPS, extraction time, temperature and solvent-to-material ratio were investigated by UV-vis analysis. Under the optimum conditions, the yields of polysaccharides were 4.49% for the top phase, 8.80% for the bottom phase and 13.29% for total polysaccharides, respectively. Compared with heating solvent extraction and ultrasonic assisted extraction, MAATPE exhibited the higher extraction yields in shorter time. Fourier-transform infrared spectra showed that two polysaccharides extracted from SC to the top and bottom phases by MAATPE were different from each other in their chemical structures. Through acid hydrolysis and PMP derivatization prior to HPLC, analytical results by indicated that a polysaccharide of the top phases was a relatively homogeneous homepolysaccharide composed of dominant gucose glucose while that of the bottom phase was a water-soluble heteropolysaccharide with multiple components of glucose, xylose, arabinose, galactose, mannose and glucuronic acid. Molar ratios of monosaccharides were 95.13:4.27:0.60 of glucose: arabinose: galactose for the polysaccharide from the top phase and 62.96:14.07:6.67: 6.67:5.19:4.44 of glucose: xylose: arabinose: galactose: mannose: glucuronic acid for that from the bottom phase, respectively. The mechanism for MAATPE process was also discussed in detail. MAATPE with the aid of microwave and the selectivity of the ATPS not only improved yields of the extraction, but also obtained a variety of polysaccharides. Hence, it was proved as a green, efficient and promising alternative to simultaneous extraction of polysaccharides from SC. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2017-03-01

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

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.

Antioxidant activity of Rafflesia kerrii flower extract.

PubMed

Puttipan, Rinrampai; Okonogi, Siriporn

2014-02-01

Rafflesia kerrii has been used in Thai traditional remedies for treatment of several diseases. However, scientific data particularly on biological activities of this plant is very rare. The present study explores an antioxidant activity of R. kerrii flower (RKF). Extracting solvent and extraction procedure were found to play an important role on the activity of RKF extract. The extract obtained from water-ethanol system showed higher antioxidant activity than that from water-propylene glycol system. Fractionated extraction using different solvents revealed that methanol fractionated extract (RM) possessed the highest antioxidant activity with Trolox equivalent antioxidant capacity (TEAC) and inhibitory concentration of 50% inhibition (IC50) values of approximately 39 mM/mg and 3 μg/mL, respectively. Phytochemical assays demonstrated that RM contained extremely high quantity of phenolic content with gallic antioxidant equivalent (GAE) and quercetin equivalent (QE) values of approximately 312 mg/g and 16 mg/g, respectively. Ultraviolet-visible spectroscopy (UV- VIS) and high-pressure liquid chromatography (HPLC) indicated that gallic acid was a major component. RM which was stored at 40°C, 75% RH for 4 months showed slightly significant change (p < 0.05) in phytochemical content and antioxidant activity with zero order degradation. The results of this study could be concluded that R. kerrii flower was a promising natural source of strong antioxidant compounds.

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.

Optimization of microwave-assisted extraction of protopine and allocryptopine from stems of Macleaya cordata (Willd) R. Br. using response surface methodology.

PubMed

Zhong, Ming; Huang, Ke-Long; Zeng, Jian-Guo; Li, Shuang; She, Jin-Ming; Li, Guiyin; Zhang, Li

2010-07-01

The purpose of the research was to investigate the multiple response optimizations for the extraction of protopine and allocryptopine from the stems of Macleaya cordata (Willd) R. Br. by using microwave-assisted extraction (MAE). A three-level, three-factor Box-Behnken design of response surface methodology was used to develop response model, and desirability function was employed to optimize the effects of main extraction parameters. Three variables, ethanol concentration (20-80%, v/v), extraction temperature (30-70 degrees C) and solvent/solid ratio (10:1 to 30:1, mL/g), were investigated in this study. The results showed that the optimum parameters of MAE were ethanol concentration of 45.2 % (v/v), extraction temperature of 54.7 degrees C and solvent/solid ratio of 20.4:1 (mL/g). Under these conditions, the extraction yields of protopine and allocryptopine were 89.4 and 102.0%, respectively, and the extracta sicca yield was 12.5%. The combination use of response surface methodology, Box-Behnken design and the appropriate desirability function could provide an insight into a lab-scale MAE process, and help to develop procedures for commercial production of active ingredients from medical plants.

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...

Application of elevated temperature-dispersive liquid-liquid microextraction for determination of organophosphorus pesticides residues in aqueous samples followed by gas chromatography-flame ionization detection.

PubMed

Farajzadeh, Mir Ali; Afshar Mogaddam, Mohammad Reza; Rezaee Aghdam, Samaneh; Nouri, Nina; Bamorrowat, Mahdi

2016-12-01

In the present study, an elevated temperature, dispersive, liquid-liquid microextraction/gas chromatography-flame ionization detection was investigated for the determination, pre-concentration, and extraction of six organophosphorus pesticides (malathion, phosalone, dichlorvos, diazinon, profenofos, and chlorpyrifos) residues in fruit juice and aqueous samples. A mixture of 1,2-dibromoethane (extraction solvent) and dimethyl sulfoxide (disperser solvent) was injected rapidly into the sample solution heated at an elevated temperature. Analytical parameters, including enrichment factors (1600-2075), linearity (r>0.994), limits of detection (0.82-2.72ngmL(-1)) and quantification (2.60-7.36ngmL(-1)), relative standard deviations (<7%) and extraction recoveries (64-83%), showed the high efficiency of the method developed for analysis of the target analytes. The proposed procedure was used effectively to analyse selected analytes in river water and fruit juice, and diazinon was found at ngmL(-1) concentrations in apple juice. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed Central

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

2015-01-01

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

Selective treatment to reduce contamination of propolis by polycyclic aromatic hydrocarbons (PAHs) still preserving its active polyphenol component and antioxidant activity.

PubMed

Galeotti, Fabio; Crimaldi, Laura; Maccari, Francesca; Zaccaria, Vincenzo; Fachini, Alfredo; Volpi, Nicola

2017-09-01

The adverse effects on health and environment caused by polycyclic aromatic hydrocarbons (PAHs) are critical problems. EFSA has defined 16 priority PAHs that are both genotoxic and carcinogenic, and identified eight (PAH8) priority PAHs as good indicators of the toxicity and occurrence in food. Food supplements containing propolis were also found to contain relatively high quantities of PAHs. We report about an extractive procedure which is able to purify propolis from a high content of PAHs using a balanced mixture of ethanol and water solvents. Extracts were characterised for total content of polyphenols, for in vitro antioxidant activity, and single classes of polyphenols evaluated by HPLC-ESI-MS. Obtained propolis extracts were found to have PAH8 and specific benzo[a]pyrene content below limits recommended by EFSA. The reported extractive procedure is easily applicable for possible industrial productions and may also be adopted to the purification of polyphenols from other plant extracts and natural sources.

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.

Determination of Caffeine in Beverages by Capillary Zone Electrophoresis: An Experiment for the Undergraduate Analytical Laboratory

NASA Astrophysics Data System (ADS)

Conte, Eric D.; Barry, Eugene F.; Rubinstein, Harry

1996-12-01

Certain individuals may be sensitive to specific compounds in comsumer products. It is important to quantify these analytes in food products in order to monitor their intake. Caffeine is one such compound. Determination of caffeine in beverages by spectrophotometric procedures requires an extraction procedure, which can prove time-consuming. Although the corresponding determination by HPLC allows for a direct injection, capillary zone electrophoresis provides several advantages such as extremely low solvent consumption, smaller sample volume requirements, and improved sensitivity.

Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

PubMed Central

2016-01-01

Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient's plasma sample using less than 550 μL of organic solvent. PMID:27830105

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.

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.

Estrogens determination in wastewater samples by automatic in-syringe dispersive liquid-liquid microextraction prior silylation and gas chromatography.

PubMed

González, Alba; Avivar, Jessica; Cerdà, Víctor

2015-09-25

A new procedure for the extraction, preconcentration and simultaneous determination of the estrogens most used in contraception pharmaceuticals (estrone, 17β-estradiol, estriol, and 17α-ethynylestradiol), cataloged as Contaminants of Emergent Concern by the Environmental Protection Agency of the United States (US-EPA), is proposed. The developed system performs an in-syringe magnetic stirring-assisted dispersive liquid-liquid microextraction (in-syringe-MSA-DLLME) prior derivatization and gas chromatography (GC-MS). Different extraction (carbon tetrachloride, ethyl acetate, chloroform and trichloroethylene) and disperser solvents (acetone, acetonitrile and methanol) were tested. Chloroform and acetone were chosen as extraction and disperser solvent, respectively, as they provided the best extraction efficiency. Then, a multivariate optimization of the extraction conditions was carried out. Derivatization conditions were also studied to ensure the conversion of the estrogens to their respective trimethylsilyl derivatives. Low LODs and LOQs were achieved, i.e. between 11 and 82ngL(-1), and 37 and 272ngL(-1), respectively. Good values for intra and inter-day precision were obtained (RSDs≤7.06% and RSD≤7.11%, respectively). The method was successfully applied to wastewater samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

PubMed

Sadeghi, Susan; Ashoori, Vahid

2017-10-01

The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

[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.

Frontally eluted components procedure with thin layer chromatography as a mode of sample preparation for high performance liquid chromatography quantitation of acetaminophen in biological matrix.

PubMed

Klimek-Turek, A; Sikora, M; Rybicki, M; Dzido, T H

2016-03-04

A new concept of using thin-layer chromatography to sample preparation for the quantitative determination of solute/s followed by instrumental techniques is presented Thin-layer chromatography (TLC) is used to completely separate acetaminophen and its internal standard from other components (matrix) and to form a single spot/zone containing them at the solvent front position (after the final stage of the thin-layer chromatogram development). The location of the analytes and internal standard in the solvent front zone allows their easy extraction followed by quantitation by HPLC. The exctraction procedure of the solute/s and internal standard can proceed from whole solute frontal zone or its part without lowering in accuracy of quantitative analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Purification of Carbon Nanotubes: Alternative Methods

NASA Technical Reports Server (NTRS)

Files, Bradley; Scott, Carl; Gorelik, Olga; Nikolaev, Pasha; Hulse, Lou; Arepalli, Sivaram

2000-01-01

Traditional carbon nanotube purification process involves nitric acid refluxing and cross flow filtration using surfactant TritonX. This is believed to result in damage to nanotubes and surfactant residue on nanotube surface. Alternative purification procedures involving solvent extraction, thermal zone refining and nitric acid refiuxing are used in the current study. The effect of duration and type of solvent to dissolve impurities including fullerenes and P ACs (polyaromatic compounds) are monitored by nuclear magnetic reasonance, high performance liquid chromatography, and thermogravimetric analysis. Thermal zone refining yielded sample areas rich in nanotubes as seen by scanning electric microscopy. Refluxing in boiling nitric acid seem to improve the nanotube content. Different procedural steps are needed to purify samples produced by laser process compared to arc process. These alternative methods of nanotube purification will be presented along with results from supporting analytical techniques.

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.

Comparison of the atmospheric- and reduced-pressure HS-SPME strategies for analysis of residual solvents in commercial antibiotics using a steel fiber coated with a multiwalled carbon nanotube/polyaniline nanocomposite.

PubMed

Ghiasvand, Ali Reza; Nouriasl, Kolsoum; Yazdankhah, Fatemeh

2018-01-01

A low-cost, sensitive and reliable reduced-pressure headspace solid-phase microextraction (HS-SPME) setup was developed and evaluated for direct extraction of residual solvents in commercial antibiotics, followed by determination by gas chromatography with flame ionization detection (GC-FID). A stainless steel narrow wire was made porous and adhesive by platinization by a modified electrophoretic deposition method and coated with a polyaniline/multiwalled carbon nanotube nanocomposite. All experimental variables affecting the extraction efficiency were investigated for both atmospheric-pressure and reduced-pressure conditions. Comparison of the optimal experimental conditions and the results demonstrated that the reduced-pressure strategy leads to a remarkable increase in the extraction efficiency and reduction of the extraction time and temperature (10 min, 25 °Ϲ vs 20 min, 40 °Ϲ). Additionally, the reduced-pressure strategy showed better analytical performances compared with those obtained by the conventional HS-SPME-GC-FID method. Limit of detections, linear dynamic ranges, and relative standard deviations of the reduced-pressure HS-SPME procedure for benzene, toluene, ethylbenzene, and xylene (BTEX) in injectable solid drugs were obtained over the ranges of 20-100 pg g -1 , 0.02-40 μg g -1 , and 2.8-10.2%, respectively. The procedure developed was successful for the analysis of BTEX in commercial containers of penicillin, ampicillin, ceftriaxone, and cefazolin. Graphical abstract Schematic representation of the developed RP-HS-SPME setup.

Determination of amantadine in biological fluids using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection.

PubMed

Farajzadeh, Mir Ali; Nouri, Nina; Alizadeh Nabil, Ali Akbar

2013-12-01

A one-step derivatization and microextraction technique for the determination of amantadine in the human plasma and urine samples is presented. An appropriate mixture of methanol (disperser solvent), 1,2-dibromoethane (extraction solvent), and butylchloroformate (derivatization agent) is rapidly injected into samples. After centrifuging, the sedimented phase is analyzed by gas chromatography-flame ionization detection (GC-FID). The kind of extraction and disperser solvents and their volumes, amount of derivatization agent and reaction/extraction time which are effective in derivatization/dispersive liquid-liquid microextraction (DLLME) procedure are optimized. Under the optimal conditions, the enrichment factor (EF) of the target analyte was obtained to be 408 and 420, and limit of detection (LOD) 4.2 and 2.7ngmL(-1), in plasma and urine respectively. The linear range is 14-5000 and 8.7-5000ng/mL for plasma and urine, respectively (squared correlation coefficient≥0.990). The relative recoveries obtained for the spiked plasma and urine samples are between 72% and 93%. Moreover, the inter- and intra-day precisions are acceptable at all spiked concentrations (relative standard deviation <7%). Finally the method was successfully applied to determine amantadine in biological samples. Copyright © 2013 Elsevier B.V. All rights reserved.

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

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.

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.

Sequential extraction protocol for organic matter from soils and sediments using high resolution mass spectrometry

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

Tfaily, Malak M.; Chu, Rosalie K.; Toyoda, Jason

A vast number of organic compounds are present in soil organic matter (SOM) and play an important role in the terrestrial carbon cycle, facilitate interactions between organisms, and represent a sink for atmospheric CO2. The diversity of different SOM compounds and their molecular characteristics is a function of the organic source material and biogeochemical history. By understanding how SOM composition changes with sources and the processes by which it is biogeochemically altered in different terrestrial ecosystems, it may be possible to predict nutrient and carbon cycling, response to system perturbations, and impact of climate change will have on SOM composition.more » In this study, a sequential chemical extraction procedure was developed to reveal the diversity of organic matter (OM) in different ecosystems and was compared to the previously published protocol using parallel solvent extraction (PSE). We compared six extraction methods using three sample types, peat soil, spruce forest soil and river sediment, so as to select the best method for extracting a representative fraction of organic matter from soils and sediments from a wide range of ecosystems. We estimated the extraction yield of dissolved organic carbon (DOC) by total organic carbon analysis, and measured the composition of extracted OM using high resolution mass spectrometry. This study showed that OM composition depends primarily on soil and sediment characteristics. Two sequential extraction protocols, progressing from polar to non-polar solvents, were found to provide the highest number and diversity of organic compounds extracted from the soil and sediments. Water (H2O) is the first solvent used for both protocols followed by either co-extraction with methanol-chloroform (MeOH-CHCl3) mixture, or acetonitrile (ACN) and CHCl3 sequentially. The sequential extraction protocol developed in this study offers improved sensitivity, and requires less sample compared to the PSE workflow where a new sample is used for each solvent type. Furthermore, a comparison of SOM composition from the different sample types revealed that our sequential protocol allows for ecosystem comparisons based on the diversity of compounds present, which in turn could provide new insights about source and processing of organic compounds in different soil and sediment types.« less

Sequential extraction protocol for organic matter from soils and sediments using high resolution mass spectrometry.

PubMed

Tfaily, Malak M; Chu, Rosalie K; Toyoda, Jason; Tolić, Nikola; Robinson, Errol W; Paša-Tolić, Ljiljana; Hess, Nancy J

2017-06-15

A vast number of organic compounds are present in soil organic matter (SOM) and play an important role in the terrestrial carbon cycle, facilitate interactions between organisms, and represent a sink for atmospheric CO 2 . The diversity of different SOM compounds and their molecular characteristics is a function of the organic source material and biogeochemical history. By understanding how SOM composition changes with sources and the processes by which it is biogeochemically altered in different terrestrial ecosystems, it may be possible to predict nutrient and carbon cycling, response to system perturbations, and impact of climate change will have on SOM composition. In this study, a sequential chemical extraction procedure was developed to reveal the diversity of organic matter (OM) in different ecosystems and was compared to the previously published protocol using parallel solvent extraction (PSE). We compared six extraction methods using three sample types, peat soil, spruce forest soil and river sediment, so as to select the best method for extracting a representative fraction of organic matter from soils and sediments from a wide range of ecosystems. We estimated the extraction yield of dissolved organic carbon (DOC) by total organic carbon analysis, and measured the composition of extracted OM using high resolution mass spectrometry. This study showed that OM composition depends primarily on soil and sediment characteristics. Two sequential extraction protocols, progressing from polar to non-polar solvents, were found to provide the highest number and diversity of organic compounds extracted from the soil and sediments. Water (H 2 O) is the first solvent used for both protocols followed by either co-extraction with methanol-chloroform (MeOH-CHCl 3 ) mixture, or acetonitrile (ACN) and CHCl 3 sequentially. The sequential extraction protocol developed in this study offers improved sensitivity, and requires less sample compared to the PSE workflow where a new sample is used for each solvent type. Furthermore, a comparison of SOM composition from the different sample types revealed that our sequential protocol allows for ecosystem comparisons based on the diversity of compounds present, which in turn could provide new insights about source and processing of organic compounds in different soil and sediment types. Copyright © 2017 Elsevier B.V. All rights reserved.

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

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.

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

Development and practical application of accelerated solvent extraction for the isolation of cocaine/crack biomarkers in meconium samples.

PubMed

Mantovani, Cínthia de Carvalho; Lima, Marcela Bittar; Oliveira, Carolina Dizioli Rodrigues de; Menck, Rafael de Almeida; Diniz, Edna Maria de Albuquerque; Yonamine, Mauricio

2014-04-15

A method using accelerated solvent extraction (ASE) for the isolation of cocaine/crack biomarkers in meconium samples, followed by solid phase extraction (SPE) and the simultaneous quantification by gas chromatography-mass spectrometry (GC-MS) was developed and validated. Initially, meconium samples were submitted to an ASE procedure, which was followed by SPE with Bond Elut Certify I cartridges. The analytes were derivatizated with PFP/PFPA and analyzed by GC-MS. The limits of detection (LOD) were between 11 and 17ng/g for all analytes. The limits of quantification (LOQ) were 30ng/g for anhydroecgonine methyl ester, and 20ng/g for cocaine, benzoylecgonine, ecgonine methyl ester and cocaethylene. Linearity ranged from the LOQ to 1500ng/g for all analytes, with a coefficients of determination greater than 0.991, except for m-hydroxybenzoylecgonine, which was only qualitatively detected. Precision and accuracy were evaluated at three concentration levels. For all analytes, inter-assay precision ranged from 3.2 to 18.1%, and intra-assay precision did not exceed 12.7%. The accuracy results were between 84.5 and 114.2% and the average recovery ranged from 17 to 84%. The method was applied to 342 meconium samples randomly collected in the University Hospital-University of São Paulo (HU-USP), Brazil. Cocaine biomarkers were detected in 19 samples, which represent 5.6% of exposure prevalence. Significantly lower birth weight, length and head circumference were found for the exposed newborns compared with the non-exposed group. This is the first report in which ASE was used as a sample preparation technique to extract cocaine biomarkers from a complex biological matrix such as meconium samples. The advantages of the developed method are the smaller demand for organic solvents and the minor sample handling, which allows a faster and accurate procedure, appropriate to confirm fetal exposure to cocaine/crack. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

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...

Atomic-absorption determination of mercury in geological materials by flame and carbon-rod atomisation after solvent extraction and using co-extracted silver as a matrix modifier

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.

1983-01-01

Based on modifications and expansion of the original Tindall's solvent extraction flame atomic-absorption procedure, an atomic-absorption spectrophotometric method has been developed for the determination of mercury in geological materials. The sample is digested with nitric and hydrochloric acids in a boiling water-bath. The solution is made ammoniacal and potassium iodide and silver nitrate are added. The mercury is extracted into isobutyl methyl ketone as the tetraiodomercurate(ll). Added silver is co-extracted with mercury and serves as a matrix modifier in the carbon-rod atomiser. The mercury in the isobutyl methyl ketone extract may be determined by either the flame- or the carbon-rod atomisation method, depending on the concentration level. The limits of determination are 0.05-10 p.p.m. of mercury for the carbon-rod atomisation and 1 -200 p.p.m. of mercury for the flame atomisation. Mercury values for reference samples obtained by replicate analyses are in good agreement with those reported by other workers, with relative standard deviations ranging from 2.3 to 0.9%. Recoveries of mercury spiked at two levels were 93-106%. Major and trace elements commonly found in geological materials do not interfere.

A rapid and efficient DNA extraction protocol from fresh and frozen human blood samples.

PubMed

Guha, Pokhraj; Das, Avishek; Dutta, Somit; Chaudhuri, Tapas Kumar

2018-01-01

Different methods available for extraction of human genomic DNA suffer from one or more drawbacks including low yield, compromised quality, cost, time consumption, use of toxic organic solvents, and many more. Herein, we aimed to develop a method to extract DNA from 500 μL of fresh or frozen human blood. Five hundred microliters of fresh and frozen human blood samples were used for standardization of the extraction procedure. Absorbance at 260 and 280 nm, respectively, (A 260 /A 280 ) were estimated to check the quality and quantity of the extracted DNA sample. Qualitative assessment of the extracted DNA was checked by Polymerase Chain reaction and double digestion of the DNA sample. Our protocol resulted in average yield of 22±2.97 μg and 20.5±3.97 μg from 500 μL of fresh and frozen blood, respectively, which were comparable to many reference protocols and kits. Besides yielding bulk amount of DNA, our protocol is rapid, economical, and avoids toxic organic solvents such as Phenol. Due to unaffected quality, the DNA is suitable for downstream applications. The protocol may also be useful for pursuing basic molecular researches in laboratories having limited funds. © 2017 Wiley Periodicals, Inc.

Ultrasound assisted dialysis of semi-permeable membrane devices for the simultaneous analysis of a wide number of persistent organic pollutants.

PubMed

Bustamante, Julen; Navarro, Patricia; Arana, Gorka; de Diego, Alberto; Madariaga, Juan Manuel

2013-09-30

A new procedure based on ultrasound assisted dialysis (UAD) for the simultaneous and quantitative extraction of a wide number of persistent organic pollutants (POPs) such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) or some other organochlorinated pesticides (OCPs) contained in semi-permeable membrane devices (SPMDs) has been developed. This extraction technique combines the advantages of the organic solvent dialysis (OSD) and the speed of the ultrasound assisted extraction. The extraction was performed in an ultrasound bath for 32 min placing the SPMD in a glass flask covered with 80 mL of hexane. This set-up is able to extract simultaneously up to 8 samples. The proposed method entails good repeatabilities (RSD 2-13%) and recoveries (around 100% for almost every analyte). Limits of detection were at ng SPMD(-1) level and enough for the determination of the target analytes in a slightly polluted aquatic environment, as it was tested by successfully comparing the OSD to the proposed methodology. Therefore, the results obtained show that the UAD can be a good alternative for the extraction of POPs in SPMDs as it requires short extraction times and solvent volumes, and provides a cleaner extract for the subsequent clean-up step. Moreover, it fits better than the OSD to the general requirements of Green Chemistry. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Sample preparation and data interpretation procedures for the examination of xenobiotic compounds in skin by indirect imaging MALDI-MS

NASA Astrophysics Data System (ADS)

Prideaux, Brendan; Atkinson, Sally J.; Carolan, Vikki A.; Morton, Jacqueline; Clench, Malcolm R.

2007-02-01

Aspects of the indirect examination of xenobiotic distribution on the surface of and within skin sections by imaging matrix assisted laser desorption ionisation mass spectrometry (MALDI-MS) have been examined. A solvent assisted blotting technique previously developed for the examination of the absorption of agrochemicals into leaves has been examined for the analysis of the distribution of hydrocortisone on the surface of skin. It was found that by careful control of the extraction and blotting procedure an 80-fold sensitivity improvement could by obtained over dry blotting with only 10% lateral diffusion of the image. However, in contrast it was found that the use of a hydrophobic blotting membrane was more suitable for the examination of the transdermal absorption of the pesticide chlorpyrifos. The potential of incorporating a derivatisation step into the solvent assisted blotting procedure was investigated by blotting isocyanate treated skin onto a methanol soaked blotting membrane. This served the dual purpose of derivatising the isocyanate to a stable substituted urea derivative and extracting it from the skin. Preliminary data indicate that this approach may have some merit for field sampling for such compound and clearly derivatisation also offers the potential for sensitivity enhancements. Finally, the use of principal components analysis with an ion species specific normalisation procedure is proposed to identify regions of drug treated skin where the ion abundance of the compound of interest is low.

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).

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.

Comparison of methods for extraction of ethyl carbamate from alcoholic beverages in gas chromatography/mass spectrometry analysis.

PubMed

Mirzoian, Armen; Mabud, Abdul

2006-01-01

A procedure to analyze ethyl carbamate (EC) by gas chromatography/mass spectrometry was optimized and validated. Deuterated EC (d5-EC) was added to the samples as an internal standard followed by extraction with polystyrene crosslinked polystyrene cartridges using minimal volumes of ethyl acetate. The EC response was measured in selective ion monitoring (SIM) mode and found to be linear in the range between the limit of quantitation (10 micro/L) and 1000 microg/L. EC recoveries varied from 92 to 112%, with the average value of 100 +/- 8%. The procedure compared well (r2 = 0.9970) with the existing AOAC Official Method with the added benefits of minimal solvent usage and reduced matrix interferences.

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.

Analysis of malondialdehyde in human plasma samples through derivatization with 2,4-dinitrophenylhydrazine by ultrasound-assisted dispersive liquid-liquid microextraction-GC-FID approach.

PubMed

Malaei, Reyhane; Ramezani, Amir M; Absalan, Ghodratollah

2018-05-04

A sensitive and reliable ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) procedure was developed and validated for extraction and analysis of malondialdehyde (MDA) as an important lipids-peroxidation biomarker in human plasma. In this methodology, to achieve an applicable extraction procedure, the whole optimization processes were performed in human plasma. To convert MDA into readily extractable species, it was derivatized to hydrazone structure-base by 2,4-dinitrophenylhydrazine (DNPH) at 40 °C within 60 min. Influences of experimental variables on the extraction process including type and volume of extraction and disperser solvents, amount of derivatization agent, temperature, pH, ionic strength, sonication and centrifugation times were evaluated. Under the optimal experimental conditions, the enhancement factor and extraction recovery were 79.8 and 95.8%, respectively. The analytical signal linearly (R 2  = 0.9988) responded over a concentration range of 5.00-4000 ng mL -1 with a limit of detection of 0.75 ng mL -1 (S/N = 3) in the plasma sample. To validate the developed procedure, the recommend guidelines of Food and Drug Administration for bioanalytical analysis have been employed. Copyright © 2018. Published by Elsevier B.V.

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.

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.

Simultaneous derivatization and lighter-than-water air-assisted liquid-liquid microextraction using a homemade device for the extraction and preconcentration of some parabens in different samples.

PubMed

Farajzadeh, Mir Ali; Aghdam, Mehri Bakhshizadeh; Mogaddam, Mohammad Reza Afshar; Nabil, Ali Akbar Alizadeh

2018-06-06

Simultaneous derivatization and air-assisted liquid-liquid microextraction using an organic solvent lighter than water has been developed for the extraction of some parabens in different samples with the aid of a newly designed device for collecting the extractant. For this purpose, the sample solution is transferred into a glass test tube and a few microliters of acetic anhydride (as a derivatization agent) and p-xylene (as an extraction solvent) are added to the solution. After performing the procedure, the homemade device consists of an inverse funnel with a capillary tube placed into the tube. In this step, the collected extraction solvent and a part of the aqueous solution are transferred into the device and the organic phase indwells in the capillary tube of the device. Under the optimal conditions, limits of detection and quantification for the analytes were obtained in the ranges of 0.90-2.7 and 3.0-6.1 ng mL -1 , respectively. The enrichment and enhancement factors were in the ranges of 370-430 and 489-660, respectively. The method precision, expressed as the relative standard deviation, was within the ranges of 4-6% (n = 6) and 4-9% (n = 4) for intra- and inter-day precisions, respectively. The proposed method was successfully used for the determination of methyl-, ethyl-, and propyl parabens in cosmetic, hygiene, and food samples, and personal care products. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Valid internal standard technique for arson detection based on gas chromatography-mass spectrometry.

PubMed

Salgueiro, Pedro A S; Borges, Carlos M F; Bettencourt da Silva, Ricardo J N

2012-09-28

The most popular procedures for the detection of residues of accelerants in fire debris are the ones published by the American Society for Testing and Materials (ASTM E1412-07 and E1618-10). The most critical stages of these tests are the conservation of fire debris from the sampling to the laboratory, the extraction of residues of accelerants from the debris to the activated charcoal strips (ACS) and from those to the final solvent, as well as the analysis of sample extract by gas chromatography-mass spectrometry (GC-MS) and the interpretation of the instrumental signal. This work proposes a strategy for checking the quality of the sample conservation, the accelerant residues transference to final solvent and GC-MS analysis, using internal standard additions. It is used internal standards ranging from a highly volatile compound for checking debris conservation to low volatile compound for checking GC-MS repeatability. The developed quality control (QC) parameters are not affected by GC-MS sensitivity variation and, specifically, the GC-MS performance control is not affected by ACS adsorption saturation that may mask test performance deviations. The proposed QC procedure proved to be adequate to check GC-MS repeatability, ACS extraction and sample conservation since: (1) standard additions are affected by negligible uncertainty and (2) observed dispersion of QC parameters are fit for its intended use. Copyright © 2012 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...

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

PubMed

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

2005-07-13

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

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...

A new high-speed hollow fiber based liquid phase microextraction method using volatile organic solvent for determination of aromatic amines in environmental water samples prior to high-performance liquid chromatography.

PubMed

Sarafraz-Yazdi, A; Mofazzeli, F; Es'haghi, Z

2009-07-15

A new and fast hollow fiber based liquid phase microextraction (HF-LPME) method using volatile organic solvents coupled with high-performance liquid chromatography (HPLC) was developed for determination of aromatic amines in the environmental water samples. Analytes including 3-nitroaniline, 3-chloroaniline and 4-bromoaniline were extracted from 6 mL basic aqueous sample solution (donor phase, NaOH 1 mol L(-1)) into the thin film of organic solvent that surrounded and impregnated the pores of the polypropylene hollow fiber wall (toluene, 20 microL), then back-extracted into the 6 mL acidified aqueous solution (acceptor phase, HCl 0.5 mol L(-1)) in the lumen of the two-end sealed hollow fiber. After the extraction, 5 microL of the acceptor phase was withdrawn into the syringe and injected directly into the HPLC system for the analysis. The parameters influencing the extraction efficiency including the kind of organic solvent and its volume, composition of donor and acceptor phases and the volume ratio between them, extraction time, stirring rate, salt addition and the effect of the analyte complexation with 18-crown-6 ether were investigated and optimized. Under the optimal conditions (donor phase: 6 mL of 1 mol L(-1) NaOH with 10% NaCl; organic phase: 20 microL of toluene; acceptor phase: 6 microL of 0.5 mol L(-1) HCl and 600 mmol L(-1) 18-crown-6 ether; pre-extraction and back-extraction times: 75 s and 10 min, respectively; stirring rate: 800 rpm), the obtained EFs were between 259 and 674, dynamic linear ranges were 0.1-1000 microg L(-1) (R>0.9991), and also the limits of detection were in the range of 0.01-0.1 micro gL(-1). The proposed procedure worked very well for real environmental water samples with microgram per liter level of the analytes, and good relative recoveries (91-102%) were obtained for the spiked sample solutions.

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.

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.

Decontamination of soil containing POPs by the combined action of solid Fenton-like reagents and microwaves.

PubMed

Cravotto, Giancarlo; Di Carlo, Stefano; Ondruschka, Bernd; Tumiatti, Vander; Roggero, Carlo Maria

2007-10-01

The effect on halogenated aromatics of solid, non-toxic oxidants such as sodium percarbonate and the urea/hydrogen peroxide complex (Fenton-like reagents) was investigated. A microwaves-assisted, solvent-free method for soil decontamination is presented. It marks a considerable advance in the search of more efficient, environment-friendly procedures for the degradative oxidation of persistent organic pollutants. Residual pollutants in treated soil samples were determined by GC/MS analysis after solvent extraction or direct thermal desorption. Results showed that 4-chloronaphthol, 2,4-dichlorophenoxyacetic acid and p-nonylphenol had been degraded completely, 2,4-dibromophenol to a large extent.

High strength air-dried aerogels

DOEpatents

Coronado, Paul R.; Satcher, Jr., Joe H.

2012-11-06

A method for the preparation of high strength air-dried organic aerogels. The method involves the sol-gel polymerization of organic gel precursors, such as resorcinol with formaldehyde (RF) in aqueous solvents with R/C ratios greater than about 1000 and R/F ratios less than about 1:2.1. Using a procedure analogous to the preparation of resorcinol-formaldehyde (RF) aerogels, this approach generates wet gels that can be air dried at ambient temperatures and pressures. The method significantly reduces the time and/or energy required to produce a dried aerogel compared to conventional methods using either supercritical solvent extraction. The air dried gel exhibits typically less than 5% shrinkage.

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.

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.

Fast and accurate determination of arsenobetaine in fish tissues using accelerated solvent extraction and HPLC-ICP-MS determination.

PubMed

Wahlen, Raimund

2004-04-01

A high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) method has been developed for the fast and accurate analysis of arsenobetaine (AsB) in fish samples extracted by accelerated solvent extraction. The combined extraction and analysis approach is validated using certified reference materials for AsB in fish and during a European intercomparison exercise with a blind sample. Up to six species of arsenic (As) can be separated and quantitated in the extracts within a 10-min isocratic elution. The method is optimized so as to minimize time-consuming sample preparation steps and allow for automated extraction and analysis of large sample batches. A comparison of standard addition and external calibration show no significant difference in the results obtained, which indicates that the LC-ICP-MS method is not influenced by severe matrix effects. The extraction procedure can process up to 24 samples in an automated manner, yet the robustness of the developed HPLC-ICP-MS approach is highlighted by the capability to run more than 50 injections per sequence, which equates to a total run-time of more than 12 h. The method can therefore be used to rapidly and accurately assess the proportion of nontoxic AsB in fish samples with high total As content during toxicological screening studies.

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/.

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

PubMed

Mansour, Fotouh R; Danielson, Neil D

2017-08-01

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

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

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

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

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

Extraction of 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.

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.

Total flavonoids content in the raw material and aqueous extractives from Bauhinia monandra Kurz (Caesalpiniaceae).

PubMed

Fernandes, Ana Josane Dantas; Ferreira, Magda Rhayanny Assunção; Randau, Karina Perrelli; de Souza, Tatiane Pereira; Soares, Luiz Alberto Lira

2012-01-01

The aim of this work was to evaluate the spectrophotometric methodology for determining the total flavonoid content (TFC) in herbal drug and derived products from Bauhinia monandra Kurz. Several analytical parameters from this method grounded on the complex formed between flavonoids and AlCl₃ were evaluated such as herbal amount (0.25 to 1.25 g); solvent composition (ethanol 40 to 80%, v/v); as well as the reaction time and AlCl₃ concentration (2 to 9%, w/v). The method was adjusted to aqueous extractives and its performance studied through precision, linearity and preliminary robustness. The results showed an important dependence of the method response from reaction time, AlCl₃ concentration, sample amount, and solvent mixture. After choosing the optimized condition, the method was applied for the matrixes (herbal material and extractives), showing precision lower than 5% (for both parameters repeatability and intermediate precision), coefficient of determination higher than 0.99, and no important influence could be observed for slight variations from wavelength or AlCl₃ concentration. Thus, it could be concluded that the evaluated analytical procedure was suitable to quantify the total flavonoid content in raw material and aqueous extractives from leaves of B. monandra.

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.

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)

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.

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

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

PubMed

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

2014-06-01

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

Gas chromatography-mass spectrometry and high-performance liquid chromatography-diode array detection for dating of paper ink.

PubMed

Díaz-Santana, Oscar; Vega-Moreno, Daura; Conde-Hardisson, Francisco

2017-09-15

An extraction and determination method is shown for the analysis of dyes and solvents present in two types of ballpoint pen inks that are deposited onto paper. Ink extracts are analysed using a combination of gas chromatography with mass spectrometry (GC-MS), and high-pressure liquid chromatography with photodiode array detection (HPLC-DAD), within a single sample extraction procedure. Seventeen solvents and thirteen dyes contained in two Montblanc ® inks (black and blue) were monitored for 45 months at monthly intervals, in order to determine variations in the concentrations of the compounds over time. We also studied the relative variations between different compounds and the generation of degradation products such as phenol. The concentration data obtained from these compounds during their exposure have been analysed and a multiple regression model is developed for each ink type that allows an estimate of the exposure time of the ink on paper with a maximum error of between 4 and 7 months. Copyright © 2017 Elsevier B.V. All rights reserved.

Investigation of six bioactive anthraquinones in slimming tea by accelerated solvent extraction and high performance capillary electrophoresis with diode-array detection.

PubMed

Wang, Ning; Su, Ming; Liang, Shuxuan; Sun, Hanwen

2016-05-15

A rapid and effective method for effective separation and rapid simultaneous determination of six bioactive anthraquinones by capillary zone electrophoresis was developed. An accelerated solvent extraction procedure was used for the extraction of anthraquinones from slimming tea. Under the optimized conditions, the effective separation of six anthraquinones was achieved within 8 min. Good linearity was achieved, with a correlation coefficient (r) of ⩾ 0.999. The limit of detection ranged from 0.33 to 1.40 μg mL(-1). The intra- and inter-day relative standard deviation (RSD) of the six analytes was in the range of 2.3-3.9% and 3.2-4.9%, respectively. The average recovery of the six analytes from real tea samples was in the range of 86.15-98.30% with the RSD of 1.04-4.99%. The developed and validated method has speediness, high sensitivity, recovery and precision, and can be applied for the quality control of slimming tea. Copyright © 2015 Elsevier Ltd. All rights reserved.

Deodorization of Arthrospira platensis biomass for further scale-up food applications.

PubMed

Cuellar-Bermúdez, Sara P; Barba-Davila, Bertha; Serna-Saldivar, Sergio O; Parra-Saldivar, Roberto; Rodriguez-Rodriguez, José; Morales-Davila, Sandra; Goiris, Koen; Muylaert, Koenraad; Chuck-Hernández, Cristina

2017-12-01

Given the importance of A. platensis as a potential food protein source, we describe an affordable deodorization process that does not significantly affect the nutritional value of algae biomass. Ethanol, acetone or hexane were used to deodorize algae biomass and then to identify the profile of volatile compounds associated with its distinctive odor. Sensorial characteristics were improved in the biomass cake after the proposed solvent extraction. Panelists identified the ethanolic extract with the most pronounced algae-related odor. Gas chromatography-mass spectrometry analysis showed that a mixture of 20 different compounds derived from fatty acids and amino acids contributed to the characteristic smell of A. platensis biomass. The results of the present study show that the ethanol solvent-free A. platensis biomass contained > 600 g kg -1 protein, < 10 g kg -1  crude fat and > 65% in vitro protein digestibility, similar to the original biomass. The Fourier transform infrared spectroscopy secondary protein structure was comparable among samples, indicating that the only change after ethanol extraction was a reduction of the algae smell. The various extraction procedures investigated in the present study were effective in deodorizing the algae biomass. The most effective protocol was the removal of odoriferous compounds with ethanol. This particular procedure yielded an algae biomass with an improved sensorial traits. The results of the present study should help with the identification of odoriferous compounds derived from fatty acids, pigments and proteins associated with A. platensis. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

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.

Dispersive liquid-liquid microextraction for the determination of nitrophenols in soils by microvial insert large volume injection-gas chromatography-mass spectrometry.

PubMed

Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

2016-07-22

A rapid and sensitive procedure for the determination of six NPs in soils by gas chromatography and mass spectrometry (GC-MS) is proposed. Ultrasound assisted extraction (UAE) is used for NP extraction from soil matrices to an organic solvent, while the environmentally friendly technique dispersive liquid-liquid microextraction (DLLME) is used for the preconcentration of the resulting UAE extracts. NPs were derivatized by applying an "in-situ" acetylation procedure, before being injected into the GC-MS system using microvial insert large volume injection (LVI). Several parameters affecting UAE, DLLME, derivatization and injection steps were investigated. The optimized procedure provided recoveries of 86-111% from spiked samples. Precision values of the procedure (expressed as relative standard deviation, RSD) lower than 12%, and limits of quantification ranging from 1.3 to 2.6ngg(-1), depending on the compound, were obtained. Twenty soil samples, obtained from military, industrial and agricultural areas, were analyzed by the proposed method. Two of the analytes were quantified in two of the samples obtained from industrial areas, at concentrations in the 4.8-9.6ngg(-1) range. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction.

PubMed

Pena, M Teresa; Pensado, Luis; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

2007-04-01

A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 microg kg(-1) dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials.

Extraction-spectrophotometric determination of tris(2-chloroethyl)amine using phthaleins.

PubMed

Rozsypal, Tomas; Halamek, Emil

2017-06-01

Procedures for the extraction-spectrophotometric determination of tris(2-chloroethyl)amine, an alkylating agent known as a drug as well as a chemical warfare agent (nitrogen mustard HN-3), with 7 acid-base indicators of a triphenylmethane lactone type, phthaleins, were developed. Representatives of phthaleins without an oxygen bridge (thymolphthalein, o-cresolphthalein, naphtholphthalein) and with an oxygen bridge (fluorescein, 2',7'-dichlorofluorescein, eosin B and eosin Y) were used. The methods were based on the formation of ion pair complexes. Chloroform was used as a non-polar solvent for an extraction. The conditions to determine were optimized for the optimal pH of the buffer and the concentration of a phthalein as a reagent. The dependence on the reaction time in a water phase and the stoichiometry of extraction products were studied. The detection limits and the limits of the determination of separate procedures and conditional extraction constants were determined. Comparison with the spectrophotometric method of the group determination of alkyl halides and acyl halides using alkaline ethanol-water solution of thymolphthalein, the so-called T-135 agent, was conducted. While studying the selectivity, the possible interference of bis(2-chloroethyl)sulphide and 3 nitrogen mustards in the proposed procedures were verified. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

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.

Validation of an Analytical Method for Determination of 13 priority polycyclic aromatic hydrocarbons in mineral water using dispersive liquid-liquid microextraction and GC-MS

PubMed Central

Sadeghi, Ramezan; Kobarfard, Farzad; Yazdanpanah, Hassan; Eslamizad, Samira; Bayat, Mitra

2016-01-01

Dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography–mass spectrometry (GC–MS) was used for the extraction and determination of 13 polycyclic aromatic hydrocarbons (PAHs) in mineral water samples. In this procedure, the suitable combination of extraction solvent (500 µL chloroform) and disperser solvent (1000 µL acetone) were quickly injected into the water sample (10.00 mL) by Hamilton syringe. After centrifugation, 500 µL of the lower organic phase was dried under a gentle stream of nitrogen, re-dissolved in chloroform and injected into GC-MS. Chloroform and acetone were found to be the best extraction and disperser solvent, respectively. Validation of the method was performed using spiked calibration curves. The enrichment factor ranged from 93 to 129 and the recovery ranged from 71 to 90%. The linear ranges for all the PAHs were 0.10-2.80 ngmL-1. The relative standard deviations (RSDs) of PAHs in water by using anthracene-d10 as internal standard, were in the range of 4-11% for most of the analytes (n = 3). Limit of detection (LOD) for different PAHs were between 0.03 and 0.1 ngmL-1. The method was successfully applied for the analysis of PAHs in mineral water samples collected from Tehran. PMID:27610156

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.

Simultaneous determination of phenolic compounds in Equisetum palustre L. by ultra high performance liquid chromatography with tandem mass spectrometry combined with matrix solid-phase dispersion extraction.

PubMed

Wei, Zuofu; Pan, Youzhi; Li, Lu; Huang, Yuyang; Qi, Xiaolin; Luo, Meng; Zu, Yuangang; Fu, Yujie

2014-11-01

A method based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with tandem mass spectrometry is presented for the extraction and determination of phenolic compounds in Equisetum palustre. This method combines the high efficiency of matrix solid-phase dispersion extraction and the rapidity, sensitivity, and accuracy of ultra high performance liquid chromatography with tandem mass spectrometry. The influential parameters of the matrix solid-phase dispersion extraction were investigated and optimized. The optimized conditions were as follows: silica gel was selected as dispersing sorbent, the ratio of silica gel to sample was selected to be 2:1 (400/200 mg), and 8 mL of 80% methanol was used as elution solvent. Furthermore, a fast and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the determination of nine phenolic compounds in E. palustre. This method was carried out within <6 min, and exhibited satisfactory linearity, precision, and recovery. Compared with ultrasound-assisted extraction, the proposed matrix solid-phase dispersion procedure possessed higher extraction efficiency, and was more convenient and time saving with reduced requirements on sample and solvent amounts. All these results suggest that the developed method represents an excellent alternative for the extraction and determination of active components in plant matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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).

Valorization of solid wastes from chestnut industry processing: Extraction and optimization of polyphenols, tannins and ellagitannins and its potential for adhesives, cosmetic and pharmaceutical industry.

PubMed

Aires, Alfredo; Carvalho, Rosa; Saavedra, Maria José

2016-02-01

The aim of the current study was to evaluate the potential of chestnut peels to produce pomaces enhanced with tannins to be used in the formulations of wood adhesives, leather tanning or as natural antioxidants in food, cosmetic and pharmaceutical industry. An analytical procedure was planned as 2 factorial design to analyze the influence of solvent (water, Na2SO3 and NaOH at different concentrations of 1, 2, 4, and 8% in water) and extraction time (30, 60, and 120, 240, 480 and 960min) on extraction yield, pH, Stiasny index, and tannins. HPLC-diode array detector equipped with an ionization mass spectrophotometer was used to assess the polyphenol composition. Our results showed that both extraction properties and phytochemicals were significantly affected (P<0.001) by all independent factors. The main tannins identified were the hydrolyzable gallic acid, vescalagin castalagin and ellagic acid, and the condensed epigallocatechin, catechin and epicatechin. The solvent 1% Na2SO3 was more effective to extract the condensed tannins whilst hydrolyzable tannins were extracted efficiently by 1% NaOH. The multivariable analysis and the Pearson's correlation coefficients showed a direct association between Stiasny number and the average levels of condensed tannins. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

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.

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.

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

PubMed

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

2016-02-04

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

Quantitation of polymethoxylated flavones in orange juice by high-performance liquid chromatography.

PubMed

Rouseff, R L; Ting, S V

1979-08-01

A quantitative high-performance liquid chromatographic (HPLC) procedure for the determination of the five major polymethoxylated flavones (PMFs) in orange juice has been developed. It employs a unique ternary solvent system with coupled UV-fluorescence detection. The dual detectors were employed to determine the presence of interfering substances and served as a cross check on quantitation. Stop flow UV and fluorescence scanning was used to identify peaks and determine the presence of impurities. Although all five citrus PMFs fluoresce, some HPLC fluorescence peaks were too small to be of much practical use. All five citrus PMFs could be quantitated satisfactorily with the fixed wavelength UV (313 nm) detector. The HPLC procedure has been used to evaluate each step in the preparation. The optimum extracting solvent was selected and one time consuming step was eliminated, as it was found to be unnecessary. HPLC values for nobiletin and sinensetin are in good agreement with the thin-layer chromatographic (TLC) values in the literature. HPLC values for the other three flavones were considerably lower than those reported in the literature. The HPLC procedure is considerably faster than the TLC procedure with equal or superior precision and accuracy.

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.

Revisiting chlorophyll extraction methods in biological soil crusts - methodology for determination of chlorophyll a and chlorophyll a + b as compared to previous methods

NASA Astrophysics Data System (ADS)

Caesar, Jennifer; Tamm, Alexandra; Ruckteschler, Nina; Lena Leifke, Anna; Weber, Bettina

2018-03-01

Chlorophyll concentrations of biological soil crust (biocrust) samples are commonly determined to quantify the relevance of photosynthetically active organisms within these surface soil communities. Whereas chlorophyll extraction methods for freshwater algae and leaf tissues of vascular plants are well established, there is still some uncertainty regarding the optimal extraction method for biocrusts, where organism composition is highly variable and samples comprise major amounts of soil. In this study we analyzed the efficiency of two different chlorophyll extraction solvents, the effect of grinding the soil samples prior to the extraction procedure, and the impact of shaking as an intermediate step during extraction. The analyses were conducted on four different types of biocrusts. Our results show that for all biocrust types chlorophyll contents obtained with ethanol were significantly lower than those obtained using dimethyl sulfoxide (DMSO) as a solvent. Grinding of biocrust samples prior to analysis caused a highly significant decrease in chlorophyll content for green algal lichen- and cyanolichen-dominated biocrusts, and a tendency towards lower values for moss- and algae-dominated biocrusts. Shaking of the samples after each extraction step had a significant positive effect on the chlorophyll content of green algal lichen- and cyanolichen-dominated biocrusts. Based on our results we confirm a DMSO-based chlorophyll extraction method without grinding pretreatment and suggest the addition of an intermediate shaking step for complete chlorophyll extraction (see Supplement S6 for detailed manual). Determination of a universal chlorophyll extraction method for biocrusts is essential for the inter-comparability of publications conducted across all continents.

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.

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.

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.

Study of process variables in supercritical carbon dioxide extraction of soybeans.

PubMed

Wilkinson, Nikolas; Hilton, Ramsey; Hendry, Doug; Venkitasamy, Chandrasekar; Jacoby, William

2014-01-01

Soybean flakes were extracted using supercritical carbon dioxide at 48.3 MPa and 80 °C, which is a higher temperature than previously reported. Several operational parameters were explored to determine their effect on extractions. Flakes, as typically used in this industry, provided the best extraction performance. Particle size distributions were created through grinding. Reducing average particle diameters smaller than 0.069 mm had no appreciable effect on increasing extraction efficiencies. Exploration of flow rate indicated that a residence time of less than 60 s for the supercritical carbon dioxide would be sufficient for complete extractions. A solvent mass to load mass ratio of 10:1 was found to be sufficient for extraction of oils from soybean flakes. Increasing moisture in the soybeans led to decreasing extraction efficiency of oils. Finally, soybean hulls had no effect on extraction efficiency. Thus, the de-hulling procedure can be removed from the extraction process without decreasing extraction efficiency.

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.

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.

Measurement of water-soluble B vitamins in infant formula by liquid chromatography/tandem mass spectrometry.

PubMed

Huang, Min; Winters, Doug; Crowley, Richard; Sullivan, Darryl

2009-01-01

A method has been developed for the simultaneous measurement of multiple B vitamins (i.e., B1, B2, B3, B5, and B6) in infant formulas by LC-MSIMS. The vitamins were extracted with acidic solvent, followed by protein precipitation at a pH range of 4.5 to 5.5, and filtered. This simplified procedure eliminates many of the potential sources of laboratory error and facilitates rapid and efficient analysis. As is common in most cases, isotope internal standards were added to account for variations in sample preparation, as well as changes in MS measurement. In this method, isotope-labeled internal standards of B1, B3, B5, and B6 were used. The factors affecting analytical performance were investigated and optimized. In addition, the stability of these vitamins in the extraction solution was investigated. An acidic condition (5 mM HCl) was applied to successfully stabilize B1, which had shown a decrease in signal when other solvents were used. The quantitative extraction and good stability allowed isotope standards to be added to the filtered sample solution, instead of to the extraction solvent. The addition of the isotope to the small portion of the filtered sample solution significantly reduces cost. A comprehensive evaluation of the analysis of the standard reference material and good spike recovery of the vitamins (100 +/- 6%) demonstrates the accuracy of the method. The results for commercially available infant formula samples were also compared with those obtained using the current microbiological method.

Focused microwave-assisted extraction combined with solid-phase microextraction and gas chromatography-mass spectrometry for the selective analysis of cocaine from coca leaves.

PubMed

Bieri, Stefan; Ilias, Yara; Bicchi, Carlo; Veuthey, Jean-Luc; Christen, Philippe

2006-04-21

An effective combination of focused microwave-assisted extraction (FMAE) with solid-phase microextraction (SPME) prior to gas chromatography (GC) is described for the selective extraction and quantitative analysis of cocaine from coca leaves (Erythroxylum coca). This approach required switching from an organic extraction solvent to an aqueous medium more compatible with SPME liquid sampling. SPME was performed in the direct immersion mode with a universal 100 microm polydimethylsiloxane (PDMS) coated fibre. Parameters influencing this extraction step, such as solution pH, sampling time and temperature are discussed. Furthermore, the overall extraction process takes into account the stability of cocaine in alkaline aqueous solutions at different temperatures. Cocaine degradation rate was determined by capillary electrophoresis using the short end injection procedure. In the selected extraction conditions, less than 5% of cocaine was degraded after 60 min. From a qualitative point of view, a significant gain in selectivity was obtained with the incorporation of SPME in the extraction procedure. As a consequence of SPME clean-up, shorter columns could be used and analysis time was reduced to 6 min compared to 35 min with conventional GC. Quantitative results led to a cocaine content of 0.70 +/- 0.04% in dry leaves (RSD <5%) which agreed with previous investigations.

Effect of Piper betle L. and its extracts on the growth and aflatoxin production by Aspergillus parasiticus.

PubMed

Chou, C C; Yu, R C

1984-01-01

Ground powder of the leaf and fruit of Piper betle L., a tropical spice plant grown in Southeast Asia, was prepared and extracted by chloroform, ethanol and water with one solvent only or with 3 solvents in sequence. The betel powder and various extracts were added to YES broth to determine their effects on the growth and aflatoxin production by Aspergillus parasiticus. Results showed that betel leaf powder exhibited higher antimycotic activity than fruit. One half percent of ground leaf powder completely inhibited the growth and aflatoxin production by A. parasiticus. Among the solvent extracts, chloroform and ethanol extracts of betel leaf prepared from a single solvent extraction showed more antimycotic activity. The ethanol extract of betel leaf at the level of 450 micrograms/ml would eliminate A. parasiticus growth and aflatoxin production. The antimycotic activity of this ethanol extract was most pronounced at pH 4.

Comparative Analysis of Chemical Composition, Antioxidant Activity and Quantitative Characterization of Some Phenolic Compounds in Selected Herbs and Spices in Different Solvent Extraction Systems.

PubMed

Sepahpour, Shabnam; Selamat, Jinap; Abdul Manap, Mohd Yazid; Khatib, Alfi; Abdull Razis, Ahmad Faizal

2018-02-13

This study evaluated the efficacy of various organic solvents (80% acetone, 80% ethanol, 80% methanol) and distilled water for extracting antioxidant phenolic compounds from turmeric, curry leaf, torch ginger and lemon grass extracts. They were analyzed regarding the total phenol and flavonoid contents, antioxidant activity and concentration of some phenolic compounds. Antioxidant activity was determined by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging assay and the ferric reducing antioxidant power (FRAP) assay. Quantification of phenolic compounds was carried out using high-performance liquid chromatography (HPLC). All the extracts possessed antioxidant activity, however, the different solvents showed different efficiencies in the extraction of phenolic compounds. Turmeric showed the highest DPPH values (67.83-13.78%) and FRAP (84.9-2.3 mg quercetin/g freeze-dried crude extract), followed by curry leaf, torch ginger and lemon grass. While 80% acetone was shown to be the most efficient solvent for the extraction of total phenolic compounds from turmeric, torch ginger and lemon grass (221.68, 98.10 and 28.19 mg GA/g freeze dried crude extract, respectively), for the recovery of phenolic compounds from curry leaf (92.23 mg GA/g freeze-dried crude extract), 80% ethanol was the most appropriate solvent. Results of HPLC revealed that the amount of phenolic compounds varied depending on the types of solvents used.

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

Production of three types of krill oils from krill meal by a three-step solvent extraction procedure.

PubMed

Xie, Dan; Mu, Hongyan; Tang, Tianpei; Wang, Xiaosan; Wei, Wei; Jin, Jun; Wang, Xingguo; Jin, Qingzhe

2018-05-15

In this study, a three-step extraction method (separately use acetone, hexane, and ethanol as extraction solvent in each step) was conducted to selectively extract three types of krill oils with different compositions. The lipid yields were 5.08% in step 1, 4.80% in step 2, and 9.11% in step 3, with a total of 18.99%. The krill oil extracted with acetone in step 1 (A-KO) contained the lowest contents of phospholipids (PL) (2.32%) and n-3 polyunsaturated fatty acids (PUFA) (16.63%), but the highest levels of minor components (505.00 mg/kg of astaxanthin, 29.39 mg/100 g of tocopherols, 34.32 mg/100 g of vitamin A and 27.95 mg/g of cholesterol). By contrast, despite having traces of minor components, the krill oil extracted using ethanol in step 3 (E-KO) was the most abundant in PL (59.52%) and n-3 PUFA (41.74%). The krill oil extracted using hexane in step 2 (H-KO) expressed medium contents of all the testing indices. The oils showed significant differences in the antioxidant capacity (E-KO > H-KO > A-KO) which exhibited positive correlation with the PL content. These results could be used for further development of a wide range of krill oil products with tailor-made functions. Copyright © 2017 Elsevier Ltd. All rights reserved.

Dispersive solid-phase extraction followed by vortex-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet for the determination of benzoylurea insecticides in soil and sewage sludge.

PubMed

Peng, Guilong; He, Qiang; Mmereki, Daniel; Lu, Ying; Zhong, Zhihui; Liu, Hanyang; Pan, Weiliang; Zhou, Guangming; Chen, Junhua

2016-04-01

A novel dispersive solid-phase extraction combined with vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the determination of eight benzoylurea insecticides in soil and sewage sludge samples before high-performance liquid chromatography with ultraviolet detection. The analytes were first extracted from the soil and sludge samples into acetone under optimized pretreatment conditions. Clean-up of the extract was conducted by dispersive solid-phase extraction using activated carbon as the sorbent. The vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet procedure was performed by using 1-undecanol with lower density than water as the extraction solvent, and the acetone contained in the solution also acted as dispersive solvent. Under the optimum conditions, the linearity of the method was in the range 2-500 ng/g with correlation coefficients (r) of 0.9993-0.9999. The limits of detection were in the range of 0.08-0.56 ng/g. The relative standard deviations varied from 2.16 to 6.26% (n = 5). The enrichment factors ranged from 104 to 118. The extraction recoveries ranged from 81.05 to 97.82% for all of the analytes. The good performance has demonstrated that the proposed methodology has a strong potential for application in the multiresidue analysis of complex matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Determination of water-soluble vitamins in multivitamin dietary supplements and in artichokes by micellar electrokinetic chromatography.

PubMed

Serni, Enrico; Audino, Valeria; Del Carlo, Sara; Manera, Clementina; Saccomanni, Giuseppe; Macchia, Marco

2013-01-01

Several procedures of extraction with solvents for the simultaneous determination of vitamin C and some vitamins belonging to the B group (thiamine, riboflavine, nicotinic acid and nicotinamide) in multivitamin preparations and in artichokes (Cynara cardunculus subsp. scolymus [L.] Hegi) were developed. Different experimental conditions were used, in terms of heat treatment, composition and pH of the extraction mixture, with particular attention to high-temperature steps; purification of the extracts with solid phase extraction and stabilisation through lyophilisation were discussed. Analyses of the extracts were conducted by capillary electrophoresis in micellar electrokinetic chromatography modality. Borate buffer at pH 8.2 was used, and sodium dodecyl sulphate was added to the background electrolyte as surfactant. A range of linearity was determined and calibration curves were plotted for all the analytes.

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.

An interesting two-phase solvent system and its use in preparative isolation of aconitines from aconite roots by counter-current chromatography.

PubMed

Han, Quan-Bin; Tang, Wai-Lun; Dong, Cai-Xia; Xu, Hong-Xi; Jiang, Zhi-Hong

2013-04-01

Two-phase solvent system plays crucial role in successful separation of organic compounds using counter-current chromatography (CCC). An interesting two-phase solvent system, composed of chloroform/ethyl acetate/methanol/water, is reported here, in which both phases contain sufficient organic solvents to balance their dissolving capacities. Adjusting the solvent system to get satisfactory partition coefficients (K values) for target compounds becomes relatively simple. This solvent system succeeded in sample preparation of aconitine (8.07 mg, 93.69%), hypaconitine (7.74 mg, 93.17%), mesaconitine (1.95 mg, 94.52%) from raw aconite roots (102.24 mg, crude extract), benzoylmesaconine (34.79 mg, 98.67%) from processed aconite roots (400.01 mg, crude extract), and yunaconitine (253.59 mg, 98.65%) from a crude extract of Aconitum forrestii (326.69 mg, crude extract). © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of 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.

Analysis of Nonvolatile Residue (NVR) from Spacecraft Systems

NASA Technical Reports Server (NTRS)

Colony, J. A.

1985-01-01

Organic contamination on critical spacecraft surfaces can cause electronic problems, serious attenuation of various optical signals, thermal control changes, and adhesion problems. Such contaminants can be detected early by the controlled use of witness mirrors, witness plates, wipe sampling, or direct solvent extraction. Each method requires careful control of variables of technique and materials to attain the ultimate sensitivities inherent to that procedure. Subsequent chemical analysis of the contaminant sample by infrared and mass spectrometry identifies the components, gives semiquantitative estimates of contaminant thickness, indicates possible sources of the nonvolatile residue (NVR), and provides guidance for effective cleanup procedures.

Microwave-assisted of dispersive liquid-liquid microextraction and spectrophotometric determination of uranium after optimization based on Box-Behnken design and chemometrics methods.

PubMed

Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

2015-01-25

In this study an analytical procedure based on microwave-assisted dispersive liquid-liquid microextraction (MA-DLLME) and spectrophotometric coupled with chemometrics methods is proposed to determine uranium. In the proposed method, 4-(2-pyridylazo) resorcinol (PAR) is used as a chelating agent, and chloroform and ethanol are selected as extraction and dispersive solvent. The optimization strategy is carried out by using two level full factorial designs. Results of the two level full factorial design (2(4)) based on an analysis of variance demonstrated that the pH, concentration of PAR, amount of dispersive and extraction solvents are statistically significant. Optimal condition for three variables: pH, concentration of PAR, amount of dispersive and extraction solvents are obtained by using Box-Behnken design. Under the optimum conditions, the calibration graphs are linear in the range of 20.0-350.0 ng mL(-1) with detection limit of 6.7 ng mL(-1) (3δB/slope) and the enrichment factor of this method for uranium reached at 135. The relative standard deviation (R.S.D.) is 1.64% (n=7, c=50 ng mL(-1)). The partial least squares (PLS) modeling was used for multivariate calibration of the spectrophotometric data. The orthogonal signal correction (OSC) was used for preprocessing of data matrices and the prediction results of model, with and without using OSC, were statistically compared. MA-DLLME-OSC-PLS method was presented for the first time in this study. The root mean squares error of prediction (RMSEP) for uranium determination using PLS and OSC-PLS models were 4.63 and 0.98, respectively. This procedure allows the determination of uranium synthesis and real samples such as waste water with good reliability of the determination. Copyright © 2014. 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.

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.

Novel procedure for the extraction and concentration of carotenoid-containing chromoplasts from selected plant systems.

PubMed

Fish, Wayne W

2007-02-21

Natural sources of carotenoids for nutraceutical use are desired by the food industry as a result of the increased production of convenience and other highly processed foods. As new physiological roles are discovered for some of the minor carotenoids that are found in only small amounts in present sources, the need for discovery of new sources will amplify. Thus, a method is needed that will effectively and gently concentrate carotenoids from potential new sources for subsequent identification and analysis. A procedure is presented by which carotenoid-containing tissue chromoplasts can be extracted and subsequently concentrated by precipitation, all in an aqueous milieu. The chromoplasts are extracted and solubilized with 0.3% sodium dodecyl sulfate (SDS) in water. The addition of a nominally equal volume of acetonitrile to the chromoplasts in SDS immediately precipitates the chromoplasts out of solution with generally >90% recovery. Carotenoids contained in the concentrated, still-intact chromoplasts can then be solubilized by organic solvent extraction for subsequent analysis. This methodology offers a means to effectively and gently concentrate carotenoids from fruit tissues where yields are often low (e.g., yellow watermelon).

Arsenic Speciation of Solvent-Extracted Leachate from New and Weathered CCA-Treated Wood

PubMed Central

KHAN, BERNINE I.; SOLO - GABRIELE, HELENA M.; DUBEY, BRAJESH K.; TOWNSEND, TIMOTHY G.; CAI, YONG

2009-01-01

For the past 60 yr, chromate-copper-arsenate (CCA) has been used to pressure-treat millions of cubic meters of wood in the United States for the construction of many outdoor structures. Leaching of arsenic from these structures is a possible health concern as there exists the potential for soil and groundwater contamination. While previous studies have focused on total arsenic concentrations leaching from CCA-treated wood, information pertaining to the speciation of arsenic leached is limited. Since arsenic toxicity is dependent upon speciation, the objective of this study was to identify and quantify arsenic species leaching from new and weathered CCA-treated wood and CCA-treated wood ash. Solvent-extraction experiments were carried out by subjecting the treated wood and the ash to solvents of varying pH values, solvents defined in the EPA’s Synthetic Precipitation Leaching Procedure (SPLP) and Toxicity Characteristic Leaching Procedure (TCLP), rainwater, deionized water, and seawater. The generated leachates were analyzed for inorganic As(III) and As(V) and the organoarsenic species, monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA), using high-performance liquid chromatography followed by hydride generation and atomic fluorescence spectrometry (HPLC–HG-AFS). Only the inorganic species were detected in any of the wood leachates; no organoarsenic species were found. Inorganic As(V) was the major detectable species leaching from both new and weathered wood. The weathered wood leached relatively more overall arsenic and was attributed to increased inorganic As(III) leaching. The greater presence of As(III) in the weathered wood samples as compared to the new wood samples may be due to natural chemical and biological transformations during the weathering process. CCA-treated wood ash leached more arsenic than unburned wood using the SPLP and TCLP, and ash samples leached more inorganic As(III) than the unburned counterparts. Increased leaching was due to higher concentrations of arsenic within the ash and to the conversion of some As(V) to As(III) during combustion. PMID:15461159

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.

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.

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

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.

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 sensitive analytical procedure for monitoring acrylamide in environmental water samples by offline SPE-UPLC/MS/MS.

PubMed

Togola, Anne; Coureau, Charlotte; Guezennec, Anne-Gwenaëlle; Touzé, Solène

2015-05-01

The presence of acrylamide in natural systems is of concern from both environmental and health points of view. We developed an accurate and robust analytical procedure (offline solid phase extraction combined with UPLC/MS/MS) with a limit of quantification (20 ng L(-1)) compatible with toxicity threshold values. The optimized (considering the nature of extraction phases, sampling volumes, and solvent of elution) solid phase extraction (SPE) was validated according to ISO Standard ISO/IEC 17025 on groundwater, surface water, and industrial process water samples. Acrylamide is highly polar, which induces a high variability during the SPE step, therefore requiring the use of C(13)-labeled acrylamide as an internal standard to guarantee the accuracy and robustness of the method (uncertainty about 25 % (k = 2) at limit of quantification level). The specificity of the method and the stability of acrylamide were studied for these environmental media, and it was shown that the method is suitable for measuring acrylamide in environmental studies.

Separation and Recovery of Cobalt from Copper Leach Solutions

NASA Astrophysics Data System (ADS)

Jeffers, T. H.

1985-01-01

Significant amounts of cobalt, a strategic and critical metal, are present in readily accessible copper recycling leach solutions. However, cost-effective technology is not available to separate and recover the cobalt from this low-grade domestic source. The Bureau of Mines has developed a procedure using a chelating ion-exchange resin from Dow Chemical Co. to successfully extract cobalt from a pH 3.0 copper recycling solution containing only 30 mg/1 cobalt. Cyclic tests with the commercial resin XFS-4195 in 4-ft-high by 1-in.-diameter columns gave an average cobalt extraction of 95% when 65 bed volumes of solution were processed at a flow rate of 4 gpm/ft.2 Elution of the cobalt using a 50 g/l H2SO4 solution yielded an eluate containing 0.5 gli Co. Selective elution of the loaded resin and solvent extraction procedures using di-2-ethylhexyl phosphoric acid (D2EHPA) and Cyanex 272 removed the impurities and produced a cobalt sulfate solution containing 25 g/l Co.

Development of a screening method for the determination of forty-nine priority pollutants in soil

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

Kiang, P.H.T.

1985-01-01

An extraction procedure followed by capillary GC-MS analysis was used to determine soil pollutants. Dual pH solutions with methylene chloride were used as extraction solvent system. Both base/neutral and acidic fractions were analyzed on the same fused silica 30 meter SPB-1 (SE-30) column. A GC-FID with a 60 meter wide-bore SPB-1 glass capillary column was used for quantitative analysis due to its larger sample capacity and higher sensitivity. The precision and accuracy for 5.1 ppm (51 ..mu..g/10 g) concentration in zero soil was less than 25% RSD. A headspace technique was also developed for the determination of volatile compounds. Themore » same instrumental conditions and columns were used as in the extraction procedure. The precision and accuracy for 3 grams soil sample spiked with 5.1 ppm (52 ..mu..g/10 mL) pollutant mixture in a 20 mL vial was less than 3% RSD.« less

Determination of guaifenesin in human serum by capillary gas chromatography and electron capture detection.

PubMed

Sharaf, Maged H M; Stiff, Dwight D

2004-06-29

A method for the quantitation of guaifenesin in human serum has been developed and validated. The procedure involves liquid-liquid extraction of the serum sample in the presence of mephenesin as an internal standard, followed by derivatization and analysis using capillary gas chromatography (GC) and electron capture detection (ECD). Different solvents were tested for extraction of guaifenesin from serum. n-Hexane/dichloromethane (1:1, v/v) gave the highest recovery and the lowest background and was chosen as the extraction solvent. After extraction, the residue of guaifenesin was derivatized at 60 degrees C for 30 min, with trifluoroacetic acid anhydride (TFAA) in toluene in the presence of pyridine. Excess trifluoroacetic acid anhydride was removed using dilute solution of ammonium hydroxide. The method proved to be linear over the range of 25.0-1000 ng/ml. Recovery of guaifenesin from spiked samples was consistent, averaging 75.5% at 50.0 ng/ml with a range of 72.0-80.0% (N = 8 determinations) and averaging 78% at 800 ng/ml with a range of 76.0-81.0% (N = 8 determinations). The internal standard recovery was also consistent averaging 72.8% with a range of 67.0-76.0% (N = 16 determinations). Copyright 2004 Elsevier B.V.

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.

Ultrasound-assisted temperature-controlled ionic liquid emulsification microextraction coupled with capillary electrophoresis for the determination of parabens in personal care products.

PubMed

Ma, Teng; Li, Zheng; Jia, Qiong; Zhou, Weihong

2016-07-01

We developed a CE and ultrasound-assisted temperature-controlled ionic liquid emulsification microextraction method for the determination of four parabens (methyl paraben, ethyl paraben, propyl paraben, and butyl paraben) in personal care products including mouthwash and toning lotion. In the proposed extraction procedure, ionic liquid (IL, 1-octyl-3-methylimidazolium hexafluorophosphate) was used as extraction solvent, moreover, no disperser solvent was needed. Parameters affecting the extraction efficiency including volume of IL, heating temperature, ultrasonic time, extraction time, sample pH, ionic strength, and centrifugation time were optimized. Under the optimized conditions, the method was found to be linear over the range of 3-500 ng/mL with coefficient of determination (R(2) ) in the range of 0.9990-0.9998. The LODs and LOQs for the four parabens were 0.45-0.72 ng/mL and 1.50-2.40 ng/mL, respectively. Intraday and interday precisions (RSDs, n = 5) were in the range of 5.4-6.8% and 7.0-8.7%, respectively. The recoveries of parabens at different spiked levels ranged from 71.9 to 119.2% with RSDs less than 9.5%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Total Flavonoids Content in the Raw Material and Aqueous Extractives from Bauhinia monandra Kurz (Caesalpiniaceae)

PubMed Central

Fernandes, Ana Josane Dantas; Ferreira, Magda Rhayanny Assunção; Randau, Karina Perrelli; de Souza, Tatiane Pereira; Soares, Luiz Alberto Lira

2012-01-01

The aim of this work was to evaluate the spectrophotometric methodology for determining the total flavonoid content (TFC) in herbal drug and derived products from Bauhinia monandra Kurz. Several analytical parameters from this method grounded on the complex formed between flavonoids and AlCl3 were evaluated such as herbal amount (0.25 to 1.25 g); solvent composition (ethanol 40 to 80%, v/v); as well as the reaction time and AlCl3 concentration (2 to 9%, w/v). The method was adjusted to aqueous extractives and its performance studied through precision, linearity and preliminary robustness. The results showed an important dependence of the method response from reaction time, AlCl3 concentration, sample amount, and solvent mixture. After choosing the optimized condition, the method was applied for the matrixes (herbal material and extractives), showing precision lower than 5% (for both parameters repeatability and intermediate precision), coefficient of determination higher than 0.99, and no important influence could be observed for slight variations from wavelength or AlCl3 concentration. Thus, it could be concluded that the evaluated analytical procedure was suitable to quantify the total flavonoid content in raw material and aqueous extractives from leaves of B. monandra. PMID:22701375

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.

New approaches for extraction and determination of betaine from Beta vulgaris samples by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

PubMed

Rivoira, Luca; Studzińska, Sylwia; Szultka-Młyńska, Malgorzata; Bruzzoniti, Maria Concetta; Buszewski, Bogusław

2017-08-01

Betaine is one of most studied biologically active compounds, due its role in the main biological processes. Although it may be found in several plants and roots, such as the Beta vulgaris family, present in typical diets, just a few analytical methods have been developed for its extraction from roots. A new, quick and effective procedure for the isolation and determination of betaine from two different varieties of B. vulgaris (red and gold) is presented. For betaine extraction, an accelerated solvent extraction (ASE) was coupled with solid-phase extraction. For betaine determination, a separation method based on hydrophilic interaction chromatography coupled with tandem mass spectrometry was optimized for a sensible detection of betaine by means of experimental design. Recoveries were about 93%, with RSD <5%, for both the matrices, without evidence of interfering species. The total content of betaine in extracts of various parts of plants (juice, peel, root) have been determined, obtaining concentrations in the range 3000-4000 mg/L for the juice and in the range 2-5 mg/g for the pulp and for the peel. The B. vulgaris gold species exhibited a higher concentration of betaine, compared to the red variety. Additionally, a micro extraction by packed sorbent technique and a modified quick, easy, cheap, rugged and safe (QuEChERS) procedure, were also tested and compared. Despite the lower recoveries of the latter, with respect to the ASE/SPE procedure (75-89%, RSD <1.5%), the ease of the method, which can be applied without the SPE purification procedure, can represent a positive improvement. Graphical abstract Determination of betaine from Beta vulgaris samples.

Extraction of natural colorant from purple sweet potato and dyeing of fabrics with silver nanoparticles for augmented antibacterial activity against skin pathogens.

PubMed

Velmurugan, Palanivel; Kim, Jae-In; Kim, Kangmin; Park, Jung-Hee; Lee, Kui-Jae; Chang, Woo-Suk; Park, Yool-Jin; Cho, Min; Oh, Byung-Taek

2017-08-01

The main objective of this study was to extract natural colorant from purple sweet potato powder (PSPP) via a water bath and ultrasound water bath using acidified ethanol (A. EtOH) as the extraction solvent. When optimizing the colorant extraction conditions of the solvents, acidified ethanol with ultrasound yielded a high extraction capacity and color intensity at pH2, temperature of 80°C, 20mL of A. EtOH, 1.5g of PSPP, time of 45min, and ultrasonic output power of 75W. Subsequently, the colorant was extracted using the optimized conditions for dyeing of textiles (leather, silk, and cotton). This natural colorant extraction technique can avoid serious environmental pollution during the extraction and is an alternative to synthetic dyes, using less solvent and simplified abstraction procedures. The extracted purple sweet potato natural colorant (PSPC) was used to dye leather, silk, and cotton fabrics in an eco-friendly approach with augmented antibacterial activity by in situ synthesis of silver nanoparticles (AgNPs) and dyeing. The optimal dyeing conditions for higher color strength (K/S) values were pH2 and 70°C for 45min. The colorimetric parameters L ∗ , a ∗ , b ∗ , C, and H were measured to determine the depth of the color. The Fourier transform infrared spectroscopy (FTIR) spectra of undyed control, dyed with PSPC and dyed with blend of PSPC and AgNPs treated leather, silk and cotton fabric were investigated to study the interaction among fiber type, nanoparticles, and dye. The structural morphology of leather and silk and cotton fabrics and the anchoring of AgNPs with elemental compositions were investigated by scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS). The dry and wet rubbing fastness for dye alone and dye with nanoparticles were grade 4-5 and 4, respectively. Thus, the results of the present study clearly suggest that in situ synthesis of AgNPs along with dyeing should be considered in the development of antimicrobial textile finishes. Copyright © 2017. Published by Elsevier B.V.

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.

Deep Eutectic Solvents Modified Molecular Imprinted Polymers for Optimized Purification of Chlorogenic Acid from Honeysuckle.

PubMed

Li, Guizhen; Wang, Wei; Wang, Qian; Zhu, Tao

2016-02-01

Deep eutectic solvents (DES) were synthesized with choline chloride (ChCl), and DES modified molecular imprinted polymers (DES-MIPs), DES modified non-imprinted polymers (DES-NIPs, without template), MIPs and NIPs were prepared in an identical procedure. Fourier transform infrared spectrometer (FT-IR) and field emission scanning electron microscopy (FE-SEM) were used to characterize the obtained polymers. Rebinding experiment and solid-phase extraction (SPE) were used to prove the high selectivity adsorption properties of the polymers. Box-Behnken design (BBD) with three factors was used to optimize the extraction condition of chlorogenic acid (CA) from honeysuckles. The optimum extraction conditions were found to be ultrasonic time optimized (20 min), the volume fraction of ethanol (60%) and ratio of liquid to material (15 mL g(-1)). Under these conditions, the mean extraction yield of CA was 12.57 mg g(-1), which was in good agreement with the predicted BBD model value. Purification of hawthorn extract was achieved by SPE process, and SPE recoveries of CA were 72.56, 64.79, 69.34 and 60.08% by DES-MIPs, DES-NIPs, MIPs and NIPs, respectively. The results showed DES-MIPs had potential for promising functional adsorption material for the purification of bioactive compounds. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

New analytical method for the determination of musks in personal care products by Quick, Easy, Cheap, Effective, Rugged, and Safe extraction followed by GC-MS.

PubMed

Homem, Vera; Silva, José Avelino; Cunha, Carina; Alves, Arminda; Santos, Lúcia

2013-07-01

Synthetic musks are organic compounds used as fragrance additives and fixative compounds in a diversity of personal care products. A new method based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction followed by GC-MS for the analysis of 12 musks in personal care products was developed and validated. Some experimental parameters, such as total QuEChERS mass, sample mass/solvent volume ratio, type of extraction solvent, as well as salts and sorbents amount were investigated and optimized. The final method involves the musks extraction using acetonitrile, followed by the addition of anhydrous magnesium sulphate and sodium acetate. The clean-up step was performed using dispersive SPE with primary and secondary amine and octadecyl-silica sorbents. This extraction procedure is fast (about 10 min) when compared to other traditional approaches. The method was robust for the matrices studied and shows a high precision (%RSD < 15%) and accuracy (average recovery of 85%), allowing the detection of musks in minimum concentrations between 0.01 ng/g (galaxolide) and 15.80 ng/g (musk xylene). The developed method was applied to the analysis of 12 samples, which revealed musks concentrations ranging from 2 ng/g (toothpaste) to 882,340 ng/g (perfumed body lotion). © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultra preconcentration of polycyclic aromatic hydrocarbons in smoked bacon by a combination of SPE and DLLME.

PubMed

Liu, Xiaofang; Zhou, Shu; Zhu, Quanfei; Ye, Yong; Chen, Huaixia

2014-09-01

A sample pretreatment method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was established for the sensitive determination of polycyclic aromatic hydrocarbons (PAHs) in smoked bacon samples. In the SPE-DLLME process, three PAHs including naphthalene (Naph), phenanthrene (Phen) and pyrene (Pyr) were extracted from samples and transferred into C18 SPE cartridge. The target analytes were subsequently eluted with 1.2 ml of acetonitrile-dichloromethane (5:1, v/v) mixture solution. The eluent was injected directly into the 5.0 ml ultrapure water in the subsequent DLLME procedure. The sedimented phase was concentrated under a gentle nitrogen flow to 120.0 µl. Finally, the analytes in the extraction solvent were determined by high-performance liquid chromatography with a ultra-violet detector. Some important extraction parameters affecting the performance, such as the sample solution flow rate, breakthrough volume, salt addition as well as the type and volume of the elution solvent were optimized. The developed method provided an ultra enrichment factors for PAHs ranged from 3478 to 3824. The method was applied for the selective extraction and sensitive determination of PAHs in smoked bacon samples. The limits of detection (S/N = 3) were 0.05, 0.01, 0.02 μg kg(-1) for Naph, Phen, Pyr, respectively. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

Humic substances (HSs), consisting, on the basis of solubilities in aqueous acid and basic media, of humic acids (HAs), fulvic acids (FAs), and humin (Hu), are the major components of soil organic matter (SOM). Most studies of soil/natural organic matter (SOM/NOM) have been carried out on extracts of soils in dilute sodium hydroxide solutions, the solvent used to extract the Standards of the International Humic Substances Society (IHSS). However, Hu, the major component in the classical definition of HSs, is insoluble in aqueous base and is not isolated by the traditional IHSS method. Recently, a sequential exhaustive extraction (SEE) process has been shown to be capable of isolating and separating the major components of the classically defined HSs from the soils of the temperate and tropical regions. The SEE system was used in the present study to isolate the HA/FA and Hu fractions from a subtropical volcanic Taiwanese soil. Chemical and compositional properties of these extracts were then compared with similarly obtained isolates from soils from the different climatic regions. Increases in the aliphatic relative to aromatic carbon contents were observed for both the HA and FA fractions when the pH values of the extraction media were increased. HAs and FAs isolated using the SEE method have spectroscopic profiles similar to those from the IHSS isolate; however, the cumulative extraction efficiency (%) of the SEE method (65 %) for the volcanic soil was much higher than for the traditional IHSS method (33 %). When the residual volcanic soil, following extractions once, three, and eight times with 0.1 M NaOH were then extracted with dimethyl sulphoxide (DMSO) plus concentrated sulphuric acid (the final solvent in the SEE sequence) it was seen that the content of crystalline polymethylene hydrocarbon (33 ppm 13C-NMR resonance in the Hu (or DMSO/acid)) extract increased relative to the amorphous methylene (30 ppm). That highlights the difficulty in dissolving the more highly ordered hydrocarbon structures that would be expected to have closer associations with the mineral colloids. Although the SEE procedure isolated all of the HAs and FAs from the Yangmingshan soil, extractability of the Hu from the volcanic soil in the DMSO/acid solvent was low (21 %), and contrasted with the much higher yields from temperate and tropical regions. The decreased Hu extraction may arise from its associations with the extensive iron and aluminium hydroxide mineral colloids in the soil. The Hu from this sub-tropical soil was different from the Hus isolated from other soil types, indicating the need to isolate and characterise these recalcitrant organic material in order to understand the organic carbon components in soils in greater detail. Such results would indicate that more attention should be given to mineral colloids in soils, and to the organo/mineral associations that will have an important role in the stabilities of OM in the soil environment.

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.

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)

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

PubMed

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

2015-09-04

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

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.

Ionic liquid molecularly imprinted polymers for application in pipette-tip solid-phase extraction coupled with gas chromatography for rapid screening of dicofol in celery.

PubMed

Yan, Hongyuan; Yang, Chen; Sun, Yunyun; Row, Kyung Ho

2014-09-26

A new type of ionic liquid molecularly imprinted polymers (IL-MIPs) synthesized by precipitation polymerization using 1-allyl-3-methylimidazolium bromide as an auxiliary solvent and α-chloro-dichlorodiphenyltrichloroethane (α-chloro-DDT) as the template was applied as a selective sorbent of minimized pipette tip-solid-phase extraction (PT-SPE) for rapid isolation and extraction of dicofol (DCF) from celery samples. The pretreatment procedure of celery samples involved only 2.0mg of IL-MIPs, 0.8 mL of acetonitrile-water (ACN-H2O; 1:1, v/v) (washing solvent), and 1.0 mL of acetone-10% acetic acid (HOAc) (elution solvent). Compared with molecularly imprinted polymers (MIPs), ionic liquid-non-imprinted polymers (IL-NIPs) and conventional sorbents such as C18, Si, NH2, and Al2O3-N, IL-MIPs showed higher adsorption and purification capacity to DCF in aqueous solution. Good linearity for DCF was observed in the range from 2.3 to 232.5 ng g(-1) (r(2)=0.9995). The average recoveries at three spiking levels ranged from 86.6% to 101.9% with relative standard deviations (RSDs) of ≤ 6.5% (n=3). The presented IL-MIPs-PT-SPE-GC/ECD method combines the advantages of MIPs, IL, and PT-SPE, and can be used in aqueous conditions with high affinity and selectivity to analytes of complex samples. Copyright © 2014 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.

The composition of potentially bioactive triterpenoid glycosides in red raspberry is influenced by tissue, extraction procedure and genotype.

PubMed

McDougall, Gordon J; Allwood, J William; Pereira-Caro, Gema; Brown, Emma M; Latimer, Cheryl; Dobson, Gary; Stewart, Derek; Ternan, Nigel G; Lawther, Roger; O'Connor, Gloria; Rowland, Ian; Crozier, Alan; Gill, Chris I R

2017-10-18

The beneficial effects of consumption of berry fruits on a range of chronic diseases has been attributed (at least in part) to the presence of unique phytochemicals. Recently, we identified novel ursolic acid-based triterpenoid glycosides (TTPNs) in raspberry fruit and demonstrated their survival in human ileal fluids after feeding which confirmed their colon-availability in vivo. In this paper, in vitro digestion studies demonstrated that certain TTPNs were stable under gastrointestinal conditions and confirmed that these components may have been responsible for bioactivity noted in previous studies. Sequential extractions of raspberry puree, isolated seeds and unseeded puree showed that certain TTPN components (e.g. peak T1 m/z 679, and T2 m/z 1358) had different extractabilities in water/solvent mixes and were differentially associated with the seeds. Purified seed TTPNs (mainly T1 and T2) were shown to be anti-genotoxic in HT29 and CCD841 cell based in vitro colonocyte models. Further work confirmed that the seeds contained a wider range of TTPN-like components which were also differentially extractable in water/solvent mixes. This differential extractability could influence the TTPN composition and potential bioactivity of the extracts. There was considerable variation in total content of TTPNs (∼3-fold) and TTPN composition across 13 Rubus genotypes. Thus, TTPNs are likely to be present in raspberry juices and common extracts used for bioactivity studies and substantial variation exists in both content and composition due to genetics, tissue source or extraction conditions, which may all affect observed bioactivity.

Development of fast and robust multiresidual LC-MS/MS method for determination of pharmaceuticals in soils.

PubMed

Golovko, Oksana; Koba, Olga; Kodesova, Radka; Fedorova, Ganna; Kumar, Vimal; Grabic, Roman

2016-07-01

The aim of this study was to develop a simple extraction procedure and a multiresidual liquid chromatography-tandem mass spectrometry method for determination of a wide range of pharmaceuticals from various soil types. An extraction procedure for 91 pharmaceuticals from 13 soil types, followed by liquid chromatography-tandem mass spectrometry analysis, was optimized. The extraction efficiencies of three solvent mixtures for ultrasonic extraction were evaluated for 91 pharmaceuticals. The best results were obtained using acetonitrile/water (1/1 v/v with 0.1 % formic acid) followed by acetonitrile/2-propanol/water (3/3/4 v/v/v with 0.1 % formic acid) for extracting 63 pharmaceuticals. The method was validated at three fortification levels (10, 100, and 1000 ng/g) in all types of representative soils; recovery of 44 pharmaceuticals ranged between 55 and 135 % across all tested soils. The method was applied to analyze actual environmental samples of sediments, soils, and sludge, and 24 pharmaceuticals were found above limit of quantification with concentrations ranging between 0.83 ng/g (fexofenadine) and 223 ng/g (citalopram).

Improved sample treatment for the determination of insoluble soap in sewage sludge samples by liquid chromatography with fluorescence detection.

PubMed

Cantarero, Samuel; Zafra-Gómez, A; Ballesteros, O; Navalón, A; Vílchez, J L; Crovetto, G; Verge, C; de Ferrer, J A

2010-09-15

A new selective and sensitive method for the determination of insoluble fatty acid salts (soap) in sewage sludge samples is proposed. The method involves a clean up of sample with petroleum ether, the conversion of calcium and magnesium insoluble salts into soluble potassium salts, potassium salts extraction with methanol, and a derivatization procedure previous to the liquid chromatography with fluorescence detection (LC-FLD) analysis. Three different extraction techniques (Soxhlet, microwave-assisted extraction and ultrasounds) were compared and microwave-assisted extraction (MAE) was selected as appropriate for our purpose. This allowed to reduce the extraction time and solvent waste (50 mL of methanol in contrast with 250 mL for Soxhlet procedure). The absence of matrix effect was demonstrated with two standards (C(13:0) and C(17:0)) that are not commercials and neither of them has been detected in sewage sludge samples. Therefore, it was possible to evaluate the matrix effect since both standards have similar environmental behaviour (adsorption and precipitation) to commercial soaps (C(10:0)-C(18:0)). The method was successfully applied to samples from different sources and consequently, with different composition. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Dispersive liquid-liquid microextraction of lead(II) as 5-(4-dimethylaminobenzylidene) rhodanine chelates from food and water samples.

PubMed

Alothman, Zeid A; Al-Shaalan, Nora H; Habila, Mohamed A; Unsal, Yunus E; Tuzen, Mustafa; Soylak, Mustafa

2015-02-01

A dispersive liquid-liquid microextraction procedure for lead(II) as its 5-(4-dimethylaminobenzylidene) rhodanine complex has been established prior to its microsampling flame atomic absorption spectrometric determination. The influences of various analytical parameters including pH, solvent type and volume, dispersive solvent type and volume, 5-(4-dimethylaminobenzylidene) rhodanine amount, salt effect, and centrifugation time and speed were investigated. The effects of certain alkali, alkaline earth, and transition metal ions on the quantitative extraction of lead(II) were also studied. Quantitative recoveries were obtained at pH 6. The enrichment factor was calculated as 125. The detection limit for lead is 1.1 μg/L. The accuracy of the method was tested with the additions recovery test and analysis of the standard reference materials (SPS-WW2 waste water, NIST SRM 1515 apple leaves, and TMDA-51.3 fortified water). Applications of the present procedure were tested by analyzing water and food samples.

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 ...

Antimicrobial activity of methanolic extracts of Sambucus ebulus and Urtica dioica against clinical isolates of methicillin resistant Staphylococcus aureus.

PubMed

Salehzadeh, Ali; Asadpour, Leila; Naeemi, Akram Sadat; Houshmand, Elham

2014-01-01

Increase in the emergence of drug -resistant pathogens led to the development of natural antimicrobials. In this study the antimicrobial effect of methanolic extracts of Sambucus ebulus and Urtica dioica on 16 skin and wound infections isolates of methicillin resistant S. aureus have been studied. Solvent extraction procedure was done using soxhlet apparatus for extracting antimicrobial agents from freeze dried plants. Antibacterial activity was measured using agar well diffusion method. The MIC of Sambucus ebulus and Urtica dioica extracts against the standard strain of S. aureus ATCC 6538 were determined using the micro dilution method at 15 mg and 20 mg respectively. All the test bacteria were found sensitive to the Sambucus ebulus extract and only one isolate was resistant to Urtica dioica extract. Extracts of Sambucus ebulus and Urtica dioica possess antibacterial potency against MRSA isolates and may be used as a natural antiseptics and antimicrobial agents in medicine.

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.

Preparative isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. using supercritical fluid extraction combined with consecutive high-speed countercurrent chromatography.

PubMed

Yan, Rongwei; Shen, Jie; Liu, Xiaojing; Zou, Yong; Xu, Xinjun

2018-05-01

The objective of this study was to develop a consecutive preparation method for the isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. The process involved supercritical fluid extraction with CO 2 , solvent extraction, and two-step high-speed countercurrent chromatography. Pressure, temperature, and the volume of entrainer were optimized as 27 MPa, 52°C, and 60 mL by response surface methodology in supercritical fluid extraction with CO 2 , and the yield of the crude extracts was 7.91 g from 100 g of leaves. Subsequently, 80% methanol/water was used to extract and condense the three compounds from the crude extracts, and 4.23 g of methanol/water extracts was obtained. Then, a two-step high-speed countercurrent chromatography procedure was developed for the isolation of the three target compounds from methanol/water extracts, including conventional high-speed countercurrent chromatography for further enrichment and consecutive high-speed countercurrent chromatography for purification. The yield of concentrates from high-speed countercurrent chromatography was 2.50 g from 4.23 g of methanol/water extracts. Finally, the consecutive high-speed countercurrent chromatography produced 103.2 mg of hainanmurpanin, 244.7 mg of meranzin, and 255.4 mg of phebalosin with purities up to 97.66, 99.36, and 98.64%, respectively, from 900 mg of high-speed countercurrent chromatography concentrates in one run of three consecutive sample loadings without exchanging a solvent system. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

PubMed

Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

2016-04-01

An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

PubMed

Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

2016-03-16

A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

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.

A comparison of certain extracting agents for extraction of adenosine triphosphate (ATP) from microorganisms for use in the firefly luciferase ATP assay

NASA Technical Reports Server (NTRS)

Knust, E. A.; Chappelle, E. W.; Picciolo, G. L.

1975-01-01

Firefly luciferase ATP assay is used in clinical and industrial applications, such as determination of urinary infection levels, microbial susceptibility testing, and monitoring of yeast levels in beverages. Three categories of extractants were investigated for their extracting efficiency. They were ionizing organic solvents, nonionizing organic solvents, and inorganic acids. Dimethylsulfoxide and formamide represented the ionizing organic solvents, while n-butanol, chloroform, ethanol, acetone, and methylene chloride were used for the nonionizing organic solvents. Nitric acid and perchloric acid were chosen for the inorganic acids category. Pathogens were tested with each solvent. They included: Saccharomyces carlsbergensis, E. coli, Staphylococcus aureus, Klebsiella pneumoniae, Enterobacter species, Proteus mirabilis, Proteus vulgaris, Staphylococcus epidermidis, Streptococcus faecalis, Pseudomonas aeruginosa, and Candida albicans. These results are shown in graphic representations.

AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

DOEpatents

Van Berkel, Gary J.

2015-06-23

An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

Optimisation of Croton gratissimus Oil Extraction by n-Hexane and Ethyl Acetate Using Response Surface Methodology.

PubMed

Jiyane, Phiwe Charles; Tumba, Kaniki; Musonge, Paul

2018-04-01

The extraction of oil from Croton gratissimus seeds was studied using the three-factor five-level full-factorial central composite rotatable design (CCRD) of the response surface methodology (RSM). The effect of the three factors selected, viz., extraction time, extraction temperature and solvent-to-feed ratio on the extraction oil yield was investigated when n-hexane and ethyl acetate were used as extraction solvents. The coefficients of determination (R 2 ) of the models developed were 0.98 for n-hexane extraction and 0.97 for ethyl acetate extraction. These results demonstrated that the models developed adequately represented the processes they described. From the optimized model, maximum extraction yield obtained from n-hexane and ethyl acetate extraction were 23.88% and 23.25%, respectively. In both cases the extraction temperature and solvent-to-feed ratio were 35°C and 5 mL/g, respectively. In n-hexane extraction the maximum conditions were reached only after 6 min whereas in ethyl acetate extraction it took 20 min to get the maximum extraction oil yield. Oil extraction of Croton gratissimus seeds, in this work, favoured the use of n-hexane as an extraction solvent as it offered higher oil yields at low temperatures and reduced residence times.

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.

Liquid-liquid extraction assisted by a carbon nanoparticles interface. Electrophoretic determination of atrazine in environmental samples.

PubMed

Caballero-Díaz, Encarnación; Simonet, Bartolomé; Valcárcel, Miguel

2013-10-21

A novel method for the determination of atrazine, using liquid-liquid extraction assisted by a nanoparticles film formed in situ and composed of organic solvent stabilized-carbon nanoparticles, is described. The presence of nanoparticles located at the liquid-liquid interface reinforced the extraction of analyte from matrix prior to capillary electrophoresis (CE) analysis. Some influential experimental variables were optimized in order to enhance the extraction efficiency. The developed procedure confirmed that carbon nanoparticles, especially multi-walled carbon nanotubes, are suitable to be used in sample treatment processes introducing new mechanisms of interaction with the analyte. The application of the proposed preconcentration method followed by CE detection enabled the determination of atrazine in spiked river water providing acceptable RSD values (11.6%) and good recoveries (about 87.0-92.0%). Additionally, a similar extraction scheme was tested in soil matrices with a view to further applications in real soil samples.

Development and Application of a Novel SPE-Method for Bioassay-Guided Fractionation of Marine Extracts

PubMed Central

Cutignano, Adele; Nuzzo, Genoveffa; Ianora, Adrianna; Luongo, Elvira; Romano, Giovanna; Gallo, Carmela; Sansone, Clementina; Aprea, Susanna; Mancini, Francesca; D’Oro, Ugo; Fontana, Angelo

2015-01-01

The biological diversity of marine habitats is a unique source of chemical compounds with potential use as pharmaceuticals, cosmetics and dietary supplements. However, biological screening and chemical analysis of marine extracts pose specific technical constraints and require adequate sample preparation. Here we report an improved method on Solid Phase Extraction (SPE) to fractionate organic extracts containing high concentration of salt that hampers the recovery of secondary metabolites. The procedure uses a water suspension to load the extracts on a poly(styrene-divynylbenzene)-based support and a stepwise organic solvent elution to effectively desalt and fractionate the organic components. The novel protocol has been tested on MeOH-soluble material from three model organisms (Reniera sarai, Dendrilla membranosa and Amphidinium carterae) and was validated on a small panel of 47 marine samples, including sponges and protists, within discovery programs for identification of immuno-stimulatory and anti-infective natural products. PMID:26378547

Bioactive molecules in Kalanchoe pinnata leaves: extraction, purification, and identification.

PubMed

El Abdellaoui, Saïda; Destandau, Emilie; Toribio, Alix; Elfakir, Claire; Lafosse, Michel; Renimel, Isabelle; André, Patrice; Cancellieri, Perrine; Landemarre, Ludovic

2010-10-01

Kalanchoe pinnata (Lam.) Pers. (syn. Bryophyllum pinnatum; family Crassulaceae) is a popular plant used in traditional medicine in many temperate regions of the world and particularly in South America. In Guyana, the leaves are traditionally used as an anti-inflammatory and antiseptic to treat coughs, ulcers, and sores. The purpose of this study was to implement a method for targeting and identifying molecules with antimicrobial activity, which could replace chemical preservatives in cosmetic applications. The leaves were extracted by a method based on pressurized liquid extraction (PLE), using different solvents. A study of antimicrobial activity and cytotoxicity tests were performed to select the most interesting extract. To isolate one or more active molecules, the selected crude extract was fractionated by centrifugal partition chromatography (CPC) and then antimicrobial activity and cytotoxicity of each fraction were tested under the same procedure. The last step consisted of identifying the main compounds in the most active fraction by LC-MS/MS.

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.

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.

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.

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.

Proximate composition, phytochemical analysis, and in vitro antioxidant potentials of extracts of Annona muricata (Soursop).

PubMed

Agu, Kingsley C; Okolie, Paulinus N

2017-09-01

Numerous bioactive compounds and phytochemicals have been reported to be present Annona muricata (Soursop). Some of these chemical compounds have been linked to the ethnomedicinal properties of the plant and its antioxidant properties. The aim of this study was to assess the proximate composition, phytochemical constituents and in vitro antioxidant properties of A. muricata using standard biochemical procedures. The defatted Annona muricata crude methanolic extracts of the different parts of the plant were used for the estimation of proximate composition and phytochemical screening. The crude methanolic extracts of the different parts of the plant were also fractionated using solvent-solvent partitioning. Petroleum ether, chloroform, ethyl acetate, methanol, and methanol-water (90:10) were the solvents used for the fractionation. The different fractions obtained were then used to perform in vitro antioxidant analyses including, 1, 1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging ability, ferric reducing properties, and hydroxyl radical scavenging ability. The leaf methanolic extract had a higher lipid content, whereas its chloroform fraction demonstrated a better ability to quench DPPH free radical. The root-bark methanol-water, leaf methanol, fruit pulp chloroform, and leaf petroleum ether fractions demonstrated potent ferric reducing properties. The leaf and stem-bark petroleum ether fractions demonstrated better hydroxyl-free radical scavenging abilities. The leaf and fruit pulp of Annona muricata have a very potent antioxidant ability compared to the other parts of the plant. This can be associated with the rich phytochemicals and other phytoconstituents like phenols, flavonoids, alkaloids, and essential lipids, etc. Significant correlations were observed between the antioxidant status and phytochemicals present. These results thus suggest that some of the reported ethnomedicinal properties of this plant could be due to its antioxidant potentials.

[Determination of serum or plasma alpha-tocopherol by high performance liquid chromatography: optimization of operative models].

PubMed

Jezequel-Cuer, M; Le Moël, G; Mounié, J; Peynet, J; Le Bizec, C; Vernet, M H; Artur, Y; Laschi-Loquerie, A; Troupel, S

1995-01-01

A previous multicentric study set up by the Société française de biologie clinique has emphasized the usefulness of a standardized procedure for the determination by high performance liquid chromatography of alpha-tocopherol in serum or plasma. In our study, we have tested every step of the different published procedures: internal standard adduct, lipoprotein denaturation and vitamin extraction. Reproducibility of results was improved by the use of tocol as an internal standard when compared to retinol or alpha-tocopherol acetates. Lipoprotein denaturation was more efficient with ethanol addition than with methanol and when the ethanol/water ratio was > or = 0.7. Use of n-hexane or n-heptane gave the same recovery of alpha-tocopherol. When organic solvent/water ratio was > or = 1, n-hexane enabled to efficiently extract, in a one-step procedure, the alpha-tocopherol from both normo and hyperlipidemic sera. Performances of the selected procedure were: detection limit: 0.5 microM--linear range: 750 microM--within run coefficient of variation: 2.03%--day to day: 4.76%. Finally, this pluricentric study allows us to propose an optimised procedure for the determination of alpha-tocopherol in serum or plasma.

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.

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.

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.

Mosquitocidal Effect of Glycosmis pentaphylla Leaf Extracts against Three Mosquito Species (Diptera: Culicidae)

PubMed Central

Ramkumar, Govindaraju; Karthi, Sengodan; Muthusamy, Ranganathan; Suganya, Ponnusamy; Natarajan, Devarajan; Kweka, Eliningaya J.; Shivakumar, Muthugounder S.

2016-01-01

Background The resistance status of malaria vectors to different classes of insecticides used for public health has raised concern for vector control programmes. Alternative compounds to supplement the existing tools are important to be searched to overcome the existing resistance and persistence of pesticides in vectors and the environment respectively. The mosquitocidal effects of Glycosmis pentaphylla using different solvents of acetone, methanol, chloroform and ethyl acetate extracts against three medically important mosquito vectors was conducted. Methods Glycosmis pentaphylla plant leaves were collected from Kolli Hills, India. The WHO test procedures for larval and adult bioassays were used to evaluate extracts against mosquito vectors, and the chemical composition of extracts identified using GC-MS analysis. Results The larvicidal and adulticidal activity of G. pentaphylla plant extracts clearly impacted the three species of major mosquitoes vectors. Acetone extracts had the highest larvicidal effect against An. stephensi, Cx. quinquefasciatus and Ae. aegypti with the LC50 and LC90 values of 0.0004, 138.54; 0.2669, 73.7413 and 0.0585, 303.746 mg/ml, respectively. The LC50 and LC90 adulticide values of G. pentaphylla leaf extracts in acetone, methanol, chloroform and ethyl acetate, solvents were as follows for Cx. quinquefasciatus, An. stephensi and Ae. Aegypti: 2.957, 5.458, 2.708, and 4.777, 3.449, 6.676 mg/ml respectively. The chemical composition of G. pentaphylla leaf extract has been found in 20 active compounds. Conclusions The plant leaf extracts of G. pentaphylla bioactive molecules which are effective and can be developed as an eco-friendly approach for larvicides and adulticidal mosquitoes vector control. Detailed identification and characterization of mosquitocidal effect of individual bioactive molecules ingredient may result into biodegradable effective tools for the control of mosquito vectors. PMID:27391146

Mosquitocidal Effect of Glycosmis pentaphylla Leaf Extracts against Three Mosquito Species (Diptera: Culicidae).

PubMed

Ramkumar, Govindaraju; Karthi, Sengodan; Muthusamy, Ranganathan; Suganya, Ponnusamy; Natarajan, Devarajan; Kweka, Eliningaya J; Shivakumar, Muthugounder S

2016-01-01

The resistance status of malaria vectors to different classes of insecticides used for public health has raised concern for vector control programmes. Alternative compounds to supplement the existing tools are important to be searched to overcome the existing resistance and persistence of pesticides in vectors and the environment respectively. The mosquitocidal effects of Glycosmis pentaphylla using different solvents of acetone, methanol, chloroform and ethyl acetate extracts against three medically important mosquito vectors was conducted. Glycosmis pentaphylla plant leaves were collected from Kolli Hills, India. The WHO test procedures for larval and adult bioassays were used to evaluate extracts against mosquito vectors, and the chemical composition of extracts identified using GC-MS analysis. The larvicidal and adulticidal activity of G. pentaphylla plant extracts clearly impacted the three species of major mosquitoes vectors. Acetone extracts had the highest larvicidal effect against An. stephensi, Cx. quinquefasciatus and Ae. aegypti with the LC50 and LC90 values of 0.0004, 138.54; 0.2669, 73.7413 and 0.0585, 303.746 mg/ml, respectively. The LC50 and LC90 adulticide values of G. pentaphylla leaf extracts in acetone, methanol, chloroform and ethyl acetate, solvents were as follows for Cx. quinquefasciatus, An. stephensi and Ae. Aegypti: 2.957, 5.458, 2.708, and 4.777, 3.449, 6.676 mg/ml respectively. The chemical composition of G. pentaphylla leaf extract has been found in 20 active compounds. The plant leaf extracts of G. pentaphylla bioactive molecules which are effective and can be developed as an eco-friendly approach for larvicides and adulticidal mosquitoes vector control. Detailed identification and characterization of mosquitocidal effect of individual bioactive molecules ingredient may result into biodegradable effective tools for the control of mosquito vectors.

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

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

PubMed

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

2015-12-01

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

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

PubMed

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

2017-01-01

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

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...

Ultrasound-assisted oxidative process for sulfur removal from petroleum product feedstock.

PubMed

Mello, Paola de A; Duarte, Fábio A; Nunes, Matheus A G; Alencar, Mauricio S; Moreira, Elizabeth M; Korn, Mauro; Dressler, Valderi L; Flores, Erico M M

2009-08-01

A procedure using ultrasonic irradiation is proposed for sulfur removal of a petroleum product feedstock. The procedure involves the combination of a peroxyacid and ultrasound-assisted treatment in order to comply with the required sulfur content recommended by the current regulations for fuels. The ultrasound-assisted oxidative desulfurization (UAOD) process was applied to a petroleum product feedstock using dibenzothiophene as a model sulfur compound. The influence of ultrasonic irradiation time, oxidizing reagents amount, kind of solvent for the extraction step and kind of organic acid were investigated. The use of ultrasonic irradiation allowed higher efficiency for sulfur removal in comparison to experiments performed without its application, under the same reactional conditions. Using the optimized conditions for UAOD, the sulfur removal was about 95% after 9min of ultrasonic irradiation (20kHz, 750W, run at 40%), using hydrogen peroxide and acetic acid, followed by extraction with methanol.

UNIT 10.7 Electroblotting from Polyacrylamide Gels

PubMed Central

Goldman, Aaron; Speicher, David W.

2015-01-01

Transferring proteins from polyacrylamide gels onto retentive membranes is now primarily used for immunoblotting. A second application that was quite common up to about a decade ago was electroblotting of proteins for N-terminal and internal sequencing using Edman chemistry. This unit contains procedures for electroblotting proteins from polyacrylamide gels onto a variety of membranes, including polyvinylidene difluoride (PVDF) and nitrocellulose. In addition to the commonly used tank or wet transfer system, protocols are provided for electroblotting using semidry and dry systems. This unit also describes procedures for eluting proteins from membranes using detergents or acidic extraction with organic solvents for specialized applications. PMID:26521711

Electroblotting from Polyacrylamide Gels.

PubMed

Goldman, Aaron; Ursitti, Jeanine A; Mozdzanowski, Jacek; Speicher, David W

2015-11-02

Transferring proteins from polyacrylamide gels onto retentive membranes is now primarily used for immunoblotting. A second application that was quite common up to about a decade ago was electroblotting of proteins for N-terminal and internal sequencing using Edman chemistry. This unit contains procedures for electroblotting proteins from polyacrylamide gels onto a variety of membranes, including polyvinylidene difluoride (PVDF) and nitrocellulose. In addition to the commonly used tank or wet transfer system, protocols are provided for electroblotting using semidry and dry systems. This unit also describes procedures for eluting proteins from membranes using detergents or acidic extraction with organic solvents for specialized applications. Copyright © 2015 John Wiley & Sons, Inc.

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

PubMed

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

2009-01-01

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

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

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.

Chemical isolation of .sup.82 Sr from proton-irradiated Mo targets

DOEpatents

Grant, Patrick M.; Kahn, Milton; O'Brien, Jr., Harold A.

1976-01-01

Spallation reactions are induced in Mo targets with 200-800 MeV protons to produce microcurie to millicurie amounts of a variety of radionuclides. A six-step radiochemical procedure, incorporating precipitation, solvent extractions, and ion exchange techniques, has been developed for the separation and purification of Sr radioactivities from other spallation products and the bulk target material. Radiostrontium can be quantitatively recovered in a sufficiently decontaminated state for use in biomedical generator development.

Multianalyte, high-throughput liquid chromatography tandem mass spectrometry method for the sensitive determination of fungicides and insecticides in wine.

PubMed

Castro, Gabriela; Pérez-Mayán, Leticia; Rodríguez-Cabo, Tamara; Rodríguez, Isaac; Ramil, Maria; Cela, Rafael

2018-01-01

Evidence of pesticide transfer from grapes to wine, added to differences in the national regulations regarding the number and the maximum concentration of these species in wine, demands analytical procedures suitable for their routine control in this foodstuff. In this research, solid-phase extraction (SPE) and ultra-performance liquid chromatography (UPLC), with tandem mass spectrometry (MS/MS) detection, are combined to obtain a sensitive and rapid procedure to determine 50 pesticides in red and white wines. Efficiency and selectivity of sample preparation are correlated with the type of sorbent, the elution solvent, and the physicochemical properties of pesticides. SPE of 2-mL wine samples followed by direct injection of the extract in the UPLC-MS/MS system provides quantification limits (LOQs) below 1 ng mL -1 for 48 out of 50 compounds, linear responses up to 200 ng mL -1 , and acceptable accuracy, employing quantification against solvent-based standards, for 45 species. A total analysis time of 10 min, including compounds separation and re-equilibration of the UPLC column, was achieved. The developed methodology was applied to 25 wines (20 conventional and 5 ecological), produced in 7 different countries. Out of 27 pesticides quantified in these wines, 12 displayed occurrence frequencies above 24%; moreover, all wines, except one of the ecological ones, contained residues from at least one pesticide.

SOLVENT EXTRACTION PROCESSES: A SURVEY OF SYSTEMS IN THE SITE PROGRAM

EPA Science Inventory

Solvent extraction of contaminated soils, sludges and sediments has been successfully completed at a number ofSuperfund sites. Each commercialized process uses a unique operating system to extract organic contaminants from solids. These operating systems may be classified by the ...

Effective recovery of poly-β-hydroxybutyrate (PHB) biopolymer from Cupriavidus necator using a novel and environmentally friendly solvent system.

PubMed

Fei, Tao; Cazeneuve, Stacy; Wen, Zhiyou; Wu, Lei; Wang, Tong

2016-05-01

This work demonstrates a significant advance in bioprocessing for a high-melting lipid polymer. A novel and environmental friendly solvent mixture, acetone/ethanol/propylene carbonate (A/E/P, 1:1:1 v/v/v) was identified for extracting poly-hydroxybutyrate (PHB), a high-value biopolymer, from Cupriavidus necator. A set of solubility curves of PHB in various solvents was established. PHB recovery of 85% and purity of 92% were obtained from defatted dry biomass (DDB) using A/E/P. This solvent mixture is compatible with water, and from non-defatted wet biomass, PHB recovery of 83% and purity of 90% were achieved. Water and hexane were evaluated as anti-solvents to assist PHB precipitation, and hexane improved recovery of PHB from biomass to 92% and the purity to 93%. A scale-up extraction and separation reactor was designed, built and successfully tested. Properties of PHB recovered were not significantly affected by the extraction solvent and conditions, as shown by average molecular weight (1.4 × 10(6) ) and melting point (175.2°C) not being different from PHB extracted using chloroform. Therefore, this biorenewable solvent system was effective and versatile for extracting PHB biopolymers. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:678-685, 2016. © 2016 American Institute of Chemical Engineers.

Intensification of extraction of curcumin from Curcuma amada using ultrasound assisted approach: Effect of different operating parameters.

PubMed

Shirsath, S R; Sable, S S; Gaikwad, S G; Sonawane, S H; Saini, D R; Gogate, P R

2017-09-01

Curcumin, a dietary phytochemical, has been extracted from rhizomes of Curcuma amada using ultrasound assisted extraction (UAE) and the results compared with the conventional extraction approach to establish the process intensification benefits. The effect of operating parameters such as type of solvent, extraction time, extraction temperature, solid to solvent ratio, particle size and ultrasonic power on the extraction yield have been investigated in details for the approach UAE. The maximum extraction yield as 72% was obtained in 1h under optimized conditions of 35°C temperature, solid to solvent ratio of 1:25, particle size of 0.09mm, ultrasonic power of 250W and ultrasound frequency of 22kHz with ethanol as the solvent. The obtained yield was significantly higher as compared to the batch extraction where only about 62% yield was achieved in 8h of treatment. Peleg's model was used to describe the kinetics of UAE and the model showed a good agreement with the experimental results. Overall, ultrasound has been established to be a green process for extraction of curcumin with benefits of reduction in time as compared to batch extraction and the operating temperature as compared to Soxhlet extraction. Copyright © 2017. Published by Elsevier B.V.

Comparative Analysis of the Properties of Acid-Base Indicator of Rose (Rosa setigera), Allamanda (Allamanda cathartica), and Hibiscus (Hibiscus rosa-sinensis) Flowers

PubMed Central

Okoduwa, Stanley I. R.; Mbora, Lovina O.; Adu, Matthew E.; Adeyi, Ameh A.

2015-01-01

The need to develop effective alternative for synthetic indicators is the demand of present-day chemistry. The acid-base indicator properties of Rose (Rosa setigera), Allamanda (Allamanda cathartica), and Hibiscus (Hibiscus rosa-sinensis) flowers were examined. Colour pigments were extracted from the flowers via cold and solvent extraction using soxhlet extractor. The pH value of the extracts with wavelengths of absorption was determined using ultraviolet spectrophotometer. From the results obtained, all the extracts exhibited sharp contrast between their colours in acid and base. Their pH was found to be 5.5 for cold extract of Rose and 5.6 for solvent extraction, 5.24 for cold extract of a Hibiscus and 6.52 for solvent extraction, 5.35 for cold extract of Allamanda, and 5.45 for solvent extraction. The maximum wavelengths of absorption obtained for all the extract fall within the visible region of electromagnetic spectrum. These values are almost similar to that obtained from synthetic indicators. It is on these bases that we concluded that natural indicators could be an excellent replacement for synthetic indicators since they are cheap, readily available, simple to extract, not toxic, user and environmentally friendly. PMID:26819757

Maximizing Lipid Yield in Neochloris oleoabundans Algae Extraction by Stressing and Using Multiple Extraction Stages with N-Ethylbutylamine as Switchable Solvent

PubMed Central

2017-01-01

The extraction yield of lipids from nonbroken Neochloris oleoabundans was maximized by using multiple extraction stages and using stressed algae. Experimental parameters that affect the extraction were investigated. The study showed that with wet algae (at least) 18 h extraction time was required for maximum yield at room temperature and a solvent/feed ratio of 1:1 (w/w). For fresh water (FW), nonstressed, nonbroken Neochloris oleoabundans, 13.1 wt % of lipid extraction yield (based on dry algae mass) was achieved, which could be improved to 61.3 wt % for FW stressed algae after four extractions, illustrating that a combination of stressing the algae and applying the solvent N-ethylbutylamine in multiple stages of extraction results in almost 5 times higher yield and is very promising for further development of energy-efficient lipid extraction technology targeting nonbroken wet microalgae. PMID:28781427

LPS-induced NO inhibition and antioxidant activities of ethanol extracts and their solvent partitioned fractions from four brown seaweeds

NASA Astrophysics Data System (ADS)

Cho, Myoung Lae; Lee, Dong-Jin; Lee, Hyi-Seung; Lee, Yeon-Ju; You, Sang Guan

2013-12-01

The nitric oxide inhibitory (NOI) and antioxidant (ABTS and DPPH radical scavenging effects with reducing power) activities of the ethanol (EtOH) extracts and solvent partitioned fractions from Scytosiphon lomentaria, Chorda filum, Agarum cribrosum, and Desmarestia viridis were investigated, and the correlation between biological activity and total phenolic (TP) and phlorotannin (TPT) content was determined by PCA analysis. The yield of EtOH extracts from four brown seaweeds ranged from 2.6 to 6.6% with the highest yield from D. viridis, and the predominant compounds in their solvent partitioned fractions had medium and/or less polarity. The TP and TPT content of the EtOH extracts were in the ranges of 25.0-44.1 mg GAE/g sample and 0.2-4.6 mg PG/g sample, respectively, which were mostly included in the organic solvent partitioned fractions. Strong NOI activity was observed in the EtOH extracts and their solvent partitioned fractions from D. viridis and C. filum. In addition, the EtOH extract and its solvent partitioned fractions of D. viridis exhibited little cytotoxicity to Raw 264.7 cells. The most potent ABTS and DPPH radical scavenging capacity was shown in the EtOH extracts and their solvent partitioned fractions from S. lomentaria and C. filum, and both also exhibited strong reducing ability. In the PCA analysis the content of TPT had a good correlation with DPPH ( r = 0.62), ABTS ( r = 0.69) and reducing power ( r = 0.65), however, an unfair correlation was observed between the contents of TP and TPT and NOI, suggesting that the phlorotannins might be responsible for the DPPH and ABTS radical scavenging activities.

Use of solvent mixtures for total lipid extraction of Chlorella vulgaris and gas chromatography FAME analysis.

PubMed

Moradi-Kheibari, Narges; Ahmadzadeh, Hossein; Hosseini, Majid

2017-09-01

Lipid extraction is the bottleneck step for algae-based biodiesel production. Herein, 12 solvent mixture systems (mixtures of three non-polar and two polar organic solvents) were examined to evaluate their effects on the total lipid yield from Chlorella vulgaris (C. vulgaris). Moreover, the extraction yields of three solvent systems with maximum extraction efficiency of esterifiable lipids were determined by acidic transesterification and GC-FID analysis. Three solvent systems, which resulted in a higher extraction yield, were further subjected to fatty acid methyl ester (FAME) analysis. The total lipid extraction yields (based on dry biomass) were (38.57 ± 1.51), (25.33 ± 0.58), and (25.17 ± 1.14) %, for chloroform-methanol (1:2) (C1M2), hexane-methanol (1:2) (H1M2), and chloroform-methanol (2:1) (C2M1), respectively. The extraction efficiency of C1M2 was approximately 1.5 times higher than H1M2 and C2M1, whereas the FAME profile of extracted lipids by H1M2 and C1M2 were almost identical. Moreover, the esterifiable lipid extraction yields of (18.14 ± 2.60), (16.66 ± 0.35), and (13.22 ± 0.31) % (based on dry biomass) were obtained for C1M2, H1M2, and C2M1 solvent mixture systems, respectively. The biodiesel fuel properties produced from C. vulgaris were empirically predicted and compared to that of the EN 14214 and ASTM 6751 standard specifications.

A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

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

Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani

Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

DOE PAGES

Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani; ...

2017-07-11

Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

Impact of quality parameters on the recovery of putrescine and cadaverine in fish using methanol-hydrochloric acid solvent extraction.

PubMed

Richard, Nicole L; Pivarnik, Lori F; Ellis, P Christopher; Lee, Chong M

2011-01-01

Methanol (MeOH) extraction by AOAC Official Method 996.07 has resulted in low amine recoveries in fresh fish tissue. Addition of 25% 0.4 M HCl to the 75% methanol-water extraction solvent resulted in higher recoveries of putrescine and cadaverine. Average putrescine recovery increased from 55 to 92% in flounder, scup, bluefish, and salmon; from 92 to 98% in mackerel; and from 83 to 107% in processed mackerel. Average cadaverine recovery increased from 57 to 95% in flounder, scup, bluefish, and salmon; from 91 to 97% in mackerel; and from 92 to 108% in processed mackerel. Fish stored on ice for 12 days also showed differences between background concentrations determined with the two solvents. However, the values decreased with storage time, indicating that degradation of the protein matrix may cause more comparable measurements between the two solvents. However, consistently higher putrescine and cadaverine measurements were determined using MeOH-HCl. Although significant differences in the extraction of amines from the high-fat fish tissue were not seen between MeOH and MeOH-HCl, it would be ideal to have one solvent for biogenic amine extraction. This study confirms that MeOH-HCl is a better solvent for complete extraction and recovery of putrescine and cadaverine in fresh and processed fish tissues.

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.

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

40 CFR 60.624 - Test methods and procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

...-water separator. Near the end of the recovery cycle, the entire flow of recovered solvent should be... solvent from the solvent recovery dryer at the termination of the recovery cycle is no greater than 0.05... cycle and the monitoring procedure should continue until the flow rate of solvent is less than or equal...

40 CFR 60.624 - Test methods and procedures.

Code of Federal Regulations, 2014 CFR

2014-07-01

...-water separator. Near the end of the recovery cycle, the entire flow of recovered solvent should be... solvent from the solvent recovery dryer at the termination of the recovery cycle is no greater than 0.05... cycle and the monitoring procedure should continue until the flow rate of solvent is less than or equal...

40 CFR 60.624 - Test methods and procedures.

Code of Federal Regulations, 2013 CFR

2013-07-01

...-water separator. Near the end of the recovery cycle, the entire flow of recovered solvent should be... solvent from the solvent recovery dryer at the termination of the recovery cycle is no greater than 0.05... cycle and the monitoring procedure should continue until the flow rate of solvent is less than or equal...

40 CFR 60.624 - Test methods and procedures.

Code of Federal Regulations, 2012 CFR

2012-07-01

...-water separator. Near the end of the recovery cycle, the entire flow of recovered solvent should be... solvent from the solvent recovery dryer at the termination of the recovery cycle is no greater than 0.05... cycle and the monitoring procedure should continue until the flow rate of solvent is less than or equal...

Determination of ochratoxin A and T-2 toxin in alcoholic beverages by hollow fiber liquid phase microextraction and ultra high-pressure liquid chromatography coupled to tandem mass spectrometry.

PubMed

Romero-González, R; Frenich, A Garrido; Vidal, J L Martínez; Aguilera-Luiz, M M

2010-06-30

A new method for the determination of ochratoxin A and T-2 toxin in alcoholic beverages (wine and beer) by hollow fiber liquid microextraction was optimized. The extraction step was followed by ultra high-pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The extraction procedure was based on the extraction of mycotoxins from the sample to the organic solvent (1-octanol) immobilized in the fiber, and afterwards, they were desorbed in a mixture of acetonitrile/water (80:20, v/v) at pH 7 prior to chromatographic determination. Different variables affecting the extraction process such as organic solvent, salt content, extraction time and desorption solution were studied. The developed method was validated in wine and beer, using white wine and alcoholic beer as representative matrices for both types of samples. Relative recoveries higher than 70% were obtained for the selected mycotoxins. Good linearity (R(2)>0.993) was obtained and quantification limits (0.02-0.09 microg L(-1)) below European regulatory levels were achieved. Repeatability, expressed as relative standard deviation, was always lower than 12%, whereas interday precision was lower than 21%. The proposed method was applied to the analysis of several types of wines and beers and ochratoxin A was detected in a rosé wine at 1.1 microg L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

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.

Spectrophotometric Quantification of Flavonoids in Herbal Material, Crude Extract, and Fractions from Leaves of Eugenia uniflora Linn.

PubMed

Ramos, Rhayanne T M; Bezerra, Isabelle C F; Ferreira, Magda R A; Soares, Luiz Alberto Lira

2017-01-01

The traditional use of Eugenia uniflora L. ("Pitanga") is reported due to several properties, which have often been related to its flavonoid content. The aim was to evaluate analytical procedures for quantification of total flavonoids content (TFCs) by ultraviolet-visible (UV-Vis) spectrophotometry in the herbal material (HM), crude extract (CE), and fractions from leaves of E. uniflora . The method for quantification of flavonoids after complexation with aluminum chloride (AlCl 3 ) was evaluated: amount of sample (0.25-1.5 g); solvent (40%-80% ethanol); reaction time and AlCl 3 concentration (2.5%-7.5%). The procedures by direct dilution (DD) and after acid hydrolysis (AH) were used and validated for HM and CE and applied to the aqueous fraction (AqF), hexane fraction, and ethyl acetate fractions (EAF). The ideal conditions of analysis were ethanol 80% as solvent; 0.5 g of sample; λmax of 408 (DD) and 425 nm (AH); 25 min after addition of AlCl 3 5%. The procedures validated for standards and samples showed linearity ( R 2 > 0.99) with limit of detection and limit of quantification between 0.01 and 0.17 mg/mL (rutin and quercetin); and 0.03 and 0.09 mg/mL (quercetin), for DD and AH, respectively. The procedures were accurate (detect, practice, and repair < 5% and recovery >90%), and stable under robustness conditions (luminosity, storage, reagents, and equipment). The TFCs in AqF and EAF were 0.65 g% and 17.72 g%, calculated as rutin. UV-Vis methods for quantification of TFC in HM, CE, and fractions from leaves of E. uniflora were suitably validated. Regarding the analysis of fractions, the EAF achieved enrichment of about nine times in the content of flavonoids. The total flavonoids content (TFCs) of herbal material, crude extract, and fractions from Eugenia uniflora can be quantified by ultraviolet-visibleThe spectrophotometric methods (direct dilution and acid hydrolysis) were reproducible and able to quantify TFC in raw material and derivatives from leaves of E. uniflora Higher flavonoids content was observed in ethyl acetate fractions after enrichment. Abbreviations Used : HM: Herbal material, CE: Crude extract, AqF: Aqueous fraction, HF: Hexanic fraction, EAF: Ethyl acetate fraction, TFC: Total flavonoids content, HCl: Hydrochloric acid, DD: Direct dilution, AH: After hydrolysis, RSD: Relative standard, A.U.: Absorption units.

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

Pumpkin (Cucurbita maxima) seed proteins: sequential extraction processing and fraction characterization.

PubMed

Rezig, Leila; Chibani, Farhat; Chouaibi, Moncef; Dalgalarrondo, Michèle; Hessini, Kamel; Guéguen, Jacques; Hamdi, Salem

2013-08-14

Seed proteins extracted from Tunisian pumpkin seeds ( Cucurbita maxima ) were investigated for their solubility properties and sequentially extracted according to the Osborne procedure. The solubility of pumpkin proteins from seed flour was greatly influenced by pH changes and ionic strength, with higher values in the alkaline pH regions. It also depends on the seed defatting solvent. Protein solubility was decreased by using chloroform/methanol (CM) for lipid extraction instead of pentane (P). On the basis of differential solubility fractionation and depending on the defatting method, the alkali extract (AE) was the major fraction (42.1 (P), 22.3% (CM)) compared to the salt extract (8.6 (P), 7.5% (CM)). In salt, alkali, and isopropanol extracts, all essential amino acids with the exceptions of threonine and lysine met the minimum requirements for preschool children (FAO/WHO/UNU). The denaturation temperatures were 96.6 and 93.4 °C for salt and alkali extracts, respectively. Pumpkin protein extracts with unique protein profiles and higher denaturation temperatures could impart novel characteristics when used as food ingredients.

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.

Optimisation of the microplate resazurin assay for screening and bioassay-guided fractionation of phytochemical extracts against Mycobacterium tuberculosis.

PubMed

O'Neill, Taryn E; Li, Haoxin; Colquhoun, Caitlyn D; Johnson, John A; Webster, Duncan; Gray, Christopher A

2014-01-01

Because of increased resistance to current drugs, there is an urgent need to discover new anti-mycobacterial compounds for the development of novel anti-tuberculosis drugs. The microplate resazurin assay (MRA) is commonly used to evaluate natural products and synthetic compounds for anti-mycobacterial activity. However, the assay can be problematic and unreliable when screening methanolic phytochemical extracts. To optimise the MRA for the screening and bioassay-guided fractionation of phytochemical extracts using Mycobacterium tuberculosis H37Ra. The effects of varying assay duration, resazurin solution composition, solvent (dimethyl sulphoxide - DMSO) concentration and type of microtitre plate used on the results and reliability of the MRA were investigated. The optimal bioassay protocol was applied to methanolic extracts of medicinal plants that have been reported to possess anti-mycobacterial activity. The variables investigated were found to have significant effects on the results obtained with the MRA. A standardised procedure that can reliably quantify anti-mycobacterial activity of phytochemical extracts in as little as 48 h was identified. The optimised MRA uses 2% aqueous DMSO, with an indicator solution of 62.5 µg/mL resazurin in 5% aqueous Tween 80 over 96 h incubation. The study has identified an optimal procedure for the MRA when used with M. tuberculosis H37Ra that gives rapid, reliable and consistent results. The assay procedure has been used successfully for the screening and bioassay-guided fractionation of anti-mycobacterial compounds from methanol extracts of Canadian medicinal plants. Copyright © 2014 John Wiley & Sons, Ltd.

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.

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...

Ethanolic extraction, purification, and partial characterization of a fluorescent toxin from the coral reef crab, Lophozozymus pictor.

PubMed

Lau, C O; Tan, C H; Khoo, H E; Li, Q T; Yuen, R

1995-01-01

A purification procedure for Lophozozymus pictor toxin (LPTX) following ethanolic extraction of whole crab homogenate is described. The ethanol-extracted toxin (LPTX-E) had higher yield and specific activity than the hot aqueous-extracted one (LPTX-H). It was found that LPTX-E was fluorescent and cochromatographed with LPTX-H on two-dimensional thin-layer chromatography. Although LPTX-E, LPTX-H, and palytoxin (P. caribaeorum, PTX) had similar migration and retention times when analysed on high performance capillary electrophoresis and gel permeation-high performance liquid chromatography respectively, LPTX-E and LPTX-H were both fluorescent in contrast to PTX. In addition, LPTX-E had a different retention time compared with PTX when chromatographed on reversed phase high performance liquid chromatography in the solvent system 80% acetonitrile and 0.02 M Tris-HCl, pH 7.2, at a 4:1 ratio, respectively, indicating some differences in their chemical structures.