Optimization of pressurized liquid extraction of inositols from pine nuts (Pinus pinea L.).

PubMed

Ruiz-Aceituno, L; Rodríguez-Sánchez, S; Sanz, J; Sanz, M L; Ramos, L

2014-06-15

Pressurized liquid extraction (PLE) has been used for the first time to extract bioactive inositols from pine nuts. The influence of extraction time, temperature and cycles of extraction in the yield and composition of the extract was studied. A quadratic lineal model using multiple linear regression in the stepwise mode was used to evaluate possible trends in the process. Under optimised PLE conditions (50°C, 18 min, 3 cycles of 1.5 mL water each one) at 10 MPa, a noticeable reduction in extraction time and solvent volume, compared with solid-liquid extraction (SLE; room temperature, 2h, 2 cycles of 5 mL water each one) was achieved; 5.7 mg/g inositols were extracted by PLE, whereas yields of only 3.7 mg/g were obtained by SLE. Subsequent incubation of PLE extracts with Saccharomyces cerevisiae (37°C, 5h) allowed the removal of other co-extracted low molecular weight carbohydrates which may interfere in the bioactivity of inositols. Copyright © 2014 Elsevier Ltd. All rights reserved.

Isolation of Gregatin A from Phialophora gregata by Preparative High-Pressure Liquid Chromatography

PubMed Central

Taylor, Scott L.; Peterson, Robert E.; Gray, Lynn E.

1985-01-01

A method was developed for the production and purification of gregatin A from Phialophora gregata NRRL 13198 cultured on rice at 20°C for 28 days. Liquid extraction followed by high-pressure liquid chromatography afforded 247.0 mg of crystalline gregatin A per kg of rice. PMID:16346936

Rapid and quantitative determination of 10 major active components in Lonicera japonica Thunb. by ultrahigh pressure extraction-HPLC/DAD

NASA Astrophysics Data System (ADS)

Fan, Li; Lin, Changhu; Duan, Wenjuan; Wang, Xiao; Liu, Jianhua; Liu, Feng

2015-01-01

An ultrahigh pressure extraction (UPE)-high performance liquid chromatography (HPLC)/diode array detector (DAD) method was established to evaluate the quality of Lonicera japonica Thunb. Ten active components, including neochlorogenic acid, chlorogenic acid, 4-dicaffeoylquinic acid, caffeic acid, rutin, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and quercetin, were qualitatively evaluated and quantitatively determined. Scanning electron microscope images elucidated the bud surface microstructure and extraction mechanism. The optimal extraction conditions of the UPE were 60% methanol solution, 400 MPa of extraction pressure, 3 min of extraction time, and 1:30 (g/mL) solid:liquid ratio. Under the optimized conditions, the total extraction yield of 10 active components was 57.62 mg/g. All the components showed good linearity (r2 ≥ 0.9994) and recoveries. This method was successfully applied to quantify 10 components in 22 batches of L. japonica samples from different areas. Compared with heat reflux extraction and ultrasonic-assisted extraction, UPE can be considered as an alternative extraction technique for fast extraction of active ingredient from L. japonica.

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.

Extraction of S- and N-compounds from the mixture of hydrocarbons by ionic liquids as selective solvents.

PubMed

Gabrić, Beata; Sander, Aleksandra; Cvjetko Bubalo, Marina; Macut, Dejan

2013-01-01

Liquid-liquid extraction is an alternative method that can be used for desulfurization and denitrification of gasoline and diesel fuels. Recent approaches employ different ionic liquids as selective solvents, due to their general immiscibility with gasoline and diesel, negligible vapor pressure, and high selectivity to sulfur- and nitrogen-containing compounds. For that reason, five imidazolium-based ionic liquids and one pyridinium-based ionic liquid were selected for extraction of thiophene, dibenzothiophene, and pyridine from two model solutions. The influences of hydrodynamic conditions, mass ratio, and number of stages were investigated. Increasing the mass ratio of ionic liquid/model fuel and multistage extraction promotes the desulfurization and denitrification abilities of the examined ionic liquids. All selected ionic liquids can be reused and regenerated by means of vacuum evaporation.

Extraction of S- and N-Compounds from the Mixture of Hydrocarbons by Ionic Liquids as Selective Solvents

PubMed Central

Gabrić, Beata; Sander, Aleksandra; Cvjetko Bubalo, Marina; Macut, Dejan

2013-01-01

Liquid-liquid extraction is an alternative method that can be used for desulfurization and denitrification of gasoline and diesel fuels. Recent approaches employ different ionic liquids as selective solvents, due to their general immiscibility with gasoline and diesel, negligible vapor pressure, and high selectivity to sulfur- and nitrogen-containing compounds. For that reason, five imidazolium-based ionic liquids and one pyridinium-based ionic liquid were selected for extraction of thiophene, dibenzothiophene, and pyridine from two model solutions. The influences of hydrodynamic conditions, mass ratio, and number of stages were investigated. Increasing the mass ratio of ionic liquid/model fuel and multistage extraction promotes the desulfurization and denitrification abilities of the examined ionic liquids. All selected ionic liquids can be reused and regenerated by means of vacuum evaporation. PMID:23843736

A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry.

PubMed

Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Russo, Mariateresa; Valdés, Alberto; Ibáñez, Clara; Rastrelli, Luca

2015-04-01

According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30%) at 110 °C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103%) and repeatability (RSD < 8, n = 3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling high-throughput analysis and highly accurate and precise results.

Capillary liquid chromatography combined with pressurized liquid extraction and dispersive liquid-liquid microextraction for the determination of vitamin E in cosmetic products.

PubMed

Viñas, Pilar; Pastor-Belda, Marta; Campillo, Natalia; Bravo-Bravo, María; Hernández-Córdoba, Manuel

2014-06-01

Capillary liquid chromatography (LC) is used for the determination of tocopherols and tocotrienols in cosmetic products. Dispersive liquid-liquid microextraction (DLLME) allows the analytes to be preconcentrated into a very small volume of organic solvent which is then injected into the chromatograph running at a very low flow rate. Pressurized liquid extraction (PLE) at a high temperature and pressure was used to isolate vitamin E forms from cosmetics. The Taguchi experimental method was used to optimize the factors affecting DLLME. The parameters selected were 2mL of acetonitrile (disperser solvent), 100μL carbon tetrachloride (extraction solvent) and 10mL aqueous solution. A volume of 5μL of the organic phase was injected into the reversed-phase capillary LC system equipped with a diode array detector and using an isocratic mobile phase composed of an 95:5 (v/v) methanol:water mixture at a flow-rate of 20μLmin(-1). Quantification was carried out using aqueous standards and detection limits were in the range 0.1-0.5ngmL(-1), corresponding to 3-15ngg(-1) in the cosmetic sample. The recoveries were in the 87-105% range, with RSDs lower than 7.8%. The method was validated according to international guidelines and using a certified reference material. Copyright © 2014 Elsevier B.V. All rights reserved.

Liquid Microjunction Surface Sampling Coupled with High-Pressure Liquid Chromatography-Electrospray Ionization-Mass Spectrometry for Analysis of Drugs and Metabolites in Whole-Body Thin Tissue Sections

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

Kertesz, Vilmos; Van Berkel, Gary J

2010-01-01

In this work, a commercially available autosampler was adapted to perform direct liquid microjunction (LMJ) surface sampling followed by a high-pressure liquid chromatography (HPLC) separation of the extract components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the utility of coupling a separation with this direct liquid extraction based surface sampling approach, four different organs (brain, lung, kidney, and liver) from whole-body thin tissue sections of propranolol dosed and control mice were examined. The parent drug was observed in the chromatograms of the surface sampling extracts from all the organs of the dosed mouse examined. In addition, twomore » isomeric phase II metabolites of propranolol (an aliphatic and an aromatic hydroxypropranolol glucuronide) were observed in the chromatograms of the extracts from lung, kidney, and liver. Confirming the presence of one or the other or both of these glucuronides in the extract from the various organs was not possible without the separation. These drug and metabolite data obtained using the LMJ surface sampling/HPLC-MS method and the results achieved by analyzing similar samples by conventional extraction of the tissues and subsequent HPLC-MS analysis were consistent.« less

Simultaneous extraction and clean-up of polychlorinated biphenyls and their metabolites from small tissue samples using pressurized liquid extraction

PubMed Central

Kania-Korwel, Izabela; Zhao, Hongxia; Norstrom, Karin; Li, Xueshu; Hornbuckle, Keri C.; Lehmler, Hans-Joachim

2008-01-01

A pressurized liquid extraction-based method for the simultaneous extraction and in situ clean-up of polychlorinated biphenyls (PCBs), hydroxylated (OH)-PCBs and methylsulfonyl (MeSO2)-PCBs from small (< 0.5 gram) tissue samples was developed and validated. Extraction of a laboratory reference material with hexane:dichloromethane:methanol (48:43:9, v/v) and Florisil as fat retainer allowed an efficient recovery of PCBs (78–112%; RSD: 13–37%), OH-PCBs (46±2%; RSD: 4%) and MeSO2-PCBs (89±21%; RSD: 24%). Comparable results were obtained with an established analysis method for PCBs, OH-PCBs and MeSO2-PCBs. PMID:19019378

Application of response surface methodology to optimize pressurized liquid extraction of antioxidant compounds from sage (Salvia officinalis L.), basil (Ocimum basilicum L.) and thyme (Thymus vulgaris L.).

PubMed

Hossain, M B; Brunton, N P; Martin-Diana, A B; Barry-Ryan, C

2010-12-01

The present study optimized pressurized liquid extraction (PLE) conditions using Dionex ASE® 200, USA to maximize the antioxidant activity [Ferric ion Reducing Antioxidant Power (FRAP)] and total polyphenol content (TP) of the extracts from three spices of Lamiaceae family (sage, basil and thyme). Optimal conditions with regard to extraction temperature (66-129 °C) and solvent concentration (32-88% methanol) were identified using response surface methodology (RSM). For all three spices, results showed that 129 °C was the optimum temperature with regard to antioxidant activity. Optimal methanol concentrations with respect to the antioxidant activity of sage and basil extracts were 58% and 60% respectively. Thyme showed a different trend with regard to methanol concentration and was optimally extracted at 33%. Antioxidant activity yields of the optimal PLE were significantly (p < 0.05) higher than solid/liquid extracts. Predicted models were highly significant (p < 0.05) for both total phenol (TP) and FRAP values in all the spices with high regression coefficients (R(2)) ranging from 0.651 to 0.999.

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.

Liquid by-products from fish canning industry as sustainable sources of ω3 lipids.

PubMed

Monteiro, Ana; Paquincha, Diogo; Martins, Florinda; Queirós, Rui P; Saraiva, Jorge A; Švarc-Gajić, Jaroslava; Nastić, Nataša; Delerue-Matos, Cristina; Carvalho, Ana P

2018-08-01

Fish canning industry generates large amounts of liquid wastes, which are discarded, after proper treatment to remove the organic load. However, alternative treatment processes may also be designed in order to target the recovery of valuable compounds; with this procedure, these wastewaters are converted into liquid by-products, becoming an additional source of revenue for the company. This study evaluated green and economically sustainable methodologies for the extraction of ω3 lipids from fish canning liquid by-products. Lipids were extracted by processes combining physical and chemical parameters (conventional and pressurized extraction processes), as well as chemical and biological parameters. Furthermore, LCA was applied to evaluate the environmental performance and costs indicators for each process. Results indicated that extraction with high hydrostatic pressure provides the highest amounts of ω3 polyunsaturated fatty acids (3331,5 mg L -1 effluent), apart from presenting the lowest environmental impact and costs. The studied procedures allow to obtain alternative, sustainable and traceable sources of ω3 lipids for further applications in food, pharmaceutical and cosmetic industries. Additionally, such approach contributes towards the organic depuration of canning liquid effluents, therefore reducing the overall waste treatment costs. Copyright © 2018 Elsevier Ltd. All rights reserved.

Analysis of vitamin K1 in fruits and vegetables using accelerated solvent extraction and liquid chromatography tandem mass spectrometry with atmospheric pressure chemical ionization.

PubMed

Jäpelt, Rie Bak; Jakobsen, Jette

2016-02-01

The objective of this study was to develop a rapid, sensitive, and specific analytical method to study vitamin K1 in fruits and vegetables. Accelerated solvent extraction and solid phase extraction was used for sample preparation. Quantification was done by liquid chromatography tandem mass spectrometry with atmospheric pressure chemical ionization in selected reaction monitoring mode with deuterium-labeled vitamin K1 as an internal standard. The precision was estimated as the pooled estimate of three replicates performed on three different days for spinach, peas, apples, banana, and beetroot. The repeatability was 5.2% and the internal reproducibility was 6.2%. Recovery was in the range 90-120%. No significant difference was observed between the results obtained by the present method and by a method using the same principle as the CEN-standard i.e. liquid-liquid extraction and post-column zinc reduction with fluorescence detection. Limit of quantification was estimated to 0.05 μg/100g fresh weight. Copyright © 2015 Elsevier Ltd. All rights reserved.

Pressurized liquid extracts from Spirulina platensis microalga. Determination of their antioxidant activity and preliminary analysis by micellar electrokinetic chromatography.

PubMed

Herrero, Miguel; Ibáñez, Elena; Cifuentes, Alejandro; Señoráns, Javier

2004-08-27

In this work, different extracts from the microalga Spirulina platensis are obtained using pressurized liquid extraction (PLE) and four different solvents (hexane, light petroleum, ethanol and water). Different extraction temperatures (115 and 170 degrees C) were tested using extraction times ranging from 9 to 15 min. The antioxidant activity of the different extracts is determined by means of an in vitro assay using a free radical method. Moreover, a new and fast method is developed using micellar electrokinetic chromatography with diode array detection (MEKC-DAD) to provide a preliminary analysis on the composition of the extracts. This combined application (i.e., in vitro assays plus MEKC-DAD) allowed the fast characterization of the extracts based on their antioxidant activity and the UV-vis spectra of the different compounds found in the extracts. To our knowledge, this work shows for the first time the great possibilities of the combined use of PLE-in vitro assay-MEKC-DAD to investigate natural sources of antioxidants.

High-pressure liquid chromatographic analysis of pramoxine hydrochloride in high lipoid aerosol foam dosage form.

PubMed

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

A rapid and quantitative method for the determination of pramoxine hydrochloride by high-pressure liquid chromatography is presented. The drug is extracted as the salt from a preparation with a high lipoid composition by partitioning it to the aqueous phase of an ether-methanol-water-acetic acid system. The extract is chromatographed on an octadecylsilane bonded packing with a methanol-water-acetic acid-methanesulfonic acid mobile phase. The time required for each separation is approximately 6 min. Analytical recoveries of 100.4 +/- 1.5% were obtained.

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

PubMed

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

2015-06-01

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

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

PubMed

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

2007-01-01

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

Pressurized liquid extraction of diesel and air particulate standard reference materials: effect of extraction temperature and pressure.

PubMed

Schantz, Michele M; McGaw, Elizabeth; Wise, Stephen A

2012-10-02

Four particulate matter Standard Reference Materials (SRMs) available from the National Institute of Standards and Technology (NIST) were used to evaluate the effect of solvent, number of static cycles and static times, pressure, and temperature when using pressurized liquid extraction (PLE) for the extraction of polycyclic aromatic hydrocarbons (PAHs) and nitrated-PAHs. The four materials used in the study were SRM 1648a Urban Particulate Matter, SRM 1649b Urban Dust, SRM 1650b Diesel Particulate Matter, and SRM 2975 Diesel Particulate Matter (Industrial Forklift). The results from the study indicate that the choice of solvent, dichloromethane compared to toluene and toluene/methanol mixtures, had little effect on the extraction efficiency. With three to five extraction cycles, increasing the extraction time for each cycle from 5 to 30 min had no significant effect on the extraction efficiency. The differences in extraction efficiency were not significant (with over 95% of the differences being <10%) when the pressure was increased from 13.8 to 20.7 MPa. The largest increase in extraction efficiency occurred for selected PAHs when the temperature of extraction was increased from 100 to 200 °C. At 200 °C naphthalene, biphenyl, fluorene, dibenzothiophene, and anthracene show substantially higher mass fractions (>30%) than when extracted at 100 °C in all the SRMs studied. For SRM 2975, large increases (>100%) are also observed for some other PAHs including benz[a]anthracene, benzo[k]fluoranthene, benzo[e]pyrene, benzo[a]pyrene, benzo[ghi]perylene, and benzo[b]chrysene when extracted at the higher temperatures; however, similar trends were not observed for the other diesel particulate sample, SRM 1650b. The results are discussed in relation to the use of the SRMs for evaluating analytical methods.

Extraction of ranitidine and nizatidine with using imidazolium ionic liquids prior spectrophotometric and chromatographic detection.

PubMed

Kiszkiel, Ilona; Starczewska, Barbara; Leśniewska, Barbara; Późniak, Patrycja

2015-03-15

A new extraction medium was proposed for liquid-liquid extraction of the histamine H2 receptor antagonists ranitidine (RNT) and nizatidine (NZT). The ionic liquids with low vapor pressure and favorable solvating properties for a range of compounds such as 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide [C4mim][Tf2N] were tested for isolation of analytes. The extraction parameters of RNT and NZT, namely, amount of ionic liquid, pH of sample solution, shaking and centrifugation time were optimized. The isolation processes were performed with 1 mL of the ionic liquids. The extracted samples (pH values near 4) were shaken at 1750 rpm. The influence of interfering substances on the efficiency of extraction process was also studied. Methods for the histamine H2 receptor antagonists (ranitidine and nizatidine) determination after their separation using imidazolium ionic liquids by high performance liquid chromatography (HPLC) combined with UV spectrophotometry were developed. The application of ionic liquids in extraction step allows for selective isolation of analytes from aqueous matrices and their preconcentration. The above methods were applied to the determination of RNT and NZT in environmental samples (river water and wastewater after treatment). Copyright © 2014 Elsevier B.V. All rights reserved.

Are extraction methods in quantitative assays of pharmacopoeia monographs exhaustive? A comparison with pressurized liquid extraction.

PubMed

Basalo, Carlos; Mohn, Tobias; Hamburger, Matthias

2006-10-01

The extraction methods in selected monographs of the European and the Swiss Pharmacopoeia were compared to pressurized liquid extraction (PLE) with respect to the yield of constituents to be dosed in the quantitative assay for the respective herbal drugs. The study included five drugs, Belladonnae folium, Colae semen, Boldo folium, Tanaceti herba and Agni casti fructus. They were selected to cover different classes of compounds to be analyzed and different extraction methods to be used according to the monographs. Extraction protocols for PLE were optimized by varying the solvents and number of extraction cycles. In PLE, yields > 97 % of extractable analytes were typically achieved with two extraction cycles. For alkaloid-containing drugs, the addition of ammonia prior to extraction significantly increased the yield and reduced the number of extraction cycles required for exhaustive extraction. PLE was in all cases superior to the extraction protocol of the pharmacopoeia monographs (taken as 100 %), with differences ranging from 108 % in case of parthenolide in Tanaceti herba to 343 % in case of alkaloids in Boldo folium.

A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.

PubMed

Zhou, Xi; Cui, Kunyan; Zeng, Feng; Li, Shoucong; Zeng, Zunxiang

2016-06-01

In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Optimization of pressurized liquid extraction by response surface methodology of Goji berry (Lycium barbarum L.) phenolic bioactive compounds.

PubMed

Tripodo, Giusy; Ibáñez, Elena; Cifuentes, Alejandro; Gilbert-López, Bienvenida; Fanali, Chiara

2018-01-03

Pressurized liquid extraction (PLE) has been used for the first time in this work to extract phenolic compounds from Goji berries according to a multilevel factorial design using response surface methodology. The global yield (% w/dw, weight/dry-weight), total phenolic content (TPC), total flavonoid (TF) and antioxidant activity (determined via ABTS assay, expressed as TEAC value) were used as response variables to study the effects of temperature (50-180°C) and green solvent composition (mixtures of ethanol/water). Phenolic compounds characterization was performed by high performance liquid chromatography-diode array detector-tandem mass spectrometry (HPLC-DAD-MS/MS). The optimum PLE conditions predicted by the model were as follows: 180°C and 86% ethanol in water with a good desirability value of 0.815. The predicted conditions were confirmed experimentally and once the experimental design was validated for commercial fruit samples, the PLE extraction of phenolic compounds from three different varieties of fruit samples (Selvatico mongolo, Bigol, and Polonia) was performed. Nine phenolic compounds were tentatively identified in these extracts, including phenolic acids and their derivatives, and flavonols. The optimized PLE conditions were compared to a conventional solid-liquid extraction, demonstrating that PLE is a useful alternative to extract phenolic compounds from Goji berry. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimizing pressurized liquid extraction of microbial lipids using the response surface method.

PubMed

Cescut, J; Severac, E; Molina-Jouve, C; Uribelarrea, J-L

2011-01-21

Response surface methodology (RSM) was used for the determination of optimum extraction parameters to reach maximum lipid extraction yield with yeast. Total lipids were extracted from oleaginous yeast (Rhodotorula glutinis) using pressurized liquid extraction (PLE). The effects of extraction parameters on lipid extraction yield were studied by employing a second-order central composite design. The optimal condition was obtained as three cycles of 15 min at 100°C with a ratio of 144 g of hydromatrix per 100 g of dry cell weight. Different analysis methods were used to compare the optimized PLE method with two conventional methods (Soxhlet and modification of Bligh and Dyer methods) under efficiency, selectivity and reproducibility criteria thanks to gravimetric analysis, GC with flame ionization detector, High Performance Liquid Chromatography linked to Evaporative Light Scattering Detector (HPLC-ELSD) and thin-layer chromatographic analysis. For each sample, the lipid extraction yield with optimized PLE was higher than those obtained with referenced methods (Soxhlet and Bligh and Dyer methods with, respectively, a recovery of 78% and 85% compared to PLE method). Moreover, the use of PLE led to major advantages such as an analysis time reduction by a factor of 10 and solvent quantity reduction by 70%, compared with traditional extraction methods. Copyright © 2010 Elsevier B.V. All rights reserved.

Downstream valorization and comprehensive two-dimensional liquid chromatography-based chemical characterization of bioactives from black chokeberries (Aronia melanocarpa) pomace.

PubMed

Brazdauskas, T; Montero, L; Venskutonis, P R; Ibañez, E; Herrero, M

2016-10-14

In this work, a new alternative for the downstream processing and valorization of black chokeberry pomace (Aronia melanocarpa) which could be potentially coupled to a biorefinery process is proposed. This alternative is based on the application of pressurized liquid extraction (PLE) to the residue obtained after the supercritical fluid extraction of the berry pomace. An experimental design is employed to study and optimize the most relevant extraction conditions in order to attain extracts with high extraction yields, total phenols content and antioxidant activity. Moreover, the PLE extracts were characterized by using a new method based on the application of comprehensive two-dimensional liquid chromatography in order to correlate their activity with their chemical composition. Thanks to the use of this powerful analytical tool, 61 compounds could be separated being possible the tentative identification of different anthocyanins, proanthocyanidins, flavonoids and phenolic acids. By using the optimized PLE approach (using pressurized 46% ethanol in water at 165°C containing 1.8% formic acid), extracts with high total phenols content (236.6mg GAE g -1 extract) and high antioxidant activities (4.35mmol TE g -1 extract and EC 50 5.92μgmL -1 ) could be obtained with high yields (72.5%). Copyright © 2016 Elsevier B.V. All rights reserved.

Headspace single drop microextraction versus dispersive liquid-liquid microextraction using magnetic ionic liquid extraction solvents.

PubMed

An, Jiwoo; Rahn, Kira L; Anderson, Jared L

2017-05-15

A headspace single drop microextraction (HS-SDME) method and a dispersive liquid-liquid microextraction (DLLME) method were developed using two tetrachloromanganate ([MnCl 4 2- ])-based magnetic ionic liquids (MIL) as extraction solvents for the determination of twelve aromatic compounds, including four polyaromatic hydrocarbons, by reversed phase high-performance liquid chromatography (HPLC). The analytical performance of the developed HS-SDME method was compared to the DLLME approach employing the same MILs. In the HS-SDME approach, the magnetic field generated by the magnet was exploited to suspend the MIL solvent from the tip of a rod magnet. The utilization of MILs in HS-SDME resulted in a highly stable microdroplet under elevated temperatures and long extraction times, overcoming a common challenge encountered in traditional SDME approaches of droplet instability. The low UV absorbance of the [MnCl 4 2- ]-based MILs permitted direct analysis of the analyte enriched extraction solvent by HPLC. In HS-SDME, the effects of ionic strength of the sample solution, temperature of the extraction system, extraction time, stir rate, and headspace volume on extraction efficiencies were examined. Coefficients of determination (R 2 ) ranged from 0.994 to 0.999 and limits of detection (LODs) varied from 0.04 to 1.0μgL -1 with relative recoveries from lake water ranging from 70.2% to 109.6%. For the DLLME method, parameters including disperser solvent type and volume, ionic strength of the sample solution, mass of extraction solvent, and extraction time were studied and optimized. Coefficients of determination for the DLLME method varied from 0.997 to 0.999 with LODs ranging from 0.05 to 1.0μgL -1 . Relative recoveries from lake water samples ranged from 68.7% to 104.5%. Overall, the DLLME approach permitted faster extraction times and higher enrichment factors for analytes with low vapor pressure whereas the HS-SDME approach exhibited better extraction efficiencies for analytes with relatively higher vapor pressure. Copyright © 2017 Elsevier B.V. All rights reserved.

Analyzing the Use of Gaseous Helium as a Pressurant with Cryogenic Propellants with Thermodynamic Venting System Modelling and Test Data

NASA Technical Reports Server (NTRS)

Hedayat, A.; Nelson, S.L.; Hastings, L.J.; Flachbart, R.H.; Vermillion, D.J.; Tucker, S.P.

2007-01-01

Cryogens are viable candidate propellants for NASA's Lunar and Mars exploration programs. To provide adequate mass flow to the system's engines and/or to prevent feed system cavitation, gaseous helium (GHe) is frequently considered as a pressurant. During low gravity operations, a Thermodynamic Venting System (TVS) is designed to maintain tank pressure during low gravity operations without propellant resettling. Therefore, a series of tests were conducted in the Multi-purpose Hydrogen Test Bed (MHTB) of Marshall Space Flight Center (MSFC) in order to evaluate the effects of GHe pressurant on pressure control performance of a TVS with liquid hydrogen (LH2) and nitrogen (LN2) as the test liquids. The TVS used in these test series consists of a recirculation pump, Joule-Thomson (J-T) expansion valve, and a parallel flow concentric tube heat exchanger combined with a longitudinal spray bar. Using a small amount of liquid extracted from the tank recirculation line, passing it through the J-T valve, and then through the heat exchanger, thermal energy is extracted from the bulk liquid and ullage thereby enabling pressure control. The LH2/GHe tests were performed at fill levels of 90%, 50%, and 25% and LN2/GHe tests were conducted at fill levels of 50% and 25%. Moreover, each test was conducted with a specified tank ullage pressure control band. A one-dimensional TVS performance program was used to analyze and correlate the test data. Predictions and comparisons with test data of ullage pressure and temperature and bulk liquid saturation pressure and temperature with test data are presented.

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.

Simultaneous determination of nine saponins from Panax notoginseng using HPLC and pressurized liquid extraction.

PubMed

Wan, J B; Lai, C M; Li, S P; Lee, M Y; Kong, L Y; Wang, Y T

2006-04-11

A HPLC and pressurized liquid extraction (PLE) method was developed for simultaneous determination of nine saponins, including notoginsenoside R1, ginsenoside Rg1, Re, Rf, Rb1, Rc, Rb2, Rb3 and Rd in Panax notoginseng. The analysis was performed on C18 column with water-acetonitrile gradient elution and the investigated saponins were authenticated by comparing retention time and mass spectra with their reference compounds. Several methods including PLE, ultrasonication, soxhlet extraction and immersion were used for sample preparation and their extraction efficiency was compared. The results showed that PLE has the highest extraction efficiency and repeatability, which would be valuable on standardization of sample preparation for quality control of Chinese medicines. The developed HPLC and PLE is an effective approach for simultaneously quantitative determination of sapoinins in P. notoginseng, which could be used for quality control of P. notoginseng and its preparations.

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

PubMed

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

2016-04-01

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

Sample preparation for the analysis of isoflavones from soybeans and soy foods.

PubMed

Rostagno, M A; Villares, A; Guillamón, E; García-Lafuente, A; Martínez, J A

2009-01-02

This manuscript provides a review of the actual state and the most recent advances as well as current trends and future prospects in sample preparation and analysis for the quantification of isoflavones from soybeans and soy foods. Individual steps of the procedures used in sample preparation, including sample conservation, extraction techniques and methods, and post-extraction treatment procedures are discussed. The most commonly used methods for extraction of isoflavones with both conventional and "modern" techniques are examined in detail. These modern techniques include ultrasound-assisted extraction, pressurized liquid extraction, supercritical fluid extraction and microwave-assisted extraction. Other aspects such as stability during extraction and analysis by high performance liquid chromatography are also covered.

Optimisation of phenolics recovery from Vitex agnus-castus Linn. leaves by high-pressure and temperature extraction.

PubMed

Lataoui, Mohammed; Seffen, Mongi; Aliakbarian, Bahar; Casazza, Alessandro Alberto; Converti, Attilio; Perego, Patrizia

2014-01-01

To optimise recovery of phenolics from Vitex agnus-castus Linn., a non-conventional high-pressure (2-24 bar) and temperature (100-180°C) extraction method was used under nitrogen atmosphere with methanol as a solvent. Optimal temperature was between 100 and 140°C, and optimal extraction time was about one half that of conventional solid/liquid extraction at room temperature. Final yields of total polyphenols, total flavonoids, o-diphenols and anthocyanins extraction were 2.0, 3.0, 2.5 and 11-fold those obtained by conventional extraction.

Determination of benzoylurea insecticides in food by pressurized liquid extraction and LC-MS.

PubMed

Brutti, Monia; Blasco, Cristina; Picó, Yolanda

2010-01-01

A method based on pressurized liquid extraction and LC-MS/MS has been developed for determining nine benzoylureas (BUs) in fruit, vegetable, cereals, and animal products. Samples (5 g) were homogenized with diatomaceous earth and extracted in a 22 mL cell with 22 mL of ethyl acetate at 80 degrees C and 1500 psi. After solvent concentration and exchange to methanol, BUs were analyzed by LC-MS/MS using an IT mass analyzer, which achieved several transitions of precursor ions that increase selectivity providing identification. LOQs were between 0.002 and 0.01 mg/kg, which are equal or lower than maximum residue limits established by the Codex Alimentarius. Excellent linearity was achieved over a range of concentrations from 0.01 to 1 mg/kg with correlation coefficients 0.995-0.999 (n=7). Validation of the total method was performed by analyzing in quintuplicate seven different commodities (milk, eggs, meat, rice, lettuce, avocado, and lemon) at three concentration levels (0.01, 0.1, and 1 mg/kg). The recoveries ranged from 58 to 97% and the RSDs from 5 to 19% depending on the compound and the commodity. The combination of pressurized liquid extraction with LC-MS/MS provides a sensitive and selective method for the determination of BUs in food.

Chemical investigation of saponins in different parts of Panax notoginseng by pressurized liquid extraction and liquid chromatography-electrospray ionization-tandem mass spectrometry.

PubMed

Wan, Jian-Bo; Zhang, Qing-Wen; Hong, Si-Jia; Li, Peng; Li, Shao-Ping; Wang, Yi-Tao

2012-05-16

A pressurized liquid extraction (PLE) and high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS) method was developed for the qualitative determination of saponins in different parts of P. notoginseng, including rhizome, root, fibre root, seed, stem, leaf and flower. The samples were extracted using PLE. The analysis was achieved on a Zorbax SB-C18 column with gradient elution of acetonitrile and 8 mM aqueous ammonium acetate as mobile phase. The mass spectrometer was operated in the negative ion mode using the electrospray ionization, and a collision induced dissociation (CID) experiment was also carried out to aid the identification of compounds. Forty one saponins were identified in different parts of P. notoginseng according to the fragmentation patterns and literature reports, among them, 21 saponins were confirmed by comparing the retention time and ESI-MS data with those of standard compounds. The results showed that the chemical characteristics were obviously diverse in different parts of P. notoginseng, which is helpful for pharmacological evaluation and quality control of P. notoginseng.

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

PubMed

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

2005-02-15

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

Negative-pressure cavitation extraction for the determination of flavonoids in pigeon pea leaves by liquid chromatography-tandem mass spectrometry.

PubMed

Liu, Wei; Fu, Yujie; Zu, Yuangang; Kong, Yu; Zhang, Lin; Zu, Baishi; Efferth, Thomas

2009-05-01

A new method, namely negative-pressure cavitation extraction (NPCE), followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) is presented for the extraction and quantification of flavonoids in pigeon pea leaves. This method combines the high efficiency of NPCE and the sensitivity and accuracy of MS/MS. The influential parameters of the NPCE procedure including liquid/solid ratio, extraction time, nitrogen flow and number of extraction cycles were optimized. Under optimized conditions, the efficiency of NPCE for extracting five flavonoids was compared to microwave-assisted extraction (MAE), ultrasonic extraction (USE) and heating reflux extraction (HRE). Additionally, structural disruption to pigeon pea leaves samples with different extraction methods was investigated by scanning electron microscopy. The relative recovery with NPCE was equivalent to or higher than that with USE and obviously higher than those with MAE and HRE which are usually conducted in higher temperatures. Furthermore, because NPCE was performed with nitrogen at room temperature, the degradation and oxidation of analytes were avoided. In addition, the NPCE method was validated in terms of repeatability and reproducibility, relative standard deviation for relative recovery was lower than 5.84 and 8.83%, respectively. The method was also successfully applied for the quantification of five flavonoids in pigeon pea leaves. All these results suggest that the developed NPCE-LC-MS/MS method represents an excellent alternative for the extraction and quantification of flavonoids in other plant materials.

[Corrected Title: Solid-Phase Extraction of Polar Compounds from Water] Automated Electrostatics Environmental Chamber

NASA Technical Reports Server (NTRS)

Sauer, Richard; Rutz, Jeffrey; Schultz, John

2005-01-01

A solid-phase extraction (SPE) process has been developed for removing alcohols, carboxylic acids, aldehydes, ketones, amines, and other polar organic compounds from water. This process can be either a subprocess of a water-reclamation process or a means of extracting organic compounds from water samples for gas-chromatographic analysis. This SPE process is an attractive alternative to an Environmental Protection Administration liquid-liquid extraction process that generates some pollution and does not work in a microgravitational environment. In this SPE process, one forces a water sample through a resin bed by use of positive pressure on the upstream side and/or suction on the downstream side, thereby causing organic compounds from the water to be adsorbed onto the resin. If gas-chromatographic analysis is to be done, the resin is dried by use of a suitable gas, then the adsorbed compounds are extracted from the resin by use of a solvent. Unlike the liquid-liquid process, the SPE process works in both microgravity and Earth gravity. In comparison with the liquid-liquid process, the SPE process is more efficient, extracts a wider range of organic compounds, generates less pollution, and costs less.

Optimization, validation and comparison of various extraction techniques for the trace determination of polycyclic aromatic hydrocarbons in sewage sludges by liquid chromatography coupled to diode-array and fluorescence detection.

PubMed

Miège, C; Dugay, J; Hennion, M C

2003-05-02

There is a need for a better characterization of sludges from wastewater treatment plants which are destined to be spread on agricultural lands. Inorganic pollutants are regularly controlled but organic pollutants have received few attention up to now. On this paper, we have been interested on the analysis of the 16 polycyclic aromatic hydrocarbons (PAHs) listed in the US Environmental Protection Agency (US EPA) priority list and more particularly of the six PAHs listed in the European community list (fluoranthene, benzo[b and k]fluoranthene, benzo[a]pyrene, benzo[ghi]perylene, indeno[1,2,3-cd]pyrene). The analysis step consists on liquid chromatography with both fluorescence and UV detections as described in the EPA Method 8310. As for the extraction step, several techniques such as supercritical fluid extraction, pressurized liquid extraction, focused microwave extraction in open vessels, Soxhlet and ultrasonic extractions are compared after optimization of the experimental conditions (solvent nature and quantity, temperature, pressure, duration, ... ) and validation with certified sludges. When optimized, these five extraction techniques are as much efficient with similar relative standard deviation. Whatever the extraction techniques used, the whole analysis protocol permits to quantify PAHs in the range of 0.09 to 0.9 mg/kg of dried sludges.

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.

Matrix effect on the determination of synthetic corticosteroids and diuretics by liquid chromatography-tandem mass spectrometry

NASA Astrophysics Data System (ADS)

Dikunets, M. A.; Appolonova, S. A.; Rodchenkov, G. M.

2009-04-01

This work presents a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) procedure for selective and reliable screening of corticosteroids and diuretics in human urine. Sample preparation included the extraction, evaporation of the organic extract under nitrogen, and solution of the dry residue. The extract was analyzed by HPLC combined with tandem mass spectrometry using electro-spraying ionization at atmospheric pressure with negative ion recording. The mass spectra of all compounds were recorded, and the characteristic ions, retention times, and detection limits were determined. The procedure was validated by evaluating the degree of the matrix suppression of ionization, extraction of analytes from human biological liquid, and the selectivity and specificity of determination.

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.

Extraction and analysis of intact glucosinolates--a validated pressurized liquid extraction/liquid chromatography-mass spectrometry protocol for Isatis tinctoria, and qualitative analysis of other cruciferous plants.

PubMed

Mohn, Tobias; Cutting, Brian; Ernst, Beat; Hamburger, Matthias

2007-09-28

Glucosinolates have attracted significant interest due to the chemopreventive properties of some of their transformation products. Numerous protocols for the extraction and analysis of glucosinolates have been published, but limited effort has been devoted to optimize and validate crucial extraction parameters and sample preparation steps. We carried out a systematic optimization and validation of a quantitative assay for the direct analysis of intact glucosinolates in Isatis tinctoria leaves (woad, Brassicaceae). Various parameters such as solvent composition, particle size, temperature, and number of required extraction steps were optimized using pressurized liquid extraction (PLE). We observed thermal degradation of glucosinolates at temperatures above 50 degrees C, and loss of >60% within 10min at 100 degrees C, but no enzymatic degradation in the leaf samples at ambient temperature. Excellent peak shape and resolution was obtained by reversed-phase chromatography on a Phenomenex Aqua column using 10mM ammonium formate as ion-pair reagent. Detection was carried out by electrospray ionisation mass spectrometry in the negative ion mode. Analysis of cruciferous vegetables and spices such as broccoli (Brassica oleracea L. var. italica), garden cress (Lepidium sativum L.) and black mustard (Sinapis nigra L.) demonstrated the general applicability of the method.

Antioxidant White Grape Seed Phenolics: Pressurized Liquid Extracts from Different Varieties

PubMed Central

Garcia-Jares, Carmen; Vazquez, Alberto; Lamas, Juan P.; Pajaro, Marta; Alvarez-Casas, Marta; Lores, Marta

2015-01-01

Grape seeds represent a high percentage (20% to 26%) of the grape marc obtained as a byproduct from white winemaking and keep a vast proportion of grape polyphenols. In this study, seeds obtained from 11 monovarietal white grape marcs cultivated in Northwestern Spain have been analyzed in order to characterize their polyphenolic content and antioxidant activity. Seeds of native (Albariño, Caiño, Godello, Loureiro, Torrontés, and Treixadura) and non-native (Chardonnay, Gewurtzträminer, Pinot blanc, Pinot gris, and Riesling) grape varieties have been considered. Low weight phenolics have been extracted by means of pressurized liquid extraction (PLE) and further analyzed by LC-MS/MS. The results showed that PLE extracts, whatever the grape variety of origin, contained large amounts of polyphenols and high antioxidant activity. Differences in the varietal polyphenolic profiles were found, so a selective exploitation of seeds might be possible. PMID:26783956

Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

PubMed

Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

2016-03-18

Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system.

PubMed

Yang, Fan; Kubota, Fukiko; Baba, Yuzo; Kamiya, Noriho; Goto, Masahiro

2013-06-15

The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid-liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system. Copyright © 2013 Elsevier B.V. All rights reserved.

Pressurized liquid extraction and microwave-assisted extraction in the determination of organochlorine pesticides in fish muscle samples.

PubMed

Barriada-Pereira, Mercedes; Iglesias-García, Iván; González-Castro, María J; Muniategui-Lorenzo, Soledad; López-Mahía, Purificación; Prada-Rodríguez, Darío

2008-01-01

This paper describes a comparative study of 2 extraction methods, pressurized liquid extraction (PLE) and microwave-assisted extraction (MAE), for the determination of organochlorine pesticides (OCPs) in fish muscle samples. In both cases, samples were extracted with hexane-acetone (50 + 50), and the extracts were purified by solid-phase extraction using a carbon cartridge as the adsorbent. Pesticides were eluted with hexane-ethyl acetate (80 + 20) and determined by gas chromatography with electron-capture detection. Both methods demonstrated good linearity over the range studied (0.005-0.100 microg/mL). Detection limits ranged from 0.029 to 0.295 mg/kg for PLE and from 0.003 to 0.054 mg/kg for MAE. For most of the pesticides, analytical recoveries with both methods were between 80 and 120%, and the relative standard deviations were < 10%. The proposed methods were shown to be powerful techniques for the extraction of OCPs from fish muscle samples. Although good recovery rates were obtained with both extraction methods, MAE provided advantages with regard to sample handling, cost, analysis time, and solvent consumption. Acceptable validation parameters were obtained although MAE was shown to be more sensitive than PLE.

Isolation and characterization of antimicrobial food components.

PubMed

Papetti, Adele

2012-04-01

Nowadays there is an evident growing interest in natural antimicrobial compounds isolated from food matrices. According to the type of matrix, different isolation and purification steps are needed and as these active compounds belong to different chemical classes, also different chromatographic and electrophoretic methods coupled with various detectors (the most used diode array detector and mass spectrometer) have to be performed. This review covers recent steps made in the fundamental understanding of sample preparation methods as well as of analytical tools useful for the complete characterization of bioactive food compounds. The most commonly used methods for extraction of natural antimicrobial compounds are the conventional liquid-liquid or solid-liquid extraction and the modern techniques such as pressurized liquid extraction, microwave-assisted extraction, ultrasound-assisted extraction, solid-phase micro-extraction, supercritical fluid extraction, and matrix solid phase dispersion. The complete characterization of the compounds is achieved using both monodimensional chromatographic processes (LC, nano-LC, GC, and CE coupled with different type of detectors) and, recently, using comprehensive two-dimensional systems (LC×LC and GC×GC). Copyright © 2011 Elsevier Ltd. All rights reserved.

Application of ionic liquid in liquid phase microextraction technology.

PubMed

Han, Dandan; Tang, Baokun; Lee, Yu Ri; Row, Kyung Ho

2012-11-01

Ionic liquids (ILs) are novel nonmolecular solvents. Their unique properties, such as high thermal stability, tunable viscosity, negligible vapor pressure, nonflammability, and good solubility for inorganic and organic compounds, make them excellent candidates as extraction media for a range of microextraction techniques. Many physical properties of ILs can be varied, and the structural design can be tuned to impart the desired functionality and enhance the analyte extraction selectivity, efficiency, and sensitivity. This paper provides an overview of the applications of ILs in liquid phase microextraction technology, such as single-drop microextraction, hollow fiber based liquid phase microextraction, and dispersive liquid-liquid microextraction. The sensitivity, linear calibration range, and detection limits for a range of target analytes in the methods were analyzed to determine the advantages of ILs in liquid phase microextraction. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Selective pressurized liquid extraction of polychlorinated biphenyls from fat-containing food and feed samples influence of cell dimensions, solvent type, temperature and flush volume.

PubMed

Sporring, Sune; Björklund, Erland

2004-06-25

Sulphuric acid impregnated silica was used for the lipid free extraction of polychlorinated biphenyls from fat containing food and feed matrices using pressurized liquid extraction on a Dionex ASE300, with 34 mL cells. Data were compared to a previous publication where extractions had been performed on a Dionex ASE200, with 33 mL cells. Four different fat/fat retainer ratios (FFRs) were tested (0.100, 0.075, 0.050 and 0.025) at 50 and 100 degrees C using n-pentane, n-hexane or n-heptane as extraction solvent. The best results were obtained with a FFR of 0.025 when applying a temperature of 100 degrees C. Both n-pentane and n-heptane were capable of replacing n-hexane as extraction solvent. A flush volume of 60% was sufficient as suggested in US Environmental Protection Agency Method 3545. The applicability of the method was demonstrated for naturally contaminated fish meal as well as various spiked and certified materials.

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.

Effects of Ultrasound on Extraction of Saponin from Ginseng

NASA Astrophysics Data System (ADS)

Li, Hui; Ohdaira, Etsuzo; Ide, Masao

1994-05-01

We performed a study of the effects of ultrasound on the extraction of saponin from Panax ginseng C. A. Meyer. In this study, the extraction of saponin was examined as functions of irradiation time (0.5 to 6 h) and acoustic pressure (0 to 90 kPa). It has been observed that the yields of both total extract and saponin are larger with ultrasonic irradiation than those without ultrasonic irradiation; the increase in yield of total extract is approximately 15 wt%, and that of saponin is approximately 30 wt% at an acoustic pressure 67 kPa. In addition, the yield increases with the acoustic pressure. It is also demonstrated that saponin was not resolved in the acoustic intensity range of this experiment. The enhancement in liquid-solid extraction caused by ultrasound can be attributed to the phenomenon of cavitation.

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.

Arsenic species determination in human scalp hair by pressurized hot water extraction and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

PubMed

Morado Piñeiro, Andrés; Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; López-Mahía, Purificación; Muniategui-Lorenzo, Soledad; Prada-Rodríguez, Darío

2013-02-15

Analytical methods for the determination of total arsenic and arsenic species (mainly As(III) and As(V)) in human scalp hair have been developed. Inductively coupled plasma-mass spectrometry (ICP-MS) and high performance liquid chromatography (HPLC) coupled to ICP-MS have been used for total arsenic and arsenic species determination, respectively. The proposed methods include a "green", fast, high efficient and automated species leaching procedure by pressurized hot water extraction (PHWE). The operating parameters for PHWE including modifier concentration, extraction temperature, static time, extraction steps, pressure, mean particle size, diatomaceous earth (DE) mass/sample mass ratio and flush volume were studied using design of experiments (Plackett-Burman design PBD). Optimum condition implies a modifier concentration (acetic acid) of 150 mM and powdered hair samples fully mixed with diatomaceous earth (DE) as a dispersing agent at a DE mass/sample mass ratio of 5. The extraction has been carried out at 100°C and at an extraction pressure of 1500 psi for 5 min in four extraction step. Under optimised conditions, limits of quantification of 7.0, 6.3 and 50.3 ng g(-1) for total As, As(III) and As(V), respectively were achieved. Repeatability of the overall procedure (4.4, 7.2 and 2.1% for total As, As(III) and As(V), respectively) was achieved. The analysis of GBW-07601 (human hair) certified reference material was used for validation. The optimised method has been finally applied to several human scalp hair samples. Copyright © 2012 Elsevier B.V. All rights reserved.

LIQUID-LIQUID EXTRACTION COLUMNS

DOEpatents

Thornton, J.D.

1957-12-31

This patent relates to liquid-liquid extraction columns having a means for pulsing the liquid in the column to give it an oscillatory up and down movement, and consists of a packed column, an inlet pipe for the dispersed liquid phase and an outlet pipe for the continuous liquid phase located in the direct communication with the liquid in the lower part of said column, an inlet pipe for the continuous liquid phase and an outlet pipe for the dispersed liquid phase located in direct communication with the liquid in the upper part of said column, a tube having one end communicating with liquid in the lower part of said column and having its upper end located above the level of said outlet pipe for the dispersed phase, and a piston and cylinder connected to the upper end of said tube for applying a pulsating pneumatic pressure to the surface of the liquid in said tube so that said surface rises and falls in said tube.

Chromatographic analysis of Polygalae Radix by online hyphenating pressurized liquid extraction

NASA Astrophysics Data System (ADS)

Song, Yuelin; Song, Qingqing; Li, Jun; Shi, Shepo; Guo, Liping; Zhao, Yunfang; Jiang, Yong; Tu, Pengfei

2016-06-01

Practicing “green analytical chemistry” is of great importance when profiling the chemical composition of complex matrices. Herein, a novel hybrid analytical platform was developed for direct chemical analysis of complex matrices by online hyphenating pressurized warm water extraction followed by turbulent flow chromatography coupled with high performance liquid chromatography-tandem mass spectrometry (PWWE-TFC-LC-MS/MS). Two parallel hollow guard columns acted as extraction vessels connected to a long narrow polyether ether ketone tube, while warm water served as extraction solvent and was delivered at a flow rate of 2.5 mL/min to generate considerable back pressure at either vessel. A column oven heated both the solvent and crude materials. A TFC column, which is advantageous for the comprehensive trapping of small molecular substances from fluids under turbulent flow conditions, was employed to transfer analytes from the PWWE module to LC-MS/MS. Two electronic valves alternated each vessel between extraction and elution phases. As a proof-of-concept, a famous herbal medicine for the treatment of neurodegenerative disorders, namely Polygalae Radix, was selected for the qualitative and quantitative analyses. The results suggest that the hybrid platform is advantageous in terms of decreasing time, material, and solvent consumption and in its automation, versatility, and environmental friendliness.

A regulator for pressure-controlled total-liquid ventilation.

PubMed

Robert, Raymond; Micheau, Philippe; Avoine, Olivier; Beaudry, Benoit; Beaulieu, Alexandre; Walti, Hervé

2010-09-01

Total-liquid ventilation (TLV) is an innovative experimental method of mechanical-assisted ventilation in which lungs are totally filled and then ventilated with a tidal volume of perfluorochemical liquid by using a dedicated liquid ventilator. Such a novel medical device must resemble other conventional ventilators: it must be able to conduct controlled-pressure ventilation. The objective was to design a robust controller to perform pressure-regulated expiratory flow and to implement it on our latest liquid-ventilator prototype (Inolivent-4). Numerical simulations, in vitro experiments, and in vivo experiments in five healthy term newborn lambs have demonstrated that it was efficient to generate expiratory flows while avoiding collapses. Moreover, the in vivo results have demonstrated that our liquid ventilator can maintain adequate gas exchange, normal acid-base equilibrium, and achieve greater minute ventilation, better oxygenation and CO2 extraction, while nearing flow limits. Hence, it is our suggestion to perform pressure-controlled ventilation during expiration with minute ventilation equal or superior to 140 mL x min(-1) x kg(-1) in order to ensure PaCO2 below 55 mmHg. From a clinician's point of view, pressure-controlled ventilation greatly simplifies the use of the liquid ventilator, which will certainly facilitate its introduction in intensive care units for clinical applications.

Chlorogenic acid stability in pressurized liquid extraction conditions.

PubMed

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

2015-01-01

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

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.

Essential oils (EOs), pressurized liquid extracts (PLE) and carbon dioxide supercritical fluid extracts (SFE-CO2) from Algerian Thymus munbyanus as valuable sources of antioxidants to be used on an industrial level.

PubMed

Bendif, Hamdi; Adouni, Khaoula; Miara, Mohamed Djamel; Baranauskienė, Renata; Kraujalis, Paulius; Venskutonis, Petras Rimantas; Nabavi, Seyed Mohammad; Maggi, Filippo

2018-09-15

The aim of this study was to demonstrate the potential of extracts from Algerian Thymus munbyanus as a valuable source of antioxidants for use on an industrial level. To this end, a study was conducted on the composition and antioxidant activities of essential oils (EOs), pressurized liquid extracts (PLE) and supercritical fluid extracts (SFE-CO 2 ) obtained from Thymus munbyanus subsp. coloratus (TMC) and subsp. munbyanus (TMM). EOs and SFE-CO 2 extracts were analysed by GC-FID and GC×GC-TOFMS revealing significant differences. A successive extraction of the solid SFE-CO 2 residue by PLE extraction with solvents of increasing polarity such as acetone, ethanol and water, was carried out. The extracts were evaluated for total phenolic content by Folin-Ciocalteu assay, while the antioxidant power was assessed by DPPH, FRAP, and ORAC assays. SFE-CO 2 extracts were also analysed for their tocopherol content. The antioxidant activity of PLE extracts was found to be higher than that of SFE-CO 2 extracts, and this increased with solvent polarity (water > ethanol > acetone). Overall, these results support the use of T. munbyanus as a valuable source of substances to be used on an industrial level as preservative agents. Copyright © 2018 Elsevier Ltd. All rights reserved.

State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

PubMed

Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

2016-01-28

Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Liquid Nitrogen (Oxygen Simulent) Thermodynamic Venting System Test Data Analysis

NASA Technical Reports Server (NTRS)

Hedayat, A.; Nelson, S. L.; Hastings, L. J.; Flachbart, R. H.; Tucker, S. P.

2005-01-01

In designing systems for the long-term storage of cryogens in low gravity space environments, one must consider the effects of thermal stratification on excessive tank pressure that will occur due to environmental heat leakage. During low gravity operations, a Thermodynamic Venting System (TVS) concept is expected to maintain tank pressure without propellant resettling. The TVS consists of a recirculation pump, Joule-Thomson (J-T) expansion valve, and a parallel flow concentric tube heat exchanger combined with a longitudinal spray bar. Using a small amount of liquid extracted by the pump and passing it though the J-T valve, then through the heat exchanger, the bulk liquid and ullage are cooled, resulting in lower tank pressure. A series of TVS tests were conducted at the Marshall Space Flight Center using liquid nitrogen as a liquid oxygen simulant. The tests were performed at fill levels of 90%, 50%, and 25% with gaseous nitrogen and helium pressurants, and with a tank pressure control band of 7 kPa. A transient one-dimensional model of the TVS is used to analyze the data. The code is comprised of four models for the heat exchanger, the spray manifold and injector tubes, the recirculation pump, and the tank. The TVS model predicted ullage pressure and temperature and bulk liquid saturation pressure and temperature are compared with data. Details of predictions and comparisons with test data regarding pressure rise and collapse rates will be presented in the final paper.

Development and application of an in-cell cleanup pressurized liquid extraction with ultra-high-performance liquid chromatography-tandem mass spectrometry to detect prohibited antiviral agents sensitively in livestock and poultry feces.

PubMed

Wu, Huizhen; Wang, Jianmei; Yang, Hua; Li, Guoqin; Zeng, Yinhuan; Xia, Wei; Li, Zuguang; Qian, Mingrong

2017-03-10

An in-cell cleanup pressurized liquid extraction was developed to analyze prohibited antiviral agents in livestock and poultry feces. Extraction and cleanup were integrated into one step. The extraction was performed using methanol-acetonitrile (1:1, v/v) with 0.5% glacial acetic acid at 90°C, and 0.75g of PSA was used as the adsorbent during the extraction procedure. Under optimal conditions, the average recoveries for 11 antiviral drugs were 71.5-112.5% at three spiked levels (20, 40, and 100μgkg -1 ). The detection limits and detection quantitations of the analysis method for the eleven antiviral drugs were 0.6-1.4 and 1.4-4.7μgkg -1 , respectively. Finally, the method was applied to analyze amantadine, oseltamivir and its metabolites oseltamivir acid in duck feces based on an experiment of an oral dose of two antiviral drugs in duck. The amantadine, oseltamivir and oseltamivir acid can be detected in feces within approximately four weeks after amantadine and oseltamivir were orally administered. The results indicate that the residue analysis in feces is a noninvasive method to monitor inhibited antiviral agents efficiently in livestock and poultry breeding. Copyright © 2017. Published by Elsevier B.V.

Optimization of clean extraction methods to isolate carotenoids from the microalga Neochloris oleoabundans and subsequent chemical characterization using liquid chromatography tandem mass spectrometry.

PubMed

Castro-Puyana, María; Herrero, Miguel; Urreta, Iratxe; Mendiola, Jose A; Cifuentes, Alejandro; Ibáñez, Elena; Suárez-Alvarez, Sonia

2013-05-01

A novel experimental design was used to optimize the extraction of carotenoids from Neochloris oleoabundans using pressurized liquid extraction with food-grade solvents such as ethanol and limonene. Experimental factors, including the extraction temperature and the solvent composition, were optimized using a three-level factorial design. The response variables extraction yield and total amount of carotenoids were assessed. The statistical analysis of the results provided mathematical models to predict the behavior of the responses as a function of the factors involved in the process. The optimum conditions predicted by the model developed in this study were 112 °C as the extraction temperature and 100% ethanol as the extraction solvent. Chemical characterization of the extracts obtained was performed by means of high-performance liquid chromatography-tandem mass spectrometry. The results obtained demonstrated that, under certain growth conditions (photoautotrophically cultured in a medium supplemented with 0.3 g L(-1) KNO3), N. oleoabundans accumulated significant total amounts of the carotenoids (from 57.4 to 120.2 mg carotenoids per gram of extract depending on the extraction conditions), mainly lutein, cantaxanthin, zeaxanthin, and astaxanthin monoesters and diesters.

Development of a Simultaneous Extraction and Cleanup Method for Pyrethroid Pesticides from Indoor House Dust Samples

EPA Science Inventory

An efficient and reliable analytical method was developed for the sensitive and selective quantification of pyrethroid pesticides (PYRs) in house dust samples. The method is based on selective pressurized liquid extraction (SPLE) of the dust-bound PYRs into dichloromethane (DCM) wi...

Extraction of anthocyanins from red cabbage using high pressure CO2.

PubMed

Xu, Zhenzhen; Wu, Jihong; Zhang, Yan; Hu, Xiaosong; Liao, Xiaojun; Wang, Zhengfu

2010-09-01

The extraction kinetics of anthocyanins from red cabbage using high pressure CO(2) (HPCD) against conventional acidified water (CAW) was investigated. The HPCD time, temperature, pressure and volume ratio of solid-liquid mixture vs. pressurized CO(2) (R((S+L)/G)) exhibited important roles on the extraction kinetics of anthocyanins. The extraction kinetics showed two phases, the yield increased with increasing the time in the first phase, the yield defined as steady-state yield (y(*)) was constant in the second phase. The y(*) of anthocyanins using HPCD increased with higher temperature, higher pressure and lower R((S+L)/G). The general mass transfer model with higher regression coefficients (R(2)>0.97) fitted the kinetic data better than the Fick's second law diffusion model. As compared with CAW, the time (t(*)) to reach the y(*) of anthocyanins using HPCD was reduced by half while its corresponding overall volumetric mass transfer coefficients k(L)xa from the general mass transfer model increased by two folds. Copyright 2010 Elsevier Ltd. All rights reserved.

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

PubMed

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

2012-06-01

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

[Analysis of saponins from panax notoginseng using pressurized solvent extraction coupled with liquid chromatography-electrospray mass spectrum].

PubMed

Wan, Jianbo; Li, Changming; Li, Shaopin; Kong, Lingyi; Wang, Yitao

2005-10-01

To establish a method for qualitative analysis of saponins from Panax notoginseng using pressurized solvent extraction coupled with LC-ESI-MS. The PSE technology was applied to the process of extraction for Panax notoginseng, and the negative ion detection and multiple reaction monitoring model were used. The saponins were investigated based on total ion chromatogram (TIC) and MRM chromatogram. According to the fragment character of saponins, the molecular weight and their structures could be identified. The method can be used for qualitative analysis of saponins from Panax notoginseng.

Selective extraction of high-value phenolic compounds from distillation wastewater of basil (Ocimum basilicum L.) by pressurized liquid extraction.

PubMed

Pagano, Imma; Sánchez-Camargo, Andrea Del Pilar; Mendiola, Jose Antonio; Campone, Luca; Cifuentes, Alejandro; Rastrelli, Luca; Ibañez, Elena

2018-01-31

During the essential oil steam distillation from aromatic herbs, huge amounts of distillation wastewaters (DWWs) are generated. These by-products represent an exceptionally rich source of phenolic compounds such as rosmarinic acid (RA) and caffeic acid (CA). Herein, the alternative use of dried basil DWWs (dDWWs) to perform a selective extraction of RA and CA by pressurized liquid extraction (PLE) employing bio-based solvent was studied. To select the most suitable solvent for PLE, the theoretical modelling of Hansen solubility parameters (HSP) was carried out. This approach allows reducing the list of candidate to two solvents: ethanol and ethyl lactate. Due to the composition of the sample, mixtures of water with those solvents were also tested. An enriched PLE extract in RA (23.90 ± 2.06 mg/g extract) with an extraction efficiency of 75.89 ± 16.03% employing a water-ethanol mixture 25:75 (% v/v) at 50°C was obtained. In the case of CA, a PLE extract with 2.42 ± 0.04 mg/g extract, having an extraction efficiency of 13.86 ± 4.96% using ethanol absolute at 50°C was achieved. DWWs are proposed as new promising sources of natural additives and/or functional ingredients for cosmetic, nutraceutical, and food applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave-assisted extraction at atmospheric pressure coupled to different clean-up methods for the determination of organophosphorus pesticides in olive and avocado oil.

PubMed

Fuentes, Edwar; Báez, María E; Díaz, Juan

2009-12-18

An effective extraction method was devised for the determination of organophosphorus pesticides (OPPs) in olive and avocado oil samples, using atmospheric pressure microwave-assisted liquid-liquid extraction (APMAE) and solid-phase extraction or low-temperature precipitation as clean-up step. A simple glass system equipped with an air-cooled condenser was designed as an extraction vessel. The pesticides were partitioned between acetonitrile and oil solution in hexane. Analytical determinations were carried out by gas chromatography-flame photometric detection and gas chromatography-tandem mass spectrometry, using a triple quadrupole mass analyzer, for confirmation purposes. Several factors influencing the extraction efficiency were investigated and optimized through fractional factorial design and Doehlert design. Under optimal conditions the recovery of pesticides from oil at 0.025 microg g(-1) ranged from 71% to 103%, except for fenthion in avocado oil, with RSDs < or = 13% (n=5). The LOQ for the entire method ranged from 0.004 to 0.015 microg g(-1). Finally, the proposed method was successfully applied to the extraction and determination of the selected pesticides in 20 commercially packed extra virgin olive oils and four commercially packed avocado oils produced in Chile. Detectable residues of different OPPs were observed in 85% of samples.

Development of green extraction processes for Nannochloropsis gaditana biomass valorization.

PubMed

Sánchez-Camargo, Andrea Del Pilar; Pleite, Natalia; Mendiola, José Antonio; Cifuentes, Alejandro; Herrero, Miguel; Gilbert-López, Bienvenida; Ibáñez, Elena

2018-04-23

In the present work, the valorization of Nannochloropsis gaditana biomass is proposed within the concept of biorefinery. To this aim, high-pressure homogenization (HPH) was used to break down the strong cell wall and supercritical fluid extraction (SFE) with pure CO 2 was applied as a first step to extract valuable compounds (such as non-polar lipids and pigments). Extraction of the remaining residue for the recovery of bioactive compounds was studied by means of an experimental design based on response surface methodology (RSM) employing pressurized liquid extraction (PLE) with green solvents such as water and ethanol. Optimum extract was achieved with pure ethanol at 170°C for 20 min, providing an important antioxidant capacity (0.72 ± 0.03 mmol trolox eq g -1 extract). Complete chemical characterization of the optimum extract was carried out by using different chromatographic methods such as reverse-phase high-performance liquid chromatography with diode array detection (RP-HPLC-DAD), normal-phase HPLC with evaporative light scattering detection (NP-HPLC-ELSD) and gas chromatography coupled to mass spectrometry detection (GC-MS); carotenoids (e.g. violaxanthin), chlorophylls and polar lipids were the main compounds observed while palmitoleic, palmitic, myristic acids and the polyunsaturated eicosapentanoic (EPA) acid were the predominant fatty acids in all PLE extracts. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Selective Extraction of Uranium from Liquid or Supercritical Carbon Dioxide

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

Farawila, Anne F.; O'Hara, Matthew J.; Wai, Chien M.

2012-07-31

Current liquid-liquid extraction processes used in recycling irradiated nuclear fuel rely on (1) strong nitric acid to dissolve uranium oxide fuel, and (2) the use of aliphatic hydrocarbons as a diluent in formulating the solvent used to extract uranium. The nitric acid dissolution process is not selective. It dissolves virtually the entire fuel meat which complicates the uranium extraction process. In addition, a solvent washing process is used to remove TBP degradation products, which adds complexity to the recycling plant and increases the overall plant footprint and cost. A liquid or supercritical carbon dioxide (l/sc -CO2) system was designed tomore » mitigate these problems. Indeed, TBP nitric acid complexes are highly soluble in l/sc -CO2 and are capable of extracting uranium directly from UO2, UO3 and U3O8 powders. This eliminates the need for total acid dissolution of the irradiated fuel. Furthermore, since CO2 is easily recycled by evaporation at room temperature and pressure, it eliminates the complex solvent washing process. In this report, we demonstrate: (1) A reprocessing scheme starting with the selective extraction of uranium from solid uranium oxides into a TBP-HNO3 loaded Sc-CO2 phase, (2) Back extraction of uranium into an aqueous phase, and (3) Conversion of recovered purified uranium into uranium oxide. The purified uranium product from step 3 can be disposed of as low level waste, or mixed with enriched uranium for use in a reactor for another fuel cycle. After an introduction on the concept and properties of supercritical fluids, we first report the characterization of the different oxides used for this project. Our extraction system and our online monitoring capability using UV-Vis absorbance spectroscopy directly in sc-CO2 is then presented. Next, the uranium extraction efficiencies and kinetics is demonstrated for different oxides and under different physical and chemical conditions: l/sc -CO2 pressure and temperature, TBP/HNO3 complex used, reductant or complexant used for selectivity, and ionic liquids used as supportive media. To complete the extraction and recovery cycle, we then demonstrate uranium back extraction from the TBP loaded sc-CO2 phase into an aqueous phase and the characterization of the uranium complex formed at the end of this process. Another aspect of this project was to limit proliferation risks by either co-extracting uranium and plutonium, or by leaving plutonium behind by selectively extracting uranium. We report that the former is easily achieved, since plutonium is in the tetravalent or hexavalent oxidation state in the oxidizing environment created by the TBP-nitric acid complex, and is therefore co-extracted. The latter is more challenging, as a reductant or complexant to plutonium has to be used to selectively extract uranium. After undertaking experiments on different reducing or complexing systems (e.g., AcetoHydroxamic Acid (AHA), Fe(II), ascorbic acid), oxalic acid was chosen as it can complex tetravalent actinides (Pu, Np, Th) in the aqueous phase while allowing the extraction of hexavalent uranium in the sc-CO2 phase. Finally, we show results using an alternative media to commonly used aqueous phases: ionic liquids. We show the dissolution of uranium in ionic liquids and its extraction using sc-CO2 with and without the presence of AHA. The possible separation of trivalent actinides from uranium is also demonstrated in ionic liquids using neodymium as a surrogate and diglycolamides as the extractant.« less

Artificial neural network modeling and optimization of ultrahigh pressure extraction of green tea polyphenols.

PubMed

Xi, Jun; Xue, Yujing; Xu, Yinxiang; Shen, Yuhong

2013-11-01

In this study, the ultrahigh pressure extraction of green tea polyphenols was modeled and optimized by a three-layer artificial neural network. A feed-forward neural network trained with an error back-propagation algorithm was used to evaluate the effects of pressure, liquid/solid ratio and ethanol concentration on the total phenolic content of green tea extracts. The neural network coupled with genetic algorithms was also used to optimize the conditions needed to obtain the highest yield of tea polyphenols. The obtained optimal architecture of artificial neural network model involved a feed-forward neural network with three input neurons, one hidden layer with eight neurons and one output layer including single neuron. The trained network gave the minimum value in the MSE of 0.03 and the maximum value in the R(2) of 0.9571, which implied a good agreement between the predicted value and the actual value, and confirmed a good generalization of the network. Based on the combination of neural network and genetic algorithms, the optimum extraction conditions for the highest yield of green tea polyphenols were determined as follows: 498.8 MPa for pressure, 20.8 mL/g for liquid/solid ratio and 53.6% for ethanol concentration. The total phenolic content of the actual measurement under the optimum predicated extraction conditions was 582.4 ± 0.63 mg/g DW, which was well matched with the predicted value (597.2mg/g DW). This suggests that the artificial neural network model described in this work is an efficient quantitative tool to predict the extraction efficiency of green tea polyphenols. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

Extraction of benzene and cyclohexane using [BMIM][N(CN)2] and their equilibrium modeling

NASA Astrophysics Data System (ADS)

Ismail, Marhaina; Bustam, M. Azmi; Man, Zakaria

2017-12-01

The separation of aromatic compound from aliphatic mixture is one of the essential industrial processes for an economically green process. In order to determine the separation efficiency of ionic liquid (IL) as a solvent in the separation, the ternary diagram of liquid-liquid extraction (LLE) 1-butyl-3-methylimidazolium dicyanamide [BMIM][N(CN)2] with benzene and cyclohexane was studied at T=298.15 K and atmospheric pressure. The solute distribution coefficient and solvent selectivity derived from the equilibrium data were used to evaluate if the selected ionic liquid can be considered as potential solvent for the separation of benzene from cyclohexane. The experimental tie line data was correlated using non-random two liquid model (NRTL) and Margules model. It was found that the solute distribution coefficient is (0.4430-0.0776) and selectivity of [BMIM][N(CN)2] for benzene is (53.6-13.9). The ternary diagram showed that the selected IL can perform the separation of benzene and cyclohexane as it has extractive capacity and selectivity. Therefore, [BMIM][N(CN)2] can be considered as a potential extracting solvent for the LLE of benzene and cyclohexane.

Pressurized liquid extraction of anthocyanins and biflavonoids from Schinus terebinthifolius Raddi: A multivariate optimization.

PubMed

Feuereisen, Michelle M; Gamero Barraza, Mariana; Zimmermann, Benno F; Schieber, Andreas; Schulze-Kaysers, Nadine

2017-01-01

Response surface methodology was employed to investigate the effects of pressurized liquid extraction (PLE) parameters on the recovery of phenolic compounds (anthocyanins, biflavonoids) from Brazilian pepper (Schinus terebinthifolius Raddi) fruits. The effects of temperature, static time, and ethanol as well as acid concentration on the polyphenol yield were described well by quadratic models (p<0.0001). A significant influence of the ethanol concentration (p<0.0001) and several interactions (p<0.05) were identified. Identification of the biflavonoid I3',II8-binaringenin in drupes of S. terebinthifolius was achieved by UHPLC-MS(2). Interestingly, at high extraction temperatures (>75°C), an artifact occurred and was tentatively identified as a diastereomer of I3',II8-binaringenin. Multivariate optimization led to high yields of phenolic compounds from the exocarp/drupes at 100/75°C, 10/10min, 54.5/54.2% ethanol, and 5/0.03% acetic acid. This study demonstrates that PLE is well suited for the extraction of phenolic compounds from S. terebinthifolius and can efficiently be optimized by response surface methodology. Copyright © 2016 Elsevier Ltd. All rights reserved.

Exploring in vitro neurobiological effects and high-pressure liquid chromatography-assisted quantitation of chlorogenic acid in 18 Turkish coffee brands.

PubMed

Erdem, Sinem Aslan; Senol, F Sezer; Budakoglu, Esin; Orhan, Ilkay Erdogan; Sener, Bilge

2016-01-01

The hydroalcoholic extracts of the Turkish traditional coffee samples from 18 commercial brands were tested for their neurobiological effects through enzyme inhibition based on enzyme-linked immunosorbance microtiter assays against acetylcholinesterase, butyrylcholinesterase, and tyrosinase, linked to Alzheimer's and Parkinson's diseases. The extracts were also subjected to several antioxidant test systems to define their antiradical, metal-chelation capacity, and reducing power. Total phenol and flavonoid contents in the extracts were delineated by spectrophotometric methods, while chlorogenic acid in the coffee samples was quantified by high-pressure liquid chromatography. The extracts displayed low to moderate inhibition (from 2.13 ± 0.01% to 36.12 ± 1.07% at 200 μg/mL) against the tested enzymes, whereas they had notable 2,2'-diphenyl-1-picrylhydrazyl radical scavenging activity up to 56.15 ± 2.03% at 200 μg/mL. The extracts exerted a remarkable ferric-reducing antioxidant power values, while chlorogenic acid was found to range between 0.288 ± 0.005% and 2.335 ± 0.010%. Copyright © 2015. Published by Elsevier B.V.

Multi-class analysis of new psychoactive substances and metabolites in hair by pressurized liquid extraction coupled to HPLC-HRMS.

PubMed

Montesano, Camilla; Vannutelli, Gabriele; Massa, Maristella; Simeoni, Maria Chiara; Gregori, Adolfo; Ripani, Luigi; Compagnone, Dario; Curini, Roberta; Sergi, Manuel

2017-05-01

In this paper, an analytical method has been developed and validated for the analysis of new psychoactive substances (NPS) and metabolites in hair samples. The method was based on pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) clean-up and high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) analysis. To evaluate extraction efficiency and the applicability of the method, hair samples were fortified by soaking in order to obtain a good surrogate for drug users' hair; the amount of incorporated drugs related to their lipophilicity, similarly to in vivo drug incorporation. To the best of our knowledge, this is the first method that allowed for the analysis of both cathinones (5) and synthetic cannabinoids (7) in hair with a single extraction procedure and chromatographic run. A phenethylamine (2C-T-4), 4- fluorophenylpiperazine and methoxetamine were also included showing that PLE coupled to SPE clean-up was suitable for a multi-class analysis of NPS in hair. In addition, the use of PLE significantly reduced hair analysis time: decontamination, incubation, clean-up, and liquid chromatography-mass spectrometry (LC-MS) analysis were carried out in approximately 45 min. The method was fully validated according to Scientific Working Group for Forensic Toxicology (SWGTOX) and Society of Hair Testing (SoHT) guidelines. Limit of quantification (LOQ) values ranged from 8 to 50 pg mg -1 for cathinones, phenetylamines and piperazines, and from 9 to 40 pg mg -1 for synthetic cannabinoids (10 pg mg -1 for methoxetamine). Matrix effects were below 15% for all the analytes, demonstrating the effectiveness of the clean-up step. Inaccuracy was lower than 9% in terms of bias. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Identification of degradation products in loxoprofen sodium adhesive tapes by liquid chromatography-mass spectrometry and dynamic pressurized liquid extraction-solid-phase extraction coupled to liquid chromatography-nuclear magnetic resonance spectroscopy.

PubMed

Murakami, Tomonori; Kawasaki, Takao; Takemura, Akira; Fukutsu, Naoto; Kishi, Naoyuki; Kusu, Fumiyo

2008-10-24

Rapid and unambiguous identification of three degradation products (DP-1, DP-2 and DP-3) found in heat-stressed loxoprofen sodium adhesive tapes (Loxonin tapes) was achieved by LC-MS and dynamic pressurized liquid extraction (PLE)-solid-phase extraction (SPE) coupled to LC-NMR without complicated isolation or purification processes. The molecular formulae of the degradation products were determined by accurate mass measurements and product ion analyses and on-line hydrogen/deuterium (H/D) exchange experiments provided information about changes in the degradation of loxoprofen. To compensate for the low sensitivity of NMR, on-line dynamic PLE-SPE was employed and higher concentrations of degradation products trapped on the SPE column were afforded in a shorter time than they would be in such time-consuming sample preparations as pre-concentration after extraction. The loop-storage procedure was used in the LC-NMR analysis to allow the acquisition of the (1)H spectra of the three degradation products in one chromatographic run without affecting the peak separation and to avoid the carry-over of previously eluted DP-1 of high concentration by washing the NMR detection cell prior to the measurement of the DP-2 spectrum. Based on the resulting (1)H NMR spectra in combination with the MS results, DP-1 was successfully identified as an oxidation product having an oxodicarboxylic acid structure formed by the cleavage of the cyclopentanone ring of loxoprofen, DP-2 as a cyclopentanone ring-hydroxylated loxoprofen and DP-3 as a loxoprofen l-menthol ester.

Separation and purification of xenon

DOEpatents

Schlea, deceased, Carl Solomon

1978-03-14

Xenon is separated from a mixture of xenon and krypton by extractive distillation using carbon tetrafluoride as the partitioning agent. Krypton is flushed out of the distillation column with CF.sub.4 in the gaseous overhead stream while purified xenon is recovered from the liquid bottoms. The distillation is conducted at about atmospheric pressure or at subatmospheric pressure.

Direct Printing of Stretchable Elastomers for Highly Sensitive Capillary Pressure Sensors.

PubMed

Liu, Wenguang; Yan, Chaoyi

2018-03-28

We demonstrate the successful fabrication of highly sensitive capillary pressure sensors using an innovative 3D printing method. Unlike conventional capacitive pressure sensors where the capacitance changes were due to the pressure-induced interspace variations between the parallel plate electrodes, in our capillary sensors the capacitance was determined by the extrusion and extraction of liquid medium and consequent changes of dielectric constants. Significant pressure sensitivity advances up to 547.9 KPa -1 were achieved. Moreover, we suggest that our innovative capillary pressure sensors can adopt a wide range of liquid mediums, such as ethanol, deionized water, and their mixtures. The devices also showed stable performances upon repeated pressing cycles. The direct and versatile printing method combined with the significant performance advances are expected to find important applications in future stretchable and wearable electronics.

Preliminary extraction of tannins by 1-butyl-3-methylimidazole bromide and its subsequent removal from Galla chinensis extract using macroporous resins.

PubMed

Lu, Chunxia; Luo, Xiaoling; Lu, Liliang; Li, Hongmin; Chen, Xia; Ji, Yong

2013-03-01

In recent years, ionic liquids have become increasingly attractive as 'green solvents' used in the extraction of bioactive compounds from natural plant. However, the separation of ionic liquid from the target compounds was difficult, due to their low vapour pressure and high stabilities. In our study, ionic liquid-based ultrasonic and microwave-assisted extraction was used to obtain the crude tannins, then the macroporous resin adsorption technology was further employed to purify the tannins and remove the ionic liquid from crude extract. The results showed that XDA-6 had higher separation efficiency than other tested resins, and the equilibrium experimental data were well fitted to Langmuir isotherms. Dynamic adsorption and desorption were performed on XDA-6 packed in glass columns to optimise the separation process. The optimum conditions as follows: the ratio of column height to diameter bed was 1:8, flow rate 1 BV/h (bed volume per hour), 85% ethanol was used as eluant while the elution volume was 2 BV. Under the optimised conditions, the adsorption and desoption rate of tannins in XDA-6 were 94.81 and 91.63%, respectively. The content of tannins was increased from 70.24% in Galla chinensis extract to 85.12% with a recovery of 99.06%. The result of ultra-performance liquid chromatography (UPLC)-MS/MS analysis showed that [bmim]Br could be removed from extract. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phenolic and triterpenoid antioxidants from Origanum majorana L. herb and extracts obtained with different solvents.

PubMed

Vági, E; Rapavi, E; Hadolin, M; Vásárhelyiné Perédi, K; Balázs, A; Blázovics, A; Simándi, B

2005-01-12

Antioxidant properties of marjoram (Origanum majorana L.) herb and extracts obtained with ethanol, n-hexane, and supercritical CO2 extraction are presented. Individual antioxidants, ursolic acid, carnosic acid, and carnosol, were quantified with high-performance liquid chromatography. The effects of different parameters (temperature and pressure) of high-pressure extraction on the yield of carnosol were studied. Furthermore, two marjoram herbs from Hungary and Egypt were compared measuring hydrogen-donating abilities with 1,1-diphenyl-2-picrylhydrazyl by spectrophotometric and the total scavenger capacities by chemiluminometric methods from the aqueous extracts of the herbs. The antioxidant activities of the solvent extracts were performed using the Rancimat method. The Egyptian herb and its extracts possessed better antioxidant activities than Hungarian ones. Applying supercritical CO2 extraction, the highest value of carnosol was obtained at 400 bar and 60 degrees C.

Isolation and Identification of Secondary Metabolites from the Aerial Parts of Stachys lavandulifolia Vahl.

PubMed

Sajjadi, Seyed Ebrahim; Ghanadian, Seyed Mustafa; Rabbani, Mohammad; Tahmasbi, Fateme

2017-01-01

Stachys lavandulifolia Vahl is an herbaceous wild plant native to Iran which is traditionally used in Iranian folk medicine as a mild sedative tea for reducing anxiety and for treatment of gastrointestinal disorders. Our previous study on ethyl acetate extract of S. lavandulifolia proved anti-anxiolytic activity and so the present study was designed to determine chemical components of this biologically active fraction. The extract was prepared using maceration method. Column chromatography and medium pressure liquid chromatography (MPLC) was used respectively to separate the fractions. Finally, some evaluated fractions were used for high pressure liquid (HPLC) and peak shaving recycle technique to achieve more purification. Separated compounds were determined using NMR analysis and mass spectroscopy. Six compounds have been isolated from ethylacetate extract of aerial parts of S. lavandulifolia including four flavonoids (apigenin, kumatakenin, penduletin and 4', 7-dihyroxy- 3, 5, 6-trimethoxy flavon), a labdan diterpenoid (labda-13-en-8, 15-diol), and an iridoid.

Optimization of drying process and pressurized liquid extraction for recovery of bioactive compounds from avocado peel by-product.

PubMed

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

2018-04-16

The aim of the present study was to optimize the extraction of phenolic compounds in avocado peel using pressurized liquid extraction (PLE) with GRAS solvents. Response surface methodology (RSM) based on Central Composite Design 2 2 model was used in order to optimize PLE conditions. Moreover, the effect of air drying temperature on the total polyphenol content (TPC) and individual phenolic compounds concentration were evaluated. The quantification of individual compounds was performed by HPLC-DAD-ESI-TOF-MS. The optimized extraction conditions were 200°C as extraction temperature and 1:1 v/v as ethanol/water ratio. Regarding to the effect of drying, the highest TPC was obtained with a drying temperature of 85°C. Forty seven phenolic compounds were quantified in the obtained extracts, showing that phenolic acids found to be the more stables compounds to drying process, while procyanidins were the more thermolabiles analytes. To our knowledge, this is the first available study in which phenolic compounds extraction was optimized using PLE and such amount of phenolic compounds was quantified in avocado peel. These results confirm that PLE represents a powerful tool to obtain avocado peel extracts with high concentration in bioactive compounds suitable for its use in the food, cosmetic or pharmaceutical sector. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phase Equilibrium Investigation on 2-Phenylethanol in Binary and Ternary Systems: Influence of High Pressure on Density and Solid-Liquid Phase Equilibrium.

PubMed

Domańska, Urszula; Królikowski, Marek; Wlazło, Michał; Więckowski, Mikołaj

2018-05-30

Ionic liquids (ILs) are important new solvents proposed for applications in different separation processes. Herein, an idea of possible use of high pressure in a general strategy of production of 2-phenylethanol (PEA) is discussed. In this work, we present the influence of pressure on the density in binary systems of {1-hexyl-1-methylpyrrolidynium bis{(trifluoromethyl)sulfonyl}imide, [HMPYR][NTf 2 ], or 1-dodecyl-3-methylimidazolium bis{(trifluoromethyl)sulfonyl}imide, [DoMIM][NTf 2 ] + PEA} in a wide range of temperatures (298.15-348.15 K) and pressures (0.1-40 MPa). The densities at ambient and high pressures are measured to present the physicochemical properties of the ILs used in the process of separation of PEA from aqueous phase. The Tait equation was used for the correlation of density of one-component and two-component systems as a function of mole fraction, temperature, and pressure. The influence of pressure is not significant. These systems exhibit mainly negative molar excess volumes, V E . The solid-liquid phase equilibrium (SLE) of [DoMIM][NTf 2 ] in PEA at atmospheric pressure was measured and compared to the SLE high-pressure results. Additionally, the ternary liquid-liquid phase equilibrium (LLE) at ambient pressure in the {[DoMIM][NTf 2 ] (1) + PEA (2) + water (3)} at temperature T = 308.15 K was investigated. The solubility of water in the [DoMIM][NTf 2 ] is quite high in comparison with that measured by us earlier for ILs ( x 3 = 0.403) at T = 308.15 K, which results in not very successful average selectivity of extraction of PEA from the aqueous phase. The [DoMIM][NTf 2 ] has shown strong interaction with PEA without the immiscibility region. The ternary system revealed Treybal's type phase equilibrium in which two partially miscible binaries ([DoMIM][NTf 2 ] + water) and (PEA + water) exist. From the results of LLE in the ternary system, the selectivity and the solute distribution ratio of separation of water/PEA were calculated and compared to the results obtained for the ILs measured earlier by us. The popular NRTL model was used to correlate the experimental tie-lines in ternary LLE. These results may help in a new technological project of "in situ" extraction of PEA from aqueous phase during the biosynthesis.

A novel method for analysing key corticosteroids in polar bear (Ursus maritimus) hair using liquid chromatography tandem mass spectrometry.

PubMed

Weisser, Johan J; Hansen, Martin; Björklund, Erland; Sonne, Christian; Dietz, Rune; Styrishave, Bjarne

2016-04-01

This paper presents the development and evaluation of a methodology for extraction, clean-up and analysis of three key corticosteroids (aldosterone, cortisol and corticosterone) in polar bear hair. Such a methodology can be used to monitor stress biomarkers in polar bears and may provide as a useful tool for long-term and retrospective information. We developed a combined pressurized liquid extraction (PLE)-solid phase extraction (SPE) procedure for corticosteroid extraction and clean-up followed by high pressure liquid chromatography tandem mass spectrometry (HPLC-MS/MS) analysis. This procedure allows for the simultaneous determination of multiple steroids, which is in contrast to previous polar bear studies based on ELISA techniques. Absolute method recoveries were 81%, 75% and 60% for cortisol, corticosterone and aldosterone, respectively. We applied the developed method on a hair sample pooled from four East Greenland polar bears. Herein cortisol and corticosterone were successfully determined in levels of 0.32±0.02ng/g hair and 0.13±0.02ng/g hair, respectively. Aldosterone was below limit of detection (LOD<0.17ng/g). The cortisol hair concentration found in these East Greenland polar bears was consistent with cortisol levels previously determined in the Southern Hudson Bay and James Bay in Canada using ELISA kits. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Zero Gravity Cryogenic Vent System Concepts for Upper Stages

NASA Astrophysics Data System (ADS)

Ravex, Alain; Flachbart, Robin; Holt, Barney

The capability to vent in zero gravity without resettling is a technology need that involves practically all uses of sub-critical cryogenics in space. Venting without resettling would extend cryogenic orbital transfer vehicle capabilities. However, the lack of definition regarding liquid/ullage orientation coupled with the somewhat random nature of the thermal stratification and resulting pressure rise rates, lead to significant technical challenges. Typically a zero gravity vent concept, termed a thermodynamic vent system (TVS), consists of a tank mixer to destratify the propellant, combined with a Joule-Thomson (J-T) valve to extract thermal energy from the propellant. Marshall Space Flight Center's (MSFC's) Multipurpose Hydrogen Test Bed (MHTB) was used to test both spray bar and axial jet TVS concepts. The axial jet system consists of a recirculation pump heat exchanger unit. The spray bar system consists of a recirculation pump, a parallel flow concentric tube, heat exchanger, and a spray bar positioned close to the longitudinal axis of the tank. The operation of both concepts is similar. In the mixing mode, the recirculation pump withdraws liquid from the tank and sprays it into the tank liquid, ullage, and exposed tank surfaces. When energy extraction is required, a small portion of the recirculated liquid is passed sequentially through the J-T expansion valve, the heat exchanger, and is vented overboard. The vented vapor cools the circulated bulk fluid, thereby removing thermal energy and reducing tank pressure. The pump operates alone, cycling on and off, to destratify the tank liquid and ullage until the liquid vapor pressure reaches the lower set point. At that point, the J-T valve begins to cycle on and off with the pump. Thus, for short duration missions, only the mixer may operate, thus minimizing or even eliminating boil-off losses. TVS performance testing demonstrated that the spray bar was effective in providing tank pressure control within a 6.89 kPa (1psi) band for fill levels of 90%, 50%, and 25%. Complete destratification of the liquid and ullage was achieved at these fill levels. The axial jet was effective in providing tank pressure control within the same pressure control band at the 90% fill level. However, at the 50% level, the system reached a point at which it was unable to extract enough energy to keep up with the heat leak into the tank. Due to a hardware problem, the recirculation pump operated well below the axial jet design flow rate. Therefore, it is likely that the performance of the axial jet would have improved had the pump operated at the proper flow rate. A CFD model is being used to determine if the desired axial jet performance would be achieved if a higher pump flow rate were available. Testing conducted thus far has demonstrated that both TVS concepts can be effective in destratifying a propellant tank, rejecting stored heat energy, and thus, controlling tank pressure.

Phenylpropanoid-substituted procyanidins and tentatively identified procyanidin glycosides from hawthorn (Crataegus spp.).

PubMed

Sendker, Jandirk; Petereit, Frank; Lautenschläger, Marcus; Hellenbrand, Nils; Hensel, Andreas

2013-01-01

The rational use of hawthorn leafs and flowers from Crataegus spp. for declining cardiac performance is mainly due to flavon-C-glycosides and oligomeric procyanidins (OPC). From OPC-enriched extracts from different batches, a dimeric phenylpropanoid-substituted procyanidin (cinchonain II b, 1) was isolated and characterized by MS, CD, and NMR. Also the presence of higher oligomeric cinchonains (degree of polymerization 3 to 8) in hawthorn extracts was shown by a specific ultrahigh-pressure liquid chromatography-ESI-qTOF-MS method. Interestingly, strong evidence for the occurrence of oligomeric procyanidin hexosides was found by ultrahigh-pressure liquid chromatography-ESI-qTOF-MS analysis which additionally revealed the presence of peaks indicative of dimeric procyanidin hexosides by their exact mass, which were clearly distinguishable from the cinchonain II type peaks. Georg Thieme Verlag KG Stuttgart · New York.

Quantification of the antiplasmodial alkaloid carpaine in papaya (Carica papaya) leaves.

PubMed

Julianti, Tasqiah; Oufir, Mouhssin; Hamburger, Matthias

2014-08-01

Daily consumption of papaya (Carica papaya) leaves as greens and an herbal infusion is common in some parts of Indonesia as a means for preventing malaria. Antiplasmodial activity of the leaf extracts and of the main alkaloid carpaine were recently confirmed. A quantitative assay for determination of carpaine in papaya leaves was developed and validated. The assay involved pressurized liquid extraction and quantification with the aid of ultrahigh-performance liquid chromatography-tandem mass spectroscopy. Extraction conditions were optimized with respect to solvent, temperature, and number of extraction cycles. The ultrahigh-performance liquid chromatography-tandem mass spectroscopy assay was validated over a range of 20-5000 ng/mL (R(2) of 0.9908). A total of 29 papaya leaf samples were analyzed, and carpaine concentration in dry leaves was found to range from 0.02 to 0.31%. No obvious dependence on geographic origin and leaf maturity was observed. Georg Thieme Verlag KG Stuttgart · New York.

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.

Comparison between 2 methods of solid-liquid extraction for the production of Cinchona calisaya elixir: an experimental kinetics and numerical modeling approach.

PubMed

Naviglio, Daniele; Formato, Andrea; Gallo, Monica

2014-09-01

The purpose of this study is to compare the extraction process for the production of China elixir starting from the same vegetable mixture, as performed by conventional maceration or a cyclically pressurized extraction process (rapid solid-liquid dynamic extraction) using the Naviglio Extractor. Dry residue was used as a marker for the kinetics of the extraction process because it was proportional to the amount of active principles extracted and, therefore, to their total concentration in the solution. UV spectra of the hydroalcoholic extracts allowed for the identification of the predominant chemical species in the extracts, while the organoleptic tests carried out on the final product provided an indication of the acceptance of the beverage and highlighted features that were not detectable by instrumental analytical techniques. In addition, a numerical simulation of the process has been performed, obtaining useful information about the timing of the process (time history) as well as its mathematical description. © 2014 Institute of Food Technologists®

Method and apparatus for extracting water from air using a desiccant

DOEpatents

Spletzer, Barry L.; Callow, Diane Schafer

2003-01-01

The present invention provides a method and apparatus for extracting liquid water from moist air using minimal energy input. The method can be considered as four phases: (1) adsorbing water from air into a desiccant, (2) isolating the water-laden desiccant from the air source, (3) desorbing water as vapor from the desiccant into a chamber, and (4) isolating the desiccant from the chamber, and compressing the vapor in the chamber to form liquid condensate. The liquid condensate can be removed for use. Careful design of the dead volumes and pressure balances can minimize the energy required. The dried air can be exchanged for fresh moist air and the process repeated. An apparatus comprises a first chamber in fluid communication with a desiccant, and having ports to intake moist air and exhaust dried air. The apparatus also comprises a second chamber in fluid communication with the desiccant. The second chamber allows variable internal pressure, and has a port for removal of liquid condensate. Each chamber can be configured to be isolated or in communication with the desiccant. The first chamber can be configured to be isolated or in communication with a course of moist air. Various arrangements of valves, pistons, and chambers are described.

Determination of glucosinolates in rapeseed and Thlaspi caerulescens plants by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.

PubMed

Tolrà, R P; Alonso, R; Poschenrieder, C; Barceló, D; Barceló, J

2000-08-11

Liquid chromatography-atmospheric pressure chemical ionization mass spectrometry was used to identify glucosinolates in plant extracts. Optimization of the analytical conditions and the determination of the method detection limit was performed using commercial 2-propenylglucosinolate (sinigrin). Optimal values for the following parameters were determined: nebulization pressure, gas temperature, flux of drying gas, capillar voltage, corona current and fragmentor conditions. The method detection limit for sinigrin was 2.85 ng. For validation of the method the glucosinolates in reference material (rapeseed) from the Community Bureau of Reference Materials (BCR) were analyzed. The method was applied for the determination of glucosinolates in Thlaspi caerulescens plants.

Apparatus and method for phosphate-accelerated bioremediation

DOEpatents

Looney, Brian B.; Pfiffner, Susan M.; Phelps, Tommy J.; Lombard, Kenneth H.; Hazen, Terry C.; Borthen, James W.

1998-01-01

An apparatus and method for supplying a vapor-phase nutrient to contaminated soil for in situ bioremediation. The apparatus includes a housing adapted for containing a quantity of the liquid nutrient, a conduit in communication with the interior of the housing, means for causing a gas to flow through the conduit, and means for contacting the gas with the liquid so that a portion thereof evaporates and mixes with the gas. The mixture of gas and nutrient vapor is delivered to the contaminated site via a system of injection and extraction wells configured to the site and provides for the use of a passive delivery system. The mixture has a partial pressure of vaporized nutrient that is no greater than the vapor pressure of the liquid. If desired, the nutrient and/or the gas may be heated to increase the vapor pressure and the nutrient concentration of the mixture. Preferably, the nutrient is a volatile, substantially nontoxic and nonflammable organic phosphate that is a liquid at environmental temperatures, such as triethyl phosphate or tributyl phosphate.

Apparatus and method for phosphate-accelerated bioremediation

DOEpatents

Looney, B.B.; Phelps, T.J.; Hazen, T.C.; Pfiffner, S.M.; Lombard, K.H.; Borthen, J.W.

1994-01-01

An apparatus and method for supplying a vapor-phase nutrient to contaminated soil for in situ bioremediation. The apparatus includes a housing adapted for containing a quantity of the liquid nutrient, a conduit in fluid communication with the interior of the housing, means for causing a gas to flow through the conduit, and means for contacting the gas with the liquid so that a portion thereof evaporates and mixes with the gas. The mixture of gas and nutrient vapor is delivered to the contaminated site via a system of injection and extraction wells configured to the site. The mixture has a partial pressure of vaporized nutrient that is no greater than the vapor pressure of the liquid. If desired, the nutrient and/or the gas may be heated to increase the vapor pressure and the nutrient concentration of the mixture. Preferably, the nutrient is a volatile, substantially nontoxic and nonflammable organic phosphate that is a liquid at environmental temperatures, such as triethyl phosphate or tributyl phosphate.

Method for phosphate-accelerated bioremediation

DOEpatents

Looney, Brian B.; Lombard, Kenneth H.; Hazen, Terry C.; Pfiffner, Susan M.; Phelps, Tommy J.; Borthen, James W.

1996-01-01

An apparatus and method for supplying a vapor-phase nutrient to contaminated soil for in situ bioremediation. The apparatus includes a housing adapted for containing a quantity of the liquid nutrient, a conduit in fluid communication with the interior of the housing, means for causing a gas to flow through the conduit, and means for contacting the gas with the liquid so that a portion thereof evaporates and mixes with the gas. The mixture of gas and nutrient vapor is delivered to the contaminated site via a system of injection and extraction wells configured to the site. The mixture has a partial pressure of vaporized nutrient that is no greater than the vapor pressure of the liquid. If desired, the nutrient and/or the gas may be heated to increase the vapor pressure and the nutrient concentration of the mixture. Preferably, the nutrient is a volatile, substantially nontoxic and nonflammable organic phosphate that is a liquid at environmental temperatures, such as triethyl phosphate or tributyl phosphate.

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

PubMed

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

2015-06-26

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

Stereoselective quantification of methadone and a d(6)-labeled isotopomer using high performance liquid chromatography-atmospheric pressure chemical ionization mass-spectrometry: application to a pharmacokinetic study in a methadone maintained subject.

PubMed

Foster, David J R; Morton, Erin B; Heinkele, Georg; Mürdter, Thomas E; Somogyi, Andrew A

2006-08-01

There is evidence that the apparent oral clearance of rac-methadone is induced during the early phase of methadone maintenance treatment. However, it is not known if this is due to changes in bioavailability or if this phenomenon is stereoselective. This knowledge can be obtained by administering a dose of stable-labeled methadone at selected times during ongoing treatment. Therefore, the authors developed a stereoselective high performance liquid chromatography-atmospheric pressure chemical ionization mass-spectrometry assay for the quantification of the enantiomers of methadone and a d(6)-labeled isotopomer. The compounds were quantified in a single assay after liquid-liquid extraction and stereoselective high performance liquid chromatograph with atmospheric pressure chemical ionization-mass spectrometry detection. The following ions were monitored: m/z 310.15 for unlabeled methadone; m/z 316.15 for methadone-d(6); and m/z 313.15 for the methadone-d(3) (internal standard). Calibration curves ranged from 0.5 to 75 ng/mL for each compound. Extraction recovery was approximately 80% for all analytes, without evidence of differences between the unlabeled and stable-labeled compounds or concentration dependency. Minor ion promotion was observed (<15%) but this was identical for all analytes including the d(3)-labeled internal standard, with peak area ratios in extracted samples identical to control injections. The isotopomers did not alter each others' ionisation, even at 10:1 concentration ratios, and 10-fold diluted samples were within 10% of the nominal concentration. Assay performance was acceptable, with interassay and intra-assay bias and precision <10% for all compounds, including the upper and lower limits of quantitation. In conclusion, the assay was successfully applied to quantify the concentration of the methadone enantiomers of both orally administered unlabeled methadone and an intravenous 5 mg dose of methadone-d(6) in a patient receiving chronic oral methadone maintenance therapy.

Development of a high performance liquid chromatography method and a liquid chromatography-tandem mass spectrometry method with the pressurized liquid extraction for the quantification and confirmation of sulfonamides in the foods of animal origin.

PubMed

Yu, Huan; Tao, Yanfei; Chen, Dongmei; Wang, Yulian; Huang, Lingli; Peng, Dapeng; Dai, Menghong; Liu, Zhenli; Wang, Xu; Yuan, Zonghui

2011-09-01

The residues of sulfonamides (SAs) in the foods of animal origin are of the major concern because they are harmful to the consumer's health and could induce pathogens to develop resistance. Rapid and efficient determination methods are urgently in need. A quantitative high performance liquid chromatography method (HPLC) and a confirmative liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 18 sulfonamides such as sulfamidinum, sulfanilamide, sulfisomidine, sulfadiazine, sulfapyridine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamethoxypyridazine, sulfamethoxydiazine, sulfisoxazole, sulfachloropyridazine, sulfamethoxazole, sulfamonomethoxine, sulfadoxine, sulfaclozine, sulfadimethoxine, sulfaquinoxaline in the muscles, livers and kidneys of swine, bovine and chicken were developed and validated. The sample preparation procedures included a pressurized liquid extraction (PLE) with acetonitrile conducted at elevated temperature (70°C) and pressure (1400 psi). After clean-up with hydrophilic-lipophilic balance cartridge, the extraction solution was concentrated and analyzed by HPLC and LC-MS/MS analysis. 18 SAs were separated by the HPLC with a Zorbax SB-Aq-C18 column and the mobile phase of methanol/acetonitrile/1% acetic acid with a gradient system. The wavelength of UV for the HPLC detection was set at 285 nm. The LC-MS/MS analysis was achieved with a Hypersil Golden column and the mobile phase of acetonitrile and 0.1% formic acid aqueous solution with two gradient systems. The Limits of detection (LOD) and the limits of quantitation (LOQ) were 3 μg/kg and 10 μg/kg, respectively, for both of the HPLC and LC-MS/MS. Linearity was obtained with an average coefficient of determination (R) higher than 0.9980 over a dynamic range from the LOQ value up to 5000 μg/kg. The recoveries of the methods range from 71.1% to 118.3% with the relative standard derivation less than 13%. The peaks of interest with no interferences were observed throughout the chromatographic run. The sample pretreatment provided efficient extraction and cleanup that enables a sensitive and rugged determination of 18 SAs, the obtained results revealed that PLE, in comparison with other sample preparation methods applied, has significantly higher efficacy for SAs isolation from animal tissues. Copyright © 2011 Elsevier B.V. All rights reserved.

Zero Gravity Cryogenic Vent System Concepts for Upper Stages

NASA Technical Reports Server (NTRS)

Flachbart, Robin H.; Holt, James B.; Hastings, Leon J.

2001-01-01

The capability to vent in zero gravity without resettling is a technology need that involves practically all uses of sub-critical cryogenics in space, and would extend cryogenic orbital transfer vehicle capabilities. However, the lack of definition regarding liquid/ullage orientation coupled with the somewhat random nature of the thermal stratification and resulting pressure rise rates, lead to significant technical challenges. Typically a zero gravity vent concept, termed a thermodynamic vent system (TVS), consists of a tank mixer to destratify the propellant, combined with a Joule-Thomson (J-T) valve to extract thermal energy from the propellant. Marshall Space Flight Center's (MSFC's) Multipurpose Hydrogen Test Bed (MHTB) was used to test both spray-bar and axial jet TVS concepts. The axial jet system consists of a recirculation pump heat exchanger unit. The spray-bar system consists of a recirculation pump, a parallel flow concentric tube heat exchanger, and a spray-bar positioned close to the longitudinal axis of the tank. The operation of both concepts is similar. In the mixing mode, the recirculation pump withdraws liquid from the tank and sprays it into the tank liquid, ullage, and exposed tank surfaces. When energy extraction is required, a small portion of the recirculated liquid is passed sequentially through the J-T expansion valve, the heat exchanger, and is vented overboard. The vented vapor cools the circulated bulk fluid, thereby removing thermal energy and reducing tank pressure. The pump operates alone, cycling on and off, to destratify the tank liquid and ullage until the liquid vapor pressure reaches the lower set point. At that point, the J-T valve begins to cycle on and off with the pump. Thus, for short duration missions, only the mixer may operate, thus minimizing or even eliminating boil-off losses.

O the Electrohydrodynamics of Drop Extraction from a Conductive Liquid Meniscus

NASA Astrophysics Data System (ADS)

Wright, Graham Scott

This thesis is concerned with the use of an electric field in the extraction of liquid drops from a capillary orifice or nozzle. The motivating application is ink jet printing. Current drop-on-demand ink jets use pressure pulses to eject drops. Literature on electrostatic spraying suggests that by using an electric field, drops could be produced with a wider range of sizes and speeds than is possible with pressure ejection. Previous efforts to apply electric spraying to printing or similar selective coating tasks have taken an experimental approach based on steady or periodic spraying phenomena, without attempting cycle -by-cycle drop control. The centerpiece of this thesis is a simulation tool developed to explore such possibilities. A simplified analytic model is developed as a preliminary step, yielding formulas for force and time scales that provide an appropriate basis for nondimensionalization of the governing differential equations; important dimensionless parameters are identified. The complete self-consistent model permits simulation of meniscus behavior under time -varying applied voltage or pressure, with the electric field solution continually updated as the surface changes shape. The model uses a quasi-one-dimensional hydrodynamic formulation and a two-dimensional axisymmetric boundary element solution for the electric field. The simulation is checked against experimental results for meniscus stability, resonant modes, and drop emission under electric field. The simulation faithfully captures important qualitative aspects of meniscus behavior and gives reasonable quantitative agreement within the limitations of the model. Insights gained in simulation point the way to a successful laboratory demonstration of drop extraction using a shaped voltage pulse. Drop size control is pursued in simulation using pressure and voltage pulses both alone and in combination, for both light and viscous liquids. Combining pressure and field pulses is shown to be synergistic; drop volumes over a range of 175 to 1 were obtained, while maintaining good drop velocity. The differing strategies for obtaining large and small drops are described. Drop extraction using only the electric field is more difficult, but promising approaches remain open.

Pressurized liquid extraction combined with capillary electrophoresis-mass spectrometry as an improved methodology for the determination of sulfonamide residues in meat.

PubMed

Font, Guillermina; Juan-García, Ana; Picó, Yolanda

2007-08-03

A new analytical method, based on capillary electrophoresis and tandem mass spectrometry (CE-MS2), is proposed and validated for the identification and simultaneous quantification of 12 sulfonamides (SAs) in pork meat. The studied SAs include sulfathiazole, sulfadiazine, sulfamethoxypyridazine, sulfaguanidine, sulfanilamide, sulfadimethoxyne, sulfapyridine, sulfachloropyridazine, sulfisoxazole, sulfasalazine, sulfabenzamide and sulfadimidine. Different parameters (i.e. separation buffer, sheath liquid, electrospray conditions) were optimized to obtain an adequate CE separation and high MS sensitivity. MS2 experiments using an ion trap as analyzer, operating in the selected reaction monitoring (SRM) mode, were carried out to achieve the required number of identification points according to the 2002/657/EC European Decision. For the quantification in pork tissue samples, a pressurized liquid extraction (PLE) procedure, using hot water as extractant followed by an Oasis HLB cleanup, was developed. Linearity (r between 0.996 and 0.997), precision (RSD<14 %) and recoveries (from 76 to 98%) were satisfactory. The limits of detection and quantification (below 12.5 and 46.5 microg kg(-1), respectively) were in all cases lower than the maximum residue limits (MRLs), indicating the potential of CE-MS2 for the analysis of SAs, in the food quality and safety control areas.

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

PubMed

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

2011-10-01

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

High pressure liquid chromatographic determination of aflatoxins in spices.

PubMed

Awe, M J; Schranz, J L

1981-11-01

High pressure liquid chromatography with fluorescence detection is used to determine aflatoxin in 5 common spices. A 10 micrometer microparticulate silica gel column is used with a dichloromethane-cyclohexane-acetonitrile solvent system to resolve aflatoxins B1, G1, B2, and G2. The fluorescence detector contained a silica gel-packed flowcell. Samples of black, white, and red pepper, ginger, and nutmeg were extracted according to a previously published method. Recoveries from aflatoxin-free samples of white pepper, ginger, and red pepper spiked with 1-50 micrograms aflatoxin/kg ranged from 64 to 92%.

Liquid chromatography coupled to different atmospheric pressure ionization sources-quadrupole-time-of-flight mass spectrometry and post-column addition of metal salt solutions as a powerful tool for the metabolic profiling of Fusarium oxysporum.

PubMed

Cirigliano, Adriana M; Rodriguez, M Alejandra; Gagliano, M Laura; Bertinetti, Brenda V; Godeas, Alicia M; Cabrera, Gabriela M

2016-03-25

Fusarium oxysporum L11 is a non-pathogenic soil-borne fungal strain that yielded an extract that showed antifungal activity against phytopathogens. In this study, reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to different atmospheric pressure ionization sources-quadrupole-time-of-flight mass spectrometry (API-QTOF-MS) was applied for the comprehensive profiling of the metabolites from the extract. The employed sources were electrospray (ESI), atmospheric pressure chemical ionization (APCI) and atmospheric pressure photoionization (APPI). Post-column addition of metal solutions of Ca, Cu and Zn(II) was also tested using ESI. A total of 137 compounds were identified or tentatively identified by matching their accurate mass signals, suggested molecular formulae and MS/MS analysis with previously reported data. Some compounds were isolated and identified by NMR. The extract was rich in cyclic peptides like cyclosporins, diketopiperazines and sansalvamides, most of which were new, and are reported here for the first time. The use of post-column addition of metals resulted in a useful strategy for the discrimination of compound classes since specific adducts were observed for the different compound families. This technique also allowed the screening for compounds with metal binding properties. Thus, the applied methodology is a useful choice for the metabolic profiling of extracts and also for the selection of metabolites with potential biological activities related to interactions with metal ions. Copyright © 2015 Elsevier B.V. All rights reserved.

Analytical strategies for organic food packaging contaminants.

PubMed

Sanchis, Yovana; Yusà, Vicent; Coscollà, Clara

2017-03-24

In this review, we present current approaches in the analysis of food-packaging contaminants. Gas and liquid chromatography coupled to mass spectrometry detection have been widely used in the analysis of some relevant families of these compounds such as primary aromatic amines, bisphenol A, bisphenol A diglycidyl ether and related compounds, UV-ink photoinitiators, perfluorinated compounds, phthalates and non-intentionally added substances. Main applications for sample treatment and different types of food-contact material migration studies have been also discussed. Pressurized Liquid Extraction, Solid-Phase Microextraction, Focused Ultrasound Solid-Liquid Extraction and Quechers have been mainly used in the extraction of food contact material (FCM) contaminants, due to the trend of minimising solvent consumption, automatization of sample preparation and integration of extraction and clean-up steps. Recent advances in analytical methodologies have allowed unequivocal identification and confirmation of these contaminants using Liquid Chromatography coupled to High Resolution Mass Spectrometry (LC-HRMS) through mass accuracy and isotopic pattern applying. LC-HRMS has been used in the target analysis of primary aromatic amines in different plastic materials, but few studies have been carried out applying this technique in post-target and non-target analysis of FCM contaminants. Copyright © 2017 Elsevier B.V. All rights reserved.

Trace analysis of selected hormones and sterols in river sediments by liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.

PubMed

Matić, Ivana; Grujić, Svetlana; Jauković, Zorica; Laušević, Mila

2014-10-17

In this paper, development and optimization of new LC-MS method for determination of twenty selected hormones, human/animal and plant sterols in river sediments were described. Sediment samples were prepared using ultrasonic extraction and clean up with silica gel/anhydrous sodium sulphate cartridge. Extracts were analyzed by liquid chromatography-linear ion trap-tandem mass spectrometry, with atmospheric pressure chemical ionization. The optimized extraction parameters were extraction solvent (methanol), weight of the sediment (2 g) and time of ultrasonic extraction (3× 10 min). Successful chromatographic separation of hormones (estriol and estrone, 17α- and 17β-estradiol) and four human/animal sterols (epicoprostanol, coprostanol, α-cholestanol and β-cholestanol) that have identical fragmentation reactions was achieved. The developed and optimized method provided high recoveries (73-118%), low limits of detection (0.8-18 ng g(-1)) and quantification (2.5-60 ng g(-1)) with the RSDs generally lower than 20%. Applicability of the developed method was confirmed by analysis of six river sediment samples. A widespread occurrence of human/animal and plant sterols was found. The only detected hormone was mestranol in just one sediment sample. Copyright © 2014 Elsevier B.V. All rights reserved.

Solvent extraction of gold using ionic liquid based process

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Analysis of endocrine disruptor compounds in marine sediments by in cell clean up-pressurized liquid extraction-liquid chromatography tandem mass spectrometry determination.

PubMed

Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

2014-12-10

A less time-, solvent- and sorbent-consuming analytical methodology for the determination of bisphenol A and alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) in marine sediment was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The SPLE extraction conditions were optimized by a Plackett-Burman design followed by a central composite design. Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 94 and 100% and repeatability and intermediate precision were <6% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.17 (4-n-nonylphenol) and 4.01 ng g(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of this green methodology. As an application, marine sediment samples from Galicia coast (NW of Spain) were analysed. Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 20.1 and 1409 ng g(-1) dry weight, respectively. Sediment toxicity was estimated and no risk to aquatic biota was found. Copyright © 2014 Elsevier B.V. All rights reserved.

Analysis of aldehydes in beer by gas-diffusion microextraction: characterization by high-performance liquid chromatography-diode-array detection-atmospheric pressure chemical ionization-mass spectrometry.

PubMed

Gonçalves, Luís Moreira; Magalhães, Paulo Jorge; Valente, Inês Maria; Pacheco, João Grosso; Dostálek, Pavel; Sýkora, David; Rodrigues, José António; Barros, Aquiles Araújo

2010-06-11

In this work, a recently developed extraction technique for sample preparation aiming the analysis of volatile and semi-volatile compounds named gas-diffusion microextraction (GDME) is applied in the chromatographic analysis of aldehydes in beer. Aldehydes-namely acetaldehyde (AA), methylpropanal (MA) and furfural (FA)-were simultaneously extracted and derivatized with 2,4-dinitrophenylhydrazine (DNPH), then the derivatives were separated and analyzed by high-performance liquid chromatography with spectrophotometric detection (HPLC-UV). The identity of the eluted compounds was confirmed by high-performance liquid chromatography-atmospheric pressure chemical ionization-mass-spectrometry detection in the negative ion mode (HPLC-APCI-MS). The developed methodology showed good repeatability (ca. 5%) and linearity as well as good limits of detection (AA-12.3, FA-1.5 and MA 5.4microgL(-1)) and quantification (AA-41, FA-4.9 and MA 18microgL(-1)); it also appears to be competitive in terms of speed and cost of analysis. Copyright 2010 Elsevier B.V. All rights reserved.

High pressure liquid chromatography of zearalenone and zearalenols in rat urine and liver.

PubMed

James, L J; McGirr, L G; Smith, T K

1982-01-01

A high pressure liquid chromatographic technique with internal standardization has been developed for determining zearalenone and metabolites in rat urine and liver. Following extraction with methylene chloride and solvent partition, samples are cleaned up by applying the extract to a Sephadex LH-20 column and eluting with a mixture of benzene-methanol (85 + 15). Compounds were resolved on 2 Part-isil-10 columns (25 cm x 4.6 mm id) in series with a mobile phase of isooctane-chloroform-methanol (35 + 25 + 3), and detected at 280 nm. The internal standard was 6'alpha-acetoxyzearalane. Limits of detection were about 2.0 ng for zearalenone and 5.0 ng for zearalenols (6'-hydroxyzearalane). Zearalenone and zearalenols were excreted mainly in free form with relatively little glucuronide conjugation. Metabolism of zearalenone to free zearalenol was minor compared with formation of bound forms.

In vitro vasorelaxation mechanisms of bioactive compounds extracted from Hibiscus sabdariffa on rat thoracic aorta

PubMed Central

Sarr, Mamadou; Ngom, Saliou; Kane, Modou O; Wele, Alassane; Diop, Doudou; Sarr, Bocar; Gueye, Lamine; Andriantsitohaina, Ramaroson; Diallo, Aminata S

2009-01-01

Background In this study, we suggested characterizing the vasodilator effects and the phytochemical characteristics of a plant with food usage also used in traditional treatment of arterial high blood pressure in Senegal. Methods Vascular effects of crude extract of dried and powdered calyces of Hibiscus sabdariffa were evaluated on isolated thoracic aorta of male Wistar rats on organ chambers. The crude extract was also enriched by liquid-liquid extraction. The various cyclohexane, dichloromethane, ethyl acetate, butanol extracts obtained as well as the residual marc were subjected to Sephadex LH-20 column chromatography. The different methanolic eluate fractions were then analyzed by Thin Layer (TLC) and High Performance Liquid Chromatography (HPLC) and their vascular effects also evaluated. Results The H. Sabdariffa crude extract induced mainly endothelium-dependent relaxant effects. The endothelium-dependent relaxations result from NOS activation and those who not dependent to endothelium from activation of smooth muscle potassium channels. The phytochemical analysis revealed the presence of phenolic acids in the ethyl acetate extract and anthocyans in the butanolic extract. The biological efficiency of the various studied extracts, in term of vasorelaxant capacity, showed that: Butanol extract > Crude extract > Residual marc > Ethyl acetate extract. These results suggest that the strong activity of the butanolic extract is essentially due to the presence of anthocyans found in its fractions 43-67. Conclusion These results demonstrate the vasodilator potential of hibiscus sabdariffa and contribute to his valuation as therapeutic alternative. PMID:19883513

Development of a pressurized liquid extraction-solid-phase extraction followed by liquid chromatography-electrospray ionization tandem mass spectrometry method for the quantitative determination of benzoxazolinones and their degradation products in agricultural soil.

PubMed

Villagrasa, M; Guillamón, M; Navarro, A; Eljarrat, E; Barceló, D

2008-02-01

A new analytical method for the quantitative determination of benzoxazolinones and their degradation products in agricultural soils based on the use of pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) and then instrumental determination using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS) is described. Using this method, the characterization, separation and quantitative detection of a mixture of two benzoxazolinones, benzoxazolin-2-one (BOA) and 6-methoxybenzoxazolin-2-one (MBOA) and their degradation products, 2-aminophenol (APH), N-(2-hydroxyphenyl)malonamic acid (HMPMA), 2-amino-3-H-phenoxazin-3-one (APO), 9-methoxy-2-amino-3-H-phenoxazin-3-one (AMPO), 2-acetylamino-3-H-phenoxazin-3-one (AAPO) and 2-acetylamino-9-methoxy-2-amino-3-H-phenoxazin-3-one (AAMPO) was achieved. The complete LC-ESI-MS-MS precursor-product ion fragmentation pathways for the degradation products of benzoxazolinones are described for the first time. Quantitative analysis was done in the multiple reaction mode using two specific combinations of precursor-product ion transitions for each compound. The optimized method was quality assessed by the measure of parameter as recovery, linearity, sensitivity, repeatability and reproducibility. Recoveries of the analytes ranged from 53 to 123%. The developed method offered improvements to the sensitivity as compared with our previously LC-MS method, with detection limits down to 2.4-21 ng/g of dry weight. This achievement allows us to identify and quantify for the first time degradation products of benzoxazolinones in real agricultural soil samples. Analytes were found in the range of 20.6-149 ng/g dry weight.

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

PubMed

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

2017-02-20

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

Determination of acrylamide in coffee and chocolate by pressurised fluid extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Pardo, O; Yusà, V; Coscollà, C; León, N; Pastor, A

2007-07-01

A selective and sensitive procedure has been developed and validated for the determination of acrylamide in difficult matrices, such as coffee and chocolate. The proposed method includes pressurised fluid extraction (PFE) with acetonitrile, florisil clean-up purification inside the PFE extraction cell and detection by liquid chromatography (LC) coupled to atmospheric pressure ionisation in positive mode tandem mass spectrometry (APCI-MS-MS). Comparison of ionisation sources (atmospheric pressure chemical ionisation (APCI), atmospheric pressure photoionization (APPI) and the combined APCI/APPI) and clean-up procedures were carried out to improve the analytical signal. The main parameters affecting the performance of the different ionisation sources were previously optimised using statistical design of experiments (DOE). PFE parameters were also optimised by DOE. For quantitation, an isotope dilution approach was used. The limit of quantification (LOQ) of the method was 1 microg kg(-1) for coffee and 0.6 microg kg(-1) for chocolate. Recoveries ranged between 81-105% in coffee and 87-102% in chocolate. The accuracy was evaluated using a coffee reference test material FAPAS T3008. Using the optimised method, 20 coffee and 15 chocolate samples collected from Valencian (Spain) supermarkets, were investigated for acrylamide, yielding median levels of 146 microg kg(-1) in coffee and 102 microg kg(-1) in chocolate.

Ultra performance liquid chromatography atmospheric pressure photoionization high resolution mass spectrometric method for determination of multiclass pesticide residues in grape and mango juices.

PubMed

Deme, Pragney; Upadhyayula, Vijayasarathi V R

2015-04-15

A novel analytical method was developed for determination of organochlorine, synthetic pyrethroid, organophosphate and carbamate pesticide residues in fruit juices using ultra performance liquid chromatography-atmospheric pressure photoionization-high resolution mass spectrometry (UPLC-APPI-HRMS). The analytes were extracted from fruit juices by dispersive solid-phase extraction using multi-walled carbon nanotubes (MWCNTs). The analysis was carried out in full scan mode using dual ionization mode of APPI in the mass range of 100-650 units. The limit of detection and limit of quantification values for the pesticides were in the range of 0.025-0.15 ng mL(-1) and 0.1-0.5 ng mL(-1) respectively. The matrix effect of the method was found to be low and extraction recoveries were in the range of 60-110%. Some of the real fruits juice samples showed the presence of some pesticides in the range of 6.5-24.8 ng L(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

Ultrapressure liquid chromatography-tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for quantification of 4-methoxydiphenylmethane in pharmacokinetic evaluation.

PubMed

Farhan, Nashid; Fitzpatrick, Sean; Shim, Yun M; Paige, Mikell; Chow, Diana Shu-Lian

2016-09-05

4-Methoxydiphenylmethane (4-MDM), a selective augmenter of Leukotriene A4 Hydrolase (LTA4H), is a new anti-inflammatory compound for potential treatment of chronic obstructive pulmonary disease (COPD). Currently, there is no liquid chromatography tandem mass spectrometric (LC-MS/MS) method for the quantification of 4-MDM. A major barrier for developing the LC-MS/MS method is the inability of electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) to ionize 4-MDM due to its hydrophobicity and lack of any functional group for ionization. With the advent of atmospheric pressure photoionization (APPI) technique, many hydrophobic compounds have been demonstrated to ionize by charge transfer reactions. In this study, a highly sensitive ultrapressure liquid chromatography tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for the quantifications of 4-MDM in rat plasma has been developed and validated. 4-MDM was extracted from the plasma by solid phase extraction (SPE) and separated chromatographically using a reverse phase C8 column. The photoionization (PI) was achieved by introducing anisole as a dopant to promote the reaction of charge transfer. The assay with a linear range of 5 (LLOQ)-400ngmL(-1) met the regulatory requirements for accuracy, precision and stability. The validated assay was employed to quantify the plasma concentrations of 4-MDM after an oral dosing in Sprague Dawley (SD) rats. Copyright © 2016 Elsevier B.V. All rights reserved.

Carbon dioxide extraction of residual chloroform from biodegradable polymers.

PubMed

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

2002-01-01

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

The Application of a Novel Pressurized Liquid Extraction Method to Quantify Organic Tracers Combined with Historic and Novel Organic Contaminants for the Discover-AQ Houston Field Experiment

NASA Astrophysics Data System (ADS)

Clark, A. E.; Yoon, S.; Sheesley, R. J.; Usenko, S.

2014-12-01

DISCOVER-AQ is a NASA mission seeking to better understand air quality in cities across the United States. In September 2013, flight, satellite and ground-based data was collected in Houston, TX and the surrounding metropolitan area. Over 300 particulate matter filter samples were collected as part of the ground-based sampling efforts, at four sites across Houston. Samples include total suspended particle matter (TSP) and fine particulate matter (less than 2.5 μm in aerodynamic diameter; PM2.5). For this project, an analytical method has been developed for the pressurized liquid extraction (PLE) of a wide variety of organic tracers and contaminants from quartz fiber filters (QFFs). Over 100 compounds were selected including polycyclic aromatic hydrocarbons (PAHs), hopanes, levoglucosan, organochlorine pesticides, polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), and organophosphate flame retardants (OPFRs). Currently, there is no analytical method validated for the reproducible extraction of all seven compound classes in a single automated technique. Prior to extraction, QFF samples were spiked with known amounts of target analyte standards and isotopically-labeled surrogate standards. The QFF were then extracted with methylene chloride:acetone at high temperatures (100˚C) and pressures (1500 psi) using a Thermo Dionex Accelerated Solvent Extractor system (ASE 350). Extracts were concentrated, spiked with known amounts of isotopically-labeled internal standards, and analyzed by gas chromatography coupled with mass spectrometry utilizing electron ionization and electron capture negative ionization. Target analytes were surrogate recovery-corrected to account for analyte loss during sample preparation. Ambient concentrations of over 100 organic tracers and contaminants will be presented for four sites in Houston during DISCOVER-AQ.

Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for industrial and anthropogenic waste-indicator compounds in sediment

USGS Publications Warehouse

Burkhardt, M.R.; ReVello, R.C.; Smith, S.G.; Zaugg, S.D.

2005-01-01

A broad range of organic compounds is recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This method was developed to better determine the distribution of 61 compounds that are typically associated with industrial and household waste as well as some that are toxic and known (or suspected) for endocrine-disrupting potential extracted from environmental sediment samples. Pressurized liquid extraction (PLE) coupled with solid-phase extraction (SPE) was used to reduce sample preparation time, reduce solvent consumption to one-fifth of that required using dichloromethane-based Soxhlet extraction, and to minimize background interferences for full scan GC/MS analysis. Recoveries from spiked Ottawa sand, commercially available topsoil, and environmental stream sediment, fortified at 4-720 ??g per compound, averaged 76 ?? 13%. Initial method detection limits for single-component compounds ranged from 12.5 to 520 ??g/kg, based on 25 g samples. Results from 103 environmental sediment samples show that 36 out of 61 compounds (59%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, beta-sitosterol, a plant sterol, was detected in 87 of the 103 (84.5%) environmental samples with a concentration range 360-100,000 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction are also compared. ?? 2004 Published by Elsevier B.V.

Characterization via liquid chromatography coupled to diode array detector and tandem mass spectrometry of supercritical fluid antioxidant extracts of Spirulina platensis microalga.

PubMed

Mendiola, Jose A; Marín, Francisco R; Hernández, S Francisco; Arredondo, Bertha O; Señoráns, F Javier; Ibañez, Elena; Reglero, Guillermo

2005-06-01

Spirulina platensis microalga has been extracted on a pilot scale plant using supercritical fluid extraction (SFE) under various extraction conditions. The extraction yield and the antioxidant activity of the extracts were evaluated in order to select those extracts with both the highest antioxidant capacity and a good extraction yield. These extracts were characterized using LC coupled to diode array detection (DAD) and LC coupled to mass spectrometry (MS) with two different interfaces, atmospheric pressure chemical ionization (APCI) and electrospray (ESI) which allowed us to perform tandem MS by using an ion trap analyzer. The best extraction conditions were as follows: CO2 with 10% of modifier (ethanol) as extraction solvent, 55 degrees C (extraction temperature) and 220 bar (extraction pressure). Fractionation was achieved by cascade depressurization providing two extracts with different activity and chemical composition. Several compounds have been identified in the extracts, corresponding to different carotenoids previously identified in Spirulina platensis microalga along with chlorophyll a and some degradation products. Also, the structure of some phenolic compounds could be tentatively identified. The antioxidant activity of the extracts could be attributed to some of the above mentioned compounds.

Apparatus and method for phosphate-accelerated bioremediation

DOEpatents

Looney, B.B.; Pfiffner, S.M.; Phelps, T.J.; Lombard, K.H.; Hazen, T.C.; Borthen, J.W.

1998-05-19

An apparatus and method are provided for supplying a vapor-phase nutrient to contaminated soil for in situ bioremediation. The apparatus includes a housing adapted for containing a quantity of the liquid nutrient, a conduit in communication with the interior of the housing, means for causing a gas to flow through the conduit, and means for contacting the gas with the liquid so that a portion evaporates and mixes with the gas. The mixture of gas and nutrient vapor is delivered to the contaminated site via a system of injection and extraction wells configured to the site and provides for the use of a passive delivery system. The mixture has a partial pressure of vaporized nutrient that is no greater than the vapor pressure of the liquid. If desired, the nutrient and/or the gas may be heated to increase the vapor pressure and the nutrient concentration of the mixture. Preferably, the nutrient is a volatile, substantially nontoxic and nonflammable organic phosphate that is a liquid at environmental temperatures, such as triethyl phosphate or tributyl phosphate. 8 figs.

Current trends in sample preparation for cosmetic analysis.

PubMed

Zhong, Zhixiong; Li, Gongke

2017-01-01

The widespread applications of cosmetics in modern life make their analysis particularly important from a safety point of view. There is a wide variety of restricted ingredients and prohibited substances that primarily influence the safety of cosmetics. Sample preparation for cosmetic analysis is a crucial step as the complex matrices may seriously interfere with the determination of target analytes. In this review, some new developments (2010-2016) in sample preparation techniques for cosmetic analysis, including liquid-phase microextraction, solid-phase microextraction, matrix solid-phase dispersion, pressurized liquid extraction, cloud point extraction, ultrasound-assisted extraction, and microwave digestion, are presented. Furthermore, the research and progress in sample preparation techniques and their applications in the separation and purification of allowed ingredients and prohibited substances are reviewed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PUSH-PULL POWER REACTOR

DOEpatents

Froman, D.K.

1959-02-24

Power generating nuclear reactors of the homogeneous liquid fuel type are discussed. The apparatus utilizes two identical reactors interconnected by conduits through heat exchanging apparatus. Each reactor contains a critical geometry region and a vapor region separated from the critical region by a baffle. When the liquid in the first critical region becomes critical, the vapor pressure above the fuel is increased due to the rise in the temperature until it forces the liquid fuel out of the first critical region through the heat exchanger and into the second critical region, which is at a lower temperature and consequently a lower vapor pressure. The above reaction is repeated in the second critical region and the liquid fuel is forced back into the first critical region. In this manner criticality is achieved alternately in each critical region and power is extracted by the heat exchanger from the liquid fuel passing therethrough. The vapor region and the heat exchanger have a non-critical geometry and reactivity control is effected by conventional control rods in the critical regions.

Soft Listeria: actin-based propulsion of liquid drops.

PubMed

Boukellal, Hakim; Campás, Otger; Joanny, Jean-François; Prost, Jacques; Sykes, Cécile

2004-06-01

We study the motion of oil drops propelled by actin polymerization in cell extracts. Drops deform and acquire a pearlike shape under the action of the elastic stresses exerted by the actin comet, a tail of cross-linked actin filaments. We solve this free boundary problem and calculate the drop shape taking into account the elasticity of the actin gel and the variation of the polymerization velocity with normal stress. The pressure balance on the liquid drop imposes a zero propulsive force if gradients in surface tension or internal pressure are not taken into account. Quantitative parameters of actin polymerization are obtained by fitting theory to experiment.

Integrated photooxidative extractive deep desulfurization using metal doped TiO2 and eutectic based ionic liquid

NASA Astrophysics Data System (ADS)

Zaid, Hayyiratul Fatimah Mohd; Kait, Chong Fai; Mutalib, Mohamed Ibrahim Abdul

2016-11-01

A series of metal doped TiO2 namely Fe/TiO2, Cu/TiO2 and Cu-Fe/TiO2 were synthesized and characterized, to be used as a photocatalyst in the integrated photooxidative extractive deep desulfurization for model oil (dodecane) and diesel fuel. The order of the photocatalytic activity was Cu-Fe/TiO2 followed by Cu/TiO2 and then Fe/TiO2. Cu-Fe/TiO2 was an effective photocatalyst for sulfur conversion at ambient atmospheric pressure. Hydrogen peroxide was used as the source of oxidant and eutectic-based ionic liquid as the extractant. Sulfur conversion in model oil reached 100%. Removal of sulfur from model oil was done by two times extraction with a removal of 97.06% in the first run and 2.94% in the second run.

PLE in the analysis of plant compounds. Part I. The application of PLE for HPLC analysis of caffeine in green tea leaves.

PubMed

Dawidowicz, Andrzej L; Wianowska, Dorota

2005-04-29

A broad spectrum of sample preparation methods is currently used for the isolation of pharmacologically active compounds from plant and herbal materials. The paper compares the effectiveness of infusion, microwave assisted solvent extraction (MASE), matrix solid-phase dispersion (MSPD) and pressurised liquid extraction (PLE) as sample preparation methods for the isolation of caffeine from green tea leaves. The effect of PLE variables, such as extraction temperature, pressure and time, on the yield of caffeine from the investigated matrix is discussed. The obtained results revealed that PLE, in comparison with other sample preparation methods applied, has significantly lower efficacy for caffeine isolation from green tea leaves. The evaluation of PLE conditions leads to the conclusion that elevated pressure applied in the PLE process is the factor hindering the extraction.

Ionic liquids screening for desulfurization of natural gasoline by liquid-liquid extraction.

PubMed

Likhanova, Natalya V; Guzmán-Lucero, Diego; Flores, Eugenio A; García, Paloma; Domínguez-Aguilar, Marco A; Palomeque, Jorge; Martínez-Palou, Rafael

2010-11-01

Seventy five ionic liquids (ILs) were tested as a sequestering agent of sulfured compounds in natural gasoline (NG). Desulphurization of NG was performed by means of liquid-liquid extraction method at room temperature and atmospheric pressure. Experimental ILs containing imidazolium, pyridinium, and ammonium cations along with organic and inorganic anions were synthesized conventionally and under microwave and sonochemical conditions. The effect of the molecular structure of ILs on the desulfurization efficiency of NG with high sulfur content was evaluated. Analysis indicated that the anion type played a more important role than the cation on the desulphurization process. ILs based on halogen-ferrates and halogen-aluminates exhibited the highest efficiency in sulfur removal, and their efficiency is further improved when there is an excess of metallic salt in a ratio of at least 1:1.3 during the synthesis of the corresponding IL. An explanation for the ability of metallic ILs to remove sulfur-containing compounds from natural gasoline based on the ratio of the ionic charge to the atomic radius is proposed. Furthermore, a method to recover and reuse water-sensitive to halogenated precursors is described.

Development and Application of Immunoaffinity Chromatography for Coplanar PCBs in Soil and Sediment

EPA Science Inventory

An immunoaffinity chromatography (IAC) column was developed as a simple cleanup procedure for preparing environmental samples for analysis of polychlorinated biphenyls (PCBs). Soil and sediment samples were prepared using pressurized liquid extraction (PLE), followed by the IAC c...

REFINING FLUORINATED COMPOUNDS

DOEpatents

Linch, A.L.

1963-01-01

This invention relates to the method of refining a liquid perfluorinated hydrocarbon oil containing fluorocarbons from 12 to 28 carbon atoms per molecule by distilling between 150 deg C and 300 deg C at 10 mm Hg absolute pressure. The perfluorinated oil is washed with a chlorinated lower aliphatic hydrocarbon, which mairtains a separate liquid phase when mixed with the oil. Impurities detrimental to the stability of the oil are extracted by the chlorinated lower aliphatic hydrocarbon. (AEC)

Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry.

PubMed

Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Pagano, Imma; Russo, Mariateresa; Rastrelli, Luca

2016-01-08

This study reports a fast and automated analytical procedure for the analysis of aflatoxin M1 (AFM1) in milk and dairy products. The method is based on the simultaneous protein precipitation and AFM1 extraction, by salt-induced liquid-liquid extraction (SI-LLE), followed by an online solid-phase extraction (online SPE) coupled to ultra-high-pressure-liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis to the automatic pre-concentration, clean up and sensitive and selective determination of AFM1. The main parameters affecting the extraction efficiency and accuracy of the analytical method were studied in detail. In the optimal conditions, acetonitrile and NaCl were used as extraction/denaturant solvent and salting-out agent in SI-LLE, respectively. After centrifugation, the organic phase (acetonitrile) was diluted with water (1:9 v/v) and purified (1mL) by online C18 cartridge coupled with an UHPLC column. Finally, selected reaction monitoring (SRM) acquisition mode was applied to the detection of AFM1. Validation studies were carried out on different dairy products (whole and skimmed cow milk, yogurt, goat milk, and powder infant formula), providing method quantification limits about 25 times lower than AFM1 maximum levels permitted by EU regulation 1881/2006 in milk and dairy products for direct human consumption. Recoveries (86-102%) and repeatability (RSD<3, n=6) meet the performance criteria required by EU regulation N. 401/2006 for the determination of the levels of mycotoxins in foodstuffs. Moreover, no matrix effects were observed in the different milk and dairy products studied. The proposed method improves the performance of AFM1 analysis in milk samples as AFM1 determination is performed with a degree of accuracy higher than the conventional methods. Other advantages are the reduction of sample preparation procedure, time and cost of the analysis, enabling high sample throughput that meet the current concerns of food safety and the public health protection. Copyright © 2015 Elsevier B.V. All rights reserved.

[Preparation of flavonoid reference standards from Scutellariae Radix under the guidance of high performance liquid chromatography-mass spectrometry analysis].

PubMed

Guo, Henan; Yang, Xuedong; Liu, Jun; Zheng, Wenfeng

2012-07-01

Flavonoid reference standards were targeted-prepared from Scutellariae Radix under the guidance of high performance liquid chromatography-mass spectrometry (HPLC-MS) analysis. With HPLC-MS analysis of Scutellariae Radix, 19 flavonoid components were identified by analyzing and comparing their retention times, ultraviolet spectra, and mass spectrometry data with literature. The separation and purification protocols of all targeted flavonoid reference standards were optimally designed according to the results of HPLC-MS analysis and related literature. The ethanol extract of Scutellariae Radix was suspended in water and extracted with petroleum ether, ethyl acetate, and n-butanol successively. The ethyl acetate extract and n-butanol extract were separately subjected to primary separation by low pressure reverse phase preparative chromatography. Then the fractions containing targeted compounds were further purified by low pressure reverse and normal phases preparative chromatography. Finally, baicalin and wogonoside reference standards were obtained from n-butanol extract; baicaelin, wogonin, and oroxylin A reference standards were obtained from ethyl acetate extract. The structures of the 5 reference standards were identified by mass spectrometry (MS) and 1H nuclear magnetic resonance (1H NMR) spectroscopy. The HPLC analytical results showed that the purities of the 5 reference standards were all above 98%. It is demonstrated that the rapid targeted-preparation method under the guidance of the HPLC-MS analysis is applicable for the isolation and preparation of chemical components in traditional Chinese medicines.

Recovery of anhydrous hydrogen iodide

DOEpatents

O'Keefe, Dennis R.; McCorkle, Jr., Kenneth H.; de Graaf, Johannes D.

1982-01-01

Relatively dry hydrogen iodide can be recovered from a mixture of HI, I.sub.2 and H.sub.2 O. After the composition of the mixture is adjusted so that the amounts of H.sub.2 O and I.sub.2 do not exceed certain maximum limits, subjection of the mixture to superatmospheric pressure in an amount equal to about the vapor pressure of HI at the temperature in question causes distinct liquid phases to appear. One of the liquid phases contains HI and not more than about 1 weight percent water. Often the adjustment in the composition will include the step of vaporization, and the distinct layers appear following the increase in pressure of the vapor mixture. Adjustment in the composition may also include the addition of an extraction agent, such as H.sub.3 PO.sub.4, and even though the adjusted composition mixture contains a significant amount of such an agent, the creation of the distinct liquid phases is not adversely affected.

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites.

PubMed

Xie, Li; Chen, Liqin; Gu, Pan; Wei, Lanlan; Kang, Xuejun

2018-03-01

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and related diseases, but their precise measurement is still a challenge. Many protocols have been described for neurotransmitter measurement by a variety of instruments, including high-pressure liquid chromatography (HPLC). However, there are shortcomings, such as complicated operation or hard-to-detect multiple targets, which cannot be avoided, and presently, the dominant analysis technique is still HPLC coupled with sensitive electrochemical or fluorimetric detection, due to its high sensitivity and good selectivity. Here, a detailed protocol is described for the pretreatment and detection of catecholamines with high pressure liquid chromatography with electrochemical detection (HPLC-ECD) in real urine samples of infants, using electrospun composite nanofibers composed of polymeric crown ether with polystyrene as adsorbent, also known as the packed-fiber solid phase extraction (PFSPE) method. We show how urine samples can be easily precleaned by a nanofiber-packed solid phase column, and how the analytes in the sample can be rapidly enriched, desorbed, and detected on an ECD system. PFSPE greatly simplifies the pretreatment procedures for biological samples, allowing for decreased time, expense, and reduction of the loss of targets. Overall, this work illustrates a simple and convenient protocol for solid-phase extraction coupled to an HPLC-ECD system for simultaneous determination of three monoamine neurotransmitters (norepinephrine (NE), epinephrine (E), dopamine (DA)) and two of their metabolites (3-methoxy-4-hydroxyphenylglycol (MHPG) and 3,4-dihydroxy-phenylacetic acid (DOPAC)) in infants' urine. The established protocol was applied to assess the differences of urinary catecholamines and their metabolites between high-risk infants with perinatal brain damage and healthy controls. Comparative analysis revealed a significant difference in urinary MHPG between the two groups, indicating that the catecholamine metabolites may be an important candidate marker for early diagnosis of cases at risk for brain damage in infants.

Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis.

PubMed

Celano, Rita; Piccinelli, Anna Lisa; Campone, Luca; Rastrelli, Luca

2014-08-15

Pharmaceutical and personal care products (PPCPs) are one of the most important classes of emerging contaminants. The potential of ecological and environmental impacts associated with PPCPs are of particular concern because they continually penetrate the aquatic environment. This work describes a novel ultra-preconcentration technique for the rapid and highly sensitive analysis of selected PPCPs in environmental water matrices at ppt levels. Selected PPCPs were rapidly extracted and concentrated from large volumes of aqueous solutions (500 and 250mL) by solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and then analyzed using UHPLC-MS/MS. Experimental parameters were carefully investigated and optimized to achieve the best SPE-DLLME efficiency and higher enrichment factors. The best results were obtained using the ternary mixture acetonitrile/methanol/dichloromethane 3:3:4, v/v/v, both as SPE eluent and DLLME extractant/dispersive mixture. DLLME aqueous solution (5% NaCl, 10mgL(-1) TBAB) was also modified to improve the extraction efficiency of more hydrophilic PPCPs. Under the optimal conditions, an exhaustive extraction for most of the investigated analytes (recoveries >70%), with a precision (RSD <10%) and very high enrichment factors were attained for different aqueous matrices (drinking, sea, river and wastewater). Method detection and quantification limits were at very low ppt levels and below 1 and 3ngL(-1), respectively, for 15 of selected PPCPs. The proposed analytical procedure offers numerous advantages such as the simplicity of operation, rapidity, a high enrichment factor and sensitivity. So it is suitable for monitoring and studies of occurrence of PPCPs in different environmental compartments. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of polychlorinated biphenyls and polychlorinated dibenzo-p-dioxins and dibenzofurans by pressurized liquid extraction and gas chromatography coupled to mass spectrometry in street dust samples.

PubMed

Klees, Marcel; Hiester, Ernst; Bruckmann, Peter; Schmidt, Torsten C

2013-07-26

Owing to massive pollution with polychlorinated biphenyls in the harbour area of Dortmund (Germany), several dust samples were taken from surfaces at industrial sites and analyzed by the North-Rhine Westphalian State Agency for Nature, Environment, and Consumer Protection (LANUV NRW). This report describes and validates a rapid approach to screening for the presence of polychlorinated biphenyls (PCBs) in street dust. Samples were collected by using a natural bristle brush and stainless steel scoops. Mass recovery of fine-particle sea sand (a dust surrogate) on asphalt and concrete surfaces was used as a criterion for the effectiveness of sampling. Better recoveries of sea sand were achieved on concrete than on asphalt surfaces. Furthermore, temperature optimization for a pressurized liquid extraction (PLE) method used to extract PCBs and polychlorinated dibenzodioxins and polychlorinated furans (PCDD/Fs) from street dust samples was developed and compared with Soxhlet extraction for the analysis of PCBs in real street dust samples. Toluene was used as the extraction solvent in both cases. During this study, a combination of toluene and PLE achieved better extraction efficiencies than Soxhlet extraction. Finally, the performance of the PLE method was evaluated by analysing NIST Standard Reference Material 1649a for PCB and PCDD/F concentrations. This demonstrated that the accuracy of the PLE method for the determination of both substance classes was satisfactory. In addition, concentrations of PCBs and PCDD/Fs in street dust samples from industrial sites are reported. Copyright © 2013. Published by Elsevier B.V.

Multidetection of antibiotics in liver tissue by ultra-high-pressure-liquid-chromatography-tandem mass spectrometry.

PubMed

Freitas, Andreia; Barbosa, Jorge; Ramos, Fernando

2015-01-22

A multiresidue quantitative screening method covering 39 antibiotics from 7 different families by ultra-high-pressure-liquid-chromatography-tandem mass spectrometry (UHPLC-MS/MS) is described. Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol are simultaneously detected in liver tissue. A simple sample treatment method consisting of extraction with a mixture of acetonitrile and ethylenediaminetetraacetic acid (EDTA) followed by solid-phase extraction (SPE) with a hydrophilic-lipophilic balanced (HLB) cartridge was developed. The methodology was validated, in accordance with Decision 2002/657/EC, by evaluating the following required parameters: decision limit (CCα), detection capability (CCβ), specificity, repeatability and reproducibility. The precision, in terms of the relative standard deviation, was under 22% for all of the compounds, and the recoveries were between 80% and 110%. The CCα and CCβ were determined according to the maximum residue limit (MRL) or the minimum required performance limit (MRPL), when established. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of bisphenol AF (BPAF) in tissues, serum, urine and feces of orally dosed rats by ultra-high-pressure liquid chromatography-electrospray tandem mass spectrometry.

PubMed

Yang, Yunjia; Yin, Jie; Yang, Yi; Zhou, Naiyuan; Zhang, Jing; Shao, Bing; Wu, Yongning

2012-07-15

As a homologue of bisphenol A (BPA), there is concern about the potential reproductive and developmental toxicity of bisphenol AF (BPAF) based on in vitro tests. In this study, a simple and universal analytical method was developed for the determination of trace BPAF in various tissues and excreta of rats after they were orally dosed. The samples were hydrolyzed with glucuronidase/arylsulfatase followed by ultrasonic extraction with acetonitrile. The crude extract was purified with a mixed-mode anion exchange (Oasis MAX) solid-phase extraction (SPE) cartridge. Separation and quantification was then conducted by ultra-high-pressure liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in negative ionization mode. The recoveries at three fortification levels in different biological samples were from 71.0% to 102.3% with relative standard deviations no more than 13.2% (n=6). The quantification limits of the method were from 0.5 μg/kg to 3 μg/kg depending on the matrix. This method was successfully applied to the determination of BPAF in tissues, serum, urine and feces of orally dosed rats. Copyright © 2012 Elsevier B.V. All rights reserved.

"One-pot" ethyl chloroformate derivatization and liquid-liquid extraction of reduced glutathione in erythrocyte and its quantitative GC-MS analysis.

PubMed

Manca, Alessandra; Alladio, Eugenio; Massarenti, Paola; Puccinelli, M Paola; De Francesco, Antonella; Del Grosso, Erika; Mengozzi, Giulio; Pazzi, Marco; Vincenti, Marco

2017-12-01

A simple "one-pot" derivatization and liquid-liquid extraction (LLE) procedure was developed for GC-MS analysis of reduced glutathione (GSH) analysis in erythrocytes. The metabolite was extracted by 5% (w/v) TCA, the supernatant treated with ECF and ethanol-pyridine media, the derivative separated and detected by gas chromatography-mass spectrometry using a short non-polar capillary GC column at a high column-head pressure. Total analysis time was 11min. The process was optimized by a Design of Experiment. The method was validated showing a good linearity over the 25.4-813.4μM concentration range, providing satisfactory results in terms of intra-day and inter-day precision as well as an optimal accuracy. The new method was evaluated in a pilot study involving patients with severe protein malnutrition. Comparison of this group with a group of healthy subjects revealed significantly lower GSH concentrations in erythrocytes in the former, thus proving that the described GC-MS method could be employed for fast and simple GSH analysis in clinical studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Recovering Bioactive Compounds from Olive Oil Filter Cake by Advanced Extraction Techniques

PubMed Central

Lozano-Sánchez, Jesús; Castro-Puyana, María; Mendiola, Jose A.; Segura-Carretero, Antonio; Cifuentes, Alejandro; Ibáñez, Elena

2014-01-01

The potential of by-products generated during extra-virgin olive oil (EVOO) filtration as a natural source of phenolic compounds (with demonstrated bioactivity) has been evaluated using pressurized liquid extraction (PLE) and considering mixtures of two GRAS (generally recognized as safe) solvents (ethanol and water) at temperatures ranging from 40 to 175 °C. The extracts were characterized by high-performance liquid chromatography (HPLC) coupled to diode array detection (DAD) and electrospray time-of-flight mass spectrometry (HPLC-DAD-ESI-TOF/MS) to determine the phenolic-composition of the filter cake. The best isolation procedure to extract the phenolic fraction from the filter cake was accomplished using ethanol and water (50:50, v/v) at 120 °C. The main phenolic compounds identified in the samples were characterized as phenolic alcohols or derivatives (hydroxytyrosol and its oxidation product), secoiridoids (decarboxymethylated and hydroxylated forms of oleuropein and ligstroside aglycones), flavones (luteolin and apigenin) and elenolic acid derivatives. The PLE extraction process can be applied to produce enriched extracts with applications as bioactive food ingredients, as well as nutraceuticals. PMID:25226536

Measurement of Capillary Radius and Contact Angle within Porous Media.

PubMed

Ravi, Saitej; Dharmarajan, Ramanathan; Moghaddam, Saeed

2015-12-01

The pore radius (i.e., capillary radius) and contact angle determine the capillary pressure generated in a porous medium. The most common method to determine these two parameters is through measurement of the capillary pressure generated by a reference liquid (i.e., a liquid with near-zero contact angle) and a test liquid. The rate of rise technique, commonly used to determine the capillary pressure, results in significant uncertainties. In this study, we utilize a recently developed technique for independently measuring the capillary pressure and permeability to determine the equivalent minimum capillary radii and contact angle of water within micropillar wick structures. In this method, the experimentally measured dryout threshold of a wick structure at different wicking lengths is fit to Darcy's law to extract the maximum capillary pressure generated by the test liquid. The equivalent minimum capillary radii of different wick geometries are determined by measuring the maximum capillary pressures generated using n-hexane as the working fluid. It is found that the equivalent minimum capillary radius is dependent on the diameter of pillars and the spacing between pillars. The equivalent capillary radii of micropillar wicks determined using the new method are found to be up to 7 times greater than the current geometry-based first-order estimates. The contact angle subtended by water at the walls of the micropillars is determined by measuring the capillary pressure generated by water within the arrays and the measured capillary radii for the different geometries. This mean contact angle of water is determined to be 54.7°.

Novel determination of polychlorinated naphthalenes in water by liquid chromatography-mass spectrometry with atmospheric pressure photoionization.

PubMed

Moukas, Athanasios I; Thomaidis, Nikolaos S; Calokerinos, Antony C

2016-01-01

This study presents the development, optimization, and validation of a novel method for the determination of polychlorinated naphthalenes (PCNs) by liquid chromatography-atmospheric pressure photoionization (APPI), using toluene as dopant. The mass spectra of PCN 52, 54, 66, 67, 73, and 75 were recorded in negative ionization. The base ions corresponded to [M-Cl+O](-), where M is the analyte molecule. A strategy, which includes designs of experiments, for the development, the evaluation, and the optimization of the LC-APPI-MS/MS methods is also described. Finally, a highly sensitive method with low instrumental limits of detection (LoDs), ranging from 0.8 pg for PCN 75 to 16 pg for PCN 54 on column, was validated. A Thermo Hypersil Green PAH (100 mm × 2.1 mm, 3 μm) column was used with acetonitrile/water/methanol as mobile phase. The method was applied for the determination of the selected PCNs in surface and tap water samples. A simple liquid-liquid extraction method for the extraction of PCNs from water samples was used. Method LoQs ranged from 29 ng L(-1), for PCN 73, to 63 ng L(-1), for PCN 54, and the recoveries ranged from 97 to 99%, for all congeners. This is the first LC-APPI-MS/MS method for the determination of PCNs in water samples.

Numerical modeling of self-pressurization and pressure control by a thermodynamic vent system in a cryogenic tank

NASA Astrophysics Data System (ADS)

Majumdar, Alok; Valenzuela, Juan; LeClair, Andre; Moder, Jeff

2016-03-01

This paper presents a numerical model of a system-level test bed-the multipurpose hydrogen test bed (MHTB) using the Generalized Fluid System Simulation Program (GFSSP). MHTB is representative in size and shape of a space transportation vehicle liquid hydrogen propellant tank, and ground-based testing was performed at NASA Marshall Space Flight Center (MSFC) to generate data for cryogenic storage. GFSSP is a finite volume-based network flow analysis software developed at MSFC and used for thermofluid analysis of propulsion systems. GFSSP has been used to model the self-pressurization and ullage pressure control by the Thermodynamic Vent System (TVS). A TVS typically includes a Joule-Thompson (J-T) expansion device, a two-phase heat exchanger (HEX), and a mixing pump and liquid injector to extract thermal energy from the tank without significant loss of liquid propellant. For the MHTB tank, the HEX and liquid injector are combined into a vertical spray bar assembly. Two GFSSP models (Self-Pressurization and TVS) were separately developed and tested and then integrated to simulate the entire system. The Self-Pressurization model consists of multiple ullage nodes, a propellant node, and solid nodes; it computes the heat transfer through multilayer insulation blankets and calculates heat and mass transfer between the ullage and liquid propellant and the ullage and tank wall. A TVS model calculates the flow through a J-T valve, HEX, and spray and vent systems. Two models are integrated by exchanging data through User Subroutines of both models. Results of the integrated models have been compared with MHTB test data at a 50% fill level. Satisfactory comparison was observed between tests and numerical predictions.

Simulating Gas-Liquid-Water Partitioning and Fluid Properties of Petroleum under Pressure: Implications for Deep-Sea Blowouts.

PubMed

Gros, Jonas; Reddy, Christopher M; Nelson, Robert K; Socolofsky, Scott A; Arey, J Samuel

2016-07-19

With the expansion of offshore petroleum extraction, validated models are needed to simulate the behaviors of petroleum compounds released in deep (>100 m) waters. We present a thermodynamic model of the densities, viscosities, and gas-liquid-water partitioning of petroleum mixtures with varying pressure, temperature, and composition based on the Peng-Robinson equation-of-state and the modified Henry's law (Krychevsky-Kasarnovsky equation). The model is applied to Macondo reservoir fluid released during the Deepwater Horizon disaster, represented with 279-280 pseudocomponents, including 131-132 individual compounds. We define >n-C8 pseudocomponents based on comprehensive two-dimensional gas chromatography (GC × GC) measurements, which enable the modeling of aqueous partitioning for n-C8 to n-C26 fractions not quantified individually. Thermodynamic model predictions are tested against available laboratory data on petroleum liquid densities, gas/liquid volume fractions, and liquid viscosities. We find that the emitted petroleum mixture was ∼29-44% gas and ∼56-71% liquid, after cooling to local conditions near the broken Macondo riser stub (∼153 atm and 4.3 °C). High pressure conditions dramatically favor the aqueous dissolution of C1-C4 hydrocarbons and also influence the buoyancies of bubbles and droplets. Additionally, the simulated densities of emitted petroleum fluids affect previous estimates of the volumetric flow rate of dead oil from the emission source.

Ambient Mass Spectrometry Imaging Using Direct Liquid Extraction Techniques

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

Laskin, Julia; Lanekoff, Ingela

2015-11-13

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

From catastrophic acceleration to deceleration of liquid plugs in prewetted capillary tubes

NASA Astrophysics Data System (ADS)

Magniez, Juan; Baudoin, Michael; Zoueshtiagh, Farzam; Lemac/Lics Team

2016-11-01

Liquid/gas flows in capillaries are involved in a multitude of systems including flow in porous media, petroleum extraction, imbibition of paper or flows in pulmonary airways in pathological conditions. Liquid plugs, witch compose the biphasic flows, can have a dramatic impact on patients with pulmonary obstructive diseases, since they considerably alter the circulation of air in the airways and thus can lead to severe breathing difficulties. Here, the dynamics of liquid plugs in prewetted capillary tube is investigated experimentally and theoretically, with a particular emphasis on the role of the prewetting films and of the driving condition (constant flow rate, constant pressure). For both driving conditions, the plugs can either experience a continuous increase or decrease of their size. While this phenomenon is regular in the case of imposed flow rate, a constant pressure head can lead to a catastrophic acceleration of the plug and eventually its rupture or a dramatic increase of the plug size. A theoretical model is proposed to explain the transition between theses two regimes. These results give a new insight on the critical pressure required for airways obstruction and reopening. IEMN, International Laboratory LEMAC/LICS, UMR CNRS 8520, University of Lille.

Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products.

PubMed

Qiu, Ying-Kun; Chen, Fang-Fang; Zhang, Ling-Ling; Yan, Xia; Chen, Lin; Fang, Mei-Juan; Wu, Zhen

2014-04-11

An on-line comprehensive two-dimensional preparative liquid chromatography system was developed for preparative separation of minor amount components from complicated natural products. Medium-pressure liquid chromatograph (MPLC) was applied as the first dimension and preparative HPLC as the second one, in conjunction with trapping column and makeup pump. The performance of the trapping column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure from the view of medium pressure liquid chromatograph. Satisfactory trapping efficiency can be achieved using a commercially available 15 mm × 30 mm i.d. ODS pre-column. The instrument operation and the performance of this MPLC×preparative HPLC system were illustrated by gram-scale isolation of crude macro-porous resin enriched water extract of Rheum hotaoense. Automated multi-step preparative separation of 25 compounds, whose structures were identified by MS, (1)H NMR and even by less-sensitive (13)C NMR, could be achieved in a short period of time using this system, exhibiting great advantages in analytical efficiency and sample treatment capacity compared with conventional methods. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2011-10-21

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

Innovative Alternative Technologies to Extract Carotenoids from Microalgae and Seaweeds

PubMed Central

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

2016-01-01

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

Innovative Alternative Technologies to Extract Carotenoids from Microalgae and Seaweeds.

PubMed

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

2016-11-22

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

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.

Fast analysis of doping agents in urine by ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry. II: Confirmatory analysis.

PubMed

Badoud, F; Grata, E; Perrenoud, L; Saugy, M; Rudaz, S; Veuthey, J-L

2010-06-18

For doping control, analyses of samples are generally achieved in two steps: a rapid screening and, in the case of a positive result, a confirmatory analysis. A two-step methodology based on ultra-high-pressure liquid chromatography coupled to a quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) was developed to screen and confirm 103 doping agents from various classes (e.g., beta-blockers, stimulants, diuretics, and narcotics). The screening method was presented in a previous article as part I (i.e., Fast analysis of doping agents in urine by ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry. Part I: screening analysis). For the confirmatory method, basic, neutral and acidic compounds were extracted by a dedicated solid-phase extraction (SPE) in a 96-well plate format and detected by MS in the tandem mode to obtain precursor and characteristic product ions. The mass accuracy and the elemental composition of precursor and product ions were used for compound identification. After validation including matrix effect determination, the method was considered reliable to confirm suspect results without ambiguity according to the positivity criteria established by the World Anti-Doping Agency (WADA). Moreover, an isocratic method was developed to separate ephedrine from its isomer pseudoephedrine and cathine from phenylpropanolamine in a single run, what allowed their direct quantification in urine. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Antioxidant activity and characterization of volatile constituents of Taheebo (Tabebuia impetiginosa Martius ex DC).

PubMed

Park, Byeoung-Soo; Lee, Kwang-Geun; Shibamoto, Takayuki; Lee, Sung-Eun; Takeoka, Gary R

2003-01-01

Volatiles were isolated from the dried inner bark of Tabebuia impetiginosa using steam distillation under reduced pressure followed by continuous liquid-liquid extraction. The extract was analyzed by gas chromatography and gas chromatography-mass spectrometry. The major volatile constituents of T. impetiginosa were 4-methoxybenzaldehyde (52.84 microg/g), 4-methoxyphenol (38.91 microg/g), 5-allyl-1,2,3-trimethoxybenzene (elemicin; 34.15 microg/g), 1-methoxy-4-(1E)-1-propenylbenzene (trans-anethole; 33.75 microg/g), and 4-methoxybenzyl alcohol (30.29 microg/g). The antioxidant activity of the volatiles was evaluated using two different assays. The extract exhibited a potent inhibitory effect on the formation of conjugated diene hydroperoxides (from methyl linoleate) at a concentration of 1000 microg/mL. The extract also inhibited the oxidation of hexanal for 40 days at a level of 5 microg/mL. The antioxidative activity of T. impetiginosa volatiles was comparable with that of the well-known antioxidants, alpha-tocopherol, and butylated hydroxytoluene.

Procedures of determining organic trace compounds in municipal sewage sludge-a review.

PubMed

Lindholm-Lehto, Petra C; Ahkola, Heidi S J; Knuutinen, Juha S

2017-02-01

Sewage sludge is the largest by-product generated during the wastewater treatment process. Since large amounts of sludge are being produced, different ways of disposal have been introduced. One tempting option is to use it as fertilizer in agricultural fields due to its high contents of inorganic nutrients. This, however, can be limited by the amount of trace contaminants in the sewage sludge, containing a variety of microbiological pollutants and pathogens but also inorganic and organic contaminants. The bioavailability and the effects of trace contaminants on the microorganisms of soil are still largely unknown as well as their mixture effects. Therefore, there is a need to analyze the sludge to test its suitability before further use. In this article, a variety of sampling, pretreatment, extraction, and analysis methods have been reviewed. Additionally, different organic trace compounds often found in the sewage sludge and their methods of analysis have been compiled. In addition to traditional Soxhlet extraction, the most common extraction methods of organic contaminants in sludge include ultrasonic extraction (USE), supercritical fluid extraction (SFE), microwave-assisted extraction (MAE), and pressurized liquid extraction (PLE) followed by instrumental analysis based on gas or liquid chromatography and mass spectrometry.

Testing of a Spray-Bar Zero Gravity Cryogenic Vent System for Upper Stages

NASA Technical Reports Server (NTRS)

Lak, Tibor; Flachbart, Robin; Nguyen, Han; Martin, James

1999-01-01

The capability to vent in zero gravity without resettling is a fundamental technology need that involves practically all uses of subcritical cryogenics in space. Venting without resettling would extend cryogenic orbital transfer vehicle capabilities. However, the lack of definition regarding liquid/ullage orientation coupled with the somewhat random nature of the thermal stratification and resulting pressure rise rates, lead to significant technical challenges. Typically a zero gravity vent concept, termed a thermodynamic vent system (TVS), consists of a tank mixer to destratify the propellant, combined with a Joule- Thomson (J-T) valve to extract then-nal energy from the propellant. In a cooperative effort, Marshall Space Flight Center's (MSFC's) Multipurpose Hydrogen Test Bed (N4HTB) was used to test a unique "spray bar" TVS system developed by Boeing. A schematic of this system is included in Figure 1. The system consists of a recirculation pump, a parallel flow concentric tube, heat exchanger, and a spray bar positioned close to the longitudinal axis of the tank. In the mixing mode, the recirculation pump withdraws liquid from the tank and sprays it radially into the tank liquid, ullage, and exposed tank surfaces. When energy extraction is required, a small portion of the recirculated liquid is passed sequentially through the J-T expansion valve, the spray bar heat exchanger element, and is vented overboard. The vented vapor cools the circulated bulk fluid, thereby removing thermal energy and reducing tank pressure. Figure 2 is a plot of ullage pressure (P4) and liquid vapor pressure (PSAI) versus time. The pump operates alone, cycling on and off, to destratify the tank liquid and ullage until the liquid vapor pressure reaches the lower set point. At that point, the J-T valve begins to cycle on and off with the pump. Thus, for short duration missions, only the mixer may operate, thus minimizing or even eliminating boil-off losses. The primary advantage of the spray bar configuration is that pressure reduction is achieved independent of liquid and vapor location, thereby enhancing the applicability of normal gravity test data to zero gravity conditions. The in-tank components are minimized with the proposed TVS design. Because the recirculation pump is external to the tank, no electrical power penetration of the tank is required for pump or valve operation. This is especially desirable for L02 tanks since the presence of an electrical ignition source in oxygen represents a critical failure mode. Also, since the critical components (pump, motor, valve, orifice) are external to the tank, system checkout and ground servicing/replacement are easier. For zero-g operation, component replacement external to the tank may be a significant benefit. In addition to satisfying the zero g TVS design objectives, the TVS concept tested offers additional benefits to the integrated subcritical cryogenic storage and launch system.

Solubility of oxygen in liquid Fe at high pressure and consequences for the early differentiation of Earth and Mars

NASA Astrophysics Data System (ADS)

Rubie, D. C.; Gessmann, C. K.; Frost, D. J.

2003-04-01

Knowledge of the solubility of oxygen in liquid iron enables the partitioning of oxygen between metal and silicates and the oxidation state of residual silicates to be constrained during core formation in planetary bodies. We have determined oxygen solubility experimentally at 5--23 GPa, 2100--2700 K and oxygen fugacities 1--4 log units below the iron-wüstite buffer in samples of liquid Ni-Fe alloy contained in magnesiowüstite capsules using a multianvil apparatus. Results show that oxygen solubility increases with increasing temperature but decreases slightly with increasing pressure over the range of experimental conditions, at constant oxygen fugacity. Using an extrapolation of the results to higher pressures and temperatures, we have modeled the geochemical consequences of metal-silicate separation in magma oceans in order to explain the contrasting FeO contents of the mantles of Earth and Mars. We assume that both Earth and Mars accreted originally from material with a chondritic composition; because the initial oxidation state is uncertain, we vary this parameter by defining the initial oxygen content. Two metal-silicate fractionation models are considered: (1) Metal and silicate are allowed to equilibrate at fictive conditions that approximate the pressure and temperature at the base of a magma ocean. (2) The effect of settling Fe droplets in a magma ocean is determined using a simple polybaric metal-silicate fractionation model. We assume that the temperature at the base of a magma ocean is close to the peridotite liquidus. In the case of Earth, high temperatures in a magma ocean with a depth >1200 km would have resulted in significant quantities of oxygen dissolving in the liquid metal with the consequent extraction of FeO from the residual silicate. In contrast, on Mars, even if the magma ocean extended to the depth of the current core-mantle boundary, temperatures would not have been sufficiently high for oxygen solubility in liquid metal to be significant. The results show that Earth and Mars could have accreted from similar material, with an initial FeO content around 18 wt%. On Earth, oxygen was extracted from silicates by the segregating metal during core formation, leaving the mantle with its present FeO content of ˜8 wt%. On Mars, in contrast, the segregating metal extracted little or no oxygen and left the FeO content unaltered at ˜18 wt%. A consequence of this model is that oxygen should be an important light element in the Earth's core but not in the Martian core.

Quantification of the xenoestrogens 4-tert.-octylphenol and bisphenol A in water and in fish tissue based on microwave assisted extraction, solid-phase extraction and liquid chromatography-mass spectrometry.

PubMed

Pedersen, S N; Lindholst, C

1999-12-09

Extraction methods were developed for quantification of the xenoestrogens 4-tert.-octylphenol (tOP) and bisphenol A (BPA) in water and in liver and muscle tissue from the rainbow trout (Oncorhynchus mykiss). The extraction of tOP and BPA from tissue samples was carried out using microwave-assisted solvent extraction (MASE) followed by solid-phase extraction (SPE). Water samples were extracted using only SPE. For the quantification of tOP and BPA, liquid chromatography mass spectrometry (LC-MS) equipped with an atmospheric pressure chemical ionisation interface (APCI) was applied. The combined methods for tissue extraction allow the use of small sample amounts of liver or muscle (typically 1 g), low volumes of solvent (20 ml), and short extraction times (25 min). Limits of quantification of tOP in tissue samples were found to be approximately 10 ng/g in muscle and 50 ng/g in liver (both based on 1 g of fresh tissue). The corresponding values for BPA were approximately 50 ng/g in both muscle and liver tissue. In water, the limit of quantification for tOP and BPA was approximately 0.1 microg/l (based on 100 ml sample size).

Determination of acetaminophen concentrations in serum by high-pressure liquid chromatography.

PubMed

Horvitz, R A; Jatlow, P I

1977-09-01

We describe a method for determination of serum acetaminophen concentrations in serum by reversed phase high-pressure liquid chromatography. The homolog N-propionyl-p-aminophenol was used as an internal standard. The procedure, which requires only a single extraction with diethyl ether, can be optimized to be linear over the ranges of 10 to 100 or 1 to 20 mg/liter. Within-run CV was 1.2%; between-run CV was 4.4% and 4.9% at two different concentrations. Many commonly used drugs were tested and found not to interfere. The procedure is simple and rapid enough for use on an emergency basis in cases of overdosage, and can be optimized for measurement of either therapeutic or toxic concentrations.

Duration of bubble rearrangements in a coarsening foam probed by time-resolved diffusing-wave spectroscopy: Impact of interfacial rigidity

NASA Astrophysics Data System (ADS)

Le Merrer, Marie; Cohen-Addad, Sylvie; Höhler, Reinhard

2013-08-01

In aqueous foams, the diffusive gas transfer among neighboring bubbles drives a coarsening process which is accompanied by intermittent rearrangements of the structure. Using time-resolved diffusing-wave spectroscopy, we probe the dynamics of these events as a function of the rigidity of the gas-liquid interfaces, liquid viscosity, bubble size, and confinement pressure. We present in detail two independent techniques for analyzing the light scattering data, from which we extract the rearrangement duration. Our results show that interfacial rheology has a major impact on this duration. In the case of low interfacial rigidity, the rearrangements strongly slow down as the pressure is decreased close to the value zero where the bubble packing unjams. In contrast, if the interfaces are rigid, rearrangement durations are independent of the confinement pressure in the same investigated range. Using scaling arguments, we discuss dissipation mechanisms that may explain the observed dependency of the rearrangement dynamics on foam structure, pressure, and physicochemical solution properties.

Pressure gradient induced generation of microbubbles

NASA Astrophysics Data System (ADS)

Evangelio, Alvaro; Campo-Cortes, Francisco; Gordillo, Jose Manuel

2015-11-01

It is well known that the controlled production of monodisperse bubbles possesses uncountable applications in medicine, pharmacy and industry. Here we provide with a detailed physical description of the bubble formation processes taking place in a type of flow where the liquid pressure gradient can be straightforwardly controlled. In our experiments, a gas flow rate discharges through a cylindrical needle into a pressurized chamber. The pressure gradient created from the exit of the injection needle towards the entrance of a extraction duct promotes the stretching of the gas ligament downstream. In our analysis, which is supported by an exhaustive experimental study in which the liquid viscosity is varied by three orders of magnitude, different regimes can be distinguished depending mainly on the Reynolds number. Through our physical modeling, we provide closed expressions for both the bubbling frequencies and for the bubble diameters as well as the conditions under which a monodisperse generation is obtained in all regimes found. The excellent agreement between our expressions and the experimental data fully validates our physical modeling.

Process control of turboexpander plants

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

Guffey, C.G.; Heenan, W.A.

1984-05-01

The turboexpander process uses the high pressure of the natural gas stream to drive a rotating expander wheel to extract mechanical work from the flowing stream. The removal of energy and the reduced pressure result in a large refrigeration effect which condenses ethane, propane and heavier components in the natural gas as liquids for recovery and sale. The recovered work is transmitted directly to a shaft which usually drives a gas recompressor. This compressor increases the pressure of the dry residue gas after liquid recovery. Operation of the demethanizer or de-ethanizer at the low pressure of the main gas streammore » eliminates the requirement for a separate demethanizer overhead gas booster compressor. There are many variations of this simplified process including supplemental inlet refrigeration, parallel trains of heat exchangers, side reboilers on the demethanizer and multiple expanders which must be controlled and affect the dynamic response to variable changes. This paper excludes these complications in the analysis of the system.« less

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.

A protocol for pressurized liquid extraction and processing methods to isolate modern and ancient bone cholesterol for compound-specific stable isotope analysis.

PubMed

Laffey, Ann O; Krigbaum, John; Zimmerman, Andrew R

2017-02-15

Bone lipid compound-specific isotope analysis (CSIA) and bone collagen and apatite stable isotope ratio analysis are important sources of ecological and paleodietary information. Pressurized liquid extraction (PLE) is quicker and utilizes less solvent than traditional methods of lipid extraction such as soxhlet and ultrasonication. This study facilitates dietary analysis by optimizing and testing a standardized methodology for PLE of bone cholesterol. Modern and archaeological bones were extracted by PLE using varied temperatures, solvent solutions, and sample weights. The efficiency of PLE was assessed via quantification of cholesterol yields. Stable isotopic ratio integrity was evaluated by comparing isotopic signatures (δ 13 C and δ 18 O values) of cholesterol derived from whole bone, bone collagen and bone apatite. Gas chromatography/mass spectrometry (GC/MS) and gas chromatography isotope ratio mass spectrometry (GC/IRMS) were conducted on purified collagen and lipid extracts to assess isotopic responses to PLE. Lipid yield was optimized at two PLE extraction cycles of 75 °C using dichloromethane/methanol (2:1 v/v) as a solvent with 0.25-0.75 g bone sample. Following lipid extraction, saponification combined with the derivatization of the neutral fraction using trimethylsilylation yielded nearly twice the cholesterol of non-saponified or non-derivatized samples. It was also found that lipids extracted from purified bone collagen and apatite could be used for cholesterol CSIA. There was no difference in the bulk δ 13 C values of collagen extracted from bone with or without lipid. However, there was a significant depletion in 18 O of bone apatite due to lipid presence or processing. These results should assist sample selection and provide an effective, alternative extraction method for bone cholesterol that may be used for isotopic and paleodietary analysis. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

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.

Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography.

PubMed

Doshi, Gaurav Mahesh; Une, Hemant Devidas

2016-01-01

In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida.

Evaluation of carbohydrates in natural and cultured Cordyceps by pressurized liquid extraction and gas chromatography coupled with mass spectrometry.

PubMed

Guan, Jia; Yang, Feng-Qing; Li, Shao-Ping

2010-06-11

Free and polymeric carbohydrates in Cordyceps, a valued edible mushroom and well-known traditional Chinese medicine, were determined using stepwise pressurized liquid extraction (PLE) extraction and GC-MS. Based on the optimized PLE conditions, acid hydrolysis and derivatization, ten monosaccharides, namely rhamnose, ribose, arabinose, xylose, mannose, glucose, galactose, mannitol, fructose and sorbose in 13 samples of natural and cultured Cordyceps were qualitatively and quantitatively analyzed and compared with myo-inositol hexaacetate as internal standard. The results showed that natural C. sinensis contained more than 7.99% free mannitol and a small amount of glucose, while its polysaccharides were usually composed of mannose, glucose and galactose with a molar ratio of 1.00:16.61-3.82:1.60-1.28. However, mannitol in cultured C. sinensis and cultured C. militaris were less than 5.83%, and free glucose was only detected in a few samples, while their polysaccharides were mainly composed of mannose, glucose and galactose with molar ratios of 1.00:3.01-1.09:3.30-1.05 and 1.00:2.86-1.28:1.07-0.78, respectively. Natural and cultured Cordyceps could be discriminated by hierarchical clustering analysis based on its free carbohydrate contents.

Direct probing of chromatography columns by laser-induced fluorescence

NASA Astrophysics Data System (ADS)

McGuffin, V. L.

1992-12-01

This report summarizes the progress and accomplishments of this research project from 1 Sep. 1989 to 28 Feb. 1993. During this period, we have accomplished all of the primary scientific objectives of the research proposal: (1) constructed and evaluated a laser-induced fluorescence detection system that allows direct examination of the chromatographic column, (2) examined nonequilibrium processes that occur upon solute injection and elution, (3) examined solute retention in liquid chromatography as a function of temperature and pressure, (4) examined solute zone dispersion in liquid chromatography as a function of temperature and pressure, and (5) developed appropriate theoretical models to describe these phenomena. In each of these studies, substantial knowledge has been gained of the fundamental processes that are responsible for chromatographic separations. In addition to these primary research objectives, we have made significant progress in three related areas: (1) examined pyrene as a fluorescent polarity probe in supercritical fluids and liquids as a function of temperature and pressure, (2) developed methods for the class-selective identification of polynuclear aromatic hydrocarbons in coal-derived fluids by microcolumn liquid chromatography with fluorescence quenching detection, and (3) developed methods for the determination of saturated and unsaturated (including omega-3) fatty acids in fish oil extracts by microcolumn liquid chromatography with laser-induced fluorescence detection. In these studies, the advanced separation and detection techniques developed in our laboratory are applied to practical problems of environmental and biomedical significance.

COMPARISON OF PRESSURIZED LIQUID EXTRACTION AND MATRIX SOLID PHASE DISPERSION FOR THE MEASUREMENT OF SEMI-VOLATILE ORGANIC COMPOUND ACCUMULATION IN TADPOLES

EPA Science Inventory

Analytical methods capable of trace measurement of semi-volatile organic compounds (SOCs) are necessary to assess the exposure of tadpoles to contaminants as a result of long-range and regional atmospheric transport and deposition. The following study compares the results of two ...

Ultra-high-pressure liquid chromatography-tandem mass spectrometry for the analysis of six resorcylic acid lactones in bovine milk.

PubMed

Xia, Xi; Li, Xiaowei; Ding, Shuangyang; Zhang, Suxia; Jiang, Haiyang; Li, Jiancheng; Shen, Jianzhong

2009-03-20

This work reports a rapid, reliable and sensitive multi-residue method for the simultaneous determination of six resorcylic acid lactones in bovine milk by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The resorcylic acid lactones were extracted, purified, and concentrated from milk samples in one step using a solid-phase extraction (SPE) cartridge that contained a polymeric mixed-mode anion-exchange sorbent. The analysis was performed on a Waters Acquity BEH C(18) column utilizing a gradient elution profile. Each LC run was completed in 3.5 min. The analytes were detected by multiple reaction monitoring (MRM) using electrospray ionization (ESI) negative mode. Mean recoveries from fortified samples ranged from 92.6% to 112.5%, with relative standard deviations lower than 11.4%. Using 5 mL bovine milk, the limits of detection and quantification for resorcylic acid lactones were in the ranges of 0.01-0.05 and 0.05-0.2 microg/L, respectively. The application of this newly developed method was demonstrated by analyzing bovine milk samples from markets.

Systematic Analysis of Absorbed Anti-Inflammatory Constituents and Metabolites of Sarcandra glabra in Rat Plasma Using Ultra-High-Pressure Liquid Chromatography Coupled with Linear Trap Quadrupole Orbitrap Mass Spectrometry.

PubMed

Li, Xiong; Zhao, Jin; Liu, Jianxing; Li, Geng; Zhao, Ya; Zeng, Xing

2016-01-01

Ultra-high-pressure liquid chromatography (UHPLC) was coupled with linear ion trap quadrupole Orbitrap mass spectrometry (LTQ-Orbitrap) and was used for the first time to systematically analyze the absorbed components and metabolites in rat plasma after oral administration of the water extract of Sarcandra glabra. This extract is a well-known Chinese herbal medicine for the treatment of inflammation and immunity related diseases. The anti-inflammatory activities of the absorbed components were evaluated by measuring nitric oxide (NO) production and proinflammatory genes expression in lipopolysaccharide (LPS)-stimulated murine RAW 264.7 macrophages. As a result, 54 components in Sarcandra glabra were detected in dosed rat plasma, and 36 of them were positively identified. Moreover, 23 metabolites were characterized and their originations were traced. Furthermore, 20 of the 24 studied components showed anti-inflammatory activities. These results provide evidence that this method efficiency detected constituents in plasma based on the anti-inflammatory mechanism of multiple components and would be a useful technique for screening multiple targets for natural medicine research.

Determination of boldenone sulfoconjugate and related steroid sulfates in equine urine by high-performance liquid chromatography/tandem mass spectrometry.

PubMed

Weidolf, L O; Lee, E D; Henion, J D

1988-03-01

Sulfoconjugated anabolic steroids were separated by micro-bore high-performance liquid chromatography. The eluent was introduced into the atmospheric pressure ion source of the triple-quadrupole mass spectrometer via an ion spray liquid chromatograph/mass spectrometer interface operated in the negative ion mode. The limit of detection was 10 pg on-column by selected ion monitoring of the molecular ion and the response increased linearly over a concentration range of 2.4 orders of magnitude. Following work-up by a liquid-solid extraction procedure of equine urine samples, full-scan daughter ion spectra of boldenone sulfate could be obtained up to 17 days after a therapeutic dose of boldenone undecylenate to a horse.

Field-portable supercritical CO{sub 2} extractor

DOEpatents

Wright, B.W.; Zemanian, T.S.; Robins, W.H.; Woodcock, L.J.

1997-06-10

The present invention is an apparatus for extracting organic compounds from solid materials. A generator vessel has a removable closure for receiving a solid or liquid solvent which is heated with a resistive heating element to a gaseous or supercritical phase. The removable closure is unencumbered because the side wall is penetrated with an outlet for the gaseous or supercritical solvent. The generator vessel further has a pressure transducer that provides an electronic signal related to pressure of the gaseous or supercritical solvent. The apparatus of the present invention further includes at least one extraction cell having a top and a bottom and a wall extending there between, wherein the bottom is sealably penetrated by an inlet for gaseous or supercritical solvent received through a manifold connected to the outlet, the top having an easy-open removable closure cap, and the wall having an outlet port. Finally, a permeable sample cartridge is included for holding the solid materials and to provide radial-flow of the extraction fluid, which is placed within the extraction cell. 10 figs.

Field-portable supercritical CO.sub.2 extractor

DOEpatents

Wright, Bob W.; Zemanian, Thomas S.; Robins, William H.; Woodcock, Leslie J.

1997-01-01

The present invention is an apparatus for extracting organic compounds from solid materials. A generator vessel has a removable closure for receiving a solid or liquid solvent which is heated with a resistive heating element to a gaseous or supercritical phase. The removable closure is unencumbered because the side wall is penetrated with an outlet for the gaseous or supercritical solvent. The generator vessel further has a pressure transducer that provides an electronic signal related to pressure of the gaseous or supercritical solvent. The apparatus of the present invention further includes at least one extraction cell having a top and a bottom and a wall extending therebetween, wherein the bottom is sealably penetrated by an inlet for gaseous or supercritical solvent received through a manifold connected to the outlet, the top having an easy-open removable closure cap, and the wall having an outlet port. Finally, a permeable sample cartridge is included for holding the solid materials and to provide radial-flow of the extraction fluid, which is placed within the extraction cell.

Three-phase hollow-fiber liquid-phase microextraction combined with HPLC-UV for the determination of isothiazolinone biocides in adhesives used for food packaging materials.

PubMed

Rosero-Moreano, Milton; Canellas, Elena; Nerín, Cristina

2014-02-01

The present study deals with the development of a liquid microextraction procedure for enhancing the sensitivity of the determination of 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one in adhesives. The procedure involves a three-phase hollow-fiber liquid-phase microextraction using a semipermeable polypropylene membrane, which contained 1-octanol as the organic phase in the pores of the membrane. The donor and acceptor phases are aqueous acidic and alkaline media, respectively, and the final liquid phase (acceptor) is analyzed by HPLC coupled with diode array detection. The most appropriate conditions were extraction time 20 min, stirring speed 1400 rpm, extraction temperature 50°C. The quantification limits of the method were 0.123 and 0.490 μg/g for 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one, respectively. Three different adhesive samples were successfully analyzed. The procedure was compared to direct analysis using ultra high pressure liquid chromatography coupled with TOF-MS, where the identification of the compounds and the quantification values were confirmed. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous in-cell derivatization pressurized liquid extraction for the determination of multiclass preservatives in leave-on cosmetics.

PubMed

Sanchez-Prado, Lucia; Lamas, J Pablo; Lores, Marta; Garcia-Jares, Carmen; Llompart, Maria

2010-11-15

An effective one-step sample preparation methodology for the determination of multiclass preservatives in cosmetics has been developed, applying, for the first time to this kind of matrix, pressurized liquid extraction (PLE) and a very simple, cheap, and fast derivatization procedure: acetylation with acetic anhydride and pyridine. A multifactorial experimental design has been used to evaluate and optimize the main experimental parameters potentially affecting the extraction process. In the final conditions the sample was mixed with Florisil as the dispersing sorbent and extracted with ethyl acetate for 15 min at 120 °C. One of the main goals of this work was to demonstrate the possibility of carrying out direct cosmetic preservative acetylation by simply adding the derivatization reagents into the PLE cell. The extract was then analyzed by GC/MS without any further cleanup or concentration step. The accuracy, precision, linearity, and detection limits (LODs) were evaluated to assess the performance of the proposed method. Quantitative recoveries were obtained, and relative standard deviation values were lower than 10% in all cases. The obtained LODs ranged from 0.000004% to 0.0001% (w/w), values far below the established restrictions in the European Cosmetics Regulation, making this multicomponent analytical method suitable for routine control. Finally, several cosmetic products such as moisturizing and antiwrinkle creams and lotions, hand creams, sunscreen and after-sun creams, baby lotions, and hair care products were analyzed. All the samples contained several of the target cosmetic ingredients, in some cases at quite high concentrations, although the actual European Cosmetics Regulation was fulfilled in all cases.

Determination of organophosphorus flame retardants in fish by pressurized liquid extraction using aqueous solutions and solid-phase microextraction coupled with gas chromatography-flame photometric detector.

PubMed

Gao, Zhanqi; Deng, Yuehua; Yuan, Wenting; He, Huan; Yang, Shaogui; Sun, Cheng

2014-10-31

A novel method was developed for the determination of organophosphorus flame retardants (PFRs) in fish. The method consists of a combination of pressurized liquid extraction (PLE) using aqueous solutions and solid-phase microextraction (SPME), followed by gas chromatography-flame photometric detector (GC-FPD). The experimental parameters that influenced extraction efficiency were systematically evaluated. The optimal responses were observed by extracting 1g of fish meat with the solution of water:acetonitrile (90:10, v/v) at 150°C for 5min and acid-washed silica gel used as lipid sorbent. The obtained extract was then analyzed by SPME coupled with GC-FPD without any additional clean-up steps. Under the optimal conditions, the proposed procedure showed a wide linear range (0.90-5000ngg(-1)) obtained by analyzing the spiked fish samples with increasing concentrations of PFRs and correlation coefficient (R) ranged from 0.9900 to 0.9992. The detection limits (S/N=3) were in the range of 0.010-0.208ngg(-1) with standard deviations (RSDs) ranging from 2.0% to 9.0%. The intra-day and inter-day variations were less than 9.0% and 7.8%, respectively. The proposed method was successfully applied to the determination of PFRs in real fish samples with recoveries varying from 79.8% to 107.3%. The results demonstrate that the proposed method is highly effective for analyzing PFRs in fish samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of cinnamaldehyde, carvacrol and thymol in feedstuff additives by pressurized liquid extraction followed by gas chromatography-mass spectrometry.

PubMed

Jiménez-Salcedo, Marta; Tena, María Teresa

2017-03-03

Specific blends of essential oils (BEOs) are promising substitutes for antibiotics to promote livestock performance and to reduce the incidence of intestinal disorders. Microencapsulation of BEOs has shown to improve their stability, bioavailability and to control their release rate once they are added to the feedstuff. The development and validation of a method for determining essential oil components such as carvacrol, thymol and cinnamaldehyde in a microencapsulated material used as feed additive is presented. Analytes were extracted from feed additives and feedstuff by pressurized liquid extraction (PLE) with methanol at 50°C for 5min. Methanol provided good recovery values and cleaner extracts than other polar organic solvents tested. However, for certain kind of composite additives ethyl acetate showed to be a better option because trans-cinnamaldehyde undergoes chemical reaction in methanol. Then PLE extracts were analysed by gas chromatography coupled to ion trap mass spectrometry in selected ion storage (SIS) mode. The analyte stability and the absence of analyte losses during the PLE process was checked by a recovery study. Also, the matrix effect was studied to assess accuracy. Recovery values were between 85 and 115% in most cases. Intra- and inter-day relative standard deviation values were less than 4 and 14%, respectively. Finally, the developed method was applied to the analysis of a microencapsulated feed additive, several composite feed additive samples containing microencapsulated BEOs and a spiked feedstuff, for quality control and in stability studies. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Preparative Isolation and Purification of Flavone C-Glycosides from the Leaves of Ficus microcarpa L. f by Medium-Pressure Liquid Chromatography, High-Speed Countercurrent Chromatography, and Preparative Liquid Chromatography

PubMed Central

Wang, Xiaohong; Liang, Yong; Zhu, Licai; Xie, Huichun; Li, Hang; He, Junting; Pan, Man; Zhang, Tianyou; Ito, Yoichiro

2009-01-01

Combined with medium-pressure liquid chromatography (MPLC) and preparative high-performance liquid chromatography (perp-HPLC), high-speed countercurrent chromatography (HSCCC) was applied for separation and purification of flavone C-glycosides from the crude extract of leaves of Ficus microcarpae L. f. HSCCC separation was performed on a two-phase solvent system composed of methyl tert- butyl ether - ethyl acetate – 1-butanol – acetonitrile – 0.1% aqueous trifluoroacetic acid at a volume ratio of 1:3:1:1:5. Partially resolved peak fractions from HSCCC separation were further purified by preparative HPLC. Four well-separated compounds were obtained and their purities were determined by HPLC. The purities of these peaks were 97.28%, 97.20%, 92.23%, and 98.40%.. These peaks were characterized by ESI-MSn. According to the reference, they were identified as orientin (peak I), isovitexin-3″-O-glucopyranoside (peak II), isovitexin (peak III), and vitexin (peak IV), yielded 1.2 mg, 4.5 mg, 3.3 mg, and 1.8 mg, respectively. PMID:20190866

Extraction and analysis methods for the determination of pyrethroid insecticides in surface water, sediments and biological tissues at environmentally relevant concentrations.

PubMed

Mekebri, A; Crane, D B; Blondina, G J; Oros, D R; Rocca, J L

2008-05-01

The aim of this study was to develop and validate chemical methods for measuring pyrethroid insecticides at environmentally relevant concentrations in different matrices. The analytes included six synthetic pyrethroids with the highest agricultural and commercial structural uses in California: bifenthrin, cyfluthrin, cypermethrin, esfenvalerate/fenvalerate, lambda-cyhalothrin, permethrin, and their corresponding stereoisomers, which includes enantiomers, diastereomers and racemic mixtures. Fortified water samples were extracted for analysis of synthetic pyrethroids using liquid-liquid extraction, while fortified sediment and fish tissue samples were extracted using pressurized fluid extraction followed by gel permeation chromatography (GPC) to remove matrix interferences. A florisil column was used for additional cleanup and fractionation of sediment and tissue extracts. Extracts were analyzed using dual column high resolution gas chromatography with electron capture detection (GC/ECD) and confirmation was obtained with gas chromatography mass spectrometry using a quadrupole ion trap detector in MS-MS mode. Method detection limits (MDLs) have been established for water (1-3 ng/L), sediment (0.5-4 ng/g dry weight) and tissue (1-3 ng/g fresh weight). Mean percent recoveries of fortified blanks and samples ranged from 75 to 115% with relative standard deviation (RSD) values less than 20% for all target compounds.

Determination of ten monohydroxylated polycyclic aromatic hydrocarbons by liquid-liquid extraction and liquid chromatography/tandem mass spectrometry.

PubMed

Fan, Ruifang; Ramage, Robert; Wang, Dongli; Zhou, Junqiang; She, Jianwen

2012-05-15

The aim of this study is to develop and validate an analytical method for the quantitation of ten urinary monohydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) through high pressure liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). After enzymatic deconjugation, urine samples were extracted by liquid-liquid extraction (LLE) and OH-PAHs were analyzed by HPLC/MS/MS operated in negative electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode. LLE was conducted with the solvent mixture of pentane and toluene, which reduced the matrix interferences and enhanced the method sensitivity significantly. Deuterated and (13)C-labeled analogs are used as internal standards. Calibration curves of all target analytes shows favorable linearity within the concentration range of 5.9-15,000.0 ng/L for different OH-PAHs with the regression coefficients above 0.993. The limits of detection (LODs) in pooled urine ranged from 1.72 to 17.47 ng/L, which were much lower than those obtained by a gas chromatography/high resolution mass spectrometry (GC/HRMS) method. The method shows satisfactory accuracy and precision when analyzing three different levels of OH-PAHs spiked in pooled urine. Except for 1-hydroxynaphthalene, recoveries of other OH-PAHs were in the range of 100 ± 20% with a variation coefficient of less than 13%. The measurement of OH-PAHs from a QC sample of the Centers for Disease Control and Prevention (CDC) generated results close to the values measured by CDC. This method has been successfully employed in the California Biomonitoring Program. Published by Elsevier B.V.

Numerical Modeling of Self-Pressurization and Pressure Control by Thermodynamic Vent System in a Cryogenic Tank

NASA Technical Reports Server (NTRS)

Majumdar, Alok; Valenzuela, Juan; LeClair, Andre; Moder, Jeff

2015-01-01

This paper presents a numerical model of a system-level test bed - the multipurpose hydrogen test bed (MHTB) using Generalized Fluid System Simulation Program (GFSSP). MHTB is representative in size and shape of a fully integrated space transportation vehicle liquid hydrogen (LH2) propellant tank and was tested at Marshall Space Flight Center (MSFC) to generate data for cryogenic storage. GFSSP is a finite volume based network flow analysis software developed at MSFC and used for thermo-fluid analysis of propulsion systems. GFSSP has been used to model the self-pressurization and ullage pressure control by Thermodynamic Vent System (TVS). A TVS typically includes a Joule-Thompson (J-T) expansion device, a two-phase heat exchanger, and a mixing pump and spray to extract thermal energy from the tank without significant loss of liquid propellant. Two GFSSP models (Self-Pressurization & TVS) were separately developed and tested and then integrated to simulate the entire system. Self-Pressurization model consists of multiple ullage nodes, propellant node and solid nodes; it computes the heat transfer through Multi-Layer Insulation blankets and calculates heat and mass transfer between ullage and liquid propellant and ullage and tank wall. TVS model calculates the flow through J-T valve, heat exchanger and spray and vent systems. Two models are integrated by exchanging data through User Subroutines of both models. The integrated models results have been compared with MHTB test data of 50% fill level. Satisfactory comparison was observed between test and numerical predictions.

Ionic liquid-based single-drop microextraction/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene and xylene isomers in waters.

PubMed

Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

2008-08-01

The direct coupling between ionic liquid-based single-drop microextraction and gas chromatography/mass spectrometry is proposed for the rapid and simple determination of benzene, toluene, ethylbenzene and xylenes isomers (BTEX) in water samples. The extraction procedure exploits not only the high affinity of the selected ionic liquid (1-methyl-3-octyl-imidazolium hexaflourophosphate) to these aromatic compounds but also its special properties like viscosity, low vapour pressure and immiscibility with water. All the variables involved in the extraction process have been studied in depth. The developed method allows the determination of these single-ring compounds in water under the reference concentration level fixed by the international legislation. In this case, limits of detection were in the range 20 ng L(-1) (obtained for benzene) and 91 ng L(-1) (for o-xylene). The repeatability of the proposed method, expressed as RSD (n=5), varied between 3.0% (o-xylene) and 5.2% (toluene).

Simultaneous determination of 24 personal care products in fish muscle and liver tissues using QuEChERS extraction coupled with ultra pressure liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometer analyses.

PubMed

Yao, Li; Zhao, Jian-Liang; Liu, You-Sheng; Yang, Yuan-Yuan; Liu, Wang-Rong; Ying, Guang-Guo

2016-11-01

A sensitive and selective quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction combined with dispersive solid-phase extraction (d-SPE) cleanup method was developed to simultaneously extract a wide range of personal care products (16 biocides, 4 synthetic musks, and 4 benzotriazoles) in fish muscle and liver tissues. In order to get satisfactory recoveries, different extraction parameters were optimized, including extraction salts and d-SPE materials, extraction solvents and acetic acid contents in organic phase, and the ratios of solvent and water. Ultra pressure liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry were used to analyze the target compounds in the extracts. Among the 24 personal care products, the recoveries in the range of 70-120 % were obtained for 20, 19, and 12 analytes in fish muscle at the spiking concentrations of 10, 5, and 1 ng/g ww, respectively, and for 13, 12, and 11 analytes in liver at the spiking concentrations of 40, 20, and 4 ng/g ww, respectively. Method quantification limits (MQLs) of all analytes were 0.02-2.12 ng/g ww for fish muscle and 0.22-12.2 ng/g ww for fish liver tissues. The method was successfully applied to wild fish samples collected from Dongjiang River, south China. Twenty-one and 17 of the analytes were found in fish muscle and liver samples, respectively, in at least one site of the river with the concentrations between below MQLs and 119 ng/g ww, respectively. Graphical abstract Achieved satisfactory recoveries, high precision, and low method quantification limits (MQLs) for PCPs in wild fish tissues by QuEChERS procedure optimization combined with UPLC-MS/MS and GC-MS analyses.

Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography

PubMed Central

Doshi, Gaurav Mahesh; Une, Hemant Devidas

2016-01-01

Objective: In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. Materials and Methods: In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. Results: HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. Conclusion: The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. SUMMARY Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida PMID:26941534

Monolithic methacrylate packed 96-tips for high throughput bioanalysis.

PubMed

Altun, Zeki; Skoglund, Christina; Abdel-Rehim, Mohamed

2010-04-16

In the pharmaceutical industry the growing number of samples to be analyzed requires high throughput and fully automated analytical techniques. Commonly used sample-preparation methods are solid-phase extraction (SPE), liquid-liquid extraction (LLE) and protein precipitation. In this paper we will discus a new sample-preparation technique based on SPE for high throughput drug extraction developed and used by our group. This new sample-preparation method is based on monolithic methacrylate polymer as packing sorbent for 96-tip robotic device. Using this device a 96-well plate could be handled in 2-4min. The key aspect of the monolithic phase is that monolithic material can offer both good binding capacity and low back-pressure properties compared to e.g. silica phases. The present paper presents the successful application of monolithic 96-tips and LC-MS/MS by the sample preparation of busulphan, rescovitine, metoprolol, pindolol and local anaesthetics from human plasma samples and cyklophosphamid from mice blood samples. Copyright 2009 Elsevier B.V. All rights reserved.

The Development and Test of a Sensor for Measurement of the Working Level of Gas-Liquid Two-Phase Flow in a Coalbed Methane Wellbore Annulus.

PubMed

Wu, Chuan; Ding, Huafeng; Han, Lei

2018-02-14

Coalbed methane (CBM) is one kind of clean-burning gas and has been valued as a new form of energy that will be used widely in the near future. When producing CBM, the working level within a CBM wellbore annulus needs to be monitored to dynamically adjust the gas drainage and extraction processes. However, the existing method of measuring the working level does not meet the needs of accurate adjustment, so we designed a new sensor for this purpose. The principle of our sensor is a liquid pressure formula, i.e., the sensor monitors the two-phase flow patterns and obtains the mean density of the two-phase flow according to the pattern recognition result in the first step, and then combines the pressure data of the working level to calculate the working level using the liquid pressure formula. The sensor was tested in both the lab and on site, and the tests showed that the sensor's error was ±8% and that the sensor could function well in practical conditions and remain stable in the long term.

The Development and Test of a Sensor for Measurement of the Working Level of Gas–Liquid Two-Phase Flow in a Coalbed Methane Wellbore Annulus

PubMed Central

Wu, Chuan; Ding, Huafeng; Han, Lei

2018-01-01

Coalbed methane (CBM) is one kind of clean-burning gas and has been valued as a new form of energy that will be used widely in the near future. When producing CBM, the working level within a CBM wellbore annulus needs to be monitored to dynamically adjust the gas drainage and extraction processes. However, the existing method of measuring the working level does not meet the needs of accurate adjustment, so we designed a new sensor for this purpose. The principle of our sensor is a liquid pressure formula, i.e., the sensor monitors the two-phase flow patterns and obtains the mean density of the two-phase flow according to the pattern recognition result in the first step, and then combines the pressure data of the working level to calculate the working level using the liquid pressure formula. The sensor was tested in both the lab and on site, and the tests showed that the sensor’s error was ±8% and that the sensor could function well in practical conditions and remain stable in the long term. PMID:29443871

On-line hyphenation of centrifugal partition chromatography and high pressure liquid chromatography for the fractionation of flavonoids from Hippophaë rhamnoides L. berries.

PubMed

Michel, Thomas; Destandau, Emilie; Elfakir, Claire

2011-09-09

Centrifugal Partition Chromatography (CPC), a liquid-liquid preparative chromatography using two immiscible solvent systems, benefits from numerous advantages for the separation or purification of synthetic or natural products. This study presents the on-line hyphenation of CPC-Evaporative Light Scattering Detector (CPC-ELSD) with High Performance Liquid Chromatography-UV (HPLC-UV) for the fractionation of flavonols from a solvent-free microwave extract of sea buckthorn (Hippophaë rhamnoides L., Elaeagnaceae) berries. An Arizona G system was used for the fractionation of flavonoids by CPC and a fused core Halo C18 column allowed the on-line analyses of collected fractions by HPLC. The on-line CPC/HPLC procedure allowed the simultaneous fractionation step at preparative scale combined with the HPLC analyses which provide direct fingerprint of collected fractions. Thus the crude extract was simplified and immediate information on the composition of fractions could be obtained. Furthermore, this methodology reduced the time of post-fractionation steps and facilitated identification of main molecules by Mass Spectrometry (MS). Rutin, isorhamnetin-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin-3-O-glucoside, isorhamnetin-rhamnoside, quercetin and isorhamnetin were identified. CPC-ELSD/HPLC-UV could be considered as a high-throughput technique for the guided fractionation of bioactive natural products from complex crude extracts. Copyright © 2011 Elsevier B.V. All rights reserved.

Development and validation of LC-MS/MS methods for the determination of mirabegron and its metabolites in human plasma and their application to a clinical pharmacokinetic study.

PubMed

Teijlingen, Raymond van; Meijer, John; Takusagawa, Shin; Gelderen, Marcel van; Beld, Cas van den; Usui, Takashi

2012-03-01

Mirabegron is being developed for the treatment of overactive bladder. To support the development of mirabegron, including pharmacokinetic studies, liquid chromatography/tandem mass spectrometry methods for mirabegron and eight metabolites (M5, M8, M11-M16) were developed and validated for heparinized human plasma containing sodium fluoride. Four separate bioanalytical methods were developed for the analysis of: (1) mirabegron; (2) M5 and M16; (3) M8; and (4) M11-M15. Either solid-phase extraction or liquid-liquid extraction was used to extract the analytes of interest from matrix constituents. For mirabegron, an Inertsil C₈-3 analytical column was used and detection was performed using a triple-quad mass spectrometer equipped with an atmospheric pressure chemical ionization interface. For the metabolite assays, chromatographic separation was performed through a Phenomenex Synergi Fusion-RP C₁₈ analytical column and detection was performed using a triple-quad mass spectrometer equipped with a Heated Electrospray Ionization interface. The validation results demonstrated that the developed liquid chromatography/tandem mass spectrometry methods were precise, accurate, and selective for the determination of mirabegron and its metabolites in human plasma. All methods were successfully applied in evaluating the pharmacokinetic parameters of mirabegron and metabolites in human plasma. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2007-03-23

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

Sequential high pressure extractions applied to recover piceatannol and scirpusin B from passion fruit bagasse.

PubMed

Viganó, Juliane; Aguiar, Ana C; Moraes, Damila R; Jara, José L P; Eberlin, Marcos N; Cazarin, Cinthia B B; Maróstica, Mário R; Martínez, Julian

2016-07-01

Passion fruit seeds are currently discarded on the pulp processing but are known for their high piceatannol and scirpusin B contents. Using pressurized liquid extraction (PLE), these highly valuable phenolic compounds were efficiently extracted from defatted passion fruit bagasse (DPFB). PLE was performed using mixtures of ethanol and water (50 to 100% ethanol, w/w) as solvent, temperatures from 50 to 70°C and pressure at 10MPa. The extraction methods were compared in terms of the global yield, total phenolic content (TPC), piceatannol content and the antioxidant capacity of the extracts. The DPFB extracts were also compared with those from non-defatted passion fruit bagasse (nDPFB). Identification and quantification of piceatannol were performed using UHPLC-MS/MS. The results showed that high TPC and piceatannol content were achieved for the extracts obtained from DPFB through PLE at 70°C and using 50 and 75% ethanol as the solvent. The best PLE conditions for TPC (70°C, 75% ethanol) resulted in 55.237mgGAE/g dried and defatted bagasse, whereas PLE at 70°C and 50% ethanol achieved 18.590mg of piceatannol/g dried and defatted bagasse, and such yields were significantly higher than those obtained using conventional extraction techniques. The antioxidant capacity assays showed high correlation with the TPC (r>0.886) and piceatannol (r>0.772). The passion fruit bagasse has therefore proved to be a rich source of piceatannol and PLE showed high efficiency to recover phenolic compounds from defatted passion fruit bagasse. Copyright © 2016 Elsevier Ltd. 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).

Design of guanidinium ionic liquid based microwave-assisted extraction for the efficient extraction of Praeruptorin A from Radix peucedani.

PubMed

Ding, Xueqin; Li, Li; Wang, Yuzhi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

2014-12-01

A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids were confirmed by (1)H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave-assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed-phase high-performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single-factor and L9 (3(4)) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3-tetramethylguanidine]CH2CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave-assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound-assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave-assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave-assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Acrylamide: formation, occurrence in food products, detection methods, and legislation.

PubMed

Arvanitoyannis, Ioannis S; Dionisopoulou, Niki

2014-01-01

This review aims at summarizing the most recent updates in the field of acrylamide (AA) formation (mechanism, conditions) and the determination of AA in a number of foods (fried or baked potatoes, chips, coffee, bread, etc). The methods applied for AA detection [Capillary Electrophoresis-Mass Spectrometry (CE-MS), Liquid Chromatography-Mass Spectrometry (LC-MS), Non-Aqueous Capillary Electrophoresis (NACE), High Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS), Pressurized Fluid Extraction (PFE), Matrix Solid-Phase Dispersion (MSPD), Gas Chromatography-Mass Spectrometry (GC-MS), Solid-Phase MicroExtraction-Gas Chromatography (SPME-GC), Enzyme Linked Immunosorbent Assay (ELISA), and MicroEmulsion ElectroKinetic Chromatography (MEEKC) are presented and commented. Several informative figures and tables are included to show the effect of conditions (temperature, time) on the AA formation. A section is also included related to AA legislation in EU and US.

A simple, rapid atmospheric pressure chemical ionization liquid chromatography tandem mass spectrometry method for the determination of 25-hydroxyvitamin D2 and D3.

PubMed

Garg, Uttam; Munar, Ada; Frazee, Clinton; Scott, David

2012-09-01

Vitamin D plays a vital role not only in bone health but also in pathophysiology of many other body functions. In recent years, there has been significant increase in testing of 25-hydroxyvitamin D (25-OH vitamin D), a marker of vitamin D deficiency. The most commonly used methods for the measurement of 25-OH vitamin D are immunoassays and liquid chromatography tandem mass spectrometry (LC-MS-MS). Since immunoassays suffer from inaccuracies and interferences, LC-MS-MS is a preferred method. In LC-MS-MS methods, 25-OH vitamin D is extracted from serum or plasma by solid-phase or liquid-phase extraction. Because these extraction methods are time consuming, we developed an easy method that uses simple protein precipitation followed by injection of the supernatant to LC-MS-MS. Several mass-to-charge (m/z) ratio transitions, including commonly used transitions based on water loss, were evaluated and several tube types were tested. The optimal transitions for 25-OH vitamin D2 and D3 were 395.5 > 269.5 and 383.4 > 257.3, respectively. The reportable range of the method was 1-100 ng/mL, and repeatability (within-run) and within-laboratory imprecision were <4% and <6%, respectively. The method agreed well with the solid-phase extraction methods. © 2012 Wiley Periodicals, Inc.

Gas pressure assisted microliquid-liquid extraction coupled online to direct infusion mass spectrometry: a new automated screening platform for bioanalysis.

PubMed

Raterink, Robert-Jan; Witkam, Yoeri; Vreeken, Rob J; Ramautar, Rawi; Hankemeier, Thomas

2014-10-21

In the field of bioanalysis, there is an increasing demand for miniaturized, automated, robust sample pretreatment procedures that can be easily connected to direct-infusion mass spectrometry (DI-MS) in order to allow the high-throughput screening of drugs and/or their metabolites in complex body fluids like plasma. Liquid-Liquid extraction (LLE) is a common sample pretreatment technique often used for complex aqueous samples in bioanalysis. Despite significant developments that have been made in automated and miniaturized LLE procedures, fully automated LLE techniques allowing high-throughput bioanalytical studies on small-volume samples using direct infusion mass spectrometry, have not been matured yet. Here, we introduce a new fully automated micro-LLE technique based on gas-pressure assisted mixing followed by passive phase separation, coupled online to nanoelectrospray-DI-MS. Our method was characterized by varying the gas flow and its duration through the solvent mixture. For evaluation of the analytical performance, four drugs were spiked to human plasma, resulting in highly acceptable precision (RSD down to 9%) and linearity (R(2) ranging from 0.990 to 0.998). We demonstrate that our new method does not only allow the reliable extraction of analytes from small sample volumes of a few microliters in an automated and high-throughput manner, but also performs comparable or better than conventional offline LLE, in which the handling of small volumes remains challenging. Finally, we demonstrate the applicability of our method for drug screening on dried blood spots showing excellent linearity (R(2) of 0.998) and precision (RSD of 9%). In conclusion, we present the proof of principe of a new high-throughput screening platform for bioanalysis based on a new automated microLLE method, coupled online to a commercially available nano-ESI-DI-MS.

Non-porous membrane-assisted liquid-liquid extraction of UV filter compounds from water samples.

PubMed

Rodil, Rosario; Schrader, Steffi; Moeder, Monika

2009-06-12

A method for the determination of nine UV filter compounds [benzophenone-3 (BP-3), isoamyl methoxycinnamate, 4-methylbenzylidene camphor, octocrylene (OC), butyl methoxydibenzoylmethane, ethylhexyl dimethyl p-aminobenzoate (OD-PABA), ethylhexyl methoxycinnamate (EHMC), ethylhexyl salicylate and homosalate] in water samples was developed and evaluated. The procedure includes non-porous membrane-assisted liquid-liquid extraction (MALLE) and LC-atmospheric pressure photoionization (APPI)-MS/MS. Membrane bags made of different polymeric materials were examined to enable a fast and simple extraction of the target analytes. Among the polymeric materials tested, low- and high-density polyethylene membranes proved to be well suited to adsorb the analytes from water samples. Finally, 2 cm length tailor-made membrane bags were prepared from low-density polyethylene in order to accommodate 100 microL of propanol. The fully optimised protocol provides recoveries from 76% to 101% and limits of detection (LOD) between 0.4 ng L(-1) (OD-PABA) and 16 ng L(-1) (EHMC). The interday repeatability of the whole protocol was below 18%. The effective separation of matrix molecules was proved by only marginal matrix influence during the APPI-MS analysis since no ion suppression effects were observed. During the extraction step, the influence of the matrix was only significant when non-treated wastewater was analysed. The analysis of lake water indicated the presence of seven UV filter compounds included in this study at concentrations between 40 ng L(-1) (BP-3) and 4381 ng L(-1) (OC). In non-treated wastewater several UV filters were also detected at concentration levels as high as 5322 ng L(-1) (OC).

Free radical scavenging of grape pomace extracts from Cabernet sauvingnon (Vitis vinifera).

PubMed

de Campos, Luanda M A S; Leimann, Fernanda V; Pedrosa, Rozangela Curi; Ferreira, Sandra R S

2008-11-01

Pressed grape pomace obtained from the wine production of Cabernet sauvignon (Vitis vinifera) vintage was dried until 9.8% moisture content, ground and submitted to extraction of soluble components from different extraction techniques. Low pressure extractions were performed with ethanol maceration followed by fractionation with n-hexane, dichloromethane, butanol and ethyl acetate. These solvents were furthermore applied for soxhlet extraction. Supercritical fluid extraction (SFE) was also performed to obtain grape pomace extracts by using pure CO2 and CO2 with ethanol as co-solvent in concentrations of 10, 15 and 20%w/w. The operating condition used in high pressure extractions was 150bar and 40 degrees C. The antioxidant activity of the grape pomace extracts was determined considering the free radical scavenging assay using 1,1-Diphenyl-2-picrylhydrazyl (DPPH) and was correlated with the total phenol content determined according to the Folin-Ciocalteu method. The results obtained in DPPH tests indicate the highest antioxidant activity of 96.6+/-0.3%AA, with an IC50 value of 13+/-1, for the extracts obtained with ethyl acetate in solid-liquid extraction. The highest yield values were achieved in soxhlet extraction with ethanol (13.2%w/w) and with butanol (12.2%w/w), and also by SFE with 15% ethanol (9.2%w/w). The lipophilic composition of grape pomace extracts was evaluated by gas chromatography-mass spectrometry with the identification of components like linoleic acid and ethyl linoleate, with important therapeutic activities.

Quantitative ionspray liquid chromatographic/tandem mass spectrometric determination of reserpine in equine plasma.

PubMed

Anderson, M A; Wachs, T; Henion, J D

1997-02-01

A method based on ionspray liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed for the determination of reserpine in equine plasma. A comparison was made of the isolation of reserpine from plasma by liquid-liquid extraction and by solid-phase extraction. A structural analog, rescinnamine, was used as the internal standard. The reconstituted extracts were analyzed by ionspray LC/MS/MS in the selected reaction monitoring (SRM) mode. The calibration graph for reserpine extracted from equine plasma obtained using liquid-liquid extraction was linear from 10 to 5000 pg ml-1 and that using solid-phase extraction from 100 to 5000 pg ml-1. The lower level of quantitation (LLQ) using liquid-liquid and solid-phase extraction was 50 and 200 pg ml-1, respectively. The lower level of detection for reserpine by LC/MS/MS was 10 pg ml-1. The intra-assay accuracy did not exceed 13% for liquid-liquid and 12% for solid-phase extraction. The recoveries for the LLQ were 68% for liquid-liquid and 58% for solid-phase extraction.

Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for semivolatile organic compounds, polycyclic aromatic hydrocarbons (PAH), and alkylated PAH homolog groups in sediment

USGS Publications Warehouse

Burkhardt, M.R.; Zaugg, S.D.; Burbank, T.L.; Olson, M.C.; Iverson, J.L.

2005-01-01

Polycyclic aromatic hydrocarbons (PAH) are recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This paper describes a method to determine the distribution of PAH and alkylated homolog groups in sediment samples. Pressurized liquid extraction (PLE), coupled with solid-phase extraction (SPE) cleanup, was developed to decrease sample preparation time, to reduce solvent consumption, and to minimize background interferences for full-scan GC-MS analysis. Recoveries from spiked Ottawa sand, environmental stream sediment, and commercially available topsoil, fortified at 1.5-15 ??g per compound, averaged 94.6 ?? 7.8%, 90.7 ?? 5.8% and 92.8 ?? 12.8%, respectively. Initial method detection limits for single-component compounds ranged from 20 to 302 ??g/kg, based on 25 g samples. Results from 28 environmental sediment samples, excluding homologs, show 35 of 41 compounds (85.4%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, 2,6-dimethylnaphthalene, was detected in 23 of the 28 (82%) environmental samples with a concentration ranging from 15 to 907 ??g/kg. The results from the 28 environmental sediment samples for the homolog series showed that 27 of 28 (96%) samples had at least one homolog series present at concentrations ranging from 20 to 89,000 ??g/kg. The most frequently detected homolog series, C2-alkylated naphthalene, was detected in 26 of the 28 (93%) environmental samples with a concentration ranging from 25 to 3900 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction also are compared. ?? 2005 Elsevier B.V. All rights reserved.

ASE extraction method for simultaneous carbon and nitrogen stable isotope analysis in soft tissues of aquatic organisms.

PubMed

Bodin, Nathalie; Budzinski, Hélène; Le Ménach, Karyn; Tapie, Nathalie

2009-06-08

Since lipids are depleted in 13C relative to proteins and carbohydrates, variations in lipid composition among species and within individuals significantly influence delta13C and may result in misleading ecological interpretations. Whereas lipid extraction before IRMS analysis constitutes a way of stable isotope result lipid-normalisation, such a procedure was given up because of the un-controlled effects of the methods used (i.e., "Bligh & Dyer", Soxhlet, etc.) on delta15N. The aim of this work was to develop a simple, rapid and efficient lipid extraction method allowing for simultaneous C and N stable isotope analysis in the biological soft tissues of aquatic organisms. The goal was to be free from the lipid influence on delta13C values without interfering with delta15N values. For that purpose, the modern automated pressurized liquid extraction technique ASE (accelerated solvent extraction) was selected. Eel muscles representative of a broad range of fat contents were extracted via ASE by using different semi-polar solvents (100% dichloromethane and 80% n-hexane/20% acetone) and by operating at different temperature (ambient temperature and 100 degrees C) and pressure (750 and 1900 psi) conditions. The results were discussed in terms of lipid extraction efficiency as well as delta13C and delta15N variability.

Improved micromethod for mezlocillin quantitation in serum and urine by high-pressure liquid chromatography.

PubMed Central

Fiore, D; Auger, F A; Drusano, G L; Dandu, V R; Lesko, L J

1984-01-01

A rapid, sensitive, and specific method of analysis for mezlocillin in serum and urine by high-pressure liquid chromatography is described. A solid-phase extraction column was used to remove interfering substances from samples before chromatography. Quantitation included the use of an internal standard, nafcillin. Mezlocillin was chromatographed with a phosphate buffer-acetonitrile (73:27) mobile phase and a C-18 reverse-phase column and detected at a wavelength of 220 nm. The assay had a sensitivity of 1.6 micrograms/ml and a linearity of up to 600 micrograms/ml and 16 mg/ml in serum and urine, respectively, with only 0.1 ml of sample. The interday and intraday coefficients of variation for replicate analyses of spiked serum and urine specimens were less than 6.5%. PMID:6517560

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

PubMed

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

2015-08-21

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

Mobility and fluorescence of barium ions in xenon gas for the exo experiment

NASA Astrophysics Data System (ADS)

Benitez Medina, Julio Cesar

The Enriched Xenon Observatory (EXO) is an experiment which aims to observe the neutrinoless double beta decay of 136Xe. The measurement of this decay would give information about the absolute neutrino mass and whether or not the neutrino is its own antiparticle. Since this is a very rare decay, the ability to reject background events by detecting the barium ion daughter from the double beta decay would be a major advantage. EXO is currently operating a detector with 200 kg of enriched liquid xenon, and there are plans to build a ton scale xenon detector. Measurements of the purity of liquid xenon in our liquid xenon test cell are reported. These results are relevant to the research on detection of single barium ions by our research group at Colorado State University. Details of the operation of the purity monitor are described. The effects of using a purifier, recirculation and laser ablation on the purity of liquid xenon are discussed. Mobility measurements of barium in xenon gas are reported for the first time. The variation of mobility with xenon gas pressure suggests that a significant fraction of molecular ions are formed when barium ions interact with xenon gas at high pressures. The measured mobility of Ba+ in Xe gas at different pressures is compared with the predicted theoretical value, and deviations are explained by a model that describes the fraction of molecular ions in Xe gas as a function of pressure. The results are useful for the analysis of experiments of fluorescence of Ba+ in xenon gas. It is also important to know the mobility of the ions in order to calculate the time they interact with an excitation laser in fluorescence experiments and in proposed 136 Ba+ daughter detection schemes. This thesis presents results of detection of laser induced fluorescence of Ba+ ions in Xe gas. Measurements of the pressure broadening of the excitation spectra of Ba+ in xenon gas are presented. Nonradiative decays due to gas collisions and optical pumping affect the number of fluorescence counts detected. A model that treats the barium ion as a three level system is used to predict the total number of fluorescence counts and correct for optical pumping. A pressure broadening coefficient for Ba+ in xenon gas is extracted and limits for p-d and d-s nonradiative decay rates are extracted. Although fluorescence is reduced significantly at 5-10 atm xenon pressure, the measurements in this thesis indicate that it is still feasible to detect 136Ba+ ions directly in high pressure xenon gas, e.g. in a double beta decay detector.

Systematic Analysis of Absorbed Anti-Inflammatory Constituents and Metabolites of Sarcandra glabra in Rat Plasma Using Ultra-High-Pressure Liquid Chromatography Coupled with Linear Trap Quadrupole Orbitrap Mass Spectrometry

PubMed Central

Li, Xiong; Zhao, Jin; Liu, Jianxing; Li, Geng; Zhao, Ya; Zeng, Xing

2016-01-01

Ultra-high-pressure liquid chromatography (UHPLC) was coupled with linear ion trap quadrupole Orbitrap mass spectrometry (LTQ-Orbitrap) and was used for the first time to systematically analyze the absorbed components and metabolites in rat plasma after oral administration of the water extract of Sarcandra glabra. This extract is a well-known Chinese herbal medicine for the treatment of inflammation and immunity related diseases. The anti-inflammatory activities of the absorbed components were evaluated by measuring nitric oxide (NO) production and proinflammatory genes expression in lipopolysaccharide (LPS)-stimulated murine RAW 264.7 macrophages. As a result, 54 components in Sarcandra glabra were detected in dosed rat plasma, and 36 of them were positively identified. Moreover, 23 metabolites were characterized and their originations were traced. Furthermore, 20 of the 24 studied components showed anti-inflammatory activities. These results provide evidence that this method efficiency detected constituents in plasma based on the anti-inflammatory mechanism of multiple components and would be a useful technique for screening multiple targets for natural medicine research. PMID:26974321

An ultra-pressure liquid chromatography-tandem mass spectrometry method for the simultaneous determination of three physalins in rat plasma and its application to pharmacokinetic study of Physalis alkekengi var. franchetii (Chinese lantern) in rats.

PubMed

Zheng, Yunliang; Chen, Yong; Ren, Yiping; Luan, Lianjun; Wu, Yongjiang

2012-01-25

An ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the quantification of three major ingredients in Chinese lantern preparations (CLP) in rat plasma. Following extraction by ethyl acetate, the analytes were separated on an Acquity UPLC BEH Shield RP C(18) column using a gradient mobile phase system of acetonitrile-water. Electrospray ionization (ESI) tandem interface was employed prior to mass spectrometric detection. The calibration curves were linear over the range of 5.0-500.0 ng/ml for physalin D, 2.3-230.0 ng/ml for physalin G and 0.71-71.0 ng/ml for 4,7-didehydroneophysalin B. The average extraction recoveries, examined at four concentration levels, carried from 57.1% to 76.9%, and the accuracies ranged from 94.0% to 113.3% with precision (RSD) <15%. The validated method was successfully applied to the determination of the three physalins in rat plasma after intragastric administration of CLP suspension. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-01-01

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

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.

Two-phase convection in the high-pressure ice layer of the large icy moons: geodynamical implications

NASA Astrophysics Data System (ADS)

Kalousova, K.; Sotin, C.; Tobie, G.; Choblet, G.; Grasset, O.

2015-12-01

The H2O layers of large icy satellites such as Ganymede, Callisto, or Titan probably include a liquid water ocean sandwiched between the deep high-pressure ice layer and the outer ice I shell [1]. It has been recently suggested that the high-pressure ice layer could be decoupled from the silicate core by a salty liquid water layer [2]. However, it is not clear whether accumulation of liquids at the bottom of the high-pressure layer is possible due to positive buoyancy of water with respect to high-pressure ice. Numerical simulation of this two-phase (i.e. ice and water) problem is challenging, which explains why very few studies have self-consistently handled the presence and transport of liquids within the solid ice [e.g. 3]. While using a simplified description of water production and transport, it was recently showed in [4] that (i) a significant fraction of the high-pressure layer reaches the melting point and (ii) the melt generation and its extraction to the overlying ocean significantly influence the global thermal evolution and interior structure of the large icy moons.Here, we treat the high-pressure ice layer as a compressible mixture of solid ice and liquid water [5]. Several aspects are investigated: (i) the effect of the water formation on the vigor of solid-state convection and its influence on the amount of heat that is transferred from the silicate mantle to the ocean; (ii) the fate of liquids within the upper thermal boundary layer - whether they freeze or reach the ocean; and (iii) the effect of salts and volatile compounds (potentially released from the rocky core) on the melting/freezing processes. Investigation of these aspects will allow us to address the thermo-chemical evolution of the internal ocean which is crucial to evaluate the astrobiological potential of large icy moons. This work has been performed at the Jet Propulsion Laboratory, California Institute of Technology, under contract to NASA. [1] Hussmann et al. (2007), Treatise of Geophysics, 10.15, 509-539. [2] Vance et al. (2014), Planet. Space Sci., 96, 62-70. [3] Kalousova et al. (2014), J. Geophys. Res. Planets, 119(3), 532-549. [4] Tobie et al. (2014), AGU, P43C-3999. [5] Soucek et al. (2014), Geophys. Astro. Fluid, 108(6), 639-666.

[Simultaneous analysis of aromatic aldehydes and coumarins with high pressure liquid chromatography. Application to wines and brandies stored in oak barrels].

PubMed

Salagoity-Auguste, M H; Tricard, C; Sudraud, P

1987-04-17

Aromatic aldehydes (vanillin, syringaldehyde, coniferaldehyde and sinapaldehyde) and coumarins (esculetin, umbelliferone, scopoletin and methylumbelliferone) are natural wood compounds. Storage of wines and brandies in oak barrels increases notably aldehydes and coumarins (particularly scopoletin) concentrations. These compounds were separated by high-performance liquid chromatography, on hydrocarbon bonded reversed-phase packings, with a water-acetonitrile elution gradient. They were first extracted from wines and brandies by diethyl ether and then injected on chromatographic column. A double detection was used to determine simultaneously aromatic aldehydes and coumarins by UV absorption and fluorescence respectively.

Simultaneous determination of calycosin-7-O-β-D-glucoside, ononin, calycosin, formononetin, astragaloside IV, and astragaloside II in rat plasma after oral administration of Radix Astragali extraction for their pharmacokinetic studies by ultra-pressure liquid chromatography with tandem mass spectrometry.

PubMed

Liu, Xiao-hua; Zhao, Jian-bang; Guo, Long; Yang, Ying-lai; Hu, Fang; Zhu, Rui-juan; Feng, Shi-lan

2014-09-01

A sensitive and reliable ultra-pressure liquid chromatography with tandem mass spectrometry (UPLC-MS) was developed and validated for simultaneous quantification of six main bioactive components, i.e., calycosin-7-O-β-D-glucoside, ononin, calycosin, formononetin, astragaloside IV, and astragaloside II in rat plasma after oral administration of the 95 % ethanol extraction from Radix Astragali. Plasma samples were extracted with Waters Oasis(TM) HLB 1 cc (30 mg) Extraction Cartridges (SPE) separated on an UPLC™ BEH C18 column and detected by MS with electro spray ionization interface in positive selective ion monitoring mode. Calibration curves offered linear ranges of two orders of magnitude with r (2) > 0.99. The method had the lower limit quantification of 1.30, 0.73, 1.17, 2.33, 0.63, and 0.83 ng/mL for ononin, calycosin, calycosin-7-O-β-D-glucoside, formononetin, astragaloside IV, and astragaloside II, respectively, with precision less than 10 %. The RSD of intra- and inter-day variations ranged from 1.66 to 6.46 and 3.39 to 6.58 %. This developed method was applied subsequently to pharmacokinetic studies of the six compounds in rats successfully. The proposed method was for the first time to compare the pharmacokinetic difference between calycosin-7-O-β-D-glucoside and calycosin in rat plasma, so as between ononin and formononetin, and studied to the astragaloside II pharmacokinetics in rat plasma.

Production and New Extraction Method of Polyketide Red Pigments Produced by Ascomycetous Fungi from Terrestrial and Marine Habitats

PubMed Central

Lebeau, Juliana; Venkatachalam, Mekala; Fouillaud, Mireille; Petit, Thomas; Vinale, Francesco; Dufossé, Laurent; Caro, Yanis

2017-01-01

The use of ascomycetous fungi as pigment producers opens the way to an alternative to synthetic dyes, especially in the red-dye industries, which have very few natural pigment alternatives. The present paper aimed to bio-prospect and screen out 15 selected ascomycetous fungal strains, originating from terrestrial and marine habitats belonging to seven different genera (Penicillium, Talaromyces, Fusarium, Aspergillus, Trichoderma, Dreschlera, and Paecilomyces). We identified four strains, Penicillium purpurogenum rubisclerotium, Fusarium oxysporum, marine strains identified as Talaromyces spp., and Trichoderma atroviride, as potential red pigment producers. The extraction of the pigments is a crucial step, whereby the qualitative and quantitative compositions of each fungal extract need to be respected for reliable identification, as well as preserving bioactivity. Furthermore, there is a growing demand for more sustainable and cost-effective extraction methods. Therefore, a pressurized liquid extraction technique was carried out in this study, allowing a greener and faster extraction step of the pigments, while preserving their chemical structures and bioactivities in comparison to conventional extraction processes. The protocol was illustrated with the production of pigment extracts from P. purpurogenum rubisclerotium and Talaromyces spp. Extracts were analyzed by high-performance liquid-chromatography combined with photodiode array-detection (HPLC-DAD) and high-resolution mass spectrometry (UHPLC-HRMS). The more promising strain was the isolate Talaromyces spp. of marine origin. The main polyketide pigment produced by this strain has been characterized as N-threoninerubropunctamine, a non-toxic red Monascus-like azaphilone pigment. PMID:29371552

Supercritical Fluid Extraction of Bacterial and Archaeal Lipid Biomarkers from Anaerobically Digested Sludge

PubMed Central

Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

2012-01-01

Supercritical fluid extraction (SFE) was used in the analysis of bacterial respiratory quinone (RQ), bacterial phospholipid fatty acid (PLFA), and archaeal phospholipid ether lipid (PLEL) from anaerobically digested sludge. Bacterial RQ were determined using ultra performance liquid chromatography (UPLC). Determination of bacterial PLFA and archaeal PLEL was simultaneously performed using gas chromatography-mass spectrometry (GC-MS). The effects of pressure, temperature, and modifier concentration on the total amounts of RQ, PLFA, and PLEL were investigated by 23 experiments with five settings chosen for each variable. The optimal extraction conditions that were obtained through a multiple-response optimization included a pressure of 23.6 MPa, temperature of 77.6 °C, and 10.6% (v/v) of methanol as the modifier. Thirty nine components of microbial lipid biomarkers were identified in the anaerobically digested sludge. Overall, the SFE method proved to be more effective, rapid, and quantitative for simultaneously extracting bacterial and archaeal lipid biomarkers, compared to conventional organic solvent extraction. This work shows the potential application of SFE as a routine method for the comprehensive analysis of microbial community structures in environmental assessments using the lipid biomarkers profile. PMID:22489140

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

PubMed

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

2012-12-15

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

Rational and Efficient Preparative Isolation of Natural Products by MPLC-UV-ELSD based on HPLC to MPLC Gradient Transfer.

PubMed

Challal, Soura; Queiroz, Emerson Ferreira; Debrus, Benjamin; Kloeti, Werner; Guillarme, Davy; Gupta, Mahabir Prashad; Wolfender, Jean-Luc

2015-11-01

In natural product research, the isolation of biomarkers or bioactive compounds from complex natural extracts represents an essential step for de novo identification and bioactivity assessment. When pure natural products have to be obtained in milligram quantities, the chromatographic steps are generally labourious and time-consuming. In this respect, an efficient method has been developed for the reversed-phase gradient transfer from high-performance liquid chromatography to medium-performance liquid chromatography for the isolation of pure natural products at the level of tens of milligrams from complex crude natural extracts. The proposed method provides a rational way to predict retention behaviour and resolution at the analytical scale prior to medium-performance liquid chromatography, and guarantees similar performances at both analytical and preparative scales. The optimisation of the high-performance liquid chromatography separation and system characterisation allows for the prediction of the gradient at the medium-performance liquid chromatography scale by using identical stationary phase chemistries. The samples were introduced in medium-performance liquid chromatography using a pressure-resistant aluminium dry load cell especially designed for this study to allow high sample loading while maintaining a maximum achievable flow rate for the separation. The method has been validated with a mixture of eight natural product standards. Ultraviolet and evaporative light scattering detections were used in parallel for a comprehensive monitoring. In addition, post-chromatographic mass spectrometry detection was provided by high-throughput ultrahigh-performance liquid chromatography time-of-flight mass spectrometry analyses of all fractions. The processing of all liquid chromatography-mass spectrometry data in the form of an medium-performance liquid chromatography x ultra high-performance liquid chromatography time-of-flight mass spectrometry matrix enabled an efficient localisation of the compounds of interest in the generated fractions. The methodology was successfully applied for the separation of three different plant extracts that contain many diverse secondary metabolites. The advantages and limitations of this approach and the theoretical chromatographic background that rules such as liquid chromatography gradient transfer are presented from a practical viewpoint. Georg Thieme Verlag KG Stuttgart · New York.

Method for co-processing waste rubber and carbonaceous material

DOEpatents

Farcasiu, Malvina; Smith, Charlene M.

1991-01-01

In a process for the co-processing of waste rubber and carbonaceous material to form a useful liquid product, the rubber and the carbonaceous material are combined and heated to the depolymerization temperature of the rubber in the presence of a source of hydrogen. The depolymerized rubber acts as a liquefying solvent for the carbonaceous material while a beneficial catalytic effect is obtained from the carbon black released on depolymerization the reinforced rubber. The reaction is carried out at liquefaction conditions of 380.degree.-600.degree. C. and 70-280 atmospheres hydrogen pressure. The resulting liquid is separated from residual solids and further processed such as by distillation or solvent extraction to provide a carbonaceous liquid useful for fuels and other purposes.

A comprehensive metabolite profiling of Isatis tinctoria leaf extracts.

PubMed

Mohn, Tobias; Plitzko, Inken; Hamburger, Matthias

2009-05-01

A broad-based characterisation of a pharmacologically active dichloromethane extract from Isatis tinctoria leaves was carried out. For a comprehensive picture we also included the polar constituents of I. tinctoria (MeOH extract) and for comparative purposes, the taxonomically closely related plant I. indigotica. Diode array detector, evaporative light scattering detector, atmospheric pressure chemical ionisation and electrospray ionisation mass spectrometry, and electrospray ionisation time-of-flight mass spectrometry detectors were used in parallel to ensure a wide coverage of secondary metabolites with highly diverging analytical properties. Off-line microprobe nuclear magnetic resonance spectroscopy after peak purification by semi-preparative high-pressure liquid chromatography served for structure elucidation of some minor constituents. More than 65 compounds belonging to various structural classes such as alkaloids, flavonoids, fatty acids, porphyrins, lignans, carotenoids, glucosinolates and cyclohexenones were unambiguously identified, and tentative structures were proposed for additional compounds. Numerous compounds were identified for the first time in the genus Isatis, and an indolic alkaloid was discovered.

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

PubMed

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

2016-12-15

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

Method and apparatus for continuous flow injection extraction analysis

DOEpatents

Hartenstein, Steven D.; Siemer, Darryl D.

1992-01-01

A method and apparatus for a continuous flow injection batch extraction aysis system is disclosed employing extraction of a component of a first liquid into a second liquid which is a solvent for a component of the first liquid, and is immiscible with the first liquid, and for separating the first liquid from the second liquid subsequent to extraction of the component of the first liquid.

40 CFR 264.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2014 CFR

2014-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief devices in light liquid...

40 CFR 264.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2011 CFR

2011-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief devices in light liquid...

40 CFR 264.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2012 CFR

2012-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief devices in light liquid...

40 CFR 264.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2013 CFR

2013-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief devices in light liquid...

Zero Gravity Cryogenic Vent System Concepts for Upper Stages

NASA Technical Reports Server (NTRS)

Flachbart, Robin H.; Holt, James B.; Hastings, Leon J.

1999-01-01

The capability to vent in zero gravity without resettling is a technology need that involves practically all uses of sub-critical cryogenics in space. Venting without resettling would extend cryogenic orbital transfer vehicle capabilities. However, the lack of definition regarding liquid/ullage orientation coupled with the somewhat random nature of the thermal stratification and resulting pressure rise rates, lead to significant technical challenges. Typically a zero gravity vent concept, termed a thermodynamic vent system (TVS), consists of a tank mixer to destratify the propellant, combined with a Joule-Thomson (J-T) valve to extract thermal energy from the propellant. Marshall Space Flight Center's (MSFC's) Multipurpose Hydrogen Test Bed (MHTB) was used to test both spray bar and axial jet TVS concepts. The axial jet system consists of a recirculation pump heat exchanger unit. The spray bar system consists of a recirculation pump, a parallel flow concentric tube, heat exchanger, and a spray bar positioned close to the longitudinal axis of the tank. The operation of both concepts is similar. In the mixing mode, the recirculation pump withdraws liquid from the tank and sprays it into the tank liquid, ullage, and exposed tank surfaces. When energy is required. a small portion of the recirculated liquid is passed sequentially through the J-T expansion valve, the heat exchanger, and is vented overboard. The vented vapor cools the circulated bulk fluid, thereby removing thermal energy and reducing tank pressure. The pump operates alone, cycling on and off, to destratify the tank liquid and ullage until the liquid vapor pressure reaches the lower set point. At that point. the J-T valve begins to cycle on and off with the pump. Thus, for short duration missions, only the mixer may operate, thus minimizing or even eliminating, boil-off losses.

Comparison of three different dispersive liquid-liquid microextraction modes performed on their most usual configurations for the extraction of phenolic, neutral aromatic, and amino compounds from waters.

PubMed

Saraji, Mohammad; Ghambari, Hoda

2018-06-21

In this work we seek clues to select the appropriate dispersive liquid-liquid microextraction mode for extracting three categories of compounds. For this purpose, three common dispersive liquid-liquid microextraction modes were compared under optimized conditions. Traditional dispersive liquid-liquid microextraction, in situ ionic liquid dispersive liquid-liquid microextraction and conventional ionic liquid dispersive liquid-liquid microextraction using chloroform, 1-butyl-3-methylimidazolium tetrafluoroborate, and 1-hexyl-3-methylimidazolium hexafluorophosphate as the extraction solvent, respectively, were considered in this work. Phenolic, neutral aromatic and amino compounds (each category included six members) were studied as analytes. The analytes in the extracts were determined by high-performance liquid chromatography with UV detection. For the analytes with polar functionalities, the in situ ionic liquid dispersive liquid-liquid microextraction mode mostly led to better results. In contrast, for neutral hydrocarbons without polar functionalities, traditional dispersive liquid-liquid microextraction using chloroform produced better results. In this case, where dispersion forces were the dominant interactions in the extraction, the refractive index of solvent and analyte predicted the extraction performance better than the octanol-water partition coefficient. It was also revealed that none of the methods were successful in extracting very hydrophilic analytes (compounds with the log octanol-water partition coefficient < 2). The results of this study could be helpful in selecting a dispersive liquid-liquid microextraction mode for the extraction of various groups of compounds. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Natural colorants: Pigment stability and extraction yield enhancement via utilization of appropriate pretreatment and extraction methods.

PubMed

Ngamwonglumlert, Luxsika; Devahastin, Sakamon; Chiewchan, Naphaporn

2017-10-13

Natural colorants from plant-based materials have gained increasing popularity due to health consciousness of consumers. Among the many steps involved in the production of natural colorants, pigment extraction is one of the most important. Soxhlet extraction, maceration, and hydrodistillation are conventional methods that have been widely used in industry and laboratory for such a purpose. Recently, various non-conventional methods, such as supercritical fluid extraction, pressurized liquid extraction, microwave-assisted extraction, ultrasound-assisted extraction, pulsed-electric field extraction, and enzyme-assisted extraction have emerged as alternatives to conventional methods due to the advantages of the former in terms of smaller solvent consumption, shorter extraction time, and more environment-friendliness. Prior to the extraction step, pretreatment of plant materials to enhance the stability of natural pigments is another important step that must be carefully taken care of. In this paper, a comprehensive review of appropriate pretreatment and extraction methods for chlorophylls, carotenoids, betalains, and anthocyanins, which are major classes of plant pigments, is provided by using pigment stability and extraction yield as assessment criteria.

Atomizing, continuous, water monitoring module

DOEpatents

Thompson, C.V.; Wise, M.B.

1997-07-08

A system for continuously analyzing volatile constituents of a liquid is described. The system contains a pump for continuously pumping the liquid to be tested at a predetermined flow rate into an extracting container through a liquid directing tube having an orifice at one end and positioned to direct the liquid into the extracting container at a flow rate sufficient to atomize the liquid within the extracting container. A continuous supply of helium carrier gas at a predetermined flow rate is directed through a tube into the extracting container and co-mingled with the atomized liquid to extract the volatile constituents contained within the atomized liquid. The helium containing the extracted volatile constituents flows out of the extracting container into a mass spectrometer for an analysis of the volatile constituents of the liquid. 3 figs.

Atomizing, continuous, water monitoring module

DOEpatents

Thompson, Cyril V.; Wise, Marcus B.

1997-01-01

A system for continuously analyzing volatile constituents of a liquid is described. The system contains a pump for continuously pumping the liquid to be tested at a predetermined flow rate into an extracting container through a liquid directing tube having an orifice at one end and positioned to direct the liquid into the extracting container at a flow rate sufficient to atomize the liquid within the extracting container. A continuous supply of helium carrier gas at a predetermined flow rate is directed through a tube into the extracting container and co-mingled with the atomized liquid to extract the volatile constituents contained within the atomized liquid. The helium containing the extracted volatile constituents flows out of the extracting container into a mass spectrometer for an analysis of the volatile constituents of the liquid.

40 CFR 63.1010 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2012 CFR

2012-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

40 CFR 63.1010 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2014 CFR

2014-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

40 CFR 63.1010 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2013 CFR

2013-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

40 CFR 63.1010 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2010 CFR

2010-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

NMR-Based Metabolomic Study on Isatis tinctoria: Comparison of Different Accessions, Harvesting Dates, and the Effect of Repeated Harvesting.

PubMed

Guldbrandsen, Niels; Kostidis, Sarantos; Schäfer, Hartmut; De Mieri, Maria; Spraul, Manfred; Skaltsounis, Alexios-Leandros; Mikros, Emmanuel; Hamburger, Matthias

2015-05-22

Isatis tinctoria is an ancient dye and medicinal plant with potent anti-inflammatory and antiallergic properties. Metabolic differences were investigated by NMR spectroscopy of accessions from different origins that were grown under identical conditions on experimental plots. For these accessions, metabolite profiles at different harvesting dates were analyzed, and single and repeatedly harvested plants were compared. Leaf samples were shock-frozen in liquid N2 immediately after being harvested, freeze-dried, and cryomilled prior to extraction. Extracts were prepared by pressurized liquid extraction with ethyl acetate and 70% aqueous methanol. NMR spectra were analyzed using a combination of different methods of multivariate data analysis such as principal component analysis (PCA), canonical analysis (CA), and k-nearest neighbor concept (k-NN). Accessions and harvesting dates were well separated in the PCA/CA/k-NN analysis in both extracts. Pairwise statistical total correlation spectroscopy (STOCSY) revealed unsaturated fatty acids, porphyrins, carbohydrates, indole derivatives, isoprenoids, phenylpropanoids, and minor aromatic compounds as the cause of these differences. In addition, the metabolite profile was affected by the repeated harvest regime, causing a decrease of 1,5-anhydroglucitol, sucrose, unsaturated fatty acids, porphyrins, isoprenoids, and a flavonoid.

Sensitive determination of RDX, nitroso-RDX metabolites, and other munitions in ground water by solid-phase extraction and isotope dilution liquid chromatography-atmospheric pressure electro-spray [correction of chemical] ionization mass spectrometry.

PubMed

Cassada, D A; Monson, S J; Snow, D D; Spalding, R F

1999-06-04

Recent improvements in the LC-MS interface have increased the sensitivity and selectivity of this instrument in the analysis of polar and thermally-labile aqueous constituents. Determination of RDX, nitroso-RDX metabolites, and other munitions was enhanced using LC-MS with solid-phase extraction, 15N3-RDX internal standard, and electrospray ionization (ESI) in negative ion mode. ESI produced a five-fold increase in detector response over atmospheric pressure chemical ionization (APCI) for the nitramine compounds, while the more energetic APCI produced more than twenty times the ESI response for nitroaromatics. Method detection limits in ESI for nitramines varied from 0.03 microgram l-1 for MNX to 0.05 microgram l-1 for RDX.

Fast and selective pressurized liquid extraction with simultaneous in cell clean up for the analysis of alkylphenols and bisphenol A in bivalve molluscs.

PubMed

Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzoa, S; López-Mahía, P; Prada-Rodríguez, D

2012-12-28

A novel and green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol technical mixture) and bisphenol A in bivalve mollusc samples was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography–electrospray ionization tandem mass spectrometry in negative mode (LC–ESI-MS/MS). Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 80 and 107% and repeatability and intermediate precision were <20% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.34 (4-n-octylphenol) and 3.6 ng g(−1) dry weight (nonylphenol). The main advantages of the method are sensitivity, selectivity, automaticity, low volumes of solvents required and low sample analysis time (according with the principles of Green Chemistry). The method was applied to the analysis of mussel samples of Galicia coast (NW of Spain). Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 9.3 and 372 ng g(−1) dw. As an approach, the human daily intake of these compounds was estimated and no risk for human health was found.

Method of manipulating the chemical properties of water to improve the effectiveness of a desired chemical process

DOEpatents

Hawthorne, Steven B.; Miller, David J.; Yang, Yu; Lagadec, Arnaud Jean-Marie

1999-01-01

The method of the present invention is adapted to manipulate the chemical properties of water in order to improve the effectiveness of a desired chemical process. The method involves heating the water in the vessel to subcritical temperatures between 100.degree. to 374.degree. C. while maintaining sufficient pressure to the water to maintain the water in the liquid state. Various physiochemical properties of the water can be manipulated including polarity, solute solubility, surface tension, viscosity, and the disassociation constant. The method of the present invention has various uses including extracting organics from solids and semisolids such as soil, selectively extracting desired organics from nonaqueous liquids, selectively separating organics using sorbent phases, enhancing reactions by controlling the disassociation constant of water, cleaning waste water, and removing organics from water using activated carbon or other suitable sorbents.

Method of manipulating the chemical properties of water to improve the effectiveness of a desired process

DOEpatents

Hawthorne, Steven B.; Miller, David J.; Lagadec, Arnaud Jean-Marie; Hammond, Peter James; Clifford, Anthony Alan

2002-01-01

The method of the present invention is adapted to manipulate the chemical properties of water in order to improve the effectiveness of a desired process. The method involves heating the water in the vessel to subcritical temperatures between 100.degree. to 374.degree. C. while maintaining sufficient pressure to the water to maintain the water in the liquid state. Various physiochemical properties of the water can be manipulated including polarity, solute solubility, surface tension, viscosity, and the disassociation constant. The method of the present invention has various uses including extracting organics from solids and semisolids such as soil, selectively extracting desired organics from liquids, selectively separating organics using sorbent phases, enhancing reactions by controlling the disassociation constant of water, cleaning waste water, removing organics from water using activated carbon or other suitable sorbents, and degrading various compounds.

Bio-oil production from biomass via supercritical fluid extraction

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

Durak, Halil, E-mail: halildurak@yyu.edu.tr

2016-04-18

Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds weremore » identified by GC-MS obtained in acetone and ethanol respectively.« less

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

PubMed

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

2011-01-01

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

Liquid chromatography-mass spectrometry-based quantification of steroidal glycoalkaloids from Solanum xanthocarpum and effect of different extraction methods on their content.

PubMed

Paul, Atish T; Vir, Sanjay; Bhutani, K K

2008-10-24

A new liquid chromatography-mass spectrometry (LC-MS)-based method coupled with pressurized liquid extraction (PLE) as an efficient sample preparation technique has been developed for the quantification and fingerprint analysis of Solanum xanthocarpum. Optimum separations of the samples were achieved on a Waters MSC-18 XTerra column, using 0.5% (v/v) formic acid in water (A) and acetonitrile (ACN):2-propanol:formic acid (94.5:5:0.5, v/v/v) (B) as mobile phase. The separation was carried out using linear gradient elution with a flow rate of 1.0mL/min. The gradient was: 0min, 20% B; 14min, 30% B; 20min, 30% B; 27min, 60% B and the column was re-equilibrated to the initial condition (20% B) for 10min prior to next injection. The steroidal glycoalkaloids (SGAs) which are the major active constituents were isolated as pure compounds from the crude methanolic extract of S. xanthocarpum by preparative LC-MS and after characterization were used as external standards for the development and validation of the method. Extracts prepared by conventional Soxhlet extraction, PLE and ultrasonication were used for analysis. The method was validated for repeatability, precision (intra- and inter-day variation), accuracy (recovery) and sensitivity (limit of detection and limit of quantitation). The purpose of the work was to develop a validated method, which can be used for the quantification of SGAs in commercialized S. xanthocarpum products and the fingerprint analysis for their routine quality control.

40 CFR 265.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2011 CFR

2011-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief...

40 CFR 265.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2012 CFR

2012-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief...

40 CFR 265.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2013 CFR

2013-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief...

40 CFR 265.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2014 CFR

2014-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other connectors. (a) Pumps and valves in heavy liquid service, pressure relief...

Liquid chromatography-negative ion atmospheric pressure photoionization tandem mass spectrometry for the determination of brominated flame retardants in environmental water and industrial effluents.

PubMed

Bacaloni, Alessandro; Callipo, Luciano; Corradini, Eleonora; Giansanti, Piero; Gubbiotti, Riccardo; Samperi, Roberto; Laganà, Aldo

2009-09-04

We describe the development of a liquid chromatography with negative-ion atmospheric pressure photoionization tandem mass spectrometric (LC/NI-APPI/MS/MS) method for the simultaneous determination of tetrabromobisphenol A (TBBP-A) and five polybrominated diphenyl ethers (BDE-47, BDE-99, BDE-100, BDE-153 and BDE-154) in water. A mobile phase methanol/acetone/water was used, where acetone acts also as dopant. NI-APPI produced precursor ions corresponding to [M-H](-) for TBBP-A, [M-Br+O](-), and [M-2Br+O](-) for the BDE congeners studied. Each compound was quantified operating in multiple reaction monitoring mode. Linearity was observed in the range 0.025-10 ng injected for all compounds. Coefficients of determination R(2) ranged from 0.9934 to 0.9982. BDEs were poorly retained by solid-phase extraction (SPE) from river water and sewage treatment plant effluent, thus liquid-liquid extraction (LLE) by n-hexane should be used for these samples. The recoveries of TBBP-A and PBDEs from tap water (SPE), river water and industrial wastewater (LLE) were in the range of 81-88%, 78-92%, and 43-99%, respectively, with relative standard deviations below 17%. The limits of detection, based on signal-to-noise ratio of 3, ranged from 0.004 to 0.1 ng injected, and method quantification limits were 0.2-3.3 ng L(-1) but BDE47 (20.3 ng L(-1)). Only TBBP-A was found in a treated industrial sewage at 4 ng L(-1), while BDE-99 and BDE-100 were detected on suspended solids.

Determination of parts per trillion levels of organophosphorus pesticides in groundwater by automated on-line liquid-solid extraction followed by liquid chromatography/atmospheric pressure chemical ionization mass spectrometry using positive and negative ion modes of operation.

PubMed

Lacorte, S; Barceló, D

1996-08-01

Liquid chromatography/atmospheric pressure chemical ionization mass spectrometry with positive and negative ion modes of operations was used for the trace determination of several organophosphorus pesticides, (E)- and (Z)-mevinphos, dichlorvos, azinphos-methyl, azinphosethyl, parathion-methyl, parathion-ethyl, malathion, fenitrothion, fenthion, chlorfenvinphos, and diazinon, in groundwater. This method required only 100 mL of water, and it was combined with a prior automated online liquid-solid extraction step using an OSP-2 autosampler containing C18 cartridges. The limit of quantitation (LOQ) varied between 5 and 37 ng/L in positive ion (PI) mode. Under negative ion (NI) mode of operation, only the parathion group (both parathions and fenitrothion) had a better sensitivity as compared to that in PI mode, with a LOQ of 5-15 ng/L, whereas the rest of pesticides had 2-4 times higher LOQs as compared to those in PI mode. Selected ion monitoring of the group-specific fragment of the organophosphorus pesticides, e.g., [(CH3O)2PO2]- or the [M + H]+ ions, under NI or PI mode, respectively, was used. Sample cone voltage varied from 10 to 130 V. This parameter influenced the transmission and fragmentation of quasi-molecular ions, and it was optimized to achieve identification capabilities with the highest sensitivity. At 20 V, good fragmentation was obtained for most of the studied analytes. The system was used for the certification of a groundwater sample spiked at the nanograms per liter level with organophosphorus pesticides provided by Aquachek.

Wipe selection for the analysis of surface materials containing chemical warfare agent nitrogen mustard degradation products by ultra-high pressure liquid chromatography-tandem mass spectrometry.

PubMed

Willison, Stuart A

2012-12-28

Degradation products arising from nitrogen mustard chemical warfare agent were deposited on common urban surfaces and determined via surface wiping, wipe extraction, and liquid chromatography–tandem mass spectrometry detection. Wipes investigated included cotton gauze, glass fiber filter, non-woven polyester fiber and filter paper, and surfaces included several porous (vinyl tile, painted drywall, wood) and mostly non-porous (laminate, galvanized steel, glass) surfaces. Wipe extracts were analyzed by ultra-high pressure liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) and compared with high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) results. An evaluation of both techniques suggests UPLC–MS/MS provides a quick and sensitive analysis of targeted degradation products in addition to being nearly four times faster than a single HPLC run, allowing for greater throughput during a wide-spread release concerning large-scale contamination and subsequent remediation events. Based on the overall performance of all tested wipes, filter paper wipes were selected over other wipes because they did not contain interferences or native species (TEA and DEA) associated with the target analytes, resulting in high percent recoveries and low background levels during sample analysis. Other wipes, including cotton gauze, would require a pre-cleaning step due to the presence of large quantities of native species or interferences of the targeted analytes. Percent recoveries obtained from a laminate surface were 47–99% for all nitrogen mustard degradation products. The resulting detection limits achieved from wipes were 0.2 ng/cm(2) for triethanolamine (TEA), 0.03 ng/cm(2) for N-ethyldiethanolamine (EDEA), 0.1 ng/cm(2) for N-methyldiethanolamine (MDEA), and 0.1 ng/cm(2) for diethanolamine (DEA).

L-Phenylalanine and L-tyrosine catabolism by selected Streptomyces species

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

Pometto, A.L. III; Crawford, D.L.

L-Phenylalanine and L-tyrosine were completely catabolized through homogentisate by Streptomyces setonii 75Vi2 but only partially degraded by Streptomyces badius 252, Streptomyces sioyaensis P5, Streptomyces viridosporus T7A, and Streptomyces sp. strain V7. Intermediates of catabolism were confirmed by the thin-layer, gas, and high-pressure liquid chromatography. Homogentisate 1,2-dioxygenase was present in all cell extracts.

L-Phenylalanine and L-tyrosine catabolism by selected Streptomyces species.

PubMed Central

Pometto, A L; Crawford, D L

1985-01-01

L-Phenylalanine and L-tyrosine were completely catabolized through homogentisate by Streptomyces setonii 75Vi2 but only partially degraded by Streptomyces badius 252, Streptomyces sioyaensis P5, Streptomyces viridosporus T7A, and Streptomyces sp. strain V7. Intermediates of catabolism were confirmed by thin-layer, gas, and high-pressure liquid chromatography. Homogentisate 1,2-dioxygenase was present in all cell extracts. PMID:3994376

40 CFR 63.1029 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2014 CFR

2014-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... in heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

40 CFR 63.1029 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2011 CFR

2011-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... in heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

40 CFR 63.1029 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2013 CFR

2013-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... in heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

40 CFR 63.1029 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2012 CFR

2012-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... in heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

40 CFR 63.1029 - Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief devices in...

Code of Federal Regulations, 2010 CFR

2010-07-01

... agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation systems..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and... in heavy liquid service; pressure relief devices in light liquid or heavy liquid service; and...

Fischer-Tropsch synthesis in near-critical n-hexane: Pressure-tuning effects

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

Bochniak, D.J.; Subramaniam, B.

For Fe-catalyzed Fischer-Tropsch (FT) synthesis with near-critical n-hexane (P{sub c} = 29.7 bar; T{sub c} = 233.7 C) as the reaction medium, isothermal pressure tuning from 1.2--2.4 P{sub c} (for n-hexane) at the reaction temperature (240 C) significantly changes syngas conversion and product selectivity. For fixed feed rates of syngas (H{sub 2}/CO = 0.5; 50 std. cm{sup 3}/g catalyst) and n-hexane (1 mL/min), syngas conversion attains a steady state at all pressures, increasing roughly threefold in this pressure range. Effective rate constants, estimated assuming a first-order dependence of syngas conversion on hydrogen, reveal that the catalyst effectiveness increases with pressuremore » implying the alleviation of pore-diffusion limitations. Pore accessibilities increase at higher pressures because the extraction of heavier hydrocarbons from the catalyst pores is enhanced by the liquid-like densities, yet better-than-liquid transport properties, of n-hexane. This explanation is consistent with the single {alpha} (= 0.78) Anderson-Schulz-Flory product distribution, the constant chain termination probability, and the higher primary product (1-olefin) selectivities ({approximately}80%) observed at the higher pressures. Results indicate that the pressure tunability of the density and transport properties of near-critical reaction media offers a powerful tool to optimize catalyst activity and product selectivity during FT reactions on supported catalysts.« less

A Study on Micropipetting Detection Technology of Automatic Enzyme Immunoassay Analyzer.

PubMed

Shang, Zhiwu; Zhou, Xiangping; Li, Cheng; Tsai, Sang-Bing

2018-04-10

In order to improve the accuracy and reliability of micropipetting, a method of micro-pipette detection and calibration combining the dynamic pressure monitoring in pipetting process and quantitative identification of pipette volume in image processing was proposed. Firstly, the normalized pressure model for the pipetting process was established with the kinematic model of the pipetting operation, and the pressure model is corrected by the experimental method. Through the pipetting process pressure and pressure of the first derivative of real-time monitoring, the use of segmentation of the double threshold method as pipetting fault evaluation criteria, and the pressure sensor data are processed by Kalman filtering, the accuracy of fault diagnosis is improved. When there is a fault, the pipette tip image is collected through the camera, extract the boundary of the liquid region by the background contrast method, and obtain the liquid volume in the tip according to the geometric characteristics of the pipette tip. The pipette deviation feedback to the automatic pipetting module and deviation correction is carried out. The titration test results show that the combination of the segmented pipetting kinematic model of the double threshold method of pressure monitoring, can effectively real-time judgment and classification of the pipette fault. The method of closed-loop adjustment of pipetting volume can effectively improve the accuracy and reliability of the pipetting system.

Critical Evaluation of Soil Pore Water Extraction Methods on a Natural Soil

NASA Astrophysics Data System (ADS)

Orlowski, Natalie; Pratt, Dyan; Breuer, Lutz; McDonnell, Jeffrey

2017-04-01

Soil pore water extraction is an important component in ecohydrological studies for the measurement of δ2H and δ18O. The effect of pore water extraction technique on resultant isotopic signature is poorly understood. Here we present results of an intercomparison of commonly applied lab-based soil water extraction techniques on a natural soil: high pressure mechanical squeezing, centrifugation, direct vapor equilibration, microwave extraction, and two types of cryogenic extraction systems. We applied these extraction methods to a natural summer-dry (gravimetric water contents ranging from 8% to 15%) glacio-lacustrine, moderately fine textured clayey soil; excavated in 10 cm sampling increments to a depth of 1 meter. Isotope results were analyzed via OA-ICOS and compared for each extraction technique that produced liquid water. From our previous intercomparison study among the same extraction techniques but with standard soils, we discovered that extraction methods are not comparable. We therefore tested the null hypothesis that all extraction techniques would be able to replicate the natural evaporation front in a comparable manner occurring in a summer-dry soil. Our results showed that the extraction technique utilized had a significant effect on the soil water isotopic composition. High pressure mechanical squeezing and vapor equilibration techniques produced similar results with similarly sloped evaporation lines. Due to the nature of soil properties and dryness, centrifugation was unsuccessful in obtaining pore water for isotopic analysis. Cryogenic extraction on both tested techniques produced similar results to each other on a similar sloping evaporation line, but dissimilar with depth.

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.

Influence of Extraction Methods on the Yield of Steviol Glycosides and Antioxidants in Stevia rebaudiana Extracts.

PubMed

Periche, Angela; Castelló, Maria Luisa; Heredia, Ana; Escriche, Isabel

2015-06-01

This study evaluated the application of ultrasound techniques and microwave energy, compared to conventional extraction methods (high temperatures at atmospheric pressure), for the solid-liquid extraction of steviol glycosides (sweeteners) and antioxidants (total phenols, flavonoids and antioxidant capacity) from dehydrated Stevia leaves. Different temperatures (from 50 to 100 °C), times (from 1 to 40 min) and microwave powers (1.98 and 3.30 W/g extract) were used. There was a great difference in the resulting yields according to the treatments applied. Steviol glycosides and antioxidants were negatively correlated; therefore, there is no single treatment suitable for obtaining the highest yield in both groups of compounds simultaneously. The greatest yield of steviol glycosides was obtained with microwave energy (3.30 W/g extract, 2 min), whereas, the conventional method (90 °C, 1 min) was the most suitable for antioxidant extraction. Consequently, the best process depends on the subsequent use (sweetener or antioxidant) of the aqueous extract of Stevia leaves.

Integrated utilization of red radish seeds for the efficient production of seed oil and sulforaphene.

PubMed

Zhang, Jie; Zhou, Xing; Fu, Min

2016-02-01

Supercritical CO2 was used to obtain seed oil from red radish seeds. The influence of pressure, temperature, CO2 flow rate and time on extraction yield of oil were investigated in detail. The maximum extraction yield of oil was 92.07 ± 0.76% at the optimal extraction conditions. The physicochemical properties and fatty acid composition of oil indicated that the seed oil can be used as a dietary oil. Meanwhile, the high purity sulforaphene (96.84 ± 0.17%) was separated by solvent extraction coupled with preparative high performance liquid chromatography from red radish seed meal. The initial pH, R, extraction temperature and extraction time for each cycle had a considerable influence both on the extraction yield and purity of sulforaphene of crude product. The extraction of oil was directly responsible for an increase of 18.32% in the yield of sulforaphene. Copyright © 2015 Elsevier Ltd. All rights reserved.

40 CFR 60.482-8a - Standards: Pumps, valves, and connectors in heavy liquid service and pressure relief devices in...

Code of Federal Regulations, 2012 CFR

2012-07-01

... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. 60... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. (a... at pumps, valves, and connectors in heavy liquid service and pressure relief devices in light liquid...

40 CFR 60.482-8a - Standards: Pumps, valves, and connectors in heavy liquid service and pressure relief devices in...

Code of Federal Regulations, 2013 CFR

2013-07-01

... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. 60... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. (a... at pumps, valves, and connectors in heavy liquid service and pressure relief devices in light liquid...

40 CFR 60.482-8 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2014 CFR

2014-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and connectors. 60.482-8... Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid... any other detection method at pumps and valves in heavy liquid service, pressure relief devices in...

40 CFR 60.482-8 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2013 CFR

2013-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and connectors. 60.482-8... Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid... any other detection method at pumps and valves in heavy liquid service, pressure relief devices in...

40 CFR 60.482-8a - Standards: Pumps, valves, and connectors in heavy liquid service and pressure relief devices in...

Code of Federal Regulations, 2011 CFR

2011-07-01

... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. 60... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. (a... at pumps, valves, and connectors in heavy liquid service and pressure relief devices in light liquid...

40 CFR 60.482-8 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2012 CFR

2012-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and connectors. 60.482-8... Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid... any other detection method at pumps and valves in heavy liquid service, pressure relief devices in...

40 CFR 60.482-8a - Standards: Pumps, valves, and connectors in heavy liquid service and pressure relief devices in...

Code of Federal Regulations, 2014 CFR

2014-07-01

... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. 60... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. (a... at pumps, valves, and connectors in heavy liquid service and pressure relief devices in light liquid...

40 CFR 60.482-8 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2011 CFR

2011-07-01

... liquid service, pressure relief devices in light liquid or heavy liquid service, and connectors. 60.482-8... Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid... any other detection method at pumps and valves in heavy liquid service, pressure relief devices in...

40 CFR 60.482-8a - Standards: Pumps, valves, and connectors in heavy liquid service and pressure relief devices in...

Code of Federal Regulations, 2010 CFR

2010-07-01

... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. 60... connectors in heavy liquid service and pressure relief devices in light liquid or heavy liquid service. (a... at pumps, valves, and connectors in heavy liquid service and pressure relief devices in light liquid...

Rapid Characterization and Identification of Flavonoids in Radix Astragali by Ultra-High-Pressure Liquid Chromatography Coupled with Linear Ion Trap-Orbitrap Mass Spectrometry.

PubMed

Zhang, Jing; Xu, Xiao-Jie; Xu, Wen; Huang, Juan; Zhu, Da-yuan; Qiu, Xiao-Hui

2015-07-01

A simple and effective method was established for separation and characterization of flavonoid constituents in Radix Astragali (RA) by combination of ultra-high-pressure liquid chromatography with LTQ-Orbitrap tandem mass spectrometry (u-HPLC-LTQ-Orbitrap-MS(n)). For three major structural types of flavonoids, the proposed fragmentation pathways and major diagnostic fragment ions of isoflavones, pterocarpans and isoflavans were investigated to trace isoflavonoid derivatives in crude plant extracts. Based on the systematic identification strategy, 48 constituents were rapidly detected and characterized or tentatively identified, many of which were first reported in RA. The u-PHLC-LTQ-Orbitrap MS(n) platform was proved as an effective tool for rapid qualitative analysis of secondary metabolite productions from natural resources. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

PREPARATIVE ISOLATION AND PURIFICATION OF CHEMICAL CONSTITUENTS OF BELAMCANDA BY MPLC, HSCCC AND PREP-HPLC

PubMed Central

Wang, Xiaohong; Liang, Yong; Peng, Cuilin; Xie, Huichun; Pan, Man; Zhang, Tianyou; Ito, Yoichiro

2010-01-01

Combined with medium-pressure liquid chromatography (MPLC) and preparative high-pressure liquid chromatography (Prep-HPLC), high-speed countercurrent chromatography (HSCCC) was successfully applied for separation and purification of isoflavonoids from the extract of belamcanda. HSCCC separation was performed on a two-phase solvent system composed of methyl tert-butyl ether -ethyl acetate - n-butyl alcohol – acetonitrile −0.1% aqueous trifluoroacetic acid at a volume radio of 1:2:1:1:5. Semi-purified peak fractions from HSCCC separation were further purified by Prep-HPLC. Nine well-separated fractions were analyzed by HPLC-UV absorption spectrometry to determine their purities and characterized with ESI-MSn. Except for peaksland VII (unknown) seven compounds were identified as apocynin (peak II), mangiferin (peak III), 7-O-methylmangiferin (peak IV), hispidulin (peak V), 3′-hydroxyltectoridin (peak VI), iristectorin B (peak VII), isoiridin (peak IX). PMID:21552369

Neutral Fragment Filtering for Rapid Identification of New Diester-Diterpenoid Alkaloids in Roots of Aconitum carmichaeli by Ultra-High-Pressure Liquid Chromatography Coupled with Linear Ion Trap-Orbitrap Mass Spectrometry

PubMed Central

Qiu, Xiao Hui; Yang, Yi Ming; Zhu, Da Yuan; Xu, Wen

2012-01-01

A rapid and effective method was developed for separation and identification of diester-diterpenoid alkaloids (DDA) in the roots of Aconitum carmichaeli by ultra-high-pressure liquid chromatography coupled with high resolution LTQ-Orbitrap tandem mass spectrometry (UHPLC-LTQ-Orbitrap-MSn). According to accurate mass measurement and the characteristic neutral loss filtering strategy, a total of 42 diester-diterpenoid alkaloids (DDA) were rapidly detected and characterized or tentatively identified. Meanwhile, the proposed fragmentation pathways and the major diagnostic fragment ions of aconitine, mesaconitine and hypaconitine were investigated to trace DDA derivatives in crude plant extracts. 23 potential new compounds were successfully screened and characterized in Aconitum carmichaeli, including 16 short chain fatty acyls DDA, 4 N-dealkyl DDA and several isomers of aconitine, mesaconitine and hypaconitine. PMID:23285005

40 CFR 65.110 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief...

Code of Federal Regulations, 2011 CFR

2011-07-01

..., and agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and..., valves, connectors, and agitators in heavy liquid service; pressure relief devices in light liquid or...

40 CFR 65.110 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief...

Code of Federal Regulations, 2013 CFR

2013-07-01

..., and agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and..., valves, connectors, and agitators in heavy liquid service; pressure relief devices in light liquid or...

40 CFR 65.110 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief...

Code of Federal Regulations, 2014 CFR

2014-07-01

..., and agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and..., valves, connectors, and agitators in heavy liquid service; pressure relief devices in light liquid or...

40 CFR 65.110 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief...

Code of Federal Regulations, 2012 CFR

2012-07-01

..., and agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and..., valves, connectors, and agitators in heavy liquid service; pressure relief devices in light liquid or...

40 CFR 65.110 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; pressure relief...

Code of Federal Regulations, 2010 CFR

2010-07-01

..., and agitators in heavy liquid service; pressure relief devices in liquid service; and instrumentation..., connectors, and agitators in heavy liquid service; pressure relief devices in liquid service; and..., valves, connectors, and agitators in heavy liquid service; pressure relief devices in light liquid or...

Structural Characterisation of Acetogenins from Annona muricata by Supercritical Fluid Chromatography Coupled to High-Resolution Tandem Mass Spectrometry.

PubMed

Laboureur, Laurent; Bonneau, Natacha; Champy, Pierre; Brunelle, Alain; Touboul, David

2017-11-01

Acetogenins are plant polyketides known to be cytotoxic and proposed as antitumor candidates. They are also suspected to be alimentary neurotoxins. Their occurrence as complex mixtures renders their dereplication and structural identification difficult using liquid chromatography coupled to tandem mass spectrometry and efforts are required to improve the methodology. To develop a supercritical fluid chromatography (SFC) high-resolution tandem mass spectrometry method, involving lithium post-column cationisation, for the structural characterisation of Annonaceous acetogenins in crude extracts. The seeds of Annona muricata L. were extracted with methanol. Supercritical fluid chromatography of the extract, using a 2-ethylpyridine stationary phase column, was monitored using a high-resolution quadrupole time-of-flight mass spectrometer. Lithium iodide was added post-column in the make-up solvent. For comparison, the same extract was analysed using high-pressure liquid chromatography coupled to the same mass spectrometer, with a column based on solid core particles. Sensitivity was similar for both HPLC and SFC approaches. Retention behaviour and fragmentation pathways of three different isomer groups are described. A previously unknown group of acetogenins was also evidenced for the first time. The use of SFC-MS/MS allows the reduction of the time of analysis, of environmental impact and an increase in the chromatographic resolution, compared to liquid chromatography. This new methodology enlightened a new group of acetogenins, isomers of montanacin-D. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Comparative Evaluation of Different Cell Lysis and Extraction Methods for Studying Benzo(a)pyrene Metabolism in HT-29 Colon Cancer Cell Cultures

PubMed Central

Myers, Jeremy N.; Rekhadevi, Perumalla V.; Ramesh, Aramandla

2011-01-01

Lysis and extraction of cells are essential sample processing steps for investigations pertaining to metabolism of xenobiotics in cell culture studies. Of particular importance to these procedures are maintaining high lysis efficiency and analyte integrity as they influence the qualitative and quantitative distribution of drug and toxicant metabolites in the intra- and extracellular milieus. In this study we have compared the efficiency of different procedures viz. homogenization, sonication, bead beating, and molecular grinding resin treatment for disruption of HT-29 colon cells exposed to benzo(a)pyrene (BaP), a polycyclic aromatic hydrocarbon (PAH) compound and a suspected colon carcinogen. Also, we have evaluated the efficiency of various procedures for extracting BaP parent compound/metabolites from colon cells and culture media prior to High Performance Liquid Chromatography (HPLC) analyses. The extraction procedures include solid phase extraction, solid-supported liquid- liquid extraction, liquid-liquid extraction, and homogeneous liquid- liquid extraction. Our findings showed that bead-beating in combination with detergent treatment of cell pellet coupled with liquid-liquid extraction yielded greater concentrations of BaP metabolites compared to the other methods employed. Our method optimization strategy revealed that disruption of HT-29 colon cells by a combination of mechanical and chemical lysis followed by liquid-liquid extraction is efficient and robust enough for analyzing BaP metabolites from cell culture studies. PMID:21865728

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

Pressurized liquid extraction-gas chromatography-mass spectrometry for confirming the photo-induced generation of dioxin-like derivatives and other cosmetic preservative photoproducts on artificial skin.

PubMed

Alvarez-Rivera, Gerardo; Llompart, Maria; Garcia-Jares, Carmen; Lores, Marta

2016-04-01

The stability and photochemical transformations of cosmetic preservatives in topical applications exposed to UV-light is a serious but poorly understood problem. In this study, a high throughput extraction and selective method based on pressurized liquid extraction (PLE) coupled to gas chromatography-mass spectrometry (GC-MS) was validated and applied to investigate the photochemical transformation of the antioxidant butylated hydroxytoluene (BHT), as well as the antimicrobials triclosan (TCS) and phenyl benzoate (PhBz) in an artificial skin model. Two sets of photodegradation experiments were performed: (i) UV-Irradiation (8W, 254nm) of artificial skin directly spiked with the target preservatives, and (ii) UV-irradiation of artificial skin after the application of a cosmetic cream fortified with the target compounds. After irradiation, PLE was used to isolate the target preservatives and their transformation products. The follow-up of the photodegradation kinetics of the parent preservatives, the identification of the arising by-products, and the monitorization of their kinetic profiles was performed by GC-MS. The photochemical transformation of triclosan into 2,8-dichloro-dibenzo-p-dioxin (2,8-DCDD) and other dioxin-like photoproducts has been confirmed in this work. Furthermore, seven BHT photoproducts, and three benzophenones as PhBz by-products, have been also identified. These findings reveal the first evidences of cosmetic ingredients phototransformation into unwanted photoproducts on an artificial skin model. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Can matrix solid phase dispersion (MSPD) be more simplified? Application of solventless MSPD sample preparation method for GC-MS and GC-FID analysis of plant essential oil components.

PubMed

Wianowska, Dorota; Dawidowicz, Andrzej L

2016-05-01

This paper proposes and shows the analytical capabilities of a new variant of matrix solid phase dispersion (MSPD) with the solventless blending step in the chromatographic analysis of plant volatiles. The obtained results prove that the use of a solvent is redundant as the sorption ability of the octadecyl brush is sufficient for quantitative retention of volatiles from 9 plants differing in their essential oil composition. The extraction efficiency of the proposed simplified MSPD method is equivalent to the efficiency of the commonly applied variant of MSPD with the organic dispersing liquid and pressurized liquid extraction, which is a much more complex, technically advanced and highly efficient technique of plant extraction. The equivalency of these methods is confirmed by the variance analysis. The proposed solventless MSPD method is precise, accurate, and reproducible. The recovery of essential oil components estimated by the MSPD method exceeds 98%, which is satisfactory for analytical purposes. Copyright © 2016 Elsevier B.V. All rights reserved.

Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

USGS Publications Warehouse

Ferrer, I.; Furlong, E.T.

2002-01-01

Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

The high-performance liquid chromatography/multistage electrospray mass spectrometric investigation and extraction optimization of beech (Fagus sylvatica L.) bark polyphenols.

PubMed

Hofmann, Tamás; Nebehaj, Esztella; Albert, Levente

2015-05-08

The aim of the present work was the high-performance liquid chromatographic separation and multistage mass spectrometric characterization of the polyphenolic compounds of beech bark, as well as the extraction optimization of the identified compounds. Beech is a common and widely used material in the wood industry, yet its bark is regarded as a by-product. Using appropriate extraction methods these compounds could be extracted and utilized in the future. Different extraction methods (stirring, sonication, microwave assisted extraction) using different solvents (water, methanol:water 80:20 v/v, ethanol:water 80:20 v/v) and time/temperature schedules have been compared basing on total phenol contents (Folin-Ciocâlteu) and MRM peak areas of the identified compounds to investigate optimum extraction efficiency. Altogether 37 compounds, including (+)-catechin, (-)-epicatechin, quercetin-O-hexoside, taxifolin-O-hexosides (3), taxifolin-O-pentosides (4), B-type (6) and C-type (6) procyanidins, syringic acid- and coumaric acid-di-O-glycosides, coniferyl alcohol- and sinapyl alcohol-glycosides, as well as other unknown compounds with defined [M-H](-) m/z values and MS/MS spectra have been tentatively identified. The choice of the method, solvent system and time/temperature parameters favors the extraction of different types of compounds. Pure water can extract compounds as efficiently as mixtures containing organic solvents under high-pressure and high temperature conditions. This supports the implementation of green extraction methods in the future. Extraction times that are too long and high temperatures can result in the decrease of the concentrations. Future investigations will focus on the evaluation of the antioxidant capacity and utilization possibilities of the prepared extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

The effect of homogenization pressure on the flavor and flavor stability of whole milk powder.

PubMed

Park, Curtis W; Drake, MaryAnne

2017-07-01

Flavor is one of the key factors that can limit the application and shelf life of dried dairy ingredients. Many off-flavors are caused during ingredient manufacture that carry through into ingredient applications and decrease consumer acceptance. The objective of this research was to investigate the effect of homogenization pressure on the flavor and flavor stability of whole milk powder (WMP). Whole milk powder was produced from standardized pasteurized whole milk that was evaporated to 50% solids (wt/wt), homogenized in 2 stages with varying pressures (0/0, 5.5/1.4, 11.0/2.8, or 16.5/4.3 MPa), and spray dried. Whole milk powder was evaluated at 0, 3, and 6 mo of storage at 21°C. Sensory properties were evaluated by descriptive analysis. Volatile compounds were analyzed by sorptive stir bar extraction with gas chromatography-mass spectrometry. Fat globule size in condensed whole milk and particle size of powders were measured by laser diffraction. Surface free fat, inner free fat, and encapsulated fat of WMP were measured by solvent extractions. Phospholipid content was measured by ultra-high-performance liquid chromatography-evaporative light scattering. Furosine in WMP was analyzed by ultra-high-performance liquid chromatography-mass spectrometry. Increased homogenization pressure decreased cardboard and painty flavors, volatile lipid oxidation compound concentrations, fat globule size in condensed milk, surface free fat, and inner free fat in WMP. Encapsulated fat increased and phospholipid-to-encapsulated fat ratio decreased with higher homogenization pressure. Surface free fat in powders increased cardboard flavor and lipid oxidation. These results indicate that off-flavors were decreased with increased homogenization pressures in WMP due to the decrease in free fat. To decrease off-flavor intensities in WMP, manufacturers should carefully evaluate these parameters during ingredient manufacture. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Subcritical-Water Extraction of Organics from Solid Matrices

NASA Technical Reports Server (NTRS)

Amashukeli, Xenia; Grunthaner, Frank; Patrick, Steven; Kirby, James; Bickler, Donald; Willis, Peter; Pelletier, Christine; Bryson, Charles

2009-01-01

An apparatus for extracting organic compounds from soils, sands, and other solid matrix materials utilizes water at subcritical temperature and pressure as a solvent. The apparatus, called subcritical water extractor (SCWE), is a prototype of subsystems of future instrumentation systems to be used in searching for organic compounds as signs of past or present life on Mars. An aqueous solution generated by an apparatus like this one can be analyzed by any of a variety of established chromatographic or spectroscopic means to detect the dissolved organic compound( s). The apparatus can be used on Earth: indeed, in proof-of-concept experiments, SCWE was used to extract amino acids from soils of the Atacama Desert (Chile), which was chosen because the dryness and other relevant soil conditions there approximate those on Mars. The design of the apparatus is based partly on the fact that the relative permittivity (also known as the dielectric constant) of liquid water varies with temperature and pressure. At a temperature of 30 C and a pressure of 0.1 MPa, the relative permittivity of water is 79.6, due to the strong dipole-dipole electrostatic interactions between individual molecular dipoles. As the temperature increases, increasing thermal energy causes increasing disorientation of molecular dipoles, with a consequent decrease in relative permittivity. For example, water at a temperature of 325 C and pressure of 20 MPa has a relative permittivity of 17.5, which is similar to the relative permittivities of such nonpolar organic solvents as 1-butanol (17.8). In the operation of this apparatus, the temperature and pressure of water are adjusted so that the water can be used in place of commonly used organic solvents to extract compounds that have dissimilar physical and chemical properties.

Sensitive high-performance liquid chromatography/mass spectrometry method for determination of steviol in rat plasma.

PubMed

Wang, L Z; Goh, B C; Fan, L; Lee, H S

2004-01-01

The main toxicological concern of stevioside, a highly potent sweetener from S. rebaudiana, is its main metabolite, steviol. To determine very low levels of steviol in in vivo experiments, a sensitive liquid chromatography/atmospheric pressure chemical ionization mass spectrometry (LC/APCI-MS) method was developed for quantifying steviol in rat plasma after oral administration of a single dose of stevioside (0.5 g/kg). The sample preparation uses liquid-liquid extraction with tert-butyl methyl ether in an acidic environment. The retention time of steviol was 10.5 min. The assay was linear over the range 2-1000 ng/mL with a lower limit of detection of 1 ng/mL. The intra- and inter-day precision were <5 and <7%, respectively, and the accuracy was in the range 95-108%. The steviol concentration profile in rat plasma was determined. Copyright 2003 John Wiley & Sons, Ltd.

Liquid-liquid extraction of neodymium(III) by dialkylphosphate ionic liquids from acidic medium: the importance of the ionic liquid cation.

PubMed

Rout, Alok; Kotlarska, Justyna; Dehaen, Wim; Binnemans, Koen

2013-10-21

The ionic liquids 1-hexyl-3-methylimidazolium bis(2-ethylhexyl)phosphate, [C6mim][DEHP], 1-hexyl-1-methylpyrrolidinium bis(2-ethylhexyl)phosphate, [C6mpyr][DEHP], and tetrabutylammonium bis(2-ethylhexyl)phosphate, [N4444][DEHP], were prepared and characterized using (1)H and (13)C NMR spectroscopy. The extraction behavior of neodymium(iii) from nitrate medium by these ionic liquids, diluted with the room temperature ionic liquids 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, [C6mim][NTf2], 1-hexyl-3-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide, [C6mpyr][NTf2], and tributylmethylammonium bis(trifluoromethylsulfonyl)imide, [N1444][NTf2], was studied. The distribution ratio of neodymium(iii) was measured as a function of various parameters, such as pH, concentration of the ionic liquid extractant, nature of diluents, concentration of ionic liquid cations and nitrate anions in the aqueous phase. The extraction behavior was compared with that obtained for a solution of the molecular extractant bis(2-ethylhexyl)phosphoric acid (DEHPA) in an ionic liquid diluent. The extraction of neodymium(iii) in the ionic liquids [C6mim][DEHP] and [C6mpyr][DEHP] showed markedly different extraction properties in comparison with that of the quaternary ammonium analogue [N4444][DEHP], especially concerning the pH dependence of the extraction process. These results show that the extraction process can be tuned by the selection of the ionic liquid cation. The extraction experiments also included the trivalent rare-earth ions lanthanum(iii), cerium(iii), praseodymium(iii), ytterbium(iii) and yttrium(iii). Studies of the stripping behavior and the reusability of the ionic liquids were carried out, which indicate that the ionic liquids can be reused with no loss in activity.

Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

ERIC Educational Resources Information Center

Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

2015-01-01

Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

Influence of agronomic variables on the composition of mate tea leaves (Ilex paraguariensis) extracts obtained from CO2 extraction at 30 degrees C and 175 bar.

PubMed

Esmelindro, Angela Aquino; Girardi, Jonathan Dos Santos; Mossi, Altemir; Jacques, Rosângela Assis; Dariva, Cláudio

2004-04-07

The aim of this work is to assess the influence of light intensity (plants with direct sun exposure and in a controlled light intensity) and age of leaves (6-24 months) on the characteristics of the extracts of mate tea leaves obtained from carbon dioxide at high pressures. Samples of mate were collected in an experiment conducted under agronomic control at Industria e Comercio de Erva-Mate Barão LTDA, Brazil. The content of selected organic compounds of the extracts was evaluated by gas chromatography together with mass spectrometry. Quantitative analysis of caffeine, theobromine, phytol, vitamin E, squalene, and stigmasterol was performed, and the results showed that field variables exert a strong influence on the liquid yield and on the chemical distribution of the extracts.

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.

Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

PubMed

Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

2016-12-01

Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL -1 , respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%. Copyright © 2016 Elsevier B.V. All rights reserved.

Diclofenac in municipal wastewater treatment plant: quantification using laser diode thermal desorption--atmospheric pressure chemical ionization--tandem mass spectrometry approach in comparison with an established liquid chromatography-electrospray ionization-tandem mass spectrometry method.

PubMed

Lonappan, Linson; Pulicharla, Rama; Rouissi, Tarek; Brar, Satinder K; Verma, Mausam; Surampalli, Rao Y; Valero, José R

2016-02-12

Diclofenac (DCF), a prevalent non-steroidal anti-inflammatory drug (NSAID) is often detected in wastewater and surface water. Analysis of the pharmaceuticals in complex matrices is often laden with challenges. In this study a reliable, rapid and sensitive method based on laser diode thermal desorption/atmospheric pressure chemical ionization (LDTD/APCI) coupled with tandem mass spectrometry (MS/MS) has been developed for the quantification of DCF in wastewater and wastewater sludge. An established conventional LC-ESI-MS/MS (liquid chromatography-electrospray ionization-tandem mass spectrometry) method was compared with LDTD-APCI-MS/MS approach. The newly developed LDTD-APCI-MS/MS method reduced the analysis time to 12s in lieu of 12 min for LC-ESI-MS/MS method. The method detection limits for LDTD-APCI-MS/MS method were found to be 270 ng L(-1) (LOD) and 1000 ng L(-1) (LOQ). Furthermore, two extraction procedures, ultrasonic assisted extraction (USE) and accelerated solvent extraction (ASE) for the extraction of DCF from wastewater sludge were compared and ASE with 95.6 ± 7% recovery was effective over USE with 86 ± 4% recovery. The fate and partitioning of DCF in wastewater (WW) and wastewater sludge (WWS) in wastewater treatment plant was also monitored at various stages of treatment in Quebec Urban community wastewater treatment plant. DCF exhibited affinity towards WW than WWS with a presence about 60% of DCF in WW in contrary with theoretical prediction (LogKow=4.51). Copyright © 2016 Elsevier B.V. All rights reserved.

Single solid phase extraction method for the simultaneous analysis of polar and non-polar pesticides in urine samples by gas chromatography and ultra high pressure liquid chromatography coupled to tandem mass spectrometry.

PubMed

Cazorla-Reyes, Rocío; Fernández-Moreno, José Luis; Romero-González, Roberto; Frenich, Antonia Garrido; Vidal, José Luis Martínez

2011-07-15

A new multiresidue method has been developed and validated for the simultaneous extraction of more than two hundred pesticides, including non-polar and polar pesticides (carbamates, organochlorine, organophosphorous, pyrethroids, herbicides and insecticides) in urine at trace levels by gas and ultra high pressure liquid chromatography coupled to ion trap and triple quadrupole mass spectrometry, respectively (GC-IT-MS/MS, UHPLC-QqQ-MS/MS). Non-polar and polar pesticides were simultaneously extracted from urine samples by a simple and fast solid phase extraction (SPE) procedure using C(18) cartridges as sorbent, and dichloromethane as elution solvent. Recovery was in the range of 60-120%. Precision values expressed as relative standard deviation (RSD) were lower than 25%. Identification and confirmation of the compounds were performed by the use of retention time windows, comparison of spectra (GC-amenable compounds) or the estimation of the ion ratio (LC-amenable compounds). For GC-amenable pesticides, limits of detection (LODs) ranged from 0.001 to 0.436 μg L(-1) and limits of quantification (LOQs) from 0.003 to 1.452 μg L(-1). For LC-amenable pesticides, LODs ranged from 0.003 to 1.048 μg L(-1) and LOQs ranged from 0.011 to 3.494 μg L(-1). Finally, the optimized method was applied to the analysis of fourteen real samples of infants from agricultural population. Some pesticides such as methoxyfenozide, tebufenozide, piperonyl butoxide and propoxur were found at concentrations ranged from 1.61 to 24.4 μg L(-1), whereas methiocarb sulfoxide was detected at trace levels in two samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Validation of a GC-MS/MS method for simultaneous determination of 86 persistent organic pollutants in marine sediments by pressurized liquid extraction followed by stir bar sorptive extraction.

PubMed

Camino-Sánchez, F J; Zafra-Gómez, Alberto; Pérez-Trujillo, J P; Conde-González, J E; Marques, J C; Vílchez, José Luis

2011-08-01

A multiresidue method for the analysis of 86 persistent pollutants in marine sediments at ultra-trace level has been developed and validated using pressurized liquid extraction (PLE) and stir-bar sorptive extraction (SBSE) coupled with thermal desorption and gas chromatography-triple quadrupole mass spectrometry (TD-GC-MS/MS QqQ). The compounds analyzed belong to various families such as polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenylethers, organophosphorus and organochlorine pesticides and other pesticides such as urons, and triazines. The analytes have very different polarities and log K(ow) values, which is an important parameter in the optimization of a SBSE method. Due to PLE high efficiency and throughput rates, along with the proven ability for multiresidue analysis and excellent sensitivity of SBSE, we present an efficient method. The limits of quantification obtained ranged from 0.014 to 1.0 ng g(-1), with detection limits below pg g(-1) levels. In order to validate the proposed methodology, quality parameters such as recovery, linearity and reproducibility were studied. Recoveries ranged from 63% to 119%, reproducibility (in terms of Relative Standard Deviation for ten determinations) was lower than 35% in all cases, and determination coefficients higher than 0.990 for all analytes. The main factors that affect PLE, SBSE and GC-MS/MS procedures were optimized. The method was applied to the analysis of nine marine sediments obtained from the nine main submarine wastewater discharge points (emissaries) presents along the coast of Tenerife Island (Canary Islands, Spain). Copyright © 2011 Elsevier Ltd. All rights reserved.

Application of statistical experimental design to the optimisation of microextraction by packed sorbent for the analysis of nonsteroidal anti-inflammatory drugs in human urine by ultra-high pressure liquid chromatography.

PubMed

Magiera, Sylwia; Gülmez, Şefika; Michalik, Aleksandra; Baranowska, Irena

2013-08-23

A new approach based on microextraction by packed sorbent (MEPS) and a reversed-phase ultra-high pressure liquid chromatography (UHPLC) method was developed and validated for the determination and quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) (acetylsalicylic acid, ketoprofen, diclofenac, naproxen and ibuprofen) in human urine. The important factors that could influence the extraction were previously screened using the Plackett-Burman design approach. The optimal MEPS extraction conditions were obtained using C18 phase as a sorbent, small sample volume (20μL) and a short time period (approximately 5min) for the entire sample preparation step. The analytes were separated on a core-shell column (Poroshell 120 EC-C18; 100mm×3.0mm; 2.7μm) using a binary mobile phase composed of aqueous 0.1% trifluoroacetic acid and acetonitrile in the gradient elution mode (4.5min of analysis time). The analytical method was fully validated based on linearity, limits of detection (LOD), limits of quantification (LOQ), inter- and intra-day precision and accuracy, and extraction yield. Under optimised conditions, excellent linearity (R(2)>0.9991), limits of detection (1.07-16.2ngmL(-1)) and precision (0.503-9.15% RSD) were observed for the target drugs. The average absolute recoveries of the analysed compounds extracted from the urine samples were 89.4-107%. The proposed method was also applied to the analysis of NSAIDs in human urine. The new approach offers an attractive alternative for the analysis of selected drugs from urine samples, providing several advantages including fewer sample preparation steps, faster sample throughput and ease of performance compared to traditional methodologies. Copyright © 2013 Elsevier B.V. All rights reserved.

Experimental investigation of blast mitigation and particle-blast interaction during the explosive dispersal of particles and liquids

NASA Astrophysics Data System (ADS)

Pontalier, Q.; Loiseau, J.; Goroshin, S.; Frost, D. L.

2018-04-01

The attenuation of a blast wave from a high-explosive charge surrounded by a layer of inert material is investigated experimentally in a spherical geometry for a wide range of materials. The blast wave pressure is inferred from extracting the blast wave velocity with high-speed video as well as direct measurements with pressure transducers. The mitigant consists of either a packed bed of particles, a particle bed saturated with water, or a homogeneous liquid. The reduction in peak blast wave overpressure is primarily dependent on the mitigant to explosive mass ratio, M/C, with the mitigant material properties playing a secondary role. Relative peak pressure mitigation reduces with distance and for low values of M/C (< 10) can return to unmitigated pressure levels in the mid-to-far field. Solid particles are more effective at mitigating the blast overpressure than liquids, particularly in the near field and at low values of M/C, suggesting that the energy dissipation during compaction, deformation, and fracture of the powders plays an important role. The difference in scaled arrival time of the blast and material fronts increases with M/C and scaled distance, with solid particles giving the largest separation between the blast wave and cloud of particles. Surrounding a high-explosive charge with a layer of particles reduces the positive-phase blast impulse, whereas a liquid layer has no influence on the impulse in the far field. Taking the total impulse due to the blast wave and material impact into account implies that the damage to a nearby structure may actually be augmented for a range of distances. These results should be taken into consideration in the design of explosive mitigant systems.

Experimental investigation of blast mitigation and particle-blast interaction during the explosive dispersal of particles and liquids

NASA Astrophysics Data System (ADS)

Pontalier, Q.; Loiseau, J.; Goroshin, S.; Frost, D. L.

2018-05-01

The attenuation of a blast wave from a high-explosive charge surrounded by a layer of inert material is investigated experimentally in a spherical geometry for a wide range of materials. The blast wave pressure is inferred from extracting the blast wave velocity with high-speed video as well as direct measurements with pressure transducers. The mitigant consists of either a packed bed of particles, a particle bed saturated with water, or a homogeneous liquid. The reduction in peak blast wave overpressure is primarily dependent on the mitigant to explosive mass ratio, M/ C, with the mitigant material properties playing a secondary role. Relative peak pressure mitigation reduces with distance and for low values of M/ C (< 10) can return to unmitigated pressure levels in the mid-to-far field. Solid particles are more effective at mitigating the blast overpressure than liquids, particularly in the near field and at low values of M/ C, suggesting that the energy dissipation during compaction, deformation, and fracture of the powders plays an important role. The difference in scaled arrival time of the blast and material fronts increases with M/ C and scaled distance, with solid particles giving the largest separation between the blast wave and cloud of particles. Surrounding a high-explosive charge with a layer of particles reduces the positive-phase blast impulse, whereas a liquid layer has no influence on the impulse in the far field. Taking the total impulse due to the blast wave and material impact into account implies that the damage to a nearby structure may actually be augmented for a range of distances. These results should be taken into consideration in the design of explosive mitigant systems.

Ares I Reaction Control System Propellant Feedline Decontamination Modeling

NASA Technical Reports Server (NTRS)

Pasch, James J.

2010-01-01

The objective of the work presented here is to quantify the effects of purge gas temperature, pressure, and mass flow rate on Hydrazine (Hz) decontamination rates of the Ares I Roll Control System and Reaction Control System. A survey of experts in this field revealed the absence of any decontamination rate prediction models. Three basic decontamination methods were identified for analysis and modeling. These include low pressure eduction, high flow rate purge, and pulse purge. For each method, an approach to predict the Hz mass transfer rate, as a function of system pressure, temperature, and purge gas mass flow rate, is developed based on the applicable physics. The models show that low pressure eduction is two orders of magnitude more effective than the high velocity purge, which in turn is two orders of magnitude more effective than the pure diffusion component of pulse purging of deadheads. Eduction subjects the system to low pressure conditions that promote the extraction of Hz vapors. At 120 F, Hz is saturated at approximately 1 psia. At lower pressures and 120 F, Hz will boil, which is an extremely efficient means to remove liquid Hz. The Hz boiling rate is predicted by equating the rate at which energy is added to the saturated liquid Hz through heaters at the tube outer wall with the energy removed from the liquid through evaporation. Boil-off fluxes were predicted by iterating through the range of local pressures with limits set by the minimum allowed pressure of 0.2 psia and maximum allowed wall temperature of 120 F established by the heaters, which gives a saturation pressure of approximately 1.0 psia. Figure 1 shows the resulting boil-off fluxes as a function of local eduction pressure. As depicted in figure 1, the flux is a strong inverse function of eduction pressure, and that minimizing the eduction pressure maximizes the boil-off flux. Also, higher outer wall temperatures lead to higher boil-off fluxes and allow for boil-off over a greater range of eduction pressures.

The investigation of critical burning of fuel droplets

NASA Technical Reports Server (NTRS)

Allison, C. B.; Canada, G. S.; Faeth, G. M.

1973-01-01

The combustion and evaporation of liquid fuels at high pressures were investigated. Particular emphasis was placed on conditions where the liquid surface approaches the thermodynamic critical point during combustion. The influence of transient effects on a burning liquid fuel was also investigated through both analysis and measurements of the response of liquid monopropellant combustion to imposed pressure oscillations. Work was divided into four phases (1) Droplet combustion at high pressures, which consider both measurement and analysis of the porous sphere burning rate of liquids in a natural convection environment at elevated pressure. (2) High pressure droplet burning in combustion gases, which involved steady burning and evaporation of liquids from porous spheres in a high pressure environment that simulates actual combustion chamber conditions. (3) Liquid strand combustion, which considered the burning rate, the state of the liquid surface and the liquid phase temperature distribution of a burning liquid monopropellant column over a range of pressures. (4) Oscillatory combustion, which was a theoretical and experimental investigation of the response of a burning liquid monopropellant to pressure oscillations.

Film analysis employing subtarget effect using 355 nm Nd-YAG laser-induced plasma at low pressure

NASA Astrophysics Data System (ADS)

Hedwig, Rinda; Budi, Wahyu Setia; Abdulmadjid, Syahrun Nur; Pardede, Marincan; Suliyanti, Maria Margaretha; Lie, Tjung Jie; Kurniawan, Davy Putra; Kurniawan, Koo Hendrik; Kagawa, Kiichiro; Tjia, May On

2006-12-01

The applicability of spectrochemical analysis for liquid and powder samples of minute amount in the form of thin film was investigated using ultraviolet Nd-YAG laser (355 nm) and low-pressure ambient air. A variety of organic samples such as commercial black ink usually used for stamp pad, ginseng extract, human blood, liquid milk and ginseng powder was prepared as film deposited on the surface of an appropriate hard substrate such as copper plate or glass slide. It was demonstrated that in all cases studied, good quality spectra were obtained with very low background and free from undesirable contamination by the substrate elements, featuring ppm or even sub-ppm sensitivity and worthy of application for quantitative analysis of organic samples. The proper preparation of the films was found to be crucial in achieving the high quality spectra. It was further shown that much inferior results were obtained when the atmospheric-pressure (101 kPa) operating condition of laser-induced breakdown spectroscopy or the fundamental wavelength of the Nd-YAG laser was employed due to the excessive or improper laser ablation process.

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.

Screening, separation, and evaluation of xanthine oxidase inhibitors from Paeonia lactiflora using chromatography combined with a multi-mode microplate reader.

PubMed

Wang, Jing; Shi, Dongfang; Zheng, Meizhu; Ma, Bing; Cui, Jing; Liu, Chunming; Liu, Chengyu

2017-11-01

Natural products have become one of the most important resources for discovering novel xanthine oxidase inhibitors, which are commonly employed in the treatment of hyperuricemia and gout. However, to date, few reports exist regarding the use of monoterpene glycosides as xanthine oxidase inhibitors. Thus, we herein report the use of ultrafiltration coupled with liquid chromatography in the screening of monoterpene glycoside xanthine oxidase inhibitors from the extract of Paeonia lactiflora (P. lactiflora), and both high-performance counter-current chromatography and medium-pressure liquid chromatography were employed to separate the main constituents. Furthermore, the xanthine oxidase inhibitory activities and the mechanisms of inhibition of the isolated compounds were evaluated using a multi-mode microplate reader by Molecular Devices. As a result, three monoterpene glycosides were separated by combined high-performance counter-current chromatography and medium-pressure liquid chromatography in purities of 90.4, 98.0, and 86.3%, as determined by liquid chromatography. These three compounds were identified as albiflorin, paeoniflorin, and 1-O-β-ᴅ-glucopyranosyl-8-O-benzoylpaeonisuffrone by electrospray ionization tandem mass spectrometry, and albiflorin and paeoniflorin were screened as potential xanthine oxidase inhibitors by ultrafiltration with liquid chromatography. The evaluation results of xanthine oxidase inhibitory activity corresponded with the screening results, as only albiflorin and paeoniflorin exhibited xanthine oxidase inhibitory activity. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid Solid-Liquid Dynamic Extraction (RSLDE): a New Rapid and Greener Method for Extracting Two Steviol Glycosides (Stevioside and Rebaudioside A) from Stevia Leaves.

PubMed

Gallo, Monica; Vitulano, Manuela; Andolfi, Anna; DellaGreca, Marina; Conte, Esterina; Ciaravolo, Martina; Naviglio, Daniele

2017-06-01

Stevioside and rebaudioside A are the main diterpene glycosides present in the leaves of the Stevia rebaudiana plant, which is used in the production of foods and low-calorie beverages. The difficulties associated with their extraction and purification are currently a problem for the food processing industries. The objective of this study was to develop an effective and economically viable method to obtain a high-quality product while trying to overcome the disadvantages derived from the conventional transformation processes. For this reason, extractions were carried out using a conventional maceration (CM) and a cyclically pressurized extraction known as rapid solid-liquid dynamic extraction (RSLDE) by the Naviglio extractor (NE). After only 20 min of extraction using the NE, a quantity of rebaudioside A and stevioside equal to 1197.8 and 413.6 mg/L was obtained, respectively, while for the CM, the optimum time was 90 min. From the results, it can be stated that the extraction process by NE and its subsequent purification developed in this study is a simple, economical, environmentally friendly method for producing steviol glycosides. Therefore, this method constitutes a valid alternative to conventional extraction by reducing the extraction time and the consumption of toxic solvents and favouring the use of the extracted metabolites as food additives and/or nutraceuticals. As an added value and of local interest, the experiment was carried out on stevia leaves from the Benevento area (Italy), where a high content of rebaudioside A was observed, which exhibits a sweet taste compared to stevioside, which has a significant bitter aftertaste.

The limit of the film extraction technique for annular two-phase flow in a small tube

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

Helm, D.E.; Lopez de Bertodano, M.; Beus, S.G.

1999-07-01

The limit of the liquid film extraction technique was identified in air-water and Freon-113 annular two-phase flow loops. The purpose of this research is to find the limit of the entrainment rate correlation obtained by Lopez de Bertodano et. al. (1998). The film extraction technique involves the suction of the liquid film through a porous tube and has been widely used to obtain annular flow entrainment and entrainment rate data. In these experiments there are two extraction probes. After the first extraction the entrained droplets in the gas core deposit on the tube wall. A new liquid film develops entirelymore » from liquid deposition and a second liquid film extraction is performed. While it is assumed that the entire liquid film is removed after the first extraction unit, this is not true for high liquid flow. At high liquid film flows the interfacial structure of the film becomes frothy. Then the entire liquid film cannot be removed at the first extraction unit, but continues on and is extracted at the second extraction unit. A simple model to characterize the limit of the extraction technique was obtained based on the hypothesis that the transition occurs due to a change in the wave structure. The resulting dimensionless correlation agrees with the data.« less

The limit of the film extraction technique for annular two-phase flow in a small tube

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

Helm, D.E.; Lopez de Bertodano, M.; Beus, S.G.

1999-07-01

The limit of the liquid film extraction technique was identified in air-water and Freon-113 annular two-phase flow loops. The purpose of this research is to find the limit of the entrainment rate correlation obtained by Lopez de Bertodano et al. (1998). The film extraction technique involves the suction of the liquid film through a porous tube and has been widely used to obtain annular flow entrainment and entrainment rate data. In the experiments there are two extraction probes. After the first extraction the entrained droplets in the gas core deposit on the tube wall. A new liquid film develops entirelymore » from liquid deposition and a second liquid film extraction is performed. While it is assumed that the entire liquid film is removed after the first extraction unit, this is not true for high liquid flow. At high liquid film flows the interfacial structure of the film becomes frothy. Then the entire liquid film cannot be removed at the first extraction unit, but continues on and is extracted at the second extraction unit. A simple model to characterize the limit of the extraction technique was obtained based on the hypothesis that the transition occurs due to a change in the wave structure. The resulting dimensionless correlation agrees with the data.« less

Development and Validation of a Technique for Detection of Stress and Pregnancy in Large Whales

DTIC Science & Technology

2015-09-30

humpback whales, blue whales, and possibly insular false killer whales). 2 2) The second objective is to complete the biological validation using...identification using high-pressure liquid chromatography (HPLC). Briefly, pooled blubber extract from animals of known gender will be serially diluted 1...progesterone in captive female false killer whales, pseudorca crassidens. Gen. Comp. Endocrinol. 115:323-332. Atkinson, S., Crocker, D., Houser, D

Characterization of major and minor alk(en)ylresorcinols from mango (Mangifera indica L.) peels by high-performance liquid chromatography/atmospheric pressure chemical ionization mass spectrometry.

PubMed

Knödler, Matthias; Berardini, Nicolai; Kammerer, Dietmar R; Carle, Reinhold; Schieber, Andreas

2007-01-01

5-Alkyl- and 5-alkenylresorcinols, as well as their hydroxylated derivatives, were extracted from mango (Mangifera indica L.) peels, purified on polyamide and characterized by high-performance liquid chromatography/atmospheric pressure chemical ionization mass spectrometry (HPLC/APcI-MS) for the first time. Among the 15 compounds analyzed, 3 major and 12 minor C(15)-, C(17)-, and C(19)-substituted resorcinols and related analogues, showing varying degrees of unsaturation, were characterized by their specific fragmentation patterns in collision-induced dissociation experiments. This marks the first report on the occurrence of mono-, di-, and triunsaturated C(15)-homologues, saturated and triunsaturated C(17)-homologues, and mono- and diunsaturated C(19)-homologues in mango peels. Additionally, several hydroxylated C(15)- and C(17)-homologues, also not yet described in mango, and a C(14)-monoene, unique because of its even-numbered side chain, were tentatively identified on the basis of their fragmentation patterns. The results obtained in the present study indicate that HPLC-DAD-APcI-MS(n), combined with the newly developed solid-phase extraction, is a powerful tool for the analysis of alk(en)ylresorcinols and could therefore be used for their determination in various matrices.

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.

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

PubMed

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

2018-04-01

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

[Technological process of cell disruption for extracting astaxanthin from Phaffia rhodozyma by acid method under autoclave conditions].

PubMed

Lu, Baoju; Xiao, Anfeng; Lil, Lijun; Ni, Hui; Cai, Huinong; Su, Wenjin

2008-07-01

Phaffia rhodozyma is one of the organisms for production of astaxanthin, and the key process for extracting intracellular astaxanthin is cell disruption. In this work, cell disruption for extracting astaxanthin from Phaffia rhodozyma was studied with autoclave method at low acid concentration. The optimum disrupting conditions were: autoclave pressure 0.1 MPa, 121 degrees C; hydrochloric acid concentration 0.5 mol/L; liquid to material ratio (V/W) 30 mL/g dry cell weight and disruption time 2 min. Under the optimum conditions, medium scale experiment showed that astaxanthin and total carotenoids recovery from Phaffia rhodozyma were (84.8 +/- 3.2)% and (93.3 +/- 2)%, respectively. This new method can lead to no poisonous residues and get high extraction yield, which have good prospects to be put into industrial production.

Equilibrium and rate data for the extraction of lipids using compressed carbon dioxide

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

King, M.B.; Bott, T.R.; Barr, M.J.

1987-01-01

Equilibrium data are given for the solubilities in compressed CO2 of the lipid components in freshly ground rape seed and of glycerol trioleate (a typical constituent of rape oil) at pressures up to 200 bar and temperatures 25 to 75C. Continuous flow tests in which a bed of ground rape seed was contacted with a stream of liquid CO2 at 25C and varied flow conditions are also reported. The results are collated in terms of an empirical mass transfer coefficient. A sharp change took place in the lipid concentration in the extractant stream leaving the bed when about 65% ofmore » the available oil had been extracted. This, and changes in the composition of the extract, are discussed, together with the use of this type of data for design purposes.« less

On-site comprehensive analysis of explosives using HPLC-UV-PAED

NASA Astrophysics Data System (ADS)

Marple, Ronita L.; LaCourse, William R.

2004-03-01

High-performance liquid chromatography with ultra violet and photo-assisted electrochemical detection (HPLC-UV-PAED) has been developed for the sensitive and selective detection of explosives in ground water and soil extracts. Fractionation and preconcentration of explosives is accomplished with on-line solid phase extraction (SPE), which minimizes sample pretreatment and enables faster and more accurate on-site assessment of a contaminated site. Detection limits are equivalent or superior (i.e., <1 part-per-trillion for HMX) to those achieved using the Environmental Protection Agency (EPA) Method 8330. This approach is more broadly applicable, as it is capable of determining a wider range of organic nitro compounds. Soil samples are extracted using pressurized fluid extraction (PFE), and this technique is automatable, field-compatible, and environmentally friendly, adding to the overall efficiency of the methodology.

Cryogenic Cathode Cooling Techniques for Improved SABRE Extraction Ion Diode Li Beam Generation

NASA Astrophysics Data System (ADS)

Hanson, D. L.; Johnston, R. R.; Cuneo, M. E.; Menge, P. R.; Fowler, W. E.; Armijo, J.; Nielsen, D. S.; Petmecky, D.

1997-11-01

We are developing techniques for cryogenic cooling of the SABRE extraction ion diode cathode that, combined with source cleaning, should improve the purity and brightness of Li beams for ICF light ion fusion. By liquid helium (LHe) cathode cooling, we have been able to maintain A-K gap base pressures in the range of 5 - 7x10-8 Torr for about 45 minutes. These base pressures extend the monolayer formation time for the worst beam contaminants (H2 and water vapor) to 10 - 100 sec or longer, which should allow the accelerator to be fired without significant Li source recontamination. This technique is compatible with He glow discharge cleaning, laser cleaning, and in situ Li deposition. We are also developing techniques for Ti-gettering of H2 and for cryogenic cooling of cathode electrodes to delay cathode plasma expansion.

Large-Scale Membrane- and Lignin-Modified Adsorbent-Assisted Extraction and Preconcentration of Triazine Analogs and Aflatoxins

PubMed Central

Hu, Shun-Wei; Chen, Shushi

2017-01-01

The large-scale simultaneous extraction and concentration of aqueous solutions of triazine analogs, and aflatoxins, through a hydrocarbon-based membrane (e.g., polyethylene, polyethylene/polypropylene copolymer) under ambient temperature and atmospheric pressure is reported. The subsequent adsorption of analyte in the extraction chamber over the lignin-modified silica gel facilitates the process by reducing the operating time. The maximum adsorption capacity values for triazine analogs and aflatoxins are mainly adsorption mechanism-dependent and were calculated to be 0.432 and 0.297 mg/10 mg, respectively. The permeation, and therefore the percentage of analyte extracted, ranges from 1% to almost 100%, and varies among the solvents examined. It is considered to be vapor pressure- and chemical polarity-dependent, and is thus highly affected by the nature and thickness of the membrane, the discrepancy in the solubility values of the analyte between the two liquid phases, and the amount of adsorbent used in the process. A dependence on the size of the analyte was observed in the adsorption capacity measurement, but not in the extraction process. The theoretical interaction simulation and FTIR data show that the planar aflatoxin molecule releases much more energy when facing toward the membrane molecule when approaching it, and the mechanism leading to the adsorption. PMID:28398252

Large-Scale Membrane- and Lignin-Modified Adsorbent-Assisted Extraction and Preconcentration of Triazine Analogs and Aflatoxins.

PubMed

Hu, Shun-Wei; Chen, Shushi

2017-04-11

The large-scale simultaneous extraction and concentration of aqueous solutions of triazine analogs, and aflatoxins, through a hydrocarbon-based membrane (e.g., polyethylene, polyethylene/polypropylene copolymer) under ambient temperature and atmospheric pressure is reported. The subsequent adsorption of analyte in the extraction chamber over the lignin-modified silica gel facilitates the process by reducing the operating time. The maximum adsorption capacity values for triazine analogs and aflatoxins are mainly adsorption mechanism-dependent and were calculated to be 0.432 and 0.297 mg/10 mg, respectively. The permeation, and therefore the percentage of analyte extracted, ranges from 1% to almost 100%, and varies among the solvents examined. It is considered to be vapor pressure- and chemical polarity-dependent, and is thus highly affected by the nature and thickness of the membrane, the discrepancy in the solubility values of the analyte between the two liquid phases, and the amount of adsorbent used in the process. A dependence on the size of the analyte was observed in the adsorption capacity measurement, but not in the extraction process. The theoretical interaction simulation and FTIR data show that the planar aflatoxin molecule releases much more energy when facing toward the membrane molecule when approaching it, and the mechanism leading to the adsorption.

Liquid Hydrogen Zero-Boiloff Testing and Analysis for Long-Term Orbital Storage

NASA Astrophysics Data System (ADS)

Hastings, L. J.; Hedayat, A.; Bryant, C. B.; Flachbart, R. H.

2004-06-01

Advancement of cryocooler and passive insulation technologies in recent years has improved the prospects for zero-boiloff (ZBO) storage of cryogenic fluids. The ZBO concept involves the use of a cryocooler/radiator system to balance storage system incoming and extracted energy such that zero boiloff (no venting) occurs. A large-scale demonstration of the ZBO concept was conducted using the Marshall Space Flight Center (MSFC) multipurpose hydrogen test bed (MHTB) along with a commercial cryocooler unit. The liquid hydrogen (LH2) was withdrawn from the tank, passed through the cryocooler heat exchanger, and then the chilled liquid was sprayed back into the tank through a spray bar. The spray bar recirculation system was designed to provide destratification independent of ullage and liquid positions in a zero-gravity environment. The insulated MHTB tank, combined with the vacuum chamber conditions, enabled orbital storage simulation. ZBO was demonstrated for fill levels of 95%, 50%, and 25%. At each fill level, a steady-state boiloff test was performed prior to operating the cryocooler to establish the baseline heat leak. Control system logic based on real-time thermal data and ullage pressure response was implemented to automatically provide a constant tank pressure. A comparison of test data and analytical results is presented in this paper.

Liquid-Liquid Extraction of Insecticides from Juice: An Analytical Chemistry Laboratory Experiment

ERIC Educational Resources Information Center

Radford, Samantha A.; Hunter, Ronald E., Jr.; Barr, Dana Boyd; Ryan, P. Barry

2013-01-01

A laboratory experiment was developed to target analytical chemistry students and to teach them about insecticides in food, sample extraction, and cleanup. Micro concentrations (sub-microgram/mL levels) of 12 insecticides spiked into apple juice samples are extracted using liquid-liquid extraction and cleaned up using either a primary-secondary…

Hyphenating size‐exclusion chromatography with electrospray mass spectrometry; using on‐line liquid‐liquid extraction to study the lipid composition of lipoprotein particles

PubMed Central

Osei, Michael; Griffin, Julian L.

2015-01-01

Rationale Lipoproteins belong to the most commonly measured clinical biochemical parameters. Lipidomics is an orthogonal approach and aims to profile the individual lipid molecules that jointly form the lipoprotein particles. However, in the first step of the extraction of lipid molecules from serum, an organic solvent is used leading to dissociation of the lipoproteins. Thus far it has been impossible to combine lipidomics and lipoprotein analysis in one analytical system. Methods Human plasma was diluted in phosphate‐buffered saline (PBS) and injected onto a Superose 6 PC 3.2 column with PBS as a mobile phase to separate lipoproteins. The eluent was led to a Syrris FLLEX module, which also received CHCl3/MeOH (3:1). The two phases were mixed and subsequently separated using a Teflon membrane in an especially designed pressurized flow chamber. The organic phase was led to a standard electrospray source of an Orbitrap mass spectrometer. Results Size‐exclusion chromatography (SEC) has been commonly applied to separate lipoproteins and is considered a practical alternative to ultracentrifugation. Through the on‐line liquid‐liquid extraction method it becomes possible to obtained detailed mass spectra of lipids across different lipoprotein fractions. The extracted ion chromatograms of specific lipid signals showed their distribution against the size of lipoprotein particles. Conclusions The application of on‐line liquid‐liquid extraction allows for the continuous electrospray‐based mass spectral analysis of SEC eluent, providing the detailed lipid composition of lipoprotein particles separated by size. This approach provides new possibilities for the study of the biochemistry of lipoproteins. © 2015 The Authors. Rapid Communications in Mass Spectrometry Published by John Wiley & Sons Ltd. PMID:26443395

Glycoalkaloid content in pet food by UPLC-tandem mass spectrometry.

PubMed

Sheridan, Robert S; Kemnah, Jennifer L

2010-11-01

The glycoalkaloid content of pet food containing potatoes is investigated using a liquid-liquid solvent extraction followed by analysis by ultra-high pressure liquid chromatography tandem mass spectrometry (UPLC-MS-MS). Pet food samples are homogenized and extracted with a solution of 50:50 (v/v) acetonitrile-deionized water containing 5% acetic acid. Following vortexing and centrifugation, 3 mL of the supernatant is filtered and diluted in deionized water. The extract is injected onto a reverse phase C18 UPLC column with an initial mobile phase composed of 0.15% acetic acid in water (A) and 0.15% acetic acid in methanol (B) in a ratio of 70:30, respectively. The mobile phase reaches a final concentration of 15% A and 85% B over 10 min, at which point it is returned to the initial conditions. α-Solanine is measured by monitoring transitions m/z = 868.50 → 398.40 and 868.50 → 722.50, while α-chaconine is measure by monitoring transitions m/z = 852.60 → 97.80 and 852.60 → 706.50. Each analyte is measured and combined to determine total glycoalkaloid content (TGA). The results of the analysis of 52 pet food samples indicate both glycoalkaloids are present in all samples and two pet foods were found to contain > 100 μg/g total glycoalkaloid.

Quantification of the predominant monomeric catechins in baking chocolate standard reference material by LC/APCI-MS.

PubMed

Nelson, Bryant C; Sharpless, Katherine E

2003-01-29

Catechins are polyphenolic plant compounds (flavonoids) that may offer significant health benefits to humans. These benefits stem largely from their anticarcinogenic, antioxidant, and antimutagenic properties. Recent epidemiological studies suggest that the consumption of flavonoid-containing foods is associated with reduced risk of cardiovascular disease. Chocolate is a natural cocoa bean-based product that reportedly contains high levels of monomeric, oligomeric, and polymeric catechins. We have applied solid-liquid extraction and liquid chromatography coupled with atmospheric pressure chemical ionization-mass spectrometry to the identification and determination of the predominant monomeric catechins, (+)-catechin and (-)-epicatechin, in a baking chocolate Standard Reference Material (NIST Standard Reference Material 2384). (+)-Catechin and (-)-epicatechin are detected and quantified in chocolate extracts on the basis of selected-ion monitoring of their protonated [M + H](+) molecular ions. Tryptophan methyl ester is used as an internal standard. The developed method has the capacity to accurately quantify as little as 0.1 microg/mL (0.01 mg of catechin/g of chocolate) of either catechin in chocolate extracts, and the method has additionally been used to certify (+)-catechin and (-)-epicatechin levels in the baking chocolate Standard Reference Material. This is the first reported use of liquid chromatography/mass spectrometry for the quantitative determination of monomeric catechins in chocolate and the only report certifying monomeric catechin levels in a food-based Standard Reference Material.

[Simultaneous determination of the migrations of bisphenol A and phenol in polycarbonate bottles based on subcritical water extraction and high performance liquid chromatography].

PubMed

Bai, Weiwei; Liu, Shuhui; Cao, Jiangping; Fan, Yingying; Xie, Qilong

2013-03-01

A new method was established for the simultaneous determination of the migration amounts of bisphenol A (BPA) and phenol from polycarbonate (PC) bottles based on subcritical water extraction (SWE) and high performance liquid chromatography. The optimum extraction conditions included an extraction temperature of 120 degree C, a pressure of 6.89 MPa (1000 psi), a static extraction time of 1 h and one cycle. Under the conditions, the migration amounts of the BPA ranged from 6.81 to 1116 micro g/g in 11 samples. Phenol was not detectable in 5 samples, and in other ones the migration amounts of phenol varied in the range of 3.25 -6. 08 micro g/g. The traditional soaking extraction experiments showed that PC was subjected to weak hydrolysis after long-time leaching. The BPA and phenol were separated in 8 min. Good linearities were obtained in the range of 0. 05 - 20 mg/L for BPA and 0.02 - 20 mg/L for phenol ( r > 0.999 7). The limits of detection were 7.6 micro g/L for BPA and 2.0 micro g/L for phenol. Intra-day and inter-day repeatabilities (expressed as RSD) were less than 5.21% and 11.63%, respectively. Compared with traditional water soaking extraction, the extraction efficiencies increased 49 - 106 times using this developed SWE method. The procedure is simple, rapid and environment friendly, and can be utilized to determine the migration amounts of BPA and phenol in PC bottles.

Supercritical fluid extraction of selected pharmaceuticals from water and serum.

PubMed

Simmons, B R; Stewart, J T

1997-01-24

Selected drugs from benzodiazepine, anabolic agent and non-steroidal anti-inflammatory drug (NSAID) therapeutic classes were extracted from water and serum using a supercritical CO2 mobile phase. The samples were extracted at a pump pressure of 329 MPa, an extraction chamber temperature of 45 degrees C, and a restrictor temperature of 60 degrees C. The static extraction time for all samples was 2.5 min and the dynamic extraction time ranged from 5 to 20 min. The analytes were collected in appropriate solvent traps and assayed by modified literature HPLC procedures. Analyte recoveries were calculated based on peak height measurements of extracted vs. unextracted analyte. The recovery of the benzodiazepines ranged from 80 to 98% in water and from 75 to 94% in serum. Anabolic drug recoveries from water and serum ranged from 67 to 100% and 70 to 100%, respectively. The NSAIDs were recovered from water in the 76 to 97% range and in the 76 to 100% range from serum. Accuracy, precision and endogenous peak interference, if any, were determined for blank and spiked serum extractions and compared with classical sample preparation techniques of liquid-liquid and solid-phase extraction reported in the literature. For the benzodiazepines, accuracy and precision for supercritical fluid extraction (SFE) ranged from 1.95 to 3.31 and 0.57 to 1.25%, respectively (n = 3). The SFE accuracy and precision data for the anabolic agents ranged from 4.03 to 7.84 and 0.66 to 2.78%, respectively (n = 3). The accuracy and precision data reported for the SFE of the NSAIDs ranged from 2.79 to 3.79 and 0.33 to 1.27%, respectively (n = 3). The precision of the SFE method from serum was shown to be comparable to the precision obtained with other classical preparation techniques.

Selective pressurized liquid extraction of pesticides, polychlorinated biphenyls and polybrominated diphenyl ethers in a whale earplug (earwax): a novel method for analyzing organic contaminants in lipid-rich matrices.

PubMed

Robinson, Eleanor M; Trumble, Stephen J; Subedi, Bikram; Sanders, Rebel; Usenko, Sascha

2013-12-06

Lipid-rich matrices are often sinks for lipophilic contaminants, such as pesticides, polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs). Typically methods for contaminant extraction and cleanup for lipid-rich matrices require multiple cleanup steps; however, a selective pressurized liquid extraction (SPLE) technique requiring no additional cleanup has been developed for the simultaneous extraction and cleanup of whale earwax (cerumen; a lipid-rich matrix). Whale earwax accumulates in select whale species over their lifetime to form wax earplugs. Typically used as an aging technique in cetaceans, layers or laminae that comprise the earplug are thought to be associated with annual or semiannual migration and feeding patterns. Whale earplugs (earwax) represent a unique matrix capable of recording and archiving whales' lifetime contaminant profiles. This study reports the first analytical method developed for identifying and quantifying lipophilic persistent organic pollutants (POPs) in a whale earplug including organochlorine pesticides, polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs). The analytical method was developed using SPLE to extract contaminants from ∼0.25 to 0.5g aliquots of each lamina of sectioned earplug. The SPLE was optimized for cleanup adsorbents (basic alumina, silica gel, and Florisil(®)), adsorbent to sample ratio, and adsorbent order. In the optimized SPLE method, the earwax homogenate was placed within the extraction cell on top of basic alumina (5g), silica gel (15g), and Florisil(®) (10g) and the target analytes were extracted from the homogenate using 1:1 (v/v) dichloromethane:hexane. POPs were analyzed using gas chromatography-mass spectrometry with electron capture negative ionization and electron impact ionization. The average percent recoveries for the POPs were 91% (±6% relative standard deviation), while limits of detection and quantification ranged from 0.00057 to 0.96ngg(-1) and 0.0017 to 2.9ngg(-1), respectively. Pesticides, PCBs, and PBDEs, were measured in a single blue whale (Balaenoptera musculus) cerumen lamina at concentrations ranging from 0.11 to 150ng g(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of chloropropanols in foods by one-step extraction and derivatization using pressurized liquid extraction and gas chromatography-mass spectrometry.

PubMed

Racamonde, I; González, P; Lorenzo, R A; Carro, A M

2011-09-28

3-Chloropropane-1,2-diol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) were determined for the first time in bakery foods using pressurized liquid extraction (PLE) combined with in situ derivatization and GC-MS analysis. This one-step protocol uses N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) as silylation reagent. Initially, screening experimental design was applied to evaluate the effects of the variables potentially affecting the extraction process, namely extraction time (min) and temperature (°C), number of cycles, dispersant reagent (diatomaceous earth in powder form and as particulate matter with high pore volume Extrelut NT) and percent of flush ethyl acetate volume (%). To reduce the time of analysis and improve the sensitivity, derivatization of the compounds was performed in the cell extraction. Conditions, such as the volume of BSTFA, temperature and time for the in situ derivatization of analytes using PLE, were optimized by a screening design followed to a Doehlert response surface design. The effect of the in-cell dispersants/adsorbents with diatomaceous earth, Florisil and sodium sulfate anhydrous was investigated using a Box-Behnken design. Using the final best conditions, 1 g of sample dispersed with 0.1 g of sodium sulfate anhydrous and 2.5 g diatomaceous earth was extracted with ethyl acetate. 1 g of Florisil, as clean-up adsorbent, and 70 μL of BSTFA were used for 3 min at 70°C. Under the optimum conditions, the calibration curves showed good linearity (R(2)>0.9994) and precision (relative standard deviation, RSD≤2.4%) within the tested ranges. The limits of quantification for 1,3-DCP and 3-MCDP, 1.6 and 1.7 μg kg(-1), respectively, are far below the established limits in the European and American legislations. The accuracy, precision, linearity, and limits of quantification provided make this analytical method suitable for routine control. The method was applied to the analysis of several toasted bread, snacks, cookies and cereal samples, none of which contained chloropropanols at concentrations above the legislation levels. Copyright © 2011 Elsevier B.V. All rights reserved.

Pressurized solvent extraction followed by gas chromatography tandem mass spectrometry for the determination of benzotriazole light stabilizers in indoor dust.

PubMed

Carpinteiro, I; Abuín, B; Rodríguez, I; Ramil, M; Cela, R

2010-06-11

A novel and sensitive method for the determination of five benzotriazole compounds (commonly used as light stabilizers) in indoor dust is presented. Pressurized liquid extraction (PLE) and gas chromatography followed by tandem in time mass spectrometry (GC-MS/MS) were used as sample preparation and determination techniques, respectively. Extraction and clean-up were integrated on-line and, after an evaporative concentration step, the extract provided by the PLE instrument was injected directly in the GC-MS/MS system. Parameters affecting the performance of the sample preparation process were evaluated using experimental factorial designs. Under optimized conditions, analytes were recovered from 0.5g samples in 3 static extraction cycles of 10min, using a hexane:dichloromethane (7:3) mixture, at 90 degrees C. Silica (1g) was placed in the bottom of the extraction cells as clean-up sorbent. The recoveries of the method varied from 82 to 122%, with standard deviations below 13. The inter-day precision ranged from 9 to 12%, and the limits of quantification (LOQs) remained below 10ngg(-1) for all species. For the first time, four of the five investigated species were found in dust from indoor environments. Their mean concentrations ranged from 71 to 780ngg(-1). Copyright 2010 Elsevier B.V. All rights reserved.

Chemical composition, antioxidative and anti-inflammatory activity of extracts prepared from aerial parts of Oenothera biennis L. and Oenothera paradoxa Hudziok obtained after seeds cultivation.

PubMed

Granica, Sebastian; Czerwińska, Monika E; Piwowarski, Jakub P; Ziaja, Maria; Kiss, Anna K

2013-01-30

In the present study we investigated the chemical composition of extracts prepared from aerial parts of Oenothera paradoxa Hudziok and Oenothera biennis L. and their antioxidative and anti-inflammatory activities. Ultra high pressure liquid chromatography (UHPLC)-DAD-MS/MS studies showed that both extracts contain a wide variety of polyphenols (39 identified constituents) among which macrocyclic ellagitannin turned out to be the main constituent. During the in vitro studies, using noncellular models, both extracts scavenged reactive oxygen species (ROS) in a concentration-dependent manner, and the lowest SC(50) values were obtained for O(2)(-) and H(2)O(2). Both extracts inhibited ROS production by stimulated human neutrophils. The stronger activity in the case of formyl-met-leu-phenylalanine stimulation suggests that both extracts may act through the receptor-dependent pathway. O. paradoxa extract and O. biennis extract exhibited anti-inflammatory activity by the inhibition of hyaluronidase and lipoxygenase in a concentration-dependent manner. The stronger activity of O.biennis extract toward lipoxygenase may be explained by its higher oenothein B content.

Identification of pesticide transformation products in agricultural soils using liquid chromatography/quadrupole-time-of-flight mass spectrometry.

PubMed

Padilla-Sánchez, Juan A; Michael Thurman, E; Plaza-Bolaños, Patricia; Ferrer, Imma

2012-05-15

A study of pesticide transformation products (TPs) was carried out in soils of agricultural areas working under integrated pest management programs (IPMs). Bupirimate and cyromazine were the pesticides detected in soils after an initial pre-screening. The aim of this work was the identification of relevant TPs of these two pesticides. Soil samples were extracted by pressurized liquid extraction (PLE), using a mixture of ethyl acetate/methanol (3:1, v/v), and analyzed by ultra-high-pressure liquid chromatography coupled to hybrid quadrupole-time-of-flight mass spectrometry (UHPLC-QTOF-MS). For confirmation purposes, tandem mass spectrometry (MS(2) ) experiments were carried out using QTOF-MS, obtaining specific fragment structures of the pesticides and their degradates. Retention times and exact masses of the protonated molecules were used for the identification of the pesticides bupirimate (m/z 317.1642) and cyromazine (m/z 167.1040) and their respective TPs, namely ethirimol (m/z 210.1601) and melamine (m/z 127.0727). A novel strategy using pseudo-MS(3) experiments was developed to confirm the structure of bupirimate TP (ethirimol). This strategy consists of generating the particular TP in the ion source, via collision-induced fragmentation, and then performing MS/MS to the fragment ion formed in-source. Ethirimol and melamine were identified as degradation products of bupirimate and cyromazine, respectively. The study was applied to the analysis of 15 agricultural soil samples finding bupirimate and ethirimol in seven samples, cyromazine in one sample and melamine in four samples. Copyright © 2012 John Wiley & Sons, Ltd.

Ionic-liquid-impregnated resin for the microwave-assisted solid-liquid extraction of triazine herbicides in honey.

PubMed

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

2015-09-01

Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Subcritical water extractor for Mars analog soil analysis.

PubMed

Amashukeli, Xenia; Grunthaner, Frank J; Patrick, Steven B; Yung, Pun To

2008-06-01

Abstract Technologies that enable rapid and efficient extraction of biomarker compounds from various solid matrices are a critical requirement for the successful implementation of in situ chemical analysis of the martian regolith. Here, we describe a portable subcritical water extractor that mimics multiple organic solvent polarities by tuning the dielectric constant of liquid water through adjustment of temperature and pressure. Soil samples, collected from the Yungay region of the Atacama Desert (martian regolith analogue) in the summer of 2005, were used to test the instrument's performance. The total organic carbon was extracted from the samples at concentrations of 0.2-55.4 parts per million. The extraction data were compared to the total organic carbon content in the bulk soil, which was determined via a standard analytical procedure. The instrument's performance was examined over the temperature range of 25-250 degrees C at a fixed pressure of 20.7 MPa. Under these conditions, water remains in a subcritical fluid state with a dielectric constant varying between approximately 80 (at 25 degrees C) and approximately 30 (at 250 degrees C).

Quantification of caffeine, trigonelline and nicotinic acid in espresso coffee: the influence of espresso machines and coffee cultivars.

PubMed

Caprioli, Giovanni; Cortese, Manuela; Maggi, Filippo; Minnetti, Caterina; Odello, Luigi; Sagratini, Gianni; Vittori, Sauro

2014-06-01

Caffeine, trigonelline and nicotinic acid are important bioactive constituents of coffee. In this work, the combination of different water temperatures and pressures in the settings of the espresso coffee (EC) machine was evaluated, to assess how these factors influence how effectively caffeine, trigonelline and nicotinic acid are extracted from both Arabica and Robusta samples. The proposed analytical method, based on a high performance liquid chromatography (HPLC) system coupled to a variable wavelength detector (VWD), showed good linearity (R²> 0.9985) and good recoveries (71-92%); after validation for three monitored compounds, the method was used to analyze 20 commercial samples. The combination of a temperature of 92 °C and pressure at 7 or 9 bar seems to be the ideal setting for the most efficient extraction of these compounds and consequently for their intake; the compound extracted in the greatest quantity was caffeine, which was in the range of 116.87-199.68 mg in a 25 ml cup of coffee.

Ternary liquid-liquid equilibria for the phenolic compounds extraction from artificial textile industrial waste

NASA Astrophysics Data System (ADS)

Fardhyanti, Dewi Selvia; Prasetiawan, Haniif; Hermawan, Sari, Lelita Sakina

2017-03-01

Liquid waste in textile industry contains large amounts of dyes and chemicals which are capable of harming the environment and human health. It is due to liquid waste characteristics which have high BOD, COD, temperature, dissolved and suspended solid. One of chemical compound which might be harmful for environment when disposed in high concentration is phenol. Currently, Phenol compound in textile industrial waste has reached 10 ppm meanwhile maximum allowable phenol concentration is not more than 0.2 ppm. Otherwise, Phenol also has economic value as feedstock of plastic, pharmaceutical and cosmetic industry. Furthermore, suitable method to separate phenol from waste water is needed. In this research, liquid - liquid extraction method was used with extraction time for 70 minutes. Waste water sample was then separated into two layers which are extract and raffinate. Thereafter, extract and raffinate were then tested by using UV-Vis Spectrophotometer to obtained liquid - liquid equilibrium data. Aim of this research is to study the effect of temperature, stirring speed and type of solvent to obtain distribution coefficient (Kd), phenol yield and correlation of Three-Suffix Margules model for the liquid - liquid extraction data equilibrium. The highest extraction yield at 80.43 % was found by using 70% methanol as solvent at extraction temperature 50 °C with stirring speed 300 rpm, coefficient distribution was found 216.334. From this research it can be concluded that Three-Suffix Margules Model is suitable to predict liquid - liquid equilibrium data for phenol system.

Selective pressurized liquid extraction of replacement and legacy brominated flame retardants from soil.

PubMed

McGrath, Thomas J; Morrison, Paul D; Ball, Andrew S; Clarke, Bradley O

2016-08-05

Polybrominated diphenyl ethers (PBDEs) are a class of flame retardant registered as UN POPs due to their persistence in the environment, bioaccumulation potential and toxicity. Replacement novel brominated flame retardants (NBFRs) have exhibited similar health hazards and environmental distribution, becoming recognized as significant contaminants. This work describes the development and validation of a sensitive and reliable method for the simultaneous quantitation of PBDEs and NBFRs in environmental soil samples using selective pressurized liquid extraction (S-PLE) and gas chromatography coupled to triple quadrupole mass spectrometry (GC-(EI)-MS/MS). Under optimal conditions, extraction of eight PBDEs (-28, -47, -99, -100, -153, -154, -183 and -209) and five NBFRs; pentabromotoluene (PBT), pentabromoethylbenzene (PBEB), hexabromobenzene (HBB), 2-ethylhexyl-2,3,4,5-tetrabromobenzoate (EH-TBB) and bis(2,4,6-tribromophenoxy)ethane (BTBPE) was performed at 100°C and 1500psi using a 1:1 mixture of hexane and dichloromethane. The method utilized 33mL capacity PLE cells containing, from bottom to top, a single cellulose filter, 3g activated Florisil, 6g acid silica (10% w/w), 3g Na2SO4, another cellulose filter, 2g activated copper powder and 3g soil sample dispersed in 2g Na2SO4 and 1g of Hydromatrix. The method was evaluated by repeated extraction and analysis of all analytes from 3g soil at three spike concentrations. Good recoveries were observed for most analytes at each of the spiking levels with RSD values generally below 20%. MDLs ranged from 0.01 to 4.8ng/g dw for PBDEs and 0.01-0.55ng/g dw for NBFRs. The described one-step combined extraction and cleanup method reduces sample processing times compared with traditional procedures, while delivering comparable analytical performance. The method was successfully applied to environmental soil samples (n=5), detecting PBDEs in each sample and providing the first account of NBFR contamination in Australian soils. Copyright © 2016 Elsevier B.V. All rights reserved.

Pressure Induced Liquid-to-Liquid Transition in Zr-based Supercooled Melts and Pressure Quenched Glasses.

PubMed

Dmowski, W; Gierlotka, S; Wang, Z; Yokoyama, Y; Palosz, B; Egami, T

2017-07-26

Through high-energy x-ray diffraction and atomic pair density function analysis we find that Zr-based metallic alloy, heated to the supercooled liquid state under hydrostatic pressure and then quenched to room temperature, exhibits a distinct glassy structure. The PDF indicates that the Zr-Zr distances in this glass are significantly reduced compared to those quenched without pressure. Annealing at the glass transition temperature at ambient pressure reverses structural changes and the initial glassy state is recovered. This result suggests that pressure causes a liquid-to-liquid phase transition in this metallic alloy supercooled melt. Such a pressure induced transition is known for covalent liquids, but has not been observed for metallic liquids. The High Pressure Quenched glasses are stable in ambient conditions after decompression.

Bergamot (Citrus bergamia Risso) fruit extracts as γ-globin gene expression inducers: phytochemical and functional perspectives.

PubMed

Guerrini, Alessandra; Lampronti, Ilaria; Bianchi, Nicoletta; Zuccato, Cristina; Breveglieri, Giulia; Salvatori, Francesca; Mancini, Irene; Rossi, Damiano; Potenza, Rocco; Chiavilli, Francesco; Sacchetti, Gianni; Gambari, Roberto; Borgatti, Monica

2009-05-27

Epicarps of Citrus bergamia fruits from organic farming were extracted with the objective of obtaining derived products differently rich in coumarins and psoralens. The extracts were chemically characterized by (1)H nuclear magnetic resonance (NMR), gas chromatography-flame ionization detection (GC-FID), gas chromatography-mass spectrometry (GC-MS), and high-pressure liquid chromatography (HPLC) for detecting and quantifying the main constituents. Both bergamot extracts and chemical standards corresponding to the main constituents detected were then assayed for their capacity to increase erythroid differentiation of K562 cells and expression of γ-globin genes in human erythroid precursor cells. Three experimental cell systems were employed: (a) the human leukemic K562 cell line, (b) K562 cell clones stably transfected with a pCCL construct carrying green-enhanced green fluorescence protein (EGFP) under the γ-globin gene promoter, and (c) the two-phase liquid culture of human erythroid progenitors isolated from healthy donors. The results suggest that citropten and bergapten are powerful inducers of differentiation and γ-globin gene expression in human erythroid cells. These data could have practical relevance, because pharmacologically mediated regulation of human γ-globin gene expression, with the consequent induction of fetal hemoglobin, is considered to be a potential therapeutic approach in hematological disorders, including β-thalassemia and sickle cell anemia.

SEPARATION AND PURIFICATION OF TWO MINOR COMPOUNDS FROM RADIX ISATIDIS BY INTEGRATIVE MPLC AND HSCCC WITH PREPARATIVE HPLC.

PubMed

Liang, Zhenjie; Li, Bin; Liang, Yong; Su, Yaping; Ito, Yoichiro

2015-01-01

Radix isatidis has been widely used as a Chinese traditional medicine for its anti-virus and anticancer activities where the minor components may contribute to these beneficial pharmaceutical effects. In order to enrich the target minor compounds effectively and rapidly, extraction, medium-pressure liquid chromatography (MPLC), high-speed countercurrent chromatography (HSCCC) and preparative high-performance liquid chromatography (pre-HPLC) were integratively used for separation and purification of two target minor compounds indole-3-acetonitrile-6-O-β-D-glucopyranoside (target 1) and clemastanin B (target 2) in the present study. Radix isatidis was dried, pulverized and extracted with 50% methanol at room temperature, then concentrated and subjected to pretreatment with D-101 macroporous resin chromatography and extraction by MPLC. The first target compound was separated by MPLC at the purity raised to 70-80%, but without the second minor compounds which were irreversibly adsorbed by C18 solid support. Therefore, the second target compound in the crude extract was directly separated by HSCCC at purity of 80-90%. Finally these refined samples were further separated by pre-HPLC to obtain a high purity at 98-99%. The chemical structure identification of each target compound was carried out by IR, ESI-MS and 1 H NMR.

Secondary Metabolites in Ramalina terebrata Detected by UHPLC/ESI/MS/MS and Identification of Parietin as Tau Protein Inhibitor.

PubMed

Cornejo, Alberto; Salgado, Francisco; Caballero, Julio; Vargas, Reinaldo; Simirgiotis, Mario; Areche, Carlos

2016-08-18

Liquid chromatography coupled with mass spectrometry is an outstanding methodology for fast analysis of phenolic compounds in biological samples. Twenty two compounds were quickly and accurately identified in the methanolic extract of the Antarctic lichen Ramalina terebrata for the first time using ultra high pressure liquid chromatography coupled with photodiode array detector and high resolution mass spectrometry (UHPLC-PDA-Q/Orbitrap/MS/MS). In addition, the extract and the four compounds isolated from this species were tested for the inhibitory activity of tau protein aggregation, which is a protein involved in Alzheimer's disease (AD). All compounds showed null activity with the exception of parietin, which it was able to inhibit aggregation process of tau in a concentration range between 3 µg/mL (10 µM) to 28 µg/mL (100 µM). In addition, we show how parietin interact with tau (306)VQIVYK(311) hexapeptide inside of the microtubule binding domain (4R) with the help of molecular docking experiments. Finally, the constituents present in the methanolic extract could possibly contribute to the established anti-aggregation activity for this extract and this in-depth analysis of the chemical composition of R. terebrata could guide further research into its medicinal properties and potential uses.

Secondary Metabolites in Ramalina terebrata Detected by UHPLC/ESI/MS/MS and Identification of Parietin as Tau Protein Inhibitor

PubMed Central

Cornejo, Alberto; Salgado, Francisco; Caballero, Julio; Vargas, Reinaldo; Simirgiotis, Mario; Areche, Carlos

2016-01-01

Liquid chromatography coupled with mass spectrometry is an outstanding methodology for fast analysis of phenolic compounds in biological samples. Twenty two compounds were quickly and accurately identified in the methanolic extract of the Antarctic lichen Ramalina terebrata for the first time using ultra high pressure liquid chromatography coupled with photodiode array detector and high resolution mass spectrometry (UHPLC-PDA-Q/Orbitrap/MS/MS). In addition, the extract and the four compounds isolated from this species were tested for the inhibitory activity of tau protein aggregation, which is a protein involved in Alzheimer’s disease (AD). All compounds showed null activity with the exception of parietin, which it was able to inhibit aggregation process of tau in a concentration range between 3 µg/mL (10 µM) to 28 µg/mL (100 µM). In addition, we show how parietin interact with tau 306VQIVYK311 hexapeptide inside of the microtubule binding domain (4R) with the help of molecular docking experiments. Finally, the constituents present in the methanolic extract could possibly contribute to the established anti-aggregation activity for this extract and this in-depth analysis of the chemical composition of R. terebrata could guide further research into its medicinal properties and potential uses. PMID:27548142

Effect of purity on adsorption capacities of a Mars-like clay mineral at different pressures

NASA Technical Reports Server (NTRS)

Jenkins, Traci; Mcdoniel, Bridgett; Bustin, Roberta; Allton, Judith H.

1992-01-01

There has been considerable interest in adsorption of carbon dioxide on Marslike clay minerals. Some estimates of the carbon dioxide reservoir capacity of the martian regolith were calculated from the amount of carbon dioxide adsorbed on the ironrich smectite nontronite under martian conditions. The adsorption capacity of pure nontronite could place upper limits on the regolith carbon dioxide reservoir, both at present martian atmospheric pressure and at the postulated higher pressures required to permit liquid water on the surface. Adsorption of carbon dioxide on a Clay Mineral Society standard containing nontronite was studied over a wide range of pressures in the absence of water. Similar experiments were conducted on the pure nontronite extracted from the natural sample. Heating curves were obtained to help characterize and determine the purity of the clay sample.

Effect of aqueous extracts of Mentha arvensis (mint) and Piper betle (betel) on growth and citrinin production from toxigenic Penicillium citrinum.

PubMed

Panda, Pragyanshree; Aiko, Visenuo; Mehta, Alka

2015-06-01

Due to growing concern of consumers about chemical residues in food products, the demand for safe and natural food is increasing greatly. The use of natural additives such as spices and herbal oil as seasoning agents for their antimicrobial activity has been extensively investigated. This paper discusses the efficacy of the aqueous extract of mint (Mentha arvensis) and betel (Piper betle) on the mycelial growth and citrinin production of Penicillium citrinum. The present investigation revealed that mint extract inhibited citrinin production up to 73 % without inhibiting the mycelium growth. The citrinin production decreased with increase in the concentration of mint extract as observed from the data obtained from High pressure liquid chromatography. The samples also showed reduced cytotoxicity on HeLa cells. On the other hand betel extract resulted in stimulatory effect on citrinin production and mycelial growth. The study showed that mint extract has the potential to be used safely for restraining citrinin contamination.

Analysis of Phenolic Compounds and Antioxidant Activity in Wild Blackberry Fruits

PubMed Central

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

2015-01-01

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

Summer 2017 Microfluidics Research Report

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

Mcculloch, Quinn

Liquid-liquid Extraction (LLE), also known as solvent extraction, represents a large subset of chemistry where one or more solutes are transferred across an interface between two immiscible liquids. This type of chemistry is used in industrial scale processes to purify solvents, refine ore, process petroleum, treat wastewater, and much more. Although LLE has been successfully employed at the macroscale, where many liters/kgs of species are processed at large flow rates, LLE stands to benefit from lab-on-a-chip technology, where reactions take place quickly and efficiently at the microscale. A device, called a screen contactor, has been invented at Los Alamos Nationalmore » Laboratory (LANL) to perform solvent extraction at the microscale. This invention has been submitted to LANL’s Feynman Center for Innovation, and has been filed for provisional patent under U.S. Patent Application No. 62/483,107 1. The screen contactor consists of a housing that contains two different screen materials, flametreated stainless steel and polyether ether ketone (PEEK) thermoplastic, that are uniquely wetted by either an aqueous or an organic liquid phase, respectively. Liquids in this device flow longitudinally through the screens. The fine pore size of the screens (tens of microns) provide large capillary/adhesional forces while maintaining small hydraulic pressure drops. These physical characteristics are paramount to efficient microscale liquid phase separation. To demonstrate mass transfer using the screen contactor, a well-known chemical system 2 consisting of water and n-decane as solvents and trimethylamine (TEA) as a solute was selected. TEA is basic in water so its concentration can easily be quantified using a digital pH meter and an experimentally determined base dissociation constant. Characterization of this solvent system and its behavior in the screen contactor have been the focus of my research activities this summer. In the following sections, I have detailed experimental results that have been gathered.« less

Preparation of magnetic chitosan and graphene oxide-functional guanidinium ionic liquid composite for the solid-phase extraction of protein.

PubMed

Ding, Xueqin; Wang, Yuzhi; Wang, Ying; Pan, Qi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

2015-02-25

A series of novel cationic functional hexaalkylguanidinium ionic liquids and anionic functional tetraalkylguanidinium ionic liquids have been synthesized, and then magnetic chitosan graphene oxide (MCGO) composite has been prepared and coated with these functional guanidinium ionic liquids to extract protein by magnetic solid-phase extraction. MCGO-functional guanidinium ionic liquid has been characterized by vibrating sample magnetometer, field emission scanning electron microscopy, X-ray diffraction spectrometer and Fourier transform infrared spectrometer. After extraction, the concentrations of protein were determined by measuring the absorbance at 278 nm using an ultra violet visible spectrophotometer. The advantages of MCGO-functional guanidinium ionic liquid in protein extraction were compared with magnetic chitosan, graphene oxide, MCGO and MCGO-ordinary imidazolium ionic liquid. The proposed method has been applied to extract trypsin, lysozyme, ovalbumin and bovine serum albumin. A comprehensive study of the adsorption conditions such as the concentration of protein, the amount of MCGO-functional guanidinium ionic liquid, the pH, the temperature and the extraction time were also presented. Moreover, the MCGO-functional guanidinium ionic liquid can be easily regenerated, and the extraction capacity was about 94% of the initial one after being used three times. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

PubMed

Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

2016-10-01

A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An integrated platform for directly widely-targeted quantitative analysis of feces part I: Platform configuration and method validation.

PubMed

Song, Yuelin; Song, Qingqing; Li, Jun; Zheng, Jiao; Li, Chun; Zhang, Yuan; Zhang, Lingling; Jiang, Yong; Tu, Pengfei

2016-07-08

Direct analysis is of great importance to understand the real chemical profile of a given sample, notably biological materials, because either chemical degradation or diverse errors and uncertainties might be resulted from sophisticated protocols. In comparison with biofluids, it is still challenging for direct analysis of solid biological samples using high performance liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Herein, a new analytical platform was configured by online hyphenating pressurized liquid extraction (PLE), turbulent flow chromatography (TFC), and LC-MS/MS. A facile, but robust PLE module was constructed based on the phenomenon that noticeable back-pressure can be generated during rapid fluid passing through a narrow tube. TFC column that is advantageous at extracting low molecular analytes from rushing fluid was employed to link at the outlet of the PLE module to capture constituents-of-interest. An electronic 6-port/2-position valve was introduced between TFC column and LC-MS/MS to fragment each measurement into extraction and elution phases, whereas LC-MS/MS took the charge of analyte separation and monitoring. As a proof of concept, simultaneous determination of 24 endogenous substances including eighteen steroids, five eicosanoids, and one porphyrin in feces was carried out in this paper. Method validation assays demonstrated the analytical platform to be qualified for directly simultaneous measurement of diverse endogenous analytes in fecal matrices. Application of this integrated platform on homolog-focused profiling of feces is discussed in a companion paper. Copyright © 2016 Elsevier B.V. All rights reserved.

Superbase-derived protic ionic liquid extractants for metal ion separation

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

Bell, Jason R.; Dai, Sheng; Luo, Huimin

2014-04-19

Solvent extraction of La 3+ and Ba 2+ by an ionic liquid extractant in an imidazolium-based ionic liquid diluent was investigated. Seven protic ionic liquid extractants were examined and these protic ILs are based on five organic superbases and either 6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octadione (Hfod) or 1,1,1,5,5,5-hexafluoroacetylacetone (Hhfac) -diketones as anion. For fod-based extractants, the extraction efficiencies and separation factors were found to be concentration dependent. The effects of aqueous phase acidity, extractant structure, and extractant concentration on separation properties of La 3+ and Ba 2+ are discussed in this paper.

Pressure Induced Liquid-to-Liquid Transition in Zr-based Supercooled Melts and Pressure Quenched Glasses

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

Dmowski, W.; Gierlotka, S.; Wang, Z.

Through high-energy x-ray diffraction and atomic pair density function analysis we find that Zr-based metallic alloy, heated to the supercooled liquid state under hydrostatic pressure and then quenched to room temperature, exhibits a distinct glassy structure. The PDF indicates that the Zr-Zr distances in this glass are significantly reduced compared to those quenched without pressure. Annealing at the glass transition temperature at ambient pressure reverses structural changes and the initial glassy state is recovered. This result suggests that pressure causes a liquid-to-liquid phase transition in this metallic alloy supercooled melt. Such a pressure induced transition is known for covalent liquids,more » but has not been observed for metallic liquids. The High Pressure Quenched glasses are stable in ambient conditions after decompression.« less

Recent progress of task-specific ionic liquids in chiral resolution and extraction of biological samples and metal ions.

PubMed

Wu, Datong; Cai, Pengfei; Zhao, Xiaoyong; Kong, Yong; Pan, Yuanjiang

2018-01-01

Ionic liquids have been functionalized for modern applications. The functional ionic liquids are also called task-specific ionic liquids. Various task-specific ionic liquids with certain groups have been constructed and exploited widely in the field of separation. To take advantage of their properties in separation science, task-specific ionic liquids are generally used in techniques such as liquid-liquid extraction, solid-phase extraction, gas chromatography, high-performance liquid chromatography, and capillary electrophoresis. This review mainly covers original research papers published in the last five years, and we will focus on task-specific ionic liquids as the chiral selectors in chiral resolution and as extractant or sensor for biological samples and metal ion purification. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Matrix effect and correction by standard addition in quantitative liquid chromatographic-mass spectrometric analysis of diarrhetic shellfish poisoning toxins.

PubMed

Ito, Shinya; Tsukada, Katsuo

2002-01-11

An evaluation of the feasibility of liquid chromatography-mass spectrometry (LC-MS) with atmospheric pressure ionization was made for quantitation of four diarrhetic shellfish poisoning toxins, okadaic acid, dinophysistoxin-1, pectenotoxin-6 and yessotoxin in scallops. When LC-MS was applied to the analysis of scallop extracts, large signal suppressions were observed due to coeluting substances from the column. To compensate for these matrix signal suppressions, the standard addition method was applied. First, the sample was analyzed and then the sample involving the addition of calibration standards is analyzed. Although this method requires two LC-MS runs per analysis, effective correction of quantitative errors was found.

Application of liquid chromatography-electrospray ionization mass spectrometry for study of steroid-converting enzymes.

PubMed

Miksík, Ivan; Mikulíková, Katerina; Pácha, Jirí; Kucka, Marek; Deyl, Zdenek

2004-02-05

A high-performance liquid chromatography-atmospheric pressure ionization-electrospray ionization mass spectrometry (HPLC-API-ESI-MS) method was developed for the analysis of steroids in a study of steroid-converting enzymes. Separations ware done on a Zorbax Eclipse XDB-C18 column (eluted with a linear methanol-water-acetic acid gradient) and identification of the steroids involved was done by API-ESI-MS using positive ion mode and extracted ion analysis. The applicability of the present method for studying steroid metabolism was proven in assaying two steroid-converting enzymes (20beta-hydroxysteroid dehydrogenase and 11beta-hydroxysteroid dehydrogenase) in various biological samples (rat and chicken intestine, chicken oviduct).

Phytochemical analysis of Hibiscus caesius using high performance liquid chromatography coupled with mass spectrometry.

PubMed

Ain, Quratul; Naveed, Muhammad Na; Mumtaz, Abdul Samad; Farman, Muhammad; Ahmed, Iftikhar; Khalid, Nauman

2015-09-01

Various species in genus Hibiscus are traditionally known for their therapeutic attributes. The present study focused on the phytochemical analysis of a rather unexplored species Hibiscus caesius (H. caesius), using high-pressure liquid chromatography coupled with mass spectrometry (HPLC-MS). The analysis revealed five major compounds in the aqueous extract, viz. vanillic acid, protocatechoic acid, quercetin, quercetin glucoside and apigenin, being reported for the first time in H. caesius. Literature suggests that these compounds have important pharmacological traits such as anti-cancer, anti-inflammatory, anti-bacterial and hepatoprotective etc. however, this requires further pharmacological investigations at in vitro and in vivo scale. The above study concluded the medicinal potential of H. caesius.

Displacement-dispersive liquid-liquid microextraction based on solidification of floating organic drop of trace amounts of palladium in water and road dust samples prior to graphite furnace atomic absorption spectrometry determination.

PubMed

Ghanbarian, Maryam; Afzali, Daryoush; Mostafavi, Ali; Fathirad, Fariba

2013-01-01

A new displacement-dispersive liquid-liquid microextraction method based on the solidification of floating organic drop was developed for separation and preconcentration of Pd(ll) in road dust and aqueous samples. This method involves two steps of dispersive liquid-liquid microextraction based on solidification. In Step 1, Cu ions react with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which is extracted by dispersive liquid-liquid microextraction based on a solidification procedure using 1-undecanol (extraction solvent) and ethanol (dispersive solvent). In Step 2, the extracted complex is first dispersed using ethanol in a sample solution containing Pd ions, then a dispersive liquid-liquid microextraction based on a solidification procedure is performed creating an organic drop. In this step, Pd(ll) replaces Cu(ll) from the pre-extracted Cu-DDTC complex and goes into the extraction solvent phase. Finally, the Pd(ll)-containing drop is introduced into a graphite furnace using a microsyringe, and Pd(ll) is determined using atomic absorption spectrometry. Several factors that influence the extraction efficiency of Pd and its subsequent determination, such as extraction and dispersive solvent type and volume, pH of sample solution, centrifugation time, and concentration of DDTC, are optimized.

Visual outcomes after balanced salt solution infiltration during lenticule separation in small-incision lenticule extraction for myopic astigmatism.

PubMed

Liu, Ting; Zhu, Xiaomin; Chen, Kaijian; Bai, Ji

2017-07-01

To evaluate the refractive outcomes of balanced salt solution infiltration during small-incision lenticule extraction (SMILE).This randomized prospective study enrolled 52 patients (104 eyes) with myopic astigmatism. Patients underwent SMILE to correct the myopic astigmatism in Daping Hospital of the Third Military Medical University between January and July 2013. One eye of each patient received traditional SMILE (control group) and the other received a modified SMILE procedure (liquid infiltration group). The corrected distance visual acuity (CDVA), postoperative uncorrected distance visual acuity (UDVA), refraction, wavefront aberration, intraocular pressure (IOP), modulation transfer function (MTF) cut-off frequency, and objective scattering index (OSI) were evaluated.UDVA in the liquid infiltration group was significantly higher than that in the control group at 1 day postoperatively, but not at 1 month after surgery. Moreover, OSI and MTF cut-off frequency in the liquid infiltration group were higher than those in the control group at early follow-up. However, no significant intergroup difference was observed in the OSI and MTF cut-off frequency at 3 months after surgery. In addition, the predictability was better in the liquid infiltration group than in the control group. The changes of horizontal coma in the liquid infiltration group were lesser than those in the control group. However, no intergroup difference was observed in the reduction of IOP at 1 month after surgery.The modified SMILE procedure results in better visual outcomes than did the traditional SMILE procedure when used for treating myopic astigmatism.

40 CFR 265.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 25 2010-07-01 2010-07-01 false Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service...

40 CFR 264.1058 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 25 2010-07-01 2010-07-01 false Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and other... heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and flanges and...

Analysis of the extracts of Isatis tinctoria by new analytical approaches of HPLC, MS and NMR.

PubMed

Zhou, Jue; Qu, Fan

2011-01-01

The methods of extraction, separation and analysis of alkaloids and indole glucosinolates (GLs) ofIsatis tinctoria were reviewed. Different analytical approaches such as High-pressure Liquid Chromatography (HPLC), Liquid Chromatography with Electrospray Ionization Mass Spectrometry (LC/ESI/MS), Electrospray Ionization Time-Of-Flight Mass Spectrometry (ESI-TOF-MS), and Nuclear Magnetic Resonance (NMR) were used to validate and identity of these constituents. These methods provide rapid separation, identification and quantitative measurements of alkaloids and GLs of Isatis tinctoria. By connection with different detectors to HPLC such as PDA, ELSD, ESI- and APCI-MS in positive and negative ion modes, complicated compounds could be detected with at least two independent detection modes. The molecular formula can be derived in a second step of ESI-TOF-MS data. But for some constituents, UV and MS cannot provide sufficient structure identification. After peak purification, NMR by semi-preparative HPLC can be used as a complementary method.

Apparatus and method for excluding gas from a liquid

DOEpatents

Murphy, Jr., Robert J.

1985-01-01

The present invention is directed to an apparatus and method for preventing diffusion of a gas under high pressure into the bulk of a liquid filling a substantially closed chamber. This apparatus and method is particularly useful in connection with test devices for testing fluid characteristics under harsh conditions of extremely high pressure and high temperature. These devices typically pressurize the liquid by placing the liquid in pressure and fluid communication with a high pressure inert gas. The apparatus and method of the present invention prevent diffusion of the pressurizing gas into the bulk of the test liquid by decreasing the chamber volume at a rate sufficient to maintain the bulk of the liquid free of absorbed or dissolved gas by expelling that portion of the liquid which is contaminated by the pressurizing gas.

Biological properties of the Chilean native moss Sphagnum magellanicum.

PubMed

Montenegro, Gloria; Portaluppi, Mariana C; Salas, Francisco A; Díaz, María F

2009-01-01

An ethanol extract prepared from the gametophyte Chilean native moss Sphagnum magellanicum was dried out, weighed and dissolved in distilled water. This extract was then assayed for its antibacterial activity against the G(-) bacteria Azotobacter vinelandii, Erwinia carotovora subsp. carotovora, Enterobacter aerogenes, Escherichia coli, Pseudomonas aeruginosa, Salmonella typhi, Vibrio cholerae, and the G(+) bacteria Staphylococcus aureus subsp. aureus, and Streptococcus type beta. The growth of the cultures of E. carotovora subsp. carotovora, and V. cholerae was inhibited at a concentration of 581 microg/ml of extract, while the cultures of E. coli, S. typhi and Streptococcus type beta were inhibited at a concentration of 1.16 microg/mL of extract. The concentration of phenolic compounds was 4.294 mg/mL; the presence of vanillic, chlorogenic, syringic, caffeic, gallic, 3-4 hydrozybenzoic, p-coumaric and salicylic acids was identified using RP- High Pressure Liquid Chromatography.

Ultrasound-Assisted Extraction of Carnosic Acid and Rosmarinic Acid Using Ionic Liquid Solution from Rosmarinus officinalis

PubMed Central

Zu, Ge; Zhang, Rongrui; Yang, Lei; Ma, Chunhui; Zu, Yuangang; Wang, Wenjie; Zhao, Chunjian

2012-01-01

Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C8mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid–liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential. PMID:23109836

40 CFR 63.169 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation...

Code of Federal Regulations, 2013 CFR

2013-07-01

..., and agitators in heavy liquid service; instrumentation systems; and pressure relief devices in liquid...: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation systems; and pressure..., pressure relief devices in light liquid or heavy liquid service, and instrumentation systems shall be...

40 CFR 63.169 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation...

Code of Federal Regulations, 2011 CFR

2011-07-01

..., and agitators in heavy liquid service; instrumentation systems; and pressure relief devices in liquid...: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation systems; and pressure..., pressure relief devices in light liquid or heavy liquid service, and instrumentation systems shall be...

40 CFR 63.169 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation...

Code of Federal Regulations, 2014 CFR

2014-07-01

..., and agitators in heavy liquid service; instrumentation systems; and pressure relief devices in liquid...: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation systems; and pressure..., pressure relief devices in light liquid or heavy liquid service, and instrumentation systems shall be...

40 CFR 63.169 - Standards: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation...

Code of Federal Regulations, 2012 CFR

2012-07-01

..., and agitators in heavy liquid service; instrumentation systems; and pressure relief devices in liquid...: Pumps, valves, connectors, and agitators in heavy liquid service; instrumentation systems; and pressure..., pressure relief devices in light liquid or heavy liquid service, and instrumentation systems shall be...

METHOD OF LIQUID-LIQUID EXTRACTION OF BLOOD SURROGATES FOR ASSESSING HUMAN EXPOSURE TO JET FUEL

EPA Science Inventory

A baseline method of liquid?liquid extraction for assessing human exposure to JP-8 jet fuel was established by extracting several representative compounds ranging from very volatile to semi-volatile organic compounds, including benzene, toluene, nonane, decane, undecane, tridec...

Design criteria for extraction with chemical reaction and liquid membrane permeation

NASA Technical Reports Server (NTRS)

Bart, H. J.; Bauer, A.; Lorbach, D.; Marr, R.

1988-01-01

The design criteria for heterogeneous chemical reactions in liquid/liquid systems formally correspond to those of classical physical extraction. More complex models are presented which describe the material exchange at the individual droplets in an extraction with chemical reaction and in liquid membrane permeation.

Membrane contactor assisted extraction/reaction process employing ionic liquids

DOEpatents

Lin, Yupo J [Naperville, IL; Snyder, Seth W [Lincolnwood, IL

2012-02-07

The present invention relates to a functionalized membrane contactor extraction/reaction system and method for extracting target species from multi-phase solutions utilizing ionic liquids. One preferred embodiment of the invented method and system relates to an extraction/reaction system wherein the ionic liquid extraction solutions act as both extraction solutions and reaction mediums, and allow simultaneous separation/reactions not possible with prior art technology.

Hybrid joule heating/electro-osmosis process for extracting contaminants from soil layers

DOEpatents

Carrigan, Charles R.; Nitao, John J.

2003-06-10

Joule (ohmic) heating and electro-osmosis are combined in a hybrid process for removal of both water-soluble contaminants and non-aqueous phase liquids from contaminated, low-permeability soil formations that are saturated. Central to this hybrid process is the partial desaturation of the formation or layer using electro-osmosis to remove a portion of the pore fluids by induction of a ground water flow to extraction wells. Joule heating is then performed on a partially desaturated formation. The joule heating and electro-osmosis operations can be carried out simultaneously or sequentially if the desaturation by electro-osmosis occurs initially. Joule heating of the desaturated formation results in a very effective transfer or partitioning of liquid state contaminants to the vapor phase. The heating also substantially increases the vapor phase pressure in the porous formation. As a result, the contaminant laden vapor phase is forced out into soil layers of a higher permeability where other conventional removal processes, such as steam stripping or ground water extraction can be used to capture the contaminants. This hybrid process is more energy efficient than joule heating or steam stripping for cleaning low permeability formations and can share electrodes to minimize facility costs.

Quantitative analysis of anti-inflammatory and radical scavenging triterpenoid esters in evening primrose seeds.

PubMed

Zaugg, Janine; Potterat, Olivier; Plescher, Andreas; Honermeier, Bernd; Hamburger, Matthias

2006-09-06

Lipophilic triterpenoidal esters with radical scavenging and cyclooxygenase inhibitory properties were recently found in cold-pressed, nonraffinated evening primrose oil (EPO). A quantitative assay for the analysis of 3-O-trans-caffeoyl derivatives of betulinic, morolic, and oleanolic acid in evening primrose seeds was developed and validated. Extraction efficiency >99% was achieved by means of pressurized liquid extraction with two extraction cycles and 80% (v/v) ethanol at 120 degrees C. Analysis of esters was by normal-phase high-performance liquid chromatography on a Diol column and hexane/ethyl acetate (containing 0.1% formic acid) (65:35) as the eluent. The analytes were determined without further prepurification. Seeds from defined cultures of Oenothera biennis, Oenothera lamarckiana, and Oenothera ammophila, grown under identical conditions, were analyzed. The cultures originated from seeds from eight collections in the wild and from selections from five cultivars. The content of total triterpenoidal esters in seeds varied between 1.34 and 2.78 mg/g. Three types of qualitative patterns were observed for the triterpenoidal esters. The influence of different harvest times and plant treatments was studied with the cultivar Anothera. Variations between 1.5 and 2.3 mg/g were found.

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

PubMed

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

2016-01-15

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

Empirical Correlations for the Solubility of Pressurant Gases in Cryogenic Propellants

NASA Technical Reports Server (NTRS)

Zimmerli, Gregory A.; Asipauskas, Marius; VanDresar, Neil T.

2010-01-01

We have analyzed data published by others reporting the solubility of helium in liquid hydrogen, oxygen, and methane, and of nitrogen in liquid oxygen, to develop empirical correlations for the mole fraction of these pressurant gases in the liquid phase as a function of temperature and pressure. The data, compiled and provided by NIST, are from a variety of sources and covers a large range of liquid temperatures and pressures. The correlations were developed to yield accurate estimates of the mole fraction of the pressurant gas in the cryogenic liquid at temperature and pressures of interest to the propulsion community, yet the correlations developed are applicable over a much wider range. The mole fraction solubility of helium in all these liquids is less than 0.3% at the temperatures and pressures used in propulsion systems. When nitrogen is used as a pressurant for liquid oxygen, substantial contamination can result, though the diffusion into the liquid is slow.

40 CFR 60.482-8 - Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or...

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 6 2010-07-01 2010-07-01 false Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid service, and connectors. 60.482-8... Standards: Pumps and valves in heavy liquid service, pressure relief devices in light liquid or heavy liquid...

Novel Fission-Product Separation based on Room-Temperature Ionic Liquids

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

Rogers, Robin D.

2004-12-31

U.S. DOE's underground storage tanks at Hanford, SRS, and INEEL contain liquid wastes with high concentrations of radioactive cesium-137 and strontium-90. Because the primary chemical components of alkaline supernatants are sodium nitrate and sodium hydroxide, the majority of this could be disposed of as low level waste if radioactive cesium-137 and strontium- 90 could be selectively removed. The underlying goal of this project was to investigate the application of ionic liquids as novel solvents for new solvent extraction processes for separation of cesium-137 and strontium-90 from tank wastes. Ionic liquids are a distinct sub-set of liquids, comprising only of cationsmore » and anions they are proving to be increasingly interesting fluids for application in systems from electrochemistry to energetic materials, and are also rapidly establishing their promise as viable media for synthesis and separations operations. Properties including low melting points, electrochemical conductivity, wide liquid ranges, lack of vapor-pressure, and chemical tunability have encouraged researchers to explore the uses of ILs in place of volatile organic solvents. The most promising current developments arise from control of the unique combinations of chemical and physical properties characteristic of ionic liquids.« less

An ultrasound-based liquid pressure measurement method in small diameter pipelines considering the installation and temperature.

PubMed

Li, Xue; Song, Zhengxiang

2015-04-09

Liquid pressure is a key parameter for detecting and judging faults in hydraulic mechanisms, but traditional measurement methods have many deficiencies. An effective non-intrusive method using an ultrasound-based technique to measure liquid pressure in small diameter (less than 15 mm) pipelines is presented in this paper. The proposed method is based on the principle that the transmission speed of an ultrasonic wave in a Kneser liquid correlates with liquid pressure. Liquid pressure was calculated using the variation of ultrasonic propagation time in a liquid under different pressures: 0 Pa and X Pa. In this research the time difference was obtained by an electrical processing approach and was accurately measured to the nanosecond level through a high-resolution time measurement module. Because installation differences and liquid temperatures could influence the measurement accuracy, a special type of circuit called automatic gain control (AGC) circuit and a new back propagation network (BPN) model accounting for liquid temperature were employed to improve the measurement results. The corresponding pressure values were finally obtained by utilizing the relationship between time difference, transient temperature and liquid pressure. An experimental pressure measurement platform was built and the experimental results confirm that the proposed method has good measurement accuracy.

Determination of patulin in apple and derived products by UHPLC-MS/MS. Study of matrix effects with atmospheric pressure ionisation sources.

PubMed

Beltrán, Eduardo; Ibáñez, María; Sancho, Juan Vicente; Hernández, Félix

2014-01-01

Sensitive and reliable analytical methodology has been developed for the measurement of patulin in regulated foodstuffs by using ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) with triple quadrupole analyser. Solid samples were extracted with ethyl acetate, while liquid samples were directly injected into the chromatographic system after dilution and filtration without any clean-up step. Chromatographic separation was achieved in less than 4min. Electrospray (ESI) and atmospheric pressure chemical ionisation (APCI) sources were evaluated, in order to assess matrix effects. The use of ESI source caused strong signal suppression in samples; however, matrix effect was negligible using APCI, allowing quantification with calibration standards prepared in solvent. The method was validated in four different apple matrices (juice, fruit, puree and compote) at two concentrations at the low μgkg(-1) level. Average recoveries (n=5) ranged from 71% to 108%, with RSDs lower than 14%. Copyright © 2013 Elsevier Ltd. All rights reserved.

Liquid-Crystalline Collapse of Pulmonary Surfactant Monolayers

PubMed Central

Schief, William R.; Antia, Meher; Discher, Bohdana M.; Hall, Stephen B.; Vogel, Viola

2003-01-01

During exhalation, the surfactant film of lipids and proteins that coats the alveoli in the lung is compressed to high surface pressures, and can remain metastable for prolonged periods at pressures approaching 70 mN/m. Monolayers of calf lung surfactant extract (CLSE), however, collapse in vitro, during an initial compression at ∼45 mN/m. To gain information on the source of this discrepancy, we investigated how monolayers of CLSE collapse from the interface. Observations with fluorescence, Brewster angle, and light scattering microscopies show that monolayers containing CLSE, CLSE-cholesterol (20%), or binary mixtures of dipalmitoyl phosphatidylcholine(DPPC)-dihydrocholesterol all form bilayer disks that reside above the monolayer. Upon compression and expansion, lipids flow continuously from the monolayer into the disks, and vice versa. In several respects, the mode of collapse resembles the behavior of other amphiphiles that form smectic liquid-crystal phases. These findings suggest that components of surfactent films must collapse collectively rather than being squeezed out individually. PMID:12770885

A sensitive high-pressure liquid chromatography/particle beam/mass spectrometry assay for the determination of all-trans-retinoic acid and 13-cis-retinoic acid in human plasma.

PubMed

Lehman, P A; Franz, T J

1996-03-01

A highly sensitive assay for the measurement of all-trans-retinoic acid (tretinoin) and 13-cis-retinoic acid (isotretinoin) has been developed. Collected plasma samples were protein precipitated with 2-propanol followed by solid phase extraction. The retinoic acids were subsequently derivatized to their pentafluorobenzyl esters followed by separation and isolation by reverse phase high-pressure liquid chromatography. The HPLC eluate was directed to a mass spectrometer via a particle beam interface. Selected ion monitoring (299 m/z) for the retinoic acid's carboxylate anion produced by negative chemical ionization using methane reagent gas achieved minimum detection limits of 25 pg injected. Endogenous blood levels in 19 male and 9 female subjects were measured. It was found that females have significantly more all-trans-retinoic acid than males and that both sexes demonstrate significantly more all-trans-retinoic acid then 13-cis-retinoic acid.

Sequential Injection Chromatography with an Ultra-short Monolithic Column for the Low-Pressure Separation of α-Tocopherol and γ-Oryzanol in Vegetable Oils and Nutrition Supplements.

PubMed

Thaithet, Sujitra; Kradtap Hartwell, Supaporn; Lapanantnoppakhun, Somchai

2017-01-01

A low-pressure separation procedure of α-tocopherol and γ-oryzanol was developed based on a sequential injection chromatography (SIC) system coupled with an ultra-short (5 mm) C-18 monolithic column, as a lower cost and more compact alternative to the HPLC system. A green sample preparation, dilution with a small amount of hexane followed by liquid-liquid extraction with 80% ethanol, was proposed. Very good separation resolution (R s = 3.26), a satisfactory separation time (10 min) and a total run time including column equilibration (16 min) were achieved. The linear working range was found to be 0.4 - 40 μg with R 2 being more than 0.99. The detection limits of both analytes were 0.28 μg with the repeatability within 5% RSD (n = 7). Quantitative analyses of the two analytes in vegetable oil and nutrition supplement samples, using the proposed SIC method, agree well with the results from HPLC.

Variation law of gas holdup in an autoclave during the pressure leaching process by using a mixed-flow agitator

NASA Astrophysics Data System (ADS)

Tian, Lei; Liu, Yan; Tang, Jun-jie; Lü, Guo-zhi; Zhang, Ting-an

2017-08-01

The multiphase reaction process of pressure leaching is mainly carried out in the liquid phase. Therefore, gas holdup is essential for the gas-liquid-solid phase reaction and the extraction rate of valuable metals. In this paper, a transparent quartz autoclave, a six blades disc turbine-type agitator, and a high-speed camera were used to investigate the gas holdup of the pressure leaching process. Furthermore, experiments determining the effects of agitation rate, temperature, and oxygen partial pressure on gas holdup were carried out. The results showed that when the agitation rate increased from 350 to 600 r/min, the gas holdup increased from 0.10% to 0.64%. When the temperature increased from 363 to 423 K, the gas holdup increased from 0.14% to 0.20%. When the oxygen partial pressure increased from 0.1 to 0.8 MPa, the gas holdup increased from 0.13% to 0.19%. A similar criteria relationship was established by Homogeneous Principle and Buckingham's theorem. Comprehensively, empirical equation of gas holdup was deduced on the basis of experimental data and the similarity theory, where the criterion equation was determined as ɛ = 4.54 × 10-11 n 3.65 T 2.08 P g 0.18. It can be seen from the formula that agitation rate made the most important impact on gas holdup in the pressure leaching process using the mixed-flow agitator.

Analysis of trimethoprim, lincomycin, sulfadoxin and tylosin in swine manure using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry.

PubMed

Solliec, Morgan; Massé, Daniel; Sauvé, Sébastien

2014-10-01

A new extraction method coupled to a high throughput sample analysis technique was developed for the determination of four veterinary antibiotics. The analytes belong to different groups of antibiotics such as chemotherapeutics, sulfonamides, lincosamides and macrolides. Trimethoprim (TMP), sulfadoxin (SFX), lincomycin (LCM) and tylosin (TYL) were extracted from lyophilized manure using a sonication extraction. McIlvaine buffer and methanol (MeOH) were used as extraction buffers, followed by cation-exchange solid phase extraction (SPE) for clean-up. Analysis was performed by laser diode thermal desorption-atmospheric pressure chemical-ionization (LDTD-APCI) tandem mass spectrometry (MS/MS) with selected reaction monitoring (SRM) detection. The LDTD is a high throughput sample introduction method that reduces total analysis time to less than 15s per sample, compared to minutes when using traditional liquid chromatography (LC). Various SPE parameters were optimized after sample extraction: the stationary phase, the extraction solvent composition, the quantity of sample extracted and sample pH. LDTD parameters were also optimized: solvent deposition, carrier gas, laser power and corona discharge. The method limit of detection (MLD) ranged from 2.5 to 8.3 µg kg(-1) while the method limit of quantification (MLQ) ranged from 8.3 to 28µgkg(-1). Calibration curves in the manure matrix showed good linearity (R(2)≥ 0.996) for all analytes and the interday and intraday coefficients of variation were below 14%. Recoveries of analytes from manure ranged from 53% to 69%. The method was successfully applied to real manure samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparison of salting-out and sugaring-out liquid-liquid extraction methods for the partition of 10-hydroxy-2-decenoic acid in royal jelly and their co-extracted protein content.

PubMed

Tu, Xijuan; Sun, Fanyi; Wu, Siyuan; Liu, Weiyi; Gao, Zhaosheng; Huang, Shaokang; Chen, Wenbin

2018-01-15

Homogeneous liquid-liquid extraction (h-LLE) has been receiving considerable attention as a sample preparation method due to its simple and fast partition of compounds with a wide range of polarities. To better understand the differences between the two h-LLE extraction approaches, salting-out assisted liquid-liquid extraction (SALLE) and sugaring-out assisted liquid-liquid extraction (SULLE), have been compared for the partition of 10-hydroxy-2-decenoic acid (10-HDA) from royal jelly, and for the co-extraction of proteins. Effects of the amount of phase partition agents and the concentration of acetonitrile (ACN) on the h-LLE were discussed. Results showed that partition efficiency of 10-HDA depends on the phase ratio in both SALLE and SULLE. Though the partition triggered by NaCl and glucose is less efficient than MgSO 4 in the 50% (v/v) ACN-water mixture, their extraction yields can be improved to be similar with that in MgSO 4 SALLE by increasing the initial concentration of ACN in the ACN-water mixture. The content of co-extracted protein was correlated with water concentration in the obtained upper phase. MgSO 4 showed the largest protein co-extraction at the low concentration of salt. Glucose exhibited a large protein co-extraction in the high phase ratio condition. Furthermore, NaCl with high initial ACN concentration is recommended because it produced high extraction yield for 10-HDA and the lowest amount of co-extracted protein. These observations would be valuable for the sample preparation of royal jelly. Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of hypobaric pressure on human skin: implications for cryogen spray cooling (part II).

PubMed

Aguilar, Guillermo; Franco, Walfre; Liu, Jie; Svaasand, Lars O; Nelson, J Stuart

2005-02-01

Clinical results have demonstrated that dark purple port wine stain (PWS) birthmarks respond favorably to laser induced photothermolysis after the first three to five treatments. Nevertheless, complete blanching is rarely achieved and the lesions stabilize at a red-pink color. In a feasibility study (Part I), we showed that local hypobaric pressure on PWS human skin prior to laser irradiation induced significant lesion blanching. The objective of the present study (Part II) is to investigate the effects of hypobaric pressures on the efficiency of cryogen spray cooling (CSC), a technique that assists laser therapy of PWS and other dermatoses. Experiments were carried out within a suction cup and vacuum chamber to study the effect of hypobaric pressure on the: (1) interaction of cryogen sprays with human skin; (2) spray atomization; and (3) thermal response of a model skin phantom. A high-speed camera was used to acquire digital images of spray impingement on in vivo human skin and spray cones generated at different hypobaric pressures. Subsequently, liquid cryogen was sprayed onto a skin phantom at atmospheric and 17, 34, 51, and 68 kPa (5, 10, 15, and 20 in Hg) hypobaric pressures. A fast-response temperature sensor measured sub-surface phantom temperature as a function of time. Measurements were used to solve an inverse heat conduction problem to calculate surface temperatures, heat flux, and overall heat extraction at the skin phantom surface. Under hypobaric pressures, cryogen spurts did not produce skin indentation and only minimal frost formation. Sprays also showed shorter jet lengths and better atomization. Lower minimum surface temperatures and higher overall heat extraction from skin phantoms were reached. The combined effects of hypobaric pressure result in more efficient cryogen evaporation that enhances heat extraction and, therefore, improves the epidermal protection provided by CSC. (c) 2005 Wiley-Liss, Inc.

Effectiveness of Liquid-Liquid Extraction, Solid Phase Extraction, and Headspace Technique for Determination of Some Volatile Water-Soluble Compounds of Rose Aromatic Water

PubMed Central

2017-01-01

Steam distillation is used to isolate scent of rose flowers. Rose aromatic water is commonly used in European cuisine and aromatherapy besides its use in cosmetic industry for its lovely scent. In this study, three different sampling techniques, liquid-liquid extraction (LLE), headspace technique (HS), and solid phase extraction (SPE), were compared for the analysis of volatile water-soluble compounds in commercial rose aromatic water. Some volatile water-soluble compounds of rose aromatic water were also analyzed by gas chromatography mass spectrometry (GCMS). In any case, it was concluded that one of the solid phase extraction methods led to higher recoveries for 2-phenylethyl alcohol (PEA) in the rose aromatic water than the liquid-liquid extraction and headspace technique. Liquid-liquid extraction method provided higher recovery ratios for citronellol, nerol, and geraniol than others. Ideal linear correlation coefficient values were observed by GCMS for quantitative analysis of volatile compounds (r2 ≥ 0.999). Optimized methods showed acceptable repeatability (RSDs < 5%) and excellent recovery (>95%). For compounds such as α-pinene, linalool, β-caryophyllene, α-humulene, methyl eugenol, and eugenol, the best recovery values were obtained with LLE and SPE. PMID:28791049

Intercomparison of Lab-Based Soil Water Extraction Methods for Stable Water Isotope Analysis

NASA Astrophysics Data System (ADS)

Pratt, D.; Orlowski, N.; McDonnell, J.

2016-12-01

The effect of pore water extraction technique on resultant isotopic signature is poorly understood. Here we present results of an intercomparison of five common lab-based soil water extraction techniques: high pressure mechanical squeezing, centrifugation, direct vapor equilibration, microwave extraction, and cryogenic extraction. We applied five extraction methods to two physicochemically different standard soil types (silty sand and clayey loam) that were oven-dried and rewetted with water of known isotopic composition at three different gravimetric water contents (8, 20, and 30%). We tested the null hypothisis that all extraction techniques would provide the same isotopic result independent from soil type and water content. Our results showed that the extraction technique had a significant effect on the soil water isotopic composition. Each method exhibited deviations from spiked reference water, with soil type and water content showing a secondary effect. Cryogenic extraction showed the largest deviations from the reference water, whereas mechanical squeezing and centrifugation provided the closest match to the reference water for both soil types. We also compared results for each extraction technique that produced liquid water on both an OA-ICOS and IRMS; differences between them were negligible.

Isolation of essential oil from different plants and herbs by supercritical fluid extraction.

PubMed

Fornari, Tiziana; Vicente, Gonzalo; Vázquez, Erika; García-Risco, Mónica R; Reglero, Guillermo

2012-08-10

Supercritical fluid extraction (SFE) is an innovative, clean and environmental friendly technology with particular interest for the extraction of essential oil from plants and herbs. Supercritical CO(2) is selective, there is no associated waste treatment of a toxic solvent, and extraction times are moderate. Further, supercritical extracts were often recognized of superior quality when compared with those produced by hydro-distillation or liquid-solid extraction. This review provides a comprehensive and updated discussion of the developments and applications of SFE in the isolation of essential oils from plant matrices. SFE is normally performed with pure CO(2) or using a cosolvent; fractionation of the extract is commonly accomplished in order to isolate the volatile oil compounds from other co-extracted substances. In this review the effect of pressure, temperature and cosolvent on the extraction and fractionation procedure is discussed. Additionally, a comparison of the extraction yield and composition of the essential oil of several plants and herbs from Lamiaceae family, namely oregano, sage, thyme, rosemary, basil, marjoram and marigold, which were produced in our supercritical pilot-plant device, is presented and discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

Simultaneous quantification of vitamin E, γ-oryzanols and xanthophylls from rice bran essences extracted by supercritical CO2.

PubMed

Sookwong, Phumon; Suttiarporn, Panawan; Boontakham, Pittayaporn; Seekhow, Pattawat; Wangtueai, Sutee; Mahatheeranont, Sugunya

2016-11-15

Since the nutrition value of rice is diminished during rice processing, technology that can preserve and sustain functional compounds is necessary. In this study, supercritical carbon dioxide (SC-CO2) extraction was optimized for operational conditions (time, temperature, pressure and modifier) to extract vitamin E, γ-oryzanols and xanthophylls from rice bran. The simultaneous quantification of the compounds was developed using high-performance liquid chromatography with diode array and fluorescence detectors. Central composite design and respond surface methodology were applied to achieve optimum extraction conditions. The optimized conditions were 60min, 43°C, 5420psi with 10% ethanol as a modifier. Pigmented rice bran extracts contained greater amounts of functional phytochemicals than non-pigmented rice bran extracts (0.68, 1410, and non-detectable μg/g compared with 16.65, 2480, and 0.10μg/g of vitamin E, γ-oryzanols and xanthophylls in pigmented and non-pigmented ones, respectively). SC-CO2 extraction with modifier would be promising for preparation of phytochemical essences for therapeutic purpose. Copyright © 2016 Elsevier Ltd. All rights reserved.

Removal of common organic solvents from aqueous waste streams via supercritical C02 extraction: a potential green approach to sustainable waste management in the pharmaceutical industry.

PubMed

Leazer, Johnnie L; Gant, Sean; Houck, Anthony; Leonard, William; Welch, Christopher J

2009-03-15

Supercritical CO2 extraction of aqueous streams is a convenient and effective method to remove commonly used solvents of varying polarities from aqueous waste streams. The resulting aqueous layers can potentially be sewered; whereas the organic layer can be recovered for potential reuse. Supercritical fluid extraction (SFE) is a technology that is increasingly being used in commercial processes (1). Supercritical fluids are well suited for extraction of a variety of media, including solids, natural products, and liquid products. Many supercritical fluids have low critical temperatures, allowing for extractions to be done at modestly low temperatures, thus avoiding any potential thermal decomposition of the solutes under study (2). Furthermore, the CO2 solvent strength is easily tuned by adjusting the density of the supercritical fluid (The density is proportional to the pressure of the extraction process). Since many supercritical fluids are gases at ambient temperature, the extract can be concentrated by simply venting the reaction mixture to a cyclone collection vessel, using appropriate safety protocols.

Optimization of squalene produced from crude palm oil waste

NASA Astrophysics Data System (ADS)

Wandira, Irda; Legowo, Evita H.; Widiputri, Diah I.

2017-01-01

Squalene is a hydrocarbon originally and still mostly extracted from shark liver oil. Due to environmental issues over shark hunting, there have been efforts to extract squalene from alternative sources, such as Palm Fatty Acid Distillate (PFAD), one of crude palm oil (CPO) wastes. Previous researches have shown that squalene can be extracted from PFAD using saponification process followed with liquid-liquid extraction process although the method had yet to be optimized in order to optimize the amount of squalene extracted from PFAD. The optimization was done by optimizing both processes of squalene extraction method: saponification and liquid-liquid extraction. The factors utilized in the saponification process optimization were KOH concentration and saponification duration while during the liquid-liquid extraction (LLE) process optimization, the factors used were the volumes of distilled water and dichloromethane. The optimum percentage of squalene content in the extract (24.08%) was achieved by saponifying the PFAD with 50%w/v KOH for 60 minutes and subjecting the saponified PFAD to LLE, utilizing 100 ml of distilled water along with 3 times addition of fresh dichloromethane, 75 ml each; those factors would be utilized in the optimum squalene extraction method.

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

PubMed

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

2015-05-01

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

Pressurized hot water extraction followed by miniaturized membrane assisted solvent extraction for the green analysis of alkylphenols in sediments.

PubMed

Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

2015-02-27

A novel and Green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol) in sediments was developed and validated. The method was based on pressurized hot water extraction (PHWE) followed by miniaturized membrane assisted solvent extraction (MASE) and liquid chromatography-electrospray ionization tandem mass spectrometry detection (LC-ESI-MS/MS). The extraction conditions were optimized by a Plackett-Burman design in order to minimize the number of assays according to Green principles. Matrix effect was studied and compensated using deuterated labeled standards as surrogate standards for the quantitation of the target compounds. The analytical features of the method were satisfactory: relative recoveries varied between 92 and 103% and repeatability and intermediate precision were <9% for all compounds. Quantitation limits of the method (MQL) ranged from 0.061 (4-n-nonylphenol) to 1.7ngg(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of the exposed methodology. Reagent consumption, analysis time and waste generation were minimized. The "greenness" of the proposed method was evaluated using an analytical Eco-Scale approach and satisfactory results were obtained. The applicability of the proposed method was demonstrated analysing sediment samples of Galicia coast (NW of Spain) and the ubiquity of alkylphenols in the environment was demonstrated. Copyright © 2015 Elsevier B.V. All rights reserved.

Final test results for the ground operations demonstration unit for liquid hydrogen

NASA Astrophysics Data System (ADS)

Notardonato, W. U.; Swanger, A. M.; Fesmire, J. E.; Jumper, K. M.; Johnson, W. L.; Tomsik, T. M.

2017-12-01

Described herein is a comprehensive project-a large-scale test of an integrated refrigeration and storage system called the Ground Operations and Demonstration Unit for Liquid Hydrogen (GODU LH2), sponsored by the Advanced Exploration Systems Program and constructed at Kennedy Space Center. A commercial cryogenic refrigerator interfaced with a 125,000 l liquid hydrogen tank and auxiliary systems in a manner that enabled control of the propellant state by extracting heat via a closed loop Brayton cycle refrigerator coupled to a novel internal heat exchanger. Three primary objectives were demonstrating zero-loss storage and transfer, gaseous liquefaction, and propellant densification. Testing was performed at three different liquid hydrogen fill-levels. Data were collected on tank pressure, internal tank temperature profiles, mass flow in and out of the system, and refrigeration system performance. All test objectives were successfully achieved during approximately two years of testing. A summary of the final results is presented in this paper.

Alternative first-principles calculation of entropy for liquids

DOE PAGES

Meyer, Edmund R.; Ticknor, Christopher; Kress, Joel D.; ...

2016-04-15

Here, w present an alternative method for interpreting the velocity autocorrelation function (VACF) of a fluid with application to extracting the entropy in a manner similar to the methods developed by Lin et al. [J. Chem. Phys. 119, 11792 (2003)] and improved upon by Desjarlais [Phys. Rev. E 88, 062145 (2013)]. The liquid VACF is decomposed into two components, one gas and one solid, and each contribution's entropic portion is calculated. But, we fit both the gas and solid portions of the VACF in the time domain. This approach is applied to a single-component liquid (a two-phase model of liquidmore » Al at the melt line) and two different two-component systems: a superionic-to-superionic (bcc to fcc) phase transition in H 2 O at high temperatures and pressures and a metastable liquid state of MgO. Finally, for all three examples, comparisons to existing results in the literature demonstrate the validity of our alternative.« less

Inviscid dynamics of a wet foam drop with monodisperse bubble size distribution

NASA Astrophysics Data System (ADS)

McDaniel, J. Gregory; Akhatov, Iskander; Holt, R. Glynn

2002-06-01

Motivated by recent experiments involving the acoustic levitation of foam drops, we develop a model for nonlinear oscillations of a spherical drop composed of monodisperse aqueous foam with void fraction below 0.1. The model conceptually divides a foam drop into many cells, each cell consisting of a spherical volume of liquid with a bubble at its center. By treating the liquid as incompressible and inviscid, a nonlinear equation is obtained for bubble motion due to a pressure applied at the outer radius of the liquid sphere. Upon linearizing this equation and connecting the cells at their outer radii, a wave equation is obtained with a dispersion relation for the sound waves in a bubbly liquid. For the spherical drop, this equation is solved by a normal mode expansion that yields the natural frequencies as functions of standard foam parameters. Numerical examples illustrate how the analysis may be used to extract foam parameters, such as void fraction and bubble radius, from the experimentally measured natural frequencies of a foam drop.

Method of producing a high pressure gas

DOEpatents

Bingham, Dennis N.; Klingler, Kerry M.; Zollinger, William T.

2006-07-18

A method of producing a high pressure gas is disclosed and which includes providing a container; supplying the container with a liquid such as water; increasing the pressure of the liquid within the container; supplying a reactant composition such as a chemical hydride to the liquid under pressure in the container and which chemically reacts with the liquid to produce a resulting high pressure gas such as hydrogen at a pressure of greater than about 100 pounds per square inch of pressure; and drawing the resulting high pressure gas from the container.

New metabolic pathway for N,N-dimethyltryptamine

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

Hryhorczuk, L.M.; Rainey, J.M. Jr.; Frohman, C.E.

1986-01-01

N,N-Dimethyltryptamine (DMT) undergoes a major structural alteration when added to whole human blood or its red blood cells in vitro. A new high-pressure liquid chromatography (HPLC) peak is present in extracts of these treated tissues. The compound responsible for this peak has been identified by ultraviolet spectrophotometry and by mass spectrometry as dimethylkynuramine (DMK). The enzyme responsible for this appears to be different from tryptophan 2,3-dioxygenase and also from indoleamine 2,3-dioxygenase.

Determination of polycyclic aromatic hydrocarbons in fractions in asphalt mixtures using liquid chromatography coupled to mass spectrometry with atmospheric pressure chemical ionization.

PubMed

Nascimento, Paulo Cicero; Gobo, Luciana Assis; Bohrer, Denise; Carvalho, Leandro Machado; Cravo, Margareth Coutinho; Leite, Leni Figueiredo Mathias

2015-07-01

An analytical method using liquid chromatography coupled to mass spectrometry with atmospheric pressure chemical ionization for the determination of polycyclic aromatic hydrocarbons in asphalt fractions has been developed. The 14 compounds determined, characterized by having two or more condensed aromatic rings, are expected to be present in asphalt and are considered carcinogenic and mutagenic. The parameters of the atmospheric pressure chemical ionization interface were optimized to obtain the highest possible sensitivity for all of the compounds. The limits of detection ranged from 0.5 to 346.5 μg/L and the limits of quantification ranged from 1.7 to 1550 μg/L. The method was validated against a diesel particulate extract standard reference material (NIST SRM 1975), and the obtained concentrations agreed with the certified values. The method was applied to asphalt samples after its fractionation according to ASTM D4124 and the method of Green. The concentrations of the seven polycyclic aromatic hydrocarbons quantified in the sample ranged from 0.86 mg/kg for benzo[ghi]perylene to 98.32 mg/kg for fluorene. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid chromatography/mass spectrometric determination of patulin in apple juice using atmospheric pressure photoionization.

PubMed

Takino, Masahiko; Daishima, Shigeki; Nakahara, Taketoshi

2003-01-01

This paper describes a comparison between atmospheric pressure chemical ionization (APCI) and the recently introduced atmospheric pressure photoionization (APPI) technique for the liquid chromatography/mass spectrometric (LC/MS) determination of patulin in clear apple juice. A column switching technique for on-line extraction of clear apple juice was developed. The parameters investigated for the optimization of APPI were the ion source parameters fragmentor voltage, capillary voltage, and vaporizer temperature, and also mobile phase composition and flow rate. Furthermore, chemical noise and signal suppression of analyte signals due to sample matrix interference were investigated for both APCI and APPI. The results indicated that APPI provides lower chemical noise and signal suppression in comparison with APCI. The linear range for patulin in apple juice (correlation coefficient >0.999) was 0.2-100 ng mL(-1). Mean recoveries of patulin in three apple juices ranged from 94.5 to 103.2%, and the limit of detection (S/N = 3), repeatability and reproducibility were 1.03-1.50 ng mL(-1), 3.9-5.1% and 7.3-8.2%, respectively. The total analysis time was 10.0 min. Copyright 2003 John Wiley & Sons, Ltd.

Concept of a self-pressurized feed system for liquid rocket engines and its fundamental experiment results

NASA Astrophysics Data System (ADS)

Matsumoto, Jun; Okaya, Shunichi; Igoh, Hiroshi; Kawaguchi, Junichiro

2017-04-01

A new propellant feed system referred to as a self-pressurized feed system is proposed for liquid rocket engines. The self-pressurized feed system is a type of gas-pressure feed system; however, the pressurization source is retained in the liquid state to reduce tank volume. The liquid pressurization source is heated and gasified using heat exchange from the hot propellant using a regenerative cooling strategy. The liquid pressurization source is raised to critical pressure by a pressure booster referred to as a charger in order to avoid boiling and improve the heat exchange efficiency. The charger is driven by a part of the generated pressurization gas using a closed-loop self-pressurized feed system. The purpose of this study is to propose a propellant feed system that is lighter and simpler than traditional gas pressure feed systems. The proposed system can be applied to all liquid rocket engines that use the regenerative cooling strategy. The concept and mathematical models of the self-pressurized feed system are presented first. Experiment results for verification are then shown and compared with the mathematical models.

Liposomes Size Engineering by Combination of Ethanol Injection and Supercritical Processing.

PubMed

Santo, Islane Espirito; Campardelli, Roberta; Albuquerque, Elaine Cabral; Vieira De Melo, Silvio A B; Reverchon, Ernesto; Della Porta, Giovanna

2015-11-01

Supercritical fluid extraction using a high-pressure packed tower is proposed not only to remove the ethanol residue from liposome suspensions but also to affect their size and distribution leading the production of nanosomes. Different operating pressures, temperatures, and gas to liquid ratios were explored and ethanol was successfully extracted up to a value of 400 ppm; liposome size and distribution were also reduced by the supercritical processing preserving their integrity, as confirmed by Z-potential data and Trasmission Electron Microscopy observations. Operating at 120 bar and 38°C, nanosomes with a mean diameter of about 180 ± 40 nm and good storage stability were obtained. The supercritical processing did not interfere on drug encapsulation, and no loss of entrapped drug was observed when the water-soluble fluorescein was loaded as a model compound. Fluorescein encapsulation efficiency was 30% if pure water was used during the supercritical extraction as processing fluid; whereas an encapsulation efficiency of 90% was obtained if the liposome suspension was processed in water/fluorescein solution. The described technology is easy to scale up to an industrial production and merge in one step the solvent extraction, liposome size engineering, and an excellent drug encapsulation in a single operation unit. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Simultaneous extraction of acetylsalicylic acid and salicylic acid from human plasma and simultaneous estimation by liquid chromatography and atmospheric pressure chemical ionization/tandem mass spectrometry detection. Application to a pharmacokinetic study.

PubMed

Nirogi, Ramakrishna; Kandikere, Vishwottam; Mudigonda, Koteshwara; Ajjala, Devender; Suraneni, Ramakrishna; Thoddi, Parthasarathi

2011-01-01

A simple analytical method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in atmospheric chemical ionization mode (APCI) for the simultaneous estimation of acetylsalicylic acid (ASA, CAS 50-78-2) and its active metabolite salicylic acid (SA, CAS 69-72-7) in human plasma has been developed and validated. ASA and SA were analyzed simultaneously despite differences in plasma concentration ranges of ASA and SA after oral administration of ASA. In spite of having different chemical, ionization and chromatographic properties, ASA and SA were extracted simultaneously from the plasma sample using acetonitrile protein precipitation followed by liquid-liquid extraction. The analytes were separated on a reversed phase column with rapid gradient program using mobile phase consisting of ammonium acetate buffer and methanol. The structural analogue diclofenac was used as an internal standard. The multiple reaction monitoring (MRM) transitions m/z 179 --> 137 for ASA, m/z 137 --> 65 for SA and m/z 294 --> 250 for IS were used. The assay exhibited a linear dynamic range of 0.02-10 microg/mL for ASA and 0.1-50 microg/mL for SA. The between-batch precision (%CV) ranged from 2.1 to 7.9% for ASA and from 0.2 to 5.2% for SA. The between-batch accuracy ranged from 95.4 to 96.7% for ASA and from 94.6 to 111.3% for SA. The validated method was successfully applied for the evaluation of pharmacokinetics of ASA after single oral administration of 650 mg test formulation versus two 325 mg reference formulations of ASA in human subjects.

Identification of novel sulfur-containing steroids in sediments and petroleum: probable incorporation of sulfur into δ 5,7-sterols during early diagenesis

NASA Astrophysics Data System (ADS)

Sinninghe Damsté, Jaap S.; Schouten, Stefan; de Leeuw, Jan W.; van Duin, Adri C. T.; Geenevasen, Jan A. J.

1999-01-01

A novel sulfur-containing sterane, 4α,7α-epithio-5β-cholestane, has been identified in a sediment extract from the Miocene Northern Apennines marl (Italy) after its isolation by column chromatography and high pressure liquid chromatography. The compound has been characterised by GC-MS and mild Nickel boride desulfurisation and one and two-dimensional 1H NMR techniques. C 27-C 29 homologs have been detected in sediment extracts of three different formations and in one petroleum sample. These sulfur-containing steroids are probably formed by an intramolecular reaction of inorganic sulfides with early diagenetic products of Δ 5,7-sterols.

A new chemical tool for absinthe producers, quantification of α/β-thujone and the bitter components in Artemisia absinthium.

PubMed

Bach, Benoit; Cleroux, Marilyn; Saillen, Mayra; Schönenberger, Patrik; Burgos, Stephane; Ducruet, Julien; Vallat, Armelle

2016-12-15

The concentrations of α/β-thujone and the bitter components of Artemisia absinthium were quantified from alcoholic wormwood extracts during four phenological stages of their harvest period. A solid-phase micro-extraction method coupled to gas chromatography-mass spectrometry was used to determine the concentration of the two isomeric forms of thujone. In parallel, the combination of ultra-high pressure liquid chromatography and high resolution mass spectrometry allowed to quantify the compounds absinthin, artemisetin and dihydro-epi-deoxyarteannuin B. This present study aimed at helping absinthe producers to determine the best harvesting period. Copyright © 2016 Elsevier Ltd. All rights reserved.

Using Dalton's Law of Partial Pressures to Determine the Vapor Pressure of a Volatile Liquid

ERIC Educational Resources Information Center

Hilgeman, Fred R.; Bertrand, Gary; Wilson, Brent

2007-01-01

This experiment, designed for a general chemistry laboratory, illustrates the use of Dalton's law of partial pressures to determine the vapor pressure of a volatile liquid. A predetermined volume of air is injected into a calibrated tube filled with a liquid whose vapor pressure is to be measured. The volume of the liquid displaced is greater than…

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.

Combination of Cyclodextrin and Ionic Liquid in Analytical Chemistry: Current and Future Perspectives.

PubMed

Hui, Boon Yih; Raoov, Muggundha; Zain, Nur Nadhirah Mohamad; Mohamad, Sharifah; Osman, Hasnah

2017-09-03

The growth in driving force and popularity of cyclodextrin (CDs) and ionic liquids (ILs) as promising materials in the field of analytical chemistry has resulted in an exponentially increase of their exploitation and production in analytical chemistry field. CDs belong to the family of cyclic oligosaccharides composing of α-(1,4) linked glucopyranose subunits and possess a cage-like supramolecular structure. This structure enables chemical reactions to proceed between interacting ions, radical or molecules in the absence of covalent bonds. Conversely, ILs are an ionic fluids comprising of only cation and anion often with immeasurable vapor pressure making them as green or designer solvent. The cooperative effect between CD and IL due to their fascinating properties, have nowadays contributed their footprints for a better development in analytical chemistry nowadays. This comprehensive review serves to give an overview on some of the recent studies and provides an analytical trend for the application of CDs with the combination of ILs that possess beneficial and remarkable effects in analytical chemistry including their use in various sample preparation techniques such as solid phase extraction, magnetic solid phase extraction, cloud point extraction, microextraction, and separation techniques which includes gas chromatography, high-performance liquid chromatography, capillary electrophoresis as well as applications of electrochemical sensors as electrode modifiers with references to recent applications. This review will highlight the nature of interactions and synergic effects between CDs, ILs, and analytes. It is hoped that this review will stimulate further research in analytical chemistry.

Liquid-liquid extraction of actinides, lanthanides, and fission products by use of ionic liquids: from discovery to understanding.

PubMed

Billard, Isabelle; Ouadi, Ali; Gaillard, Clotilde

2011-06-01

Liquid-liquid extraction of actinides and lanthanides by use of ionic liquids is reviewed, considering, first, phenomenological aspects, then looking more deeply at the various mechanisms. Future trends in this developing field are presented.

21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 8 2011-04-01 2011-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 8 2014-04-01 2014-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 8 2012-04-01 2012-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 8 2013-04-01 2013-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

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

PubMed

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

2011-07-01

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

High-pressure liquid-monopropellant strand combustion.

NASA Technical Reports Server (NTRS)

Faeth, G. M.

1972-01-01

Examination of the influence of dissolved gases on the state of the liquid surface during high-pressure liquid-monopropellant combustion through the use of a strand burning experiment. Liquid surface temperatures were measured, using fine-wire thermocouples, during the strand combustion of ethyl nitrate, normal propyl nitrate, and propylene glycol dinitrate at pressures up to 81 atm. These measurements were compared with the predictions of a variable-property gas-phase analysis assuming an infinite activation energy for the decomposition reaction. The state of the liquid surface was estimated using a conventional low-pressure phase equilibrium model, as well as a high-pressure version that considered the presence of dissolved combustion-product gases in the liquid phase. The high-pressure model was found to give a superior prediction of measured liquid surface temperatures. Computed total pressures required for the surface to reach its critical mixing point during strand combustion were found to be in the range from 2.15 to 4.62 times the critical pressure of the pure propellant. Computed dissolved gas concentrations at the liquid surface were in the range from 35 to 50% near the critical combustion condition.

Characterization of lecithin isolated from anchovy (Engraulis japonica) residues deoiled by supercritical carbon dioxide and organic solvent extraction.

PubMed

Lee, Seung-Mi; Asaduzzaman, A K M; Chun, Byung-Soo

2012-07-01

Lecithin was isolated and characterized from anchovy (Engraulis japonica) deoiled residues using supercritical carbon dioxide (SC-CO(2)) at a semibatch flow extraction process and an organic solvent (hexane) extraction. SC-CO(2) extraction was carried out to extract oil from anchovy at different temperatures (35 to 45 °C) and pressures (15 to 25 MPa). Extraction yield of oil was influenced by physical properties of SC-CO(2) with temperature and pressure changes. The major phospholipids of anchovy lecithin were quantitatively analyzed by high-performance liquid chromatography. Phosphatidylcholine (PC) (68%± 1.00%) and phosphatidylethanolamine (PE) (29%± 0.50%) were the main phospholipids. Thin layer chromatography was performed to purify the individual phospholipids. The fatty acid compositions of lecithin, PC, and PE were analyzed by gas chromatography. A significant amount of eicosapentaenoic acid and docosahexaenoic acid were present in both phospholipids of PC and PE. Emulsions of lecithin in water were prepared through the use of a homogenizer. Oxidative stability of anchovy lecithin was high in spite of its high concentration of long-chain polyunsaturated fatty acids. Lecithin can be totally metabolized by humans, so is well tolerated by humans and nontoxic when ingested. Lecithin from anchovy contain higher amounts of ω-3 fatty acids especially EPA and DHA, it may have positive outcome to use in food and pharmaceutical industries. © 2012 Institute of Food Technologists®

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

PubMed

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

2018-01-19

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

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

PubMed

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

2018-03-01

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

Similitude of membrane helical coil with membrane serpentine tube for characteristics of high-pressure syngas: A review

NASA Astrophysics Data System (ADS)

Gaddamwar, Sagar. S.; Pawar, Anand N.; Naik, Pramod A.

2018-05-01

Heat exchangers remain one primary engineering methods besides this broad category of purposes including various waste heat recovery systems, power sectors, nuclear reactors. Natural convection is a method concerning heat transfer, during which flow of fluid occurs by density variations in the fluid occurring due to different temperature conditions. A fluid which encompasses a heat reservoir holds heat becomes light dense and rises. Operating fluid that is enclosing the high-temperature liquid remains frozen and later flows in to supplant it. Following this chilling liquid gets heated, and this method persists, resulting from convection flow. Forced convection into a heat exchanger is this movement of heat from one moving water to different stream through the surface from a pipe. The low-temperature liquid extracts heat of this comparatively high-temperature water because that flows along or over it.

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.

Determination of hydroxylated polycyclic aromatic hydrocarbons by HPLC-photoionization tandem mass spectrometry in wood smoke particles and soil samples.

PubMed

Avagyan, Rozanna; Nyström, Robin; Boman, Christoffer; Westerholm, Roger

2015-06-01

A simple and fast method for analysis of hydroxylated polycyclic aromatic hydrocarbons using pressurized liquid extraction and high performance liquid chromatography utilizing photoionization tandem mass spectrometry was developed. Simultaneous separation and determination of nine hydroxylated polycyclic aromatic hydrocarbons and two hydroxy biphenyls could be performed in negative mode with a run time of 12 min, including equilibration in 5 min. The calibration curves were in two concentration ranges; 1-50 ng/mL and 0.01-50 μg/mL, with coefficients of correlation R (2) > 0.997. The limits of detection and method quantification limits were in the range of 9-56 pg and 5-38 ng/g, respectively. A two-level full factorial experimental design was used for screening of conditions with the highest impact on the extraction. The extraction procedure was automated and suitable for a large number of samples. The extraction recoveries ranged from 70 to 102 % and the matrix effects were between 92 and 104 %. The overall method was demonstrated on wood smoke particles and soil samples with good analytical performance, and five OH-PAHs were determined in the concentration range of 0.19-210 μg/g. As far as we know, hydroxylated polycyclic aromatic hydrocarbons were determined in wood smoke and soil samples using photoionization mass spectrometry for the first time in this present study. Accordingly, this study shows that high performance liquid chromatography photoionization tandem mass spectrometry can be a good option for the determination of hydroxylated polycyclic aromatic hydrocarbons in complex environmental samples. Graphical Abstract The method developed in this study was used to determine hydroxylated polycyclic aromatic hydrocarbons in wood smoke and soil.

Biosynthesis and characterization of gold nanoparticles using extracts of tamarindus indica L leaves

NASA Astrophysics Data System (ADS)

Correa, S. N.; Naranjo, A. M.; Herrera, A. P.

2016-02-01

This study reports the biosynthesis of gold nanoparticles using an extract of Tamarindus indica L. leaves. Phenols, ketones and carboxyls were present in the leaves of T. indica. These organic compounds that allowed the synthesis of nanoparticles were identified by gas chromatography coupled to mass spectrometry (GC/MS) and High Pressure Liquid Chromatographic (HPLC). Synthesis of gold nanoparticles was performed with the extract of T. indica leaves and an Au+3 aqueous solutions (HAuCl4) at room temperature with one hour of reaction time. Characterization of gold nanoparticles was performed by UV visible spectroscopy, scanning electron microscopy (SEM) and EDX. The results indicated the formation of gold nanoparticles with a wavelength of 576nm and an average size of 52±5nm. The EDX technique confirmed the presence of gold nanoparticles with 12.88% in solution.

Analysis of acrylamide in coffee and cocoa by isotope dilution liquid chromatography-tandem mass spectrometry.

PubMed

Aguas, Patricia C; Fitzhenry, Matthew J; Giannikopoulos, Georgina; Varelis, Peter

2006-08-01

An accurate and precise method for the quantification of acrylamide using stable isotope dilution liquid chromatography-tandem mass spectrometry was developed and used to measure acrylamide in coffee and cocoa samples. The sample preparation involved extraction of the analyte and its internal standard, 13C3-acrylamide, into water and subsequent defatting of the aqueous extract with dichloromethane. An aliquot of the resulting aqueous extract was then azeotropically dried under reduced pressure and subsequently purified using an aminopropyl-bonded silica cartridge. The purified extracts were then chromatographed on a 5-microm 2.1 x 150 mm Hypercarb column, the effluent of which was monitored for the analyte and its internal standard using positive-ion APCI-selected reaction monitoring. The intra-laboratory reproducibility of the method, expressed as a relative coefficient of variation (%, n=5), was determined at four levels of concentration (12.3, 42.3, 139.3 and 464.8 microg kg(-1)) and was found to vary between 0.6-2.5%. The accuracy of the method was assessed using a reference sample of coffee. The average result obtained using our method differed from the assigned value of the reference material by less than 1%. An analysis of a cocoa sample revealed that the method is capable of precisely estimating acrylamide in challenging matrices down to a level of at least 12.3 microg kg(-1).

Ultrasound-assisted oxidative desulfurization of liquid fuels and its industrial application.

PubMed

Wu, Zhilin; Ondruschka, Bernd

2010-08-01

Latest environmental regulations require a very deep desulfurization to meet the ultra-low sulfur diesel (ULSD, 15 ppm sulfur) specifications. Due to the disadvantages of hydrotreating technology on the slashing production conditions, costs and safety as well as environmental protection, the ultrasound-assisted oxidative desulfurization (UAOD) as an alternative technology has been developed. UAOD process selectively oxidizes sulfur in common thiophenes in diesel to sulfoxides and sulfones which can be removed via selective adsorption or extractant. SulphCo has successfully used a 5000 barrel/day mobile "Sonocracking" unit to duplicate on a commercial scale its proprietary process that applies ultrasonics at relatively low temperatures and pressures. The UAOD technology estimate capital costs less than half the cost of a new high-pressure hydrotreater. The physical and chemical mechanisms of UAOD process are illustrated, and the effective factors, such as ultrasonic frequency and power, oxidants, catalysts, phase-transfer agent, extractant and adsorbent, on reaction kinetics and product recovery are discussed in this review. Copyright 2009 Elsevier B.V. All rights reserved.

Miniature flowing atmospheric-pressure afterglow ion source for facile interfacing of CE with MS.

PubMed

Jecklin, Matthias C; Schmid, Stefan; Urban, Pawel L; Amantonico, Andrea; Zenobi, Renato

2010-10-01

Here, we present a miniaturized version of the flowing atmospheric-pressure afterglow (miniFAPA) ion source and use it for sheathless coupling of CE with MS. The simple design of the CE-miniFAPA-MS interface makes it easy to separate the electric potentials used for CE and for ionization. A pneumatically assisted nebulization of the CE effluent transfers the analytes from the liquid phase into the gas phase before they are ionized by interacting with reactive species produced by the FAPA. An important advantage of this interface is its high stability during operation: optimization of five different parameters indicated that the interface is not sensitive to minor deviations from the optimum values. Other advantages include ease of construction and maintenance, as well as relatively low cost. Samples with complex matrices, such as yeast extract, soil extract and urine, spiked with the test compounds, were successfully analyzed using the CE-miniFAPA-MS setup.

Chemical tailoring of steam to remediate underground mixed waste contaminents

DOEpatents

Aines, Roger D.; Udell, Kent S.; Bruton, Carol J.; Carrigan, Charles R.

1999-01-01

A method to simultaneously remediate mixed-waste underground contamination, such as organic liquids, metals, and radionuclides involves chemical tailoring of steam for underground injection. Gases or chemicals are injected into a high pressure steam flow being injected via one or more injection wells to contaminated soil located beyond a depth where excavation is possible. The injection of the steam with gases or chemicals mobilizes contaminants, such as metals and organics, as the steam pushes the waste through the ground toward an extraction well having subatmospheric pressure (vacuum). The steam and mobilized contaminants are drawn in a substantially horizontal direction to the extraction well and withdrawn to a treatment point above ground. The heat and boiling action of the front of the steam flow enhance the mobilizing effects of the chemical or gas additives. The method may also be utilized for immobilization of metals by using an additive in the steam which causes precipitation of the metals into clusters large enough to limit their future migration, while removing any organic contaminants.

Evaluation of two membrane-based microextraction techniques for the determination of endocrine disruptors in aqueous samples by HPLC with diode array detection.

PubMed

Luiz Oenning, Anderson; Lopes, Daniela; Neves Dias, Adriana; Merib, Josias; Carasek, Eduardo

2017-11-01

In this study, the viability of two membrane-based microextraction techniques for the determination of endocrine disruptors by high-performance liquid chromatography with diode array detection was evaluated: hollow fiber microporous membrane liquid-liquid extraction and hollow-fiber-supported dispersive liquid-liquid microextraction. The extraction efficiencies obtained for methylparaben, ethylparaben, bisphenol A, benzophenone, and 2-ethylhexyl-4-methoxycinnamate from aqueous matrices obtained using both approaches were compared and showed that hollow fiber microporous membrane liquid-liquid extraction exhibited higher extraction efficiency for most of the compounds studied. Therefore, a detailed optimization of the extraction procedure was carried out with this technique. The optimization of the extraction conditions and liquid desorption were performed by univariate analysis. The optimal conditions for the method were supported liquid membrane with 1-octanol for 10 s, sample pH 7, addition of 15% w/v of NaCl, extraction time of 30 min, and liquid desorption in 150 μL of acetonitrile/methanol (50:50 v/v) for 5 min. The linear correlation coefficients were higher than 0.9936. The limits of detection were 0.5-4.6 μg/L and the limits of quantification were 2-16 μg/L. The analyte relative recoveries were 67-116%, and the relative standard deviations were less than 15.5%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

NASA Technical Reports Server (NTRS)

Gilmour, Iain; Pillinger, Colin

1993-01-01

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

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

NASA Astrophysics Data System (ADS)

Gilmour, Iain; Pillinger, Colin

1993-03-01

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

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

PubMed

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

2012-01-01

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

Selective extraction and separation of oxymatrine from Sophora flavescens Ait. extract by silica-confined ionic liquid.

PubMed

Bi, Wentao; Tian, Minglei; Row, Kyung Ho

2012-01-01

This study highlighted the application of a two-stepped extraction method for extraction and separation of oxymatrine from Sophora flavescens Ait. extract by utilizing silica-confined ionic liquids as sorbent. The optimized silica-confined ionic liquid was firstly mixed with plant extract to adsorb oxymatrine. Simultaneously, some interference, such as matrine, was removed. The obtained suspension was then added to a cartridge for solid phase extraction. Through these two steps, target compound was adequately separated from interferences with 93.4% recovery. In comparison with traditional solid phase extraction, this method accelerates loading and reduces the use of organic solvents during washing. Moreover, the optimization of loading volume was simplified as optimization of solid/liquid ratio. Copyright © 2011 Elsevier B.V. All rights reserved.

Measurement of the differential pressure of liquid metals

DOEpatents

Metz, H.J.

1975-09-01

This patent relates to an improved means for measuring the differential pressure between any two points in a process liquid metal coolant loop, wherein the flow of liquid metal in a pipe is opposed by a permanent magnet liquid metal pump until there is almost zero flow shown by a magnetic type flowmeter. The pressure producing the liquid metal flow is inferred from the rate of rotation of the permanent magnet pump. In an alternate embodiment, a differential pressure transducer is coupled to a process pipeline by means of high-temperature bellows or diaphragm seals, and a permanent magnet liquid metal pump in the high-pressure transmission line to the pressure transducer can be utilized either for calibration of the transducer or for determining the process differential pressure as a function of the magnet pump speed. (auth)

Remediation of Contaminated Soils By Supercritical Carbon Dioxide Extraction

NASA Astrophysics Data System (ADS)

Ferri, A.; Zanetti, M. C.; Banchero, M.; Fiore, S.; Manna, L.

The contaminants that can be found in soils are many, inorganic, like heavy metals, as well as organic. Among the organic contaminants, oil and coal refineries are responsi- ble for several cases of soil contamination with PAHs (Polycyclic Aromatic Hydrocar- bons). Polynuclear aromatic hydrocarbons (PAHs) have toxic, carcinogenic and mu- tagenic effects. Limits have been set on the concentration of most contaminants, and growing concern is focusing on soil contamination issues. USA regulations set the maximum acceptable level of contamination by PAHs equal to 40 ppm at residential sites and 270 ppm at industrial sites. Stricter values are usually adopted in European Countries. Supercritical carbon dioxide extraction is a possible alternative technology to remove volatile organic compounds from contaminated soils. Supercritical fluid extraction (SFE) offers many advantages over conventional solvent extraction. Super- critical fluids combine gaseous properties as a high diffusion coefficient, and liquid properties as a high solvent power. The solvent power is strongly pressure-dependent near supercritical conditions: selective extractions are possible without changing the solvent. Solute can be separate from the solvent depressurising the system; therefore, it is possible to recycle the solvent and recover the contaminant. Carbon dioxide is frequently used as supercritical fluid, because it has moderate critical conditions, it is inert and available in pure form. In this work, supercritical fluid extraction technology has been used to remove a polynuclear aromatic hydrocarbon from contaminated soils. The contaminant choice for the experiment has been naphthalene since several data are available in literature. G. A. Montero et al. [1] studied soil remediation with supercrit- ical carbon dioxide extraction technology; these Authors have found that there was a mass-transfer limitation. In the extraction vessel, the mass transfer coefficient in- creases with the superficial velocity of the supercritical carbon dioxide; therefore, the mass transfer resistance can be reduced increasing such velocity. In this work, higher values of superficial velocity were investigated. The experimental apparatus includes a pump, an extraction vessel, an adjustable restrictor and a trap to collect the extracted substance. Liquid carbon dioxide coming from a cylinder with a dip-tube is cooled by a cryostatic bath and then it is compressed by a pneumatic drive pump (the max- imum available pressure is 69 MPa). Subsequently, the pressurised current flows into 1 a heating coil and then into the extraction vessel, which is contained in a stove; the outlet flow is depressurised in an adjustable restrictor and the extracted substance is collected in a trap by dissolution into a solvent. The extracted naphthalene quantity was obtained by weighting the solvent and measuring the naphthalene concentration with a gas chromatograph. The soil sample is a sandy soil geologically representative of the North of Italy that was sampled and physically and chemically characterized: particle-size distribution analysis, diffractometric analysis, Cation Exchange Capac- ity, Total Organic Carbon, iron content and manganese content in order to evaluate the potential sorption degree. The soil was artificially polluted by means of a naphta- lene and methylene chloride solution. The experimental work consists in a number of naphthalene extractions from the spiked soil, that were carried out at different operat- ing conditions, temperature, pressure and flow rate by means of supercritical carbon dioxide evaluating the corresponding recovery efficiencies. The results obtained were analysed and compared in order to determine which parameters influence the system. [1] G. A. Montero, T.D. Giorgio, and K. B. Schnelle, Jr..Removal of Hazardous ,1994, Contaminants form Soils by Supercritical Fluid Extraction. Innovations in Supercriti- cal Fluids. ACS Symposium Series, 608, 280-197. 2

Multidimensional Separation of Natural Products Using Liquid Chromatography Coupled to Hadamard Transform Ion Mobility Mass Spectrometry

NASA Astrophysics Data System (ADS)

Liu, Wenjie; Zhang, Xing; Knochenmuss, Richard; Siems, William F.; Hill, Herbert H.

2016-05-01

A high performance liquid chromatograph (HPLC)was interfaced to an atmospheric drift tube ion mobility time of flight mass spectrometry. The power of multidimensional separation was demonstrated using chili pepper extracts. The ambient pressure drift tube ion mobility provided high resolving powers up to 166 for the HPLC eluent. With implementation of Hadamard transform (HT), the duty cycle for the ion mobility drift tube was increased from less than 1% to 50%, and the ion transmission efficiency was improved by over 200 times compared with pulsed mode, improving signal to noise ratio 10 times. HT ion mobility and TOF mass spectrometry provide an additional dimension of separation for complex samples without increasing the analysis time compared with conventional HPLC.

Thermal boundary resistance between liquid helium and silver sinter at low temperatures

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

Voncken, A.P.J.; Koenig, R.; Pobell, F.

1996-10-01

The authors present measurements of the thermal coupling between Ag sinter (nominal grain size {approx} 700{angstrom}) and superfluid {sup 3}He-B at p=0.3, 10, and 20 bar as well as a phase-separated {sup 3}He-{sup 4}He mixture at p=0.5 bar in the submillikelvin regime. In order to analyze the data of the pure {sup 3}He-B sample with respect to different contributions to the thermal resistance, a one-dimensional model for the heat flow in the sinter is presented. As a result it is shown that the thermal conductivity of the liquid in the sinter has to be taken into account to extract themore » temperature and pressure dependence of the boundary resistance in the confining geometry of the sinter. Depending on the value of this thermal conductivity, a boundary resistance proportional to T{sup {minus}2} or T{sup {minus}3} is found. Moreover, it is shown that a pressure dependence of the boundary resistance might be explained by a pressure dependence of the thermal conductivity of the liquid in the sinter. The data on the phase-separated mixture are equally well described by a T{sup {minus}2}- and a T{sup {minus}3}-dependence of the boundary resistance. The authors point out that a common problem in most measurements of the Kapitza resistance performed so far is the small temperature interval investigated, which usually does not allow a definite conclusion concerning the temperature dependence.« less

Solvent extraction separation of Th-227 and Ac-225 in room temperature ionic liquids

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

Bell, Jason R; Boll, Rose Ann; Dai, Sheng

2012-01-01

The solvent extractions of Th-227 and Ac-225 from the aqueous phase into ionic liquids (ILs) were investigated by using N,N,N ,N - tetraoctyldiglycolamide (TODGA) or di(2-ethylhexyl)phosphoric acid (HDEHP) as an extractant. Four ionic liquids, 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide ([C4mim][NTf2]), 1-butyl-3-methylimidazolium bis(perfluoroethanesulfonyl)imide ([C4mim][BETI]), 1-butyl-2,3-trimethyleneimidazolium (trifluoromethanesulfonyl)imide [BuI5][NTf2], and 1-benzyl pyridinium bis(trifluoromethanesulfonyl)imide ([PhCH2Py][NTf2]) were used as extraction solvents for separation of Th-227 and Ac-225 in this study. Excellent extraction efficiencies and selectivities were found for Th-227/Ac-225 when HDEHP was used as an extractant in these ionic liquids. The effects of different extractant concentrations in ionic liquids and acidities of the aqueous phase on extraction efficienciesmore » and selectivities of Th-227/Ac-225 are also presented in this article.« less

Pyridinium ionic liquid-based liquid-solid extraction of inorganic and organic iodine from Laminaria.

PubMed

Peng, Li-Qing; Yu, Wen-Yan; Xu, Jing-Jing; Cao, Jun

2018-01-15

A simple, green and effective extraction method, namely, pyridinium ionic liquid- (IL) based liquid-solid extraction (LSE), was first designed to extract the main inorganic and organic iodine compounds (I - , monoiodo-tyrosine (MIT) and diiodo-tyrosine (DIT)). The optimal extraction conditions were as follows: ultrasonic intensity 100W, IL ([EPy]Br) concentration 200mM, extraction time 30min, liquid/solid ratio 10mL/g, and pH value 6.5. The morphologies of Laminaria were studied by scanning electron microscopy and transmission electron microscopy. The recovery values of I - , MIT and DIT from Laminaria were in the range of 88% to 94%, and limits of detection were in the range of 59.40 to 283.6ng/g. The proposed method was applied to the extraction and determination of iodine compounds in three Laminaria. The results showed that IL-based LSE could be a promising method for rapid extraction of bioactive iodine from complex food matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast, low-pressure gas chromatography and liquid chromatography tandem mass spectrometry.

PubMed

González-Curbelo, Miguel Ángel; Lehotay, Steven J; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel

2014-09-05

The "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) approach to sample preparation is widely applied in pesticide residue analysis, but the use of magnesium sulfate and other nonvolatile compounds for salting out in the method is not ideal for mass spectrometry. In this study, we developed and evaluated three new different versions of the QuEChERS method using more volatile salts (ammonium chloride and ammonium formate and acetate buffers) to induce phase separation and extraction of 43 representative pesticide analytes of different classes. Fast low-pressure gas chromatography tandem mass spectrometry (LPGC-MS/MS) and liquid chromatography (LC)-MS/MS were used for analysis. The QuEChERS AOAC Official Method 2007.01 was also tested for comparison purposes. Of the studied methods, formate buffering using 7.5g of ammonium formate and 15mL of 5% (v/v) formic acid in acetonitrile for the extraction of 15g of sample (5g for wheat grain) provided the best performance and practical considerations. Method validation was carried out with and without the use of dispersive solid-phase extraction for cleanup, and no significant differences were observed for the majority of pesticides. The method was demonstrated in quantitative analysis for GC- and LC-amenable pesticides in 4 representative food matrices (apple, lemon, lettuce, and wheat grain). With the typical exceptions of certain pH-dependent and labile pesticides, 90-110% recoveries and <10% RSD were obtained. Detection limits were mostly <5ng/g, which met the general need to determine pesticide concentrations as low as 10ng/g for monitoring purposes in food applications. Published by Elsevier B.V.

Hydrogen-Enhanced Lunar Oxygen Extraction and Storage Using Only Solar Power

NASA Technical Reports Server (NTRS)

Burton, rodney; King, Darren

2013-01-01

The innovation consists of a thermodynamic system for extracting in situ oxygen vapor from lunar regolith using a solar photovoltaic power source in a reactor, a method for thermally insulating the reactor, a method for protecting the reactor internal components from oxidation by the extracted oxygen, a method for removing unwanted chemical species produced in the reactor from the oxygen vapor, a method for passively storing the oxygen, and a method for releasing high-purity oxygen from storage for lunar use. Lunar oxygen exists in various types of minerals, mostly silicates. The energy required to extract the oxygen from the minerals is 30 to 60 MJ/kg O. Using simple heating, the extraction rate depends on temperature. The minimum temperature is approximately 2,500 K, which is at the upper end of available oven temperatures. The oxygen is released from storage in a purified state, as needed, especially if for human consumption. This method extracts oxygen from regolith by treating the problem as a closed batch cycle system. The innovation works equally well in Earth or Lunar gravity fields, at low partial pressure of oxygen, and makes use of in situ regolith for system insulation. The innovation extracts oxygen from lunar regolith using a method similar to vacuum pyrolysis, but with hydrogen cover gas added stoichiometrically to react with the oxygen as it is produced by radiatively heating regolith to 2,500 K. The hydrogen flows over and through the heating element (HE), protecting it from released oxygen. The H2 O2 heat of reaction is regeneratively recovered to assist the heating process. Lunar regolith is loaded into a large-diameter, low-height pancake reactor powered by photovoltaic cells. The reactor lid contains a 2,500 K HE that radiates downward onto the regolith to heat it and extract oxygen, and is shielded above by a multi-layer tungsten radiation shield. Hydrogen cover gas percolates through the perforated tungsten shielding and HE, preventing oxidation of the shielding and HE, and reacting with the oxygen to form water vapor. The water vapor is filtered through solid regolith to remove unwanted extraction byproducts, and then condensed to a liquid state and stored at 300 to 325 K. Conversion to usable oxygen is achieved by pumping liquid water into a high-pressure electrolyzer, storing the gaseous oxygen at high pressure for use, and diverting the hydrogen back to the reactor or to storage. The results from this design effort show that this oxygen-generating concept can be developed in an efficient system with low specific mass. Advantages include use of regolith as an oxygen source, filter, and thermal insulator. The system can be tested in Earth gravity and can be expected to operate similarly in lunar gravity. The system is scalable, either by increasing the power level and output of a standard module, or by employing multiple modules.

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...

The challenges of developing a generic extraction procedure to analyze multi-class veterinary drug residues in milk and honey using ultra-high pressure liquid chromatography quadrupole time-of-flight mass spectrometry.

PubMed

Wang, Jian; Leung, Daniel

2012-08-01

This paper discusses the analytical challenges to develop a generic extraction procedure to analyze or screen multi-class veterinary drugs in milk and honey using ultra-high pressure liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC QqTOF MS). The veterinary drugs in this study included aminoglycosides, endectocides, fluoroquinolones, ionophores, β-lactams or penicillins, macrolides, NSAIDs, phenicols, sulfonamides and tetracyclines. Veterinary drugs were extracted using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which entailed the use of acetonitrile containing 1% acetic acid, sodium acetate, ethylenediaminetetra acetic acid disodium (EDTA) and magnesium sulfate, and no clean-up was performed. Chromatographic separation was achieved on a reversed-phase Acquity UPLC BEH C(18) , 100 × 2.1 mm, 1.7 µm column with 0.1% formic acid and 10 mM ammonium formate in water, and acetonitrile as mobile phases. Due to poor chromatographic retention, aminoglycosides were first dropped from the list, and because of poor extractability, β-lactams and tetracyclines were also excluded from the method. The method was able to quantify 31 or screen up to 54 drugs (unbound) in honey, and to quantify 34 or screen up to 59 drugs in milk. UHPLC QqTOF data were acquired in TOF MS full-scan mode that allowed both quantification and confirmation of veterinary drugs and identification of their degradation products in samples. The method could achieve detection limits as low as 1 µg/kg with analytical range from 1 to 100 µg/kg. The developed method was intended to be used for screening of as many analytes as possible in one single analysis, or unequivocal confirmation of positive findings and degradation product identification based on accurate mass measurement and isotopic patterns. © Her Majesty the Queen in Right of Canada 2012. Reproduced with the permission of the Minister of Agriculture.

Antioxidant, Anti-inflammatory, Analgesic Properties, and Phytochemical Characterization of Stem Bark Extract and Fractions of Anthocleista nobilis

PubMed Central

Ngwoke, Kenneth Gerald; Akwagbulam, Amaka Godsaveus; Erhirhie, Ernest Oghenesuvwe; Ajaghaku, Daniel Lotanna; Okoye, Festus Basden Chiedu; Esimone, Charles Okechukwu

2018-01-01

Background: Anthocleista nobilis (Loganiaceae) is used by Mbano people of Imo State, Nigeria, for the treatment of various ailments Objective: The aim of this study is to evaluate the antioxidant, anti-inflammatory, and analgesic properties of the methanol extract, fractions, and subfractions of A. nobilis. Materials and Methods: The powdered stem bark was extracted with methanol and sequentially fractionated into n-hexane, ethyl acetate, and butanol fractions. The constituents of the fractions were analyzed using high-pressure liquid chromatography (HPLC), and the components were identified by dereplication. Antioxidant potential of the extracts and fractions was investigated using 2,2-diphenyl-1-picrylhydrazyl free-radical scavenging method. Anti-inflammatory and analgesic activities of the extract and fractions were also investigated using xylene-induced inflammation and acetic acid-induced writhing models, respectively. Results: A total of five compounds isovitexin (Rt = 18.77 min), isovitexin-2''-O-xyl (Rt = 19.68 min), p-Hydroxybenzoic acid (Rt = 11.88 min), Sarasinoside L (Rt = 19.64 min), isovitexin (Rt = 18.77), and apigenin monoglycoside (Rt = 19.64 min) were identified by HPLC analysis and dereplication. The ethyl acetate fraction and subfraction elicited the best anti-inflammatory activity. The ethyl acetate subfraction also inhibited acetic acid-induced pain by 79% and 85.0% at the doses of 100 mg/kg and 200 mg/kg, respectively, which was better than 71.1% and 81.3% observed for diclofenac at similar doses. Conclusion: A. nobilis could be a potential source of anti-inflammatory and analgesic lead compounds. SUMMARY The extract, fractions and subfractions of Anthocleista nobilis were screened or antioxidant, anti-inflammatory and Analgesic properties in vitro and in mice models. Some of the components were identified by dereplication after HPLC analysis. The results demonstrated potent anti-inflammatory and analgesic property of the extracts and fractions. The dereplication analysis also identified vitexin and related compounds. Abbreviation used: HPLC: High performance Liquid Chromatography; VLC: Vacuum Liquid Chromatography; DPPH: 2,2-Diphenyl-1-pycrylhydrazine; SPSS: Statistical Package for the Social Sciences; ROS: Reactive Oxygen Species PMID:29568192

Antioxidant, Anti-inflammatory, Analgesic Properties, and Phytochemical Characterization of Stem Bark Extract and Fractions of Anthocleista nobilis.

PubMed

Ngwoke, Kenneth Gerald; Akwagbulam, Amaka Godsaveus; Erhirhie, Ernest Oghenesuvwe; Ajaghaku, Daniel Lotanna; Okoye, Festus Basden Chiedu; Esimone, Charles Okechukwu

2018-01-01

Anthocleista nobilis ( Loganiaceae ) is used by Mbano people of Imo State, Nigeria, for the treatment of various ailments. The aim of this study is to evaluate the antioxidant, anti-inflammatory, and analgesic properties of the methanol extract, fractions, and subfractions of A. nobilis . The powdered stem bark was extracted with methanol and sequentially fractionated into n-hexane, ethyl acetate, and butanol fractions. The constituents of the fractions were analyzed using high-pressure liquid chromatography (HPLC), and the components were identified by dereplication. Antioxidant potential of the extracts and fractions was investigated using 2,2-diphenyl-1-picrylhydrazyl free-radical scavenging method. Anti-inflammatory and analgesic activities of the extract and fractions were also investigated using xylene-induced inflammation and acetic acid-induced writhing models, respectively. A total of five compounds isovitexin ( R t = 18.77 min), isovitexin-2''-O-xyl ( R t = 19.68 min), p-Hydroxybenzoic acid ( R t = 11.88 min), Sarasinoside L ( R t = 19.64 min), isovitexin ( R t = 18.77), and apigenin monoglycoside ( R t = 19.64 min) were identified by HPLC analysis and dereplication. The ethyl acetate fraction and subfraction elicited the best anti-inflammatory activity. The ethyl acetate subfraction also inhibited acetic acid-induced pain by 79% and 85.0% at the doses of 100 mg/kg and 200 mg/kg, respectively, which was better than 71.1% and 81.3% observed for diclofenac at similar doses. A. nobilis could be a potential source of anti-inflammatory and analgesic lead compounds. The extract, fractions and subfractions of Anthocleista nobilis were screened or antioxidant, anti-inflammatory and Analgesic properties in vitro and in mice models. Some of the components were identified by dereplication after HPLC analysis. The results demonstrated potent anti-inflammatory and analgesic property of the extracts and fractions. The dereplication analysis also identified vitexin and related compounds. Abbreviation used: HPLC: High performance Liquid Chromatography; VLC: Vacuum Liquid Chromatography; DPPH: 2,2-Diphenyl-1-pycrylhydrazine; SPSS: Statistical Package for the Social Sciences; ROS: Reactive Oxygen Species.

Preparation and Characterization of Micronized Artemisinin via a Rapid Expansion of Supercritical Solutions (RESS) Method

PubMed Central

Yu, Huimin; Zhao, Xiuhua; Zu, Yuangang; Zhang, Xinjuan; Zu, Baishi; Zhang, Xiaonan

2012-01-01

The particle sizes of pharmaceutical substances are important for their bioavailability. Bioavailability can be improved by reducing the particle size of the drug. In this study, artemisinin was micronized by the rapid expansion of supercritical solutions (RESS). The particle size of the unprocessed white needle-like artemisinin particles was 30 to 1200 μm. The optimum micronization conditions are determined as follows: extraction temperature of 62 °C, extraction pressure of 25 MPa, precipitation temperature 45 °C and nozzle diameter of 1000 μm. Under the optimum conditions, micronized artemisinin with a (mean particle size) MPS of 550 nm is obtained. By analysis of variance (ANOVA), extraction temperature and pressure have significant effects on the MPS of the micronized artemisinin. The particle size of micronized artemisinin decreased with increasing extraction temperature and pressure. Moreover, the SEM, LC-MS, FTIR, DSC and XRD allowed the comparison between the crystalline initial state and the micronization particles obtained after the RESS process. The results showed that RESS process has not induced degradation of artemisinin and that processed artemisinin particles have lower crystallinity and melting point. The bulk density of artemisinin was determined before and after RESS process and the obtained results showed that it passes from an initial density of 0.554 to 0.128 g·cm−3 after the processing. The decrease in bulk density of the micronized powder can increase the liquidity of drug particles when they are applied for medicinal preparations. These results suggest micronized powder of artemisinin can be of great potential in drug delivery systems. PMID:22606030

Ionic Liquids as Quasihydrostatic Pressure Media for Diamond Anvil Cell Experiments

NASA Astrophysics Data System (ADS)

Mayorga, Sierra; Moldowan, Kaela; Dan, Ioana; Forster, Paul; Iota, Valentin

2012-02-01

Ionic liquids (ILs) are salts in which the ions are poorly coordinated to the point where the eutectic mixture remains liquid at room temperature. In general, ILs exhibit high chemical and thermal stability, have extended liquid regions in the pressure-temperature domain, and can be easily obtained. Commercial ionic liquids are relatively inexpensive and custom ionic solutions can be easily synthesized by mixing common reactants. These properties make ionic liquids attractive candidates for high-pressure media in Diamond Anvil Cell (DAC) experiments. In this presentation we explore the use of ionic liquids as DAS quasihydrostatic pressure media for pressures up to 50 GPa. As a measure of hydrostaticity we monitor the splitting and peak-widths of the R1 andR 2 fluorescence lines from small ruby chips (Al2O3 :Cr^3+) imbedded in the pressure medium. We present results on a series of commercially available ionic fluids against standard pressure media: methanol-ethanol mixtures, silicone oil, sodium chloride (NaCl) and noble gases (Ar, Ne, He).

Ionic-Liquid-Mediated Extraction and Separation Processes for Bioactive Compounds: Past, Present, and Future Trends.

PubMed

Ventura, Sónia P M; E Silva, Francisca A; Quental, Maria V; Mondal, Dibyendu; Freire, Mara G; Coutinho, João A P

2017-05-24

Ionic liquids (ILs) have been proposed as promising media for the extraction and separation of bioactive compounds from the most diverse origins. This critical review offers a compilation on the main results achieved by the use of ionic-liquid-based processes in the extraction and separation/purification of a large range of bioactive compounds (including small organic extractable compounds from biomass, lipids, and other hydrophobic compounds, proteins, amino acids, nucleic acids, and pharmaceuticals). ILs have been studied as solvents, cosolvents, cosurfactants, electrolytes, and adjuvants, as well as used in the creation of IL-supported materials for separation purposes. The IL-based processes hitherto reported, such as IL-based solid-liquid extractions, IL-based liquid-liquid extractions, IL-modified materials, and IL-based crystallization approaches, are here reviewed and compared in terms of extraction and separation performance. The key accomplishments and future challenges to the field are discussed, with particular emphasis on the major lacunas found within the IL community dedicated to separation processes and by suggesting some steps to overcome the current limitations.

Selective Solid-liquid Extraction and Liquid-liquid Extraction of Lithium Chloride using Strapped Calix[4]pyrroles

DOE PAGES

He, Qing; Williams, Neil J.; Oh, Ju; ...

2018-05-25

LiCl is a classic "hard" ion salt that is present in lithium-rich brines and a key component in end-of-life materials (i.e., used lithium-ion batteries). Its isolation and purification from like salts is a recognized challenge with potential strategic and economic implications. Here in this paper, we describe two ditopic calix[4]pyrrole-based ion pair receptors (2 and 3), that are capable of selectively capturing LiCl. Under solid-liquid extraction conditions, using 2 as the extractant, LiCl could be separated from a NaCl-KCl salt mixture containing as little as 1% LiCl with ~100% selectivity, while receptor 3 achieved similar separations when the LiCl levelmore » was as low as 200 ppm. Under liquid-liquid extraction conditions using nitrobenzene as the non-aqueous phase, the extraction preference displayed by 2 is KCl > NaCl > LiCl. Lastly, in contrast, 3 exhibits high selectivity towards LiCl over NaCl and KCl, with no appreciable extraction being observed for the latter two salts.« less

Selective Solid-liquid Extraction and Liquid-liquid Extraction of Lithium Chloride using Strapped Calix[4]pyrroles

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

He, Qing; Williams, Neil J.; Oh, Ju

LiCl is a classic "hard" ion salt that is present in lithium-rich brines and a key component in end-of-life materials (i.e., used lithium-ion batteries). Its isolation and purification from like salts is a recognized challenge with potential strategic and economic implications. Here in this paper, we describe two ditopic calix[4]pyrrole-based ion pair receptors (2 and 3), that are capable of selectively capturing LiCl. Under solid-liquid extraction conditions, using 2 as the extractant, LiCl could be separated from a NaCl-KCl salt mixture containing as little as 1% LiCl with ~100% selectivity, while receptor 3 achieved similar separations when the LiCl levelmore » was as low as 200 ppm. Under liquid-liquid extraction conditions using nitrobenzene as the non-aqueous phase, the extraction preference displayed by 2 is KCl > NaCl > LiCl. Lastly, in contrast, 3 exhibits high selectivity towards LiCl over NaCl and KCl, with no appreciable extraction being observed for the latter two salts.« less

Production and uses of liquefied atmosphere (CO2) on Mars

NASA Technical Reports Server (NTRS)

Waldron, R. D.

1991-01-01

Carbon dioxide is universally accessible on Mars, and can be liquefied and separated from residual atmospheric gases by various compress-refrigeration cycles. Liquid CO2, stored under elevated pressures, can be used as a source of high pressure gas for nighttime power generation at a Martian base powered by solar energy during the daytime. Carbon dioxide can also be used for vehicular power. The extractable energy per unit mass of CO2 can exceed that of commercial lead-acid batteries for operating cycles without heat addition. Improved performance is possible using heat input from the ambient atmosphere or thermochemical agents. A unique vehicular application uses pressurized CO2 as a non-combustion low performance propellant for intermediate distance surface transportation. The thermodynamic properties of CO2 are presented with typical operating cycles for the application classes described above.

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2010 CFR

2010-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

Development of a dispersive liquid-liquid microextraction method using a lighter-than-water ionic liquid for the analysis of polycyclic aromatic hydrocarbons in water.

PubMed

Medina, Giselle S; Reta, Mario

2016-11-01

A dispersive liquid-liquid microextraction method using a lighter-than-water phosphonium-based ionic liquid for the extraction of 16 polycyclic aromatic hydrocarbons from water samples has been developed. The extracted compounds were analyzed by liquid chromatography coupled to fluorescence/diode array detectors. The effects of several experimental parameters on the extraction efficiency, such as type and volume of ionic liquid and disperser solvent, type and concentration of salt in the aqueous phase and extraction time, were investigated and optimized. Three phosphonium-based ionic liquids were assayed, obtaining larger extraction efficiencies when trihexyl-(tetradecyl)phosphonium bromide was used. The optimized methodology requires a few microliters of a lighter-than-water phosphonium-based ionic liquid, which allows an easy separation of the extraction solvent phase. The obtained limits of detection were between 0.02 and 0.56 μg/L, enrichment factors between 109 and 228, recoveries between 60 and 108%, trueness between 0.4 and 9.9% and reproducibility values between 3 and 12% were obtained. These figures of merit combined with the simplicity, rapidity and low cost of the analytical methodology indicate that this is a viable and convenient alternative to the methods reported in the literature. The developed method was used to analyze polycyclic aromatic hydrocarbons in river water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ionic-liquid-based ultrasound-assisted extraction of isoflavones from Belamcanda chinensis and subsequent screening and isolation of potential α-glucosidase inhibitors by ultrafiltration and semipreparative high-performance liquid chromatography.

PubMed

Li, Senlin; Li, Sainan; Huang, Yu; Liu, Chunming; Chen, Lina; Zhang, Yuchi

2017-06-01

The separation of a compound of interest from its structurally similar homologues to produce high-purity natural products is a challenging problem. This work proposes a novel method for the separation of iristectorigenin A from its structurally similar homologues by ionic-liquid-based ultrasound-assisted extraction and the subsequent screening and isolation of potential α-glucosidase inhibitors via ultrafiltration and semipreparative high-performance liquid chromatography. Ionic-liquid-based ultrasound-assisted extraction was successfully applied to the extraction of tectorigenin, iristectorigenin A, irigenin, and irisflorentin from Belamcanda chinensis. The optimum conditions for the efficient extraction of isoflavones were determined as 1.0 M 1-ethyl-3-methylimidazolium tetrafluoroborate with extraction time of 30 min and a solvent to solid ratio of 30 mL/g. Ultrafiltration with liquid chromatography and mass spectrometry was applied to screen and identify α-glucosidase inhibitors from B. chinensis, followed by the application of semipreparative high-performance liquid chromatography to separate and isolate the active constituents. Four major compounds including tectorigenin, iristectorigenin A, irigenin, and irisflorentin were screened and identified as α-glucosidase inhibitors, and then the four active compounds abovementioned were subsequently isolated by semipreparative high-performance liquid chromatography (99.89, 88.97, 99.79, and 99.97% purity, respectively). The results demonstrate that ionic liquid extraction can be successfully applied to the extraction of isoflavones from B. chinensis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines.

PubMed

Silva, Catarina L; Gonçalves, João L; Câmara, José S

2012-08-20

A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250μL) in five extraction cycle and in a short time period (about 5min for the entire sample preparation step). Under optimized conditions, excellent linearity (R(values)(2)>0.9963), limits of detection of 0.006μgmL(-1) (quercetin) to 0.013μgmL(-1) (myricetin) and precision within 0.5-3.1% were observed for the target flavonols. The average recoveries of myricetin, quercetin and kaempferol for real samples were 83.0-97.7% with relative standard deviation (RSD, %) lower than 1.6%. The results obtained showed that the most abundant flavonol in the analyzed samples was myricetin (5.8±3.7μgmL(-1)). Quercetin (0.97±0.41μgmL(-1)) and kaempferol (0.66±0.24μgmL(-1)) were found in a lower concentration. The optimized MEPS(C8) method was compared with a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis HLB) were used as reference. MEPS(C8) approach offers an attractive alternative for analysis of flavonols in wines, providing a number of advantages including highest extraction efficiency (from 85.9±0.9% to 92.1±0.5%) in the shortest extraction time with low solvent consumption, fast sample throughput, more environmentally friendly and easy to perform. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed Central

Hong, Show-Jen

2015-01-01

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

33 CFR 156.170 - Equipment tests and inspections.

Code of Federal Regulations, 2014 CFR

2014-07-01

... distort under static liquid pressure at least 11/2 times the maximum allowable working pressure; and (iv... static liquid pressure test is successfully completed in the presence of the COTP. The test medium is not... static liquid pressure at least 11/2 times the maximum allowable working pressure; and (5) Each item of...

33 CFR 156.170 - Equipment tests and inspections.

Code of Federal Regulations, 2012 CFR

2012-07-01

... distort under static liquid pressure at least 11/2 times the maximum allowable working pressure; and (iv... static liquid pressure test is successfully completed in the presence of the COTP. The test medium is not... static liquid pressure at least 11/2 times the maximum allowable working pressure; and (5) Each item of...

33 CFR 156.170 - Equipment tests and inspections.

Code of Federal Regulations, 2013 CFR

2013-07-01

... distort under static liquid pressure at least 11/2 times the maximum allowable working pressure; and (iv... static liquid pressure test is successfully completed in the presence of the COTP. The test medium is not... static liquid pressure at least 11/2 times the maximum allowable working pressure; and (5) Each item of...

Review on pressure swirl injector in liquid rocket engine

NASA Astrophysics Data System (ADS)

Kang, Zhongtao; Wang, Zhen-guo; Li, Qinglian; Cheng, Peng

2018-04-01

The pressure swirl injector with tangential inlet ports is widely used in liquid rocket engine. Commonly, this type of pressure swirl injector consists of tangential inlet ports, a swirl chamber, a converging spin chamber, and a discharge orifice. The atomization of the liquid propellants includes the formation of liquid film, primary breakup and secondary atomization. And the back pressure and temperature in the combustion chamber could have great influence on the atomization of the injector. What's more, when the combustion instability occurs, the pressure oscillation could further affects the atomization process. This paper reviewed the primary atomization and the performance of the pressure swirl injector, which include the formation of the conical liquid film, the breakup and atomization characteristics of the conical liquid film, the effects of the rocket engine environment, and the response of the injector and atomization on the pressure oscillation.

Thermodynamic Vent System Test in a Low Earth Orbit Simulation

NASA Technical Reports Server (NTRS)

VanOverbeke, Thomas J.

2004-01-01

A thermodynamic vent system for a cryogenic nitrogen tank was tested in a vacuum chamber simulating oxygen storage in low earth orbit. The nitrogen tank was surrounded by a cryo-shroud at -40 F. The tank was insulated with two layers of multi-layer insulation. Heat transfer into cryogenic tanks causes phase change and increases tank pressure which must be controlled. A thermodynamic vent system was used to control pressure as the location of vapor is unknown in low gravity and direct venting would be wasteful. The thermodynamic vent system consists of a Joule-Thomson valve and heat exchanger installed on the inlet side of the tank mixer-pump. The combination is used to extract thermal energy from the tank fluid, reducing temperature and ullage pressure. The system was sized so that the tank mixer-pump operated a small fraction of the time to limit motor heating. Initially the mixer used sub-cooled liquid to cool the liquid-vapor interface inducing condensation and pressure reduction. Later, the thermodynamic vent system was used. Pressure cycles were performed until steady-state operation was demonstrated. Three test runs were conducted at tank fills of 97, 80, and 63 percent. Each test was begun with a boil-off test to determine heat transfer into the tank. The lower tank fills had time averaged vent rates very close to steady-state boil-off rates showing the thermodynamic vent system was nearly as efficient as direct venting in normal gravity.

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

PubMed

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

2016-06-05

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

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.

Inhibitory activities of selected Sudanese medicinal plants on Porphyromonas gingivalis and matrix metalloproteinase-9 and isolation of bioactive compounds from Combretum hartmannianum (Schweinf) bark.

PubMed

Mohieldin, Ebtihal Abdalla M; Muddathir, Ali Mahmoud; Mitsunaga, Tohru

2017-04-20

Periodontal diseases are one of the major health problems and among the most important preventable global infectious diseases. Porphyromonas gingivalis is an anaerobic Gram-negative bacterium which has been strongly implicated in the etiology of periodontitis. Additionally, matrix metalloproteinases-9 (MMP-9) is an important factor contributing to periodontal tissue destruction by a variety of mechanisms. The purpose of this study was to evaluate the selected Sudanese medicinal plants against P. gingivalis bacteria and their inhibitory activities on MMP-9. Sixty two methanolic and 50% ethanolic extracts from 24 plants species were tested for antibacterial activity against P. gingivalis using microplate dilution assay method to determine the minimum inhibitory concentration (MIC). The inhibitory activity of seven methanol extracts selected from the 62 extracts against MMP-9 was determined by Colorimetric Drug Discovery Kit. In search of bioactive lead compounds, Combretum hartmannianum bark which was found to be within the most active plant extracts was subjected to various chromatographic (medium pressure liquid chromatography, column chromatography on a Sephadex LH-20, preparative high performance liquid chromatography) and spectroscopic methods (liquid chromatography-mass spectrometry, Nuclear Magnetic Resonance (NMR)) to isolate and characterize flavogalonic acid dilactone and terchebulin as bioactive compounds. About 80% of the crude extracts provided a MIC value ≤4 mg/ml against bacteria. The extracts which revealed the highest potency were: methanolic extracts of Terminalia laxiflora (wood; MIC = 0.25 mg/ml) followed by Acacia totrtilis (bark), Ambrosia maritima (aerial part), Argemone mexicana (seed), C. hartmannianum (bark), Terminalia brownii (wood) and 50% ethanolic extract of T. brownii (bark) with MIC values of 0.5 mg/ml. T. laxiflora (wood) and C. hartmannianum (bark) which belong to combretaceae family showed an inhibitory activity over 50% at the concentration of 10 μg/ml against MMP-9. Additionally, MMP-9 was significantly inhibited by terchebulin with IC 50 value of 6.7 μM. To the best of our knowledge, flavogalonic acid dilactone and terchebulin were isolated from C. hartmannianium bark for the first time in this study. Because of terchebulin and some crude extracts acting on P. gingivalis bacteria and MMP-9 enzyme that would make them promising natural preference for preventing and treating periodontal diseases.

Space Shuttle Upgrade Liquid Oxygen Tank Thermal Stratification

NASA Technical Reports Server (NTRS)

Tunc, Gokturk; Wagner, Howard; Bayazitoglu, Yildiz

2001-01-01

In 1997, NASA initiated a study of a liquid oxygen and ethanol orbital maneuvering and reaction control system for space shuttle upgrades as well as other reusable launch vehicle applications. The pressure-fed system uses sub-cooled liquid oxygen at 2413.2 KPa (350 psia) stored passively using insulation. Thermal stratification builds up while the space shuttle is docked at the international space station. The venting from the space shuttle's liquid oxygen tank is not desired during this 96-hr time period. Once the shuttle undocks from the space station there could be a pressure collapse in the liquid oxygen tank caused by fluid mixing due to the thruster fU"ings . The thermal stratification and resulting pressure rise in the tank were examined by a computational fluid dynamic model. Since the heat transfer from the pressurant gas to the liquid will result in a decrease in tank pressure the final pressure after the 96 hours will be significantly less when the tank is pressurized with ambient temperature helium. Therefore, using helium at ambient temperature to pressurize the tank is preferred to pressurizing the tank with helium at the liquid oxygen temperature. The higher helium temperature will also result in less mass of helium to pressurize the tank.

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2011 CFR

2011-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... UF4 to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

Laboratory Production of Lemon Liqueur (Limoncello) by Conventional Maceration and a Two-Syringe System to Illustrate Rapid Solid-Liquid Dynamic Extraction

ERIC Educational Resources Information Center

Naviglio, Daniele; Montesano, Domenico; Gallo, Monica

2015-01-01

Two experimental techniques of solid-liquid extraction are compared relating to the lab-scale production of lemon liqueur, most commonly named "limoncello"; the first is the official method of maceration for the solid-liquid extraction of analytes and is widely used to extract active ingredients from a great variety of natural products;…

Compressed liquid densities, saturated liquid densities, and vapor pressures of 1,1-difluoroethane

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

Defibaugh, D.R.; Morrison, G.

1996-05-01

The compressed liquid densities and vapor pressures of 1,1-difluoroethane (HFC-152a) have been measured, correlated, and compared with other data. The liquid densities were measured with a combined standard uncertainty of {+-}0.05% using a vibrating tube densimeter over a temperature range of 243 K to 371 K and at pressures from near the saturated vapor pressure to 6,500 kPa; thus the data extend nearly to the critical point ({Tc} = 386.41 K and P{sub c} = 4514.7 kPa). The vapor pressures were measured with a combined standard uncertainty of {+-}0.02% using a stainless steel ebulliometer in the temperature range from 280more » K to 335 K. Saturated liquid densities were calculated by extrapolating the compressed liquid isotherms to the saturation pressure.« less

Thermal stratification in LH2 tank of cryogenic propulsion stage tested in ISRO facility

NASA Astrophysics Data System (ADS)

Xavier, M.; Raj, R. Edwin; Narayanan, V.

2017-02-01

Liquid oxygen and hydrogen are used as oxidizer and fuel respectively in cryogenic propulsion system. These liquids are stored in foam insulated tanks of cryogenic propulsion system and are pressurized using warm pressurant gas supplied for tank pressure maintenance during cryogenic engine operation. Heat leak to cryogenic propellant tank causes buoyancy driven liquid stratification resulting in formation of warm liquid stratum at liquid free surface. This warm stratum is further heated by the admission of warm pressurant gas for tank pressurization during engine operation. Since stratified layer temperature has direct bearing on the cavitation free operation of turbo pumps integrated in cryogenic engine, it is necessary to model the thermal stratification for predicting stratified layer temperature and mass of stratified liquid in tank at the end of engine operation. These inputs are required for estimating the minimum pressure to be maintained by tank pressurization system. This paper describes configuration of cryogenic stage for ground qualification test, stage hot test sequence, a thermal model and its results for a foam insulated LH2 tank subjected to heat leak and pressurization with hydrogen gas at 200 K during liquid outflow at 38 lps for engine operation. The above model considers buoyancy flow in free convection boundary layer caused by heat flux from tank wall and energy transfer from warm pressurant gas etc. to predict temperature of liquid stratum and mass of stratified liquid in tank at the end of engine operation in stage qualification tests carried out in ISRO facility.

Liquid CO2 extraction of Jasminum grandiflorum and comparison with conventional processes.

PubMed

Prakash, Om; Sahoo, Deeptanjali; Rout, Prasant Kumar

2012-01-01

The concrete (0.35%) of Jasminum grandiflorum L. flowers was prepared by extraction in n-pentane, and the absolute (0.27%) by fractionation of the n-pentane extract (concrete) with cold methanol. Direct extraction of flowers with liquid CO2 gave a relatively fat-free product in 0.26% yield. The liquid CO2 extract was enriched with terpenoids and benzenoids, thus providing the organoleptically accepted product. The major compounds, such as benzyl acetate, (E,E)-alpha-farnesene and (Z)-3-hexenyl benzoate, along with compounds like indole, methyl anthranilate, (Z)-jasmone, (Z)-methyl jasmonoate and (Z)-methyl epi-jasmonoate, are responsible for the high diffusivity of the jasmine fragrance. These compounds have been obtained with improved recoveries in the liquid CO2 extract. On the other hand, the yield of the essential oil was poor (0.05%), and some polar compounds (oxygenated terpenoids) were recovered in less amounts in comparison with either the n-pentane or liquid CO2 extract.

Use of liquid/supercritical CO2 extraction process for butanol recovery from fermentation broth

USDA-ARS?s Scientific Manuscript database

In order for butanol fermentation to be a viable option, it is essential to recover it from fermentation broth using economical alternate in-situ product recovery techniques such as liquid/supercritical CO2 extraction as compared to distillation. This technique (liquid CO2 extraction & supercritical...

Screening of commercial and pecan shell-extracted liquid smoke agents as natural antimicrobials against foodborne pathogens.

PubMed

Van Loo, Ellen J; Babu, D; Crandall, Philip G; Ricke, Steven C

2012-06-01

Liquid smoke extracts have traditionally been used as flavoring agents, are known to possess antioxidant properties, and serve as natural alternatives to conventional antimicrobials. The antimicrobial efficacies of commercial liquid smoke samples may vary depending on their source and composition and the methods used to extract and concentrate the smoke. We investigated the MICs of eight commercial liquid smoke samples against Salmonella Enteritidis, Staphylococcus aureus, and Escherichia coli . The commercial liquid smoke samples purchased were supplied by the manufacturer as water-based or concentrated extracts of smoke from different wood sources. The MICs of the commercial smokes to inhibit the growth of foodborne pathogens ranged from 0.5 to 6.0% for E. coli, 0.5 to 8.0% for Salmonella, and 0.38 to 6% for S. aureus. The MIC for each liquid smoke sample was similar in its effect on both E. coli and Salmonella. Solvent-extracted antimicrobials prepared using pecan shells displayed significant differences between their inhibitory concentrations depending on the type of solvent used for extraction. The results indicated that the liquid smoke samples tested in this study could serve as effective natural antimicrobials and that their inhibitory effects depended more on the solvents used for extraction than the wood source.

Trilinolein identified as a sex-specific component of tergal glands in alates of Coptotermes formosanus.

PubMed

Bland, John M; Park, Yong Ihl; Raina, Ashok K; Dickens, Joseph C; Hollister, Benedict

2004-04-01

Hexane extracts of the tergal glands from female alates of the Formosan subterranean termite Coptotermes formosanus were analyzed by high performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry with collision-induced dissociation. Double bond configuration was determined by chemical modifications with gas chromatography-mass spectrometry. A single component, identified as the triacylglycerol, trilinolein, was unique to the female tergal glands. This compound was not found in other areas of the female alate abdomen or in the corresponding area of male alates. Neither gland extract nor trilinolein caused a behavioral response from male alates. However, significant differences were found between males and females for responses from neurons within sensilla of the maxillary palps.

Expedient preparative isolation and tandem mass spectrometric characterization of C-seco triterpenoids from Neem oil.

PubMed

Haldar, Saikat; Mulani, Fayaj A; Aarthy, Thiagarayaselvam; Dandekar, Devdutta S; Thulasiram, Hirekodathakallu V

2014-10-31

C-seco triterpenoids are widely bioactive class of natural products with high structural complexity and diversity. The preparative isolation of these molecules with high purity is greatly desirable, although restricted due to the complexity of natural extracts. In this article we have demonstrated a Medium Pressure Liquid Chromatography (MPLC) based protocol for the isolation of eight major C-seco triterpenoids of salannin skeleton from Neem (Azadirachta indica) oil. Successive application of normal phase pre-packed silica-gel columns for the fractionation followed by reverse phase in automated MPLC system expedited the process and furnished highly pure metabolites. Furthermore, eight isolated triterpenoids along with five semi-synthesized derivatives were characterized using ultra performance liquid chromatography-electrospray ionization-quadrupole/orbitrap-MS/MS spectrometry as a rapid and sensitive identification technique. The structure-fragment relationships were established on the basis of plausible mechanistic pathway for the generation of daughter ions. The MS/MS spectral information of the triterpenoids was further utilized for the identification of studied molecules in the complex extract of stem and bark tissues from Neem. Copyright © 2014 Elsevier B.V. All rights reserved.

Screening and Identification of the Metabolites in Rat Plasma and Urine after Oral Administration of Areca catechu L. Nut Extract by Ultra-High-Pressure Liquid Chromatography Coupled with Linear Ion Trap-Orbitrap Tandem Mass Spectrometry.

PubMed

Li, Lulu; Luo, Zhiqiang; Liu, Yang; Wang, Hao; Liu, Aoxue; Yu, Guohua; Li, Mengwei; Yang, Ruirui; Chen, Xinjing; Zhu, Jialian; Zhao, Baosheng

2017-06-21

Areca catechu L. nut, a well-known toxic traditional herbal medicine, has been widely used to treat various diseases in China and many other Asian countries for centuries. However, to date the in vivo absorption and metabolism of its multiple bioactive or toxic components still remain unclear. In this study, liquid chromatography coupled with tandem mass spectrometry was used to analyze the major components and their metabolites in rat plasma and urine after oral administration of Areca catechu L. nut extract (ACNE). A total of 12 compounds, including 6 alkaloids, 3 tannins and 3 amino acids, were confirmed or tentatively identified from ACNE. In vivo, 40 constituents, including 8 prototypes and 32 metabolites were identified in rat plasma and urine samples. In summary, this study showed an insight into the metabolism of ACNE in vivo, which may provide helpful chemical information for better understanding of the toxicological and pharmacological profiles of ACNE.

Literature Review: Crud Formation at the Liquid/Liquid Interface of TBP-Based Solvent-Extraction Processes

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

Delegard, Calvin H.; Casella, Amanda J.

2016-09-30

This report summarizes the literature reviewed on crud formation at the liquid:liquid interface of solvent extraction processes. The review is focused both on classic PUREX extraction for industrial reprocessing, especially as practiced at the Hanford Site, and for those steps specific to plutonium purification that were used at the Plutonium Reclamation Facility (PRF) within the Plutonium Finishing Plant (PFP) at the Hanford Site.

An inkjet-printed microfluidic device for liquid-liquid extraction.

PubMed

Watanabe, Masashi

2011-04-07

A microfluidic device for liquid-liquid extraction was quickly produced using an office inkjet printer. An advantage of this method is that normal end users, who are not familiar with microfabrication, can produce their original microfluidic devices by themselves. In this method, the printer draws a line on a hydrophobic and oil repellent surface using hydrophilic ink. This line directs a fluid, such as water or xylene, to form a microchannel along the printed line. Using such channels, liquid-liquid extraction was successfully performed under concurrent and countercurrent flow conditions. © The Royal Society of Chemistry 2011

Removal of actinide elements from liquid scintillation cocktail wastes using liquid-liquid extraction and demulsification techniques

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

Foltz, K.; Landsberger, S.; Srinivasan, B.

1994-12-31

A method for the separation of radionuclides with Z greater than 88, from lower-level radioactive wastes (liquid scintillation cocktail or LSC wastes), is described. The method is liquid-liquid extraction (LLX) and demulsification. The actinide elements are removed from the LSC wastes by extraction into an aqueous phase after the cocktail has been demulsified. The aqueous and organic phases are separated, then the wastes type remaining may be incinerated. Future experiments will be performed to study the effects of pH and temperature and to extend the study to wastes containing americium.

Liquid and solid self-microemulsifying drug delivery systems for improving the oral bioavailability of andrographolide from a crude extract of Andrographis paniculata.

PubMed

Sermkaew, Namfa; Ketjinda, Wichan; Boonme, Prapaporn; Phadoongsombut, Narubodee; Wiwattanapatapee, Ruedeekorn

2013-11-20

The purpose of this study was to develop self-microemulsifying formulations of an Andrographis paniculata extract in liquid and pellet forms for an improved oral delivery of andrographolide. The optimized liquid self-microemulsifying drug delivery system (SMEDDS) was composed of A. paniculata extract (11.1%), Capryol 90 (40%), Cremophor RH 40 (40%) and Labrasol (8.9%). This liquid SMEDDS was further adsorbed onto colloidal silicon dioxide and microcrystalline cellulose, and converted to SMEDDS pellets by the extrusion/spheronization technique. The microemulsion droplet sizes of the liquid and pellet formulations after dilution with water were in the range of 23.4 and 30.3 nm. The in vitro release of andrographolide from the liquid SMEDDS and SMEDDS pellets was 97.64% (SD 1.97%) and 97.74% (SD 3.36%) within 15 min, respectively while the release from the initial extract was only 10%. The oral absorption of andrographolide was determined in rabbits. The C(max) value of andrographolide from the A. paniculata extract liquid SMEDDS and SMEDDS pellet formulations (equivalent to 17.5mg/kg of andrographolide) was 6-fold and 5-fold greater than the value from the initial extract in aqueous suspension (equivalent to 35 mg/kg of andrographolide), respectively. In addition, the AUC(0-12h) was increased 15-fold by the liquid SMEDDS and 13-fold by the SMEDDS pellets compared to the extract in aqueous suspension, respectively. The results clearly indicated that the liquid and solid SMEDDS could be effectively used to improve the dissolution and oral bioavailability that would also enable a reduction in the dose of the poorly water soluble A. paniculata extract. Copyright © 2013 Elsevier B.V. All rights reserved.

Task-specific ionic liquid-assisted extraction and separation of astaxanthin from shrimp waste.

PubMed

Bi, Wentao; Tian, Minglei; Zhou, Jun; Row, Kyung Ho

2010-08-15

Astaxanthin, as an outstanding antioxidant reagent, was successfully extracted from shrimp waste by the ionic liquids based ultrasonic-assisted extraction. Seven kinds of imidazolium ionic liquids with different cations and anions were investigated in this work and one task-specific ionic liquid in ethanol with 0.50molL(-1) was selected as the solvent. At the optimized ultrasonic extraction conditions, the extraction amount of astaxanthin increased 98% (92.7microg g(-1)) compared to the conventional method (46.7microg g(-1)). Furthermore, the extracted solution was isolated through the solid-phase extraction with a molecularly imprinted polymer sorbent. After loading the samples on molecularly imprinted polymer cartridge, the different washing and elution solvents, such as water, methanol, n-hexane, acetone and dichloromethane, were evaluated, and finally, astaxanthin was separated from the shrimp waste extract. Copyright 2010 Elsevier B.V. All rights reserved.