An Improved Method for the Extraction and Thin-Layer Chromatography of Chlorophyll A and B from Spinach

ERIC Educational Resources Information Center

Quach, Hao T.; Steeper, Robert L.; Griffin, William G.

2004-01-01

A simple and fast method, which resolves chlorophyll a and b from spinach leaves on analytical plates while minimizing the appearance of chlorophyll degradation products is shown. An improved mobile phase for the Thin-layer chromatographic analysis of spinach extract that allows for the complete resolution of the common plant pigments found in…

FAST TRACK COMMUNICATION: Spontaneous symmetry breaking in a bridge model fed by junctions

NASA Astrophysics Data System (ADS)

Popkov, Vladislav; Evans, Martin R.; Mukamel, David

2008-10-01

We introduce a class of 1D models mimicking a single-lane bridge with two junctions and two particle species driven in opposite directions. The model exhibits spontaneous symmetry breaking (SSB) for a range of injection/extraction rates. In this phase the steady-state currents of the two species are not equal. Moreover, there is a co-existence region in which the symmetry-broken phase co-exists with a symmetric phase. Along a path in which the extraction rate is varied, keeping the injection rate fixed and large, hysteresis takes place. The mean-field phase diagram is calculated and supporting Monte Carlo simulations are presented. One of the transition lines exhibits a kink, a feature which cannot exist in transition lines of equilibrium phase transitions.

Rapid method for the simultaneous detection of boar taint compounds by means of solid phase microextraction coupled to gas chromatography/mass spectrometry.

PubMed

Verplanken, Kaat; Wauters, Jella; Van Durme, Jim; Claus, Dirk; Vercammen, Joeri; De Saeger, Sarah; Vanhaecke, Lynn

2016-09-02

Because of animal welfare issues, the voluntary ban on surgical castration of male piglets, starting January 2018 was announced in a European Treaty. One viable alternative is the fattening of entire male pigs. However, this can cause negative consumer reactions due to the occurrence of boar taint and possibly lead to severe economic losses in pig husbandry. In this study, headspace solid phase microextraction (HS-SPME) coupled to GC-MS was used in the development and optimization of a candidate method for fast and accurate detection of the boar taint compounds. Remarkably fast extraction (45s) of the boar taint compounds from adipose tissue was achieved by singeing the fat with a soldering iron while released volatiles were extracted in-situ using HS-SPME. The obtained method showed good performance characteristics after validation according to CD 2002/657/EC and ISO/IEC 17025 guidelines. Moreover, cross-validation with an in-house UHPLC-HR-Orbitrap-MS method showed good agreement between an in-laboratory method and the new candidate method for the fast extraction and detection of skatole and androstenone, which emphasizes the accuracy of this new SPME-GC-MS method. Threshold detection of the boar taint compounds on a portable GC-MS could not be achieved. However, despite the lack of sensitivity obtained on the latter instrument, a very fast method with run-to-run time of 3.5min for the detection of the boar taint compounds was developed. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2014-11-01

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

Fast fringe pattern phase demodulation using FIR Hilbert transformers

NASA Astrophysics Data System (ADS)

Gdeisat, Munther; Burton, David; Lilley, Francis; Arevalillo-Herráez, Miguel

2016-01-01

This paper suggests the use of FIR Hilbert transformers to extract the phase of fringe patterns. This method is computationally faster than any known spatial method that produces wrapped phase maps. Also, the algorithm does not require any parameters to be adjusted which are dependent upon the specific fringe pattern that is being processed, or upon the particular setup of the optical fringe projection system that is being used. It is therefore particularly suitable for full algorithmic automation. The accuracy and validity of the suggested method has been tested using both computer-generated and real fringe patterns. This novel algorithm has been proposed for its advantages in terms of computational processing speed as it is the fastest available method to extract the wrapped phase information from a fringe pattern.

Fast trace determination of nine odorant and estrogenic chloro- and bromo-phenolic compounds in real water samples through automated solid-phase extraction coupled with liquid chromatography tandem mass spectrometry.

PubMed

Yuan, Su-Fen; Liu, Ze-Hua; Lian, Hai-Xian; Yang, Chuang-Tao; Lin, Qing; Yin, Hua; Lin, Zhang; Dang, Zhi

2018-02-01

A fast and reliable method was developed for simultaneous trace determination of nine odorous and estrogenic chloro- and bromo-phenolic compounds (CPs and BPs) in water samples using solid-phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS). For sample preparation, the extraction efficiencies of two widely applied cartridges Oasis HLB and Sep-Pak C18 were compared, and the Oasis HLB cartridge showed much better extraction performance; pH of water sample also plays important role on extraction, and pH = 2-3 was found to be most appropriate. For separation of the target compounds, small addition of ammonium hydroxide can obviously improve the detection sensitivity, and the optimized addition concentration was determined as 0.2%. The developed efficient method was validated and showed excellent linearity (R 2  > 0.995), low limit of detection (LOD, 1.9-6.2 ng/L), and good recovery efficiencies of 57-95% in surface and tap water with low relative standard deviation (RSD, 1.3-17.4%). The developed method was finally applied to one tap and one surface water samples and most of these nine targets were detected, but all of them were below their odor thresholds, and their estrogen equivalent (EEQ) were also very low.

Field method for the determination of hexavalent chromium by ultrasonication and strong anion-exchange solid-phase extraction.

PubMed

Wang, J; Ashley, K; Marlow, D; England, E C; Carlton, G

1999-03-01

A simple, fast, sensitive, and economical field method was developed and evaluated for the determination of hexavalent chromium (CrVI) in environmental and workplace air samples. By means of ultrasonic extraction in combination with a strong anion-exchange solid-phase extraction (SAE-SPE) technique, the filtration, isolation, and determination of CrVI in the presence of trivalent chromium (CrIII) and potential interferents was achieved. The method entails (1) ultrasonication in basic ammonium buffer solution to extract CrVI from environmental matrixes; (2) SAE-SPE to separate CrVI from CrIII and interferences; (3) elution/acidification of the eluate; (4) complexation of chromium with 1,5-diphenylcarbazide; and (5) spectrophotometric determination of the colored chromium-diphenylcarbazone complex. Several critical parameters were optimized in order to effect the extraction of both soluble (K2CrO4) and insoluble (PbCrO4) forms of CrVI without inducing CrIII oxidation or CrVI reduction. The method allowed for the dissolution and purification of CrVI from environmental and workplace air sample matrixes for up to 24 samples simultaneously in less than 90 min (including ultrasonication). The results demonstrated that the method was simple, fast, quantitative, and sufficiently sensitive for the determination of occupational exposures of CrVI. The method is applicable for on-site monitoring of CrVI in environmental and industrial hygiene samples.

Explorative solid-phase extraction (E-SPE) for accelerated microbial natural product discovery, dereplication, and purification.

PubMed

Månsson, Maria; Phipps, Richard K; Gram, Lone; Munro, Murray H G; Larsen, Thomas O; Nielsen, Kristian F

2010-06-25

Microbial natural products (NP) cover a high chemical diversity, and in consequence extracts from microorganisms are often complex to analyze and purify. A distribution analysis of calculated pK(a) values from the 34390 records in Antibase2008 revealed that within pH 2-11, 44% of all included compounds had an acidic functionality, 17% a basic functionality, and 9% both. This showed a great potential for using ion-exchange chromatography as an integral part of the separation procedure, orthogonal to the classic reversed-phase strategy. Thus, we investigated the use of an "explorative solid-phase extraction" (E-SPE) protocol using SAX, Oasis MAX, SCX, and LH-20 columns for targeted exploitation of chemical functionalities. E-SPE provides a minimum of fractions (15) for chemical and biological analyses and implicates development into a preparative scale methodology. Overall, this allows fast extract prioritization, easier dereplication, mapping of biological activities, and formulation of a purification strategy.

PEGylation of magnetic multi-walled carbon nanotubes for enhanced selectivity of dispersive solid phase extraction.

PubMed

Zeng, Qiong; Liu, Yi-Ming; Jia, Yan-Wei; Wan, Li-Hong; Liao, Xun

2017-02-01

Carbon nanotubes (CNTs) possess large potential as extraction absorbents in solid phase extraction. They have been widely applied in biomedicine research, while very rare application in natural product chemistry has been reported. In this work, methoxypolyethylene glycol amine (mPEG-NH 2 ) is covalently coupled to CNTs-magnetic nanoparticles (CNTs-MNP) to prepare a novel magnetic nanocomposite (PEG-CNTs-MNP) for use as dispersive solid-phase extraction (DSPE) absorbent. The average particle size was 86nm, and the saturation magnetization was 52.30emu/g. This nanocomposite exhibits excellent dispersibility in aqueous systems, high selectivity and fast binding kinetics when used for extraction of Z-ligustilide, the characteristic bioactive compound from two popular Asian herbal plants, R. chuanxiong and R. ligusticum. HPLC quantification of Z-ligustilide extracted from the standard sample solution showed a high recovery of 98.9%, and the extraction rate from the extracts of the above two herbs are both around 70.0%. To our knowledge, this is the first report on using PEG-CNTs-MNP as DSPE nanosorbents for selective extraction of natural products. This nano-material has promising application in isolation and enrichment of targeted components from complex matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

Two-phase electromembrane extraction followed by gas chromatography-mass spectrometry analysis.

PubMed

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

2013-02-01

A two-phase electromembrane extraction (EME) was developed and directly coupled with gas chromatography mass spectrometry (GC-MS) analysis. The proposed method was successfully applied to the simultaneous determination of imipramine, desipramine, citalopram and sertraline. The model compounds were extracted from neutral aqueous sample solutions into the organic phase filled in the lumen of the hollow fiber. This method was accomplished with 1-heptanol as organic phase, by means of 60 V applied voltage and with the extraction time of 15 min. Experiments reported recoveries in the range of 69-87% from 1.2 mL neutral sample solution. The compounds were quantified by GC-MS instrument, with acceptable linearity ranging from 1 to 500 ng mL(-1) (R(2) in the range of 0.989 to 0.998), and repeatability (RSD) ranging between 7.5 and 11.5% (n = 5). The estimated detection limits (S/N ratio of 3:1) were less than 0.25 ng mL(-1). This novel approach based on two-phase EME brought advantages such as simplicity, low-costing, low detection limit and fast extraction with a total analysis time less than 25 min. These experimental findings were highly interesting and demonstrated the possibility of solving ionic species in the organic phase at the presence of electrical potential. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Method optimization for non-equilibrium solid phase microextraction sampling of HAPs for GC/MS analysis

NASA Astrophysics Data System (ADS)

Zawadowicz, M. A.; Del Negro, L. A.

2010-12-01

Hazardous air pollutants (HAPs) are usually present in the atmosphere at pptv-level, requiring measurements with high sensitivity and minimal contamination. Commonly used evacuated canister methods require an overhead in space, money and time that often is prohibitive to primarily-undergraduate institutions. This study optimized an analytical method based on solid-phase microextraction (SPME) of ambient gaseous matrix, which is a cost-effective technique of selective VOC extraction, accessible to an unskilled undergraduate. Several approaches to SPME extraction and sample analysis were characterized and several extraction parameters optimized. Extraction time, temperature and laminar air flow velocity around the fiber were optimized to give highest signal and efficiency. Direct, dynamic extraction of benzene from a moving air stream produced better precision (±10%) than sampling of stagnant air collected in a polymeric bag (±24%). Using a low-polarity chromatographic column in place of a standard (5%-Phenyl)-methylpolysiloxane phase decreased the benzene detection limit from 2 ppbv to 100 pptv. The developed method is simple and fast, requiring 15-20 minutes per extraction and analysis. It will be field-validated and used as a field laboratory component of various undergraduate Chemistry and Environmental Studies courses.

Fabric phase sorptive extraction: Two practical sample pretreatment techniques for brominated flame retardants in water.

PubMed

Huang, Guiqi; Dong, Sheying; Zhang, Mengfei; Zhang, Haihan; Huang, Tinglin

2016-09-15

Sample pretreatment is the critical section for residue monitoring of hazardous pollutants. In this paper, using the cellulose fabric as host matrix, three extraction sorbents such as poly (tetrahydrofuran) (PTHF), poly (ethylene glycol) (PEG) and poly (dimethyldiphenylsiloxane) (PDMDPS), were prepared on the surface of the cellulose fabric. Two practical extraction techniques including stir bar fabric phase sorptive extraction (stir bar-FPSE) and magnetic stir fabric phase sorptive extraction (magnetic stir-FPSE) have been designed, which allow stirring of fabric phase sorbent during the whole extraction process. In the meantime, three brominated flame retardants (BFRs) [tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bisallylether (TBBPA-BAE), tetrabromobisphenol A bis(2,3-dibromopropyl)ether (TBBPA-BDBPE)] in the water sample were selected as model analytes for the practical evaluation of the proposed two techniques using high-performance liquid chromatography (HPLC). Moreover, various experimental conditions affecting extraction process such as the type of fabric phase, extraction time, the amount of salt and elution conditions were also investigated. Due to the large sorbent loading capacity and unique stirring performance, both techniques possessed high extraction capability and fast extraction equilibrium. Under the optimized conditions, high recoveries (90-99%) and low limits of detection (LODs) (0.01-0.05 μg L(-1)) were achieved. In addition, the reproducibility was obtained by evaluating the intraday and interday precisions with relative standard deviations (RSDs) less than 5.1% and 6.8%, respectively. The results indicated that two pretreatment techniques were promising and practical for monitoring of hazardous pollutants in the water sample. Due to low solvent consumption and high repeated use performance, proposed techniques also could meet green analytical criteria. Copyright © 2016 Elsevier Ltd. All rights reserved.

Phase retrieval without unwrapping by single-shot dual-wavelength digital holography

NASA Astrophysics Data System (ADS)

Min, Junwei; Yao, Baoli; Zhou, Meiling; Guo, Rongli; Lei, Ming; Yang, Yanlong; Dan, Dan; Yan, Shaohui; Peng, Tong

2014-12-01

A phase retrieval method by using single-shot dual-wavelength digital holography is proposed. Each single wavelength hologram is extracted from the color CCD recorded hologram at one exposure, and the unwrapped phase image of object can be reconstructed directly. Different from the traditional multiple wavelength phase unwrapping techniques, any single complex wave-fronts at different wavelengths have no need to be calculated any more. Thus, the phase retrieval is computationally fast and straightforward, and the limitations on the total optical path difference are significantly relaxed. The practicability of the proposed method is demonstrated by both simulated and experimental results.

Fluorous tagging strategy for solution-phase synthesis of small molecules, peptides and oligosaccharides

PubMed Central

Zhang, Wei

2005-01-01

The purification of reaction mixtures is a slow process in organic synthesis, especially during the production of large numbers of analogs and compound libraries. Phase-tag methods such as solid-phase synthesis and fluorous synthesis, provide efficient ways of addressing the separation issue. Fluorous synthesis employs functionalized perfluoroalkyl groups attached to substrates or reagents. The separation of the resulting fluorous molecules can be achieved using strong and selective fluorous liquid-liquid extraction, fluorous silica gel-based solid-phase extraction or high-performance liquid chromatography. Fluorous technology is a novel solution-phase method, which has the advantages of fast reaction times in homogeneous environments, being readily adaptable to literature conditions, having easy intermediate analysis, and having flexibility in reaction scale and scope. In principle, any synthetic methods that use a solid-support could be conducted in solution-phase by replacing the polymer linker with a corresponding fluorous tag. This review summarizes the progress of fluorous tags in solution-phase synthesis of small molecules, peptides and oligosaccharides. PMID:15595439

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.

Note: Fully integrated 3.2 Gbps quantum random number generator with real-time extraction

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

Zhang, Xiao-Guang; Nie, You-Qi; Liang, Hao

2016-07-15

We present a real-time and fully integrated quantum random number generator (QRNG) by measuring laser phase fluctuations. The QRNG scheme based on laser phase fluctuations is featured for its capability of generating ultra-high-speed random numbers. However, the speed bottleneck of a practical QRNG lies on the limited speed of randomness extraction. To close the gap between the fast randomness generation and the slow post-processing, we propose a pipeline extraction algorithm based on Toeplitz matrix hashing and implement it in a high-speed field-programmable gate array. Further, all the QRNG components are integrated into a module, including a compact and actively stabilizedmore » interferometer, high-speed data acquisition, and real-time data post-processing and transmission. The final generation rate of the QRNG module with real-time extraction can reach 3.2 Gbps.« less

Matrix solid-phase dispersion on column clean-up/pre-concentration as a novel approach for fast isolation of abuse drugs from human hair.

PubMed

Míguez-Framil, Martha; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar; Alvarez-Freire, Iván; Tabernero, María Jesús; Bermejo, Ana María

2010-10-08

A simple and fast sample pre-treatment method based on matrix solid-phase dispersion (MSPD) for isolating cocaine, benzoylecgonine (BZE), codeine, morphine and 6-monoacethylmorphine (6-MAM) from human hair has been developed. The MSPD approach consisted of using alumina (1.80 g) as a dispersing agent and 0.6M hydrochloric acid (4 mL) as an extracting solvent. For a fixed hair sample mass of 0.050 g, the alumina mass to sample mass ratio obtained was 36. A previously conditioned Oasis HLB cartridge (2 mL methanol, plus 2 mL ultrapure water, plus 1 mL of 0.2M/0.2M sodium hydroxide/boric acid buffer solution at pH 9.2) was attached to the end of the MSPD syringe for on column clean-up of the hydrochloric acid extract and for transferring the target compounds to a suitable solvent for gas chromatography (GC) analysis. Therefore, the adsorbed analytes were directly eluted from the Oasis HLB cartridges with 2 mL of 2% acetic acid in methanol before concentration by N(2) stream evaporation and dry extract derivatization with N-methyl-tert-butylsilyltrifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS). The optimization/evaluation of all the factors affecting the MSPD and on column clean-up procedures has led to a fast sample treatment, and analytes extraction and pre-concentration can be finished in approximately 30 min. The developed method has been applied to eight hair samples from poli-drug abusers and measured analyte concentrations have been found to be statistically similar (95% confidence interval) to those obtained after a conventional enzymatic hydrolysis method (Pronase E). Copyright © 2010. Published by Elsevier B.V.

Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

2016-11-01

A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

HAI: A novel airborne multi-channel hygrometer for fast multi-phase H2O quantification: Performance of the HAI instrument during the first flights on the German HALO aircraft

NASA Astrophysics Data System (ADS)

Buchholz, B.; Ebert, V.; Kraemer, M.; Afchine, A.

2014-12-01

Common gas phase H2O measurements on fast airborne platforms e.g. using backward facing or "Rosemount"-inlets can lead to a high risk of ice and droplets contamination. In addition, currently no single hygrometer exists that allows a simultaneous, high-speed measurement of all phases (gas, liquid, ice) with the same detection principle. In the rare occasions multi-phase measurements are realized, gas-and condensed-phase observations rely on different methods, instruments and calibration strategies so that precision and accuracy levels are quite difficult to quantify. This is effectively avoided by the novel TDLAS instrument, HAI, Hygrometer for Atmospheric Investigation, which allows a simultaneous, high speed, multi-phase detection without any sensor calibration in a unique "2+2" channel concept. Hai combines two independent wavelength channels, at 1.4 µm and at 2.6 µm, for a wide dynamic range from 1 to 30 000 ppmv, with a simultaneous closed path (extractive) and open path detection. Thus, "Total", i.e. gas-phase plus condensed-phase water is measured by sampling via a forward facing inlet into "closed-path" extractive cells. A selective, sampling-free, high speed gas phase detection is realized via a dual-wavelength "open-path" cell placed outside of the aircraft fuselage. All channels can be sampled with 120 Hz (measurement cycle time Dt=1.6 ms) allowing an unprecedented spatial resolution of 30 cm at 900 km/h. The evaluation of the individual multi-channel raw-data is done post flight, without any channel interdependencies, in calibration-free mode, thus allowing fast, accurate and precise multi-phase water detection in flight. The performance could be shown in more than 200 net flights hours in three scientific flight campaigns (TACTS, ESMVal, ML-CIRRUS) on the new German HALO aircraft. In addition the level of the accuracy of the calibration free evaluation was evaluated at the German national primary water vapor standard.

Segmentation of hand radiographs using fast marching methods

NASA Astrophysics Data System (ADS)

Chen, Hong; Novak, Carol L.

2006-03-01

Rheumatoid Arthritis is one of the most common chronic diseases. Joint space width in hand radiographs is evaluated to assess joint damage in order to monitor progression of disease and response to treatment. Manual measurement of joint space width is time-consuming and highly prone to inter- and intra-observer variation. We propose a method for automatic extraction of finger bone boundaries using fast marching methods for quantitative evaluation of joint space width. The proposed algorithm includes two stages: location of hand joints followed by extraction of bone boundaries. By setting the propagation speed of the wave front as a function of image intensity values, the fast marching algorithm extracts the skeleton of the hands, in which each branch corresponds to a finger. The finger joint locations are then determined by using the image gradients along the skeletal branches. In order to extract bone boundaries at joints, the gradient magnitudes are utilized for setting the propagation speed, and the gradient phases are used for discriminating the boundaries of adjacent bones. The bone boundaries are detected by searching for the fastest paths from one side of each joint to the other side. Finally, joint space width is computed based on the extracted upper and lower bone boundaries. The algorithm was evaluated on a test set of 8 two-hand radiographs, including images from healthy patients and from patients suffering from arthritis, gout and psoriasis. Using our method, 97% of 208 joints were accurately located and 89% of 416 bone boundaries were correctly extracted.

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

PubMed

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

2009-09-07

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

Determination of preservatives in cosmetics, cleaning agents and pharmaceuticals using fast liquid chromatography.

PubMed

Baranowska, Irena; Wojciechowska, Iwona; Solarz, Natalia; Krutysza, Ewa

2014-01-01

This paper reports the development of a method for simultaneously determining five preservatives in cosmetics, cleaning agents and pharmaceuticals by fast liquid chromatography. Methylisothiazolinone, methylchloroisothiazolinone, benzyl alcohol, sodium benzoate and methylparaben were separated on a Chromolith Fast Gradient reversed-phase 18e column using gradient elution with acetonitrile and a 0.1% aqueous solution of formic acid, with a run time of 3 min. The preparation of solid and liquid samples included ultrasonic extraction with methanol with recoveries ranging from 69 to 119%. The developed method was used to analyze samples of cosmetics (66 samples), cleaning agents (five samples) and pharmaceutical industry products (17 samples).

[Determination of canthaxanthin and astaxanthin in egg yolks by reversed phase high performance liquid chromatography with diode array detection].

PubMed

He, Kang-Hao; Zou, Xiao-Li; Liu, Xiang; Zeng, Hong-Yan

2012-01-01

A method using reversed phase high performance liquid chromatography (RP-HPLC) coupled with diode array detector (DAD) was developed for the simultaneous determination of canthaxanthin and astaxanthin in egg yolks. Samples were extracted with acetonitrile in ultrasonic bath for 20 minutes and then purified by freezing-lipid filtration and solid phase extraction (SPE). After being vaporized to dryness by nitrogen blowing and made up to volume with methanol, the extract solution was chromatographically separated in C18 column with a unitary mobile phase consisting of acetonitrile. The proposed method was validated in terms of linearity, precision, accuracy, and limit of detection (LOD). Regression analysis revealed a good linearity between peak area of each analyte and its concentration (r > or = 0.998). The intra- and inter-day relative standard deviations (RSDs) were less than 3.6% and 5.2%, respectively. LODs of canthaxanthin and astaxanthin were 0.035 and 0.027 microg/mL (S/N = 3). The average recoveries of canthaxanthin and astaxanthin were 91.5% and 88.7%. The proposed method is simple, fast and easy to apply.

HPLC-electrospray mass spectrometric assay for the determination of (R,R)-fenoterol in rat plasma.

PubMed

Siluk, Danuta; Kim, Hee Seung; Cole, Tyler; Wainer, Irving W

2008-11-04

A fast and specific liquid chromatography-mass spectrometry method for the determination of (R,R)-fenoterol ((R,R)-Fen) in rat plasma has been developed and validated. (R,R)-Fen was extracted from 125 microl of plasma using solid phase extraction and analyzed on Atlantis HILIC Silica 3 microm column. The mobile phase was composed of acetonitrile:ammonium acetate (pH 4.1; 20mM) (85:15, v/v), at a flow rate of 0.2 ml/min. The lower limit of detection (LLOD) was 2 ng/ml . The procedure was validated and applied to the analysis of plasma samples from rats previously administered (R,R)-Fen in an intravenous bolus.

Polydopamine-coated magnetic molecularly imprinted polymer for the selective solid-phase extraction of cinnamic acid, ferulic acid and caffeic acid from radix scrophulariae sample.

PubMed

Yin, Yuli; Yan, Liang; Zhang, Zhaohui; Wang, Jing; Luo, Ningjing

2016-04-01

We describe novel cinnamic acid polydopamine-coated magnetic imprinted polymers for the simultaneous selective extraction of cinnamic acid, ferulic acid and caffeic acid from radix scrophulariae sample. The novel magnetic imprinted polymers were synthesized by surface imprinting polymerization using magnetic multi-walled carbon nanotubes as the support material, cinnamic acid as the template and dopamine as the functional monomer. The magnetic imprinted polymers were characterized by transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The results revealed that the magnetic imprinted polymers had outstanding magnetic properties, high adsorption capacity, selectivity and fast kinetic binding toward cinnamic acid, ferulic acid and caffeic acid. Coupled with high-performance liquid chromatography, the extraction conditions of the magnetic imprinted polymers as a magnetic solid-phase extraction sorbent were investigated in detail. The proposed imprinted magnetic solid phase extraction procedure has been used for the purification and enrichment of cinnamic acid, ferulic acid and caffeic acid successfully from radix scrophulariae extraction sample with recoveries of 92.4-115.0% for cinnamic acid, 89.4-103.0% for ferulic acid and 86.6-96.0% for caffeic acid. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium.

PubMed

Nakao, Ryuji; Halldin, Christer

2013-07-01

A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for (11)C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma. Copyright © 2013 Elsevier Inc. All rights reserved.

Fast-responding bio-based shape memory thermoplastic polyurethanes

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

Petrovic, Zoran S.; Milic, Jelena; Zhang, Fan

Fast response shape-memory polyurethanes were prepared from bio-based polyols, diphenyl methane diisocyanate and butane diol. The bio-based polyester polyols were synthesized from 9-hydroxynonanoic acid, a product obtained by ozonolysis of fatty acids extracted from soy oil and castor oil. The morphology of polyurethanes was investigated by synchrotron ultra-small angle X-ray scattering, which revealed the inter-domain spacing between the hard and soft phases, the degree of phase separation, and the level of intermixing between the hard and soft phases. We also conducted thorough investigations of the thermal, mechanical, and dielectric properties of the polyurethanes, and found that high crystallization rate ofmore » the soft segment gives these polyurethanes unique properties suitable for shapememory applications, such as adjustable transition temperatures, high degree of elastic elongations, and good mechanical strength. In conclusion, these materials are also potentially biodegradable and biocompatible, therefore suitable for biomedical and environmental applications.« less

Fast-responding bio-based shape memory thermoplastic polyurethanes

DOE PAGES

Petrovic, Zoran S.; Milic, Jelena; Zhang, Fan; ...

2017-05-31

Fast response shape-memory polyurethanes were prepared from bio-based polyols, diphenyl methane diisocyanate and butane diol. The bio-based polyester polyols were synthesized from 9-hydroxynonanoic acid, a product obtained by ozonolysis of fatty acids extracted from soy oil and castor oil. The morphology of polyurethanes was investigated by synchrotron ultra-small angle X-ray scattering, which revealed the inter-domain spacing between the hard and soft phases, the degree of phase separation, and the level of intermixing between the hard and soft phases. We also conducted thorough investigations of the thermal, mechanical, and dielectric properties of the polyurethanes, and found that high crystallization rate ofmore » the soft segment gives these polyurethanes unique properties suitable for shapememory applications, such as adjustable transition temperatures, high degree of elastic elongations, and good mechanical strength. In conclusion, these materials are also potentially biodegradable and biocompatible, therefore suitable for biomedical and environmental applications.« less

Fast-Responding Bio-Based Shape Memory Thermoplastic Polyurethanes.

PubMed

Petrović, Zoran S; Milić, Jelena; Zhang, Fan; Ilavsky, Jan

2017-07-14

Novel fast response shape-memory polyurethanes were prepared from bio-based polyols, diphenyl methane diisocyanate and butane diol for the first time. The bio-based polyester polyols were synthesized from 9-hydroxynonanoic acid, a product obtained by ozonolysis of fatty acids extracted from soy oil and castor oil. The morphology of polyurethanes was investigated by synchrotron ultra-small angle X-ray scattering, which revealed the inter-domain spacing between the hard and soft phases, the degree of phase separation, and the level of intermixing between the hard and soft phases. We also conducted thorough investigations of the thermal, mechanical, and dielectric properties of the polyurethanes, and found that high crystallization rate of the soft segment gives these polyurethanes unique properties suitable for shape-memory applications, such as adjustable transition temperatures, high degree of elastic elongations, and good mechanical strength. These materials are also potentially biodegradable and biocompatible, therefore suitable for biomedical and environmental applications.

Development of a fast scintillator based beam phase measurement system for compact superconducting cyclotrons

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

Bhattacharjee, Tanushyam; Kanti Dey, Malay; Dhara, Partha

2013-05-15

In an isochronous cyclotron, measurements of central phase of the ion beam with respect to rf and the phase width provide a way to tune the cyclotron for maximum energy gain per turn and efficient extraction. We report here the development of a phase measurement system and the measurements carried out at the Variable Energy Cyclotron Centre's (VECC's) K= 500 superconducting cyclotron. The technique comprises detecting prompt {gamma}-rays resulting from the interaction of cyclotron ion beam with an aluminium target mounted on a radial probe in coincidence with cyclotron rf. An assembly comprising a fast scintillator and a liquid light-guidemore » inserted inside the cyclotron was used to detect the {gamma}-rays and to transfer the light signal outside the cyclotron where a matching photo-multiplier tube was used for light to electrical signal conversion. The typical beam intensity for this measurement was a few times 10{sup 11} pps.« less

Fast high performance liquid chromatography and ultraviolet-visible quantification of principal phenolic antioxidants in fresh rosemary.

PubMed

Troncoso, N; Sierra, H; Carvajal, L; Delpiano, P; Günther, G

2005-12-23

An improved HPLC method is reported for the determination of rosemary's principal phenolic antioxidants, rosmarinic and carnosic acids, providing a fast and simultaneous determination for both of them by using a solid phase column. The analysis was performed with fresh methanolic extractions of Rosmarinus officinalis. To quantify the amount of antioxidants in a fast and reproducible way by means of UV-vis absorption measurements, a spectrophotometric multi-wavelength calibration curve was constructed based on the antioxidant contents obtained with the recently developed HPLC method. This UV-vis methodology can be extended to the determination of other compounds and herbs if the restrictions mentioned in the text are respected.

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

PubMed

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

2009-07-01

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

Cost-effective imprinting combining macromolecular crowding and a dummy template for the fast purification of punicalagin from pomegranate husk extract.

PubMed

Sun, Guang-Ying; Wang, Chao; Luo, Yu-Qin; Zhao, Yong-Xin; Yang, Jian; Liu, Zhao-Sheng; Aisa, Haji Akber

2016-05-01

The combination of molecular crowding and virtual imprinting was employed to develop a cost-effective method to prepare molecularly imprinted polymers. By using linear polymer polystyrene as a macromolecular crowding agent, an imprinted polymer recognizable to punicalagin had been successfully synthesized with punicalin as the dummy template. The resulting punicalin-imprinted polymer presented a remarkable selectivity to punicalagin with an imprinting factor of 3.17 even at extremely low consumption of the template (template/monomer ratio of 1:782). In contrast, the imprinted polymer synthesized without crowding agent, did not show any imprinting effect at so low template amount. The imprinted polymers made by combination of molecular crowding and virtual imprinting can be utilized for the fast separation of punicalagin from pomegranate husk extract after optimizing the protocol of solid-phase extraction with the recovery of 85.3 ± 1.2%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

HPLC–electrospray mass spectrometric assay for the determination of (R,R)-fenoterol in rat plasma

PubMed Central

Siluk, Danuta; Kim, Hee Seung; Cole, Tyler; Wainer, Irving W.

2008-01-01

A fast and specific liquid chromatography–mass spectrometry method for the determination of (R,R)-fenoterol ((R,R)-Fen) in rat plasma has been developed and validated. (R,R)-Fen was extracted from 125 µl of plasma using solid phase extraction and analyzed on Atlantis HILIC Silica 3 µm column. The mobile phase was composed of acetonitrile:ammonium acetate (pH 4.1; 20 mM) (85:15, v/v), at a flow rate of 0.2 ml/min. The lower limit of detection (LLOD) was 2 ng/ml . The procedure was validated and applied to the analysis of plasma samples from rats previously administered (R,R)-Fen in an intravenous bolus. PMID:18617349

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

PubMed

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

2009-07-15

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

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

PubMed

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

2017-05-01

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

Preliminary studies of bio-oil from fast pyrolysis of coconut fibers.

PubMed

Almeida, Tarciana M; Bispo, Mozart D; Cardoso, Anne R T; Migliorini, Marcelo V; Schena, Tiago; de Campos, Maria Cecilia V; Machado, Maria Elisabete; López, Jorge A; Krause, Laiza C; Caramão, Elina B

2013-07-17

This work studied fast pyrolysis as a way to use the residual fiber obtained from the shells of coconut ( Cocos nucifera L. var. Dwarf, from Aracaju, northeastern Brazil). The bio-oil produced by fast pyrolysis and the aqueous phase (formed during the pyrolysis) were characterized by GC/qMS and GC×GC/TOF-MS. Many oxygenated compounds such as phenols, aldehydes, and ketones were identified in the extracts obtained in both phases, with a high predominance of phenolic compounds, mainly alkylphenols. Eighty-one compounds were identified in the bio-oil and 42 in the aqueous phase using GC/qMS, and 95 and 68 in the same samples were identified by GC×GC/TOF-MS. The better performance of GC×GC/TOF-MS was due to the possibility of resolving some coeluted peaks in the one-dimension gas chromatography. Semiquantitative analysis of the samples verified that 59% of the area on the chromatogram of bio-oil is composed by phenols and 12% by aldehydes, mainly furfural. Using the same criterion, 77% of the organic compounds in the aqueous phase are phenols. Therefore, this preliminary assessment indicates that coconut fibers have the potential to be a cost-effective and promising alternative to obtain new products and minimize environmental impact.

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

PubMed

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

2015-12-01

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

A fast and sensitive method for the simultaneous analysis of a wide range of per- and polyfluoroalkyl substances in indoor dust using on-line solid phase extraction-ultrahigh performance liquid chromatography-time-of-flight-mass spectrometry.

PubMed

Padilla-Sánchez, Juan Antonio; Haug, Line Småstuen

2016-05-06

A fast and sensitive method for simultaneous determination of 18 traditional and 6 alternative per- and polyfluoroalkyl substances (PFASs) using solid-liquid extraction (SLE), off-line clean-up using activated carbon and on-line solid phase extraction-ultrahigh performance liquid chromatography-time-of-flight-mass spectrometry (on-line SPE-UHPLC-TOF-MS) was developed. The extraction efficiency was studied and recoveries in range the 58-114% were obtained. Extraction and injection volumes were also optimized to 2mL and 400μL, respectively. The method was validated by spiking dust from a vacuum cleaner bag that had been found to contain low levels of the PFASs in focus. Low method detection limits (MDLs) and method quantification limits (MQLs) in the range 0.008-0.846ngg(-1) and 0.027-2.820ngg(-1) were obtained, respectively. For most of the PFASs, the accuracies were between 70 and 125% in the range from 2 to100ngg(-1) dust. Intra-day and inter-day precisions were in general well below 30%. Analysis of a Standard Reference Material (SRM 2585) showed high accordance with results obtained by other laboratories. Finally, the method was applied to seven indoor dust samples, and PFAS concentrations in the range 0.02-132ngg(-1) were found. The highest median concentrations were observed for some of the alternative PFASs, such as 6:2-diPAP (25ngg(-1)), 8:2-diPAP (49ngg(-1)), and PFOPA (23ngg(-1)), illustrating the importance of inclusion of new PFASs in the analytical methods. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

PubMed

Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2015-12-18

A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

Anisotropy of the Earth's inner inner core from autocorrelations of earthquake coda in China Regional Seismic Networks

NASA Astrophysics Data System (ADS)

Xia, H.; Song, X.; Wang, T.

2014-12-01

The Earth's inner core possesses strong cylindrical anisotropy with the fast symmetry axis parallel to the rotation axis. However, recent study has suggested that the inner part of the inner core has a fast symmetry axis near the equator with a different form of anisotropy from the outer part (Wang et al., this session). To confirm the observation, we use data from dense seismic arrays of the China Regional Seismic Networks. We perform autocorrelation (ACC) of the coda after major earthquakes (Mw>=7.0) at each station and then stack the ACCs at each cluster of stations. The PKIKP2 and PKIIKP2 phases (round-trip phase from the Earth's surface reflections) can be clearly extracted from the stacked empirical Green's functions. We observe systematic variation of the differential times between PKIKP2 and PKIIKP2 phases, which are sensitive to the bulk anisotropy of the inner core. The differential times show large variations with both latitudes and longitudes, even though our ray paths are not polar (with our stations at mid-range latitudes of about 20 to 45 degrees). The observations cannot be explained by an averaged anisotropy model with the fast axis along the rotation axis. The pattern appears consistent with an inner inner core that has a fast axis near the equator.

Fast UPLC/PDA determination of squalene in Sicilian P.D.O. pistachio from Bronte: Optimization of oil extraction method and analytical characterization.

PubMed

Salvo, Andrea; La Torre, Giovanna Loredana; Di Stefano, Vita; Capocchiano, Valentina; Mangano, Valentina; Saija, Emanuele; Pellizzeri, Vito; Casale, Katia Erminia; Dugo, Giacomo

2017-04-15

A fast reversed-phase UPLC method was developed for squalene determination in Sicilian pistachio samples that entry in the European register of the products with P.D.O. In the present study the SPE procedure was optimized for the squalene extraction prior to the UPLC/PDA analysis. The precision of the full analytical procedure was satisfactory and the mean recoveries were 92.8±0.3% and 96.6±0.1% for 25 and 50mgL -1 level of addition, respectively. Selected chromatographic conditions allowed a very fast squalene determination; in fact it was well separated in ∼0.54min with good resolution. Squalene was detected in all the pistachio samples analyzed and the levels ranged from 55.45-226.34mgkg -1 . Comparing our results with those of other studies it emerges that squalene contents in P.D.O. Sicilian pistachio samples, generally, were higher than those measured for other samples of different geographic origins. Copyright © 2016 Elsevier Ltd. All rights reserved.

On-cartridge derivatisation using a calixarene solid-phase extraction sorbent for facile, sensitive and fast determination of formaldehyde in beer.

PubMed

Deng, Zhifen; Hu, Kai; Zhang, Yongming; Zhao, Wenjie; Wang, Fei; Guo, Ling; Zhang, Wenfen; He, Juan; Huang, Yanjie; Zhang, Shusheng

2016-11-15

This work demonstrates the successful application of an on-cartridge derivatisation procedure for facile, fast and sensitive determination of formaldehyde in beer by HPLC-UV. The derivatisation and solid-phase extraction (SPE) were integrated into a novel calixarene SPE sorbent: tetraazacalix[2]arene[2]triazine bonded silica gel. Specifically, 2,4-dinitrophenylhydrazine was adsorbed onto the sorbent in advance, based on the charge-transfer interaction between the macrocyclic molecule and nitrobenzenes. The method was optimised and validated: under the optimal conditions of derivatisation, SPE and HPLC separation, good linearity was obtained in the range of 0.080-3.2μgmL(-1) with a correlation coefficient of 0.9939, the limit of detection was 3.0ngmL(-1) (S/N=3), the limit of quantification was 10ngmL(-1) (S/N=10), and the recovery level using this method was desirable at 75-84%. The developed method was successfully applied to determine formaldehyde content in real beer samples; the results were in the range of 0.11-1.1μgmL(-1). Copyright © 2016. Published by Elsevier Ltd.

On-line MSPD-SPE-HPLC/FLD analysis of polycyclic aromatic hydrocarbons in bovine tissues.

PubMed

Gutiérrez-Valencia, Tania M; García de Llasera, Martha P

2017-05-15

A fast method was optimized and validated for simultaneous trace determination of four polycyclic aromatic hydrocarbons: benzo[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene and benzo[a]pyrene in bovine tissues. The determination was performed by matrix solid-phase dispersion (MSPD) coupled on-line to solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection (FLD). The sample was dispersed on C 18 silica sorbent and then the on-line MSPD-SPE-HPLC/FLD method was applied. Several parameters were optimized: cleaning and elution sequences applied to the MSPD cartridge, the flow rate and dilution of extract used for SPE loading. The on-line method was validated over a concentration range of 0.1-0.6ngg -1 obtaining good linearity (r⩾0.998) and precision (RSD)⩽10%. Recovery ranged from 96 to 99% and the limits of detection were 0.012ngg -1 . This methodology was applied to liver samples from unhealthy animals. The results demonstrate that MSDP-SPE-HPLC/FLD method provides reliable, sensitive, accurate and fast data to the food control. Copyright © 2016 Elsevier Ltd. All rights reserved.

Fast radio burst search: cross spectrum vs. auto spectrum method

NASA Astrophysics Data System (ADS)

Liu, Lei; Zheng, Weimin; Yan, Zhen; Zhang, Juan

2018-06-01

The search for fast radio bursts (FRBs) is a hot topic in current radio astronomy studies. In this work, we carry out a single pulse search with a very long baseline interferometry (VLBI) pulsar observation data set using both auto spectrum and cross spectrum search methods. The cross spectrum method, first proposed in Liu et al., maximizes the signal power by fully utilizing the fringe phase information of the baseline cross spectrum. The auto spectrum search method is based on the popular pulsar software package PRESTO, which extracts single pulses from the auto spectrum of each station. According to our comparison, the cross spectrum method is able to enhance the signal power and therefore extract single pulses from data contaminated by high levels of radio frequency interference (RFI), which makes it possible to carry out a search for FRBs in regular VLBI observations when RFI is present.

Novel amide polar-embedded reversed-phase column for the fast liquid chromatography-tandem mass spectrometry method to determine polyether ionophores in environmental waters.

PubMed

Herrero, P; Borrull, F; Pocurull, E; Marcé, R M

2012-11-09

A fast chromatographic method has been developed that takes less than 5 min per run to determine five polyether ionophores with a novel amide polar-embedded reversed-phase column coupled to a triple quadrupole mass spectrometer. A comparison between Oasis HLB and Oasis MAX sorbents for the solid-phase extraction was done. Oasis HLB sorbent gave recoveries close to 90% and the repeatability (%RSD, 25-100 ng/L, n=3) of the method was less than 7% for all compounds in all matrices. The presence of polyether ionophores in environmental waters such as river water and sewage was investigated. Monensin and narasin were frequently determined in influent and effluent sewage at concentrations from 10 ng/L to 47 ng/L in influents and from 6 ng/L to 34 ng/L in effluents. In river waters, polyether ionophores were not detected in any sample. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2007-12-01

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

Onion cell imaging by using Talbot/self-imaging effect

NASA Astrophysics Data System (ADS)

Agarwal, Shilpi; Kumar, Varun; Shakher, Chandra

2017-08-01

This paper presents the amplitude and phase imaging of onion epidermis cell using the self-imaging capabilities of a grating (Talbot effect) in visible light region. In proposed method, the Fresnel diffraction pattern from the first grating and object is recorded at self-image plane. Fast Fourier Transform (FFT) is used for extracting the 3D amplitude and phase image of onion epidermis cell. The stability of the proposed system, from environmental perturbation as well as its compactness and portability give the proposed system a high potential for several clinical applications.

Direct immersion-solid phase microextraction for the determination of chlorinated pesticide residues in tomatoes by gas chromatography with an electron capture detector.

PubMed

Mariani, Maurizio Boccacci; Giannetti, Vanessa; Testani, Elena; Ceccarelli, Valentina

2013-01-01

The use of pesticides in agriculture has grown dramatically over the last decades. Environmental exposure of humans to agrochemicals is common and results in both acute and chronic health effects. In this study, direct immersion-solid phase microextraction (SPME) was coupled with electron capture detection for trace determination of 19 chlorinated pesticides in tomato samples, using a 100 pm polydimethylsiloxane fiber. The experimental parameters extraction time, extraction temperature, stirring, and salting out were evaluated and optimized. The LODs ranged from 0.5 to 8 microg/kg, and the LOQs from 5 to 30 microg/kg. A linear response was confirmed by correlation coefficients ranging from 0.97 to 0.9985. The developed method was tested by analyzing real samples purchased within the network of Italian distribution. The samples were found to be free from detectable residues of the studied pesticides. SPME has been shown to be a fast extraction technique that has several advantages such as solvent-free extraction, simplicity, and compatibility with the chromatographic analytical system.

Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

PubMed

Magiera, Sylwia; Kwietniowska, Ewelina

2016-11-15

In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

PubMed

Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

2016-01-15

A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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

2007-01-19

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

Determination of 15 polycyclic aromatic hydrocarbons in aquatic products by solid-phase extraction and GC-MS.

PubMed

Liu, Qiying; Guo, Yuanming; Sun, Xiumei; Hao, Qing; Cheng, Xin; Zhang, Lu

2018-02-22

We propose a method for the simultaneous determination of 15 kinds of polycyclic aromatic hydrocarbons in marine samples (muscle) employing gas chromatography with mass spectrometry after saponification with ultrasound-assisted extraction and solid-phase extraction. The experimental conditions were optimized by the response surface method. In addition, the effects of different lyes and extractants on polycyclic aromatic hydrocarbons extraction were discussed, and saturated sodium carbonate was first used as the primary saponification reaction and extracted with 10 mL of ethyl acetate and secondly 1 mol/L of sodium hydroxide and 10 mL of n-hexane were used to achieve better results. The average recovery was 67-112%. Satisfactory data showed that the method has good reproducibility with a relative standard deviation of <13%. The detection limits of polycyclic aromatic hydrocarbons were 0.02-0.13 ng/g. Compared with other methods, this method has the advantages of simple pretreatment, low solvent consumption, maximum polycyclic aromatic hydrocarbons extraction, the fast separation speed, and the high extraction efficiency. It is concluded that this method meets the batch processing requirements of the sample and can also be used to determine polycyclic aromatic hydrocarbons in other high-fat (fish, shrimp, crab, shellfish) biological samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of Cinnamomum zeylanicum (Ceylon cinnamon) on blood glucose and lipids in a diabetic and healthy rat model

PubMed Central

Ranasinghe, Priyanga; Perera, Sanja; Gunatilake, Mangala; Abeywardene, Eranga; Gunapala, Nuwan; Premakumara, Sirimal; Perera, Kamal; Lokuhetty, Dilani; Katulanda, Prasad

2012-01-01

Objectives: To evaluate short- and long-term effects of Cinnamomum zeylanicum on food consumption, body weight, glycemic control, and lipids in healthy and diabetes-induced rats. Materials and Methods: The study was conducted in two phases (Phase I and Phase II), using Sprague-Dawley rats in four groups. Phase I evaluated acute effects on fasting blood glucose (FBG) (Groups 1 and 2) and on post-oral glucose (Groups 3 and 4) blood glucose. Groups 1 and 3 received distilled-water and Groups 2 and 4 received cinnamon-extracts. Phase II evaluated effects on food consumption, body weight, blood glucose, and lipids over 1 month. Group A (n = 8, distilled-water) and Group B (n = 8, cinnamon-extracts) were healthy rats, while Group C (n = 5, distilled-water) and Group D (n = 5, cinnamon-extracts) were diabetes-induced rats. Serum lipid profile and HbA1c were measured on D-0 and D-30. FBG, 2-h post-prandial blood glucose, body weight, and food consumption were measured on every fifth day. Results: Phase I: There was no significant difference in serial blood glucose values in cinnamon-treated group from time 0 (P > 0.05). Following oral glucose, the cinnamon group demonstrated a faster decline in blood glucose compared to controls (P < 0.05). Phase II: Between D0 and D30, the difference in food consumption was shown only in diabetes-induced rats (P < 0.001). Similarly, the significant difference following cinnamon-extracts in FBG and 2-h post-prandial blood glucose from D0 to D30 was shown only in diabetes-induced rats. In cinnamon-extracts administered groups, total and LDL cholesterol levels were lower on D30 in both healthy and diabetes-induced animals (P < 0.001). Conclusions: C. zeylanicum lowered blood glucose, reduced food intake, and improved lipid parameters in diabetes-induced rats. PMID:22518078

Evaluation of a molecularly imprinted polymer for determination of steroids in goat milk by matrix solid phase dispersion.

PubMed

Gañán, Judith; Morante-Zarcero, Sonia; Gallego-Picó, Alejandrina; Garcinuño, Rosa María; Fernández-Hernando, Pilar; Sierra, Isabel

2014-08-01

A molecularly imprinted polymer-matrix solid-phase dispersion methodology for simultaneous determination of five steroids in goat milk samples was proposed. Factors affecting the extraction recovery such as sample/dispersant ratio and washing and elution solvents were investigated. The molecularly imprinted polymer used as dispersant in the matrix solid-phase dispersion procedure showed high affinity to steroids, and the obtained extracts were sufficiently cleaned to be directly analyzed. Analytical separation was performed by micellar electrokinetic chromatography using a capillary electrophoresis system equipped with a diode array detector. A background electrolyte composed of borate buffer (25mM, pH 9.3), sodium dodecyl sulfate (10mM) and acetonitrile (20%) was used. The developed MIP-MSPD methodology was applied for direct determination of testosterone (T), estrone (E1), 17β-estradiol (17β-E2), 17α-ethinylestradiol (EE2) and progesterone (P) in different goat milk samples. Mean recoveries obtained ranged from 81% to 110%, with relative standard deviations (RSD)≤12%. The molecularly imprinted polymer-matrix solid-phase dispersion method is fast, selective, cost-effective and environment-friendly compared with other pretreatment methods used for extraction of steroids in milk. Copyright © 2014 Elsevier B.V. All rights reserved.

A fully automated and fast method using direct sample injection combined with fused-core column on-line SPE-HPLC for determination of ochratoxin A and citrinin in lager beers.

PubMed

Lhotská, Ivona; Šatínský, Dalibor; Havlíková, Lucie; Solich, Petr

2016-05-01

A new fast and sensitive method based on on-line solid-phase extraction on a fused-core precolumn coupled to liquid chromatography with fluorescence detection has been developed for ochratoxin A (OTA) and citrinin (CIT) determination in lager beer samples. Direct injection of 100 μL filtered beer samples into an on-line SPE-HPLC system enabled fast and effective sample extraction including separation in less than 6 min. Preconcentration of OTA and CIT from beer samples was performed on an Ascentis Express RP C18 guard column (5 × 4.6 mm), particle size 2.7 μm, with a mobile phase of methanol/0.5% aqueous acetic acid pH 2.8 (30:70, v/v) at a flow rate of 2.0 mL min(-1). The flow switch from extraction column to analytical column in back-flush mode was set at 2.0 min and the separation was performed on the fused-core column Ascentis Express Phenyl-Hexyl (100 × 4.6 mm), particle size 2.7 μm, with a mobile phase acetonitrile/0.5% aqueous acetic acid pH 2.8 in a gradient elution at a flow rate of 1.0 mL min(-1) and temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 335/497 nm. The accuracy of the method, defined as the mean recoveries of OTA and CIT from light and dark beer samples, was in the range 98.3-102.1%. The method showed high sensitivity owing to on-line preconcentration; LOQ values were found to be 10 and 20 ng L(-1) for OTA and CIT, respectively. The found values of OTA and CIT in all tested light, dark and wheat beer samples were significantly below the maximum tolerable limits (3.0 μg kg(-1) for OTA and 2000 μg kg(-1) for CIT) set by the European Union.

Fast analysis of glycosides based on HKUST-1-coated monolith solid-phase microextraction and direct analysis in real-time mass spectrometry.

PubMed

Li, Xianjiang; Wang, Xin; Ma, Wen; Ai, Wanpeng; Bai, Yu; Ding, Li; Liu, Huwei

2017-04-01

Glycosides are a kind of highly important natural aromatic precursors in tobacco leaves. In this study, a novel HKUST-1-coated monolith dip-it sampler was designed for the fast and sensitive analysis of trace glycosides using direct analysis in real-time mass spectrometry. This device was prepared in two steps: in situ polymerization of monolith in a glass capillary of dip-it and layer-by-layer growth of HKUST-1 on the surface of monolith. Sufficient extraction was realized by immersing the tip to solution and in situ desorption was carried out by plasma direct analysis in real time. Compared with traditional solid-phase microextraction protocols, sample desorption was not needed anymore, and only extraction conditions were needed to be optimized in this method, including the gas temperature of direct analysis in real time, extraction time, and CH 3 COONH 4 additive concentration. This method enabled the simultaneous detection of six kinds of glycosides with the limits of detection of 0.02-0.05 μg/mL and the linear ranges covering two orders of magnitude with the limits of quantitation of 0.05-0.1 μg/mL. Moreover, the developed method was applied for the glycosides analysis of three tobacco samples, which only took about 2 s for every sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Advantages of using tetrahydrofuran-water as mobile phases in the quantitation of cyclosporin A in monkey and rat plasma by liquid chromatography-tandem mass spectrometry.

PubMed

Li, Austin C; Li, Yinghe; Guirguis, Micheal S; Caldwell, Robert G; Shou, Wilson Z

2007-01-04

A new analytical method is described here for the quantitation of anti-inflammatory drug cyclosporin A (CyA) in monkey and rat plasma. The method used tetrahydrofuran (THF)-water mobile phases to elute the analyte and internal standard, cyclosporin C (CyC). The gradient mobile phase program successfully eluted CyA into a sharp peak and therefore improved resolution between the analyte and possible interfering materials compared with previously reported analytical approaches, where CyA was eluted as a broad peak due to the rapid conversion between different conformers. The sharp peak resulted from this method facilitated the quantitative calculation as multiple smoothing and large number of bunching factors were not necessary. The chromatography in the new method was performed at 30 degrees C instead of 65-70 degrees C as reported previously. Other advantages of the method included simple and fast sample extraction-protein precipitation, direct injection of the extraction supernatant to column for analysis, and elimination of evaporation and reconstitution steps, which were needed in solid phase extraction or liquid-liquid extraction reported before. This method is amenable to high-throughput analysis with a total chromatographic run time of 3 min. This approach has been verified as sensitive, linear (0.977-4000 ng/mL), accurate and precise for the quantitation of CyA in monkey and rat plasma. However, compared with the usage of conventional mobile phases, the only drawback of this approach was the reduced detection response from the mass spectrometer that was possibly caused by poor desolvation in the ionization source. This is the first report to demonstrate the advantages of using THF-water mobile phases to elute CyA in liquid chromatography.

Fast determination of seven synthetic pigments from wine and soft drinks using magnetic dispersive solid-phase extraction followed by liquid chromatography-tandem mass spectrometry.

PubMed

Chen, Xiao-Hong; Zhao, Yong-Gang; Shen, Hao-Yu; Zhou, Li-Xin; Pan, Sheng-Dong; Jin, Mi-Cong

2014-06-13

A novel, simple and sensitive method based on the use of magnetic dispersive solid-phase extraction (M-dSPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) was developed to determine seven synthetic pigments (tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wines and soft drinks. An amino-functionalized low degrees of cross-linking magnetic polymer (NH2-LDC-MP) was synthesized via suspension polymerization, and characterized by transmission electron microscopy (TEM). The NH2-LDC-MP was used as the M-dSPE sorbent to remove the matrix from the solution, and the main factors affecting the extraction were investigated in detail. The obtained results demonstrated the higher extraction capacity of NH2-LDC-MP with recoveries between 84.0 and 116.2%. The limits of quantification (LOQs) for the seven synthetic pigments were between 1.51 and 5.0μg/L in wines and soft drinks. The developed M-dSPE UFLC-MS/MS method had been successfully applied to the real wines and soft drinks for food-safety risk monitoring in Zhejiang Province, China. The results showed that sunset yellow was in three out of thirty soft drink samples (2.95-42.6μg/L), and erythrosine in one out of fifteen dry red wine samples (3.22μg/L), respectively. It was confirmed that the NH2-LDC-MP was a kind of highly effective M-dSPE materials for the pigments analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

Foreground extraction for moving RGBD cameras

NASA Astrophysics Data System (ADS)

Junejo, Imran N.; Ahmed, Naveed

2017-02-01

In this paper, we propose a simple method to perform foreground extraction for a moving RGBD camera. These cameras have now been available for quite some time. Their popularity is primarily due to their low cost and ease of availability. Although the field of foreground extraction or background subtraction has been explored by the computer vision researchers since a long time, the depth-based subtraction is relatively new and has not been extensively addressed as of yet. Most of the current methods make heavy use of geometric reconstruction, making the solutions quite restrictive. In this paper, we make a novel use RGB and RGBD data: from the RGB frame, we extract corner features (FAST) and then represent these features with the histogram of oriented gradients (HoG) descriptor. We train a non-linear SVM on these descriptors. During the test phase, we make used of the fact that the foreground object has distinct depth ordering with respect to the rest of the scene. That is, we use the positively classified FAST features on the test frame to initiate a region growing to obtain the accurate segmentation of the foreground object from just the RGBD data. We demonstrate the proposed method of a synthetic datasets, and demonstrate encouraging quantitative and qualitative results.

Fast PSP measurements of wall-pressure fluctuation in low-speed flows: improvements using proper orthogonal decomposition

NASA Astrophysics Data System (ADS)

Peng, Di; Wang, Shaofei; Liu, Yingzheng

2016-04-01

Fast pressure-sensitive paint (PSP) is very useful in flow diagnostics due to its fast response and high spatial resolution, but its applications in low-speed flows are usually challenging due to limitations of paint's pressure sensitivity and the capability of high-speed imagers. The poor signal-to-noise ratio in low-speed cases makes it very difficult to extract useful information from the PSP data. In this study, unsteady PSP measurements were made on a flat plate behind a cylinder in a low-speed wind tunnel (flow speed from 10 to 17 m/s). Pressure fluctuations (Δ P) on the plate caused by vortex-plate interaction were recorded continuously by fast PSP (using a high-speed camera) and a microphone array. Power spectrum of pressure fluctuations and phase-averaged Δ P obtained from PSP and microphone were compared, showing good agreement in general. Proper orthogonal decomposition (POD) was used to reduce noise in PSP data and extract the dominant pressure features. The PSP results reconstructed from selected POD modes were then compared to the pressure data obtained simultaneously with microphone sensors. Based on the comparison of both instantaneous Δ P and root-mean-square of Δ P, it was confirmed that POD analysis could effectively remove noise while preserving the instantaneous pressure information with good fidelity, especially for flows with strong periodicity. This technique extends the application range of fast PSP and can be a powerful tool for fundamental fluid mechanics research at low speed.

Application of dispersive solid-phase extraction and ultra-fast liquid chromatography-tandem quadrupole mass spectrometry in food additive residue analysis of red wine.

PubMed

Chen, Xiao-Hong; Zhao, Yong-Gang; Shen, Hao-Yu; Jin, Mi-Cong

2012-11-09

A novel and effective dispersive solid-phase extraction (dSPE) procedure with rapid magnetic separation using ethylenediamine-functionalized magnetic polymer as an adsorbent was developed. The new procedure had excellent clean-up ability for the selective removal of the matrix in red wine. An accurate, simple, and rapid analytical method using ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) for the simultaneous determination of nine food additives (i.e., acesulfame, saccharin, sodium cyclamate, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid, and neotame) in red wine was also used and validated. Recoveries ranging from 78.5% to 99.2% with relative standard deviations ranging from 0.46% to 6.3% were obtained using the new method. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.9993. The limits of quantification for the nine food additives were between 0.10 μg/L and 50.0 μg/L. The proposed dSPE-UFLC-MS/MS method was successfully applied in the food-safety risk monitoring of real red wine in Zhejiang Province, China. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

A simple assay for the simultaneous determination of human plasma albendazole and albendazole sulfoxide levels by high performance liquid chromatography in tandem mass spectrometry with solid-phase extraction.

PubMed

Wojnicz, Aneta; Cabaleiro-Ocampo, Teresa; Román-Martínez, Manuel; Ochoa-Mazarro, Dolores; Abad-Santos, Francisco; Ruiz-Nuño, Ana

2013-11-15

A simple, reproducible and fast (4 min chromatogram) method of liquid chromatography in tandem with mass spectrometry (LC/MS-MS) was developed to determine simultaneously the plasma levels of albendazole (ABZ) and its metabolite albendazole sulfoxide (ABZOX) for pharmacokinetic and clinical analysis. Each plasma sample was extracted by solid phase extraction (SPE) using phenacetin as internal standard (IS). The extracted sample was eluted with a Zorbax XDB-CN column using an isocratic method. The mobile phase consisting of water with 1% acetic acid (40%, A) and MeOH (60%, B), was used at a flow rate of 1 mL/min. ABZ and ABZOX were detected and identified by mass spectrometry with electrospray ionization (ESI) in the positive ion and multiple-reaction monitoring (MRM) mode. The method was linear in the range of 5-1000 ng/mL for ABZ and 10-1500 ng/mL (full validation) or 10-5000 ng/mL (partial validation) for ABZOX, with 5 and 10 ng/mL lower limit of quantification (LLOQ) for ABZ and ABZOX, respectively. The tests of accuracy and precision, matrix effect, extraction recovery and stability of the samples for both ABZ and ABZOX did not deviate more than 20% for the LLOQ and no more than 15% for other quality controls (QCs), according to regulatory agencies. © 2013.

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

PubMed

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

2018-04-14

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

Magnetic micro-solid-phase extraction based on magnetite-MCM-41 with gas chromatography-mass spectrometry for the determination of antidepressant drugs in biological fluids.

PubMed

Kamaruzaman, Sazlinda; Sanagi, Mohd Marsin; Yahaya, Noorfatimah; Wan Ibrahim, Wan Aini; Endud, Salasiah; Wan Ibrahim, Wan Nazihah

2017-11-01

A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 μg/L (r 2  = 0.996-0.999). Good limits of detection (0.008-0.010 μg/L) were obtained for the analytes with good relative standard deviations of <8.0% (n = 5) for the determination of 0.1, 5.0, and 500.0 μg/L of antidepressant drugs. This method was successfully applied to the determination of amitriptyline and chlorpromazine in plasma and urine samples. The recoveries of spiked plasma and urine samples were in the range of 86.1-115.4%. Results indicate that magnetite micro-solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Magnetic metal-organic frameworks for fast and efficient solid-phase extraction of six Sudan dyes in tomato sauce.

PubMed

Shi, Xin-Ran; Chen, Xue-Lei; Hao, Yu-Lan; Li, Li; Xu, Hou-Jun; Wang, Man-Man

2018-06-01

Magnetic solid-phase extraction is an effective and useful technique to preconcentrate trace analytes from food samples. In this study, a magnetic trimeric chromium octahedral metal-organic framework (Fe 3 O 4 -NH 2 @MIL-101) was fabricated and characterized. Fe 3 O 4 -NH 2 @MIL-101 was applied as an adsorbent of magnetic solid-phase extraction combined with high performance liquid chromatography to effectively isolate and simultaneously determine six Sudan dyes (Para Red, Sudan I-IV, and Sudan Red 7B) from tomato sauce. Potential factors affecting the MSPE were investigated in detail, and adsorption efficiency of Fe 3 O 4 -NH 2 @MIL-101 was compared with those of conventional adsorbents, such as neutral alumina, HLB, and C 18 . The developed method facilitated the extraction with using only 3 mg of adsorbent in 2 min. In addition, enhancement factors of 50, linear range of 0.01-25 μg/mL, and detection limit (S/N = 3) of 0.5-2.5 μg/kg were obtained. The intra-day and inter-day recoveries for spiked Sudan dyes were in the range of 72.6%-92.9% and 69.6%-91.6%, respectively, with relative standard deviations of ≤9.2%. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of Aroclor 1260 in soil samples by gas chromatography with mass spectrometry and solid-phase microextraction.

PubMed

Zhang, Mengliang; Jackson, Glen P; Kruse, Natalie A; Bowman, Jennifer R; Harrington, Peter de B

2014-10-01

A novel fast screening method was developed for the determination of polychlorinated biphenyls that are constituents of the commercial mixture, Aroclor 1260, in soil matrices by gas chromatography with mass spectrometry combined with solid-phase microextraction. Nonequilibrium headspace solid-phase microextraction with a 100 μm polydimethylsiloxane fiber was used to extract polychlorinated biphenyls from 0.5 g of soil matrix. The use of 2 mL of saturated potassium dichromate in 6 M sulfuric acid solution improved the reproducibility of the extractions and the mass transfer of the polychlorinated biphenyls from the soil matrix to the microextraction fiber via the headspace. The extraction time was 30 min at 100°C. The percent recoveries, which were evaluated using an Aroclor 1260 standard and liquid injection, were within the range of 54.9-65.7%. Two-way extracted ion chromatogram data were used to construct calibration curves. The relative error was <±15% and the relative standard deviation was <15%, which are respective measures of the accuracy and precision. The method was validated with certified soil samples and the predicted concentrations for Aroclor 1260 agreed with the certified values. The method was demonstrated to be linear from 10 to 1000 ng/g for Aroclor 1260 in dry soil. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of trace rare-earth elements in simulated water samples using ICP-OES with TODGA extraction/back-extraction.

PubMed

Li, FuKai; Gong, AiJun; Qiu, LiNa; Zhang, WeiWei; Li, JingRui; Liu, Yu; Liu, YuNing; Yuan, HuiTing

2017-01-01

The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N', N'-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4-1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples.

Simultaneous determination of trace rare-earth elements in simulated water samples using ICP-OES with TODGA extraction/back-extraction

PubMed Central

Li, FuKai; Qiu, LiNa; Zhang, WeiWei; Li, JingRui; Liu, Yu; Liu, YuNing; Yuan, HuiTing

2017-01-01

The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N′, N′-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4–1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples. PMID:28945788

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

PubMed

Ye, Diru; Wu, Susu; Xu, Jianqiao; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

2016-02-01

Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

High-Resolution Tracking Asymmetric Lithium Insertion and Extraction and Local Structure Ordering in SnS2.

PubMed

Gao, Peng; Wang, Liping; Zhang, Yu-Yang; Huang, Yuan; Liao, Lei; Sutter, Peter; Liu, Kaihui; Yu, Dapeng; Wang, En-Ge

2016-09-14

In the rechargeable lithium ion batteries, the rate capability and energy efficiency are largely governed by the lithium ion transport dynamics and phase transition pathways in electrodes. Real-time and atomic-scale tracking of fully reversible lithium insertion and extraction processes in electrodes, which would ultimately lead to mechanistic understanding of how the electrodes function and why they fail, is highly desirable but very challenging. Here, we track lithium insertion and extraction in the van der Waals interactions dominated SnS2 by in situ high-resolution TEM method. We find that the lithium insertion occurs via a fast two-phase reaction to form expanded and defective LiSnS2, while the lithium extraction initially involves heterogeneous nucleation of intermediate superstructure Li0.5SnS2 domains with a 1-4 nm size. Density functional theory calculations indicate that the Li0.5SnS2 is kinetically favored and structurally stable. The asymmetric reaction pathways may supply enlightening insights into the mechanistic understanding of the underlying electrochemistry in the layered electrode materials and also suggest possible alternatives to the accepted explanation of the origins of voltage hysteresis in the intercalation electrode materials.

Precipitation behavior in austenitic and ferritic steels during fast neutron irradiation and thermal aging*1

NASA Astrophysics Data System (ADS)

Kawanishi, H.; Hajima, R.; Sekimura, N.; Arai, Y.; Ishino, S.

1988-07-01

Precipitation behavior has been studied using a carbon extraction replica technique in Ti-modified Type 316 stainless steels (JPCA-2) and 9Cr-2Mo ferritic/martensitic steels (JFMS) irradiated to 8.1 × 10 24 n/m 2 at 873 and 673 K, respectively, in the experimental fast breeder reactor JOYO. Precipitate identification and compositional analysis were carried out on extracted replicas. The results were compared to those from the as-received steel and a control which had been given the same thermal as-treatment as the specimens received during irradiations. Carbides, Ti-sulphides and phosphides were precipitated in JPCA-2. Precipitate observed in JFMS included carbides, Laves-phases and phosphides. The precipitates in both steels were concluded to be stable under irradiation except for MC and M 6C in JPCA-2. Small MC particles were found precipitated in JPCA-2 during both irradiation and aging. Irradiation proved to promote the precipitation of M 6C in JPCA-2.

[Determination of seven phenoxyacid herbicides in environmental water by high performance liquid chromatography coupled with three phase hollow fiber liquid phase microextraction].

PubMed

Peng, Xiaojun; Pang, Jinshan; Deng, Aihua

2011-12-01

A novel method for the simultaneous determination of seven phenoxyacid herbicides such as dicamba, fluroxypyr, 4-chlorophenoxyacetic acid (4-CPA), 2-methyl-4-chlorophenoxyacetic acid (MCPA), 2, 4-dichlorophenoxyacetic acid (2,4-D), 2,4-dichlorophenoxybutyric acid (2,4-DB) and 4-(2-methyl-4-chlorophenoxy) butyric acid (MCPB) in environmental water by three phase hollow fiber liquid phase microextraction (HF-LPME) coupled with high performance liquid chromatography (HPLC) was developed. In order to optimize the experimental conditions, the orthogonal test has been used. The effects of extraction solvent, pH of the donor phase and acceptor phase, extraction time, stirring speed and salt concentration on the detection were investigated. The optimal experimental conditions were as follows: octanol as organic solvent, pH 3 of donor phase, pH 12 of acceptor phase, extraction time of 30 min, stirring speed of 400 r/min. The results showed that the proposed method provided a wide linear range for 7 phenoxyacid herbicides with correlation coefficients of 0.995 3 - 0.998 8. The detection limits ranged from 0.2 to 1.0 microg/L. The enrichment factors were in the range of 76.7 - 121. The recoveries were in the range of 68% - 104% and the relative standard deviations (RSDs) were less than 8.1% for the environmental water samples. The method has the advantages of sensitivity, simplicity, fastness and the use of very small amounts of organic solvent. The method can meet the requirements of the determination of trace phenoxyacid herbicides in the environmental water samples, and the study provided a useful method for the analysis of trace substances in water samples.

Comparison of sample preparation methods combined with fast gas chromatography-mass spectrometry for ultratrace analysis of pesticide residues in baby food.

PubMed

Hercegová, Andrea; Dömötörová, Milena; Kruzlicová, Dása; Matisová, Eva

2006-05-01

Four sample preparation techniques were compared for the ultratrace analysis of pesticide residues in baby food: (a) modified Schenck's method based on ACN extraction with SPE cleaning; (b) quick, easy, cheap, effective, rugged, and safe (QuEChERS) method based on ACN extraction and dispersive SPE; (c) modified QuEChERS method which utilizes column-based SPE instead of dispersive SPE; and (d) matrix solid phase dispersion (MSPD). The methods were combined with fast gas chromatographic-mass spectrometric analysis. The effectiveness of clean-up of the final extract was determined by comparison of the chromatograms obtained. Time consumption, laboriousness, demands on glassware and working place, and consumption of chemicals, especially solvents, increase in the following order QuEChERS < modified QuEChERS < MSPD < modified Schenck's method. All methods offer satisfactory analytical characteristics at the concentration levels of 5, 10, and 100 microg/kg in terms of recoveries and repeatability. Recoveries obtained for the modified QuEChERS method were lower than for the original QuEChERS. In general the best LOQs were obtained for the modified Schenck's method. Modified QuEChERS method provides 21-72% better LOQs than the original method.

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

PubMed

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

2016-09-01

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

Development of magnetic octadecylsilane particles as solid-phase extraction adsorbent for the determination of fat-soluble vitamins in fruit juice-milk beverage by capillary liquid chromatography.

PubMed

Hu, Chaofan; Jia, Li; Liu, Qingqing; Zhang, Sheng

2010-07-01

A sensitive, fast and simple method based on magnetic octadecylsilane particles was developed for the extraction of three fat-soluble vitamins followed by capillary LC (CLC) analysis with UV detection. Magnetic octadecylsilane particles were prepared based on three-step reactions including co-precipitation, sol-gel polymerization and alkylation. The characterization of the prepared product was studied by scanning electron microscope and Fourier-transform infrared spectrometry. The particles were used as magnetic SPE adsorbent for the extraction of fat-soluble vitamins in fruit juice-milk beverage. The extraction condition and efficiency of the particles for fat-soluble vitamins were investigated. By coupling magnetic SPE with capillary LC with UV detection, low concentrations of fat-soluble vitamins in fruit juice-milk beverage can be detected without the interference from other substances in the sample matrix.

Analysis of trace levels of pesticides in rainwater by SPME and GC-tandem mass spectrometry after derivatisation with PFBBr.

PubMed

Scheyer, Anne; Briand, Olivier; Morville, Stéphane; Mirabel, Philippe; Millet, Maurice

2007-01-01

Solid-phase microextraction (SPME) was used for the analysis of some pesticides (bromoxynil, chlorotoluron, diuron, isoproturon, 2,4-MCPA, MCPP and 2,4-D) in rainwater after derivatisation with PFBBr and gas chromatography-ion trap mass spectrometry. The derivatisation procedure was optimized by testing different methods: direct derivatisation in the aqueous phase followed by SPME extraction, on-fibre derivatisation and derivatisation in the injector. The best result was obtained by headspace coating the PDMS/DVB fibre with PFBBr for 10 min followed by direct SPME extraction for 60 min at 68 degrees C (pH 2 and 75% NaCl). Good detection limits were obtained for all the compounds: these ranged between 10 and 1,000 ng L-1 with a relatively high uncertainty due to the combination of derivatisation and SPME extraction steps. The optimized procedure was applied to the analysis of pesticides in rainwater and results obtained shows that this method is a fast and simple technique to assess the spatial and temporal variations of concentrations of pesticides in rainwater.

Cellulose Nanofibril Based-Aerogel Microreactors: A High Efficiency and Easy Recoverable W/O/W Membrane Separation System

PubMed Central

Zhang, Fang; Ren, Hao; Dou, Jing; Tong, Guolin; Deng, Yulin

2017-01-01

Hereby we report a novel cellulose nanofirbril aerogel-based W/O/W microreactor system that can be used for fast and high efficient molecule or ions extraction and separation. The ultra-light cellulose nanofibril based aerogel microspheres with high porous structure and water storage capacity were prepared. The aerogel microspheres that were saturated with stripping solution were dispersed in an oil phase to form a stable water-in-oil (W/O) suspension. This suspension was then dispersed in large amount of external waste water to form W/O/W microreactor system. Similar to a conventional emulsion liquid membrane (ELM), the molecules or ions in external water can quickly transport to the internal water phase. However, the microreactor is also significantly different from traditional ELM: the water saturated nanocellulose cellulose aerogel microspheres can be easily removed by filtration or centrifugation after extraction reaction. The condensed materials in the filtrated aerogel particles can be squeezed and washed out and aerogel microspheres can be reused. This novel process overcomes the key barrier step of demulsification in traditional ELM process. Our experimental indicates the novel microreactor was able to extract 93% phenol and 82% Cu2+ from external water phase in a few minutes, suggesting its great potential for industrial applications. PMID:28059153

Cellulose Nanofibril Based-Aerogel Microreactors: A High Efficiency and Easy Recoverable W/O/W Membrane Separation System

NASA Astrophysics Data System (ADS)

Zhang, Fang; Ren, Hao; Dou, Jing; Tong, Guolin; Deng, Yulin

2017-01-01

Hereby we report a novel cellulose nanofirbril aerogel-based W/O/W microreactor system that can be used for fast and high efficient molecule or ions extraction and separation. The ultra-light cellulose nanofibril based aerogel microspheres with high porous structure and water storage capacity were prepared. The aerogel microspheres that were saturated with stripping solution were dispersed in an oil phase to form a stable water-in-oil (W/O) suspension. This suspension was then dispersed in large amount of external waste water to form W/O/W microreactor system. Similar to a conventional emulsion liquid membrane (ELM), the molecules or ions in external water can quickly transport to the internal water phase. However, the microreactor is also significantly different from traditional ELM: the water saturated nanocellulose cellulose aerogel microspheres can be easily removed by filtration or centrifugation after extraction reaction. The condensed materials in the filtrated aerogel particles can be squeezed and washed out and aerogel microspheres can be reused. This novel process overcomes the key barrier step of demulsification in traditional ELM process. Our experimental indicates the novel microreactor was able to extract 93% phenol and 82% Cu2+ from external water phase in a few minutes, suggesting its great potential for industrial applications.

Development of coatings for automated 96-blade solid phase microextraction-liquid chromatography-tandem mass spectrometry system, capable of extracting a wide polarity range of analytes from biological fluids.

PubMed

Mirnaghi, Fatemeh S; Pawliszyn, Janusz

2012-10-26

This work presents the development and evaluation of biocompatible polyacrylonitrile-polystyrene-divinylbenzene (PAN-PS-DVB) and polyacrylonitrile-phenylboronic acid (PAN-PBA) coatings for automated 96-blades (thin-film) solid phase microextraction (SPME) system, using high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS). The SPME condition was optimized for 60 min equilibrium extraction and 40 min desorption for PAN-PS-DVB, and 120 min equilibrium extraction and 60 min desorption for PAN-PBA for parallel sample preparation of up to 96 samples. The thin film geometry of the SPME blades provided good extraction efficiency due to the larger surface area of the coating, and simultaneous sample preparation provided fast and accurate analysis. The PAN-PS-DVB and PAN-PBA 96-blade SPME coatings were evaluated for extraction of analytes in a wide range of polarity (log P=2.8 to -3.7), and they demonstrated efficient extraction recovery (3.5-98.9% for PAN-PS-DVB and 4.0-74.1% for PAN-PBA) for both polar and non-polar groups of compounds. Reusability, reproducibility, and reliability of the system were evaluated. The results demonstrated that both coatings presented chemical and mechanical stability and long-lasting extraction efficiency for more than 100 usages in phosphate-buffered saline (PBS) and human plasma. Copyright © 2012 Elsevier B.V. All rights reserved.

A Simple and Fast Extraction Method for the Determination of Multiclass Antibiotics in Eggs Using LC-MS/MS.

PubMed

Wang, Kun; Lin, Kunde; Huang, Xinwen; Chen, Meng

2017-06-21

The purpose of this study was to develop and validate a simple, fast, and specific extraction method for the analysis of 64 antibiotics from nine classes (including sulfonamides, quinolones, tetracyclines, macrolides, lincosamide, nitrofurans, β-lactams, nitromidazoles, and cloramphenicols) in chicken eggs. Briefly, egg samples were simply extracted with a mixture of acetonitrile-water (90:10, v/v) and 0.1 mol·L -1 Na 2 EDTA solution assisted with ultrasonic. The extract was centrifuged, condensed, and directly analyzed on a liquid chromatography coupled to tandem mass spectrometry. Compared with conventional cleanup methods (passing through solid phase extract cartridges), the established method demonstrated comparable efficiencies in eliminating matrix effects and higher or equivalent recoveries for most of the target compounds. Typical validation parameters including specificity, linearity, matrix effect, limits of detection (LODs) and quantification (LOQs), the decision limit, detection capability, trueness, and precision were evaluated. The recoveries of target compounds ranged from 70.8% to 116.1% at three spiking levels (5, 20, and 50 μg·kg -1 ), with relative standard deviations less than 14%. LODs and LOQs were in the ranges of 0.005-2.00 μg·kg -1 and 0.015-6.00 μg·kg -1 for all of the antibiotics, respectively. A total of five antibiotics were successfully detected in 22 commercial eggs from local markets. This work suggests that the method is suitable for the analysis of multiclass antibiotics in eggs.

Determination of Five Major 8-Prenylflavones in Leaves of Epimedium by Solid-Phase Extraction Coupled with Capillary Electrophoresis

PubMed Central

Xie, Juan-ping; Xiang, Ji-ming; Zhu, Zhong-liang

2016-01-01

A simple, accurate and reproducible method which is based on the capillary electrophoresis, coupled with solid-phase extraction, has been developed for simultaneous determination of multiple 8-prenylflavones from Chinese Herba Epimedii. In this study, the author has mainly illustrated the experimental process and research results of five major components including epimedin C, icariin, diphylloside A, epimedoside A and icarisoside A that have been extracted and identified from Herba Epimedii for the first time. Experimental conditions have been optimized to achieve the best separation efficiency for the following factors: the buffer pH, buffer concentration and applied voltage. The experiment can be conducted through two separable stages: the first stage is to obtain the crude extracts through the solid-phase extraction; and the second stage is to further separate five major components by using the capillary electrophoresis. The separation of the five components and the analysis of the experiment are relatively fast and can be completed within 20 min. The concentration ranges of the construction of standard curves of five major 8-prenylflavones are 32.0–395.0, 23.4–292.0, 42.1–526.0, 18.8–233.5 and 29.7–371.0 µg mL−1 respectively, which have showed acceptable linearity with a correlation coefficient, r ≥ 0.999. The coefficient varies within 2.0% for both intra- and inter-days tests. The recoveries of five components range from 92.3 to 104.1%. The relative standard deviations of recoveries of five components range from 1.2 and 2.8%. This new method will facilitate the extraction and expedite the determination of medical components from Herba Epimedii. PMID:26865656

Operator care and eco-concerned development of a fast, facile and economical assay for basic nitrogenous drugs based on simplified ion-pair mini-scale extraction using safer solvent combined with drop-based spectrophotometry.

PubMed

Plianwong, Samarwadee; Sripattanaporn, Areerut; Waewsa-nga, Kwanrutai; Buacheen, Parin; Opanasopit, Praneet; Ngawhirunpat, Tanasait; Rojanarata, Theerasak

2012-08-30

A fast, facile, and economical assay for basic nitrogenous drugs has been developed based on the mini-scale extraction of the drug-dye ion pair complex combined with the use of safe-for-analyst and eco-friendlier organic extractant and drop-based micro-spectrophotometry. Instead of using large volume devices, the extraction was simply carried out in typical 1.5 mL microcentrifuge tubes along with the use of micropipettes for accurate transfer of liquids, vortex mixer for efficient partitioning of solutes and benchtop centrifuge for rapid phase separation. In the last step, back-extraction was performed by using the microvolume of acidic solution in order to concentrate the colored species into a confined aqueous microdrop and to keep the analyst away from unwanted contact and inhalation of organic solvents during the quantitation step which was achieved by using cuvetteless UV-vis micro-spectrophotometry without any prior dilutions. Using chlorpheniramine maleate as a representative analyte and n-butyl acetate as a less toxic and non-ozone depleting extractant, the miniaturized method was less laborious and much faster. It was accurate, precise and insensitive to the interferences from common excipients. Notably, it gave the assay results of drug in tablets and oral solution comparable to the large-scale pharmacopeial method while the consumption of organic solvents and the release of wastes were lowered by 200-400 folds. Copyright © 2012 Elsevier B.V. All rights reserved.

Design of extraction system in BRing at HIAF

NASA Astrophysics Data System (ADS)

Ruan, Shuang; Yang, Jiancheng; Zhang, Jinquan; Shen, Guodong; Ren, Hang; Liu, Jie; Shangguan, Jingbing; Zhang, Xiaoying; Zhang, Jingjing; Mao, Lijun; Sheng, Lina; Yin, Dayu; Wang, Geng; Wu, Bo; Yao, Liping; Tang, Meitang; Cai, Fucheng; Chen, Xiaoqiang

2018-06-01

The Booster Ring (BRing), which is the key part of HIAF (High Intensity heavy ion Accelerator Facility) complex at IMP (Institute of Modern Physics, Chinese Academy of Sciences), can provide uranium (A / q = 7) beam with a wide extraction energy range of 200-800 MeV/u. To fulfill a flexible beam extraction for multi-purpose experiments, both fast and slow extraction systems will be accommodated in the BRing. The fast extraction system is used for extracting short bunched beam horizontally in single-turn. The slow extraction system is used to provide quasi-continuous beam by the third order resonance and RF-knockout scheme. To achieve a compact structure, the two extraction systems are designed to share the same extraction channel. The general design of the fast and slow extraction systems and simulation results are discussed in this paper.

A Pedestrian Detection Scheme Using a Coherent Phase Difference Method Based on 2D Range-Doppler FMCW Radar

PubMed Central

Hyun, Eugin; Jin, Young-Seok; Lee, Jong-Hun

2016-01-01

For an automotive pedestrian detection radar system, fast-ramp based 2D range-Doppler Frequency Modulated Continuous Wave (FMCW) radar is effective for distinguishing between moving targets and unwanted clutter. However, when a weak moving target such as a pedestrian exists together with strong clutter, the pedestrian may be masked by the side-lobe of the clutter even though they are notably separated in the Doppler dimension. To prevent this problem, one popular solution is the use of a windowing scheme with a weighting function. However, this method leads to a spread spectrum, so the pedestrian with weak signal power and slow Doppler may also be masked by the main-lobe of clutter. With a fast-ramp based FMCW radar, if the target is moving, the complex spectrum of the range- Fast Fourier Transform (FFT) is changed with a constant phase difference over ramps. In contrast, the clutter exhibits constant phase irrespective of the ramps. Based on this fact, in this paper we propose a pedestrian detection for highly cluttered environments using a coherent phase difference method. By detecting the coherent phase difference from the complex spectrum of the range-FFT, we first extract the range profile of the moving pedestrians. Then, through the Doppler FFT, we obtain the 2D range-Doppler map for only the pedestrian. To test the proposed detection scheme, we have developed a real-time data logging system with a 24 GHz FMCW transceiver. In laboratory tests, we verified that the signal processing results from the proposed method were much better than those expected from the conventional 2D FFT-based detection method. PMID:26805835

A Pedestrian Detection Scheme Using a Coherent Phase Difference Method Based on 2D Range-Doppler FMCW Radar.

PubMed

Hyun, Eugin; Jin, Young-Seok; Lee, Jong-Hun

2016-01-20

For an automotive pedestrian detection radar system, fast-ramp based 2D range-Doppler Frequency Modulated Continuous Wave (FMCW) radar is effective for distinguishing between moving targets and unwanted clutter. However, when a weak moving target such as a pedestrian exists together with strong clutter, the pedestrian may be masked by the side-lobe of the clutter even though they are notably separated in the Doppler dimension. To prevent this problem, one popular solution is the use of a windowing scheme with a weighting function. However, this method leads to a spread spectrum, so the pedestrian with weak signal power and slow Doppler may also be masked by the main-lobe of clutter. With a fast-ramp based FMCW radar, if the target is moving, the complex spectrum of the range- Fast Fourier Transform (FFT) is changed with a constant phase difference over ramps. In contrast, the clutter exhibits constant phase irrespective of the ramps. Based on this fact, in this paper we propose a pedestrian detection for highly cluttered environments using a coherent phase difference method. By detecting the coherent phase difference from the complex spectrum of the range-FFT, we first extract the range profile of the moving pedestrians. Then, through the Doppler FFT, we obtain the 2D range-Doppler map for only the pedestrian. To test the proposed detection scheme, we have developed a real-time data logging system with a 24 GHz FMCW transceiver. In laboratory tests, we verified that the signal processing results from the proposed method were much better than those expected from the conventional 2D FFT-based detection method.

Impact of Using a High Surface Area Solid Phase Micro Extraction Device and Fast Gas Chromatography Heating Rates in the Sampling and Analysis of Trace Level Chemical Warfare Agents and CWA-Like Compounds

DTIC Science & Technology

2009-09-21

35(5):38-41. 27. Smith, P. A., Sng , M.T., et al. (2005). "Towards Smaller and Faster Gas Chromatography Mass Spectrometry Systems for Field...Analytical Methods. Chapter 10. West Sussex, Wiley & Sons Ltd. 9. Smith, P. A., Sng , M.T., et al. (2005). "Towards Smaller and Faster Gas

Studies on the Tempo of Bubble Formation in Recently Cavitated Vessels: A Model to Predict the Pressure of Air Bubbles1

PubMed Central

Wang, Yujie; Pan, Ruihua; Tyree, Melvin T.

2015-01-01

A cavitation event in a vessel replaces water with a mixture of water vapor and air. A quantitative theory is presented to argue that the tempo of filling of vessels with air has two phases: a fast process that extracts air from stem tissue adjacent to the cavitated vessels (less than 10 s) and a slow phase that extracts air from the atmosphere outside the stem (more than 10 h). A model was designed to estimate how water tension (T) near recently cavitated vessels causes bubbles in embolized vessels to expand or contract as T increases or decreases, respectively. The model also predicts that the hydraulic conductivity of a stem will increase as bubbles collapse. The pressure of air bubbles trapped in vessels of a stem can be predicted from the model based on fitting curves of hydraulic conductivity versus T. The model was validated using data from six stem segments each of Acer mono and the clonal hybrid Populus 84K (Populus alba × Populus glandulosa). The model was fitted to results with root mean square error less than 3%. The model provided new insight into the study of embolism formation in stem tissue and helped quantify the bubble pressure immediately after the fast process referred to above. PMID:25907963

Studies on the tempo of bubble formation in recently cavitated vessels: a model to predict the pressure of air bubbles.

PubMed

Wang, Yujie; Pan, Ruihua; Tyree, Melvin T

2015-06-01

A cavitation event in a vessel replaces water with a mixture of water vapor and air. A quantitative theory is presented to argue that the tempo of filling of vessels with air has two phases: a fast process that extracts air from stem tissue adjacent to the cavitated vessels (less than 10 s) and a slow phase that extracts air from the atmosphere outside the stem (more than 10 h). A model was designed to estimate how water tension (T) near recently cavitated vessels causes bubbles in embolized vessels to expand or contract as T increases or decreases, respectively. The model also predicts that the hydraulic conductivity of a stem will increase as bubbles collapse. The pressure of air bubbles trapped in vessels of a stem can be predicted from the model based on fitting curves of hydraulic conductivity versus T. The model was validated using data from six stem segments each of Acer mono and the clonal hybrid Populus 84 K (Populus alba × Populus glandulosa). The model was fitted to results with root mean square error less than 3%. The model provided new insight into the study of embolism formation in stem tissue and helped quantify the bubble pressure immediately after the fast process referred to above. © 2015 American Society of Plant Biologists. All Rights Reserved.

Selective capture and rapid identification of Panax notoginseng metabolites in rat faeces by the integration of magnetic molecularly imprinted polymers and high-performance liquid chromatography coupled with orbitrap mass spectrometry.

PubMed

Cai, Qizhi; Yang, Zaiyue; Chen, Ning; Zhou, Xuemin; Hong, Junli

2016-07-15

In the present work, an advanced pretreatment method magnetic molecular imprinted polymers-dispersive solid phase extraction (MMIPs-DSPE) combined with the high sensitivity LTQ-Orbitrap mass spectrometry was applied to the complicated metabolites analysis of Traditional Chinese Medicines (TCMs) in complex matrices. The ginsenoside Rb1 magnetic molecular imprinted polymers (Rb1-MMIPs) were successfully synthesized for specific recognition and selective enrichment of Panax notoginseng saponin metabolites in rat faeces. The polymers were prepared by using Fe3O4@SiO2 as the supporting material, APTES as the functional monomer and TEOS as the cross-linker. The Rb1-MMIPs showed quick separation (10.8 emu/g), large adsorption capacity (636μmol/g), high selectivity and fast binding kinetics (25min). Dispersion solid-phase extraction using Rb1-MMIPs (Rb1-MMIPs-DSPE) integrated with LTQ-Orbitrap MS was applied to fish out and identify saponin metabolites from rat faeces, and totally 58 related compounds were detected within 20min, including 26 PPD-group and 32 PPT-group notoginsenoside metabolites. Parallel tests showed that Rb1-MMIPs-DSPE obtained the lowest matrix effects of 0.98-14.84% and captured the largest number of structural analogues compared with traditional pretreatment methods organic solvent extraction (OSE) and solid phase extraction (SPE). Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2008-02-01

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

Magnetic molecularly imprinted polymer for the selective extraction of quercetagetin from Calendula officinalis extract.

PubMed

Ma, Run-Tian; Shi, Yan-Ping

2015-03-01

A new magnetic molecularly imprinted polymers (MMIPs) for quercetagetin was prepared by surface molecular imprinting method using super paramagnetic core-shell nanoparticle as the supporter. Acrylamide as the functional monomer, ethyleneglycol dimethacrylate as the crosslinker and acetonitrile as the porogen were applied in the preparation process. Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and Vibrating sample magnetometer (VSM) were applied to characterize the MMIPs, and High performance liquid chromatography (HPLC) was utilized to analyze the target analytes. The selectivity of quercetagetin MMIPs was evaluated according to their recognition to template and its analogues. Excellent binding for quercetagetin was observed in MMIPs adsorption experiment, and the adsorption isotherm models analysis showed that the homogeneous binding sites were distributed on the surface of the MMIPs. The MMIPs were employed as adsorbents in solid phase extraction for the determination of quercetagetin in Calendula officinalis extracts. Furthermore, this method is fast, simple and could fulfill the determination and extraction of quercetagetin from herbal extract. Copyright © 2014 Elsevier B.V. All rights reserved.

Activity assay of mangosteen (Garcinia mangostana L.) pericarp extract for decreasing fasting blood cholesterol level and lipid peroxidation in type-2 diabetic mice

NASA Astrophysics Data System (ADS)

Husen, Saikhu Akhmad; Winarni, Dwi; Khaleyla, Firas; Kalqutny, Septian Hary; Ansori, Arif Nur Muhammad

2017-09-01

This study aimed to explore the activity of pericarp extract of mangosteen (Garcinia mangostana L.). Mangosteen pericarp contains various active compounds which are beneficial for human health. In-vivo antioxidant assay of pericarp extract was carried out using 3-4 month male mice of strain BALB/c weighed 30-40 g. The mice were divided into two groups: normal control (KN) group and STZ-induced diabetic group. STZ induction was performed using multiple low-dose method 30 mg/kg body weight treated daily for five consecutive days. Diabetic group was separated into two subgroups: diabetic control (KD), metformin control (KM), and crude extract treatment subgroups. The fasting blood glucose and the cholesterol level were measured before and after lard treatment, we also did it on the first, seventh, and fourteenth day of mangosteen pericarp crude extract treatment. The mice were treated with mangosteen pericarp crude extract for 14 days. The MDA level of the fasting blood serum was measured. The body weight and fasting blood cholesterol level before and after lard treatment were analyzed by t-test, whereas, the fasting blood cholesterol and the MDA level were analyzed using one-way variant analysis continued with Duncan test. The correlation between the increasing body weight and the fasting blood cholesterol level was determined by Pearson correlation test. The results of the study showed that the administration of mangosteen pericarp crude extract was able to reduce the fasting blood cholesterol and the malondialdehide level significantly.

Fast simulated annealing inversion of surface waves on pavement using phase-velocity spectra

USGS Publications Warehouse

Ryden, N.; Park, C.B.

2006-01-01

The conventional inversion of surface waves depends on modal identification of measured dispersion curves, which can be ambiguous. It is possible to avoid mode-number identification and extraction by inverting the complete phase-velocity spectrum obtained from a multichannel record. We use the fast simulated annealing (FSA) global search algorithm to minimize the difference between the measured phase-velocity spectrum and that calculated from a theoretical layer model, including the field setup geometry. Results show that this algorithm can help one avoid getting trapped in local minima while searching for the best-matching layer model. The entire procedure is demonstrated on synthetic and field data for asphalt pavement. The viscoelastic properties of the top asphalt layer are taken into account, and the inverted asphalt stiffness as a function of frequency compares well with laboratory tests on core samples. The thickness and shear-wave velocity of the deeper embedded layers are resolved within 10% deviation from those values measured separately during pavement construction. The proposed method may be equally applicable to normal soil site investigation and in the field of ultrasonic testing of materials. ?? 2006 Society of Exploration Geophysicists.

A phase-based stereo vision system-on-a-chip.

PubMed

Díaz, Javier; Ros, Eduardo; Sabatini, Silvio P; Solari, Fabio; Mota, Sonia

2007-02-01

A simple and fast technique for depth estimation based on phase measurement has been adopted for the implementation of a real-time stereo system with sub-pixel resolution on an FPGA device. The technique avoids the attendant problem of phase warping. The designed system takes full advantage of the inherent processing parallelism and segmentation capabilities of FPGA devices to achieve a computation speed of 65megapixels/s, which can be arranged with a customized frame-grabber module to process 211frames/s at a size of 640x480 pixels. The processing speed achieved is higher than conventional camera frame rates, thus allowing the system to extract multiple estimations and be used as a platform to evaluate integration schemes of a population of neurons without increasing hardware resource demands.

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.

Automation of ⁹⁹Tc extraction by LOV prior ICP-MS detection: application to environmental samples.

PubMed

Rodríguez, Rogelio; Leal, Luz; Miranda, Silvia; Ferrer, Laura; Avivar, Jessica; García, Ariel; Cerdà, Víctor

2015-02-01

A new, fast, automated and inexpensive sample pre-treatment method for (99)Tc determination by inductively coupled plasma-mass spectrometry (ICP-MS) detection is presented. The miniaturized approach is based on a lab-on-valve (LOV) system, allowing automatic separation and preconcentration of (99)Tc. Selectivity is provided by the solid phase extraction system used (TEVA resin) which retains selectively pertechnetate ion in diluted nitric acid solution. The proposed system has some advantages such as minimization of sample handling, reduction of reagents volume, improvement of intermediate precision and sample throughput, offering a significant decrease of both time and cost per analysis in comparison to other flow techniques and batch methods. The proposed LOV system has been successfully applied to different samples of environmental interest (water and soil) with satisfactory recoveries, between 94% and 98%. The detection limit (LOD) of the developed method is 0.005 ng. The high durability of the resin and its low amount (32 mg), its good intermediate precision (RSD 3.8%) and repeatability (RSD 2%) and its high extraction frequency (up to 5 h(-1)) makes this method an inexpensive, high precision and fast tool for monitoring (99)Tc in environmental samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Three-dimensional spatiotemporal features for fast content-based retrieval of focal liver lesions.

PubMed

Roy, Sharmili; Chi, Yanling; Liu, Jimin; Venkatesh, Sudhakar K; Brown, Michael S

2014-11-01

Content-based image retrieval systems for 3-D medical datasets still largely rely on 2-D image-based features extracted from a few representative slices of the image stack. Most 2 -D features that are currently used in the literature not only model a 3-D tumor incompletely but are also highly expensive in terms of computation time, especially for high-resolution datasets. Radiologist-specified semantic labels are sometimes used along with image-based 2-D features to improve the retrieval performance. Since radiological labels show large interuser variability, are often unstructured, and require user interaction, their use as lesion characterizing features is highly subjective, tedious, and slow. In this paper, we propose a 3-D image-based spatiotemporal feature extraction framework for fast content-based retrieval of focal liver lesions. All the features are computer generated and are extracted from four-phase abdominal CT images. Retrieval performance and query processing times for the proposed framework is evaluated on a database of 44 hepatic lesions comprising of five pathological types. Bull's eye percentage score above 85% is achieved for three out of the five lesion pathologies and for 98% of query lesions, at least one same type of lesion is ranked among the top two retrieved results. Experiments show that the proposed system's query processing is more than 20 times faster than other already published systems that use 2-D features. With fast computation time and high retrieval accuracy, the proposed system has the potential to be used as an assistant to radiologists for routine hepatic tumor diagnosis.

Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

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

2015-07-01

The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100 mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL-1 with low detection limit of 0.03 ng mL-1 were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method.

Cardiovascular response to short-term fasting in menstrual phases in young women: an observational study.

PubMed

Ohara, Kumiko; Okita, Yoshimitsu; Kouda, Katsuyasu; Mase, Tomoki; Miyawaki, Chiemi; Nakamura, Harunobu

2015-08-28

Menstrual cycle-related symptoms are an important health issue for many women, and some may affect cardiac autonomic regulation. In the present study, we evaluated the cardiovascular and physiological stress response to 12-h short-term fasting in the menstrual phases of healthy young women. We performed a randomized crossover study. Subjects were seven female university students (age: 22.3 ± 1.0 years). The experiments comprised four sessions: meal intake in the follicular phase, meal intake in the luteal phase, fasting in the follicular phase, and fasting in the luteal phase. All subjects participated in a total of four experimental sessions during two successive phases (follicular and luteal phase in the same menstrual cycle, or luteal phase and follicular phase in the next menstrual cycle) according to a randomized crossover design. R-R intervals were continuously recorded before and after meals, and power spectral analysis of heart rate variability was performed. Other physiological data were obtained before and 20, 40, 60, and 80 min after meal intake or after the corresponding time point of meal intake (fasting in the follicular or luteal phase). Heart rate decreased during fasting in the follicular and luteal phases. High frequency power increased during fasting in the follicular and luteal phases. In addition, salivary cortisol concentrations decreased during fasting in the luteal phase. In the present study, short-term fasting resulted in higher parasympathetic activity and lower cortisol levels in the luteal phase in these young women. These results indicate a possibility to produce an anti-stress effect in the luteal phase, which may reduce menstrual symptoms.

Equatorial anisotropy of the Earth's inner-inner core

NASA Astrophysics Data System (ADS)

Song, X.; Wang, T.; Xia, H.

2015-12-01

Anisotropy of Earth's inner core is a key to understand its evolution and the generation of the Earth's magnetic field. All the previous inner core anisotropy models have assumed a cylindrical anisotropy with the symmetry axis parallel (or nearly parallel) to the Earth's spin axis. However, we have recently found that the fast axis in the inner part of the inner core is close to the equator from inner-core waves extracted from earthquake coda. We obtained inner core phases, PKIIKP2 and PKIKP2 (round-trip phases between the station and its antipode that passes straight through the center of the Earth and that is reflected from the inner core boundary, respectively), from stackings of autocorrelations of the coda of large earthquakes (10,000~40,000 s after Mw>=7.0 earthquakes) at seismic station clusters around the world. We observed large variation of up to 10 s along equatorial paths in the differential travel times PKIIKP2 - PKIKP2, which are sensitive to inner-core structure. The observations can be explained by a cylindrical anisotropy in the inner inner core (IIC) (with a radius of slightly less than half the inner core radius) that has a fast axis aligned near the equator and a cylindrical anisotropy in the outer inner core (OIC) that has a fast axis along the north-south direction. We have obtained more observations using the combination of autocorrelations and cross-correlations at low-latitude station arrays. The results further confirm that the IIC has an equatorial anisotropy and a pattern different from the OIC. The equatorial fast axis of the IIC is near the Central America and the Southeast Asia. The drastic change in the fast axis and the form of anisotropy from the IIC to the OIC may suggest a phase change of the iron or a major shift in the crystallization and deformation during the formation and growth of the inner core.

Simultaneous UHPLC-UV analysis of hydroxychloroquine, minocycline and doxycycline from serum samples for the therapeutic drug monitoring of Q fever and Whipple's disease.

PubMed

Armstrong, Nicholas; Richez, Magali; Raoult, Didier; Chabriere, Eric

2017-08-15

A fast UHPLC-UV method was developed for the simultaneous analysis of Hydroxychloroquine, Minocycline and Doxycycline drugs from 100μL of human serum samples. Serum samples were extracted by liquid-liquid extraction and injected into a phenyl hexyl reverse phase column. Compounds were separated using a mobile phase linear gradient and monitored by UV detection at 343nm. Chloroquine and Oxytetracycline were used as internal standards. Lower and upper limits of quantifications, as well as the other levels of calibration, were validated with acceptable accuracy (<15% deviation) and precision (<15% coefficient of variation) according to the European Medicines Agency guidelines. This new method enables cost and time reduction and was considered suitable for the clinical laboratory. It is the first published assay for the therapeutic drug monitoring of patients diagnosed with Q fever or Whipple's disease. Copyright © 2017 Elsevier B.V. All rights reserved.

Ulcerogenic tumor syndrome of the pancreas associated with a nongastrin acid secretagogue.

PubMed Central

Chey, W Y; Chang, T M; Lee, K Y; Sun, G; Kim, C K; You, C H; Hamilton, D L; Shah, A; Rhee, J C; Mutt, V

1989-01-01

Among 30 patients with islet cell neoplasms or hyperplasia who exhibited marked gastric acid hypersecretion and peptic ulceration and/or diarrhea, fasting plasma gastrin concentrations were less than 150 pg/ml in 11 patients, whereas the remaining 19 patients had hypergastrinemia. Plasma extracts from seven of these 11 patients were assayed for acid secretagogue activity in rats. All seven plasma extracts had secretagogue activity that was not found in the plasma extracts of ten patients with ordinary duodenal ulcer disease. Each of the tumor or pancreatic tissue extracts obtained from nine patients exhibited secretagogue activity in rats even though tissue gastrin content was 101.9 pmol (213.8 ng).g-1 or less. The secretagogue activity of the tumor extracts was confirmed in conscious gastric fistula dogs. The tumors' secretagogue activity, in contrast to gastrin, was destroyed by trypsin. It was eluted between porcine motilin and human gastrin I from a Sephadex G-50 (Pharmacia LKB Biotechnology, Inc., Piscataway, NJ) superfine column and was not retained by CM-cellulose, at pH 8.5. Its retention time during reverse phase HPLC on a C18 column also differed from those of G17 and G34. Thus, this secretagogue activity appeared mediated by a small, acidic peptide with a molecular size of about 2000 to 3000 daltons. The present study indicates that plasma and tumor extracts of these 11 patients contain a gastric acid secretagogue activity mediated by a nongastrin peptide. We suggest that what may be a distinct clinical entity associated with endocrine neoplasms of the pancreas should be considered in the face of excessive acid hypersecretion without fasting hypergastrinemia. PMID:2757418

Environmentally Friendly Method: Development and Application to Carbon Aerogel as Sorbent for Solid-Phase Extraction.

PubMed

Dong, Sheying; Huang, Guiqi; Su, Meiling; Huang, Tinglin

2015-10-14

We developed two simple, fast, and environmentally friendly methods using carbon aerogel (CA) and magnetic CA (mCA) materials as sorbents for micro-solid-phase extraction (μ-SPE) and magnetic solid-phase extraction (MSPE) techniques. The material performances such as adsorption isotherm, adsorption kinetics, and specific surface area were discussed by N2 adsorption-desorption isotherm measurements, ultraviolet and visible (UV-vis) spectrophotometry, scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HR-TEM). The experimental results proved that the heterogeneities of CA and mCA were well modeled with the Freundlich isotherm model, and the sorption process well followed the pseudo-second-order rate equation. Moreover, plant growth regulators (PGRs) such as kinetin (6-KT), 6-benzylaminopurine (6-BA), 2,4-dichlorophenoxyacetic acid (2,4-D), and uniconazole (UN) in a reservoir raw water sample were selected as the evaluation of applicability for the proposed μ-SPE and MSPE techniques using high performance liquid chromatography (HPLC). The experimental conditions of two methods such as the amount of sorbent, extraction time, pH, salt concentration, and desorption conditions were studied. Under the optimized conditions, two extraction methods provided high recoveries (89-103%), low the limits of detection (LODs) (0.01-0.2 μg L(-1)), and satisfactory analytical features in terms of precision (relative standard deviation, RSD, 1.7-5.1%, n=3). This work demonstrates the feasibility and the potential of CA and mCA materials as sorbents for μ-SPE and MSPE techniques. Besides, it also could serve as a basis for future development of other functional CAs in pretreatment technology and make them valuable for analysis of pollutants in environmental applications.

Excitation power quantities in phase resonance testing of nonlinear systems with phase-locked-loop excitation

NASA Astrophysics Data System (ADS)

Peter, Simon; Leine, Remco I.

2017-11-01

Phase resonance testing is one method for the experimental extraction of nonlinear normal modes. This paper proposes a novel method for nonlinear phase resonance testing. Firstly, the issue of appropriate excitation is approached on the basis of excitation power considerations. Therefore, power quantities known from nonlinear systems theory in electrical engineering are transferred to nonlinear structural dynamics applications. A new power-based nonlinear mode indicator function is derived, which is generally applicable, reliable and easy to implement in experiments. Secondly, the tuning of the excitation phase is automated by the use of a Phase-Locked-Loop controller. This method provides a very user-friendly and fast way for obtaining the backbone curve. Furthermore, the method allows to exploit specific advantages of phase control such as the robustness for lightly damped systems and the stabilization of unstable branches of the frequency response. The reduced tuning time for the excitation makes the commonly used free-decay measurements for the extraction of backbone curves unnecessary. Instead, steady-state measurements for every point of the curve are obtained. In conjunction with the new mode indicator function, the correlation of every measured point with the associated nonlinear normal mode of the underlying conservative system can be evaluated. Moreover, it is shown that the analysis of the excitation power helps to locate sources of inaccuracies in the force appropriation process. The method is illustrated by a numerical example and its functionality in experiments is demonstrated on a benchmark beam structure.

On-line comprehensive two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography for preparative isolation of toad venom.

PubMed

Li, Jia-Fu; Fang, Hua; Yan, Xia; Chang, Fang-Rong; Wu, Zhen; Wu, Yun-Long; Qiu, Ying-Kun

2016-07-22

An on-line comprehensive preparative two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography (2D NPLC×RPLC) system was constructed with a newly developed vacuum evaporation assisted adsorption (VEAA) interface, allowing fast removal of NPLC solvent in the vacuum condition and successfully solving the solvent incompatibility problem between NPLC and RPLC. The system achieved on-line solvent exchange within the two dimensions and its performance was illustrated by gram-scale isolation of crude extract from the venom of Bufo bufo gargarizans. Within separation time of ∼20h, 19 compounds were obtained with high purity in a single run. With the VEAA interface, the 2D system exhibited apparent advantages in separation efficiency and automation compared with conventional methods, indicating its promising application in the routine separation process for complicated natural products. Copyright © 2016 Elsevier B.V. All rights reserved.

Miniature wireless recording and stimulation system for rodent behavioural testing

NASA Astrophysics Data System (ADS)

Pinnell, R. C.; Dempster, J.; Pratt, J.

2015-12-01

Objective. Elucidation of neural activity underpinning rodent behaviour has traditionally been hampered by the use of tethered systems and human involvement. Furthermore the combination of deep-brain stimulation (DBS) and various neural recording modalities can lead to complex and time-consuming laboratory setups. For studies of this type, novel tools are required to drive forward this research. Approach. A miniature wireless system weighing 8.5 g (including battery) was developed for rodent use that combined multichannel DBS and local-field potential (LFP) recordings. Its performance was verified in a working memory task that involved 4-channel fronto-hippocampal LFP recording and bilateral constant-current fimbria-fornix DBS. The system was synchronised with video-tracking for extraction of LFP at discrete task phases, and DBS was activated intermittently at discrete phases of the task. Main results. In addition to having a fast set-up time, the system could reliably transmit continuous LFP at over 8 hours across 3-5 m distances. During the working memory task, LFP pertaining to discrete task phases was extracted and compared with well-known neural correlates of active exploratory behaviour in rodents. DBS could be wirelessly activated/deactivated at any part of the experiment during EEG recording and transmission, allowing for a seamless integration of this modality. Significance. The wireless system combines a small size with a level of robustness and versatility that can greatly simplify rodent behavioural experiments involving EEG recording and DBS. Designed for versatility and simplicity, the small size and low-cost of the system and its receiver allow for enhanced portability, fast experimental setup times, and pave the way for integration with more complex behaviour.

Fast methodology of analysing major steviol glycosides from Stevia rebaudiana leaves.

PubMed

Lorenzo, Cándida; Serrano-Díaz, Jéssica; Plaza, Miguel; Quintanilla, Carmen; Alonso, Gonzalo L

2014-08-15

The aim of this work is to propose an HPLC method for analysing major steviol glycosides as well as to optimise the extraction and clarification conditions for obtaining these compounds. Toward this aim, standards of stevioside and rebaudioside A with purities ⩾99.0%, commercial samples from different companies and Stevia rebaudiana Bertoni leaves from Paraguay supplied by Insobol, S.L., were used. The analytical method proposed is adequate in terms of selectivity, sensitivity and accuracy. Optimum extraction conditions and adequate clarification conditions have been set. Moreover, this methodology is safe and eco-friendly, as we use only water for extraction and do not use solid-phase extraction, which requires solvents that are banned in the food industry to condition the cartridge and elute the steviol glycosides. In addition, this methodology consumes little time as leaves are not ground and the filtration is faster, and the peak resolution is better as we used an HPLC method with gradient elution. Copyright © 2014 Elsevier Ltd. All rights reserved.

Development and validation of an RP-HPLC method for quantitative determination of vanillin and related phenolic compounds in Vanilla planifolia.

PubMed

Sinha, Arun Kumar; Verma, Subash Chandra; Sharma, Upendra Kumar

2007-01-01

A simple and fast method was developed using RP-HPLC for separation and quantitative determination of vanillin and related phenolic compounds in ethanolic extract of pods of Vanilla planifolia. Ten phenolic compounds, namely 4-hydroxybenzyl alcohol, vanillyl alcohol, 3,4-dihydroxybenzaldehyde, 4-hydroxybenzoic acid, vanillic acid, 4-hydroxybenzaldehyde, vanillin, p-coumaric acid, ferulic acid, and piperonal were quantitatively determined using ACN, methanol, and 0.2% acetic acid in water as a mobile phase with a gradient elution mode. The method showed good linearity, high precision, and good recovery of compounds of interest. The present method would be useful for analytical research and for routine analysis of vanilla extracts for their quality control.

Green synthesis of ZnO nanoparticles via complex formation by using Curcuma longa extract

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

Fatimah, Is, E-mail: isfatimah@uii.ac.id; Yudha, Septian P.; Mutiara, Nur Afisa Lintang

Synthesis of ZnO nanoparticles(NPs) were conducted via Zn(II) complex formation by using Curcuma longa extract as template. Curcuma longa extract has the ability to form zinc ions complex with curcumin as ligating agent. Study on synthesis was conducted by monitoring thermal degradation of the material. Successful formation of zinc oxide nanoparticles was confirmed by employing x-ray diffraction, surface area analysis and transmission electron microscopy(TEM) studies. From the XRD analysis it is denoted that ZnO in hexagonal wurtzite phase was formed and particle size was varied as varied temperature. The data are also confirmed by TEM analysis which shows the particlemore » sie at the range 20-80nm. The NPs exhibited excelent photocatalytic activity for methylene blue degradation and also significant antibacterial activity for Eschericia coli. The activity in methylene blue degradation was also confirmed from fast chemical oxygen demand (COD) reduction.« less

Green synthesis of ZnO nanoparticles via complex formation by using Curcuma longa extract

NASA Astrophysics Data System (ADS)

Fatimah, Is; Yudha, Septian P.; Mutiara, Nur Afisa Lintang

2016-02-01

Synthesis of ZnO nanoparticles(NPs) were conducted via Zn(II) complex formation by using Curcuma longa extract as template. Curcuma longa extract has the ability to form zinc ions complex with curcumin as ligating agent. Study on synthesis was conducted by monitoring thermal degradation of the material. Successful formation of zinc oxide nanoparticles was confirmed by employing x-ray diffraction, surface area analysis and transmission electron microscopy(TEM) studies. From the XRD analysis it is denoted that ZnO in hexagonal wurtzite phase was formed and particle size was varied as varied temperature. The data are also confirmed by TEM analysis which shows the particle sie at the range 20-80nm. The NPs exhibited excelent photocatalytic activity for methylene blue degradation and also significant antibacterial activity for Eschericia coli. The activity in methylene blue degradation was also confirmed from fast chemical oxygen demand (COD) reduction.

Application of ionic liquid-based dispersive liquid phase microextraction for highly sensitive simultaneous determination of three endocrine disrupting compounds in food packaging.

PubMed

Wang, Lingling; Zhang, Danfeng; Xu, Xu; Zhang, Lei

2016-04-15

Ionic liquid (IL) dispersive liquid-liquid microextraction (DLLME) method was successfully developed for extracting three endocrine disrupting compounds (EDCs) (bisphenol A, bisphenol AF and bisphenol AP) from the food packaging. 1-Octyl-3-methylimidazoliumhexafluorophosphate ([C8MIM][PF6]) was selected as extraction solution. The extraction procedure did not require a dispersive solvent. Three EDCs extraction kinetics were found to be very fast and the equilibrium was attained within 3.0 min following the pseudo-first-order model. The H-bonding and hydrophobic interactions play an important role in the partitioning of EDCs into IL from aqueous solution. The recovered IL could be reused for three runs without significant loss of extraction efficiencies. The spiked recoveries of three targets in food packaging were in the range of 97.8-103.1%. The limits of detection ranged from 0.50 to 1.50 ng mL(-1) (S/N=3). As a result, this method has been successfully applied for the sensitive detection of three EDCs in real samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

PubMed

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

2018-04-01

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

Removal of sudan dyes from water with C18-functional ultrafine magnetic silica nanoparticles.

PubMed

Jiang, Chunzhu; Sun, Ying; Yu, Xi; Zhang, Lei; Sun, Xiumin; Gao, Yan; Zhang, Hanqi; Song, Daqian

2012-01-30

In this study, the new C(18)-functionalized ultrafine magnetic silica nanoparticles (C(18)-UMS NPs) were successfully synthesized and applied for extraction of sudan dyes in water samples based on the magnetic solid-phase extraction (MSPE). The extraction and concentration were carried out in one step by blending C(18)-UMS NPs and water samples. The sudan dyes adsorbed C(18)-UMS NPs were isolated from the matrix easily with an external magnetic field. After desorption the quantitation of sudan dyes was done by ultra fast liquid chromatography (UFLC). Satisfactory extraction recovery can be obtained with only 50 mg C(18)-UMS NPs. The effects of experimental parameters, including the amount of the nanoparticles, extraction time, pH value, desorption solvent, volume of desorption solvent and desorption time were investigated. The limits of detection for sudan I, II, III and IV were 0.066, 0.070, 0.12 and 0.12 ng mL(-1), respectively. Recoveries obtained by analyzing the six spiked water samples were between 68% and 103%. Copyright © 2011 Elsevier B.V. All rights reserved.

Characterization and identification of multiple constituents in Yinhuang granules by high-performance liquid chromatography with diode-array and time-of-flight mass spectrometry detection.

PubMed

Liu, E-Hu; Liu, Qun; Chu, Chu; Li, Ping

2011-10-01

A fast high-performance liquid chromatography (HPLC) method with diode-array detection (DAD) and time-of-flight mass spectrometry (TOF/MS) has been developed for the analysis of multi-constituent in Yinhuang granules, a well-known combined herbal remedy prepared from the extract mixtures of Flos Lonicerae and Radix Scutellariae. The fast HPLC analysis was performed on an Agilent ZorBax SB-C(18) column (4.6×50 mm, 1.8 μm) and 0.2% aqueous formic acid and acetonitrile was the optimum mobile phase for gradient elution in 17 min, which is five times faster than the performance of conventional columns packed with 5.0 μm particles. With various fragmentor voltages in TOF/MS, accurate mass measurements (<5 ppm error) for molecular ions and characteristic fragment ions represented reliable identification criteria for different constituents. A total of 28 compounds, including nine phenolic acids, three iridoid glycosides and nine saponins from Flos Lonicerae and seven flavonoids from Radix Scutellariae, were identified or tentatively characterized in the extract of Yinhuang granules. The established fast HPLC-DAD-TOF/MS method turns out to be useful and efficient for quality control of this commonly used Chinese herbal preparation. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fast targeted analysis of 132 acidic and neutral drugs and poisons in whole blood using LC-MS/MS.

PubMed

Di Rago, Matthew; Saar, Eva; Rodda, Luke N; Turfus, Sophie; Kotsos, Alex; Gerostamoulos, Dimitri; Drummer, Olaf H

2014-10-01

The aim of this study was to develop an LC-MS/MS based screening technique that covers a broad range of acidic and neutral drugs and poisons by combining a small sample volume and efficient extraction technique with simple automated data processing. After protein precipitation of 100μL of whole blood, 132 common acidic and neutral drugs and poisons including non-steroidal anti-inflammatory drugs, barbiturates, anticonvulsants, antidiabetics, muscle relaxants, diuretics and superwarfarin rodenticides (47 quantitated, 85 reported as detected) were separated using a Shimadzu Prominence HPLC system with a C18 separation column (Kinetex XB-C18, 4.6mm×150mm, 5μm), using gradient elution with a mobile phase of 25mM ammonium acetate buffer (pH 7.5)/acetonitrile. The drugs were detected using an ABSciex(®) API 2000 LC-MS/MS system (ESI+ and -, MRM mode, two transitions per analyte). The method was fully validated in accordance with international guidelines. Quantification data obtained using one-point calibration compared favorably to that using multiple calibrants. The presented LC-MS/MS assay has proven to be applicable for determination of the analytes in blood. The fast and reliable extraction method combined with automated processing gives the opportunity for high throughput and fast turnaround times for forensic and clinical toxicology. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Magnetic nanoparticles solid phase extraction for determination of ochratoxin A in cereals using high-performance liquid chromatography with fluorescence detection.

PubMed

Mashhadizadeh, Mohammad Hossein; Amoli-Diva, Mitra; Pourghazi, Kamyar

2013-12-13

A new, simple, fast, and environmental friendly sample preconcentration technique based on the modified Fe3O4 nanoparticles has been developed for extraction, and determination of ochratoxin A (OTA). Magnetic nanoparticles were coated with 3-(trimethoxysilyl)-1-propanethiol and modified by ethylene glycol bis-mercaptoacetate. Transmission electron microscopy, X-ray diffraction, and Fourier transform infrared spectrometry were used to characterize the adsorbents and the main parameters affecting the extraction and desorption efficiencies, such as pH of sample solution, sample volume, desorption conditions, extraction and desorption times, salt addition, and co-existing interferences have been investigated and established. Under optimal conditions, OTA was extracted and analyzed using high performance liquid chromatography with fluorescence detection. The mobile phase consists of acetonitrile:water:acetic acid (99:99:2, v/v/v) and fluorescence detection was performed with excitation and emission wavelengths at 333 and 477nm, respectively. An enrichment factor of 24 was achieved for OTA with relative standard deviation of <7%. The proposed method was applied to twenty samples of cereals (rice, wheat, and corn). The limits of detection of 0.06, 0.03, and 0.05ngmL(-1) and limits of quantitation of 0.19, 0.11, and 0.15ngmL(-1), were found for rice, wheat, and corn samples, respectively. The recoveries of OTA for spiked samples were ranged from 87 to 93%. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Simple and fast analysis of tetrabromobisphenol A, hexabromocyclododecane isomers, and polybrominated diphenyl ethers in serum using solid-phase extraction or QuEChERS extraction followed by tandem mass spectrometry coupled to HPLC and GC.

PubMed

Li, Jian; Chen, Tian; Wang, Yuwei; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei; Wang, Dejun; Wu, Yongning

2017-02-01

Two simplified sample preparation procedures for simultaneous extraction and clean-up of tetrabromobisphenol A, α-, β-, and γ-hexabromocyclododecane and polybrominated diphenyl ethers in human serum were developed and validated. The first procedure was based on solid-phase extraction. Sample extraction, purification, and lipid removal were carried out directly on an Oasis HLB cartridge. The second procedure was a quick, easy, cheap, effective, rugged, and safe-based approach using octadecyl-modified silica particles as a sorbent. After sample extraction and cleanup, tetrabromobisphenol A/hexabromocyclododecane was separated from polybrominated diphenyl ethers by using a Si-based cartridge. Tetrabromobisphenol A and hexabromocyclododecane were then detected by high-performance liquid chromatography coupled to tandem mass spectrometry, while polybrominated diphenyl ethers were detected by gas chromatography coupled to tandem mass spectrometry. The results of the spike recovery test using fetal bovine serum showed that the average recoveries of the analytes ranged from 87.3 to 115.3% with relative standard deviations equal to or lower than 13.4 %. Limits of detection of the analytes were in the range of 0.4-19 pg/mL except for decabromodiphenyl ether. The developed method was successfully applied to routine analysis of human serum samples from occupational workers and the general population. Extremely high serum polybrominated diphenyl ethers levels up to 3.32 × 10 4 ng/g lipid weight were found in occupational workers. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Temporal partitioning of adaptive responses of the murine heart to fasting.

PubMed

Brewer, Rachel A; Collins, Helen E; Berry, Ryan D; Brahma, Manoja K; Tirado, Brian A; Peliciari-Garcia, Rodrigo A; Stanley, Haley L; Wende, Adam R; Taegtmeyer, Heinrich; Rajasekaran, Namakkal Soorappan; Darley-Usmar, Victor; Zhang, Jianhua; Frank, Stuart J; Chatham, John C; Young, Martin E

2018-03-15

Recent studies suggest that the time of day at which food is consumed dramatically influences clinically-relevant cardiometabolic parameters (e.g., adiposity, insulin sensitivity, and cardiac function). Meal feeding benefits may be the result of daily periods of feeding and/or fasting, highlighting the need for improved understanding of the temporal adaptation of cardiometabolic tissues (e.g., heart) to fasting. Such studies may provide mechanistic insight regarding how time-of-day-dependent feeding/fasting cycles influence cardiac function. We hypothesized that fasting during the sleep period elicits beneficial adaptation of the heart at transcriptional, translational, and metabolic levels. To test this hypothesis, temporal adaptation was investigated in wild-type mice fasted for 24-h, or for either the 12-h light/sleep phase or the 12-h dark/awake phase. Fasting maximally induced fatty acid responsive genes (e.g., Pdk4) during the dark/active phase; transcriptional changes were mirrored at translational (e.g., PDK4) and metabolic flux (e.g., glucose/oleate oxidation) levels. Similarly, maximal repression of myocardial p-mTOR and protein synthesis rates occurred during the dark phase; both parameters remained elevated in the heart of fasted mice during the light phase. In contrast, markers of autophagy (e.g., LC3II) exhibited peak responses to fasting during the light phase. Collectively, these data show that responsiveness of the heart to fasting is temporally partitioned. Autophagy peaks during the light/sleep phase, while repression of glucose utilization and protein synthesis is maximized during the dark/active phase. We speculate that sleep phase fasting may benefit cardiac function through augmentation of protein/cellular constituent turnover. Copyright © 2018 Elsevier Inc. All rights reserved.

The difference between oats and beta-glucan extract intake in the management of HbA1c, fasting glucose and insulin sensitivity: a meta-analysis of randomized controlled trials.

PubMed

He, Li-xia; Zhao, Jian; Huang, Yuan-sheng; Li, Yong

2016-03-01

Increasing oats and beta-glucan extract intake has been associated with improved glycemic control, which is associated with the reduction in the development of diabetes. This study aims to assess the different effects between oat (whole and bran) and beta-glucan extract intake on glycemic control and insulin sensitivity. PubMed, Embase, Medline, The Cochrane Library, CINAHL and Web of Science were searched up to February 2014. We included randomized controlled trials with interventions that lasted at least four weeks that compared oats and beta-glucan (extracted from oats or other sources) intake with a control. A total of 1351 articles were screened for eligibility, and relevant data were extracted from 18 studies (n = 1024). Oat product dose ranged from 20 g d(-1) to 136 g d(-1), and beta-glucan extract dose ranged from 3 g d(-1) to 10 g d(-1). Compared with the control, oat intake resulted in a greater decrease in fasting glucose and insulin of subjects (P < 0.05), but beta-glucan extract intake did not. Furthermore, oat intake resulted in a greater decrease in glycosylated hemoglobin (HbA1c) (P < 0.001, I(2) = 0%) and fasting glucose (P < 0.001, I(2) = 68%) after removing one study using a concentrate and a different design and fasting insulin of type 2 diabetes (T2D) (P < 0.001, I(2) = 0%). The intake of oats and beta-glucan extracted from oats were effective in decreasing fasting glucose (P = 0.007, I(2) = 91%) and fasting insulin of T2D (P < 0.001, I(2) = 0%) and tented to lower HbA1c (P = 0.09, I(2) = 92%). Higher consumption of whole oats and oat bran, but not oat or barley beta-glucan extracts, are associated with lower HbA1c, fasting glucose and fasting insulin of T2D, hyperlipidaemic and overweight subjects, especially people with T2D, which supports the need for clinical trials to evaluate the potential role of oats in approaching to the management of glycemic control and insulin sensitivity of diabetes or metabolic syndrome subjects.

Kinematic principles of primate rotational vestibulo-ocular reflex. I. Spatial organization of fast phase velocity axes

NASA Technical Reports Server (NTRS)

Hess, B. J.; Angelaki, D. E.

1997-01-01

The spatial organization of fast phase velocity vectors of the vestibulo-ocular reflex (VOR) was studied in rhesus monkeys during yaw rotations about an earth-horizontal axis that changed continuously the orientation of the head relative to gravity ("barbecue spit" rotation). In addition to a velocity component parallel to the rotation axis, fast phases also exhibited a velocity component that invariably was oriented along the momentary direction of gravity. As the head rotated through supine and prone positions, torsional components of fast phase velocity axes became prominent. Similarly, as the head rotated through left and right ear-down positions, fast phase velocity axes exhibited prominent vertical components. The larger the speed of head rotation the greater the magnitude of this fast phase component, which was collinear with gravity. The main sequence properties of VOR fast phases were independent of head position. However, peak amplitude as well as peak velocity of fast phases were both modulated as a function of head orientation, exhibiting a minimum in prone position. The results suggest that the fast phases of vestibulo-ocular reflexes not only redirect gaze and reposition the eye in the direction of head motion but also reorient the eye with respect to earth-vertical when the head moves relative to gravity. As further elaborated in the companion paper, the underlying mechanism could be described as a dynamic, gravity-dependent modulation of the coordinates of ocular rotations relative to the head.

Effect of flash release treatment on phenolic extraction and wine composition.

PubMed

Morel-Salmi, Cécile; Souquet, Jean-Marc; Bes, Magali; Cheynier, Véronique

2006-06-14

The flash release (FR) process, consisting of rapidly heating the grapes and then applying strong vacuum, has been proposed to increase the polyphenol content of red wines. Its impact on polyphenol extraction kinetics and on the polyphenol composition of red juice and wines was studied over two seasons on different grape varieties (Grenache, Mourvedre, Carignan). The FR process allows fast extraction of all phenolic compounds (hydroxycinnamic acids, flavonols, anthocyanins, catechins, proanthocyanidins) and can be used to produce polyphenol-enriched grape juices. However, the concentration of all polyphenols dramatically decreased throughout fermentation when pressing was achieved immediately after FR. The FR wines made with pomace maceration were also enriched in polyphenols compared to the corresponding control wines. Increasing the duration of high-temperature exposure in the FR treatment further increased extraction of phenolic compounds but also accelerated their conversion to derived species. The tannin-to-anthocyanin ratio was particularly low in the wine fermented in the liquid phase, higher after FR than in the control, and even higher after longer heating. FR resulted in an increased tannin-to-anthocyanin ratio and an increased conversion of anthocyanins to tannin-anthocyanin adducts showing the same color properties as anthocyanins. The tannin-to-anthocyanin ratio was particularly low in the wine fermented in the liquid phase that also contained larger amounts of orange sulfite bleaching-resistant pigments.

Characterization of rice starch and protein obtained by a fast alkaline extraction method.

PubMed

Souza, Daiana de; Sbardelotto, Arthur Francisco; Ziegler, Denize Righetto; Marczak, Ligia Damasceno Ferreira; Tessaro, Isabel Cristina

2016-01-15

This study evaluated the characteristics of rice starch and protein obtained by a fast alkaline extraction method on rice flour (RF) derived from broken rice. The extraction was conducted using 0.18% NaOH at 30°C for 30min followed by centrifugation to separate the starch rich and the protein rich fractions. This fast extraction method allowed to obtain an isoelectric precipitation protein concentrate (IPPC) with 79% protein and a starchy product with low protein content. The amino acid content of IPPC was practically unchanged compared to the protein in RF. The proteins of the IPPC underwent denaturation during extraction and some of the starch suffered the cold gelatinization phenomenon, due to the alkaline treatment. With some modifications, the fast method can be interesting in a technological point of view as it enables process cost reduction and useful ingredients obtention to the food and chemical industries. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

Multi-scale imaging and elastic simulation of carbonates

NASA Astrophysics Data System (ADS)

Faisal, Titly Farhana; Awedalkarim, Ahmed; Jouini, Mohamed Soufiane; Jouiad, Mustapha; Chevalier, Sylvie; Sassi, Mohamed

2016-05-01

Digital Rock Physics (DRP) is an emerging technology that can be used to generate high quality, fast and cost effective special core analysis (SCAL) properties compared to conventional experimental techniques and modeling techniques. The primary workflow of DRP conssits of three elements: 1) image the rock sample using high resolution 3D scanning techniques (e.g. micro CT, FIB/SEM), 2) process and digitize the images by segmenting the pore and matrix phases 3) simulate the desired physical properties of the rocks such as elastic moduli and velocities of wave propagation. A Finite Element Method based algorithm, that discretizes the basic Hooke's Law equation of linear elasticity and solves it numerically using a fast conjugate gradient solver, developed by Garboczi and Day [1] is used for mechanical and elastic property simulations. This elastic algorithm works directly on the digital images by treating each pixel as an element. The images are assumed to have periodic constant-strain boundary condition. The bulk and shear moduli of the different phases are required inputs. For standard 1.5" diameter cores however the Micro-CT scanning reoslution (around 40 μm) does not reveal smaller micro- and nano- pores beyond the resolution. This results in an unresolved "microporous" phase, the moduli of which is uncertain. Knackstedt et al. [2] assigned effective elastic moduli to the microporous phase based on self-consistent theory (which gives good estimation of velocities for well cemented granular media). Jouini et al. [3] segmented the core plug CT scan image into three phases and assumed that micro porous phase is represented by a sub-extracted micro plug (which too was scanned using Micro-CT). Currently the elastic numerical simulations based on CT-images alone largely overpredict the bulk, shear and Young's modulus when compared to laboratory acoustic tests of the same rocks. For greater accuracy of numerical simulation prediction, better estimates of moduli inputs for this current unresolved phase is important. In this work we take a multi-scale imaging approach by first extracting a smaller 0.5" core and scanning at approx 13 µm, then further extracting a 5mm diameter core scanned at 5 μm. From this last scale, region of interests (containing unresolved areas) are identified for scanning at higher resolutions using Focalised Ion Beam (FIB/SEM) scanning technique reaching 50 nm resolution. Numerical simulation is run on such a small unresolved section to obtain a better estimate of the effective moduli which is then used as input for simulations performed using CT-images. Results are compared with expeirmental acoustic test moduli obtained also at two scales: 1.5" and 0.5" diameter cores.

An Effective Palmprint Recognition Approach for Visible and Multispectral Sensor Images.

PubMed

Gumaei, Abdu; Sammouda, Rachid; Al-Salman, Abdul Malik; Alsanad, Ahmed

2018-05-15

Among several palmprint feature extraction methods the HOG-based method is attractive and performs well against changes in illumination and shadowing of palmprint images. However, it still lacks the robustness to extract the palmprint features at different rotation angles. To solve this problem, this paper presents a hybrid feature extraction method, named HOG-SGF that combines the histogram of oriented gradients (HOG) with a steerable Gaussian filter (SGF) to develop an effective palmprint recognition approach. The approach starts by processing all palmprint images by David Zhang's method to segment only the region of interests. Next, we extracted palmprint features based on the hybrid HOG-SGF feature extraction method. Then, an optimized auto-encoder (AE) was utilized to reduce the dimensionality of the extracted features. Finally, a fast and robust regularized extreme learning machine (RELM) was applied for the classification task. In the evaluation phase of the proposed approach, a number of experiments were conducted on three publicly available palmprint databases, namely MS-PolyU of multispectral palmprint images and CASIA and Tongji of contactless palmprint images. Experimentally, the results reveal that the proposed approach outperforms the existing state-of-the-art approaches even when a small number of training samples are used.

Analysis of digital communication signals and extraction of parameters

NASA Astrophysics Data System (ADS)

Al-Jowder, Anwar

1994-12-01

The signal classification performance of four types of electronics support measure (ESM) communications detection systems is compared from the standpoint of the unintended receiver (interceptor). Typical digital communication signals considered include binary phase shift keying (BPSK), quadrature phase shift keying (QPSK), frequency shift keying (FSK), and on-off keying (OOK). The analysis emphasizes the use of available signal processing software. Detection methods compared include broadband energy detection, FFT-based narrowband energy detection, and two correlation methods which employ the fast Fourier transform (FFT). The correlation methods utilize modified time-frequency distributions, where one of these is based on the Wigner-Ville distribution (WVD). Gaussian white noise is added to the signal to simulate various signal-to-noise ratios (SNR's).

Effect of microstructure on the elasto-viscoplastic deformation of dual phase titanium structures

NASA Astrophysics Data System (ADS)

Ozturk, Tugce; Rollett, Anthony D.

2018-02-01

The present study is devoted to the creation of a process-structure-property database for dual phase titanium alloys, through a synthetic microstructure generation method and a mesh-free fast Fourier transform based micromechanical model that operates on a discretized image of the microstructure. A sensitivity analysis is performed as a precursor to determine the statistically representative volume element size for creating 3D synthetic microstructures based on additively manufactured Ti-6Al-4V characteristics, which are further modified to expand the database for features of interest, e.g., lath thickness. Sets of titanium hardening parameters are extracted from literature, and The relative effect of the chosen microstructural features is quantified through comparisons of average and local field distributions.

Optimization of large-volume injection for the determination of polychlorinated biphenyls in children's fast-food menus by low-resolution mass spectrometry.

PubMed

Esteve-Turrillas, Francesc A; Caupos, Emilie; Llorca, Isabel; Pastor, Agustín; de la Guardia, Miguel

2008-03-26

This study includes the determination of five indicator polychlorinated biphenyls (PCBs) (52, 101, 153, 138, and 180), six non-ortho PCBs (35, 80, 81, 77, 126, and 169), and two mono-ortho PCBs (28 and 118) in fast food for children. A freeze-dried sample of 10 g is extracted by using pressurized n-hexane in two 5 min cycles at 120 degrees C and 100 mbar. Fatty extracts were cleaned up by means of acetonitrile/n-hexane partitioning and gel-permeation chromatography. The fractionation of non-ortho, mono-ortho, and indicator PCBs was made on graphitized carbon solid-phase extraction cartridges by using n-hexane, n-hexane/toluene (99:1, v/v), and toluene as elution solvents. Gas chromatography coupled to tandem mass spectrometry and large-volume injections with a programmed-temperature vaporizer (PTV-LV) were used to increase sensitivity and selectivity of the PCB determination. The PTV-LV injection settings, that is, vaporizing temperature, vaporizing time, and purge flow, were optimized by using a central composite design. A 15-40 times increased sensitivity was reached as compared with that obtained with the conventional 1 microL splitless injection. The limits of detection achieved were between 0.3 and 1.2 pg/g, and repeatability data, as relative standard deviation varied, ranged from 2 to 9% for the 0.05 ng/mL PCB level.

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

PubMed

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

2015-11-04

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

The segmentation of bones in pelvic CT images based on extraction of key frames.

PubMed

Yu, Hui; Wang, Haijun; Shi, Yao; Xu, Ke; Yu, Xuyao; Cao, Yuzhen

2018-05-22

Bone segmentation is important in computed tomography (CT) imaging of the pelvis, which assists physicians in the early diagnosis of pelvic injury, in planning operations, and in evaluating the effects of surgical treatment. This study developed a new algorithm for the accurate, fast, and efficient segmentation of the pelvis. The proposed method consists of two main parts: the extraction of key frames and the segmentation of pelvic CT images. Key frames were extracted based on pixel difference, mutual information and normalized correlation coefficient. In the pelvis segmentation phase, skeleton extraction from CT images and a marker-based watershed algorithm were combined to segment the pelvis. To meet the requirements of clinical application, physician's judgment is needed. Therefore the proposed methodology is semi-automated. In this paper, 5 sets of CT data were used to test the overlapping area, and 15 CT images were used to determine the average deviation distance. The average overlapping area of the 5 sets was greater than 94%, and the minimum average deviation distance was approximately 0.58 pixels. In addition, the key frame extraction efficiency and the running time of the proposed method were evaluated on 20 sets of CT data. For each set, approximately 13% of the images were selected as key frames, and the average processing time was approximately 2 min (the time for manual marking was not included). The proposed method is able to achieve accurate, fast, and efficient segmentation of pelvic CT image sequences. Segmentation results not only provide an important reference for early diagnosis and decisions regarding surgical procedures, they also offer more accurate data for medical image registration, recognition and 3D reconstruction.

A simple and fast method based on mixed hemimicelles coated magnetite nanoparticles for simultaneous extraction of acidic and basic pollutants.

PubMed

Asgharinezhad, Ali Akbar; Ebrahimzadeh, Homeira

2016-01-01

One of the considerable and disputable areas in analytical chemistry is a single-step simultaneous extraction of acidic and basic pollutants. In this research, a simple and fast coextraction of acidic and basic pollutants (with different polarities) with the aid of magnetic dispersive micro-solid phase extraction based on mixed hemimicelles assembly was introduced for the first time. Cetyltrimethylammonium bromide (CTAB)-coated Fe3O4 nanoparticles as an efficient sorbent was successfully applied to adsorb 4-nitrophenol and 4-chlorophenol as two acidic and chlorinated aromatic amines as basic model compounds. Using a central composite design methodology combined with desirability function approach, the optimal experimental conditions were evaluated. The opted conditions were pH = 10; concentration of CTAB = 0.86 mmol L(-1); sorbent amount = 55.5 mg; sorption time = 11.0 min; no salt addition to the sample, type, and volume of the eluent = 120 μL methanol containing 5% acetic acid and 0.01 mol L(-1) HCl; and elution time = 1.0 min. Under the optimum conditions, detection limits and linear dynamic ranges were achieved in the range of 0.05-0.1 and 0.25-500 μg L(-1), respectively. The percent of extraction recoveries and relative standard deviations (n = 5) were in the range of 71.4-98.0 and 4.5-6.5, respectively. The performance of the optimized method was certified by coextraction of other acidic and basic compounds. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of the target analytes in various water samples, and satisfactory results were obtained.

Preparation of an exponentially rising optical pulse for efficient excitation of single atoms in free space.

PubMed

Dao, Hoang Lan; Aljunid, Syed Abdullah; Maslennikov, Gleb; Kurtsiefer, Christian

2012-08-01

We report on a simple method to prepare optical pulses with exponentially rising envelope on the time scale of a few ns. The scheme is based on the exponential transfer function of a fast transistor, which generates an exponentially rising envelope that is transferred first on a radio frequency carrier, and then on a coherent cw laser beam with an electro-optical phase modulator. The temporally shaped sideband is then extracted with an optical resonator and can be used to efficiently excite a single (87)Rb atom.

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

PubMed

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

2001-05-07

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

Core-shell Fe3O4 polydopamine nanoparticles as sorbent for magnetic dispersive solid-phase extraction of copper from food samples.

PubMed

Yavuz, Emre; Tokalıoğlu, Şerife; Patat, Şaban

2018-10-15

In the present study, core-shell Fe 3 O 4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L -1 HNO 3 .The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L -1 , respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g -1 , respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid-phase dispersion extraction of bioactive flavonoids from toothpaste, plant, and saliva.

PubMed

Cao, Wan; Cao, Jun; Ye, Li-Hong; Xu, Jing-Jing; Hu, Shuai-Shuai; Peng, Li-Qing

2015-12-01

This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a fast screening and confirmatory method by liquid chromatography-quadrupole-time-of-flight mass spectrometry for glucuronide-conjugated methyltestosterone metabolite in tilapia.

PubMed

Amarasinghe, Kande; Chu, Pak-Sin; Evans, Eric; Reimschuessel, Renate; Hasbrouck, Nicholas; Jayasuriya, Hiranthi

2012-05-23

This paper describes the development of a fast method to screen and confirm methyltestosterone 17-O-glucuronide (MT-glu) in tilapia bile. The method consists of solid-phase extraction (SPE) followed by high-performance liquid chromatography-mass spectrometry. The system used was an Agilent 6530 Q-TOF with an Agilent Jet stream electrospray ionization interface. The glucuronide detected in the bile was characterized as MT-glu by comparison with a chemically synthesized standard. MT-glu was detected in bile for up to 7 days after dosing. Semiquantification was done with matrix-matched calibration curves, because MT-glu showed signal suppression due to matrix effects. This method provides a suitable tool to monitor the illegal use of methyltestosterone in tilapia culture.

A method for fast automated microscope image stitching.

PubMed

Yang, Fan; Deng, Zhen-Sheng; Fan, Qiu-Hong

2013-05-01

Image stitching is an important technology to produce a panorama or larger image by combining several images with overlapped areas. In many biomedical researches, image stitching is highly desirable to acquire a panoramic image which represents large areas of certain structures or whole sections, while retaining microscopic resolution. In this study, we develop a fast normal light microscope image stitching algorithm based on feature extraction. At first, an algorithm of scale-space reconstruction of speeded-up robust features (SURF) was proposed to extract features from the images to be stitched with a short time and higher repeatability. Then, the histogram equalization (HE) method was employed to preprocess the images to enhance their contrast for extracting more features. Thirdly, the rough overlapping zones of the images preprocessed were calculated by phase correlation, and the improved SURF was used to extract the image features in the rough overlapping areas. Fourthly, the features were corresponded by matching algorithm and the transformation parameters were estimated, then the images were blended seamlessly. Finally, this procedure was applied to stitch normal light microscope images to verify its validity. Our experimental results demonstrate that the improved SURF algorithm is very robust to viewpoint, illumination, blur, rotation and zoom of the images and our method is able to stitch microscope images automatically with high precision and high speed. Also, the method proposed in this paper is applicable to registration and stitching of common images as well as stitching the microscope images in the field of virtual microscope for the purpose of observing, exchanging, saving, and establishing a database of microscope images. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simultaneous determination of ethyl carbamate and 4-(5-)methylimidazole in yellow rice wine and soy sauce by gas chromatography with mass spectrometry.

PubMed

Wu, Pinggu; Zhang, Liqun; Wang, Liyuan; Zhang, Jing; Tan, Ying; Tang, Jun; Ma, Bingjie; Pan, Xiaodong; Jiang, Wei

2014-08-01

We developed a new method, based on alkaline diatomite solid-phase extraction followed by gas chromatography with mass spectrometry, for the simultaneous determination of the toxic contaminants ethyl carbamate (EC) and 4-(5-)methylimidazole (4-MEI) in yellow rice wine and soy sauce. The optimal extraction conditions were defined. With the application of alkaline diatomite solid-phase extraction, damage to the capillary column by organic acids was greatly reduced. With deuterated EC used as the internal standard, the linearity of the calibration curves for EC and 4-MEI was good with correlation coefficient above 0.99. In a spiked experiment with EC and 4-MEI in yellow rice wine and soy sauce, recovery of the added EC was 80.5-102.5% and that of 4-MEI was 78.3-92.8%. The limit of quantification and limit of detection for EC were 6.0 and 2.0 μg/kg, respectively, and for 4-MEI were 15.0 and 5.0 μg/kg, respectively. The validation results demonstrate that the method is fast, simple, and selective, and therefore is suitable for simultaneously determining the presence of EC and 4-MEI in fermented food. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2005-11-01

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

Fast chemical and isotopic exchange of nitrogen during reaction with hot molybdenum

NASA Astrophysics Data System (ADS)

Yokochi, Reika; Marty, Bernard

2006-07-01

Molybdenum crucibles are commonly used to extract nitrogen from geological samples by induction heating. Because nitrogen is known to be reactive with certain metals (e.g., Ti and Fe), we have tested the reactivity of gaseous nitrogen with a Mo crucible held at 1800°C. The consumption of nitrogen, determined by monitoring the N2/40Ar ratio of the gas phase, varied between 25 and 100%, depending on the reaction duration. Nitrogen of the reacted gas was found to be systematically enriched in 15N relative to 14N by 10‰ compared to the initial isotopic composition, without any correlation with nitrogen consumption. We propose that a rapid isotopic exchange occurs between nitrogen originally trapped in the crucible and nitrogen from the gas phase, which modifies the isotopic composition of the reacted gas. This process can significantly bias the isotopic determination of nitrogen in rocks and minerals when a Mo furnace is used for gas extraction. Meanwhile, the rate of N-Mo chemical bonding may be controlled by the formation of nitride (rather than solid solution), a process slower than the isotopic exchange. The use of a Mo furnace for the extraction of trace nitrogen from rocks and minerals should therefore be avoided.

Determination of perfluorinated carboxylic acids in fish fillet by micro-solid phase extraction, followed by liquid chromatography-triple quadrupole mass spectrometry.

PubMed

Lashgari, Maryam; Lee, Hian Kee

2014-11-21

In the current study, a simple, fast and efficient combination of protein precipitation and micro-solid phase extraction (μ-SPE) followed by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) was developed for the determination of perfluorinated carboxylic acids (PFCAs) in fish fillet. Ten PFCAs with different hydrocarbon chain lengths (C5-C14) were analysed simultaneously using this method. Protein precipitation by acetonitrile and μ-SPE by surfactant-incorporated ordered mesoporous silica were applied to the extraction and concentration of the PFCAs as well as for removal of interferences. Determination of the PFCAs was carried out by LC-MS/MS in negative electrospray ionization mode. MS/MS parameters were optimized for multiple reaction monitoring of the analytes. (13)C mass labelled PFOA as a stable-isotopic internal standard, was used for calibration. The detection limits of the method ranged from 0.97 ng/g to 2.7 ng/g, with a relative standard deviation of between 5.4 and 13.5. The recoveries were evaluated for each analyte and were ranged from 77% to 120%. The t-test at 95% confidence level showed that for all the analytes, the relative recoveries did not depend on their concentrations in the explored concentration range. The effect of the matrix on MS signals (suppression or enhancement) was also evaluated. Contamination at low levels was detected for some analytes in the fish samples. The protective role of the polypropylene membrane used in μ-SPE in the elimination of matrix effects was evaluated by parallel experiments in classical dispersive solid phase extraction. The results evidently showed that the polypropylene membrane was significantly effective in reducing matrix effects. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid monitoring of residual UV-stabilizers in seawater samples from beaches using fabric phase sorptive extraction and UHPLC-MS/MS.

PubMed

García-Guerra, Romualdo B; Montesdeoca-Esponda, Sarah; Sosa-Ferrera, Zoraida; Kabir, Abuzar; Furton, Kenneth G; Santana-Rodríguez, José Juan

2016-12-01

Benzotriazole UV stabilizers (BUVSs) are a group of compounds added to personal care products such as sunscreens, hair dyes, make up formulations, soaps or shampoos, among others. Direct input from beaches or another aquatic recreational areas is the main source of BUVSs incorporation to the environment, where they can be mutagenic, toxic, pseudo-persistent and bioaccumulative. Due to the low levels of concentration of these compounds found in environmental samples, an extraction process is required prior to their determination. Fabric phase sorptive extraction integrates the advanced material properties of sol-gel hybrid inorganic-organic sorbents with flexible, permeable and functionally active fabric substrates, being a highly responsive, efficient and cheap device that also can be reused. In this paper, we applied fabric phase sorptive extraction methodology to analyse six BUVSs in twenty-four seawater samples from different coastal areas of Gran Canaria Island (Spain). It was coupled to ultra high performance liquid chromatography with tandem mass spectrometry in order to achieve a fast, reliable and sensitive separation and determination of the analytes from different simple matrices, regardless of its complexity and composition. Under the optimum conditions, the proposed method provided enrichment factors of 25 times with limits of detection from 1.06 to 8.96 ng L -1 and limits of quantification from 3.54 to 29.9 ng L -1 for the analytes under study in spiked samples. Intra and inter-day relative standard deviations were between 3.97 and 20.8% for all compounds. The application of the optimized methodology to non-spiked seawater samples allows detecting and quantifying the UV 360 in the range from 41.12 to 544.9 ng L -1 . Copyright © 2016 Elsevier Ltd. All rights reserved.

An optical Fourier transform coprocessor with direct phase determination.

PubMed

Macfaden, Alexander J; Gordon, George S D; Wilkinson, Timothy D

2017-10-20

The Fourier transform is a ubiquitous mathematical operation which arises naturally in optics. We propose and demonstrate a practical method to optically evaluate a complex-to-complex discrete Fourier transform. By implementing the Fourier transform optically we can overcome the limiting O(nlogn) complexity of fast Fourier transform algorithms. Efficiently extracting the phase from the well-known optical Fourier transform is challenging. By appropriately decomposing the input and exploiting symmetries of the Fourier transform we are able to determine the phase directly from straightforward intensity measurements, creating an optical Fourier transform with O(n) apparent complexity. Performing larger optical Fourier transforms requires higher resolution spatial light modulators, but the execution time remains unchanged. This method could unlock the potential of the optical Fourier transform to permit 2D complex-to-complex discrete Fourier transforms with a performance that is currently untenable, with applications across information processing and computational physics.

Using colloidal silica as isolator, diverter and blocking agent for subsurface geological applications

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

Bourcier, William L.; Roberts, Sarah K.; Roberts, Jeffery J.

A system for blocking fast flow paths in geological formations includes preparing a solution of colloidal silica having a nonviscous phase and a solid gel phase. The solution of colloidal silica is injected into the geological formations while the solution of colloidal silica is in the nonviscous phase. The solution of colloidal silica is directed into the fast flow paths and reaches the solid gel phase in the fast flow paths thereby blocking flow of fluid in the fast paths.

Purification and characterization of antimicrobial peptides from fish isolate Carnobacterium maltaromaticum C2: Carnobacteriocin X and carnolysins A1 and A2.

PubMed

Tulini, Fabricio L; Lohans, Christopher T; Bordon, Karla C F; Zheng, Jing; Arantes, Eliane C; Vederas, John C; De Martinis, Elaine C P

2014-03-03

Carnobacterium maltaromaticum C2, isolated from Brazilian smoked fish (Surubim, Pseudoplatystoma sp.), was found to exert antimicrobial activity against Listeria monocytogenes, an important foodborne pathogen. In this study, the bacteriocins produced by C. maltaromaticum C2 were purified via an extraction with XAD-16 resin, a C18 solid phase extraction, followed by reversed-phase fast protein liquid chromatography. The purified active fractions were characterized using tandem mass spectrometry, permitting the identification of multiple bacteriocins. Carnobacteriocins BM1, B1, and a variant of carnobacteriocin B2 were all found, providing much of the antilisterial activity. Additionally, we herein report the first isolation of the previously predicted antimicrobial peptide carnobacteriocin X. Moreover, C. maltaromaticum C2 produces a novel two-component lantibiotic, termed carnolysin, homologous to enterococcal cytolysin. This lantibiotic is antimicrobially inactive when tested against the non-bacteriocinogenic strain C. maltaromaticum A9b-, likely requiring an additional proteolytic cleavage to reach maturity. Copyright © 2013 Elsevier B.V. All rights reserved.

New materials for solid-phase extraction and multiclass high-performance liquid chromatographic analysis of pesticides in grapes.

PubMed

Melo, Lucio F C; Collins, Carol H; Jardim, Isabel C S F

2004-04-02

Sample preparation procedures which included the use of new aminopropyl (NH2) and octadecyl (C18) solid-phase extraction (SPE) sorbents are proposed for the simultaneous multiclass determination of the fungicide benomyl and of the herbicides tebuthiuron, diuron, simazine, atrazine, and ametryn in grapes, using single wavelength high-performance liquid chromatography. Sorbent preparation uses a fast, easy, and effective procedure to obtain silica-based materials, made by depositing polysiloxanes on a silica support followed by thermal immobilization. Recovery results of the compounds, after elution from the SPE cartridges, indicate that the most efficient system employed silica loaded with 40% of an aminofunctional polydimethylsiloxane as sorbent, using dichloromethane:methanol (95:5, v/v) as eluent. Method validation, carried out in agreement with International Conference on Harmonization directives, was performed at three fortification levels (100, 200, and 1000 microg kg(-1)). Limits of detection and quantification show that the method developed can be used to detect the pesticides at concentrations below the maximum residue levels established by Codex Alimentarius, the US Environmental Protection Agency, the European Union, and Brazilian legislation.

Precursor Ion Scan Mode-Based Strategy for Fast Screening of Polyether Ionophores by Copper-Induced Gas-Phase Radical Fragmentation Reactions.

PubMed

Crevelin, Eduardo J; Possato, Bruna; Lopes, João L C; Lopes, Norberto P; Crotti, Antônio E M

2017-04-04

The potential of copper(II) to induce gas-phase fragmentation reactions in macrotetrolides, a class of polyether ionophores produced by Streptomyces species, was investigated by accurate-mass electrospray tandem mass spectrometry (ESI-MS/MS). Copper(II)/copper(I) transition directly induced production of diagnostic acylium ions with m/z 199, 185, 181, and 167 from α-cleavages of [macrotetrolides + Cu] 2+ . A UPLC-ESI-MS/MS methodology based on the precursor ion scan of these acylium ions was developed and successfully used to identify isodinactin (1), trinactin (2), and tetranactin (3) in a crude extract of Streptomyces sp. AMC 23 in the precursor ion scan mode. In addition, copper(II) was also used to induce radical fragmentation reactions in the carboxylic acid polyether ionophore nigericin. The resulting product ions with m/z 755 and 585 helped to identify nigericin in a crude extract of Streptomyces sp. Eucal-26 by means of precursor ion scan experiments, demonstrating that copper-induced fragmentation reactions can potentially identify different classes of polyether ionophores rapidly and selectively.

Poly(styrene-co-N-methacryloyl-l-phenylalanine methyl ester)-functionalized magnetic nanoparticles as sorbents for the analysis of sodium benzoate in beverages.

PubMed

Ji, Shilei; Li, Nan; Qi, Li; Wang, Minglin

2017-01-01

In this study, poly(styrene-co-N-methacryloyl-l-phenylalanine methyl ester)-functionalized magnetic nanoparticles were constructed and used as magnetic solid-phase extraction sorbents for analysis of food preservatives in beverages. To prepare the poly(amino acid)-based sorbents, N-methacryloyl-l-phenylalanine methyl ester, and styrene served as the functional monomers and modified onto the magnetic nanoparticles via free radical polymerization. Interestingly, compared with propylparaben and potassium sorbate, the proposed poly(amino acid)-based sorbents showed a good selectivity to sodium benzoate. The adsorption capacity of the sorbents to sodium benzoate was 6.08 ± 0.31 mg/g. Moreover, the fast adsorption equilibrium could be reached within 5 min. Further, the resultant poly(amino acid)-based sorbents were applied in the analysis of sodium benzoate in real beverage samples. The results proved that the proposed magnetic solid-phase extraction sorbents have a great potential for the analysis of preservatives in food samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Characteristic fingerprint analysis and determination of main components on Andrographis paniculata extract by UPLC].

PubMed

Zhang, Hui-ye; Xu, Xiao-fei; Huang, Yong; Wamg, De-qin; Deng, Qiao-hua

2014-06-01

To establish an analytical method for characteristic fingerprint and determination of main components of Andrographis paniculata Extract by UPLC. The chromatographic conditions were Waters ACQUITY UPLC BEH-C18 (2. 1 mm x 0 mm,1.7 μm)by gradient elute using acetonitrile-water as mobile phase(0 -2 min,20% ~ 25% A;2 ~ 5 min,25% ~ 35% A;5 ~ 7 min,35% A;7 ~10 min,35%~ 55% A) at a flow rate of 0. 5 min/mL,detecting wavelength at 220 nm. Results:Contents of the andrographolide, neoandrographolide, 14-deoxyandrographolide and 14-deoxy-l11,12-didehydroandrographolide had good resolution with the correlation coefficients exceed 0. 9999 and the average percent recovery lied in 97. 2% to 103.9%, RSD was less than 3.0% (n = 6). The chromatograms of Andrographis paniculata Extract shared seven common peaks in which four of them were recognized by reference standard with the similarities over 0. 9. It is a fast,accurate and validated method,and can be useful in quality evaluations of Andrographis paniculata Extract.

Dithizone modified magnetic nanoparticles for fast and selective solid phase extraction of trace elements in environmental and biological samples prior to their determination by ICP-OES.

PubMed

Cheng, Guihong; He, Man; Peng, Hanyong; Hu, Bin

2012-01-15

A fast and simple method for analysis of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II) in environmental and biological samples was developed by combining magnetic solid phase extraction (MSPE) with inductively coupled plasma-optical emission spectrometry (ICP-OES) detection. Dithizone modified silica-coated magnetic Fe(3)O(4) nanoparticles (H(2)Dz-SCMNPs) were prepared and used for MSPE of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II). The prepared magnetic nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The factors affecting the extraction of the target metal ions such as pH, sample volume, eluent, and interfering ions had been investigated and the adsorption mechanism of the target metals on the self-prepared H(2)Dz-SCMNPs was investigated by FT-IR and X-ray photo electron spectroscopy (XPS). Under the optimized conditions, the detection limits of the developed method for Cr(III), Cu(II), Pb(II) and Zn(II) were 35, 11, 62, and 8ngL(-1), respectively, with the enrichment factor of 100. The relative standard deviations (RSDs, c=10μgL(-1), n=7) were in the range of 1.7-3.1% and the linear range was 0.1-100μgL(-1). The proposed method had been validated by two certified reference materials (GSBZ50009-88 environmental water and GBW07601 human hair), and the determined values were in good agreement with the certified values. The method was also applied for the determination of trace metals in real water and human hair samples with recoveries in the range of 85-110% for the spiked samples. The developed MSPE-ICP-OES method has the advantages of simplicity, rapidity, selectivity, high extraction efficiency and is suitable for the analysis of samples with large volume and complex matrix. Copyright © 2011 Elsevier B.V. All rights reserved.

Development of a fast LC-MS/MS assay for the determination of deferiprone in human plasma and application to pharmacokinetics.

PubMed

Song, Ta-Shu; Hsieh, Yow-Wen; Peng, Ching-Tien; Liu, Cheng-Hsiung; Chen, Tai-Lin; Hour, Mann-Jen

2012-12-01

A fast and accurate liquid chromatography/tandem mass spectrometric (LC-MS/MS) assay was first developed and validated for the determination of deferiprone in human plasma. The analytes were extracted with acetonitrile from only 50 μL aliquots of human plasma to achieve the protein precipitation. After extraction, chromatographic separation of analytes in human plasma was performed using a Synergi Fusion-RP 80A column at 30 °C. The mobile phase consisted of methanol and 0.2% formic acid containing 0.2 mM EDTA (60:40, v/v). The flow rate of the mobile phase was 0.8 mL/min. The total run time for each sample analysis was 4 min. Detection was performed using electrospray ionization in positive ion multiple reaction monitoring mode by monitoring the precursor-to-parent ion transitions m/z 140.1 → 53.1 for deferiprone and m/z 143.1 → 98.1 for internal standard. A linear range was established from 0.1 to 20 µg/mL. The limit of detection was determined as 0.05 µg/mL. The validated method was estimated for linearity, recovery, stability, precision and accuracy. Intraday and interday precisions were 4.3-5.5 and 4.6-7.3%, respectively. The recovery of deferiprone was in the range of 80.1-86.8%. The method was successfully applied to a pharmacokinetic study of deferiprone in six thalassemia patients. Copyright © 2012 John Wiley & Sons, Ltd.

High sensitivity phase retrieval method in grating-based x-ray phase contrast imaging

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

Wu, Zhao; Gao, Kun; Chen, Jian

2015-02-15

Purpose: Grating-based x-ray phase contrast imaging is considered as one of the most promising techniques for future medical imaging. Many different methods have been developed to retrieve phase signal, among which the phase stepping (PS) method is widely used. However, further practical implementations are hindered, due to its complex scanning mode and high radiation dose. In contrast, the reverse projection (RP) method is a novel fast and low dose extraction approach. In this contribution, the authors present a quantitative analysis of the noise properties of the refraction signals retrieved by the two methods and compare their sensitivities. Methods: Using themore » error propagation formula, the authors analyze theoretically the signal-to-noise ratios (SNRs) of the refraction images retrieved by the two methods. Then, the sensitivities of the two extraction methods are compared under an identical exposure dose. Numerical experiments are performed to validate the theoretical results and provide some quantitative insight. Results: The SNRs of the two methods are both dependent on the system parameters, but in different ways. Comparison between their sensitivities reveals that for the refraction signal, the RP method possesses a higher sensitivity, especially in the case of high visibility and/or at the edge of the object. Conclusions: Compared with the PS method, the RP method has a superior sensitivity and provides refraction images with a higher SNR. Therefore, one can obtain highly sensitive refraction images in grating-based phase contrast imaging. This is very important for future preclinical and clinical implementations.« less

Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

NASA Astrophysics Data System (ADS)

Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

2018-05-01

In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

Wind turbine extraction from high spatial resolution remote sensing images based on saliency detection

NASA Astrophysics Data System (ADS)

Chen, Jingbo; Yue, Anzhi; Wang, Chengyi; Huang, Qingqing; Chen, Jiansheng; Meng, Yu; He, Dongxu

2018-01-01

The wind turbine is a device that converts the wind's kinetic energy into electrical power. Accurate and automatic extraction of wind turbine is instructive for government departments to plan wind power plant projects. A hybrid and practical framework based on saliency detection for wind turbine extraction, using Google Earth image at spatial resolution of 1 m, is proposed. It can be viewed as a two-phase procedure: coarsely detection and fine extraction. In the first stage, we introduced a frequency-tuned saliency detection approach for initially detecting the area of interest of the wind turbines. This method exploited features of color and luminance, was simple to implement, and was computationally efficient. Taking into account the complexity of remote sensing images, in the second stage, we proposed a fast method for fine-tuning results in frequency domain and then extracted wind turbines from these salient objects by removing the irrelevant salient areas according to the special properties of the wind turbines. Experiments demonstrated that our approach consistently obtains higher precision and better recall rates. Our method was also compared with other techniques from the literature and proves that it is more applicable and robust.

Spectrophotometric determination of basic fuchsin from various water samples after vortex assisted solid phase extraction using reduced graphene oxide as an adsorbent.

PubMed

Tokalıoğlu, Şerife; Yavuz, Emre; Aslantaş, Ayşe; Şahan, Halil; Taşkın, Ferhat; Patat, Şaban

2015-01-01

In this study, a fast and simple vortex assisted solid phase extraction method was developed for the separation/preconcentration of basic fuchsin in various water samples. The determination of basic fuchsin was carried out at a wavelength of 554 nm by spectrophotometry. Reduced graphene oxide which was used as a solid phase extractor was synthesized and characterized by X-ray diffraction, scanning electron microscopy and the Brunauer, Emmett and Teller. The optimum conditions are as follows: pH 2, contact times for adsorption and elution of 30 s and 90 s, respectively, 10 mg adsorbent, and eluent (ethanol) volume of 1 mL. The effects of some interfering ions and dyes were investigated. The method was linear in the concentration range of 50-250 μg L(-1). The adsorption capacity was 34.1 mg g(-1). The preconcentration factor, limit of detection and precision (RSD, %) of the method were found to be 400, 0.07 μg L(-1) and 1.2%, respectively. The described method was validated by analyzing basic fuchsin spiked certified reference material (SPS-WW1 Batch 114-Wastewater) and spiked real water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish.

PubMed

Hertzog, Gabriel I; Soares, Karina L; Caldas, Sergiane S; Primel, Ednei G

2015-06-01

A procedure based on vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of 15 pharmaceuticals from fish samples with determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was validated. Florisil, C18, diatomaceous earth, chitin, and chitosan were evaluated as solid supports. Best results were obtained with 0.5 g of diatomaceous earth, 0.5 g of sodium sulfate, and 5 mL of methanol. Analytical recoveries ranged from 58 to 128 % with relative standard deviation (RSD) lower than 15 %. Limit of quantification (LOQ) values for the 15 compounds ranged from 5 to 1000 ng g(-1). The method under investigation has shown to be a simple and fast extraction tool with minimum instrumentation and low amount of reagent, resulting in method low cost. Besides, alternative materials, such as chitin and chitosan, which were applied to the dispersion step for the first time, were found to be interesting alternatives.

Fast determination of pyrethroid pesticides in tobacco by GC-MS-SIM coupled with modified QuEChERS sample preparation procedure.

PubMed

Gao, Yan; Sun, Ying; Jiang, Chunzhu; Yu, Xi; Wang, Yuanpeng; Zhang, Hanqi; Song, Daqian

2013-01-01

An analytical method was developed for the extraction and determination of pyrethroid pesticide residues in tobacco. The modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was applied for preparing samples. In this study, methyl cyanide (MeCN)-saturated salt aqueous was used as the two-phase extraction solvent for the first time, and a vortex shaker was used for the simultaneous shaking and concentration of the analytes. The effects of experimental parameters on extraction and clean-up efficiency were investigated and optimized. The analytes were determined by gas chromatography-mass spectrometry-selected ion monitoring (GC-MS-SIM). The obtained recoveries of the analytes at three different fortification levels were 76.85-114.1% and relative standard deviations (RSDs) were lower than 15.7%. The limits of quantification (LOQs) were from 1.28 to 26.6 μg kg(-1). This method was also applied to the analysis of actual commercial tobacco products and the analytical results were satisfactory.

Phenolic compounds containing/neutral fractions extract and products derived therefrom from fractionated fast-pyrolysis oils

DOEpatents

Chum, H.L.; Black, S.K.; Diebold, J.P.; Kreibich, R.E.

1993-06-29

A process is described for preparing phenol-formaldehyde novolak resins and molding compositions in which portions of the phenol normally contained in said resins are replaced by a phenol/neutral fractions extract obtained from fractionating fast-pyrolysis oils. The fractionation consists of a neutralization stage which can be carried out with aqueous solutions of bases or appropriate bases in the dry state, followed by solvent extraction with an organic solvent having at least a moderate solubility parameter and good hydrogen bonding capacity. Phenolic compounds-containing/neutral fractions extracts obtained by fractionating fast-pyrolysis oils from a lignocellulosic material, is such that the oil is initially in the pH range of 2-4, being neutralized with an aqueous bicarbonate base, and extracted into a solvent having a solubility parameter of approximately 8.4-9.11 [cal/cm[sup 3

Graphene oxide/Fe3O4 as sorbent for magnetic solid-phase extraction coupled with liquid chromatography to determine 2,4,6-trinitrotoluene in water samples.

PubMed

Costa Dos Reis, Luciana; Vidal, Lorena; Canals, Antonio

2017-04-01

A fast, simple, economical, and environmentally friendly magnetic solid-phase extraction (MSPE) procedure has been developed to preconcentrate 2,4,6-trinitrotoluene (TNT) from water samples prior to determination by liquid chromatography-UV-Vis employing graphene oxide/Fe 3 O 4 nanocomposite as sorbent. The nanocomposite synthesis was investigated, and the MSPE was optimized by a multivariate approach. The optimum MSPE conditions were 40 mg of nanocomposite, 10 min of vortex extraction, 1 mL of acetonitrile as eluent, and 6 min of desorption in an ultrasonic bath. Under the optimized experimental conditions, the method was evaluated to obtain a preconcentration factor of 153. The linearity of the method was studied from 1 to 100 μg L -1 (N = 5), obtaining a correlation coefficient of 0.994. The relative standard deviation and limit of detection were found to be 12% (n = 6, 10 μg L -1 ) and 0.3 μg L -1 , respectively. The applicability of the method was investigated, analyzing three types of water samples (i.e., reservoir and drinking water and effluent wastewater) and recovery values ranged between 87 and 120% (50 μg L -1 spiking level), showing that the matrix had a negligible effect upon extraction. Finally, the semiquantitative Eco-Scale metrics confirmed the greenness of the developed method.

A Rapid LC-HRMS Method for the Determination of Domoic Acid in Urine Using a Self-Assembly Pipette Tip Solid-Phase Extraction

PubMed Central

Zhang, Yiping; Chen, Dawei; Hong, Zhuan

2015-01-01

In this study, we developed a self-assembly pipette tip solid-phase extraction (PTSPE) method using a high molecular weight polymer material (PAX) as the adsorbent for the determination of domoic acid (DA) in human urine samples by liquid chromatography high-resolution mass spectrometry (LC-HRMS) analysis. The PTSPE cartridge, assembled by packing 9.1 mg of PAX as sorbent into a 200 μL pipette tip, showed high adsorption capacity for DA owing to the strong cationic properties of PAX. Compared with conventional SPE, the PTSPE is simple and fast, and shows some advantages in the aspects of less solvent consumption, low cost, the absence of the evaporation step, and short time requirement. All the parameters influencing the extraction efficiency such as pH, the amount of sorbent, the number of aspirating/dispensing cycles, and the type and volume of eluent in PTSPE were carefully investigated and optimized. Under the optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) values of DA were 0.12 μg/L and 0.37 μg/L respectively. The extraction recoveries of DA from the urine samples spiked at four different concentrations were in a range from 88.4% to 102.5%. The intra- and inter-day precisions varied from 2.1% to 7.6% and from 2.6% to 12.7%, respectively. The accuracy ranged from −1.9% to −7.4%. PMID:26729165

FAST TRACK COMMUNICATION: Freezing and extreme-value statistics in a random energy model with logarithmically correlated potential

NASA Astrophysics Data System (ADS)

Fyodorov, Yan V.; Bouchaud, Jean-Philippe

2008-09-01

We investigate some implications of the freezing scenario proposed by Carpentier and Le Doussal (CLD) for a random energy model (REM) with logarithmically correlated random potential. We introduce a particular (circular) variant of the model, and show that the integer moments of the partition function in the high-temperature phase are given by the well-known Dyson Coulomb gas integrals. The CLD freezing scenario allows one to use those moments for extracting the distribution of the free energy in both high- and low-temperature phases. In particular, it yields the full distribution of the minimal value in the potential sequence. This provides an explicit new class of extreme-value statistics for strongly correlated variables, manifestly different from the standard Gumbel class.

Bounded tracking for nonminimum phase nonlinear systems with fast zero dynamics

DOT National Transportation Integrated Search

1996-12-01

A PostScript file. In this paper, tracking control laws for nonminimum phase nonlinear systems with both fast and slow, possibly unstable, zero dynamics are derived. The fast zero dynamics arise from a perturbation of a nominal system. These fast zer...

Comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for analysis of toad skin.

PubMed

Li, Jia-Fu; Yan, Xia; Wu, Yun-Long; Fang, Mei-Juan; Wu, Zhen; Qiu, Ying-Kun

2017-04-15

An analytical two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was constructed with a newly developed thermal evaporation assisted adsorption (TEAA) interface. This novel TEAA interface with heating temperature above solvent boiling point allowed fast removal of organic NPLC solvent and successfully solved the solvent incompatibility problem between NPLC and RPLC. The system achieved rapid on-line solvent exchange between the two dimensions within a short modulation time of 190 s and was applied in the analysis of an extract from the skin of Bufo bufo gargarizans. This is the first time to realize the on-line comprehensive analysis of a moderate polar natural product by coupling NPLC with reversed phase ultra-high performance liquid chromatography (UHPLC). To be highlighted, with the TEAA interface, the 2D NPLC × RPLC system provided excellent resolution and orthogonality (75.2%), when compared with that of 2D RPLC × RPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

An Effective Palmprint Recognition Approach for Visible and Multispectral Sensor Images

PubMed Central

Sammouda, Rachid; Al-Salman, Abdul Malik; Alsanad, Ahmed

2018-01-01

Among several palmprint feature extraction methods the HOG-based method is attractive and performs well against changes in illumination and shadowing of palmprint images. However, it still lacks the robustness to extract the palmprint features at different rotation angles. To solve this problem, this paper presents a hybrid feature extraction method, named HOG-SGF that combines the histogram of oriented gradients (HOG) with a steerable Gaussian filter (SGF) to develop an effective palmprint recognition approach. The approach starts by processing all palmprint images by David Zhang’s method to segment only the region of interests. Next, we extracted palmprint features based on the hybrid HOG-SGF feature extraction method. Then, an optimized auto-encoder (AE) was utilized to reduce the dimensionality of the extracted features. Finally, a fast and robust regularized extreme learning machine (RELM) was applied for the classification task. In the evaluation phase of the proposed approach, a number of experiments were conducted on three publicly available palmprint databases, namely MS-PolyU of multispectral palmprint images and CASIA and Tongji of contactless palmprint images. Experimentally, the results reveal that the proposed approach outperforms the existing state-of-the-art approaches even when a small number of training samples are used. PMID:29762519

Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

PubMed

Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

2011-11-01

This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in biological or environmental samples. Due to low consumption of eluent (usually 0.3-1mL/run) mainly composed of water-alcohol binary mixtures, this method can be considered as environmentally friendly and green chemistry focused analytical tool, supplementary to analytical protocols involving column chromatography or planar micro-fluidic devices. Copyright © 2011 Elsevier Ltd. All rights reserved.

Silk fabric dyed with extract of sophora flower bud.

PubMed

Yan, Su; Pan, Shanshan; Ji, Junling

2018-02-01

This study analysed the use of sophora flower bud extract for dyeing and the resulting colour character and fastness of dyed silk fabric. The pigment composition on the silk fabric and recycling of this extract were also studied. The results indicated that the dyed silk fabric possessed good washing, rubbing and perspiration fastness, and the pigment composition on the silk fabric was mainly rutin and quercetin. The average recovery rate of the dye was 55.00%. These results demonstrate that the sophora flower bud extract is an effective natural dye.

Microstructural effects of Ramadan fasting on the brain: a diffusion tensor imaging study.

PubMed

Bakan, Ayse Ahsen; Yıldız, Seyma; Alkan, Alpay; Yetis, Huseyin; Kurtcan, Serpil; Ilhan, Mahmut Muzaffer

2015-01-01

We aimed to examine whether the brain displays any microstructural changes after a three-week Ramadan fasting period using diffusion tenson imaging. This study included a study and a control group of 25 volunteers each. In the study group, we examined and compared apparent diffusion coefficient (ADC) and fractional anisotropy (FA) values of the participants during (phase 1) and after (phase 2) a period of fasting. The control group included individuals who did not fast. ADC and FA values obtained in phase 1 and phase 2 were compared between the study and control groups. In the study group, ADC values of hypothalamus and, to a lesser extent, of insula were lower in phase 1 compared with phase 2 and the control group. The FA values of amygdala, middle temporal cortex, thalamus and, to a lesser extent, of medial prefrontal cortex were lower in phase 1 compared with phase 2 and the control group. Phase 2 ADC and FA values of the study group were not significantly different compared with the control group at any brain location. A three-week Ramadan fasting period can cause microstructural changes in the brain, and diffusion tensor imaging enables the visualization of these changes. The identification of brain locations where changes occurred in ADC and FA values during fasting can be helpful in diagnostic imaging and understanding the pathophysiology of eating disorders.

Microstructural effects of Ramadan fasting on the brain: a diffusion tensor imaging study

PubMed Central

Bakan, Ayse Ahsen; Yıldız, Seyma; Alkan, Alpay; Yetis, Huseyin; Kurtcan, Serpil; Ilhan, Mahmut Muzaffer

2015-01-01

PURPOSE We aimed to examine whether the brain displays any microstructural changes after a three-week Ramadan fasting period using diffusion tenson imaging. METHODS This study included a study and a control group of 25 volunteers each. In the study group, we examined and compared apparent diffusion coefficient (ADC) and fractional anisotropy (FA) values of the participants during (phase 1) and after (phase 2) a period of fasting. The control group included individuals who did not fast. ADC and FA values obtained in phase 1 and phase 2 were compared between the study and control groups. RESULTS In the study group, ADC values of hypothalamus and, to a lesser extent, of insula were lower in phase 1 compared with phase 2 and the control group. The FA values of amygdala, middle temporal cortex, thalamus and, to a lesser extent, of medial prefrontal cortex were lower in phase 1 compared with phase 2 and the control group. Phase 2 ADC and FA values of the study group were not significantly different compared with the control group at any brain location. CONCLUSION A three-week Ramadan fasting period can cause microstructural changes in the brain, and diffusion tensor imaging enables the visualization of these changes. The identification of brain locations where changes occurred in ADC and FA values during fasting can be helpful in diagnostic imaging and understanding the pathophysiology of eating disorders. PMID:25835077

Fast, safe, and reliable methods for extraction of major inorganic cations from small quantities of woody plant tissues

Treesearch

Rakesh Minocha; Walter C. Shortle

1993-01-01

Two simple and fast methods for the extraction of major inorganic cations (Ca, Mg, Mn, K) from small quantities of stemwood and needles of woody plants were developed. A 3.2- or 6.4-mm cobalt drill bit was used to shave samples from disks and increment cores of stemwood. For ion extraction, wood (ground or shavings) or needles were either homogenzied using a Tekmar...

Polyphenolic characterization and chromatographic methods for fast assessment of culinary Salvia species from South East Europe.

PubMed

Cvetkovikj, I; Stefkov, G; Acevska, J; Stanoeva, J Petreska; Karapandzova, M; Stefova, M; Dimitrovska, A; Kulevanova, S

2013-03-22

Although the knowledge and use of several Salvia species (Salvia officinalis, Salvia fruticosa, and Salvia pomifera) can be dated back to Greek Era and have a long history of culinary and effective medicinal use, still there is a remarkable interest concerning their chemistry and especially the polyphenolic composition. Despite the demand in the food and pharmaceutical industry for methods for fast quality assessment of the herbs and spices, even now there are no official requirements for the minimum content of polyphenols in sage covered by current regulations neither the European Pharmacopoeia monographs nor the ISO 11165 standard. In this work a rapid analytical method for extraction, characterization and quantification of the major polyphenolic constituents in Sage was developed. Various extractions (infusion - IE; ultrasound-assisted extraction - USE and microwave-assisted extraction - MWE) were performed and evaluated for their effectiveness. Along with the optimization of the mass-detector and chromatographic parameters, the applicability of three different reverse C18 stationary phases (extra-density bonded, core-shell technology and monolith column) for polyphenolics characterization was evaluated. A comprehensive overview of the very variable polyphenolic composition of 118 different plant samples of 68 populations of wild growing culinary Salvia species (S. officinalis: 101; S. fruticosa: 15; S. pomifera: 2) collected from South East Europe (SEE) was performed using HPLC-DAD-ESI-MS(n) and more than 50 different compounds were identified and quantified. With this work the knowledge about polyphenols of culinary Sage was expanded thus the possibility for gaining an insight into the chemodiversity of culinary Salvia species in South East Europe was unlocked. Copyright © 2013 Elsevier B.V. All rights reserved.

Distinguishing splanchnic nerve and chromaffin cell stimulation in mouse adrenal slices with fast-scan cyclic voltammetry

PubMed Central

Walsh, Paul L.; Petrovic, Jelena

2011-01-01

Electrical stimulation is an indispensible tool in studying electrically excitable tissues in neurobiology and neuroendocrinology. In this work, the consequences of high-intensity electrical stimulation on the release of catecholamines from adrenal gland slices were examined with fast-scan cyclic voltammetry at carbon fiber microelectrodes. A biphasic signal, consisting of a fast and slow phase, was observed when electrical stimulations typically used in tissue slices (10 Hz, 350 μA biphasic, 2.0 ms/phase pulse width) were applied to bipolar tungsten-stimulating electrodes. This signal was found to be stimulation dependent, and the slow phase of the signal was abolished when smaller (≤250 μA) and shorter (1 ms/phase) stimulations were used. The slow phase of the biphasic signal was found to be tetrodotoxin and hexamethonium independent, while the fast phase was greatly reduced using these pharmacological agents. Two different types of calcium responses were observed, where the fast phase was abolished by perfusion with a low-calcium buffer while both the fast and slow phases could be modulated when Ca2+ was completely excluded from the solution using EGTA. Perfusion with nifedipine resulted in the reduction of the slow catecholamine release to 29% of the original signal, while the fast phase was only decreased to 74% of predrug values. From these results, it was determined that high-intensity stimulations of the adrenal medulla result in depolarizing not only the splanchnic nerves, but also the chromaffin cells themselves resulting in a biphasic catecholamine release. PMID:21048165

Evaluation of mobile phase characteristics on three zwitterionic columns in hydrophilic interaction liquid chromatography mode for liquid chromatography-high resolution mass spectrometry based untargeted metabolite profiling of Leishmania parasites.

PubMed

Zhang, Rong; Watson, David G; Wang, Lijie; Westrop, Gareth D; Coombs, Graham H; Zhang, Tong

2014-10-03

It has been reported that HILIC column chemistry has a great effect on the number of detected metabolites in LC-HRMS-based untargeted metabolite profiling studies. However, no systematic investigation has been carried out with regard to the optimisation of mobile phase characteristics. In this study using 223 metabolite standards, we explored the retention mechanisms on three zwitterionic columns with varied mobile phase composition, demonstrated the interference from poor chromatographic peak shapes on the output of data extraction, and assessed the quality of chromatographic signals and the separation of isomers under each LC condition. As expected, on the ZIC-cHILIC column the acidic metabolites showed improved chromatographic performance at low pH which can be attributed to the opposite arrangement of the permanently charged groups on this column in comparison with the ZIC-HILIC column. Using extracts from the protozoan parasite Leishmania, we compared the numbers of repeatedly detected LC-HRMS features under different LC conditions with putative identification of metabolites not amongst the standards being based on accurate mass (±3ppm). Besides column chemistry, the pH of the mobile phase plays a key role in not only determining the retention mechanisms of solutes but also the output of the LC-HRMS data processing. Fast evaporation of ammonium carbonate produced less ion suppression in ESI source and consequently improved the detectability of the metabolites in low abundance in comparison with other ammonium salts. Our results show that the combination of a ZIC-pHILIC column with an ammonium carbonate mobile phase, pH 9.2, at 20mM in the aqueous phase or 10mM in both aqueous and organic mobile phase components, provided the most suitable LC conditions for LC-HRMS-based untargeted metabolite profiling of Leishmania parasite extracts. The signal reliability of the mass spectrometer used in this study (Exactive Orbitrap) was also investigated. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Metabolic profiles and bile acid extraction rate in the liver of cows with fasting-induced hepatic lipidosis.

PubMed

Mohamed, T; Oikawa, S; Iwasaki, Y; Mizunuma, Y; Takehana, K; Endoh, D; Kurosawa, T; Sato, H

2004-04-01

This study was designed to monitor lipid profile in the portal and hepatic blood of cows with fasting-induced hepatic lipidosis, and to compare the results with those in the jugular blood. The work was also carried out to investigate bile acid (BA) in these vessels, and further to investigate BA extraction rate in the liver. Five cows were equipped with catheters in the portal, hepatic and jugular veins (day 0), fasted for 4 days (day 1-day 4) and then refed (day 5-day 11). Before morning feeding, blood was sampled before, during and after fasting from the catheterized vessels. In the portal blood, the concentration of non-esterified fatty acids (NEFA) showed a progressive increase and at day 5 there was an approximate twofold rise. Increased NEFA concentrations were also found similarly in the other two veins. At day 5, beta-hydroxybutyrate (BHBA) in the portal, hepatic and jugular blood rose to 197, 190 and 186% of the pre-fasting value, respectively. However, the concentrations of NEFA and BHBA in the three veins gradually returned to pre-fasting concentration during the refeeding period. Compared with the pre-fasting value at day 0, the content of liver triglyceride (TG) increased significantly at day 5 (P < 0.01). In the liver, the hepatic extraction rate of BA dropped from 3.1 times pre-fasting to 2.2 times during fasting. There were no significant differences in the concentrations of glucose, TG, total cholesterol, cholesterol esters, free cholesterol and phospholipids. The results of the current study show that metabolic alterations occur in the portal, hepatic and jugular veins during induction of hepatic lipidosis in cows, and mostly metabolites, with exception of BA concentration, run parallel. The decreased BA extraction rate in the liver of fasted cows was considered to reflect hepatic cell impairment caused by TG accumulation. Hopefully, the findings, at least in part, contribute to the explanation of the pathophysiology of hepatic lipidosis in dairy cows.

Determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce by headspace derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry.

PubMed

Lee, Maw-Rong; Chiu, Tzu-Chun; Dou, Jianpeng

2007-05-22

This study proposes a method for identifying 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous matrices by using headspace on-fiber derivatization following solid-phase microextraction combined with gas chromatography-mass spectrometry. The optimized SPME experimental procedures for extracting 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous solutions involved a 85 microm polyacrylate-coated fiber at pH 6, a sodium chloride concentration of 0.36 g mL(-1), extraction at 50 degrees C for 15 min and desorption of analytes at 260 degrees C for 3 min. Headspace derivatization was conducted in a laboratory-made design with N-methyl-N-(trimethylsilyl)-trifluoroacetamide vapor following solid-phase microextraction by using 3 microL N-methyl-N-(trimethylsilyl)-trifluoroacetamide at an oil bath temperature of 230 degrees C for 40 s. This method had good repeatability (R.S.D.s < or = 19%, n = 8) and good linearity (r2 > or = 0.9972) for ultrapure water and soy sauce samples that were spiked with two analytes. Detection limits were obtained at the ng mL(-1). The result demonstrated that headspace on-fiber derivatization following solid-phase microextraction was a simple, fast and accurate technique for identifying trace 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce.

Ultrasonic real-time in-die monitoring of the tablet compaction process-a proof of concept study.

PubMed

Stephens, James D; Kowalczyk, Brian R; Hancock, Bruno C; Kaul, Goldi; Cetinkaya, Cetin

2013-02-14

The mechanical properties of a drug tablet can affect its performance (e.g., dissolution profile and its physical robustness. An ultrasonic system for real-time in-die tablet mechanical property monitoring during compaction has been demonstrated. The reported set-up is a proof of concept compaction monitoring system which includes an ultrasonic transducer mounted inside the upper punch of the compaction apparatus. This upper punch is utilized to acquire ultrasonic pressure wave phase velocity waveforms and extract the time-of-flight of pressure waves travelling within the compact at a number of compaction force levels during compaction. The reflection coefficients for the waves reflecting from punch tip-powder bed interface are extracted from the acquired waveforms. The reflection coefficient decreases with an increase in compaction force, indicating solidification. The data acquisition methods give an average apparent Young's moduli in the range of 8-20 GPa extracted during the compaction and release/decompression phases in real-time. A monitoring system employing such methods is capable of determining material properties and the integrity of the tablet during compaction. As compared to the millisecond time-scale dwell time of a typical commercial compaction press, the micro-second pulse duration and ToF of an acoustic pulse are sufficiently fast for real-time monitoring. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-03-01

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

Easy and Fast Method for the Determination of Biogenic Amines in Fish and Fish Products with Liquid Chromatography Coupled to Orbitrap Tandem Mass Spectrometry.

PubMed

Kaufmann, Anton; Maden, Kathryn

2018-03-01

A quantitative method for the determination of biogenic amines was developed. The method is characterized by the virtual absence of sample cleanup and does not require a derivatization reaction. Diluted extracts are centrifuged, filtrated, and directly injected into an ultra-HPLC column, which is coupled to a single-stage high-resolution mass spectrometer (Orbitrap). The chromatography is based on a reversed-phase column and an eluent containing an ion-pairing agent (heptafluorobutyric acid). The high sensitivity of the instrument permits the injection of very diluted extracts, which ensures stable retention times and the virtual absence of signal suppression effects. In addition, the quantification of histamine (a regulated compound) is further aided by the use of an isotopically labeled internal standard. The method was validated for three fish-based matrixes. Both the sample processing and the analytical measurement are very fast; hence, the methodology is ideal for high-throughput work. In addition, the method is significantly more selective than conventional methods (i.e., derivatization followed by LC with UV/fluorescence (FL) detection) for biogenic amines. A comparison showed that LC-UV/FL methods can produce false-positive findings due to coeluting matrix compounds.

Technical Note: Fast two-dimensional GC-MS with thermal extraction for anhydro-sugars in fine aerosols

EPA Science Inventory

A fast two-dimensional gas chromatography (GC-MS) method that uses heart-cutting and thermal extraction (TE) and requires no chemical derivatization is developed for the determination of anhydro-sugars in fine aerosols. Evaluation of the TE-GC-GC-MS method shows high average rela...

Determination of initiation of DNA replication before and after nuclear formation in Xenopus egg cell free extracts

PubMed Central

1993-01-01

Xenopus egg extracts prepared before and after egg activation retain M- and S-phase specific activity, respectively. Staurosporine, a potent inhibitor of protein kinase, converted M-phase extracts into interphase- like extracts that were capable of forming nuclei upon the addition of sperm DNA. The nuclei formed in the staurosporine treated M-phase extract were incapable of replicating DNA, and they were unable to initiate replication upon the addition of S-phase extracts. Furthermore, replication was inhibited when the staurosporine-treated M- phase extract was added in excess to the staurosporine-treated S-phase extract before the addition of DNA. The membrane-depleted S-phase extract supported neither nuclear formation nor replication; however, preincubation of sperm DNA with these extracts allowed them to form replication-competent nuclei upon the addition of excess staurosporine- treated M-phase extract. These results demonstrate that positive factors in the S-phase extracts determined the initiation of DNA replication before nuclear formation, although these factors were unable to initiate replication after nuclear formation. PMID:8253833

Green tea extract-induced lethal toxicity in fasted but not in nonfasted dogs.

PubMed

Wu, Kuei-Meng; Yao, Jiaqin; Boring, Daniel

2011-02-01

Recent chronic toxicity studies performed on green tea extracts in fasted dogs have revealed some unique dose-limiting lethal liver, gastrointestinal, and renal toxicities. Key findings included necrosis of hepatic cells, gastrointestinal epithelia and renal tubules, atrophy of reproductive organs, atrophy and necrosis of hematopoietic tissues, and associated hematological changes. The polyphenol cachetins (a mixture of primarily epigallocatechin gallate [≥55%]; plus up to 10% each of epigallocatechin, epicatechin, and epigallocatechin gallate) appeared to be the causative agents for the observed toxicities because they are the active ingredients of green tea extract studied. Conduct of the study in nonfasted dogs under the same testing conditions and dose levels showed unremarkable results. Assuming both studies were valid, at the identified no observed adverse effect levels (NOAEL) of each study, systemic exposures (based on area under the curve [AUC]) were actually lower in fasted than nonfasted dogs, suggesting that fasting may have rendered the target organ systems potentially more vulnerable to the effects of green tea extract. The toxicity mechanisms that produced lethality are not known, but the results are scientifically intriguing. Because tea drinking has become more popular in the United States and abroad, the mode of action and site of action of green tea extract-induced lethal toxicities during fasting and the role of other phytochemical components of Folia Camellia sinensis (including nonpolyphenol fractions, which are often consumed when whole-leaf products are presented) warrant further investigation.

Constraints on the lithosphere in and surrounding the Arctic basin from combined ambient noise and earthquake tomography

NASA Astrophysics Data System (ADS)

Krogh, J.; Dalton, C. A.; Ma, Z.

2017-12-01

Rayleigh wave dispersion extracted from ambient seismic noise has been widely used to image crustal and uppermost mantle structure in continents, but there have been relatively few studies within ocean basins. Here, we extract Rayleigh wave dispersion from ambient noise across the Arctic basin and surrounding continents. Continuous time series were collected from 427 broadband stations for the time period 1990-2016. Following the method described by Ma and Dalton (2017), we cross-correlated the noise records for 57,782 pairs of stations and measured phase arrival times for the frequency range 5-30 mHz. After data selection, which utilized criteria for path length, signal-to-noise ratio, and waveform quality, between 670 and 20,284 paths remained. Phase-velocity maps for the study region were determined from only the ambient noise Rayleigh waves and from a combined data set of ambient noise and earthquakes. Resolution tests and hit count maps illustrate the enhanced path coverage and resolution that is afforded by combining the two data sets. The maps show a clear association with tectonic features, including: fast velocities associated with the Siberian, Baltic, and North American cratons; very slow velocities associated with Iceland and the Alaska-Aleutian subduction zone; and an abrupt transition between the low-velocity North American Cordillera and fast-velocity craton that corresponds nearly perfectly with surface topography. The ultra-slow spreading Gakkel Ridge has only a weak seismic signature, although the dependence of seismic velocity on seafloor age is apparent in the maps. These results will be used to investigate the variations in temperature, composition, and melt and volatile content in the Arctic lithosphere and asthenosphere.

Quantitative multiresidue analysis of antibiotics in milk and milk powder by ultra-performance liquid chromatography coupled to tandem quadrupole mass spectrometry.

PubMed

Tian, He; Wang, Jiaqi; Zhang, Yangdong; Li, Songli; Jiang, Jindou; Tao, Dali; Zheng, Nan

2016-10-15

A simple and fast multiresidue extraction and purification method was developed for the determination of 61 veterinary drugs, belonging to seven classes, in milk and milk powder. The extraction depends on the acetonitrile solvent, followed by a single step to remove lipids with fatty acid chains using a new reversed phase SPE without traditional pre-equilibration and washing steps before eluting SPE. The purifying lipid effect of the present preparation method was evaluated by comparing the response changes of ion peak areas of the milk endogenous metabolites before and after SPE treatment using ultra-fast LC coupled to tandem quadrupole and TOF MS. Subsequently, UPLC coupled to tandem quadrupole MS was performed for the quantitative analysis of milk and milk powder samples spiked with 61 veterinary drugs, including β-lactam, macrolide, amide alcohol, forest amine, sulfanilamide, tetracyclines, and quinolones antibiotics. This method is very simple, fast, sensitive, and selective, and allows the good recoveries of all compounds, with a recovery range of 61.5-118.6%, and coefficients of variation of less than 11.6%. The 61 compounds behave in the dynamic range 0.01-200μgkg(-1), with correlation coefficient >0.99. The limits of quantification for the analytes are in the range 0.01-5.18μgkg(-1). Finally, this method has been successfully applied to the screening of veterinary drugs in 50 commercial bovine milk and milk powder samples, and ceftiofur and ciprofloxacin were detected in some brand samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Fast microwave-assisted extraction of rotenone for its quantification in seeds of yam bean (Pachyrhizus sp.).

PubMed

Lautié, Emmanuelle; Rasse, Catherine; Rozet, Eric; Mourgues, Claire; Vanhelleputte, Jean-Paul; Quetin-Leclercq, Joëlle

2013-02-01

The aim of this study was to find if fast microwave-assisted extraction could be an alternative to the conventional Soxhlet extraction for the quantification of rotenone in yam bean seeds by SPE and HPLC-UV. For this purpose, an experimental design was used to determine the optimal conditions of the microwave extraction. Then the values of the quantification on three accessions from two different species of yam bean seeds were compared using the two different kinds of extraction. A microwave extraction of 11 min at 55°C using methanol/dichloromethane (50:50) allowed rotenone extraction either equivalently or more efficiently than the 8-h-Soxhlet extraction method and was less sensitive to moisture content. The selectivity, precision, trueness, accuracy, and limit of quantification of the method with microwave extraction were also demonstrated. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fast and sensitive analysis of beta blockers by ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry.

PubMed

Tomková, Jana; Ondra, Peter; Kocianová, Eva; Václavík, Jan

2017-07-01

This paper presents a method for the determination of acebutolol, betaxolol, bisoprolol, metoprolol, nebivolol and sotalol in human serum by liquid-liquid extraction and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. After liquid-liquid extraction, beta blockers were separated on a reverse-phase analytical column (Acclaim RS 120; 100 × 2.1 mm, 2.2 μm). The total run time was 6 min for each sample. Linearity, limit of detection, limit of quantification, matrix effects, specificity, precision, accuracy, recovery and sample stability were evaluated. The method was successfully applied to the therapeutic drug monitoring of 108 patients with hypertension. This method was also used for determination of beta blockers in 33 intoxicated patients. Copyright © 2016 John Wiley & Sons, Ltd.

Fast Extraction and Detection of 4-Methylimidazole in Soy Sauce Using Magnetic Molecularly Imprinted Polymer by HPLC.

PubMed

Feng, Zufei; Lu, Yan; Zhao, Yingjuan; Ye, Helin

2017-11-02

On the basis of magnetic molecularly imprinted polymer (MMIP) solid-phase extraction coupled with high performance liquid chromatography, we established a new method for the determination of the 4-methylimidazole (4-MEI) in soy sauce. Scanning electron microscopy (SEM), Fourier transform infrared (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) were used to characterize the synthesized MMIPs. To evaluate the polymers, batch rebinding experiments were carried out. The binding strength and capacity were determined from the derived Freundlich isotherm (FI) equation. The selective recognition capability of MMIPs was investigated with a reference compound and a structurally similar compound. As a selective pre-concentration sorbents for 4-methylimidazole in soy sauce, the MMIPs showed a satisfied recoveries rate of spiked samples, ranged from 97% to 105%. As a result, the prepared MMIPs could be applied to selectively pre-concentrate and determine 4-methylimidazole in soy sauce samples.

Application of PLE for the determination of essential oil components from Thymus vulgaris L.

PubMed

Dawidowicz, Andrzej L; Rado, Ewelina; Wianowska, Dorota; Mardarowicz, Marek; Gawdzik, Jan

2008-08-15

Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed. Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation. According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants.

Determination of inorganic arsenic in algae using bromine halogenation and on-line nonpolar solid phase extraction followed by hydride generation atomic fluorescence spectrometry.

PubMed

Zhang, Weihong; Qi, Yuehan; Qin, Deyuan; Liu, Jixin; Mao, Xuefei; Chen, Guoying; Wei, Chao; Qian, Yongzhong

2017-08-01

Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydride generation atomic fluorescence spectrometry (HG-AFS). The separation of iAs from algae was first performed by nonpolar SPE sorbent using Br - for arsenic halogenation. Algae samples were extracted with 1% perchloric acid. Then, 1.5mL extract was reduced by 1% thiourea, and simultaneously reacted (for 30min) with 50μL of 10% KBr for converting iAs to AsBr 3 after adding 3.5mL of 70% HCl to 5mL. A polystyrene (PS) resin cartridge was employed to retain arsenicals, which were hydrolyzed, eluted from the PS resin with H 2 O, and categorized as iAs. The total iAs was quantified by HG-AFS. Under optimum conditions, the spiked recoveries of iAs in real algae samples were in the 82-96% range, and the method achieved a desirable limit of detection of 3μgkg -1 . The inter-day relative standard deviations were 4.5% and 4.1% for spiked 100 and 500μgkg -1 respectively, which proved acceptable for this method. For real algae samples analysis, the highest presence of iAs was found in sargassum fusiforme, followed by kelp, seaweed and laver. Copyright © 2017 Elsevier B.V. All rights reserved.

Magnetic solid-phase extraction of heterocyclic pesticides in environmental water samples using metal-organic frameworks coupled to high performance liquid chromatography determination.

PubMed

Ma, Jiping; Wu, Gege; Li, Shuang; Tan, Weiqiang; Wang, Xiaoyan; Li, Jinhua; Chen, Lingxin

2018-06-08

A simple method of magnetic solid-phase extraction (MSPE) coupled to high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of four kinds of heterocyclic pesticides (carbendazim, triadimefon, chlorfenapyr and fenpyroximate) in environmental water samples. Magnetic metal-organic frameworks (MOFs) of type MOF-5 were prepared and used as adsorbents of MSPE. Several main parameters influencing MSPE efficiency were investigated, including amount of magnetic MOF-5, sample solution pH, extraction time, salt concentration, type and volume of desorption solvents and desorption time. Under optimal conditions, the MSPE-HPLC method presented fast simple separation and analysis, and excellent linearity in the range of 0.3-500.0 μg/L for carbendazim and triadimefon, and 0.1-500.0 μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients (r) higher than 0.9992. High sensitivity with limits of detection and quantification ranging from 0.04-0.11 μg/L and 0.13-0.35 μg/L, respectively, were achieved, as well as good precision with relative standard deviations of 2.98-7.11% (intra-day) and 3.31-7.12% (inter-day). Furthermore, the method was successfully applied to reservoir and Yellow River water samples, and satisfactory recoveries at three spiked concentration levels were between 80.20% and 108.33%.The magnetic MOF-5 composites based MSPE followed by HPLC proved promising for convenient and efficient determination of heterocyclic pesticides in environmental water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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

2018-03-30

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

Profiling of polar metabolites in biological extracts using diamond hydride-based aqueous normal phase chromatography.

PubMed

Callahan, Damien L; De Souza, David; Bacic, Antony; Roessner, Ute

2009-07-01

Highly polar metabolites, such as sugars and most amino acids are not retained by conventional RP LC columns. Without sufficient retention low concentration compounds are not detected due ion suppression and structural isomers are not resolved. In contrast, hydrophilic interaction chromatography (HILIC) and aqueous normal phase chromatography (ANP) retain compounds based on their hydrophilicity and therefore provides a means of separating highly polar compounds. Here, an ANP method based on the diamond hydride stationary phase is presented for profiling biological small molecules by LC. A rapid separation system based upon a fast gradient that delivers reproducible chromatography is presented. Approximately 1000 compounds were reproducibly detected in human urine samples and clear differences between these samples were identified. This chromatography was also applied to xylem fluid from soyabean (Glycine max) plants to which 400 compounds were detected. This method greatly increases the metabolite coverage over RP-only metabolite profiling in biological samples. We show that both forms of chromatography are necessary for untargeted comprehensive metabolite profiling and that the diamond hydride stationary phase provides a good option for polar metabolite analysis.

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.

The phase-space dependence of fast-ion interaction with tearing modes

DOE PAGES

Heidbrink, William W.; Bardoczi, Laszlo; Collins, Cami S.; ...

2018-03-19

Modulation of various neutral beam sources probes the interaction of fast ions with tearing modes (TM) in the DIII-D tokamak. As measured by electron cyclotron emission, the (m,n) = (2,1) tearing modes have an island width of ~8 cm and change phase 180 at the q = 2 surface. (Here, m is the poloidal mode number and n is the toroidal mode number.) Deuterium neutral beam injection by six sources with differing injection geometries produces the fast ions. To study the interaction in different parts of phase space, on successive discharges, one of the six sources is modulated at 20more » Hz to populate different fast-ion orbits. The modulation only changes the island width by a few millimeters, implying that any fast-ion effect on mode stability is below detection limits. When compared to the expected signals in the absence of TM-induced transport, both the average and modulated neutron signals deviate, implying that fast-ion transport occurs in much of phase space. Fast-ion D-α (FIDA) measurements detect reductions in signal at wavelengths that are sensitive to counter-passing ions. Neutral particle analyzer data imply poor confinement of trapped fast ions. Lastly, calculations of the expected fast-ion transport that use measured TM properties successfully reproduce the data.« less

The phase-space dependence of fast-ion interaction with tearing modes

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

Heidbrink, William W.; Bardoczi, Laszlo; Collins, Cami S.

Modulation of various neutral beam sources probes the interaction of fast ions with tearing modes (TM) in the DIII-D tokamak. As measured by electron cyclotron emission, the (m,n) = (2,1) tearing modes have an island width of ~8 cm and change phase 180 at the q = 2 surface. (Here, m is the poloidal mode number and n is the toroidal mode number.) Deuterium neutral beam injection by six sources with differing injection geometries produces the fast ions. To study the interaction in different parts of phase space, on successive discharges, one of the six sources is modulated at 20more » Hz to populate different fast-ion orbits. The modulation only changes the island width by a few millimeters, implying that any fast-ion effect on mode stability is below detection limits. When compared to the expected signals in the absence of TM-induced transport, both the average and modulated neutron signals deviate, implying that fast-ion transport occurs in much of phase space. Fast-ion D-α (FIDA) measurements detect reductions in signal at wavelengths that are sensitive to counter-passing ions. Neutral particle analyzer data imply poor confinement of trapped fast ions. Lastly, calculations of the expected fast-ion transport that use measured TM properties successfully reproduce the data.« less

2D DOST based local phase pattern for face recognition

NASA Astrophysics Data System (ADS)

Moniruzzaman, Md.; Alam, Mohammad S.

2017-05-01

A new two dimensional (2-D) Discrete Orthogonal Stcokwell Transform (DOST) based Local Phase Pattern (LPP) technique has been proposed for efficient face recognition. The proposed technique uses 2-D DOST as preliminary preprocessing and local phase pattern to form robust feature signature which can effectively accommodate various 3D facial distortions and illumination variations. The S-transform, is an extension of the ideas of the continuous wavelet transform (CWT), is also known for its local spectral phase properties in time-frequency representation (TFR). It provides a frequency dependent resolution of the time-frequency space and absolutely referenced local phase information while maintaining a direct relationship with the Fourier spectrum which is unique in TFR. After utilizing 2-D Stransform as the preprocessing and build local phase pattern from extracted phase information yield fast and efficient technique for face recognition. The proposed technique shows better correlation discrimination compared to alternate pattern recognition techniques such as wavelet or Gabor based face recognition. The performance of the proposed method has been tested using the Yale and extended Yale facial database under different environments such as illumination variation and 3D changes in facial expressions. Test results show that the proposed technique yields better performance compared to alternate time-frequency representation (TFR) based face recognition techniques.

Iron dissolution kinetics of mineral dust at low pH during simulated atmospheric processing

NASA Astrophysics Data System (ADS)

Shi, Z.; Bonneville, S.; Krom, M. D.; Carslaw, K. S.; Jickells, T. D.; Baker, A. R.; Benning, L. G.

2010-11-01

We investigated the iron (Fe) dissolution kinetics of African (Tibesti) and Asian (Beijing) dust samples at acidic pH with the aim of reproducing the low pH conditions in atmospheric aerosols. The Beijing dust and three size fractions of the Tibesti dust (<20 μm: PM20; <10 μm: PM10; and <2.5 μm: PM2.5) were dissolved at pH 1, 2 and/or 3 for up to 1000 h. In the first 10 min, all dust samples underwent an extremely fast Fe solubilisation. Subsequently, the Fe dissolution proceeded at a much slower rate before reaching a stable dissolution plateau. The time-dependant Fe dissolution datasets were best described by a model comprising three acid-extractable Fe pools each dissolving according to first-order kinetics. The dissolution rate constant k of each pool was independent of the source (Saharan or Asian) and the size (PM20, PM10 or PM2.5) of the dust but highly dependent on pH. The "fast" Fe pool had a k (25 h-1 at pH=1) of a similar magnitude to "dry" ferrihydrite nanoparticles and/or poorly crystalline Fe(III) oxyhydroxide, while the "intermediate" and "slow" Fe pools had k values respectively 50-60 times and 3000-4000 times smaller than the "fast" pool. The "slow" Fe pool was likely to consist of both crystalline Fe oxide phases (i.e., goethite and/or hematite) and Fe contained in the clay minerals. The initial mass of the "fast", "intermediate" and "slow" Fe pools represented respectively about 0.5-2%, 1-3% and 15-40% of the total Fe in the dust samples. Furthermore, we showed that in systems with low dust/liquid ratios, Fe can be dissolved from all three phases, whereas at high dust/liquid ratios (e.g., in aerosols), sufficient Fe is solubilised from the "fast" phase to dominate the Fe dissolved and to suppress the dissolution of Fe from the other Fe pools. These data demonstrated that dust/liquid ratio and pH are fundamental parameters controlling Fe dissolution kinetics in the dust. In order to reduce errors in atmospheric and climate models, these fundamental controlling factors need to be included.

Fast analysis of curcuminoids from turmeric (Curcuma longa L.) by high-performance liquid chromatography using a fused-core column.

PubMed

Osorio-Tobón, J Felipe; Carvalho, Pedro I N; Barbero, Gerardo Fernández; Nogueira, Gislaine Chrystina; Rostagno, Mauricio Ariel; Meireles, Maria Angela de Almeida

2016-06-01

The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of a fast method for the analysis of main curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) present in extracts of turmeric (Curcuma longa L.). A step-by-step strategy was used to optimize temperature (40-55 °C), flow rate (1.0-2.5 mL min(-1)), mobile phase composition and equilibration time (1-5 min). A gradient method was developed using acidified water and acetonitrile combined with high column temperature (55 °C) and flow rate (2.5 mL min(-1)). Optimized conditions provided a method for the separation of these three curcuminoids in approximately 1.3 min with a total analysis time (sample-to-sample) of 7 min, including the clean-up and the re-equilibration of the column. Evaluation of chromatographic performance revealed excellent intraday and interday reproducibility (>99%), resolution (>2.23), selectivity (>1.12), peak symmetry (1.24-1.42) while presenting low limits of detection (<0.40 mg L(-1)) and quantification (<1.34 mg L(-1)). The robustness of the method was calculated according to the concentration/dilution of the sample and the injection volume. Several combinations of methanol and ethanol with water as sample solvents were evaluated and the best chromatographic results and extraction rate were obtained using 100% methanol. Finally, the developed method was validated with different extracts of turmeric rhizome and products that use turmeric in their formulation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Unusually high levels of bisphenol A (BPA) in thermal paper cash register receipts (CRs): development and application of a robust LC-UV method to quantify BPA in CRs.

PubMed

Babu, Sainath; Uppu, Sannihith N; Martin, Brittany; Agu, Ogad A; Uppu, Rao M

2015-01-01

We have developed a simple, reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of bisphenol A (BPA) in thermal paper cash register receipts (CRs). The method is suitable for analysis of other types of bisphenols and it involves an overnight extraction of CRs with acetonitrile (AN) at 50 °C followed by the HPLC analysis on a Supelcosil LC18 column (150 × 4.6 mm, particle size: 5 μ) using 50% AN in water as the mobile phase (5 min, isocratic). The composition of AN in the mobile phase changed to 100% over a 10 min period (linear gradient) and then held at 100% AN for 10 min (isocratic). The flow rate was set at 1 mL/min (injection volume: 20 μL) and the eluent was monitored at 234 nm. The authentic BPA eluted with a retention time of 5.9 min and gave a linear detector response in the concentration range of 0.23-50 mg/L. BPA in the CR extracts also eluted with the same retention and had identical absorbance properties as the standard. When CR extracts were co-injected with authentic BPA, they were resolved as a single peak. Further, GC/MS/EI analysis of authentic BPA and the HPLC-purified CR extracts have identical ion chromatograms and fragmentation of the molecular ion (m/z = 228). We have analyzed 170 CRs collected from 62 different vendors including supermarkets, fast food restaurants, gas stations and banking outlets. Almost all cash receipts (n = 168) showed the presence of BPA in the concentration range of 0.45-4.26% (M ± SD, 1.54 ± 0.73%).

Disposable pipette extraction for gas chromatographic determination of codeine, morphine, and 6-monoacetylmorphine in vitreous humor.

PubMed

Kovatsi, Leda; Rentifis, Konstantinos; Giannakis, Dimitrios; Njau, Samuel; Samanidou, Victoria

2011-07-01

The availability of a sensitive and rapid analytical method for the determination of opiates, and other substances of forensic interest, in a variety of biological specimens is of utmost importance to forensic laboratories. Solid-phase extraction is very popular in the pre-treatment of forensic samples. Nevertheless, a new approach, disposable pipette extraction (DPX), is gaining increasing interest in sample preparation. DPX has already been applied to the analysis of drugs of abuse in common biological matrices, such as urine and blood, but has not yet been evaluated on alternative biological samples, such as vitreous humor. The objective of this study was to evaluate the applicability of DPX on the analysis of opiates in vitreous humor. The currently developed method is fast, reliable, and easy to perform. The sensitivity, precision, and accuracy are satisfactory. Recoveries obtained are within the range of 72-91%, whereas the sample volume of vitreous humor required is only 100 μL. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-throughput screening for multi-class veterinary drug residues in animal muscle using liquid chromatography/tandem mass spectrometry with on-line solid-phase extraction.

PubMed

Tang, Hubert Po-On; Ho, Clare; Lai, Shirley Sau-Ling

2006-01-01

A rapid qualitative method using on-line column-switching liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed and validated for screening 13 target veterinary drugs: four macrolides - erythromycin A, josamycin (leucomycin A3), kitasamycin (leucomycin A5), and tylosin A; six (fluoro)quinolones - ciprofloxacin, danofloxacin, enrofloxacin, flumequine, oxolinic acid, and sarafloxacin; and lincomycin, virginiamycin M1, and trimethoprim in different animal muscles. Clindamycin, norfloxacin, nalidixic acid, oleandomycin, ormetoprim, and roxithromycin were used as the internal standards. After simple deproteination and analyte extraction of muscle samples using acetonitrile, the supernatant was subjected to on-line cleanup and direct analysis by LC/MS/MS. On-line cleanup with an extraction cartridge packed with hydrophilic-hydrophobic polymer sorbent followed by fast LC using a short C18 column resulted in a total analysis cycle of 6 min for 19 drugs. This screening method considerably reduced the time and the cost for the quantitative and confirmatory analyses. The application of a control point approach was also introduced and explained. Copyright (c) 2006 John Wiley & Sons, Ltd.

Fast determination of Ziziphora tenuior L. essential oil by inorganic-organic hybrid material based on ZnO nanoparticles anchored to a composite made from polythiophene and hexagonally ordered silica.

PubMed

Piryaei, Marzieh; Abolghasemi, Mir Mahdi; Nazemiyeh, Hossein

2015-01-01

In this paper, for the first time, an inorganic-organic hybrid material based on ZnO nanoparticles was anchored to a composite made from polythiophene and hexagonally ordered silica (ZnO/PT/SBA-15) for use in solid-phase fibre microextraction (SPME) of medicinal plants. A homemade SPME apparatus was used for the extraction of volatile components of Ziziphora tenuior L. A simplex method was used for optimisation of five different parameters affecting the efficiency of the extraction. The main constituents extracted by ZnO/PT/SBA-15 and PDMS fibres and hydrodistillation (HD) methods, respectively, included pulegone (51.25%, 53.64% and 56.68%), limonene (6.73%, 6.58% and 8.3%), caryophyllene oxide (5.33%, 4.31% and 4.53%) and 1,8-cineole (4.21%, 3.31% and 3.18%). In comparison with the HD method, the proposed technique could equally monitor almost all the components of the sample, in an easier way, in a shorter time and requiring a much lower amount of the sample.

Ultra-fast LC-ESI-MS/MS method for the simultaneous determination of six highly toxic Aconitum alkaloids from Aconiti kusnezoffii radix in rat plasma and its application to a pharmacokinetic study.

PubMed

Liu, Jingjing; Li, Qing; Yin, Yidi; Liu, Ran; Xu, Huarong; Bi, Kaishun

2014-01-01

A fast, sensitive, and efficient ultra-fast LC-ESI-MS/MS method was developed for the simultaneous quantitation of six highly toxic Aconitum alkaloids, that is, aconitine, mesaconitine, hypaconitine, benzoylaconine, benzoylmesaconine, and benzoylhypaconine, in rat plasma after oral administration of crude ethanol extracts from Aconiti kusnezoffii radix by ultrasonic extraction, reflux extraction for 1 h, and reflux extraction for 3 h, respectively. The separation of six Aconitum alkaloids and aminopyrine (internal standard) was performed on an InertSustain® C18 column, and the quantification of the analytes was performed on a 4000Q ultra-fast LC-MS/MS system with turbo ion spray source in the positive ion and multiple-reaction monitoring mode. Absolute recoveries ranged within 65.06-85.1% for plasma samples. The intra- and interday precision and accuracy of analytes were satisfactory. The methods were validated with sensitivity reaching the lower LOQ for aconitine, mesaconitine, hypaconitine, benzoylaconine, benzoylmesaconine, and benzoylhypaconine, which were 0.025, 0.025, 0.050, 0.025, 0.025, and 0.100 ng/mL, respectively. The method was successfully applied to a pharmacokinetic study of six Aconitum alkaloids in rat plasma after oral administration of crude ethanol extracts from the raw root of Aconitum kusnezoffii Reichb. by three different extraction processes. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Metal-organic framework MIL-101 as sorbent based on double-pumps controlled on-line solid-phase extraction coupled with high-performance liquid chromatography for the determination of flavonoids in environmental water samples.

PubMed

Liu, Yue; Hu, Jia; Li, Yan; Li, Xiao-Shuang; Wang, Zhong-Liang

2016-10-01

A novel method with high sensitivity for the rapid determination of chrysin, apigenin and luteolin in environment water samples was developed by double-pumps controlled on-line solid-phase extraction (SPE) coupled with high-performance liquid chromatography (HPLC). In the developed technique, metal organic framework MIL-101 was synthesized and applied as a sorbent for SPE. The as-synthesized MIL-101 was characterized by scanning electron microscope, X-ray diffraction spectrometry, thermal gravimetric analysis and micropore physisorption analysis. The MIL-101 behaved as a fast kinetics in the adsorption of chrysin, apigenin and luteolin. On-line SPE of chrysin, apigenin and luteolin was processed by loading a sample solution at a flow rate of 1.0 mL/min for 10 min. The extracted analytes were subsequently eluted into a ZORBAX Bonus-RP analytical column (25 cm long × 4.6 mm i.d.) for HPLC separation under isocratic condition with a mobile phase (MeOH: ACN: 0.02 M H 3 PO 4 = 35:35:30) at a flow rate of 1.0 mL/min. Experimental conditions, including ionic strength, sample pH, sample loading rates, sample loading time and desorption analytes time, were further optimized to obtain efficient preconcentration and high-precision determination of the analytes mentioned above. The method achieved the merits of simplicity, rapidity, sensitivity, wide linear range and high sample throughput. The possible mechanism for the adsorption of flavonoids on MIL-101 was proposed. The developed method has been applied to determine trace chrysin, apigenin and luteolin in a variety of environmental water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Advanced functional materials in solid phase extraction for ICP-MS determination of trace elements and their species - A review.

PubMed

He, Man; Huang, Lijin; Zhao, Bingshan; Chen, Beibei; Hu, Bin

2017-06-22

For the determination of trace elements and their species in various real samples by inductively coupled plasma mass spectrometry (ICP-MS), solid phase extraction (SPE) is a commonly used sample pretreatment technique to remove complex matrix, pre-concentrate target analytes and make the samples suitable for subsequent sample introduction and measurements. The sensitivity, selectivity/anti-interference ability, sample throughput and application potential of the methodology of SPE-ICP-MS are greatly dependent on SPE adsorbents. This article presents a general overview of the use of advanced functional materials (AFMs) in SPE for ICP-MS determination of trace elements and their species in the past decade. Herein the AFMs refer to the materials featuring with high adsorption capacity, good selectivity, fast adsorption/desorption dynamics and satisfying special requirements in real sample analysis, including nanometer-sized materials, porous materials, ion imprinting polymers, restricted access materials and magnetic materials. Carbon/silica/metal/metal oxide nanometer-sized adsorbents with high surface area and plenty of adsorption sites exhibit high adsorption capacity, and porous adsorbents would provide more adsorption sites and faster adsorption dynamics. The selectivity of the materials for target elements/species can be improved by using physical/chemical modification, ion imprinting and restricted accessed technique. Magnetic adsorbents in conventional batch operation offer unique magnetic response and high surface area-volume ratio which provide a very easy phase separation, greater extraction capacity and efficiency over conventional adsorbents, and chip-based magnetic SPE provides a versatile platform for special requirement (e.g. cell analysis). The performance of these adsorbents for the determination of trace elements and their species in different matrices by ICP-MS is discussed in detail, along with perspectives and possible challenges in the future development. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of Mars analogue soil samples using solid-phase microextraction, organic solvent extraction and gas chromatography/mass spectrometry

NASA Astrophysics Data System (ADS)

Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

2011-07-01

Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g-1. The texture of soils is mostly sandy loam with few samples being 100 % silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

NASA Technical Reports Server (NTRS)

Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

2011-01-01

Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

Employment of High-Performance Thin-Layer Chromatography for the Quantification of Oleuropein in Olive Leaves and the Selection of a Suitable Solvent System for Its Isolation with Centrifugal Partition Chromatography.

PubMed

Boka, Vasiliki-Ioanna; Argyropoulou, Aikaterini; Gikas, Evangelos; Angelis, Apostolis; Aligiannis, Nektarios; Skaltsounis, Alexios-Leandros

2015-11-01

A high-performance thin-layer chromatographic methodology was developed and validated for the isolation and quantitative determination of oleuropein in two extracts of Olea europaea leaves. OLE_A was a crude acetone extract, while OLE_AA was its defatted residue. Initially, high-performance thin-layer chromatography was employed for the purification process of oleuropein with fast centrifugal partition chromatography, replacing high-performance liquid-chromatography, in the stage of the determination of the distribution coefficient and the retention volume. A densitometric method was developed for the determination of the distribution coefficients, KC = CS/CM. The total concentrations of the target compound in the stationary phase (CS) and in the mobile phase (CM) were calculated by the area measured in the high-performance thin-layer chromatogram. The estimated Kc was also used for the calculation of the retention volume, VR, with a chromatographic retention equation. The obtained data were successfully applied for the purification of oleuropein and the experimental results confirmed the theoretical predictions, indicating that high-performance thin-layer chromatography could be an important counterpart in the phytochemical study of natural products. The isolated oleuropein (purity > 95%) was subsequently used for the estimation of its content in each extract with a simple, sensitive and accurate high-performance thin-layer chromatography method. The best fit calibration curve from 1.0 µg/track to 6.0 µg/track of oleuropein was polynomial and the quantification was achieved by UV detection at λ 240 nm. The method was validated giving rise to an efficient and high-throughput procedure, with the relative standard deviation % of repeatability and intermediate precision not exceeding 4.9% and accuracy between 92% and 98% (recovery rates). Moreover, the method was validated for robustness, limit of quantitation, and limit of detection. The amount of oleuropein for OLE_A, OLE_AA, and an aqueous extract of olive leaves was estimated to be 35.5% ± 2.7, 51.5% ± 1.4, and 12.5% ± 0.12, respectively. Statistical analysis proved that the method is repeatable and selective, and can be effectively applied for the estimation of oleuropein in olive leaves' extracts, and could potentially replace high-performance liquid chromatography methodologies developed so far. Thus, the phytochemical investigation of oleuropein could be based on high-performance thin-layer chromatography coupled with separation processes, such as fast centrifugal partition chromatography, showing efficacy and credibility. Georg Thieme Verlag KG Stuttgart · New York.

Electron transfer and atom exchange between aqueous Fe(II) and structural Fe(III) in clays. Role in U and Hg(II) transformations

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

Scherer, Michelle

2016-08-31

During this project, we investigated Fe electron transfer and atom exchange between aqueous Fe(II) and structural Fe(III) in clay minerals. We used selective chemical extractions, enriched Fe isotope tracer experiments, computational molecular modeling, and Mössbauer spectroscopy. Our findings indicate that structural Fe(III) in clay minerals is reduced by aqueous Fe(II) and that electron transfer occurs when Fe(II) is sorbed to either basal planes and edge OH-groups of clay mineral. Findings from highly enriched isotope experiments suggest that up to 30 % of the Fe atoms in the structure of some clay minerals exhanges with aqueous Fe(II). First principles calculations usingmore » a small polaron hopping approach suggest surprisingly fast electron mobility at room temperature in a nontronite clay mineral and are consistent with temperature dependent Mössbauer data Fast electron mobility suggests that electrons may be able to conduct through the mineral fast enough to enable exchange of Fe between the aqueous phase and clay mineral structure. over the time periods we observed. Our findings suggest that Fe in clay minerals is not as stable as previously thought.« less

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

PubMed

Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax

2015-07-01

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

Validation of an automated solid-phase extraction method for the analysis of 23 opioids, cocaine, and metabolites in urine with ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Ramírez Fernández, María del Mar; Van Durme, Filip; Wille, Sarah M R; di Fazio, Vincent; Kummer, Natalie; Samyn, Nele

2014-06-01

The aim of this work was to automate a sample preparation procedure extracting morphine, hydromorphone, oxymorphone, norcodeine, codeine, dihydrocodeine, oxycodone, 6-monoacetyl-morphine, hydrocodone, ethylmorphine, benzoylecgonine, cocaine, cocaethylene, tramadol, meperidine, pentazocine, fentanyl, norfentanyl, buprenorphine, norbuprenorphine, propoxyphene, methadone and 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine from urine samples. Samples were extracted by solid-phase extraction (SPE) with cation exchange cartridges using a TECAN Freedom Evo 100 base robotic system, including a hydrolysis step previous extraction when required. Block modules were carefully selected in order to use the same consumable material as in manual procedures to reduce cost and/or manual sample transfers. Moreover, the present configuration included pressure monitoring pipetting increasing pipetting accuracy and detecting sampling errors. The compounds were then separated in a chromatographic run of 9 min using a BEH Phenyl analytical column on a ultra-performance liquid chromatography-tandem mass spectrometry system. Optimization of the SPE was performed with different wash conditions and elution solvents. Intra- and inter-day relative standard deviations (RSDs) were within ±15% and bias was within ±15% for most of the compounds. Recovery was >69% (RSD < 11%) and matrix effects ranged from 1 to 26% when compensated with the internal standard. The limits of quantification ranged from 3 to 25 ng/mL depending on the compound. No cross-contamination in the automated SPE system was observed. The extracted samples were stable for 72 h in the autosampler (4°C). This method was applied to authentic samples (from forensic and toxicology cases) and to proficiency testing schemes containing cocaine, heroin, buprenorphine and methadone, offering fast and reliable results. Automation resulted in improved precision and accuracy, and a minimum operator intervention, leading to safer sample handling and less time-consuming procedures.

A review on development of solid phase microextraction fibers by sol-gel methods and their applications.

PubMed

Kumar, Ashwini; Gaurav; Malik, Ashok Kumar; Tewary, Dhananjay Kumar; Singh, Baldev

2008-03-03

Solid phase microextraction (SPME) is an innovative, solvent free technology that is fast, economical and versatile. SPME is a fiber coated with a liquid (polymer), a solid (sorbent) or a combination of both. The fiber coating takes up the compounds from the sample by absorption in the case of liquid coatings or adsorption in the case of solid coatings. The SPME fiber is then transferred with the help of a syringe like device into the analytical instrument for desorption and analysis of the target analytes. The sol-gel process provides a versatile method to prepare size, shape and charge selective materials of high purity and homogeneity by means of preparation techniques different from the traditional ones, for the chemical analysis. This review is on the current state of the art and future trends in the developments of solid phase microextraction (SPME) fibers using sol-gel method. To achieve more selective determination of different compound classes, the variety of different coating material for SPME fibers has increased. Further developments in SPME as a highly efficient extraction technique, will greatly depend on new breakthroughs in the area of new coating material developments for the SPME fibers. In sol-gel approach, appropriate sol-gel precursors and other building blocks can be selected to create a stationary phase with desired structural and surface properties. This approach is efficient in integrating the advantageous properties of organic and inorganic material systems and thereby increasing and improving the extraction selectivity of the produced amalgam organic-inorganic stationary phases. This review is mainly focused on recent advanced developments in the design, synthesis, characterisation, properties and application of sol-gel in preparation of coatings for the SPME fibers.

Microwave assisted solvent extraction and coupled-column reversed-phase liquid chromatography with UV detection use of an analytical restricted-access-medium column for the efficient multi-residue analysis of acidic pesticides in soils.

PubMed

Hogendoom, E A; Huls, R; Dijkman, E; Hoogerbrugge, R

2001-12-14

A screening method has been developed for the determination of acidic pesticides in various types of soils. Methodology is based on the use of microwave assisted solvent extraction (MASE) for fast and efficient extraction of the analytes from the soils and coupled-column reversed-phase liquid chromatography (LC-LC) with UV detection at 228 nm for the instrumental analysis of uncleaned extracts. Four types of soils, including sand, clay and peat, with a range in organic matter content of 0.3-13% and ten acidic pesticides of different chemical families (bentazone, bromoxynil, metsulfuron-methyl, 2,4-D, MCPA, MCPP, 2,4-DP, 2,4,5-T, 2,4-DB and MCPB) were selected as matrices and analytes, respectively. The method developed included the selection of suitable MASE and LC-LC conditions. The latter consisted of the selection of a 5-microm GFF-II internal surface reversed-phase (ISRP, Pinkerton) analytical column (50 x 4.6 mm, I.D.) as the first column in the RAM-C18 configuration in combination with an optimised linear gradient elution including on-line cleanup of sample extracts and reconditioning of the columns. The method was validated with the analysis of freshly spiked samples and samples with aged residues (120 days). The four types of soils were spiked with the ten acidic pesticides at levels between 20 and 200 microg/kg. Weighted regression of the recovery data showed for most analyte-matrix combinations, including freshly spiked samples and aged residues, that the method provides overall recoveries between 60 and 90% with relative standard deviations of the intra-laboratory reproducibility's between 5 and 25%; LODs were obtained between 5 and 50 microg/kg. Evaluation of the data set with principal component analysis revealed that the parameters (i) increase of organic matter content of the soil samples and (ii) aged residues negatively effect the recovery of the analytes.

Fast and sensitive high performance liquid chromatography analysis of cosmetic creams for hydroquinone, phenol and six preservatives.

PubMed

Gao, Wenhui; Legido-Quigley, Cristina

2011-07-15

A fast and sensitive HPLC method for analysis of cosmetic creams for hydroquinone, phenol and six preservatives has been developed. The influence of sample preparation conditions and the composition of the mobile phase and elution mode were investigated to optimize the separation of the eight studied components. Final conditions were 60% methanol and 40% water (v/v) extraction of the cosmetic creams. A C18 column (100 mm × 2.1 mm) was used as the separation column and the mobile phase consisted of methanol and 0.05 mol/L ammonium formate in water (pH=3.0) with gradient elution. The results showed that complete separation of the eight studied components was achieved within 10 min, the linear ranges were 1.0-200 μg/mL for phenol, 0.1-150 μg/mL for sorbic acid, 2.0-200 μg/mL for benzoic acid, 0.5-200 μg/mL for hydroquinone, methyl paraben, ethyl paraben and propyl paraben, butyl paraben, and good linear correlation coefficient (≥0.9997) were obtained, the detection limit was in the range of 0.05-1.0 μg/mL, the average recovery was between 86.5% and 116.3%, and the relative standard deviation (RSD) was less than 5.0% (n=6). The method is easy, fast and sensitive, it can be employed to analyze component residues in cosmetic creams especially in a quality control setting. Copyright © 2011 Elsevier B.V. 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.

Nanoparticles with photoinduced precipitation for the extraction of pollutants from water and soil

PubMed Central

Brandl, Ferdinand; Bertrand, Nicolas; Lima, Eliana Martins; Langer, Robert

2015-01-01

Nanotechnology may offer fast and effective solutions for environmental clean-up. Herein, amphiphilic diblock copolymers are used to develop a platform of photosensitive core-shell nanoparticles. Irradiation with ultraviolet light removes the protective layer responsible for colloidal stability; as a result, the nanoparticles are rapidly and irreversibly converted to macroscopic aggregates. The associated phase separation allows measuring the partitioning of small molecules between the aqueous phase and nanoparticles; data suggests that interactions are enhanced by decreasing the particle size. Adsorption onto nanoparticles can be exploited to efficiently remove hydrophobic pollutants from water and contaminated soil. Preliminary in vivo experiments suggest that treatment with photocleavable nanoparticles can significantly reduce the teratogenicity of bisphenol A, triclosan and 17α-ethinyl estradiol without generating obviously toxic byproducts. Small-scale pilot experiments on wastewater, thermal printing paper and contaminated soil demonstrate the applicability of the approach. PMID:26196119

MIDAS, prototype Multivariate Interactive Digital Analysis System, phase 1. Volume 3: Wiring diagrams

NASA Technical Reports Server (NTRS)

Kriegler, F. J.; Christenson, D.; Gordon, M.; Kistler, R.; Lampert, S.; Marshall, R.; Mclaughlin, R.

1974-01-01

The Midas System is a third-generation, fast, multispectral recognition system able to keep pace with the large quantity and high rates of data acquisition from present and projected sensors. A principal objective of the MIDAS Program is to provide a system well interfaced with the human operator and thus to obtain large overall reductions in turn-around time and significant gains in throughput. The hardware and software generated in Phase I of the overall program are described. The system contains a mini-computer to control the various high-speed processing elements in the data path and a classifier which implements an all-digital prototype multivariate-Gaussian maximum likelihood decision algorithm operating at 2 x 100,000 pixels/sec. Sufficient hardware was developed to perform signature extraction from computer-compatible tapes, compute classifier coefficients, control the classifier operation, and diagnose operation. The MIDAS construction and wiring diagrams are given.

MIDAS, prototype Multivariate Interactive Digital Analysis System, Phase 1. Volume 2: Diagnostic system

NASA Technical Reports Server (NTRS)

Kriegler, F. J.; Christenson, D.; Gordon, M.; Kistler, R.; Lampert, S.; Marshall, R.; Mclaughlin, R.

1974-01-01

The MIDAS System is a third-generation, fast, multispectral recognition system able to keep pace with the large quantity and high rates of data acquisition from present and projected sensors. A principal objective of the MIDAS Program is to provide a system well interfaced with the human operator and thus to obtain large overall reductions in turn-around time and significant gains in throughout. The hardware and software generated in Phase I of the over-all program are described. The system contains a mini-computer to control the various high-speed processing elements in the data path and a classifier which implements an all-digital prototype multivariate-Gaussian maximum likelihood decision algorithm operating 2 x 105 pixels/sec. Sufficient hardware was developed to perform signature extraction from computer-compatible tapes, compute classifier coefficients, control the classifier operation, and diagnose operation. Diagnostic programs used to test MIDAS' operations are presented.

Nanoparticles with photoinduced precipitation for the extraction of pollutants from water and soil

NASA Astrophysics Data System (ADS)

Brandl, Ferdinand; Bertrand, Nicolas; Lima, Eliana Martins; Langer, Robert

2015-07-01

Nanotechnology may offer fast and effective solutions for environmental clean-up. Herein, amphiphilic diblock copolymers are used to develop a platform of photosensitive core-shell nanoparticles. Irradiation with ultraviolet light removes the protective layer responsible for colloidal stability; as a result, the nanoparticles are rapidly and irreversibly converted to macroscopic aggregates. The associated phase separation allows measuring the partitioning of small molecules between the aqueous phase and nanoparticles; data suggests that interactions are enhanced by decreasing the particle size. Adsorption onto nanoparticles can be exploited to efficiently remove hydrophobic pollutants from water and contaminated soil. Preliminary in vivo experiments suggest that treatment with photocleavable nanoparticles can significantly reduce the teratogenicity of bisphenol A, triclosan and 17α-ethinyl estradiol without generating obviously toxic byproducts. Small-scale pilot experiments on wastewater, thermal printing paper and contaminated soil demonstrate the applicability of the approach.

Rapid Catalyst Capture Enables Metal-Free para-Hydrogen-Based Hyperpolarized Contrast Agents.

PubMed

Barskiy, Danila A; Ke, Lucia A; Li, Xingyang; Stevenson, Vincent; Widarman, Nevin; Zhang, Hao; Truxal, Ashley; Pines, Alexander

2018-05-10

Hyperpolarization techniques based on the use of para-hydrogen provide orders of magnitude signal enhancement for magnetic resonance spectroscopy and imaging. The main drawback limiting widespread applicability of para-hydrogen-based techniques in biomedicine is the presence of organometallic compounds (the polarization transfer catalysts) in solution with hyperpolarized contrast agents. These catalysts are typically complexes of platinum-group metals, and their administration in vivo should be avoided. Herein, we show how extraction of a hyperpolarized compound from an organic phase to an aqueous phase combined with a rapid (less than 10 s) Ir-based catalyst capture by metal scavenging agents can produce pure para-hydrogen-based hyperpolarized contrast agents, as demonstrated by high-resolution nuclear magnetic resonance (NMR) spectroscopy and inductively coupled plasma atomic emission spectroscopy (ICP-AES). The presented methodology enables fast and efficient means of producing pure hyperpolarized aqueous solutions for biomedical and other uses.

3D mouse shape reconstruction based on phase-shifting algorithm for fluorescence molecular tomography imaging system.

PubMed

Zhao, Yue; Zhu, Dianwen; Baikejiang, Reheman; Li, Changqing

2015-11-10

This work introduces a fast, low-cost, robust method based on fringe pattern and phase shifting to obtain three-dimensional (3D) mouse surface geometry for fluorescence molecular tomography (FMT) imaging. We used two pico projector/webcam pairs to project and capture fringe patterns from different views. We first calibrated the pico projectors and the webcams to obtain their system parameters. Each pico projector/webcam pair had its own coordinate system. We used a cylindrical calibration bar to calculate the transformation matrix between these two coordinate systems. After that, the pico projectors projected nine fringe patterns with a phase-shifting step of 2π/9 onto the surface of a mouse-shaped phantom. The deformed fringe patterns were captured by the corresponding webcam respectively, and then were used to construct two phase maps, which were further converted to two 3D surfaces composed of scattered points. The two 3D point clouds were further merged into one with the transformation matrix. The surface extraction process took less than 30 seconds. Finally, we applied the Digiwarp method to warp a standard Digimouse into the measured surface. The proposed method can reconstruct the surface of a mouse-sized object with an accuracy of 0.5 mm, which we believe is sufficient to obtain a finite element mesh for FMT imaging. We performed an FMT experiment using a mouse-shaped phantom with one embedded fluorescence capillary target. With the warped finite element mesh, we successfully reconstructed the target, which validated our surface extraction approach.

New Method To Estimate Total Polyphenol Excretion: Comparison of Fast Blue BB versus Folin-Ciocalteu Performance in Urine.

PubMed

Hinojosa-Nogueira, Daniel; Muros, Joaquín; Rufián-Henares, José A; Pastoriza, Silvia

2017-05-24

Polyphenols are bioactive substances of vegetal origin with a significant impact on human health. The assessment of polyphenol intake and excretion is therefore important. The Folin-Ciocalteu (F-C) method is the reference assay to measure polyphenols in foods as well as their excretion in urine. However, many substances can influence the method, making it necessary to conduct a prior cleanup using solid-phase extraction (SPE) cartridges. In this paper, we demonstrate the use of the Fast Blue BB reagent (FBBB) as a new tool to measure the excretion of polyphenols in urine. Contrary to F-C, FBBB showed no interference in urine, negating the time-consuming and costly SPE cleanup. In addition, it showed excellent linearity (r 2 = 0.9997), with a recovery of 96.4% and a precision of 1.86-2.11%. The FBBB method was validated to measure the excretion of polyphenols in spot urine samples from Spanish children, showing a good correlation between polyphenol intake and excretion.

Acacia nilotica leave extract and glyburide: comparison of fasting blood glucose, serum insulin, beta-thromboglubulin levels and platelet aggregation in streptozotocin induced diabetic rats.

PubMed

Asad, Munnaza; Munir, Tahir Ahmad; Afzal, Nasir

2011-03-01

To evaluate the hypoglycaemic and anti-platelet aggregation effect of aqueous methanol extract of Acacia Nilotica (AN) leaves compared with glyburide on streptozotocin induced diabetic rats. Diabetes mellitus was induced in 90 out of 120 albino rats by administering 50 mg/kg body weight (b.w) streptozotocin and was confirmed by measuring fasting blood glucose level >200 mg/dL on 4th post-induction day. The rats were equally divided into 4 groups, A (normal control), B (diabetic control), C (diabetic rats treated with AN extract) and group D (diabetic rats treated with glyburide). The rats of group C and D were given 300 mg/kg b.w AN extract and 900 microgm/kg b.w glyburide respectively for 3 weeks. Blood glucose was measured by glucometer, platelet aggregation by Dia-Med method and insulin and beta-thromboglobulin by ELISA technique. A significant increase (p<0.05) in fasting blood glucose, beta-thromboglobulin and platelet aggregation and a significant decrease (p<0.05) in insulin levels was observed in streptozotocin induced diabetic rats than the normal controls. The rats treated with AN extract and glyburide showed a significant decrease (p<0.05) in fasting blood glucose and increase (p<0.05) in insulin levels than the diabetic control rats. However, the levels in both the treatment groups remained significantly different than the normal controls. A significant decrease (p<0.05) in beta-thromboglobulin levels was seen in diabetic rats treated with glyburide than the diabetic control rats and diabetic rats treated with AN extract. AN leaves extract result into hypoglycaemic and anti-platelet aggregation activity in diabetic rats as that of glyburide.

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

PubMed

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

2018-07-01

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

Occurrence of naproxen, ibuprofen, and diclofenac residues in wastewater and river water of KwaZulu-Natal Province in South Africa.

PubMed

Madikizela, Lawrence Mzukisi; Chimuka, Luke

2017-07-01

The present paper reports a detailed study that is based on the monitoring of naproxen, ibuprofen, and diclofenac in Mbokodweni River and wastewater treatment plants (WWTPs) located around the city of Durban in KwaZulu-Natal Province of South Africa. Target compounds were extracted from water samples using a multi-template molecularly imprinted solid-phase extraction prior to separation and quantification on a high-performance liquid chromatography equipped with photo diode array detector. The analytical method yielded the detection limits of 0.15, 1.00, and 0.63 μg/L for naproxen, ibuprofen, and diclofenac, respectively. Solid-phase extraction method was evaluated for its performance using deionized water samples that were spiked with 5 and 50 μg/L of target compounds. Recoveries were greater than 80% for all target compounds with RSD values in the range of 4.1 to 10%. Target compounds were detected in most wastewater and river water samples with ibuprofen being the most frequently detected pharmaceutical. Maximum concentrations detected in river water for naproxen, ibuprofen, and diclofenac were 6.84, 19.2, and 9.69 μg/L, respectively. The concentrations of target compounds found in effluent and river water samples compared well with some studies. The analytical method employed in this work is fast, selective, sensitive, and affordable; therefore, it can be used routinely to evaluate the occurrence of acidic pharmaceuticals in South African water resources.

Selective and rapid determination of tadalafil and finasteride using solid phase extraction by high performance liquid chromatography and tandem mass spectrometry.

PubMed

Pappula, Nagaraju; Kodali, Balaji; Datla, Peda Varma

2018-04-15

Highly selective and fast liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for simultaneous determination of tadalafil (TDL) and finasteride (FNS) in human plasma. The method was successfully applied for analysis of TDL and FNS samples in clinical study. The method was validated as per USFDA (United States Food and Drug Administration), EMA (European Medicines Agency), and ANVISA (Agência Nacional de Vigilância Sanitária-Brazil) bio analytical method validation guidelines. Glyburide (GLB) was used as common internal standard (ISTD) for both analytes. The selected multiple reaction monitoring (MRM) transitions for mass spectrometric analysis were m/z 390.2/268.2, m/z 373.3/305.4 and m/z 494.2/369.1 for TDL, FNS and ISTD respectively. The extraction of analytes and ISTD was accomplished by a simple solid phase extraction (SPE) procedure. Rapid analysis time was achieved on Zorbax Eclipse C18 column (50 × 4.6 mm, 5 μm). The calibration ranges for TDL and FNS were 5-800 ng/ml and 0.2-30 ng/ml respectively. The results of precision and accuracy, linearity, recovery and matrix effect of the method are acceptable. The accuracy was in the range of 92.9%-106.4% and method precision was also good; %CV was less than 8.1%. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of phthalates released from paper packaging materials by solid-phase extraction-high-performance liquid chromatography.

PubMed

Gao, Xin; Yang, Bofeng; Tang, Zhixu; Luo, Xin; Wang, Fengmei; Xu, Hui; Cai, Xue

2014-01-01

A solid phase extraction (SPE) high-performance liquid chromatography (HPLC) method was developed for the simultaneous determination of 10 phthalic acid esters (dimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzylbutyl phthalate, diisobutyl phthalate, dicyclohexyl phthalate, diamyl phthalate, di-n-hexyl phthalate, di-n-octyl phthalate and di-2-ethylhexyl phthalate) released from food paper packaging materials. The use of distilled water, 3% acetic acid (w/v), 10% ethanol (v/v) and 95% ethanol (v/v) instead of the different types of food simulated the migration of 10 phthalic acid esters from food paper packaging materials; the phthalic acid esters in four food simulants were enriched and purified by a C18 SPE column and nitrogen blowing, and quantified by HPLC with a diode array detector. The chromatographic conditions and extraction conditions were optimized and all 10 of the phthalate acid esters had a maximum absorbance at 224 nm. The method showed limitations of detection in the range of 6.0-23.8 ng/mL the correlation coefficients were greater than 0.9999 in all cases, recovery values ranged between 71.27 and 106.97% at spiking levels of 30, 60 and 90 ng/mL and relative standard deviation values ranged from 0.86 to 8.00%. The method was considered to be simple, fast and reliable for a study on the migration of these 10 phthalic acid esters from food paper packaging materials into food.

Screening for anabolic steroids in urine of forensic cases using fully automated solid phase extraction and LC-MS-MS.

PubMed

Andersen, David W; Linnet, Kristian

2014-01-01

A screening method for 18 frequently measured exogenous anabolic steroids and the testosterone/epitestosterone (T/E) ratio in forensic cases has been developed and validated. The method involves a fully automated sample preparation including enzyme treatment, addition of internal standards and solid phase extraction followed by analysis by liquid chromatography-tandem mass spectrometry (LC-MS-MS) using electrospray ionization with adduct formation for two compounds. Urine samples from 580 forensic cases were analyzed to determine the T/E ratio and occurrence of exogenous anabolic steroids. Extraction recoveries ranged from 77 to 95%, matrix effects from 48 to 78%, overall process efficiencies from 40 to 54% and the lower limit of identification ranged from 2 to 40 ng/mL. In the 580 urine samples analyzed from routine forensic cases, 17 (2.9%) were found positive for one or more anabolic steroids. Only seven different steroids including testosterone were found in the material, suggesting that only a small number of common steroids are likely to occur in a forensic context. The steroids were often in high concentrations (>100 ng/mL), and a combination of steroids and/or other drugs of abuse were seen in the majority of cases. The method presented serves as a fast and automated screening procedure, proving the suitability of LC-MS-MS for analyzing anabolic steroids. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Multi-mJ energy extraction using Yb-fiber based coherent pulse stacking amplification of fs pulses (Conference Presentation)

NASA Astrophysics Data System (ADS)

Ruppe, John M.; Pei, Hanzhang; Chen, Siyun; Sheikhsofla, Morteza; Wilcox, Russell B.; Nees, John A.; Galvanauskas, Almantas

2017-03-01

We report multi-mJ energy (>5mJ) extraction from femtosecond-pulse Yb-doped fiber CPA using coherent pulse stacking amplification (CPSA) technique. This high energy extraction has been enabled by amplifying 10's of nanosecond long pulse sequence, and by using 85-µm core Yb-doped CCC fiber based power amplification stage. The CPSA system consists of 1-GHz repetition rate mode-locked fiber oscillator, followed by a pair of fast phase and amplitude electro-optic modulators, a diffraction-grating based pulse stretcher, a fiber amplifier chain, a GTI-cavity based pulse stacker, and a diffraction grating pulse compressor. Electro-optic modulators are used to carve out from the 1-GHz mode-locked pulse train an amplitude and phase modulated pulse burst, which after stretching and amplification, becomes equal-amplitude pulse burst consisting of 27 stretched pulses, each approximately 1-ns long. Initial pulse-burst shaping accounts for the strong amplifier saturation effects, so that it is compensated at the power amplifier output. This 27-pulse burst is then coherently stacked into a single pulse using a multiplexed sequence of 5 GTI cavities. The compact-footprint 4+1 multiplexed pulse stacker consists of 4 cavities having rountrip of 1 ns, and one Herriott-cell folded cavity - with 9ns roundtrip. After stacking, stretched pulses are compressed down to the bandwidth-limited 300 fs duration using a standard diffraction-grating pulse compressor.

SNS Extraction Fast Kicker System Development

DTIC Science & Technology

2003-06-01

SNS EXTRACTION FAST KICKER SYSTEM DEVELOPMENT * W. Zhang ξ, J. Sandberg, R. Lambiase, Y.Y. Lee, R. Lockey, J. Mi, T. Nehring, C. Pai, N. Tsoupas...Oak Ridge, TN 37831 * SNS is managed by UT-Battelle, LLC, under contract DE-AC05-00OR22725 for...the U.S. Department of Energy. SNS is a partnership of six national laboratories: Argonne, Brookhaven, Jefferson, Lawrence Berkeley, Los Alamos, and

Heterocyclic aromatic amine content in chicken burgers and chicken nuggets sold in fast food restaurants and effects of green tea extract and microwave thawing on their formation

USDA-ARS?s Scientific Manuscript database

The aims of the current study were to investigate the presence of carcinogenic and mutagenic heterocyclic aromatic amines (HAAs) in chicken burgers (CBs) and chicken nuggets (CNs) purchased from fast food restaurants and the effects of green tea extract addition (GTE) to the covering material as wel...

Fast and Efficient Feature Engineering for Multi-Cohort Analysis of EHR Data.

PubMed

Ozery-Flato, Michal; Yanover, Chen; Gottlieb, Assaf; Weissbrod, Omer; Parush Shear-Yashuv, Naama; Goldschmidt, Yaara

2017-01-01

We present a framework for feature engineering, tailored for longitudinal structured data, such as electronic health records (EHRs). To fast-track feature engineering and extraction, the framework combines general-use plug-in extractors, a multi-cohort management mechanism, and modular memoization. Using this framework, we rapidly extracted thousands of features from diverse and large healthcare data sources in multiple projects.

Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants in fish using fast, low-pressure gas chromatography-tandem mass spectrometry.

PubMed

Sapozhnikova, Yelena; Lehotay, Steven J

2013-01-03

A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS-MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1h/analyst, and LP-GC/MS-MS analysis provided fast separation of multiple analytes within 9min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n=5). The measured values for both SRMs agreed with certified/reference values (72-119% accuracy) for the majority of analytes. The detection limits were 0.1-0.5ng g(-1) for PCBs, 0.5-10ng g(-1) for PBDEs, 0.5-5ng g(-1) for select pesticides and PAHs and 1-10ng g(-1) for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market. Published by Elsevier B.V.

Effect of muscle tone on ankle kinetics during gait with ankle-foot orthoses in persons with stroke.

PubMed

Mizuno, Shiho; Sonoda, Shigeru; Takeda, Kotaro; Maeshima, Shinichiro

2017-12-01

Background Individuals exhibiting hemiplegia and increased ankle plantar flexors muscle tone following stroke are frequently prescribed an ankle-foot orthosis (AFO) to regain functional ambulation. The effect of muscle tone on ankle kinetics when walking with an AFO remains unknown. Objectives To investigate the effect of plantar flexion (PF) muscle tone on ankle plantar flexion torque during walking with an ankle-foot orthosis Methods The study included 80 participants with first-ever stroke whose manual muscle testing (MMT) of ankle DF 0-4, and 10 healthy subjects. Participants were instructed to walk on a treadmill, at a comfortable speed, wearing an instrumented AFO. Minimum PF torque during the last half of swing was extracted as an outcome measure. Resistive PF torques during passive slow and fast stretches were measured with a custom-built device, with torques at 10° DF (T10°-slow and T10°-fast) extracted as defining parameters for stiffness and muscle tone, respectively. Results Correlations between both T10°-slow and T10°-fast variables with minimum PF torque were fair among ankle DF MMT 0-3 groups (r = 0.71 -0.74, p < 0.01), with no correlation observed among the MMT 4 group and healthy subjects. Conclusions Effects of muscle tone on ankle kinetics during swing phase, with an AFO, were observed in persons with severe ankle DF paresis. Quantitative evaluation of ankle kinetics during gait with an AFO in addition to evaluation of muscle tone at rest is contributory to objective assessment of a muscle tone, not subjective rating scale at rest, or visual inspection of walking.

Digital disaster evaluation and its application to 2015 Ms 8.1 Nepal Earthquake

NASA Astrophysics Data System (ADS)

WANG, Xiaoqing; LV, Jinxia; DING, Xiang; DOU, Aixia

2016-11-01

The purpose of the article is to probe the technique resolution of disaster information extraction and evaluation from the digital RS images based on the internet environment and aided by the social and geographic information. The solution is composed with such methods that the fast post-disaster assessment system will assess automatically the disaster area and grade, the multi-phase satellite and airborne high resolution digital RS images will provide the basis to extract the disaster areas or spots, assisted by the fast position of potential serious damage risk targets according to the geographic, administrative, population, buildings and other information in the estimated disaster region, the 2D digital map system or 3D digital earth system will provide platforms to interpret cooperatively the damage information in the internet environment, and further to estimate the spatial distribution of damage index or intensity, casualties or economic losses, which are very useful for the decision-making of emergency rescue and disaster relief, resettlement and reconstruction. The spatial seismic damage distribution of 2015 Ms 8.1 Nepal earthquake, as an example of the above solution, is evaluated by using the high resolution digital RS images, auxiliary geographic information and ground survey. The results are compared with the statistical disaster information issued by the ground truth by field surveying, and show good consistency.

Characterization of new types of stationary phases for fast and ultra-fast liquid chromatography by signal processing based on AutoCovariance Function: a case study of application to Passiflora incarnata L. extract separations.

PubMed

Pietrogrande, Maria Chiara; Dondi, Francesco; Ciogli, Alessia; Gasparrini, Francesco; Piccin, Antonella; Serafini, Mauro

2010-06-25

In this study, a comparative investigation was performed of HPLC Ascentis (2.7 microm particles) columns based on fused-core particle technology and Acquity (1.7 microm particles) columns requiring UPLC instruments, in comparison with Chromolith RP-18e columns. The study was carried out on mother and vegetal tinctures of Passiflora incarnata L. on one single or two coupled columns. The fundamental attributions of the chromatographic profiles are evaluated using a chemometric procedure, based on the AutoCovariance Function (ACVF). Different chromatographic systems are compared in terms of their separation parameters, i.e., number of total chemical components (m(tot)), separation efficiency (sigma), peak capacity (n(c)), overlap degree of peaks and peak purity. The obtained results show the improvements achieved by HPLC columns with narrow size particles in terms of total analysis time and chromatographic efficiency: comparable performance are achieved by Ascentis (2.7 microm particle) column and Acquity (1.7 microm particle) column requiring UPLC instruments. The ACVF plot is proposed as a simplified tool describing the chromatographic fingerprint to be used for evaluating and comparing chemical composition of plant extracts by using the parameters D% - relative abundance of the deterministic component - and c(EACF) - similarity index computed on ACVF. Copyright 2010 Elsevier B.V. All rights reserved.

Fast Gas Chromatography with Tandem Mass Spectrometry Analysis of Selected Persistent Organic Pollutants and Organophosphorus and Synthetic Pyrethroid Pesticides in Indian Prawn (Fenneropenaeus indicus) in Compliance with the EU-MRLs.

PubMed

Sawant, Durvesh; Kelkar, Jitendra; Rasam, Pratap; Datar, Ajit; Hase, Prashant; Handique, Dheeraj; Bhone, Ankush; Chiplunkar, Sanket; Hate, Manish

2017-05-01

A fast GC with tandem MS method was developed and validated for multiresidue determination of 95 chemical contaminants (24 synthetic pyrethroids, 17 organochlorines, 17 organophosphorus compounds, 18 polycyclic aromatic hydrocarbons, and 19 polychlorinated biphenyls) in Indian prawns (Fenneropenaeus indicus) as per the European Union maximum residual limit requirements. Chromatographic separation and MS determination were achieved within a short run time of 18 min, without compromising sensitivity and specificity. Our findings revealed a 2.5× reduction in the run time compared with conventional GC methods. Sample preparation involved a QuEChERS-based extraction of 10 g sample with 10 mL acidified acetonitrile (1% acetic acid) and phase separation with 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. The extract was cleaned in two steps, first by dispersive cleanup with primary secondary amine and then by C18 SPE cartridge. The regression coefficients of linearity (r2) for the concentration range of 5-50 ng/mL were >0.99 for all the compounds. Recoveries at 5 and 10 ng/g levels were within the acceptable range of 70-120%. The repeatability (RSDr) and within-laboratory reproducibility (RSDwR) precisions were ≤20%. The method was successfully applied for analysis of the real world samples for incurred residues.

Online analysis of five organic ultraviolet filters in environmental water samples using magnetism-enhanced monolith-based in-tube solid phase microextraction coupled with high-performance liquid chromatography.

PubMed

Mei, Meng; Huang, Xiaojia

2017-11-24

Due to the endocrine disrupting properties, organic UV filters have been a great risk for humans and other organisms. Therefore, development of accurate and effective analytical methods is needed for the determination of UV filters in environmental waters. In this work, a fast, sensitive and environmentally friendly method combining magnetism-enhanced monolith-based in-tube solid phase microextraction with high-performance liquid chromatography with diode array detection (DAD) (ME-MB-IT/SPME-HPLC-DAD) for the online analysis of five organic UV filters in environmental water samples was developed. To extract UV filters effectively, an ionic liquid-based monolithic capillary column doped with magnetic nanoparticles was prepared by in-situ polymerization and used as extraction medium of online ME-MB-IT/SPME-HPLC-DAD system. Several extraction conditions including the intensity of magnetic field, sampling and desorption flow rate, volume of sample and desorption solvent, pH value and ionic strength of sample matrix were optimized thoroughly. Under the optimized conditions, the extraction efficiencies for five organic UV filters were in the range of 44.0-100%. The limits of detection (S/N=3) and limits of quantification (S/N=10) were 0.04-0.26μg/L and 0.12-0.87μg/L, respectively. The precisions indicated by relative standard deviations (RSDs) were less than 10% for both intra- and inter-day variabilities. Finally, the developed method was successfully applied to the determination of UV filters in three environmental water samples and satisfactory results were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a novel solid-phase extraction element for the detection of nonylphenol in the surface water of Hangzhou.

PubMed

Lou, Liping; Cheng, Guanghuan; Yang, Qiang; Xu, Xinhua; Hu, Baolan; Chen, Yingxu

2012-02-01

Nonylphenol (NP) is a representative environmental endocrine-disrupting chemical and persistent toxic pollutant. Previous studies have shown that the average concentration of NP in environmental waters was approximately tens to hundreds of ng L(-1) and it could even reach up to tens of μg L(-1). A simple, fast and accurate method employing a novel solid-phase extraction element named "Magic Chemisorber" (MC) followed by high-performance liquid chromatography (HPLC) using a fluorescence detector (FLD) was used for detecting NP. The most important parameters that affect the extraction process, including extraction time, desorption time, desorption solvent and repeatability, were optimized. The MC-HPLC method showed good linearity with concentrations of NP from 10 to 200 μg L(-1), a correlation coefficient of 0.9995 and the limit of detection (LOD) and limit of quantification (LOQ) of this method was 0.44 and 1.47 μg L(-1), respectively. Compared to commercial polydimethylsiloxane (PDMS) glass fiber, MC had both higher capacity and recovery and it could be used repeatedly. Using the MC-HPLC method we found that the concentration of NP in river water from Hangzhou city ranged from 8.54 ± 1.23 μg L(-1) (Qiantang River) to 65.77 ± 3.69 μg L(-1) (Tiesha River), which was similar to that of international regions heavily polluted with NP and higher than that of Bohai Bay, the Yellow River and the Pearl River Delta in China. This level of NP pollution is possibly related to the rapid development of the textile, printing and paper industries of Zhejiang province.

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.

Vision-Based Finger Detection, Tracking, and Event Identification Techniques for Multi-Touch Sensing and Display Systems

PubMed Central

Chen, Yen-Lin; Liang, Wen-Yew; Chiang, Chuan-Yen; Hsieh, Tung-Ju; Lee, Da-Cheng; Yuan, Shyan-Ming; Chang, Yang-Lang

2011-01-01

This study presents efficient vision-based finger detection, tracking, and event identification techniques and a low-cost hardware framework for multi-touch sensing and display applications. The proposed approach uses a fast bright-blob segmentation process based on automatic multilevel histogram thresholding to extract the pixels of touch blobs obtained from scattered infrared lights captured by a video camera. The advantage of this automatic multilevel thresholding approach is its robustness and adaptability when dealing with various ambient lighting conditions and spurious infrared noises. To extract the connected components of these touch blobs, a connected-component analysis procedure is applied to the bright pixels acquired by the previous stage. After extracting the touch blobs from each of the captured image frames, a blob tracking and event recognition process analyzes the spatial and temporal information of these touch blobs from consecutive frames to determine the possible touch events and actions performed by users. This process also refines the detection results and corrects for errors and occlusions caused by noise and errors during the blob extraction process. The proposed blob tracking and touch event recognition process includes two phases. First, the phase of blob tracking associates the motion correspondence of blobs in succeeding frames by analyzing their spatial and temporal features. The touch event recognition process can identify meaningful touch events based on the motion information of touch blobs, such as finger moving, rotating, pressing, hovering, and clicking actions. Experimental results demonstrate that the proposed vision-based finger detection, tracking, and event identification system is feasible and effective for multi-touch sensing applications in various operational environments and conditions. PMID:22163990

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

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2007-11-02

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

Kinetics of hydrophobic organic contaminant extraction from sediment by granular activated carbon.

PubMed

Rakowska, M I; Kupryianchyk, D; Smit, M P J; Koelmans, A A; Grotenhuis, J T C; Rijnaarts, H H M

2014-03-15

Ex situ solid phase extraction with granular activated carbon (GAC) is a promising technique to remediate contaminated sediments. The methods' efficiency depends on the rate by which contaminants are transferred from the sediment to the surface of GAC. Here, we derive kinetic parameters for extraction of polycyclic aromatic hydrocarbons (PAH) from sediment by GAC, using a first-order multi-compartment kinetic model. The parameters were obtained by modeling sediment-GAC exchange kinetic data following a tiered model calibration approach. First, parameters for PAH desorption from sediment were calibrated using data from systems with 50% (by weight) GAC acting as an infinite sink. Second, the estimated parameters were used as fixed input to obtain GAC uptake kinetic parameters in sediment slurries with 4% GAC, representing the ex situ remediation scenario. PAH uptake rate constants (kGAC) by GAC ranged from 0.44 to 0.0005 d(-1), whereas GAC sorption coefficients (KGAC) ranged from 10(5.57) to 10(8.57) L kg(-1). These values are the first provided for GAC in the presence of sediment and show that ex situ extraction with GAC is sufficiently fast and effective to reduce the risks of the most available PAHs among those studied, such as fluorene, phenanthrene and anthracene. Copyright © 2013 Elsevier Ltd. All rights reserved.

Phenolic compounds containing/neutral fractions extract and products derived therefrom from fractionated fast-pyrolysis oils

DOEpatents

Chum, Helena L.; Black, Stuart K.; Diebold, James P.; Kreibich, Roland E.

1993-01-01

A process for preparing phenol-formaldehyde novolak resins and molding compositions in which portions of the phenol normally contained in said resins are replaced by a phenol/neutral fractions extract obtained from fractionating fast-pyrolysis oils. The fractionation consists of a neutralization stage which can be carried out with aqueous solutions of bases or appropriate bases in the dry state, followed by solvent extraction with an organic solvent having at least a moderate solubility parameter and good hydrogen bonding capacity. Phenolic compounds-containing/neutral fractions extracts obtained by fractionating fast-pyrolysis oils from a lignocellulosic material, is such that the oil is initially in the pH range of 2-4, being neutralized with an aqueous bicarbonate base, and extracted into a solvent having a solubility parameter of approximately 8.4-9.11 [cal/cm.sup.3 ].sup.1/2 with polar components in the 1.8-3.0 range and hydrogen bonding components in the 2-4.8 range and the recovery of the product extract from the solvent with no further purification being needed for use in adhesives and molding compounds. The product extract is characterized as being a mixture of very different compounds having a wide variety of chemical functionalities, including phenolic, carbonyl, aldehyde, methoxyl, vinyl and hydroxyl. The use of the product extract on phenol-formaldehyde thermosetting resins is shown to have advantages over the conventional phenol-formaldehyde resins.

Metabolic effects of green tea and of phases of weight loss.

PubMed

Diepvens, K; Kovacs, E M R; Vogels, N; Westerterp-Plantenga, M S

2006-01-30

The effect of ingestion of green tea (GT) extract along with a low-energy diet (LED) on health-related blood parameters, and the relationships among changes in metabolic parameters and phases of weight loss were assessed. A double-blind, placebo-controlled, parallel design was used. 46 female subjects (BMI 27.7+/-1.8 kg/m(2)) were fed in energy balance from days 1 to 3, followed by a LED with GT (n=23) or placebo (PLAC, n=23) from days 4 to 87. The LED-period consisted of a phase 1 of 4 weeks (days 4-32) followed by a phase 2 of 8 weeks (days 32-87). Body composition and fasting blood samples were determined on days 4, 32 and 87. No significant differences were observed between the blood parameters of the PLAC and GT group. In phase 1 compared to phase 2 the rate of weight loss was 0.09+/-0.05 kg/day vs. 0.03+/-0.03 kg/day (p<0.001); Fat free mass (FFM) was 21% of weight loss in phase 1 vs. 7% in phase 2 (ns). Surprisingly, favourable changes in free fatty acids, triacylglycerol, beta-hydroxybutyrate, glucose and total cholesterol in phase 1 were reversed in phase 2 (p<0.01). Taken together, GT supplementation during a LED had no effect on health-related blood parameters. Initial improvements in several blood measures at day 32 were reversed by day 87, despite continued weight loss. Modest weight loss improved HDL cholesterol and blood pressure.

Determination of 15 N-nitrosodimethylamine precursors in different water matrices by automated on-line solid-phase extraction ultra-high-performance-liquid chromatography tandem mass spectrometry.

PubMed

Farré, Maria José; Insa, Sara; Mamo, Julian; Barceló, Damià

2016-08-05

A new methodology based on on-line solid-phase extraction (SPE) ultra-high-performance-liquid chromatography coupled to a triple quadrupole mass spectrometer (UHPLC-MS-MS) for the determination of 15 individual anthropogenic N-nitrosodimethylamine (NDMA) precursors was developed. On-line SPE was performed by passing 2mL of the water sample through a Hypersil GOLD aQ column and chromatographic separation was done using a Kinetex Biphenyl column using methanol and 0.1% formic acid aqueous solution as a mobile phase. For unequivocal identification and confirmation, two selected reaction monitoring (SRM) transitions were monitored per compound. Quantification was performed by internal standard approach and matrix match calibration. The main advantages of the developed method are high sensitivity (limits of detection in the sub ng/L range), selectivity due to the use of tandem mass spectrometry, precision and minimum sample manipulation as well as fast analytical response. Process efficiency and recovery were also evaluated for all the target compounds. As part of the validation procedure, the method was applied in a sampling campaign for the analysis of influent and secondary effluent of a wastewater treatment plant (WWTP) in Girona, Spain. Additionally, the effluent from a nanofiltration (NF) membrane system used for water recycling was monitored. The percentage of NDMA formation explained by the measured precursors was also quantified. Copyright © 2016 Elsevier B.V. All rights reserved.

High throughput screening and antioxidant assay of dibenzo[a,c]cyclooctadiene lignans in modified-ultrasonic and supercritical fluid extracts of Schisandra chinensis Baill by liquid chromatography--mass spectrometry and a free radical-scavenging method.

PubMed

Wang, Ming-Chih; Lai, Yih-Cherng; Chang, Chia-Lin

2008-05-01

Dibenzo[a,c]cyclooctadiene lignans of Schisandra chinensis Baill are well known because of their hepatoprotective activity, antioxidant activity, and anticancer effect. For the isolation of the dibenzo[a,c]cyclooctadiene lignans of Schisandra chinensis Baill two extraction methods were used: modified-ultrasonic extraction and supercritical fluid extraction. A specific and fast analytical method for structure identification is established for quality control because structure elucidation could be accomplished by means of liquid chromatography-mass spectrometry (LC-MS) technologies. The separation and identification of the compounds were completed by: (i) a water-acetonitrile gradient system using a C18 reversed-phase column; (ii) UV detection at 225 nm; (iii) MS/MS experiments with electrospray ionization interface (ESI) ion trap mass spectrometry in the positive mode. Normalized collision energy was used to obtain fragment ions of structural relevance in the LC-MS/MS. These results provided a reliable LC-MS/MS method for the determination of the dibenzo[a,c]cyclooctadiene lignans from Schisandra chinensis Baill. Finally, we also detected 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging effects (%) of the modified-ultrasonic and supercritical fluid extracts of Schisandra chinensis Baill compared with 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (Trolox). The antioxidant activities of the modified-ultrasonic and supercritical fluid extracts were lower than that of trolox.

Synthesis and characterization of core-shell magnetic molecularly imprinted polymers for solid-phase extraction and determination of Rhodamine B in food.

PubMed

Su, Xiaomeng; Li, Xiaoyan; Li, Junjie; Liu, Min; Lei, Fuhou; Tan, Xuecai; Li, Pengfei; Luo, Weiqiang

2015-03-15

Core-shell magnetic molecularly imprinted polymers (MIPs) nanoparticles (NPs), in which a Rhodamine B-imprinted layer was coated on Fe3O4 NPs. were synthesized. First, Fe3O4 NPs were prepared by a coprecipitation method. Then, amino-modified Fe3O4 NPs (Fe3O4@SiO2-NH2) was prepared. Finally, the MIPs were coated on the Fe3O4@SiO2-NH2 surface by the copolymerization with functional monomer, acrylamide, using a cross-linking agent, ethylene glycol dimethacrylate; an initiator, azobisisobutyronitrile and a template molecule, Rhodamine B. The Fe3O4@MIPs were characterized using a scanning electron microscope, Fourier transform infrared spectrometer, vibrating sample magnetometer, and re-binding experiments. The Fe3O4@MIPs showed a fast adsorption equilibrium, a highly improved imprinting capacity, and significant selectivity; they could be used as a solid-phase extraction material and detect illegal addition Rhodamine B in food. A method was developed for the selective isolation and enrichment of Rhodamine B in food samples with recoveries in the range 78.47-101.6% and the relative standard deviation was <2%. Copyright © 2014 Elsevier Ltd. All rights reserved.

A feasibility study for high-temperature titanium reduction from TiCl4 using a magnesiothermic process

NASA Astrophysics Data System (ADS)

Ivanov, S. L.; Zablotsky, D.

2018-05-01

The current industrial practice for titanium extraction is a complex procedure, which produces a porous reaction mass of sintered titanium particulates fused to a steel retort wall with magnesium and MgCl2 trapped in the interstices. The reactor temperature is limited to approx. 900 °C due to the formation of fusible TiFe eutectic, which corrodes the retort and degrades the quality of titanium sponge. Here we examine the theoretical foundations and technological possibilities to design a shielded retort of niobium-zirconium alloy NbZr(1%), which is resistant to corrosion by titanium at high temperature. We consider the reactor at a temperature of approx. 1150 °C. Supplying stoichiometric quantities of reagents enables the reaction in the gas phase, whereas the exothermic process sustains the combustion of the reaction zone. When the pathway to the condenser is open, vacuum separation and evacuation of vaporized magnesium dichloride and excess magnesium into the water-cooled condenser take place. As both the reaction and the evacuation occur within seconds, the yield of the extraction is improved. We anticipate new possibilities for designing a device combining the retort function to conduct the reduction in the gas phase with fast vacuum separation of the reaction products and distillation of magnesium dichloride.

Determination of antazoline hydrochloride in rat plasma and excreta by reversed-phase ion-pair chromatography and its application to pharmacokinetics.

PubMed

Wang, Rui; Chu, Yanle; Li, Xiaotian; Wan, Baoluo; Yu, Tong; Wang, Linxi; Hao, Lianqi; Guo, Maowen

2013-12-01

A reversed-phase ion pair chromatography method with liquid-liquid extraction analytical method was developed and validated for the determination of antazoline hydrochloride in plasma and excreta of rat. The aim of our study was to characterize the preclinical pharmacokinetics and excretion profiles of antazoline hydrochloride in rats after intravenous injection at the dose of 10 mg/kg. Plasma and excreta samples were extracted with ethyl acetate, and phenacetin was used as the internal standard. The result showed that the method is suitable for the quantification of antazoline hydrochloride in plasma and excreta samples. Analysis of accuracy (90.89-112.33%), imprecision (<7.1%) and recovery (>82.5%) showed adequate values. After a single intravenous administration at 10 mg/kg to rats, plasma concentration profile showed a relative fast elimination proceeding with a terminal elimination half-life of 3.53 h. Approximately 61.8 and 14.2% of the administered dose were recovered in urine and bile after 72 and 24 h post-dosing respectively; 5.9% of the administered dose was recovered in feces after 72 h post-dosing. The above results show that the major elimination route is urinary excretion. Copyright © 2013 John Wiley & Sons, Ltd.

Fast title extraction method for business documents

NASA Astrophysics Data System (ADS)

Katsuyama, Yutaka; Naoi, Satoshi

1997-04-01

Conventional electronic document filing systems are inconvenient because the user must specify the keywords in each document for later searches. To solve this problem, automatic keyword extraction methods using natural language processing and character recognition have been developed. However, these methods are slow, especially for japanese documents. To develop a practical electronic document filing system, we focused on the extraction of keyword areas from a document by image processing. Our fast title extraction method can automatically extract titles as keywords from business documents. All character strings are evaluated for similarity by rating points associated with title similarity. We classified these points as four items: character sitting size, position of character strings, relative position among character strings, and string attribution. Finally, the character string that has the highest rating is selected as the title area. The character recognition process is carried out on the selected area. It is fast because this process must recognize a small number of patterns in the restricted area only, and not throughout the entire document. The mean performance of this method is an accuracy of about 91 percent and a 1.8 sec. processing time for an examination of 100 Japanese business documents.

Antinociception produced by Thalassia testudinum extract BM-21 is mediated by the inhibition of acid sensing ionic channels by the phenolic compound thalassiolin B

PubMed Central

2011-01-01

Background Acid-sensing ion channels (ASICs) have a significant role in the sensation of pain and constitute an important target for the search of new antinociceptive drugs. In this work we studied the antinociceptive properties of the BM-21 extract, obtained from the sea grass Thalassia testudinum, in chemical and thermal models of nociception in mice. The action of the BM-21 extract and the major phenolic component isolated from this extract, a sulphated flavone glycoside named thalassiolin B, was studied in the chemical nociception test and in the ASIC currents of the dorsal root ganglion (DRG) neurons obtained from Wistar rats. Results Behavioral antinociceptive experiments were made on male OF-1 mice. Single oral administration of BM-21 produced a significant inhibition of chemical nociception caused by acetic acid and formalin (specifically during its second phase), and increased the reaction time in the hot plate test. Thalassiolin B reduced the licking behavior during both the phasic and tonic phases in the formalin test. It was also found that BM-21 and thalassiolin B selectively inhibited the fast desensitizing (τ < 400 ms) ASIC currents in DRG neurons obtained from Wistar rats, with a nonsignificant action on ASIC currents with a slow desensitizing time-course. The action of thalassiolin B shows no pH or voltage dependence nor is it modified by steady-state ASIC desensitization or voltage. The high concentration of thalassiolin B in the extract may account for the antinociceptive action of BM-21. Conclusions To our knowledge, this is the first report of an ASIC-current inhibitor derived of a marine-plant extract, and in a phenolic compound. The antinociceptive effects of BM-21 and thalassiolin B may be partially because of this action on the ASICs. That the active components of the extract are able to cross the blood-brain barrier gives them an additional advantage for future uses as tools to study pain mechanisms with a potential therapeutic application. PMID:21261973

Antinociception produced by Thalassia testudinum extract BM-21 is mediated by the inhibition of acid sensing ionic channels by the phenolic compound thalassiolin B.

PubMed

Garateix, Anoland; Salceda, Emilio; Menéndez, Roberto; Regalado, Erik L; López, Omar; García, Teidy; Morales, Ruth A; Laguna, Abilio; Thomas, Olivier P; Soto, Enrique

2011-01-24

Acid-sensing ion channels (ASICs) have a significant role in the sensation of pain and constitute an important target for the search of new antinociceptive drugs. In this work we studied the antinociceptive properties of the BM-21 extract, obtained from the sea grass Thalassia testudinum, in chemical and thermal models of nociception in mice. The action of the BM-21 extract and the major phenolic component isolated from this extract, a sulphated flavone glycoside named thalassiolin B, was studied in the chemical nociception test and in the ASIC currents of the dorsal root ganglion (DRG) neurons obtained from Wistar rats. Behavioral antinociceptive experiments were made on male OF-1 mice. Single oral administration of BM-21 produced a significant inhibition of chemical nociception caused by acetic acid and formalin (specifically during its second phase), and increased the reaction time in the hot plate test. Thalassiolin B reduced the licking behavior during both the phasic and tonic phases in the formalin test. It was also found that BM-21 and thalassiolin B selectively inhibited the fast desensitizing (τ < 400 ms) ASIC currents in DRG neurons obtained from Wistar rats, with a nonsignificant action on ASIC currents with a slow desensitizing time-course. The action of thalassiolin B shows no pH or voltage dependence nor is it modified by steady-state ASIC desensitization or voltage. The high concentration of thalassiolin B in the extract may account for the antinociceptive action of BM-21. To our knowledge, this is the first report of an ASIC-current inhibitor derived of a marine-plant extract, and in a phenolic compound. The antinociceptive effects of BM-21 and thalassiolin B may be partially because of this action on the ASICs. That the active components of the extract are able to cross the blood-brain barrier gives them an additional advantage for future uses as tools to study pain mechanisms with a potential therapeutic application.

Low-parachor solvents extraction and thermostated micro-thin-layer chromatography separation for fast screening and classification of spirulina from pharmaceutical formulations and food samples.

PubMed

Zarzycki, Paweł K; Zarzycka, Magdalena B; Clifton, Vicki L; Adamski, Jerzy; Głód, Bronisław K

2011-08-19

The goal of this paper is to demonstrate the separation and detection capability of eco-friendly micro-TLC technique for the classification of spirulina and selected herbs from pharmaceutical and food products. Target compounds were extracted using relatively low-parachor liquids. A number of the spirulina samples which originated from pharmaceutical formulations and food products, were isolated using a simple one step extraction with small volume of methanol, acetone or tetrahydrofuran. Herb samples rich in chlorophyll dyes were analyzed as reference materials. Quantitative data derived from micro-plates under visible light conditions and after iodine staining were explored using chemometrics tools including cluster analysis and principal components analysis. Using this method we could easily distinguish genuine spirulina and non-spirulina samples as well as fresh from expired commercial products and furthermore, we could identify some biodegradation peaks appearing on micro-TLC profiles. This methodology can be applied as a fast screening or fingerprinting tool for the classification of genuine spirulina and herb samples and in particular may be used commercially for the rapid quality control screening of products. Furthermore, this approach allows low-cost fractionation of target substances including cyanobacteria pigments in raw biological or environmental samples for preliminary chemotaxonomic investigations. Due to the low consumption of the mobile phase (usually less than 1 mL per run), this method can be considered as environmentally friendly analytical tool, which may be an alternative for fingerprinting protocols based on HPLC machines and simple separation systems involving planar micro-fluidic or micro-chip devices. Copyright © 2011 Elsevier B.V. All rights reserved.

A NAD(P) reductase like protein is the salicylic acid receptor in the appendix of the Sauromatum guttatum inflorescence

PubMed Central

Skubatz, Hanna; Orellana, Mónica V; Howald, William N

2013-01-01

The mode of action of the thermogenic inducers (salicylic acid, aspirin, and 2,6-dihydroxybenzoic acid) in the appendix of the Sauromatum guttatum inflorescence is poorly understood. Using ESI-MS and light scattering analysis, we have demonstrated that NAD(P) reductase like protein (RL) is the salicylic acid receptor in the Sauromatum appendix. RL was self-assembled in water into a large unit with a hydrodynamic diameter of 800 nm. In the presence of 1 pM salicylic acid, RL exhibited discontinuous and reversible volume phase transitions. The volume phase changed from 800 to 300 nm diameter and vice versa. RL stayed at each volume phase for ~4–5 min with a fast relaxation time between the 2 phases. ESI-MS analysis of RL extracted from appendices treated with salicylic acid, aspirin, and 2,6-DHBA at a micromolar range demonstrated that these compounds are capable of inducing graded conformational changes that are concentration-dependent. A strong correlation between RL conformations and heat-production induced by salicylic acid was also observed. These preliminary findings reveal structural and conformational roles for RL by which plants regulate their temperature and synchronize their time keeping mechanisms. PMID:28516022

Increased concentrations of endogenous 13-cis- and all-trans-retinoic acids in diffuse idiopathic skeletal hyperostosis, as demonstrated by HPLC.

PubMed

Periquet, B; Lambert, W; Garcia, J; Lecomte, G; De Leenheer, A P; Mazieres, B; Thouvenot, J P; Arlet, J

1991-11-09

Endogenous 13-cis- and all-trans-retinoic acids have been quantitated in human serum using a solvent extraction procedure followed by isocratic reversed phase high performance liquid chromatography and UV detection. In healthy adults, after an overnight fasting period, the concentrations of 13-cis- and all-trans-retinoic acids yielded 5.3 +/- 2.43 nmol/l and 11.8 +/- 3.3 nmol/l, respectively (mean +/- SD). The method has been successfully applied to the analysis of both isomers in serum from patients with idiopathic skeletal hyperostosis in whom, the 13-cis- as well as all-trans-retinoic acid levels were raised as compared to the control group.

Characterization, Preparation, and Purification of Marine Bioactive Peptides

PubMed Central

Wang, Xueqin; Yu, Huahua; Xing, Ronge

2017-01-01

Marine bioactive peptides, as a source of unique bioactive compounds, are the focus of current research. They exert various biological roles, some of the most crucial of which are antioxidant activity, antimicrobial activity, anticancer activity, antihypertensive activity, anti-inflammatory activity, and so forth, and specific characteristics of the bioactivities are described. This review also describes various manufacturing techniques for marine bioactive peptides using organic synthesis, microwave assisted extraction, chemical hydrolysis, and enzymes hydrolysis. Finally, purification of marine bioactive peptides is described, including gel or size exclusion chromatography, ion-exchange column chromatography, and reversed-phase high-performance liquid chromatography, which are aimed at finding a fast, simple, and effective method to obtain the target peptides. PMID:28761878

A liquid chromatographic method for determination of theophylline in serum and capillary blood--a comparison.

PubMed

Gartzke, J; Jäger, H; Vins, I

1991-01-01

A simple, fast and reliable liquid chromatographic method for the determination of theophylline in serum and capillary blood after a solid phase extraction is described for therapeutic drug monitoring. The employment of capillary blood permits the determination of an individual drug profile and other pharmacokinetic studies in neonates and infants. There were no differences in venous- and capillary-blood levels but these values compared poorly with those in serum. An adjustment of the results by correction of the different volumes of serum and blood by haematocrit was unsuccessful. Differences in the binding of theophylline to erythrocytes could be an explanation for the differences in serum at blood levels of theophylline.

Extraction and analysis of antioxidant capacity in eight edible beans

USDA-ARS?s Scientific Manuscript database

In this work we explored the use of microwave as a fast method for the extraction of antioxidants from beans. Antioxidant capacity of the extracts from meat and the hull of eight common beans was determined, using the ß-carotene bleaching method. Microwave-assisted extraction was achieved using two ...

Diesel Engine Valve Clearance Fault Diagnosis Based on Features Extraction Techniques and FastICA-SVM

NASA Astrophysics Data System (ADS)

Jing, Ya-Bing; Liu, Chang-Wen; Bi, Feng-Rong; Bi, Xiao-Yang; Wang, Xia; Shao, Kang

2017-07-01

Numerous vibration-based techniques are rarely used in diesel engines fault diagnosis in a direct way, due to the surface vibration signals of diesel engines with the complex non-stationary and nonlinear time-varying features. To investigate the fault diagnosis of diesel engines, fractal correlation dimension, wavelet energy and entropy as features reflecting the diesel engine fault fractal and energy characteristics are extracted from the decomposed signals through analyzing vibration acceleration signals derived from the cylinder head in seven different states of valve train. An intelligent fault detector FastICA-SVM is applied for diesel engine fault diagnosis and classification. The results demonstrate that FastICA-SVM achieves higher classification accuracy and makes better generalization performance in small samples recognition. Besides, the fractal correlation dimension and wavelet energy and entropy as the special features of diesel engine vibration signal are considered as input vectors of classifier FastICA-SVM and could produce the excellent classification results. The proposed methodology improves the accuracy of feature extraction and the fault diagnosis of diesel engines.

[Effect of a dehydrated extract of nopal (Opuntia ficus indica Mill.) on blood glucose].

PubMed

Frati-Munari, A C; de León, C; Ariza-Andraca, R; Bañales-Ham, M B; López-Ledesma, R; Lozoya, X

1989-01-01

To assess if a dehydrated extract of nopal stems retains the effect on glycemia of the entire nopal stems two experiments were performed. A. Six patients with type II diabetes mellitus in fasting condition received 30 capsules containing 10.1 +/- 0.3 g of the extract, and serum glucose levels were measured hourly from 0 to 180 minutes. B. Six healthy volunteers received 30 capsules with the extract followed by 74 g of dextrose orally. Serum glucose measurements were made in a similar fashion. In each experiment a control test with empty capsules was performed. Nopal extract did not reduce fasting glycemia in diabetic subjects. Nevertheless, the extract diminished the increase of serum glucose which followed a dextrose load. Peak serum glucose was 20.3 +/- 18.2 mg/dl (X +/- SD) lower in the test with nopal than in the control one (P less than 0.025). Dehydrated extract of nopal (Opuntia ficus-indica Mill) did not show acute hypoglycemic effect, although could attenuate postprandial hyperglycemia.

Solvent extraction system for plutonium colloids and other oxide nano-particles

DOEpatents

Soderholm, Lynda; Wilson, Richard E; Chiarizia, Renato; Skanthakumar, Suntharalingam

2014-06-03

The invention provides a method for extracting plutonium from spent nuclear fuel, the method comprising supplying plutonium in a first aqueous phase; contacting the plutonium aqueous phase with a mixture of a dielectric and a moiety having a first acidity so as to allow the plutonium to substantially extract into the mixture; and contacting the extracted plutonium with second a aqueous phase, wherein the second aqueous phase has a second acidity higher than the first acidity, so as to allow the extracted plutonium to extract into the second aqueous phase. The invented method facilitates isolation of plutonium polymer without the formation of crud or unwanted emulsions.

A star-shaped polythiophene dendrimer coating for solid-phase microextraction of triazole agrochemicals.

PubMed

Abolghasemi, Mir Mahdi; Habibiyan, Rahim; Jaymand, Mehdi; Piryaei, Marzieh

2018-02-14

A nanostructured star-shaped polythiophene dendrimer was prepared and used as a fiber coating for headspace solid phase microextraction of selected triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole) from water samples. The dendrimer with its large surface area was characterized by thermogravimetric analysis, UV-Vis spectroscopy and field emission scanning electron microscopy. It was placed on a stainless steel wire for use in SPME. The experimental conditions for fiber coating, extraction, stirring rate, ionic strength, pH value, desorption temperature and time were optimized. Following thermal desorption, the pesticides were quantified by GC-MS. Under optimum conditions, the repeatability (RSD) for one fiber (for n = 3) ranges from 4.3 to 5.6%. The detection limits are between 8 and 12 pg mL -1 . The method is fast, inexpensive (in terms of equipment), and the fiber has high thermal stability. Graphical abstract Schematic presentation of a nanostructured star-shaped polythiophene dendrimer for use in headspace solid phase microextraction of the triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole). They were then quantified by gas chromatography-mass spectrometry.

Electrochemical characterization of repaglinide and its determination in human plasma using liquid chromatography with dual-channel coulometric detection.

PubMed

Jirovský, David; Bartošová, Zdenka; Skopalová, Jana; Maier, Vítezslav

2010-12-01

A simple, fast and sensitive HPLC method employing dual-channel coulometric detection for the determination of repaglinide in human plasma is presented. The assay involved extraction of repaglinide by ethyl acetate and isocratic reversed-phase liquid chromatography with dual-channel coulometric detection. The mobile phase composition was 50mM disodium hydrogen phosphate/acetonitrile (60:40, v/v), pH of the mobile phase 7.5 set up with phosphoric acid. For all analyses, the first cell working potential was +380mV, the second was +750mV (vs. Pd/H(2)). Calibration curve was linear over the concentration range of 5-500nmolL(-1). Rosiglitazone was used as an internal standard. The limit of detection (LOD) was established at 2.8nmolL(-1), and the lower limit of quantification (LLOQ) at 8.5nmolL(-1). The developed method was applied to human plasma samples spiked with repaglinide at therapeutical concentrations. It was confirmed that the method is suitable for pharmacokinetic studies or therapeutic monitoring. Copyright © 2010 Elsevier B.V. All rights reserved.

On the use of pulsed Dielectric Barrier Discharges to control the gas-phase composition of atmospheric pressure air plasmas

NASA Astrophysics Data System (ADS)

Barni, R.; Biganzoli, I.; Dell'Orto, E.; Riccardi, C.

2014-11-01

We presents results obtained from the numerical simulation of the gas-phase chemical kinetics in atmospheric pressure air non-equilibrium plasmas. In particular we have addressed the effect of pulsed operation mode of a plane dielectric barrier discharge. It was conjectured that the large difference in the time scales involved in the fast dissociation of oxygen molecules in plasma and their subsequent reactions to produce ozone and nitrogen oxides, makes the presence of a continuously repeated plasma production unnecessary and a waste of electrical power and thus efficiency. In order to test such suggestion we have performed a numerical study of the composition and the temporal evolution of the gas-phase of atmospheric pressure air non-equilibrium plasmas. Comparison with experimental findings in a dielectric barrier discharge with an electrode configuration symmetrical and almost ideally plane is briefly addressed too, using plasma diagnostics to extract the properties of the single micro-discharges and a sensor to measure the concentration of ozone produced by the plasma.

Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes.

PubMed

Lehotay, Steven J; Mastovská, Katerina; Yun, Seon Jong

2005-01-01

Two rapid methods of sample preparation and analysis of fatty foods (e.g., milk, eggs, and avocado) were evaluated and compared for 32 pesticide residues representing a wide range of physicochemical properties. One method, dubbed the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residue analysis, entailed extraction of 15 g sample with 15 mL acetonitrile (MeCN) containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 1 mL of the buffered MeCN extract underwent a cleanup step (in a technique known as dispersive solid-phase extraction) using 50 mg each of C18 and primary secondary amine sorbents plus 150 mg MgSO4. The second method incorporated a form of matrix solid-phase dispersion (MSPD), in which 0.5 g sample plus 2 g C18 and 2 g anhydrous sodium sulfate was mixed in a mortar and pestle and added above a 2 g Florisil column on a vacuum manifold. Then, 5 x 2 mL MeCN was used to elute the pesticide analytes from the sample into a collection tube, and the extract was concentrated to 0.5 mL by evaporation. Extracts in both methods were analyzed concurrently by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry. The recoveries of semi-polar and polar pesticides were typically 100% in both methods (except that basic pesticides, such as thiabendazole and imazalil, were not recovered in the MSPD method), but recovery of nonpolar pesticides decreased as fat content of the sample increased. This trend was more pronounced in the QuEChERS method, in which case the most lipophilic analyte tested, hexachlorobenzene, gave 27 +/- 1% recovery (n=6) in avocado (15% fat) with a<10 ng/g limit of quantitation.

Magnetic solid-phase extraction of five pyrethroids from environmental water samples followed by ultrafast liquid chromatography analysis.

PubMed

Yu, Xi; Sun, Ying; Jiang, Chunzhu; Sun, Xiumin; Gao, Yan; Wang, Yuanpeng; Zhang, Hanqi; Song, Daqian

2012-08-30

In this study, the polystyrene-coated magnetic nanoparticles (MNPs/PSt) were successfully prepared and characterized by Fourier transform infrared spectroscopy, transmission electron microscopy and vibrating sample magnetometry. The as-prepared MNPs/PSt were used as the adsorbent in magnetic solid phase extraction of five pyrethroids, including lambda-cyhalothrin, deltamethrin, esfenvalerate, permethrin, bifenthrin, in environmental water samples. The five pyrethroids were determined by ultra fast liquid chromatography-ultraviolet spectrometry. The influencing factors, including amount of MNPs/Pst, extraction time, pH value, type and volume of desorption solvent and desorption time, were examined and optimized. The extraction recoveries obtained with merely 50mg of MNPs/Pst were very satisfactory. The whole extraction process could be completed within 0.5h. The MNPs/PSt can be reused after an easy washing process. Thus, a simple, green, economical, time saving and effective method for pyrethroids analysis in environmental water samples was established. A high enrichment factor of 500 was achieved and the limits of detection for lambda-cyhalothrin, deltamethrin, esfenvalerate, permethrin, bifenthrin were 0.015±0.001 ng mL(-1), 0.012±0.001 ng mL(-1), 0.026±0.001 ng mL(-1), 0.020±0.001 ng mL(-1), 0.013±0.001 ng mL(-1), respectively. Recoveries obtained by analyzing spiked water samples at three concentration levels (0.100±0.001 ng mL(-1), 1.000±0.001 ng mL(-1), 10.000±0.001 ng mL(-1)) were between 78.97±8.38% and 96.05±8.38%. The standard curves for the five pyrethroids showed good linearity with the correlation coefficients in the range of 0.9994-0.9999. The intra-day and inter-day precision were satisfactory with the RSDs in the range of 2.05-5.52% and 2.73-8.38%, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-03-01

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

Graphene-based solid-phase extraction disk for fast separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Wang, Zonghua; Han, Qiang; Xia, Jianfei; Xia, Linhua; Ding, Mingyu; Tang, Jie

2013-06-01

Graphene has great potentials for the use in sample preparation due to its ultra high specific surface area, superior chemical stability, and excellent thermal stability. In our work, a novel graphene-based SPE disk was developed for separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples. Based on the strong π-π stacking interaction between the analytes and graphene, the analytes extracted by graphene were eluted by cyclohexane and then determined by GC-MS. Under the optimized conditions, high flow rate (30 mL/min) and sensitivity (0.84-13 ng/L) were achieved. The proposed method was successfully applied to the analysis of real environmental water samples with recoveries ranging from 72.8 to 106.2%. Furthermore, the property of anticlogging and reusability was also improved. This work reveals great potentials of graphene-based SPE disk in environmental analytical. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry Analysis of Fosetyl-Aluminum in Airborne Particulate Matter

PubMed Central

Di Filippo, Patrizia; Riccardi, Carmela; Pomata, Donatella; Marsiglia, Riccardo; Console, Carla; Puri, Daniele

2018-01-01

Fosetyl-aluminum is a synthetic fungicide administered to plants especially to prevent diseases caused by the members of the Peronosporales and several Phytophthora species. Herein, we present a selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to analyze residues of fosetyl-A1 in air particulate matter. This study was performed in perspective of an exposure assessment of this substance of health concern in environments where high levels of fosetly-Al, relatively to airborne particulate matter, can be found after spraying it. The cleanup procedure of the analyte, from sampled filters of atmospheric particulate matter, was optimized using a Strata X solid-phase extraction cartridge, after accelerated extraction by using water. The chromatographic separation was achieved using a polymeric column based on hydrophilic interaction in step elution with water/acetonitrile, whereas the mass spectrometric detection was performed in negative electrospray ionization. The proposed method resulted to be a simple, fast, and suitable method for confirmation purposes. PMID:29686933

[Spectrum-effect Relationship Between Total Antioxidant Activity and HPLC Fingerprint of Arctium lappa Root].

PubMed

Wang, Xiao-juan; Jiang, Lin

2014-12-01

To explore the spectrum-effect relationship between the HPLC fingerprint of Arctium lappa root methanol extract and the total antioxidant activity. The experiment was carried out with Gemini C18 110A (250 mm x 4.6 mm, 5 µm) column using methanol-0.04% phosphoric acid as gradient mobile phase at the flow rate of 1.0 mL/min, detection wavelength of 320 nm. The total antioxidant activity was determined by measuring the absorbance of each sample after being reacted with ammonium molybdate reagent. The spectrum-effect relationship was investigated using canonical correlation analysis (CCA). The spectrum-effect relationship between the HPLC fingerprint of Arctium lappa root methanol extract and the total antioxidant activity were established, the similarity of fingerprint of all samples was above 0.9. Peaks 1, 6, 9, 12 and 14 were principle components of Arctium lappa root for the total antioxidant activity. This method contributes to the fast comprehensive evaluation of quality of Arctium lappa root.

Pharmacokinetics and tissue distribution study of Praeruptorin D from Radix peucedani in rats by high-performance liquid chromatography (HPLC).

PubMed

Liang, Taigang; Yue, Wenyan; Du, Xue; Ren, Luhui; Li, Qingshan

2012-01-01

Praeruptorin D (PD), a major pyranocoumarin isolated from Radix Peucedani, exhibited antitumor and anti-inflammatory activities. The aim of this study was to investigate the pharmacokinetics and tissue distribution of PD in rats following intravenous (i.v.) administration. The levels of PD in plasma and tissues were measured by a simple and sensitive reversed-phase high-performance liquid chromatography (HPLC) method. The biosamples were treated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE) and osthole was used as the internal standard (IS). The chromatographic separation was accomplished on a reversed-phase C(18) column using methanol-water (75:25, v/v) as mobile phase at a flow rate of 0.8 mL/min and ultraviolet detection wave length was set at 323 nm. The results demonstrate that this method has excellent specificity, linearity, precision, accuracy and recovery. The pharmacokinetic study found that PD fitted well into a two-compartment model with a fast distribution phase and a relative slow elimination phase. Tissue distribution showed that the highest concentration was observed in the lung, followed by heart, liver and kidney. Furthermore, PD can also be detected in the brain, which indicated that PD could cross the blood-brain barrier after i.v. administration.

Versatile quantitative phase imaging system applied to high-speed, low noise and multimodal imaging (Conference Presentation)

NASA Astrophysics Data System (ADS)

Federici, Antoine; Aknoun, Sherazade; Savatier, Julien; Wattellier, Benoit F.

2017-02-01

Quadriwave lateral shearing interferometry (QWLSI) is a well-established quantitative phase imaging (QPI) technique based on the analysis of interference patterns of four diffraction orders by an optical grating set in front of an array detector [1]. As a QPI modality, this is a non-invasive imaging technique which allow to measure the optical path difference (OPD) of semi-transparent samples. We present a system enabling QWLSI with high-performance sCMOS cameras [2] and apply it to perform high-speed imaging, low noise as well as multimodal imaging. This modified QWLSI system contains a versatile optomechanical device which images the optical grating near the detector plane. Such a device is coupled with any kind of camera by varying its magnification. In this paper, we study the use of a sCMOS Zyla5.5 camera from Andor along with our modified QWLSI system. We will present high-speed live cell imaging, up to 200Hz frame rate, in order to follow intracellular fast motions while measuring the quantitative phase information. The structural and density information extracted from the OPD signal is complementary to the specific and localized fluorescence signal [2]. In addition, QPI detects cells even when the fluorophore is not expressed. This is very useful to follow a protein expression with time. The 10 µm spatial pixel resolution of our modified QWLSI associated to the high sensitivity of the Zyla5.5 enabling to perform high quality fluorescence imaging, we have carried out multimodal imaging revealing fine structures cells, like actin filaments, merged with the morphological information of the phase. References [1]. P. Bon, G. Maucort, B. Wattellier, and S. Monneret, "Quadriwave lateral shearing interferometry for quantitative phase microscopy of living cells," Opt. Express, vol. 17, pp. 13080-13094, 2009. [2] P. Bon, S. Lécart, E. Fort and S. Lévêque-Fort, "Fast label-free cytoskeletal network imaging in living mammalian cells," Biophysical journal, 106(8), pp. 1588-1595, 2014

Support for equatorial anisotropy of Earth's inner-inner core from seismic interferometry at low latitudes

NASA Astrophysics Data System (ADS)

Wang, Tao; Song, Xiaodong

2018-03-01

Anisotropy of Earth's inner core provides a key role to understand its evolution and the Earth's magnetic field. Recently, using autocorrelations from earthquake's coda, we found an equatorial anisotropy of the inner-inner core (IIC), in apparent contrast to the polar anisotropy of the outer-inner core (OIC). To reduce the influence of the polar anisotropy and reduce possible contaminations from the large Fresnel zone of the PKIKP2 and PKIIKP2 phases at low frequencies, we processed coda noise of large earthquakes (10,000-40,000 s after magnitude ≥7.0) from stations at low latitudes (within ±35°) during 1990-2013. Using a number of improved procedures of both autocorrelation and cross-correlation, we extracted 52 array-stacked high-quality empirical Green's functions (EGFs), an increase of over 60% from our previous study. The high-quality data allow us to measure the relative arrival times by automatic waveform cross correlation. The results show large variation (∼10.9 s) in the differential times between the PKIKP2 and PKIIKP2 phases. The estimated influence of the Fresnel zone is insignificant (<1.1 s), compared to the observed data variation and measurement uncertainty. The observed time residuals match very well previous IIC model with a quasi-equatorial fast axis (near Central America and the Southeast Asia) and the spatial pattern from the low-latitude measurements is similar to the previous global dataset, including the fast axis and two low-velocity open rings, thus providing further support for the equatorial anisotropy model of the IIC. Speculations for the shift of the fast axis between the OIC and the IIC include: change of deformation regimes during the inner core history, change of geomagnetic field, and a proto-inner core.

Solvent Extraction of Rare Earth Elements from a Nitric Acid Leach Solution of Apatite by Mixtures of Tributyl Phosphate and Di-(2-ethylhexyl) Phosphoric Acid

NASA Astrophysics Data System (ADS)

Ferdowsi, Ali; Yoozbashizadeh, Hossein

2017-12-01

Solvent extraction of rare earths from nitrate leach liquor of apatite using mixtures of tributyl phosphate (TBP) and di-(2-ethylhexyl) phosphoric acid (D2EHPA) was studied. The effects of nitrate and hydrogen ion concentration of the aqueous phase as well as the composition and concentration of extractants in the organic phase on the extraction behavior of lanthanum, cerium, neodymium, and yttrium were investigated. The distribution ratio of REEs increases by increasing the nitrate concentration in aqueous phase and concentration of extractants in organic phase, but the hydrogen ion concentration in aqueous phase has a decreasing effect. Yttrium as a heavy rare earth is more sensitive to these parameters than light rare earth elements. Although the composition of organic phase has a minor effect on the extraction of light rare earths, the percent of extraction of yttrium decreases dramatically by increasing the TBP content of organic phase. Mixtures of TBP and D2EHPA can show either synergism or antagonism extraction depending on the concentration and composition of extractants in organic phase. The best condition for separating rare earth elements in groups of heavy and light REEs can be achieved at high nitrate concentration, low H+ concentration, and high concentration of D2EHPA in organic phase. Separation of Ce and La by TBP and D2EHPA is practically impossible in the studied conditions; however, low nitrate concentration and high hydrogen ion concentration in aqueous phase and low concentration of extractants in organic phase favor the separation of Nd from other light rare earth elements.

Synthesis of polydopamine-functionalized magnetic graphene and carbon nanotubes hybrid nanocomposites as an adsorbent for the fast determination of 16 priority polycyclic aromatic hydrocarbons in aqueous samples.

PubMed

Chen, Kun; Jin, Rongrong; Luo, Chen; Song, Guoxin; Hu, Yaoming; Cheng, Hefa

2018-04-01

A novel adsorbent made of polydopamine-functionalized magnetic graphene and carbon nanotubes hybrid nanocomposite was synthesized and applied to determine 16 priority polycyclic aromatic hydrocarbons by magnetic solid phase extraction in water samples. FTIR spectroscopy, transmission electron microscopy, scanning electron microscopy, and Raman spectroscopy consistently indicate that the synthesized adsorbents are made of core-shell nanoparticles well dispersed on the surface of graphene and carbon nanotubes. The major factors affecting the extraction efficiency, including the pH value of samples, the amount of adsorbent, adsorption time and desorption time, type and volume of desorption solvent, were systematically optimized. Under the optimum extraction conditions, a linear response was obtained for polycyclic aromatic hydrocarbons between concentrations of 10 and 500 ng/L with the correlation coefficients ranging from 0.9958 to 0.9989, and the limits of detection (S/N = 3) were between 0.1 and 3.0 ng/L. Satisfactory results were also obtained when applying these magnetic graphene/carbon nanotubes/polydopamine hybrid nanocomposites to detect polycyclic aromatic hydrocarbons in several environmental aqueous samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of fast neuronal changes from multichannel functional near-infrared spectroscopy signals using independent component analysis

NASA Astrophysics Data System (ADS)

Morren, Geert; Wolf, Martin; Lemmerling, Philippe; Wolf, Ursula; Choi, Jee H.; Gratton, Enrico; De Lathauwer, Lieven; Van Huffel, Sabine

2002-06-01

Fast changes in the range of milliseconds in the optical properties of cerebral tissue, which are associated with brain activity, can be detected using non-invasive near-infrared spectroscopy (NIRS). These changes in light scattering are due to an alteration in the refractive index at neuronal membranes. The aim of this study was to develop highly sensitive data analysis algorithms to detect this fast signal, which is small compared to other physiological signals. A frequency-domain tissue oximeter, whose laser diodes were modulated at 110MHz was used. The amplitude, mean intensity and phase of the modulated optical signal was measured at 96Hz sample rate. The probe consisting of 4 crossed source detector pairs was placed above the motor cortex, contralateral to the hand performing a tapping exercise consisting of alternating rest- and tapping periods of 20s each. The tapping frequency, which was set to 3.55Hz or 2.5 times the heart rate of the subject to avoid the influence of harmonics on the signal, could not be observed in any of the individual signals measured by the detectors. An adaptive filter was used to remove the arterial pulsatility from the optical signals. Independent Component Analysis allowed to separate signal components in which the tapping frequency was clearly visible.

Fast Determination of Toxic Arsenic Species in Food Samples Using Narrow-bore High-Performance Liquid-Chromatography Inductively Coupled Plasma Mass Spectrometry.

PubMed

Terol, Amanda; Marcinkowska, Monika; Ardini, Francisco; Grotti, Marco

2016-01-01

A new method for the speciation analysis of arsenic in food using narrow-bore high-performance liquid-chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) has been developed. Fast separation of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid was carried out in 7 min using an anion-exchange narrow-bore Nucleosil 100 SB column and 12 mM ammonium dihydrogen phosphate of pH 5.2 as the mobile phase, at a flow rate of 0.3 mL min(-1). A PFA-ST micronebulizer jointed to a cyclonic spray chamber was used for HPLC-ICP-MS coupling. Compared with standard-bore HPLC-ICP-MS, the new method has provided higher sensitivity, reduced mobile-phase consumption, a lower matrix plasma load and a shorter analysis time. The achieved instrumental limits of detection were in the 0.3 - 0.4 ng As mL(-1) range, and the precision was better than 3%. The arsenic compounds were efficiently (>80%) extracted from various food samples using a 1:5 methanol/water solution, with additional ultrasonic treatment for rice products. The applicability of this method was demonstrated by the analysis of several samples, such as seafood (fish, mussels, shrimps, edible algae) and rice-based products (Jasmine and Arborio rice, spaghetti, flour, crackers), including three certified reference materials.

Simulating a topological transition in a superconducting phase qubit by fast adiabatic trajectories

NASA Astrophysics Data System (ADS)

Wang, Tenghui; Zhang, Zhenxing; Xiang, Liang; Gong, Zhihao; Wu, Jianlan; Yin, Yi

2018-04-01

The significance of topological phases has been widely recognized in the community of condensed matter physics. The well controllable quantum systems provide an artificial platform to probe and engineer various topological phases. The adiabatic trajectory of a quantum state describes the change of the bulk Bloch eigenstates with the momentum, and this adiabatic simulation method is however practically limited due to quantum dissipation. Here we apply the "shortcut to adiabaticity" (STA) protocol to realize fast adiabatic evolutions in the system of a superconducting phase qubit. The resulting fast adiabatic trajectories illustrate the change of the bulk Bloch eigenstates in the Su-Schrieffer-Heeger (SSH) model. A sharp transition is experimentally determined for the topological invariant of a winding number. Our experiment helps identify the topological Chern number of a two-dimensional toy model, suggesting the applicability of the fast adiabatic simulation method for topological systems.

Development of SPME-LC-MS method for screening of eight beta-blockers and bronchodilators in plasma and urine samples.

PubMed

Goryński, Krzysztof; Kiedrowicz, Alicja; Bojko, Barbara

2016-08-05

The current work describes the development and validation of a simple, efficient, and fast method using solid phase microextraction coupled to liquid chromatography-tandem mass spectrometry (SPME-LC-MS/MS) for the concomitant measurement of eight beta-blockers and bronchodilators in plasma and urine. The presented assay enables quantitative determination of acebutolol, atenolol, fenoterol, nadolol, pindolol, procaterol, sotalol, and timolol. In this work, samples were prepared on a high-throughput platform using the 96-well plate format of the thin film solid phase microextraction (TFME) system, and a biocompatible extraction phase made of hydrophilic-lipophilic balance particles. Analytes were separated on a pentafluorophenyl column (100mm×2.1mm, 3μm) by gradient elution using an UPLC Nexera coupled with an LCMS-8060 mass spectrometer. The mobile phase consisted of water-acetonitrile (0.1% formic acid) at a flow rate of 0.4mLmin(-1). The linearity of the method was checked within therapeutic blood-plasma concentrations, and shown to adequately reflect typically expected concentrations of future study samples. Post-extraction addition experiments showed that the matrix effect ranged in plasma from 98% for procaterol to 115% for nadolol, and in urine, from 85% for nadolol and pindolol to 119% for atenolol. The method was successfully validated using Food and Drug Administration (FDA) guidelines, and met all acceptance criteria for bioanalytical assays at five concentration levels for all selected drugs. The final protocol can be successfully applied for monitoring concentrations of the selected drugs in both plasma and urine matrices obtained from patients or athletes. Copyright © 2016 Elsevier B.V. All rights reserved.

SOLVENT EXTRACTION PROCESS

DOEpatents

Jonke, A.A.

1957-10-01

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

Determination of terpenoid content in pine by organic solvent extraction and fast-GC analysis

DOE PAGES

Harman-Ware, Anne E.; Sykes, Robert; Peter, Gary F.; ...

2016-01-25

Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts frommore » the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. In conclusion, diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.« less

A new strategy for accelerated extraction of target compounds using molecularly imprinted polymer particles embedded in a paper-based disk.

PubMed

Zarejousheghani, Mashaalah; Schrader, Steffi; Möder, Monika; Schmidt, Matthias; Borsdorf, Helko

2018-03-01

In this study, a general simple and inexpensive method is introduced for the preparation of a paper-based selective disk-type solid phase extraction (SPE) technique, appropriate for fast and high throughput monitoring of target compounds. An ion exchange molecularly imprinted polymer (MIP) was synthesized for the extraction and analysis of acesulfame, an anthropogenic water quality marker. Acesulfame imprinting was used as an example for demonstrating the benefits of a nanosized, swellable MIP extraction sorbents integrated in an on-site compatible concept for water quality monitoring. Compared with an 8 mL standard SPE cartridge, the paper-based MIP disk (47 mm ø) format allowed (1) high sample flow rates up to 30 mL•min -1 without losing extraction efficiency (2) extracting sample volumes up to 500 mL in much shorter times than with standard SPE, (3) the reuse of the disks (up to 3 times more than SPE cartridge) due to high robustness and an efficient post-cleaning, and (4) reducing the sampling time from 100 minutes (using the standard SPE format) to about 2 minutes with the MIP paper disk for 50 mL water sample. Different parameters like cellulose fiber/polymer ratios, sample volume, sample flow-rate, washing, and elution conditions were evaluated and optimized. Using developed extraction technique with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) analysis, a new protocol was established that provides detection and quantification limits of 0.015 μg•L -1 and 0.05 μg•L -1 , respectively. The developed paper disks were used in-field for the selective extraction of target compounds and transferred to the laboratory for further analysis. Copyright © 2017 John Wiley & Sons, Ltd.

Human forearm metabolism during progressive starvation.

PubMed

Owen, O E; Reichard, G A

1971-07-01

Forearm muscle metabolism was studied in eight obese subjects after an overnight, 3 and 24 day fast. Arterio-deep-venous differences of oxygen, carbon dioxide, glucose, lactate, pyruvate, free fatty acids, acetoacetate, and beta-hydroxybutyrate with simultaneous forearm blood flow were measured. Rates of metabolite utilization and production were thus estimated. Oxygen consumption and lactate and pyruvate production remained relatively constant at each fasting period. Glucose, initially the major substrate consumed, showed decreased consumption after 3 and 24 days of fasting. Acetoacetate and beta-hydroxybutyrate consumption after an overnight fast was low. At 3 days of fasting with increased arterial concentrations of acetoactate and beta-hydroxybutyrate, consumption of these substrates rose dramatically. At 24 days of fasting, despite further elevation of arterial levels of acetoacetate and beta-hydroxybutyrate, the utilization of acetoacetate did not increase further and if anything decreased, while five out of eight subjects released beta-hydroxybutyrate across the forearm. Acetoacetate was preferentially extracted over beta-hydroxybutyrate. At 24 days of starvation, free fatty acids were the principal fuels extracted by forearm muscle; at this time there was a decreased glucose and also ketone-body consumption by skeletal muscle.

Speciation analysis of inorganic arsenic by magnetic solid phase extraction on-line with inductively coupled mass spectrometry determination.

PubMed

Montoro Leal, P; Vereda Alonso, E; López Guerrero, M M; Cordero, M T Siles; Cano Pavón, J M; García de Torres, A

2018-07-01

Arsenic, one of the main environmental pollutants and potent natural poison, is a chemical element that is spread throughout the Earth's crust. It is well known that the toxicity of arsenic is highly dependent on its chemical forms. Generally, the inorganic species are more toxic than its organics forms, and As(III) is 60 times more toxic than As(V). In environmental waters, arsenic exists predominantly in two chemical forms: As(III) and As(V). In view of these facts, fast, sensitive, accurate and simple analytical methods for the speciation of inorganic arsenic in environmental waters are required. In this work, a new magnetic solid phase extraction with a hydride generation system was coupled on line with inductively coupled plasma mass spectrometry (MSPE-HG-ICP-MS). The new system was based on the retention of As(III) and As(V) in two knotted reactors filled with (Fe 3 O 4 ) magnetic nanoparticles functionalized with [1,5-bis (2-pyridyl) 3-sulfophenylmethylene] thiocarbonohydrazide (PSTH-MNPs). As(III) and total inorganic As were sequentially eluted in different reduction conditions. The concentration of As(V) was obtained by subtracting As(III) from total As. The system runs in a fully automated way and the method has proved to have a wide linear range and to be precise, sensitive and fast. The detection limits found were 2.7 and 3.2 ng/L for As(III) and total As, respectively; with relative standard deviations (RSDs) of 2.5% and 2.7% and a sample throughput of 14.4 h -1 . In order to validate the developed method, several certified reference samples of environmental waters including sea water, were analyzed and the determined values were in good agreement with the certified values. The proposed method was successfully applied to the speciation analysis of inorganic arsenic in well-water and sea water. Copyright © 2018 Elsevier B.V. All rights reserved.

Extratropical response to Fast and Slow episodes of Madden-Julian Oscillation in observation and using intervention experiments with CFSv2

NASA Astrophysics Data System (ADS)

Yadav, P.; Straus, D. M.

2017-12-01

The Madden-Julian Oscillation (MJO) is a potential source of predictability in the extratropics in extended range weather forecasting. The nature of MJO is sporadic and therefore, the mid-latitude response may depend on the nature of the MJO event, in particular the phase speed. We discuss the results of our observational and modeling study of mid-latitude circulation response to Fast and Slow MJO episodes using wintertime ERA-Interim reanalysis data and the CFSv2 coupled model of NOAA. The observational study shows that the mid-latitude response to different propagating speeds is not the same. The propagation speed is defined by the time the OLR takes to propagate from phase 3 to phase 6. The mid-latitude response is assessed in terms of composite maps and frequency of occurrence of robust circulation regimes. Fast episode composite anomalies of 500hPa height show a developing Rossby wave in the mid-Pacific with downstream propagation through MJO phases 2- 4. Development of NAO+ teleconnection pattern is stronger in Slow that in Fast MJO episodes, and occurs with a greater time lag after MJO heating is in the Indian Ocean (phase 3). Previous results find an increase in occurrence of NAO- regime following phase 6. We have found that much of this behavior is due to the slow episodes. Based on these observational results, intervention experiments using CFSv2 are designed to better understand the impact of heating/cooling and to estimate mid-latitude response to Fast and Slow MJO episodes. The added heating experiments consist of 31 year reforecasts for December 1 initial conditions from CFS reanalysis (1980-2011) in which the identical MJO evolution of three-dimensional diabatic heating has been added, thus producing fast and slow MJO episodes with well-defined phase speeds. We will discuss the results of these experiments with a focus on understanding the role of phase speed and interference in setting up the response, and to understand the mechanisms that distinguish fast and slow types of response We will also discuss the diagnostics using Predictable Component Analysis to distinguish the signal forced by common diabatic heating signal from noise, and weather regime response to fast and slow MJO using cluster analysis.

Covalent triazine framework-1 as adsorbent for inline solid phase extraction-high performance liquid chromatographic analysis of trace nitroimidazoles in porcine liver and environmental waters.

PubMed

Zhong, Cheng; Chen, Beibei; He, Man; Hu, Bin

2017-02-03

In this study, covalent triazine framework-1 (CTF-1) was adopted as solid phase extraction (SPE) sorbents, and a method of SPE inline coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for trace analysis of three nitroimidazolaes (including metronidazole, ronidazole and dimetridazole) in porcine liver and environmental water samples. CTF-1 has rich π-electron and N containing triazine, thus can form π-π interaction and intermolecular hydrogen bond with three target polar nitroimidazoles, resulting in high extraction efficiency (87%-98%). Besides, CTF-1 has large specific area, which benefits rapid mass transfer and low column pressure, leading to fast adsorption/desorption dynamics. Several parameters affecting inline SPE including pH, sample flow rate, sample volume, desorption reagents, elution flow rate, elution volume, and ionic strength were investigated. Under the optimal experimental conditions, the limits of detection (S/N=3) were found to be in the range of 0.11-0.13μg/L. The enrichment factors (EFs) ranged from 52 to 59 fold (theoretical EF was 60-fold). The relative standard deviations were in the range of 4.3-9.4% (n=7, c=1μg/L), and the linear range was 0.5-500μg/L for three target analytes. The sample throughput is 7/h. The proposed method was successfully applied to the analysis of nitroimidazoles in porcine liver and environmental water samples with good recoveries for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

[Magnetic solid phase extraction combined with gas chromatography-flame photometric detection for the determination of organophosphorus pesticides in juice samples].

PubMed

Huang, Qian; He, Man; Chen, Beibei; Hu, Bin

2014-10-01

A novel method for the determination of organophosphorous pesticides (OPPs) in fresh juice samples was developed. Fe3O4 @ P (St-co-MAA) magnetic microparticles were synthesized and modified with styrene (St) and methacrylic acid (MAA) by coating St and MAA on magnetic particles and characterized by a series of techniques. The results indicated that Fe3 O4 magnetic nanoparticles (MNPs) have been successfully modified with St and MAA. Based on the prepared FeO4 @ P (St-co-MAA) magnetic microparticles, a novel method of magnetic solid phase extraction (MSPE)-gas chromatography (GC)-flame photometric detection (FPD) was developed for the determination of OPPs. The extraction/desorption conditions of MSPE were optimized, and the analytical performance was evaluated under the optimal conditions. The limits of detection (LODs, S/N = 3) for target OPPs were in the range of 0.013-0.305 μg/L with the RSDs (n = 7) ranging from 3.1% to 8.8%. The enrichment factors varied from 406 to 951. The linear ranges were over three orders of magnitudes (R2 > 0.99) and the reproducibilities were 7.4%-14.5% (n = 5). Finally, the proposed MSPE-GC-FPD method was successfully applied to the analysis of the five OPPs in fresh tomato and strawberry juice samples, with the recoveries of target OPPs in the range of 85.4%-118.9% for the spiked samples. The proposed MSPE-GC-FPD method is featured with low cost, fast separation and high enrichment factor.

[Determination of three exogenous plant hormone residues in bean sprout by high performance liquid chromatography-quadrupole-time of flight mass spectrometry].

PubMed

Xie, Hanbing; Zhou, Mingying; Zhao, Haifeng; Wang, Yigang; Jiang, Wanfeng; Zhao, Shan

2014-05-01

This study was aimed to the establishment of an analytical method for the determination of three exogenous plant hormone residues in bean sprout by high performance liquid chromatography-quadrupole-time of flight mass spectrometry (HPLC-Q-TOF-MS). The target compounds were gibberellins, 6-benzylaminopurine and parachlorophenoxyacetic acid. The QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used for sample preparation. The analytes were extracted with a solution containing 1% (v/v, if not specified) acetic, 50% ethanol, 49% acetonitrile, and cleaned-up by dispersive solid-phase extraction with diatomite dispersant, then degreased by hexane. The three target compounds were separated on an Eclipse Plus C18 column (100 mm x 3.0 mm, 1.8 microm) with mobile phases A (water containing 0.1% formic acid) and B (methanol) by gradient elution within 15 min, and detected under negative electrospray ionization (ESI) mode. The quantitative analysis was carried out by extracting the peak area with accurate mass. The confirmatory analysis of the target compounds was performed with the qualitative fragments. The results showed that the limits of quantification (LOQs, S/N = 10) for the three target compounds were from 5.0 microg/kg to 10 microg/kg. The respective mean recoveries were found to be in the range of 79.1%-96.1%, and the RSDs were 5.7%-10.4%. It was applicable to the analysis of the three exogenous plant hormones in bean sprout samples. This method is simple, fast and efficient.

Sulfur Speciation and Extraction in Jet A (Briefing Charts)

DTIC Science & Technology

2015-08-16

Extraction fluid: denatured ethanol from Fisher Scientific and deionized water – Jet A fuel , approximately 500-800 ppm sulfur by weight – Data...Outline • Background • Experimental Setup – Extraction of sulfur compounds from fuel to alcohol/water extraction fluid – Each rinse is...Hydrophobic / Oleophillic Membrane Oleophobic / Hydrophillic Membrane Emulsion Phase Fuel Phase Water (Extraction Fluid) Phase DISTRIBUTION A

Separation of cannabinoids on three different mixed-mode columns containing carbon/nanodiamond/amine-polymer superficially porous particles.

PubMed

Hung, Chuan-Hsi; Zukowski, Janusz; Jensen, David S; Miles, Andrew J; Sulak, Clayton; Dadson, Andrew E; Linford, Matthew R

2015-09-01

Three mixed-mode high-performance liquid chromatography columns packed with superficially porous carbon/nanodiamond/amine-polymer particles were used to separate mixtures of cannabinoids. Columns evaluated included: (i) reversed phase (C18 ), weak anion exchange, 4.6 × 33 mm, 3.6 μm, and 4.6 × 100 mm, 3.6 μm, (ii) reversed phase, strong anion exchange (quaternary amine), 4.6×33 mm, 3.6 μm, and (iii) hydrophilic interaction liquid chromatography, 4.6 × 150 mm, 3.6 μm. Different selectivities were achieved under various mobile phase and stationary phase conditions. Efficiencies and peak capacities were as high as 54 000 N/m and 56, respectively. The reversed phase mixed-mode column (C18 ) retained tetrahydrocannabinolic acid strongly under acidic conditions and weakly under basic conditions. Tetrahydrocannabinolic acid was retained strongly on the reversed phase, strong anion exchange mixed-mode column under basic polar organic mobile phase conditions. The hydrophilic interaction liquid chromatography column retained polar cannabinoids better than the (more) neutral ones under basic conditions. A longer reversed phase (C18 ) mixed-mode column (4.6 × 100 mm) showed better resolution for analytes (and a contaminant) than a shorter column. Fast separations were achieved in less than 5 min and sometimes 2 min. A real world sample (bubble hash extract) was also analyzed by gradient elution. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Estimation of terpene content in loblolly pine biomass using a hybrid fast-GC and pyrolysis-molecular beam mass spectrometry method

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

Harman-Ware, Anne E.; Davis, Mark F.; Peter, Gary F.

Terpenes can be used as renewable fuels and chemicals and quantifying their presence in biomass is becoming increasingly important. A novel method was developed to rapidly quantify total diterpenoid resin acids using pyrolysis-molecular beam mass spectrometry (py-MBMS). Pine sapling monoterpenes and diterpenoids were extracted from wood using a 1:1 (v/v) mixture of hexane and acetone and analyses were performed before and after extraction to determine the extraction efficiency of the solvent system. The resulting extract was analyzed for total diterpenoid content using py-MBMS and was combined with total monoterpene content that was determined using a low thermal mass modular acceleratedmore » column heater (LTM MACH) fast-GC/FID to measure the terpene content present in pine saplings. Oleoresin extruded from larger pine trees was used to validate mass balance closure of the terpene content in the extract solvent.« less

Estimation of terpene content in loblolly pine biomass using a hybrid fast-GC and pyrolysis-molecular beam mass spectrometry method

DOE PAGES

Harman-Ware, Anne E.; Davis, Mark F.; Peter, Gary F.; ...

2017-01-16

Terpenes can be used as renewable fuels and chemicals and quantifying their presence in biomass is becoming increasingly important. A novel method was developed to rapidly quantify total diterpenoid resin acids using pyrolysis-molecular beam mass spectrometry (py-MBMS). Pine sapling monoterpenes and diterpenoids were extracted from wood using a 1:1 (v/v) mixture of hexane and acetone and analyses were performed before and after extraction to determine the extraction efficiency of the solvent system. The resulting extract was analyzed for total diterpenoid content using py-MBMS and was combined with total monoterpene content that was determined using a low thermal mass modular acceleratedmore » column heater (LTM MACH) fast-GC/FID to measure the terpene content present in pine saplings. Oleoresin extruded from larger pine trees was used to validate mass balance closure of the terpene content in the extract solvent.« less

Effect of aqueous bark extract of Garuga pinnata Roxb. in streptozotocin-nicotinamide induced type-II diabetes mellitus.

PubMed

Shirwaikar, Annie; Rajendran, K; Barik, Rakesh

2006-09-19

A study was undertaken to evaluate the antihyperglycemic activity of aqueous extract of bark of Garuga pinnata Roxb. (Burseraceae). The various parameters studied included fasting blood sugar levels, serum lipid levels, liver glycogen content, serum insulin level and glycated hemoglobin in diabetic and normal rats. Streptozotocin-nicotinamide was used to induce type-II diabetes mellitus. Treatment with the extract at two dose levels showed a significant increase in the liver glycogen and serum insulin level and a significant decrease in fasting blood glucose and glycated hemoglobin levels. The total cholesterol and serum triglycerides levels were also significantly reduced and the HDL cholesterol levels were significantly increased upon treatment with the extract thus proving the potent antidiabetic property of the plant.

FAST Spacecraft Battery Design and Performance

NASA Technical Reports Server (NTRS)

Jung, David S.; Rao, Gopalakrishna; Ahmad, Anisa

1997-01-01

The Fast Auroral Snapshot (FAST) Explorer spacecraft is to study the physical processes that produce the aurora borealis and aurora australis. It is a unique plasma physics experiment that will take fundamental measurements of the magnetic and electrical fields. This investigation will add significantly to our understanding of the near-earth space environments and its effect. The FAST has a 1 year requirement and 3-year goal for its mission life in low earth orbit. The FAST power power system topology is a Direct Energy Transfer (DET) system based on the SAMPEX design. The FAST flight battery supplies power to the satellite during pre-launch operations, the launch phase, the eclipse periods for all mission phases, and when the load is about 50 watts.

High-throughput method based on quick, easy, cheap, effective, rugged and safe followed by liquid chromatography-multi-wavelength detection for the quantification of multiclass polyphenols in wines.

PubMed

Fontana, Ariel R; Bottini, Rubén

2014-05-16

In this work, a reliable, simple, fast, inexpensive and robust sample preparation approach for the determination of multiclass polyphenols in wine samples is proposed. The polyphenols selected for this work were gallic acid, (+)-catechin, (-)-epicatechin, caffeic acid, syringic acid, coumaric acid, ferulic acid, trans-resveratrol, quercetin and cinnamic acid. The method is based on QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction technique coupled with dispersive solid-phase extraction (d-SPE) clean-up. Under optimized conditions, the analytes were extracted from 5mL wine samples (previously acidified with 1% formic acid) using 2.5mL acetonitrile. For phase separation, 1.5g NaCl and 4g anhydrous MgSO4 were added. Then, a 1mL aliquot of the partitioned supernatant was cleaned-up using d-SPE with a combination of 150mg CaCl2, 50mg primary-secondary amine (PSA) and 50mgC18 as sorbents. A 250μL aliquot of the obtained cleaned extract was concentrated to dryness and taken up with the initial mobile phase previous to liquid chromatography-multi-wavelength detection (LC-MWD). The proposed method provided limits of detection (LODs) ranging from 0.004 to 0.079μgmL(-1) and an inter-day variability below 12% RSD for all analytes in red and white wine samples. Considering external calibration (red wines) and matrix-matched calibration (white wines) as quantification techniques, the overall recoveries (accuracy) of the method ranged between 75.0% and 119.6% for red and white wine samples, respectively. The developed method was applied for the determination of polyphenols in 10 wines produced in Argentina. Nine phenolic compounds were determined, at concentrations above detectable levels in the method. The maximum concentrations corresponded to (-)-epicatechin in white wines, while gallic acid and (+)-catechin were the most abundant in red wines. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparative analysis of feature extraction methods in satellite imagery

NASA Astrophysics Data System (ADS)

Karim, Shahid; Zhang, Ye; Asif, Muhammad Rizwan; Ali, Saad

2017-10-01

Feature extraction techniques are extensively being used in satellite imagery and getting impressive attention for remote sensing applications. The state-of-the-art feature extraction methods are appropriate according to the categories and structures of the objects to be detected. Based on distinctive computations of each feature extraction method, different types of images are selected to evaluate the performance of the methods, such as binary robust invariant scalable keypoints (BRISK), scale-invariant feature transform, speeded-up robust features (SURF), features from accelerated segment test (FAST), histogram of oriented gradients, and local binary patterns. Total computational time is calculated to evaluate the speed of each feature extraction method. The extracted features are counted under shadow regions and preprocessed shadow regions to compare the functioning of each method. We have studied the combination of SURF with FAST and BRISK individually and found very promising results with an increased number of features and less computational time. Finally, feature matching is conferred for all methods.

Recovery of Ni Metal from Spent Catalyst with Emulsion Liquid Membrane Using Cyanex 272 as Extractant

NASA Astrophysics Data System (ADS)

Yuliusman; Huda, M.; Ramadhan, I. T.; Farry, A. R.; Wulandari, P. T.; Alfia, R.

2018-03-01

In this study was conducted to recover nickel metal from spent nickel catalyst resulting from hydrotreating process in petroleum industry. The nickel extraction study with the emulsion liquid membrane using Cyanex 272 as an extractant to extract and separate nickel from the feed phase solution. Feed phase solution was preapred from spent catalyst using sulphuric acid. Liquid membrane consists of a kerosene as diluent, a Span 80 as surfactant, a Cyanex 272 as carrier and sulphuric acid solutions have been used as the stripping solution. The important parameters governing the permeation of nickel and their effect on the separation process have been studied. These parameters are surfactant concentration, extractant concentration feed phase pH. The optimum conditions of the emulsion membrane making process is using 0.06 M Cyanex 272, 8% w/v SPAN 80, 0.05 M H2SO4, internal phase extractant / phase volume ratio: 1/1, and stirring speed 1150 rpm for 60 Minute that can produce emulsion membrane with stability level above 90% after 4 hours. In the extraction process with optimum condition pH 6 for feed phase, ratio of phase emulsion/phase of feed: 1/2, and stirring speed 175 rpm for 15 minutes with result 81.51% nickel was extracted.

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.

Ultra-fast liquid chromatography with tandem mass spectrometry determination of eight bioactive components of Kai-Xin-San in rat plasma and its application to a comparative pharmacokinetic study in normal and Alzheimer's disease rats.

PubMed

Wang, Xiaotong; Zhang, Yue; Niu, Huibin; Geng, Yajing; Wang, Bing; Yang, Xiaomei; Yan, Pengyu; Li, Qing; Bi, Kaishun

2017-05-01

A method of ultra-fast liquid chromatography with tandem mass spectrometry was developed and validated for the simultaneous quantitation of eight bioactive components, including polygalaxanthone III, sibiricaxanthone B, tenuifolin, sibiricose A5, sibiricose A6, tenuifoliside A, ginsenoside Re and ginsenoside Rb1 in rat plasma after oral administration of Kai-Xin-San. The plasma samples were extracted by liquid-liquid extraction using digoxin as an internal standard. Chromatographic separation was performed on a Venusil MP C 18 column (100 mm × 2.1 mm, 3 μm) with methanol and 0.05% acetic acid in water as mobile phase. The tandem mass spectrometric detection was performed in the multiple reaction monitoring with turbo ion spray source in the negative ionization. Validation parameters were within acceptable ranges. The established method has been successfully applied to compare the pharmacokinetic profiles of the analytes between normal and Alzheimer's disease rats. The results indicated that there were significant differences in pharmacokinetic parameters of some components between two groups, which may be due to the mechanisms of Alzheimer's disease and pharmacological effects of the analytes. The pharmacokinetic research in the pathological state might provide more useful information to guide the clinical usage of herbal medicine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antihyperglycemic effect of the traditional Chinese scutellaria-coptis herb couple and its main components in streptozotocin-induced diabetic rats.

PubMed

Liu, Sheng-Zi; Deng, Yuan-Xiong; Chen, Bo; Zhang, Xiao-Jie; Shi, Qun-Zhi; Qiu, Xi-Min

2013-01-30

Scutellaria-coptis herb couple (SC) is the main herb couple in many traditional Chinese compound formulas used for the treatment of diabetes mellitus, which has been used to treat diabetes mellitus for thousands of years in China. In this study we provide experimental evidence for the clinical use of SC in the treatment of diabetes mellitus. To confirm the anti-diabetic effect of SC extract and its main components, and to explore its mechanism from the effect on intestinal disaccharidases by in vivo and in vitro experiment. SC extract was prepared and the main components (namely berberine and baicalin) contained in the extract were assayed with high performance liquid chromatography (HPLC). And diabetic model rats were induced by intraperitoneal injection of streptozotocin (STZ). After grouped randomly, diabetic rats were administered SC extract, berberine, baicalin, berberine+baicalin, acarbose and vehicle for 33d, respectively. Body weight, food intake, urine volume, urine sugars, fasting plasma glucose and fasting plasma insulin were monitored to evaluate the antidiabetic effects on diabetic rats. Intestinal mucosa homogenate was prepared and the activities of intestinal disaccharidases were assayed. Moreover, oral sucrose tolerance test (OSTT) was performed and the inhibitory effects of SC extract and its main components (berberine and baicalin) on the maltase and sucrase in vitro was evaluated. After the treatment of SC extract and its main components, the body weight and the fasting plasma insulin level were found to be increased while food intake, urine volume, urine sugars and fasting plasma were decreased. OSTT showed that SC extract and its main components could lower the postprandial plasma glucose level of diabetic rats. Furthermore, SC extract and its main components could inhibit the activities of intestinal disaccharidases in diabetic rats, whereas only SC extract and berberine could inhibit the activity of maltase in vitro. According to our present findings, scutellaria-coptis herb couple (SC) possessed potent anti-hyperglycemic effect on STZ-induced diabetic rats. And SC extract and its main components exerted anti-hyperglycemic effect partly via inhibiting the increased activities of intestinal disaccharidases and elevating the level of plasma insulin in diabetic rats induced by STZ. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

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

PubMed

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

2016-06-01

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

Rapid characterization of the chemical constituents of Cortex Fraxini by homogenate extraction followed by UHPLC coupled with Fourier transform ion cyclotron resonance mass spectrometry and GC-MS.

PubMed

Wang, Yinan; Han, Fei; Song, Aihua; Wang, Miao; Zhao, Min; Zhao, Chunjie

2016-11-01

Cortex Fraxini is an important traditional Chinese medicine. In this work, a rapid and reliable homogenate extraction method was applied for the fast extraction for Cortex Fraxini, and the method was optimized by response surface methodology. Ultra high performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry and gas chromatography with mass spectrometry were established for the separation and characterization of the constituents of Cortex Fraxini. Liquid chromatography separation was conducted on a C 18 column (150 mm × 2.1 mm, 1.8 μm), and gas chromatography separation was performed on a capillary with a 5% phenyl-methylpolysiloxane stationary phase (30 m × 0.25 mm × 0.25 mm) by injection of silylated samples. According to the results, 33 chemical compounds were characterized by liquid chromatography with mass spectrometry, and 11 chemical compounds were characterized by gas chromatography with mass spectrometry, and coumarins were the major components characterized by both gas chromatography with mass spectrometry and liquid chromatography with mass spectrometry. The proposed homogenate extraction was an efficient and rapid method, and coumarins, phenylethanoid glycosides, iridoid glycosides, phenylpropanoids, and lignans were the main constituents of Cortex Fraxini. This work laid the foundation for further study of Cortex Fraxini and will be helpful for the rapid extraction and characterization of ingredients in other traditional Chinese medicines. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

General purpose algorithms for characterization of slow and fast phase nystagmus

NASA Technical Reports Server (NTRS)

Lessard, Charles S.

1987-01-01

In the overall aim for a better understanding of the vestibular and optokinetic systems and their roles in space motion sickness, the eye movement responses to various dynamic stimuli are measured. The vestibulo-ocular reflex (VOR) and the optokinetic response, as the eye movement responses are known, consist of slow phase and fast phase nystagmus. The specific objective is to develop software programs necessary to characterize the vestibulo-ocular and optokinetic responses by distinguishing between the two phases of nystagmus. The overall program is to handle large volumes of highly variable data with minimum operator interaction. The programs include digital filters, differentiation, identification of fast phases, and reconstruction of the slow phase with a least squares fit such that sinusoidal or psuedorandom data may be processed with accurate results. The resultant waveform, slow phase velocity eye movements, serves as input data to the spectral analysis programs previously developed for NASA to analyze nystagmus responses to pseudorandom angular velocity inputs.

Fast-scale non-linear distortion analysis of peak-current-controlled buck-boost inverters

NASA Astrophysics Data System (ADS)

Zhang, Hao; Dong, Shuai; Yi, Chuanzhi; Guan, Weimin

2018-02-01

This paper deals with fast-scale non-linear distortion behaviours including asymmetrical period-doubling bifurcation and zero-crossing distortion in peak-current-controlled buck-boost inverters. The underlying mechanisms of the fast-scale non-linear distortion behaviours in inverters are revealed. The folded bifurcation diagram is presented to analyse the asymmetrical phenomenon of fast-scale period-doubling bifurcation. In view of the effect of phase shift and current ripple, the analytical expressions for one pair of critical phase angles are derived by using the design-oriented geometrical current approach. It is shown that the phase shift between inductor current and capacitor voltage should be responsible for the zero-crossing distortion phenomenon. These results obtained here are useful to optimise the circuit design and improve the circuit performance.

Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

PubMed

Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

2017-03-01

An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Real-time high-resolution heterodyne-based measurements of spectral dynamics in fibre lasers

PubMed Central

Sugavanam, Srikanth; Fabbri, Simon; Le, Son Thai; Lobach, Ivan; Kablukov, Sergey; Khorev, Serge; Churkin, Dmitry

2016-01-01

Conventional tools for measurement of laser spectra (e.g. optical spectrum analysers) capture data averaged over a considerable time period. However, the generation spectrum of many laser types may involve spectral dynamics whose relatively fast time scale is determined by their cavity round trip period, calling for instrumentation featuring both high temporal and spectral resolution. Such real-time spectral characterisation becomes particularly challenging if the laser pulses are long, or they have continuous or quasi-continuous wave radiation components. Here we combine optical heterodyning with a technique of spatio-temporal intensity measurements that allows the characterisation of such complex sources. Fast, round-trip-resolved spectral dynamics of cavity-based systems in real-time are obtained, with temporal resolution of one cavity round trip and frequency resolution defined by its inverse (85 ns and 24 MHz respectively are demonstrated). We also show how under certain conditions for quasi-continuous wave sources, the spectral resolution could be further increased by a factor of 100 by direct extraction of phase information from the heterodyned dynamics or by using double time scales within the spectrogram approach. PMID:26984634

Fast multiclonal clusterization of V(D)J recombinations from high-throughput sequencing.

PubMed

Giraud, Mathieu; Salson, Mikaël; Duez, Marc; Villenet, Céline; Quief, Sabine; Caillault, Aurélie; Grardel, Nathalie; Roumier, Christophe; Preudhomme, Claude; Figeac, Martin

2014-05-28

V(D)J recombinations in lymphocytes are essential for immunological diversity. They are also useful markers of pathologies. In leukemia, they are used to quantify the minimal residual disease during patient follow-up. However, the full breadth of lymphocyte diversity is not fully understood. We propose new algorithms that process high-throughput sequencing (HTS) data to extract unnamed V(D)J junctions and gather them into clones for quantification. This analysis is based on a seed heuristic and is fast and scalable because in the first phase, no alignment is performed with germline database sequences. The algorithms were applied to TR γ HTS data from a patient with acute lymphoblastic leukemia, and also on data simulating hypermutations. Our methods identified the main clone, as well as additional clones that were not identified with standard protocols. The proposed algorithms provide new insight into the analysis of high-throughput sequencing data for leukemia, and also to the quantitative assessment of any immunological profile. The methods described here are implemented in a C++ open-source program called Vidjil.

Fast preconcentration of trace rare earth elements from environmental samples by di(2-ethylhexyl)phosphoric acid grafted magnetic nanoparticles followed by inductively coupled plasma mass spectrometry detection

NASA Astrophysics Data System (ADS)

Yan, Ping; He, Man; Chen, Beibei; Hu, Bin

2017-10-01

In this work, di(2-ethylhexyl)phosphoric acid (P204) grafted magnetic nanoparticles were synthesized by fabricating P204 onto Fe3O4@TiO2 nanoparticles based on Lewis acid-base interaction between Ti and phosphate group under weakly acidic condition. The prepared Fe3O4@TiO2@P204 nanoparticles exhibited excellent selectivity for rare earth elements, and good anti-interference ability. Based on it, a method of magnetic solid phase extraction (MSPE) combined with inductively coupled plasma mass spectrometry (ICP-MS) was developed for fast preconcentration and determination of trace rare earth elements in environmental samples. Under the optimal conditions, the detection limits of rare earth elements were in the range of 0.01 (Tm)-0.12 (Nd) ng L- 1 with an enrichment factor of 100-fold, and the relative standard deviations ranged from 4.9 (Pr) to 10.7% (Er). The proposed method was successfully applied to the determination of rare earth elements in environmental samples, including river water, lake water, seawater and sediment.

A Novel Framework Based on FastICA for High Density Surface EMG Decomposition

PubMed Central

Chen, Maoqi; Zhou, Ping

2015-01-01

This study presents a progressive FastICA peel-off (PFP) framework for high density surface electromyogram (EMG) decomposition. The novel framework is based on a shift-invariant model for describing surface EMG. The decomposition process can be viewed as progressively expanding the set of motor unit spike trains, which is primarily based on FastICA. To overcome the local convergence of FastICA, a “peel off” strategy (i.e. removal of the estimated motor unit action potential (MUAP) trains from the previous step) is used to mitigate the effects of the already identified motor units, so more motor units can be extracted. Moreover, a constrained FastICA is applied to assess the extracted spike trains and correct possible erroneous or missed spikes. These procedures work together to improve the decomposition performance. The proposed framework was validated using simulated surface EMG signals with different motor unit numbers (30, 70, 91) and signal to noise ratios (SNRs) (20, 10, 0 dB). The results demonstrated relatively large numbers of extracted motor units and high accuracies (high F1-scores). The framework was also tested with 111 trials of 64-channel electrode array experimental surface EMG signals during the first dorsal interosseous (FDI) muscle contraction at different intensities. On average 14.1 ± 5.0 motor units were identified from each trial of experimental surface EMG signals. PMID:25775496

[Safety assessment of stevia rebaudiana bertoni grown in southeastern Mexico as food sweetener].

PubMed

Aranda-González, Irma; Barbosa-Martín, Enrique; Toraya-Avilés, Rocío; Segura-Campos, Maira; Moguel-Ordoñez, Yolanda; Betancur-Ancona, David

2014-09-01

Stevia rebaudiana leaves and their glycosides have been recently and significantly used so important as sweeteners. However, it has been reported an antihyperglycemic effect of the extract and a glycoside. The aim of this study was to quantify S. rebaudiana glycosides, assess cytotoxicity of the extract and its acute and chronic effect on blood glucose in animal models and in human. The glycosides of the Morita II and Criolla extract were quantified by HPLC, using a C18 column (250 mm x 4.6 mm and particle size of 5 uM) with UV detection at 210 nm, mobile phase of acetonitrile/sodium phosphate buffer 10 mmol/L, pH 2.6 (32:68 v/v). Cytotoxicity study was performed in Vero cells, whereas an intraperitoneal glucose tolerance test (IPGTT) and a chronic consumption assay (4 weeks) were executed in an animal model of diabetes; finally the glycemic index (G.I.) was determined in healthy individuals. The glycoside content is higher in the Morita variety II although both had a CC50 >300 g/mL. The areas under the curve of the IPGTT and fasting glucose of the animals were not significantly different (p> 0.05) and the I.G. extract was 11.11 %, which classifies the extract as low I.G. The extract of S. rebaudiana Morita II has a low glycemic index and, in the doses tested, is not cytotoxic nor has acute or chronic effect on blood sugar, which makes it a safe sweetener. Copyright AULA MEDICA EDICIONES 2014. Published by AULA MEDICA. All rights reserved.

Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry

USGS Publications Warehouse

Zhang, Caixiang; Eganhouse, Robert P.; Pontolillo, James; Cozzarelli, Isabelle M.; Wang, Yanxin

2012-01-01

4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid–liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC × GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment.

Process for radioisotope recovery and system for implementing same

DOEpatents

Meikrantz, David H [Idaho Falls, ID; Todd, Terry A [Aberdeen, ID; Tranter, Troy J [Idaho Falls, ID; Horwitz, E Philip [Naperville, IL

2009-10-06

A method of recovering daughter isotopes from a radioisotope mixture. The method comprises providing a radioisotope mixture solution comprising at least one parent isotope. The at least one parent isotope is extracted into an organic phase, which comprises an extractant and a solvent. The organic phase is substantially continuously contacted with an aqueous phase to extract at least one daughter isotope into the aqueous phase. The aqueous phase is separated from the organic phase, such as by using an annular centrifugal contactor. The at least one daughter isotope is purified from the aqueous phase, such as by ion exchange chromatography or extraction chromatography. The at least one daughter isotope may include actinium-225, radium-225, bismuth-213, or mixtures thereof. A liquid-liquid extraction system for recovering at least one daughter isotope from a source material is also disclosed.

Process for radioisotope recovery and system for implementing same

DOEpatents

Meikrantz, David H.; Todd, Terry A.; Tranter, Troy J.; Horwitz, E. Philip

2007-01-02

A method of recovering daughter isotopes from a radioisotope mixture. The method comprises providing a radioisotope mixture solution comprising at least one parent isotope. The at least one parent isotope is extracted into an organic phase, which comprises an extractant and a solvent. The organic phase is substantially continuously contacted with an aqueous phase to extract at least one daughter isotope into the aqueous phase. The aqueous phase is separated from the organic phase, such as by using an annular centrifugal contactor. The at least one daughter isotope is purified from the aqueous phase, such as by ion exchange chromatography or extraction chromatography. The at least one daughter isotope may include actinium-225, radium-225, bismuth-213, or mixtures thereof. A liquid-liquid extraction system for recovering at least one daughter isotope from a source material is also disclosed.

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

PubMed

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

2016-06-25

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

Fast liquid chromatographic-tandem mass spectrometric method using mixed-mode phase chromatography and solid phase extraction for the determination of 12 mono-hydroxylated brominated diphenyl ethers in human serum.

PubMed

Petropoulou, Syrago-Styliani E; Duong, Wendy; Petreas, Myrto; Park, June-Soo

2014-08-22

Hydroxylated polybrominated diphenyl ethers (OH-PBDEs) are formed from the oxidative metabolism of polybrominated diphenyl ethers (PBDEs) in humans, rats and mice, but their quantitation in human blood and other matrices with liquid chromatography-mass spectrometric techniques has been a challenge. In this study, a novel analytical method was developed and validated using only 250 μL of human serum for the quantitation of twelve OH-PBDEs, fully chromatographically separated in a 15 min analytical run. This method includes two novel approaches: an enzymatic hydrolysis procedure and a chromatographic separation using a mixed mode chromatography column. The enzymatic hydrolysis (EH) was found critical for 4'-OH-BDE17, which was not detectable without it. For the sample clean up, a solid phase extraction protocol was developed and validated for the extraction of the 12 congeners from human serum. In addition, for the first time baseline resolution of two components was achieved that correspond to a single peak previously identified as 6'-OH-BDE99. The method was validated for linearity, accuracy, precision, matrix effects, limit of quantification, limit of detection, sample stability and overall efficiency. Recoveries (absolute and relative) ranged from 66 to 130% with relative standard deviations <21% for all analytes. Limit of detection and quantitation ranged from 4 to 90 pg mL(-1) and 6-120 pg mL(-1), respectively, with no carry over effects. This method was applied in ten commercially available human serum samples from the general US population. The mean values of the congeners detected in all samples are 4'-OH-BDE17 (34.2 pg mL(-1)), 4-OH-BDE42 (33.9 pg mL(-1)), 5-OH-BDE47 (17.5 pg mL(-1)) and 4'-OH-BDE49 (12.4 pg mL(-1)). Copyright © 2014 Elsevier B.V. All rights reserved.

Speckle-interferometric measurement system of 3D deformation to obtain thickness changes of thin specimen under tensile loads

NASA Astrophysics Data System (ADS)

Kowarsch, Robert; Zhang, Jiajun; Sguazzo, Carmen; Hartmann, Stefan; Rembe, Christian

2017-06-01

The analysis of materials and geometries in tensile tests and the extraction of mechanic parameters is an important field in solid mechanics. Especially the measurement of thickness changes is important to obtain accurate strain information of specimens under tensile loads. Current optical measurement methods comprising 3D digital image correlation enable thickness-change measurement only with nm-resolution. We present a phase-shifting electronic speckle-pattern interferometer in combination with speckle-correlation technique to measure the 3D deformation. The phase-shift for the interferometer is introduced by fast wavelength tuning of a visible diode laser by injection current. In a post-processing step, both measurements can be combined to reconstruct the 3D deformation. In this contribution, results of a 3Ddeformation measurement for a polymer membrane are presented. These measurements show sufficient resolution for the detection of 3D deformations of thin specimen in tensile test. In future work we address the thickness changes of thin specimen under tensile loads.

Exploring a Multiphysics Resolution Approach for Additive Manufacturing

NASA Astrophysics Data System (ADS)

Estupinan Donoso, Alvaro Antonio; Peters, Bernhard

2018-06-01

Metal additive manufacturing (AM) is a fast-evolving technology aiming to efficiently produce complex parts while saving resources. Worldwide, active research is being performed to solve the existing challenges of this growing technique. Constant computational advances have enabled multiscale and multiphysics numerical tools that complement the traditional physical experimentation. In this contribution, an advanced discrete-continuous concept is proposed to address the physical phenomena involved during laser powder bed fusion. The concept treats powder as discrete by the extended discrete element method, which predicts the thermodynamic state and phase change for each particle. The fluid surrounding is solved with multiphase computational fluid dynamics techniques to determine momentum, heat, gas and liquid transfer. Thus, results track the positions and thermochemical history of individual particles in conjunction with the prevailing fluid phases' temperature and composition. It is believed that this methodology can be employed to complement experimental research by analysis of the comprehensive results, which can be extracted from it to enable AM processes optimization for parts qualification.

3S (Safeguards, Security, Safety) based pyroprocessing facility safety evaluation plan

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

Ku, J.H.; Choung, W.M.; You, G.S.

The big advantage of pyroprocessing for the management of spent fuels against the conventional reprocessing technologies lies in its proliferation resistance since the pure plutonium cannot be separated from the spent fuel. The extracted materials can be directly used as metal fuel in a fast reactor, and pyroprocessing reduces drastically the volume and heat load of the spent fuel. KAERI has implemented the SBD (Safeguards-By-Design) concept in nuclear fuel cycle facilities. The goal of SBD is to integrate international safeguards into the entire facility design process since the very beginning of the design phase. This paper presents a safety evaluationmore » plan using a conceptual design of a reference pyroprocessing facility, in which 3S (Safeguards, Security, Safety)-By-Design (3SBD) concept is integrated from early conceptual design phase. The purpose of this paper is to establish an advanced pyroprocessing hot cell facility design concept based on 3SBD for the successful realization of pyroprocessing technology with enhanced safety and proliferation resistance.« less

Incorporation of the Time-Varying Postprandial Increase in Splanchnic Blood Flow into a PBPK Model to Predict the Effect of Food on the Pharmacokinetics of Orally Administered High-Extraction Drugs.

PubMed

Rose, Rachel H; Turner, David B; Neuhoff, Sibylle; Jamei, Masoud

2017-07-01

Following a meal, a transient increase in splanchnic blood flow occurs that can result in increased exposure to orally administered high-extraction drugs. Typically, physiologically based pharmacokinetic (PBPK) models have incorporated this increase in blood flow as a time-invariant fed/fasted ratio, but this approach is unable to explain the extent of increased drug exposure. A model for the time-varying increase in splanchnic blood flow following a moderate- to high-calorie meal (TV-Q Splanch ) was developed to describe the observed data for healthy individuals. This was integrated within a PBPK model and used to predict the contribution of increased splanchnic blood flow to the observed food effect for two orally administered high-extraction drugs, propranolol and ibrutinib. The model predicted geometric mean fed/fasted AUC and C max ratios of 1.24 and 1.29 for propranolol, which were within the range of published values (within 1.0-1.8-fold of values from eight clinical studies). For ibrutinib, the predicted geometric mean fed/fasted AUC and C max ratios were 2.0 and 1.84, respectively, which was within 1.1-fold of the reported fed/fasted AUC ratio but underestimated the reported C max ratio by up to 1.9-fold. For both drugs, the interindividual variability in fed/fasted AUC and C max ratios was underpredicted. This suggests that the postprandial change in splanchnic blood flow is a major mechanism of the food effect for propranolol and ibrutinib but is insufficient to fully explain the observations. The proposed model is anticipated to improve the prediction of food effect for high-extraction drugs, but should be considered with other mechanisms.

Functionalized nanoparticles based solid-phase membrane micro-tip extraction and high-performance liquid chromatography analyses of vitamin B complex in human plasma.

PubMed

Ali, Imran; Kulsum, Umma; Al-Othman, Zeid A; Alwarthan, Abdulrahman; Saleem, Kishwar

2016-07-01

Iron nanoparticles were prepared by a green method following functionalization using 1-butyl-3-methylimidazolium bromide. 1-Butyl-3-methylimidazole iron nanoparticles were characterized using FTIR spectroscopy, energy dispersive X-ray fluorescence, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The nanoparticles were used in solid-phase membrane micro-tip extraction to separate vitamin B complex from plasma before high-performance liquid chromatography. The optimum conditions obtained were sorbent (15 mg), agitation time (30 min), pH (9.0), desorbing solvent [water (5 mL) + methanol (5 mL) + sodium hydroxide (0.1 N) + acetic acid (d = 1.05 kg/L, pH 5.5), desorbing volume (10 mL) and desorption time (30 min). The percentage recoveries of all the eight vitamin B complex were from 60 to 83%. A high-performance liquid chromatography method was developed using a PhE column (250 × 4.6 mm, 5.0 μm) and water/acetonitrile (95:5, v/v; pH 4.0 with 0.1% formic acid) mobile phase. The flow rate was 1.0 mL/min with detection at 270 and 210 nm. The values of the capacity, separation and resolution factor were 0.57-39.47, 1.12-6.00 and 1.84-26.26, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economic and reproducible. The developed method can be applied for analyzing these drugs in biological and environmental matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Simple, Fast, Low Cost, HPLC/UV Validated Method for Determination of Flutamide: Application to Protein Binding Studies.

PubMed

Esmaeilzadeh, Sara; Valizadeh, Hadi; Zakeri-Milani, Parvin

2016-06-01

The main goal of this study was development of a reverse phase high performance liquid chromatography (RP-HPLC) method for flutamide quantitation which is applicable to protein binding studies. Ultrafilteration method was used for protein binding study of flutamide. For sample analysis, flutamide was extracted by a simple and low cost extraction method using diethyl ether and then was determined by HPLC/UV. Acetanilide was used as an internal standard. The chromatographic system consisted of a reversed-phase C8 column with C8 pre-column, and the mobile phase of a mixture of 29% (v/v) methanol, 38% (v/v) acetonitrile and 33% (v/v) potassium dihydrogen phosphate buffer (50 mM) with pH adjusted to 3.2. Acetanilide and flutamide were eluted at 1.8 and 2.9 min, respectively. The linearity of method was confirmed in the range of 62.5-16000 ng/ml (r(2) > 0.99). The limit of quantification was shown to be 62.5 ng/ml. Precision and accuracy ranges found to be (0.2-1.4%, 90-105%) and (0.2-5.3 %, 86.7-98.5 %) respectively. Acetanilide and flutamide capacity factor values of 1.35 and 2.87, tailing factor values of 1.24 and 1.07 and resolution values of 1.8 and 3.22 were obtained in accordance with ICH guidelines. Based on the obtained results a rapid, precise, accurate, sensitive and cost-effective analysis procedure was proposed for quantitative determination of flutamide.

A Simple, Fast, Low Cost, HPLC/UV Validated Method for Determination of Flutamide: Application to Protein Binding Studies

PubMed Central

Esmaeilzadeh, Sara; Valizadeh, Hadi; Zakeri-Milani, Parvin

2016-01-01

Purpose: The main goal of this study was development of a reverse phase high performance liquid chromatography (RP-HPLC) method for flutamide quantitation which is applicable to protein binding studies. Methods: Ultrafilteration method was used for protein binding study of flutamide. For sample analysis, flutamide was extracted by a simple and low cost extraction method using diethyl ether and then was determined by HPLC/UV. Acetanilide was used as an internal standard. The chromatographic system consisted of a reversed-phase C8 column with C8 pre-column, and the mobile phase of a mixture of 29% (v/v) methanol, 38% (v/v) acetonitrile and 33% (v/v) potassium dihydrogen phosphate buffer (50 mM) with pH adjusted to 3.2. Results: Acetanilide and flutamide were eluted at 1.8 and 2.9 min, respectively. The linearity of method was confirmed in the range of 62.5-16000 ng/ml (r2 > 0.99). The limit of quantification was shown to be 62.5 ng/ml. Precision and accuracy ranges found to be (0.2-1.4%, 90-105%) and (0.2-5.3 %, 86.7-98.5 %) respectively. Acetanilide and flutamide capacity factor values of 1.35 and 2.87, tailing factor values of 1.24 and 1.07 and resolution values of 1.8 and 3.22 were obtained in accordance with ICH guidelines. Conclusion: Based on the obtained results a rapid, precise, accurate, sensitive and cost-effective analysis procedure was proposed for quantitative determination of flutamide. PMID:27478788

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review.

PubMed

Rahman, Md Musfiqur; Abd El-Aty, A M; Kim, Sung-Woo; Shin, Sung Chul; Shin, Ho-Chul; Shim, Jae-Han

2017-01-01

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A wide range real-time synchronous demodulation system for the dispersion interferometer on HL-2M

NASA Astrophysics Data System (ADS)

Wu, Tongyu; Zhang, Wei; Yin, Zejie

2017-09-01

A real-time synchronous demodulation system has been developed for the dispersion interferometer on a HL-2M tokamak. The system is based on the phase extraction method which uses a ratio of modulation amplitudes. A high-performance field programmable gate array with pipeline process capabilities is used to realize the real time synchronous demodulation algorithm. A fringe jump correction algorithm is applied to follow the fast density changes of the plasma. By using the Peripheral Component Interconnect Express protocol, the electronics can perform real-time density feedback with a temporal resolution of 100 ns. Some experimental results presented show that the electronics can obtain a wide measurement range of 2.28 × 1022 m-2 with high precision.

Modulating complex beams in amplitude and phase using fast tilt-micromirror arrays and phase masks.

PubMed

Roth, Matthias; Heber, Jörg; Janschek, Klaus

2018-06-15

The Letter proposes a system for the spatial modulation of light in amplitude and phase at kilohertz frame rates and high spatial resolution. The focus is fast spatial light modulators (SLMs) consisting of continuously tiltable micromirrors. We investigate the utilization of such SLMs in combination with a static phase mask in a 4f setup. The phase mask enables the complex beam modulation in a linear optical arrangement. Furthermore, adding so-called phase steps to the phase mask increases both the number of image pixels at constant SLM resolution and the optical efficiency. We illustrate our concept based on numerical simulations.

Recent advances in analytical methods for the determination of 4-alkylphenols and bisphenol A in solid environmental matrices: A critical review.

PubMed

Salgueiro-González, N; Castiglioni, S; Zuccato, E; Turnes-Carou, I; López-Mahía, P; Muniategui-Lorenzo, S

2018-09-18

The problem of endocrine disrupting compounds (EDCs) in the environment has become a worldwide concern in recent decades. Besides their toxicological effects at low concentrations and their widespread use in industrial and household applications, these pollutants pose a risk for non-target organisms and also for public safety. Analytical methods to determine these compounds at trace levels in different matrices are urgently needed. This review critically discusses trends in analytical methods for well-known EDCs like alkylphenols and bisphenol A in solid environmental matrices, including sediment and aquatic biological samples (from 2006 to 2018). Information about extraction, clean-up and determination is covered in detail, including analytical quality parameters (QA/QC). Conventional and novel analytical techniques are compared, with their advantages and drawbacks. Ultrasound assisted extraction followed by solid phase extraction clean-up is the most widely used procedure for sediment and aquatic biological samples, although softer extraction conditions have been employed for the latter. The use of liquid chromatography followed by tandem mass spectrometry has greatly increased in the last five years. The majority of these methods have been employed for the analysis of river sediments and bivalve molluscs because of their usefulness in aquatic ecosystem (bio)monitoring programs. Green, simple, fast analytical methods are now needed to determine these compounds in complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis of lab-in-a-pipette-tip extraction using hydrophilic nano-sized dummy molecularly imprinted polymer for purification and analysis of prednisolone.

PubMed

Arabi, Maryam; Ghaedi, Mehrorang; Ostovan, Abbas; Wang, Shaobin

2016-10-15

A novel pipette-tip based on nano-sized dummy molecularly imprinted polymer (PT-DMIP) assisted by ultrasonication for the effective enrichment and analysis of prednisolone from urine samples was developed. The PT-DMIP cartridge was prepared by packing the dummy molecularly imprinted polymer at the tip of the micropipette. The polymerization used betamethasone (BM) as the dummy template, 3-aminopropyltrimethoxysilane (APTMS) as the functionalized monomer, tetraethyl orthosilicate (TEOS) as the cross-linker and aluminum ion (Al(3+)) as a dopant to produce Lewis acid sites in the silica matrix for metal coordinative interactions with the analyte. Compared to conventional solid phase extraction (SPE), the PT-DMIP is cost-effective, fast, and easy to handle, while the system is very approachable and reduces the consumption of toxic organic solvent. HPLC-UV analysis revealed successful applicability of the sorbent for highly efficient extraction of perdnisolone from urine matrices. The extraction recovery was investigated and optimum conditions were obtained using central composite design. Good linearity for prednisolone in the range of 0.22-220μgL(-1) with regression coefficients of 0.99 reveals high applicability of the method for trace analysis. Under the optimized conditions, the recoveries are 89.0-96.1 with relative standard deviations (RSD) of less than 9.0%. Copyright © 2016 Elsevier Inc. All rights reserved.

FastChem: An ultra-fast equilibrium chemistry

NASA Astrophysics Data System (ADS)

Kitzmann, Daniel; Stock, Joachim

2018-04-01

FastChem is an equilibrium chemistry code that calculates the chemical composition of the gas phase for given temperatures and pressures. Written in C++, it is based on a semi-analytic approach, and is optimized for extremely fast and accurate calculations.

Solid state amorphization of metastable Al 0.5TiZrPdCuNi high entropy alloy investigated by high voltage electron microscopy

DOE PAGES

Nagase, Takeshi; Takeuchi, Akira; Amiya, Kenji; ...

2017-07-18

Here, the phase stability of high entropy alloy (HEA), Al 0.5TiZrPdCuNi, under fast electron irradiation was studied by in-situ high voltage electron microscopy (HVEM). The initial phase of this alloy quenched from the melt was dependent on cooling rate. At high cooling rates an amorphous phase was obtained, whereas a body-centered cubic ( b.c.c.) phase were obtained at low cooling rates. By thermal crystallization of the amorphous phase b.c.c. phase nano-crystals were formed. Upon fast electron irradiation solid state amorphization (SSA) was observed in b.c.c. phase regardless of the initial microstructure (i.e., “coarse crystalline structure” or “nano-crystalline structure with grainmore » boundaries as a sink for point defects”). SSA behavior in the Al 0.5TiZrPdCuNi HEAs was investigated by in-situ transmission electron microscopy observations. Because the amorphization is very rarely achieved in a solid solution phase under fast electron irradiation in common metallic materials, this result suggests that the Al 0.5TiZrPdCuNi HEA from other common alloys and the other HEAs. The differences in phase stability against the irradiation between the Al 0.5TiZrPdCuNi HEA and the other HEAs were discussed. This is the first experimental evidence of SSA in HEAs stimulated by fast electron irradiation.« less

Fast Crystallization of the Phase Change Compound GeTe by Large-Scale Molecular Dynamics Simulations.

PubMed

Sosso, Gabriele C; Miceli, Giacomo; Caravati, Sebastiano; Giberti, Federico; Behler, Jörg; Bernasconi, Marco

2013-12-19

Phase change materials are of great interest as active layers in rewritable optical disks and novel electronic nonvolatile memories. These applications rest on a fast and reversible transformation between the amorphous and crystalline phases upon heating, taking place on the nanosecond time scale. In this work, we investigate the microscopic origin of the fast crystallization process by means of large-scale molecular dynamics simulations of the phase change compound GeTe. To this end, we use an interatomic potential generated from a Neural Network fitting of a large database of ab initio energies. We demonstrate that in the temperature range of the programming protocols of the electronic memories (500-700 K), nucleation of the crystal in the supercooled liquid is not rate-limiting. In this temperature range, the growth of supercritical nuclei is very fast because of a large atomic mobility, which is, in turn, the consequence of the high fragility of the supercooled liquid and the associated breakdown of the Stokes-Einstein relation between viscosity and diffusivity.

Autonomous celestial navigation based on Earth ultraviolet radiance and fast gradient statistic feature extraction

NASA Astrophysics Data System (ADS)

Lu, Shan; Zhang, Hanmo

2016-01-01

To meet the requirement of autonomous orbit determination, this paper proposes a fast curve fitting method based on earth ultraviolet features to obtain accurate earth vector direction, in order to achieve the high precision autonomous navigation. Firstly, combining the stable characters of earth ultraviolet radiance and the use of transmission model software of atmospheric radiation, the paper simulates earth ultraviolet radiation model on different time and chooses the proper observation band. Then the fast improved edge extracting method combined Sobel operator and local binary pattern (LBP) is utilized, which can both eliminate noises efficiently and extract earth ultraviolet limb features accurately. And earth's centroid locations on simulated images are estimated via the least square fitting method using part of the limb edges. Taken advantage of the estimated earth vector direction and earth distance, Extended Kalman Filter (EKF) is applied to realize the autonomous navigation finally. Experiment results indicate the proposed method can achieve a sub-pixel earth centroid location estimation and extremely enhance autonomous celestial navigation precision.

Panofsky magnet for the beam extraction from the synchrotron using a fast Q-magnet and RF-knockout

NASA Astrophysics Data System (ADS)

Masubuchi, S.; Nakanishi, T.

2011-12-01

The fast control of the beam spill extracted from a synchrotron is a key function for the spot scanning irradiation in cancer therapy application. The authors propose an extraction method which uses the quadruple field of fast response, as well as the RF-knockout. A Panofsky magnet was developed as a quadruple magnet, with a frequency response of around 10 kHz. The Panofsky magnet has a rectangular beam aperture and plate coils attached to the pole face. A model magnet has been manufactured with ferrite, and static and dynamic magnetic fields were measured. From the measurement we observed that the effects of eddy current in the plate coils were large and the uniformity of the magnetic field gradient in the beam aperture was worse than ±5% with a plate thickness of 0.02 cm and a frequency of current of 10 kHz. For the future, in a detailed design the eddy current effects have to be taken into account.

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.

Adaptive Learning and Pruning Using Periodic Packet for Fast Invariance Extraction and Recognition

NASA Astrophysics Data System (ADS)

Chang, Sheng-Jiang; Zhang, Bian-Li; Lin, Lie; Xiong, Tao; Shen, Jin-Yuan

2005-02-01

A new learning scheme using a periodic packet as the neuronal activation function is proposed for invariance extraction and recognition of handwritten digits. Simulation results show that the proposed network can extract the invariant feature effectively and improve both the convergence and the recognition rate.

Antioxidant effects of a cinnamon extract in people with impaired fasting glucose that are overweight or obese.

PubMed

Roussel, Anne-Marie; Hininger, Isabelle; Benaraba, Rachida; Ziegenfuss, Tim N; Anderson, Richard A

2009-02-01

To determine the effects of a dried aqueous extract of cinnamon on antioxidant status of people with impaired fasting glucose that are overweight or obese. Twenty-two subjects, with impaired fasting blood glucose with BMI ranging from 25 to 45, were enrolled in a double-blind placebo-controlled trial. Subjects were given capsules containing either a placebo or 250 mg of an aqueous extract of cinnamon (Cinnulin PF) two times per day for 12 weeks. Plasma malondialdehyde (MDA) concentrations were assessed using high performance liquid chromatography and plasma antioxidant status was evaluated using ferric reducing antioxidant power (FRAP) assay. Erythrocyte Cu-Zn superoxide (Cu-Zn SOD) activity was measured after hemoglobin precipitation by monitoring the auto-oxidation of pyrogallol and erythrocyte glutathione peroxidase (GPx) activity by established methods. FRAP and plasma thiol (SH) groups increased, while plasma MDA levels decreased in subjects receiving the cinnamon extract. Effects were larger after 12 than 6 weeks. There was also a positive correlation (r = 0.74; p = 0.014) between MDA and plasma glucose. This study supports the hypothesis that the inclusion of water soluble cinnamon compounds in the diet could reduce risk factors associated with diabetes and cardiovascular disease.

Using dynamic interferometric synthetic aperature radar (InSAR) to image fast-moving surface waves

DOEpatents

Vincent, Paul

2005-06-28

A new differential technique and system for imaging dynamic (fast moving) surface waves using Dynamic Interferometric Synthetic Aperture Radar (InSAR) is introduced. This differential technique and system can sample the fast-moving surface displacement waves from a plurality of moving platform positions in either a repeat-pass single-antenna or a single-pass mode having a single-antenna dual-phase receiver or having dual physically separate antennas, and reconstruct a plurality of phase differentials from a plurality of platform positions to produce a series of desired interferometric images of the fast moving waves.

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.

Solvent Extraction of Sodium Hydroxide Using Alkylphenols and Fluorinated Alcohols: Understanding the Extraction Mechanism by Equilibrium Modeling

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

Kang, Hyun-Ah; Engle, Nancy L.; Bonnesen Peter V.

2004-03-29

In the present work, it has been the aim to examine extraction efficiencies of nine proton-ionizable alcohols (HAs) in 1-octanol and to identify both the controlling equilibria and predominant species involved in the extraction process within a thermochemical model. Distribution ratios for sodium (DNa) extraction were measured as a function of organic-phase HA and aqueous-phase NaOH molarity at 25 °C. Extraction efficiency follows the expected order of acidity of the HAs, 4-(tert-octyl) phenol (HA 1a) and 4-noctyl- a,a-bis-(trifluoromethyl)benzyl alcohol (HA 2a) being the most efficient extractants among the compounds tested. By use of the equilibrium-modeling program SXLSQI, a model formore » the extraction of NaOH has been advanced based on an ion-pair extraction by the diluent to give organic-phase Na+OH- and corresponding free ions and cation exchange by the weak acids to form monomeric organic-phase Na+A- and corresponding free organic-phase ions.« less

Simultaneous analysis of 17 diuretics in dietary supplements by HPLC and LC-MS/MS.

PubMed

Woo, H; Kim, J W; Han, K M; Lee, J H; Hwang, I S; Lee, J H; Kim, J; Kweon, S J; Cho, S; Chae, K R; Han, S Y; Kim, J

2013-01-01

In order to test health foods for illegally added diuretics for weight loss, we developed simple, rapid, selective, and sensitive methods using HPLC and LC-MS/MS for the simultaneous analysis of 17 diuretics in dietary supplements. HPLC conditions were set with a Capcell-pak C18, using a mobile phase consisting of gradient conditions, UV detection at 254 nm and validated for linearity (r(2)> 0.999), precision (CV ≤ 3%), recoveries (90.4-102.8%) and reproducibility. Identification and quantification of 17 diuretics were accomplished by ion-spray LC-MS/MS using multiple reaction monitoring (MRM). The chromatographic separation was carried out under the reversed-phase mechanism on an HSS-T3 column. The LC-MS/MS method was validated for linearity (r(2)> 0.99) and precision (CV < 13%). Sixteen dietary supplements were tested with the developed methods. Diuretics were not detected in all samples. Extraction recovery was also investigated and the extraction recoveries in different formulations were from 88% to 110% and from 81% to 116% using HPLC and LC-MS/MS, respectively. There was no significant difference in recoveries in the type of dietary supplements. Based on this result, the developed methods to monitor illegal drug adulterations in dietary supplements using HPLC and LC-MS/MS are simple, fast and reliable. Therefore, it is applicable to routine drug-adulteration screening.

Optical sectioning microscopy using two-frame structured illumination and Hilbert-Huang data processing

NASA Astrophysics Data System (ADS)

Trusiak, M.; Patorski, K.; Tkaczyk, T.

2014-12-01

We propose a fast, simple and experimentally robust method for reconstructing background-rejected optically-sectioned microscopic images using two-shot structured illumination approach. Innovative data demodulation technique requires two grid-illumination images mutually phase shifted by π (half a grid period) but precise phase displacement value is not critical. Upon subtraction of the two frames the input pattern with increased grid modulation is computed. The proposed demodulation procedure comprises: (1) two-dimensional data processing based on the enhanced, fast empirical mode decomposition (EFEMD) method for the object spatial frequency selection (noise reduction and bias term removal), and (2) calculating high contrast optically-sectioned image using the two-dimensional spiral Hilbert transform (HS). The proposed algorithm effectiveness is compared with the results obtained for the same input data using conventional structured-illumination (SIM) and HiLo microscopy methods. The input data were collected for studying highly scattering tissue samples in reflectance mode. In comparison with the conventional three-frame SIM technique we need one frame less and no stringent requirement on the exact phase-shift between recorded frames is imposed. The HiLo algorithm outcome is strongly dependent on the set of parameters chosen manually by the operator (cut-off frequencies for low-pass and high-pass filtering and η parameter value for optically-sectioned image reconstruction) whereas the proposed method is parameter-free. Moreover very short processing time required to efficiently demodulate the input pattern predestines proposed method for real-time in-vivo studies. Current implementation completes full processing in 0.25s using medium class PC (Inter i7 2,1 GHz processor and 8 GB RAM). Simple modification employed to extract only first two BIMFs with fixed filter window size results in reducing the computing time to 0.11s (8 frames/s).

The growth and structure of dark matter haloes

NASA Astrophysics Data System (ADS)

Zhao, D. H.; Mo, H. J.; Jing, Y. P.; Börner, G.

2003-02-01

In this paper, we analyse in detail the mass-accretion histories and structural properties of dark haloes in high-resolution N-body simulations. We model the density distribution in individual haloes using the Navarro-Frenk-White (NFW) profile. For a given halo, there is a tight correlation between its inner-scale radius rs and the mass within it, Ms, for all its main progenitors. Using this correlation, one can predict quite well the structural properties of a dark halo at any time in its history from its mass-accretion history, implying that the structure properties and the mass-accretion history are closely correlated. The predicted growing rate of concentration c with time tends to increase with decreasing mass-accretion rate. The build-up of dark haloes in cold dark matter (CDM) models generally consists of an early phase of fast accretion (where the halo mass Mh increases with time much faster than the expansion rate of the Universe) and a late phase of slow accretion (where Mh increases with time approximately as the expansion rate). These two phases are separated at a time when c~ 4 and the typical binding energy of the halo is approximately equal to that of a singular isothermal sphere with the same circular velocity. Haloes in the two accretion phases show systematically different properties, for example, the circular velocity vh increases rapidly with time in the fast accretion phase but remains almost constant in the slow accretion phase, the inner properties of a halo, such as rs and Ms increase rapidly with time in the fast accretion phase but change only slowly in the slow accretion phase, the inner circular velocity vs is approximately equal to vh in the fast accretion phase but is larger in the slow accretion phase. The potential well associated with a halo is built up mainly in the fast accretion phase, while a large amount of mass can be accreted in the slow accretion phase without changing the potential well significantly. We discuss our results in connection with the formation of dark haloes and galaxies in hierarchical models.

Digital multi-channel high resolution phase locked loop for surveillance radar systems

NASA Astrophysics Data System (ADS)

Rizk, Mohamed; Shaaban, Shawky; Abou-El-Nadar, Usama M.; Hafez, Alaa El-Din Sayed

This paper present a multi-channel, high resolution, fast lock phase locked loop (PLL) for surveillance radar applications. Phase detector based PLLs are simple to design, suffer no systematic phase error, and can run at the highest speed. Reducing loop gain can proportionally improve jitter performance, but also reduces locking time and pull-in range. The proposed system is based on digital process and control the error signal to the voltage controlled oscillator (VCO) adaptively to control its gain in order to achieve fast lock times while improving in lock jitter performance. Under certain circumstances the design also improves the frequency agility capability of the radar system. The results show a fast lock, high resolution PLL with transient time less than 10 µ sec which is suitable to radar applications.

A review on solid phase extraction of actinides and lanthanides with amide based extractants.

PubMed

Ansari, Seraj A; Mohapatra, Prasanta K

2017-05-26

Solid phase extraction is gaining attention from separation scientists due to its high chromatographic utility. Though both grafted and impregnated forms of solid phase extraction resins are popular, the later is easy to make by impregnating a given organic extractant on to an inert solid support. Solid phase extraction on an impregnated support, also known as extraction chromatography, combines the advantages of liquid-liquid extraction and the ion exchange chromatography methods. On the flip side, the impregnated extraction chromatographic resins are less stable against leaching out of the organic extractant from the pores of the support material. Grafted resins, on the other hand, have a higher stability, which allows their prolong use. The goal of this article is a brief literature review on reported actinide and lanthanide separation methods based on solid phase extractants of both the types, i.e., (i) ligand impregnation on the solid support or (ii) ligand functionalized polymers (chemically bonded resins). Though the literature survey reveals an enormous volume of studies on the extraction chromatographic separation of actinides and lanthanides using several extractants, the focus of the present article is limited to the work carried out with amide based ligands, viz. monoamides, diamides and diglycolamides. The emphasis will be on reported applied experimental results rather than on data pertaining fundamental metal complexation. Copyright © 2017 Elsevier B.V. All rights reserved.

Emulating the Fast-Start Swimming Performance of the Chain Pickerel (Esox niger) Using a Mechanical Fish Design

DTIC Science & Technology

2006-09-01

locomotion. The final stage is a variable phase that may include subsequent propulsive strokes or simply coasting (Ahlborn et al ., 1997...from a simulated fast-start apparatus are (Ahlborn et al ., 1997). The apparatus included a preparatory phase and propulsive phase. The paper...Science in Oceanographic Engineering at the Massachusetts Institute of Technology and the Woods Hole Oceanographic Institution September 2006

From perception to action: phase-locked gamma oscillations correlate with reaction times in a speeded response task

PubMed Central

Fründ, Ingo; Busch, Niko A; Schadow, Jeanette; Körner, Ursula; Herrmann, Christoph S

2007-01-01

Background Phase-locked gamma oscillations have so far mainly been described in relation to perceptual processes such as sensation, attention or memory matching. Due to its very short latency (≈90 ms) such oscillations are a plausible candidate for very rapid integration of sensory and motor processes. Results We measured EEG in 13 healthy participants in a speeded reaction task. Participants had to press a button as fast as possible whenever a visual stimulus was presented. The stimulus was always identical and did not have to be discriminated from other possible stimuli. In trials in which the participants showed a fast response, a slow negative potential over central electrodes starting approximately 800 ms before the response and highly phase-locked gamma oscillations over central and posterior electrodes between 90 and 140 ms after the stimulus were observed. In trials in which the participants showed a slow response, no slow negative potential was observed and phase-locked gamma oscillations were significantly reduced. Furthermore, for slow response trials the phase-locked gamma oscillations were significantly delayed with respect to fast response trials. Conclusion These results indicate the relevance of phase-locked gamma oscillations for very fast (not necessarily detailed) integration processes. PMID:17439642

Effects of intermittent fasting on health markers in those with type 2 diabetes: A pilot study.

PubMed

Arnason, Terra G; Bowen, Matthew W; Mansell, Kerry D

2017-04-15

To determine the short-term biochemical effects and clinical tolerability of intermittent fasting (IF) in adults with type 2 diabetes mellitus (T2DM). We describe a three-phase observational study (baseline 2 wk, intervention 2 wk, follow-up 2 wk) designed to determine the clinical, biochemical, and tolerability of IF in community-dwelling volunteer adults with T2DM. Biochemical, anthropometric, and physical activity measurements (using the Yale Physical Activity Survey) were taken at the end of each phase. Participants reported morning, afternoon and evening self-monitored blood glucose (SMBG) and fasting duration on a daily basis throughout all study stages, in addition to completing a remote food photography diary three times within each study phase. Fasting blood samples were collected on the final days of each study phase. At baseline, the ten participants had a confirmed diagnosis of T2DM and were all taking metformin, and on average were obese [mean body mass index (BMI) 36.90 kg/m 2 ]. We report here that a short-term period of IF in a small group of individuals with T2DM led to significant group decreases in weight (-1.395 kg, P = 0.009), BMI (-0.517, P = 0.013), and at-target morning glucose (SMBG). Although not a study requirement, all participants preferentially chose eating hours starting in the midafternoon. There was a significant increase ( P < 0.001) in daily hours fasted in the IF phase (+5.22 h), although few attained the 18-20 h fasting goal (mean 16.82 ± 1.18). The increased fasting duration improved at-goal (< 7.0 mmol/L) morning SMBG to 34.1%, from a baseline of 13.8%. Ordinal Logistic Regression models revealed a positive relationship between the increase in hours fasted and fasting glucose reaching target values ( χ 2 likelihood ratio = 8.36, P = 0.004) but not for afternoon or evening SMBG (all P > 0.1). Postprandial SMBGs were also improved during the IF phase, with 60.5% readings below 9.05 mmol/L, compared to 52.6% at baseline, and with less glucose variation. Neither insulin resistance (HOMA-IR), nor inflammatory markers (C-reactive protein) normalized during the IF phase. IF led to an overall spontaneous decrease in caloric intake as measured by food photography (Remote Food Photography Method). The data demonstrated discernable trends during IF for lower energy, carbohydrate, and fat intake when compared to baseline. Physical activity, collected by a standardized measurement tool (Yale Physical Activity Survey), increased during the intervention phase and subsequently decreased in the follow-up phase. IF was well tolerated in the majority of individuals with 6/10 participants stating they would continue with the IF regimen after the completion of the study, in a full or modified capacity ( i.e. , every other day or reduced fasting hours). The results from this pilot study indicate that short-term daily IF may be a safe, tolerable, dietary intervention in T2DM patients that may improve key outcomes including body weight, fasting glucose and postprandial variability. These findings should be viewed as exploratory, and a larger, longer study is necessary to corroborate these findings.

Effects of intermittent fasting on health markers in those with type 2 diabetes: A pilot study

PubMed Central

Arnason, Terra G; Bowen, Matthew W; Mansell, Kerry D

2017-01-01

AIM To determine the short-term biochemical effects and clinical tolerability of intermittent fasting (IF) in adults with type 2 diabetes mellitus (T2DM). METHODS We describe a three-phase observational study (baseline 2 wk, intervention 2 wk, follow-up 2 wk) designed to determine the clinical, biochemical, and tolerability of IF in community-dwelling volunteer adults with T2DM. Biochemical, anthropometric, and physical activity measurements (using the Yale Physical Activity Survey) were taken at the end of each phase. Participants reported morning, afternoon and evening self-monitored blood glucose (SMBG) and fasting duration on a daily basis throughout all study stages, in addition to completing a remote food photography diary three times within each study phase. Fasting blood samples were collected on the final days of each study phase. RESULTS At baseline, the ten participants had a confirmed diagnosis of T2DM and were all taking metformin, and on average were obese [mean body mass index (BMI) 36.90 kg/m2]. We report here that a short-term period of IF in a small group of individuals with T2DM led to significant group decreases in weight (-1.395 kg, P = 0.009), BMI (-0.517, P = 0.013), and at-target morning glucose (SMBG). Although not a study requirement, all participants preferentially chose eating hours starting in the midafternoon. There was a significant increase (P < 0.001) in daily hours fasted in the IF phase (+5.22 h), although few attained the 18-20 h fasting goal (mean 16.82 ± 1.18). The increased fasting duration improved at-goal (< 7.0 mmol/L) morning SMBG to 34.1%, from a baseline of 13.8%. Ordinal Logistic Regression models revealed a positive relationship between the increase in hours fasted and fasting glucose reaching target values (χ2 likelihood ratio = 8.36, P = 0.004) but not for afternoon or evening SMBG (all P > 0.1). Postprandial SMBGs were also improved during the IF phase, with 60.5% readings below 9.05 mmol/L, compared to 52.6% at baseline, and with less glucose variation. Neither insulin resistance (HOMA-IR), nor inflammatory markers (C-reactive protein) normalized during the IF phase. IF led to an overall spontaneous decrease in caloric intake as measured by food photography (Remote Food Photography Method). The data demonstrated discernable trends during IF for lower energy, carbohydrate, and fat intake when compared to baseline. Physical activity, collected by a standardized measurement tool (Yale Physical Activity Survey), increased during the intervention phase and subsequently decreased in the follow-up phase. IF was well tolerated in the majority of individuals with 6/10 participants stating they would continue with the IF regimen after the completion of the study, in a full or modified capacity (i.e., every other day or reduced fasting hours). CONCLUSION The results from this pilot study indicate that short-term daily IF may be a safe, tolerable, dietary intervention in T2DM patients that may improve key outcomes including body weight, fasting glucose and postprandial variability. These findings should be viewed as exploratory, and a larger, longer study is necessary to corroborate these findings. PMID:28465792

Shoulder motor performance assessment in the sagittal plane in children with hemiplegia during single joint pointing tasks.

PubMed

Formica, Domenico; Petrarca, Maurizio; Rossi, Stefano; Zollo, Loredana; Guglielmelli, Eugenio; Cappa, Paolo

2014-07-29

Pointing is a motor task extensively used during daily life activities and it requires complex visuo-motor transformation to select the appropriate movement strategy. The study of invariant characteristics of human movements has led to several theories on how the brain solves the redundancy problem, but the application of these theories on children affected by hemiplegia is limited. This study aims at giving a quantitative assessment of the shoulder motor behaviour in children with hemiplegia during pointing tasks. Eight children with hemiplegia were involved in the study and were asked to perform movements on the sagittal plane with both arms, at low and high speed. Subject movements were recorded using an optoelectronic system; a 4-DOF model of children arm has been developed to calculate kinematic and dynamic variables. A set of evaluation indexes has been extracted in order to quantitatively assess whether and how children modify their motor control strategies when perform movements with the more affected or less affected arm. In low speed movements, no differences can be seen in terms of movement duration and peak velocity between the More Affected arm (MA) and the Less Affected arm (LA), as well as in the main characteristics of movement kinematics and dynamics. As regards fast movements, remarkable differences in terms of strategies of motor control can be observed: while movements with LA did not show any significant difference in Dimensionless Jerk Index (JI) and Dimensionless Torque-change Cost index (TC) between the elevation and lowering phases, suggesting that motor control optimization is similar for movements performed with or against gravity, movements with MA showed a statistically significant increase of both JI and TC during lowering phase. Results suggest the presence of a different control strategy for fast movements in particular during lowering phase. Results suggest that motor control is not able to optimize Jerk and Torque-change cost functions in the same way when controls the two arms, suggesting that children with hemiplegia do not actively control MA lowering fast movements, in order to take advantage of the passive inertial body properties, rather than to attempt its optimal control.

Automated nystagmus analysis. [on-line computer technique for eye data processing

NASA Technical Reports Server (NTRS)

Oman, C. M.; Allum, J. H. J.; Tole, J. R.; Young, L. R.

1973-01-01

Several methods have recently been used for on-line analysis of nystagmus: A digital computer program has been developed to accept sampled records of eye position, detect fast phase components, and output cumulative slow phase position, continuous slow phase velocity, instantaneous fast phase frequency, and other parameters. The slow phase velocity is obtained by differentiation of the calculated cumulative position rather than the original eye movement record. Also, a prototype analog device has been devised which calculates the velocity of the slow phase component during caloric testing. Examples of clinical and research eye movement records analyzed with these devices are shown.

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

PubMed

Yang, Zhi; Wu, Youqian; Wu, Shihua

2016-01-29

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

Transfer Behavior of the Weakly Acidic BCS Class II Drug Valsartan from the Stomach to the Small Intestine During Fasted and Fed States.

PubMed

Hamed, Rania; Alnadi, Sabreen Hasan

2018-05-07

The objective of this study was to investigate the transfer behavior of the weakly acidic BCS class II drug valsartan from the stomach to the small intestine during fasted and fed states. An in vitro transfer model previously introduced by Kostewicz et al. (J Pharm Pharmacol 56(1):43-51, 2004) based on a syringe pump and a USP paddle apparatus was used to determine the concentration profiles of valsartan in the small intestine. Donor phases of simulated gastric fluid during fasted (FaSSGF) and fed (FeSSGF) states were used to predisperse Diovan® tablets (160 mg valsartan). The initial concentrations of valsartan in FaSSGF and FeSSGF were 6.2 and 91.8%, respectively. Valsartan dispersions were then transferred to acceptor phases that simulate intestinal fluid and cover the physiological properties (pH, buffer capacity, and ionic strength) of the gastrointestinal fluid at a flow rate of 2 mL/min. The pH measurements were reported at time intervals corresponded to those of the transfer experiments to investigate the effect of percent dissolved of valsartan in the donor phase on lowering the pH of the acceptor phases. The f2 similarity test was used to compare the concentration profiles in the acceptor phases. In fasted state, the concentration of valsartan in the acceptor phases ranged between 33.1 and 89.4% after 240 min. Whereas in fed state, valsartan was fully dissolved in all acceptor phases within a range of 94.5-104.9% after 240 min. Therefore, the transfer model provides a useful screen for the concentrations of valsartan in the small intestine during fasted and fed states.

Lower Extremity Muscle Activity During a Women’s Overhand Lacrosse Shot

PubMed Central

Millard, Brianna M.; Mercer, John A.

2014-01-01

The purpose of this study was to describe lower extremity muscle activity during the lacrosse shot. Participants (n=5 females, age 22±2 years, body height 162.6±15.2 cm, body mass 63.7±23.6 kg) were free from injury and had at least one year of lacrosse experience. The lead leg was instrumented with electromyography (EMG) leads to measure muscle activity of the rectus femoris (RF), biceps femoris (BF), tibialis anterior (TA), and medial gastrocnemius (GA). Participants completed five trials of a warm-up speed shot (Slow) and a game speed shot (Fast). Video analysis was used to identify the discrete events defining specific movement phases. Full-wave rectified data were averaged per muscle per phase (Crank Back Minor, Crank Back Major, Stick Acceleration, Stick Deceleration). Average EMG per muscle was analyzed using a 4 (Phase) × 2 (Speed) ANOVA. BF was greater during Fast vs. Slow for all phases (p<0.05), while TA was not influenced by either Phase or Speed (p>0.05). RF and GA were each influenced by the interaction of Phase and Speed (p<0.05) with GA being greater during Fast vs. Slow shots during all phases and RF greater during Crank Back Minor and Major as well as Stick Deceleration (p<0.05) but only tended to be greater during Stick Acceleration (p=0.076) for Fast vs. Slow. The greater muscle activity (BF, RF, GA) during Fast vs. Slow shots may have been related to a faster approach speed and/or need to create a stiff lower extremity to allow for faster upper extremity movements. PMID:25114727

A fast algorithm for vertex-frequency representations of signals on graphs

PubMed Central

Jestrović, Iva; Coyle, James L.; Sejdić, Ervin

2016-01-01

The windowed Fourier transform (short time Fourier transform) and the S-transform are widely used signal processing tools for extracting frequency information from non-stationary signals. Previously, the windowed Fourier transform had been adopted for signals on graphs and has been shown to be very useful for extracting vertex-frequency information from graphs. However, high computational complexity makes these algorithms impractical. We sought to develop a fast windowed graph Fourier transform and a fast graph S-transform requiring significantly shorter computation time. The proposed schemes have been tested with synthetic test graph signals and real graph signals derived from electroencephalography recordings made during swallowing. The results showed that the proposed schemes provide significantly lower computation time in comparison with the standard windowed graph Fourier transform and the fast graph S-transform. Also, the results showed that noise has no effect on the results of the algorithm for the fast windowed graph Fourier transform or on the graph S-transform. Finally, we showed that graphs can be reconstructed from the vertex-frequency representations obtained with the proposed algorithms. PMID:28479645

Direct magnetic field estimation based on echo planar raw data.

PubMed

Testud, Frederik; Splitthoff, Daniel Nicolas; Speck, Oliver; Hennig, Jürgen; Zaitsev, Maxim

2010-07-01

Gradient recalled echo echo planar imaging is widely used in functional magnetic resonance imaging. The fast data acquisition is, however, very sensitive to field inhomogeneities which manifest themselves as artifacts in the images. Typically used correction methods have the common deficit that the data for the correction are acquired only once at the beginning of the experiment, assuming the field inhomogeneity distribution B(0) does not change over the course of the experiment. In this paper, methods to extract the magnetic field distribution from the acquired k-space data or from the reconstructed phase image of a gradient echo planar sequence are compared and extended. A common derivation for the presented approaches provides a solid theoretical basis, enables a fair comparison and demonstrates the equivalence of the k-space and the image phase based approaches. The image phase analysis is extended here to calculate the local gradient in the readout direction and improvements are introduced to the echo shift analysis, referred to here as "k-space filtering analysis." The described methods are compared to experimentally acquired B(0) maps in phantoms and in vivo. The k-space filtering analysis presented in this work demonstrated to be the most sensitive method to detect field inhomogeneities.

Theory and implementation of a very high throughput true random number generator in field programmable gate array

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

Wang, Yonggang, E-mail: wangyg@ustc.edu.cn; Hui, Cong; Liu, Chong

The contribution of this paper is proposing a new entropy extraction mechanism based on sampling phase jitter in ring oscillators to make a high throughput true random number generator in a field programmable gate array (FPGA) practical. Starting from experimental observation and analysis of the entropy source in FPGA, a multi-phase sampling method is exploited to harvest the clock jitter with a maximum entropy and fast sampling speed. This parametrized design is implemented in a Xilinx Artix-7 FPGA, where the carry chains in the FPGA are explored to realize the precise phase shifting. The generator circuit is simple and resource-saving,more » so that multiple generation channels can run in parallel to scale the output throughput for specific applications. The prototype integrates 64 circuit units in the FPGA to provide a total output throughput of 7.68 Gbps, which meets the requirement of current high-speed quantum key distribution systems. The randomness evaluation, as well as its robustness to ambient temperature, confirms that the new method in a purely digital fashion can provide high-speed high-quality random bit sequences for a variety of embedded applications.« less

Theory and implementation of a very high throughput true random number generator in field programmable gate array.

PubMed

Wang, Yonggang; Hui, Cong; Liu, Chong; Xu, Chao

2016-04-01

The contribution of this paper is proposing a new entropy extraction mechanism based on sampling phase jitter in ring oscillators to make a high throughput true random number generator in a field programmable gate array (FPGA) practical. Starting from experimental observation and analysis of the entropy source in FPGA, a multi-phase sampling method is exploited to harvest the clock jitter with a maximum entropy and fast sampling speed. This parametrized design is implemented in a Xilinx Artix-7 FPGA, where the carry chains in the FPGA are explored to realize the precise phase shifting. The generator circuit is simple and resource-saving, so that multiple generation channels can run in parallel to scale the output throughput for specific applications. The prototype integrates 64 circuit units in the FPGA to provide a total output throughput of 7.68 Gbps, which meets the requirement of current high-speed quantum key distribution systems. The randomness evaluation, as well as its robustness to ambient temperature, confirms that the new method in a purely digital fashion can provide high-speed high-quality random bit sequences for a variety of embedded applications.

Characterisation of chamomile volatiles by simultaneous distillation solid-phase extraction in comparison to hydrodistillation and simultaneous distillation extraction.

PubMed

Krüger, Hans

2010-05-01

A new method for complete separation of steam-volatile organic compounds is described using the example of chamomile flowers. This method is based on the direct combination of hydrodistillation and solid-phase extraction in a circulation apparatus. In contrast to hydrodistillation and simultaneous distillation extraction (SDE), an RP-18 solid phase as adsorptive material is used rather than a water-insoluble solvent. Therefore, a prompt and complete fixation of all volatiles takes place, and the circulation of water-soluble bisabololoxides as well as water-soluble and thermolabile en-yne-spiroethers is inhibited. This so-called simultaneous distillation solid-phase extraction (SD-SPE) provides extracts that better characterise the real composition of the vapour phase, as well as the composition of inhalation vapours, than do SDE extracts or essential oils obtained by hydrodistillation. The data indicate that during inhalation therapy with chamomile, the bisabololoxides and spiroethers are more strongly involved in the inhaling activity than so far assumed. Georg Thieme Verlag KG Stuttgart New York.

ANTIMICROBIAL ACTION OF THE LEAF EXTRACT OF MORINGA OLEIFERA LAM.

PubMed Central

Pal, Saroj K.; Mukherjee, Pulok K.; Saha, Kakali; Pal, M.; Saha, B.P.

1995-01-01

The ethnolic extract of the leaves of Moringa oleifera Lam. (Fam. Moringaceae) was tested for antimicrobial activities against Gram Positive – Bacillus cereus, Bacillus subtilis Staphylococcus aureus, Sarcina lutea: Gram negative – Escherichia coli and Acid fast Mycobacterium phlei. Significant antimicrobial activity of the extract was found in this study. PMID:22556699

Deterred drug abuse using superabsorbent polymers.

PubMed

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

2016-11-01

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

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

PubMed

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

2015-09-01

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

Isolation and purification assay of ex vivo photosystem II D1 protein toward integrated biointeraction analysis.

PubMed

Muktiono, B; Schulten, C; Heemken, O; Gandrass, J; Prange, A; Schnabl, H; Cerboncini, C

2008-02-01

Protein extracts of photosystem II were prepared from leaf chloroplasts of different plant species by fast and nondenaturing methods. Sodium dodecyl sulfate polyacrylamide gel electrophoresis and western blot analysis of the proteins obtained showed that the extracts were enriched by D1 proteins, which appeared putatively in association with the 33-kDa oxygen-evolving-complex subunits. In further isolation steps D1 proteins were purified using salt-gradient chromatography (fast protein liquid chromatography) and characterized by western blot and mass spectrometry.

Robust feature estimation by non-rigid hierarchical image registration and its application in disparity measurement

NASA Astrophysics Data System (ADS)

Badshah, Amir; Choudhry, Aadil Jaleel; Ullah, Shan

2017-03-01

Industries are moving towards automation in order to increase productivity and ensure quality. Variety of electronic and electromagnetic systems are being employed to assist human operator in fast and accurate quality inspection of products. Majority of these systems are equipped with cameras and rely on diverse image processing algorithms. Information is lost in 2D image, therefore acquiring accurate 3D data from 2D images is an open issue. FAST, SURF and SIFT are well-known spatial domain techniques for features extraction and henceforth image registration to find correspondence between images. The efficiency of these methods is measured in terms of the number of perfect matches found. A novel fast and robust technique for stereo-image processing is proposed. It is based on non-rigid registration using modified normalized phase correlation. The proposed method registers two images in hierarchical fashion using quad-tree structure. The registration process works through global to local level resulting in robust matches even in presence of blur and noise. The computed matches can further be utilized to determine disparity and depth for industrial product inspection. The same can be used in driver assistance systems. The preliminary tests on Middlebury dataset produced satisfactory results. The execution time for a 413 x 370 stereo-pair is 500ms approximately on a low cost DSP.

Fe3O4@p-Naphtholbenzein as a novel nano-sorbent for highly effective removal and recovery of Berberine: Response surface methodology for optimization of ultrasound assisted dispersive magnetic solid phase extraction.

PubMed

Aghaie, Ali B G; Hadjmohammadi, Mohammad Reza

2016-08-15

A hydrophobic surface modified iron oxide magnetic nano-sorbent was successfully synthesized, characterized and utilized for highly effective removal and recovery of Berberine (Brb) by Ultrasound Assisted Dispersive Magnetic Solid Phase Extraction (UADM-SPE). Fabrication of p-Naphtholbenzein-coated magnetic nanoparticles (PNB-MNPs) was certified by characteristic analyses such as: Fourier transform infrared spectroscopy (FT-IR), X-ray Diffraction (XRD), thermogravimetric analysis (TGA), vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The characterized PNB-MNPs were utilized to develop a UADM-SPE method for Brb, a well-known isoquinoline alkaloid with a highlighted chemical skeleton for designing selective and powerful bioactive molecules. Affecting parameters on the extraction of Brb were optimized through an orthogonal rotatable central composite design (CCD). The optimum condition is obtained when the variables are set to: pH=4, amount of MNPs=20mg, sample volume=30ml, sonication time=1min at room temperature, and desorbing solvent=500µL of methanol. Under the mentioned condition, an extraction recovery of 98.2%, with relative standard deviation of 3.7%, was obtained via five replicated measurements on a 0.1mgL(-1) Brb standard solution. Finally, the method was successfully applied for determination of Brb in human plasma and urine samples. Regarding the method calibration graphs in plasma and urine matrices, spiked in the range of 0.01-200.00µgL(-1), pre-concentration factors of 134 and 122, method detection limit (MDL) of 0.17 and 0.19µgL(-1), and lower limit of quantification of 0.57 and 0.63µgL(-1) were obtained for plasma and urine samples, respectively. The method exhibits good potentials to be a fast, efficient and reliable method for determination of Brb in human biological samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma.

PubMed

Carmo, Ana Paula Barbosa do; Borborema, Manoella; Ribeiro, Stephan; De-Oliveira, Ana Cecilia Xavier; Paumgartten, Francisco Jose Roma; Moreira, Davyson de Lima

2017-01-01

Primaquine (PQ) diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV ) analysis of PQ in the blood plasma was developed and validated. After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm) as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80) (45:55) as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD) and quantification (LOQ) limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral) PQ diphosphate. By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.

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

PubMed

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

2016-07-01

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

Iron dissolution kinetics of mineral dust at low pH during simulated atmospheric processing

NASA Astrophysics Data System (ADS)

Shi, Z.; Bonneville, S.; Krom, M. D.; Carslaw, K. S.; Jickells, T. D.; Baker, A. R.; Benning, L. G.

2011-02-01

We investigated the iron (Fe) dissolution kinetics of African (Tibesti) and Asian (Beijing) dust samples at acidic pH with the aim of reproducing the low pH conditions in atmospheric aerosols. The Beijing dust and three size fractions of the Tibesti dust (<20 μm: PM20; <10 μm: PM10; and <2.5 μm: PM2.5) were dissolved at pH 1, 2 and/or 3 for up to 1000 h. In the first 10 min, all dust samples underwent an extremely fast Fe solubilisation. Subsequently, the Fe dissolution proceeded at a much slower rate before reaching a stable dissolution plateau. The time-dependant Fe dissolution datasets were best described by a model comprising three acid-extractable Fe pools each dissolving according to first-order kinetics. The dissolution rate constant k (h-1) of each pool was independent of the source (Saharan or Asian) and the size (PM20, PM10 or PM2.5) of the dust but highly dependent on pH. The "fast" Fe pool had a k (25 h-1 at pH = 1) of a similar magnitude to "dry" ferrihydrite nanoparticles and/or poorly crystalline Fe(III) oxyhydroxide, while the "intermediate" and "slow" Fe pools had k values respectively 50-60 times and 3000-4000 times smaller than the "fast" pool. The "slow" Fe pool was likely to consist of both crystalline Fe oxide phases (i.e., goethite and/or hematite) and Fe contained in the clay minerals. The initial mass of the "fast", "intermediate" and "slow" Fe pools represented respectively about 0.5-2%, 1-3% and 15-40% of the total Fe in the dust samples. Furthermore, we showed that in systems with low dust/liquid ratios, Fe can be dissolved from all three pools, whereas at high dust/liquid ratios (e.g., in aerosols), sufficient Fe may be solubilised from the "fast" phase to dominate the Fe dissolved and to suppress the dissolution of Fe from the other Fe pools. These data demonstrated that dust/liquid ratio and pH are fundamental parameters controlling Fe dissolution kinetics in the dust. In order to reduce errors in atmospheric and climate models, these fundamental controlling factors need to be included.

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

Bhattacharyya, M.H.; Larsen, R.P.; Oldham, R.D.

The fraction of plutonium absorbed after oral administration of Pu(VI) to 24-h-fasted mice was 19 X 10(-4), 13-fold higher than in fed mice, 1.4 X 10(-4). We have investigated the relevance of the high gastrointestinal (GI) absorption value for the 24-h-fasted animals in setting drinking water standards for humans. When fasting was initiated at the beginning of the active phase of the mouse's daily activity cycle (when they would normally eat), plutonium GI absorption rose from 2.8 X 10(-4) at zero-time to a level typical of the 24-h-fasted mouse after only 2 h of fasting. In contrast, in mice allowedmore » to eat for 4 h into their active phase prior to initiation of the fast (meal-fed mice), 8 h of fasting were required before GI absorption rose to a level similar to that of the 24-h-fasted mouse. The fraction of plutonium retained after gavage administration of Pu(VI) to 1-day-old rats was 74 X 10(-4), 70-fold higher than the value for fed adults. Retention after GI absorption in neonates remained 30- to 70-fold higher than in adults until weaning. One week after weaning, the fraction absorbed and retained by fed weanling rats was the same as that for fed adults, 1 X 10(-4). Drinking water standards for plutonium have been set based on GI absorption values for fed adult animals. The 10- to 100-fold increases in plutonium absorption in young and fasted animals reported by ourselves and others, and the rapid rise to fasted levels of absorption at the start of the animal's active phase, indicate that consideration should be given to elevated levels of plutonium absorption in young and fasted individuals.« less

Fast determination of four polar contaminants in soy nutraceutical products by liquid chromatography coupled to tandem mass spectrometry.

PubMed

Domingos Alves, Renata; Romero-González, Roberto; López-Ruiz, Rosalía; Jiménez-Medina, M L; Garrido Frenich, Antonia

2016-11-01

An analytical method based on a modified QuPPe (quick polar pesticide) extraction procedure coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was evaluated for the determination of four polar compounds (chlorate, fosetyl-Al, maleic hydrazide, and perchlorate) in nutraceutical products obtained from soy. Experimental conditions including extraction such as solvent, acidification, time, and clean-up sorbents were varied. Acidified acetonitrile (1 % formic acid, v/v) was used as extraction solvent instead of methanol (conventional QuPPe), which provides a doughy mixture which cannot be injected into the LC. Clean-up or derivatization steps were avoided. For analysis, several stationary phases were evaluated and Hypercarb (porous graphitic carbon) provided the best results. The optimized method was validated and recoveries ranged between 46 and 119 %, and correction factors can be used for quantification purposes bearing in mind that inter-day precision was equal to or lower than 17 %. Limits of quantification (LOQs) ranged from 4 to 100 μg kg -1 . Soy-based nutraceutical products were analyzed and chlorate was detected in five samples at concentrations between 63 and 1642 μg kg -1 . Graphical Abstract Analysis of polar compounds in soy-based nutraceutical products.

Development and validation of a quantitative UHPLC-MS/MS method for selected brominated flame retardants in food.

PubMed

Malysheva, Svetlana V; Goscinny, Séverine; Malarvannan, Govindan; Poma, Giulia; Andjelkovic, Mirjana; Voorspoels, Stefan; Covaci, Adrian; Van Loco, Joris

2018-02-01

An ultra-high performance liquid chromatography - tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated (in-house) for the quantification of selected brominated flame retardants (BFRs), including tetrabromobisphenol A (TBBPA), hexabromocyclododecanes (HBCDs), tetrabromobisphenol S (TBBPS) and bromophenols (BPs), in various food matrices. The sample preparation consisted of extraction of TBBPS with acidified acetonitrile followed by a fast dispersive solid-phase extraction (dSPE) clean-up and extraction of the other BFRs with a mixture of hexane and dichloromethane (1:1, v/v) with subsequent clean-up using acidified silica (44%, w/w). The limits of quantification of the method varied widely for the types of food matrices and the different classes of BFRs from 4 pg g -1 wet weight (ww) to 8 ng g -1 ww. For most of the analytes the apparent recovery was in the range 70-120%, and the method precision (under repeatability conditions) was below 20%. The method was successfully applied in proficiency testing exercises as well as for analysis of various food items. Only 25% of the collected food samples contained BFRs, with 4-bromophenol and α-HBCD as the only detected compounds. The contaminated foodstuffs were fish and eggs with concentrations in the range from 48 to 305 pg g -1 ww.

Determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine, swine and poultry liver using LC-MS/MS.

PubMed

Martins, Magda Targa; Barreto, Fabiano; Hoff, Rodrigo Barcelos; Jank, Louise; Arsand, Juliana Bazzan; Feijó, Tiago Correa; Schapoval, Elfrides Eva Scherman

2015-01-01

Antibacterials are widely used in veterinary medicine. Residues of these drugs can remain in food of animal origin, including bovine liver. This paper describes a fast and simple analytical method for the determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine liver samples. Deuterated enrofloxacin, sulfapyridine and demeclocycline were used as internal standards. The homogenised liver samples were extracted with acidified acetonitrile. Steps of non-solid-phase extraction (SPE) clean-up and concentration were used in the presented method. The final extracts were analysed by sensitive and selective detection of all components in a single run using LC-MS/MS. Acceptable recoveries between 66% and 110% were obtained. Good linearity (r(2)) above 0.96, considering three different days, for all drugs was achieved in concentrations ranging from 0.0 to 2.0 × the maximum residue limit (MRL). Intraday precision with coefficient of variation (CV%) (n = 6) lower than 14.7% and inter-day precision lower than 18.8% in agreement with European Commission Decision 2002/657/EC were obtained in concentrations ranging from 0.5 to 1.5 MRL. Accuracy was between 86% and 110%. Limits of detection and quantitation, as well as decision limit (CCα) and detection capability (CCβ), were also evaluated.

Analysis of fentanyl in urine by DLLME-GC-MS.

PubMed

Gardner, Michael A; Sampsel, Sheena; Jenkins, Werner W; Owens, Janel E

2015-03-01

Fentanyl is a synthetic narcotic anesthetic ∼80-100 times more potent than morphine. Owing to the potential for its abuse, the drug may be included in a forensic toxicology work-up, which requires fast, precise and accurate measurements. Here, the stability of fentanyl was assessed when stored at three different temperatures (-20, 4 and 25°C) in synthetic urine. Stability at those three temperatures was demonstrated over 12 weeks upon analysis by gas chromatography-mass spectrometry with a deuterated internal standard (fentanyl-D5) utilizing three different extraction techniques: liquid-liquid extraction (LLE), solid-phase extraction and dispersed liquid-liquid microextraction (DLLME). The DLLME method was then optimized before use in the analysis of fentanyl in urine samples obtained from autopsy cases at the El Paso County Coroner's Office. Accuracy of the DLLME method was assessed by completing spike and recovery studies at three different fortification levels (10, 100 and 250 ng/mL) with excellent recovery (89.9-102.6%). The excellent comparability between DLLME and LLE is demonstrated (Bland-Altman difference plot with a mean difference of 4.9 ng/mL) and the use of this methodology in the analysis of forensically relevant samples is discussed. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Precision and Fast Wavelength Tuning of a Dynamically Phase-Locked Widely-Tunable Laser

NASA Technical Reports Server (NTRS)

Numata, Kenji; Chen, Jeffrey R.; Wu, Stewart T.

2012-01-01

We report a precision and fast wavelength tuning technique demonstrated for a digital-supermode distributed Bragg reflector laser. The laser was dynamically offset-locked to a frequency-stabilized master laser using an optical phase-locked loop, enabling precision fast tuning to and from any frequencies within a 40-GHz tuning range. The offset frequency noise was suppressed to the statically offset-locked level in less than 40 s upon each frequency switch, allowing the laser to retain the absolute frequency stability of the master laser. This technique satisfies stringent requirements for gas sensing lidars and enables other applications that require such well-controlled precision fast tuning.

Process for preparing phenolic formaldehyde resole resin products derived from fractionated fast-pyrolysis oils

DOEpatents

Chum, Helena L.; Kreibich, Roland E.

1992-01-01

A process for preparing phenol-formaldehyde resole resins and adhesive compositions in which portions of the phenol normally contained in said resins are replaced by a phenol/neutral fractions extract obtained from fractionating fast-pyrolysis oils.

Dual-wavelength phase-shifting digital holography selectively extracting wavelength information from wavelength-multiplexed holograms.

PubMed

Tahara, Tatsuki; Mori, Ryota; Kikunaga, Shuhei; Arai, Yasuhiko; Takaki, Yasuhiro

2015-06-15

Dual-wavelength phase-shifting digital holography that selectively extracts wavelength information from five wavelength-multiplexed holograms is presented. Specific phase shifts for respective wavelengths are introduced to remove the crosstalk components and extract only the object wave at the desired wavelength from the holograms. Object waves in multiple wavelengths are selectively extracted by utilizing 2π ambiguity and the subtraction procedures based on phase-shifting interferometry. Numerical results show the validity of the proposed technique. The proposed technique is also experimentally demonstrated.

Phase 1 remediation of jet fuel contaminated soil and groundwater at JFK International Airport using dual phase extraction and bioventing

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

Roth, R.; Bianco, P. Rizzo, M.; Pressly, N.

1995-12-31

Soil and groundwater contaminated with jet fuel at Terminal One of the JFK International Airport in New York have been remediated using dual phase extraction (DPE) and bioventing. Two areas were remediated using 51 DPE wells and 20 air sparging/air injection wells. The total area remediated by the DPE wells is estimated to be 4.8 acres. Groundwater was extracted to recover nonaqueous phase and aqueous phase jet fuel from the shallow aquifer and treated above ground by the following processes; oil/water separation, iron-oxidation, flocculation, sedimentation, filtration, air stripping and liquid-phase granular activated carbon (LPGAC) adsorption. The extracted vapors were treatedmore » by vapor-phase granular activated carbon (VPGAC) adsorption in one area, and catalytic oxidation and VPGAC adsorption in another area. After 6 months of remediation, approximately 5,490 lbs. of volatile organic compounds (VOCs) were removed by soil vapor extraction (SVE), 109,650 lbs. of petroleum hydrocarbons were removed from the extracted groundwater, and 60,550 lbs. of petroleum hydrocarbons were biologically oxidized by subsurface microorganisms. Of these three mechanisms, the rate of petroleum hydrocarbon removal was the highest for biological oxidation in one area and by groundwater extraction in another area.« less

Separation of rare earths from transition metals by liquid-liquid extraction from a molten salt hydrate to an ionic liquid phase.

PubMed

Rout, Alok; Binnemans, Koen

2014-02-28

The solvent extraction of trivalent rare-earth ions and their separation from divalent transition metal ions using molten salt hydrates as the feed phase and an undiluted fluorine-free ionic liquid as the extracting phase were investigated in detail. The extractant was tricaprylmethylammonium nitrate, [A336][NO3], and the hydrated melt was calcium nitrate tetrahydrate, Ca(NO3)2·4H2O. The extraction behavior of rare-earth ions was studied for solutions of individual elements, as well as for mixtures of rare earths in the hydrated melt. The influence of different extraction parameters was investigated: the initial metal loading in the feed phase, percentage of water in the feed solution, equilibration time, and the type of hydrated melt. The extraction of rare earths from Ca(NO3)2·4H2O was compared with extraction from CaCl2·4H2O by [A336][Cl] (Aliquat 336). The nitrate system was found to be the better one. The extraction and separation of rare earths from the transition metals nickel, cobalt and zinc were also investigated. Remarkably high separation factors of rare-earth ions over transition metal ions were observed for extraction from Ca(NO3)2·4H2O by the [A336][NO3] extracting phase. Furthermore, rare-earth ions could be separated efficiently from transition metal ions, even in melts with very high concentrations of transition metal ions. Rare-earth oxides could be directly dissolved in the Ca(NO3)2·4H2O phase in the presence of small amounts of Al(NO3)3·9H2O or concentrated nitric acid. The efficiency of extraction after dissolving the rare-earth oxides in the hydrated nitrate melt was identical to extraction from solutions with rare-earth nitrates dissolved in the molten phase. The stripping of the rare-earth ions from the loaded ionic liquid phase and the reuse of the recycled ionic liquid were also investigated in detail.

Low-Cost HTS Based Magnet System with an Inductively Coupled Pulsed Energy Extraction Protection System

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

Agustsson, Ronald

In this project, RadiaBeam Technologies was tasked with developing a novel solution for a cost effective quench protection based on fast expansion of the normal zone. By inductively coupling a strong electromagnetic pulse via a resonant LC circuit, we attempted to demonstrate accelerated normal zone propagation. The AC field induces currents in the superconducting layer with the current density exceeding that of the critical current density, J c. This creates a large normal zone, uniformly distributing the dissipation through the magnet body. The method does not rely on thermal heating of the conductor, thus enabling nearly instantaneous protection. Through themore » course of the Phase II project, RadiaBeam Technologies continued extensive numerical modeling of the inductive quench system, re-designed and built several iterations of the POC system for testing and observed evidence of a transient partial quench being induced. However the final device was not fabricated. This was a consequence of the fundamentally complex nature of the energy extraction process and the challenges associated even with demonstrating the proof of concept in a bench top device.« less

Fast profiling of anthocyanins in wine by desorption nano-electrospray ionization mass spectrometry.

PubMed

Hartmanova, Lucie; Ranc, Vaclav; Papouskova, Barbora; Bednar, Petr; Havlicek, Vladimir; Lemr, Karel

2010-06-18

Desorption electrospray ionization (DESI) mass spectrometry appears to be a useful technique applicable in different areas (e.g. analysis of pharmaceuticals, identification of biologically active compounds in tissues, imaging mass spectrometry). Its modification termed desorption nano-electrospray (nano-DESI) was tested for analysis of anthocyanins. Acidifying of samples and acidic spray liquid (methanol:water=75:25 with 0.2% HCOOH) were essential for obtaining good quality spectra. Profiles of main anthocyanins in wine samples, two vintages (2005 and 2007) of three cultivars (Alibernet, Neronet and Rubinet), were successfully acquired. They were in agreement with results of LC/MS experiments (anthocyanins isolated by solid phase extraction were separated by mu-HPLC with gradient elution and detected by ESI-MS). Nano-DESI-MS data also allowed to determine ratio of two cultivars (Neronet and Rubinet) in their mixture and to detect coloring of wine by tenturier or elderberry extract. Detection of main anthocyanins in slices of wine grape, chokeberries and elderberries or in a wine stain on cotton fabric is also presented. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Design and evaluation of self-emulsifying drug delivery systems of Rhizoma corydalis decumbentis extracts.

PubMed

Ma, Hongda; Zhao, Qingchun; Wang, Yongjun; Guo, Tao; An, Ye; Shi, Guobing

2012-10-01

To improve the dissolution and oral absorption of Rhizoma corydalis decumbentis extracts (RCDE), a famous traditional Chinese herbal medicine which contains poorly water-soluble active components, self-emulsifying drug-delivery systems (SEDDS) were designed and evaluated in vitro and in vivo for the first time. Six formulations were prepared, and pseudoternary phase diagrams were constructed to identify the efficient self-emulsication region through the modified visual test. The optimized formulation consisted of 45% Solutol, 40% ethyl oleate, and 15% Transcutol P. The mean droplet size distribution of the optimized SEDDS was less than 100 nm. The release of the active components (protopine and tetrahydropalmatine) in RCDE from SEDDS hard gelatin capsules showed a faster rate in comparison with the commercial tablets. After oral administration of RCDE SEDDS capsules or the commercial tablets to fasted rats, the relative bioavailability of SEDDS capsules for protopine and tetrahydropalmatine was 209.7% and 133.2% compared with commercial tablets, respectively. Our study indicated that SEDDS has the potential to improve the bioavailability of traditional Chinese medicines, in which many active components are hydrophobic, such as RCDE.

A chemometric method to identify enzymatic reactions leading to the transition from glycolytic oscillations to waves

NASA Astrophysics Data System (ADS)

Zimányi, László; Khoroshyy, Petro; Mair, Thomas

2010-06-01

In the present work we demonstrate that FTIR-spectroscopy is a powerful tool for the time resolved and noninvasive measurement of multi-substrate/product interactions in complex metabolic networks as exemplified by the oscillating glycolysis in a yeast extract. Based on a spectral library constructed from the pure glycolytic intermediates, chemometric analysis of the complex spectra allowed us the identification of many of these intermediates. Singular value decomposition and multiple level wavelet decomposition were used to separate drifting substances from oscillating ones. This enabled us to identify slow and fast variables of glycolytic oscillations. Most importantly, we can attribute a qualitative change in the positive feedback regulation of the autocatalytic reaction to the transition from homogeneous oscillations to travelling waves. During the oscillatory phase the enzyme phosphofructokinase is mainly activated by its own product ADP, whereas the transition to waves is accompanied with a shift of the positive feedback from ADP to AMP. This indicates that the overall energetic state of the yeast extract determines the transition between spatially homogeneous oscillations and travelling waves.

Feasibility of Surfactant-Free Supported Emulsion Liquid Membrane Extraction

NASA Technical Reports Server (NTRS)

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

2001-01-01

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

[Growth inhibition of the four species of red tide microalgae by extracts from Enteromorpha prolifera extracted with the five solvents].

PubMed

Sun, Ying-Ying; Liu, Xiao-Xiao; Wang, Chang-Hai

2010-06-01

To study the effects of extracts of Enteromorpha prolifera on the growth of the four species of red tide microalgae (Amphidinium hoefleri, Karenia mikimitoi, Alexandrium tamarense and Skeletonema costatum), the extracts were extracted with five solvents (methanol, acetone, ethyl acetate, chloroform and petroleum ether), respectively. Based on the observation of algal morphology and the measurement of algal density, cell size and the contents of physiological indicators (chlorophyll, protein and polysaccharide), the results showed methanol extracts of E. prolifera had the strongest action. The inhibitory effects of A. hoefleri, K. mikimitoi, A. tamarense and S. costatum by the methanol extracts were 54.0%, 48.1%, 44.0% and 37.5% in day 10, respectively. The extracts of E. prolifera extracted with methanol, acetone and ethyl acetate caused cavities, pieces and pigment reduction in cells, and those with chloroform and petroleum ether caused goffers on cells. The extracts of E. prolifera extracted with all the five solvents decreased athletic ability of the cells, among which those extracted with ethyl acetate, chloroform and petroleum ether decreased cell size of test microalgae. The further investigation found that the methanol extracts significantly decreased contents of chlorophyll, protein and polysaccharide in the cells of those microalgae. The inhibitory effect of chlorophyll, protein and polysaccharide contents of four species of microalgae by the methanol extracts was about 51%. On the basis of the above experiments, dry powder of E. prolifera were extracts with methanol, and extracts were obtained. The methanol extracts were partitioned to petroleum ether phase, ethyl acetate phase, n-butanol phase and distilled water phase by liquid-liquid fractionation, and those with petroleum ether and ethyl acetate significantly inhibited the growth of all test microalgae, and the inhibitory effect of four species of microalgae by those two extracts was above 25% in day 10. Our researches expressed that antialgal substances in E. prolifera extracted with methanol were obtained. And two fractions (petroleum ether phase and ethyl acetate phase) that inhibited the growth of all test microalgae were obtained when the methanol extracts was fractionated by liquid-liquid fractionation.

Aptamer-functionalized Fe3 O4 magnetic nanoparticles as a solid-phase extraction adsorbent for the selective extraction of berberine from Cortex phellodendri.

PubMed

Jiang, Ling-Feng; Chen, Bo-Cheng; Chen, Ben; Li, Xue-Jian; Liao, Hai-Lin; Zhang, Wen-Yan; Wu, Lin

2017-07-01

The extraction adsorbent was fabricated by immobilizing the highly specific recognition and binding of aptamer onto the surface of Fe 3 O 4 magnetic nanoparticles, which not only acted as recognition elements to recognize and capture the target molecule berberine from the extract of Cortex phellodendri, but also could favor the rapid separation and purification of the bound berberine by using an external magnet. The developed solid-phase extraction method in this work was useful for the selective extraction and determination of berberine in Cortex phellodendri extracts. Various conditions such as the amount of aptamer-functionalized Fe 3 O 4 magnetic nanoparticles, extraction time, temperature, pH value, Mg 2+ concentration, elution time and solvent were optimized for the solid-phase extraction of berberine. Under optimal conditions, the purity of berberine extracted from Cortex phellodendri was as high as 98.7% compared with that of 4.85% in the extract, indicating that aptamer-functionalized Fe 3 O 4 magnetic nanoparticles-based solid-phase extraction method was very effective for berberine enrichment and separation from a complex herb extract. The applicability and reliability of the developed solid-phase extraction method were demonstrated by separating berberine from nine different concentrations of one Cortex phellodendri extract. The relative recoveries of the spiked solutions of all the samples were between 95.4 and 111.3%, with relative standard deviations ranging between 0.57 and 1.85%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of High-Protein, Intermittent Fasting Low-Calorie Diet and Heart Healthy Diet for Vascular Health of the Obese.

PubMed

Zuo, Li; He, Feng; Tinsley, Grant M; Pannell, Benjamin K; Ward, Emery; Arciero, Paul J

2016-01-01

It has been debated whether different diets are more or less effective in long-term weight loss success and cardiovascular disease prevention among men and women. To further explore these questions, the present study evaluated the combined effects of a high-protein, intermittent fasting, low-calorie diet plan compared with a heart healthy diet plan during weight loss, and weight loss maintenance on blood lipids and vascular compliance of obese individuals. The experiment involved 40 obese adults (men, n = 21; women, n = 19) and was divided into two phases: (a) 12-week high-protein, intermittent fasting, low-calorie weight loss diet comparing men and women (Phase 1) and (b) a 1-year weight maintenance phase comparing high-protein, intermittent fasting with a heart healthy diet (Phase 2). Body weight, body mass index (BMI), blood lipids, and arterial compliance outcomes were assessed at weeks 1 (baseline control), 12 (weight loss), and 64 (12 + 52 week; weight loss maintenance). At the end of weight loss intervention, concomitant reductions in body weight, BMI and blood lipids were observed, as well as enhanced arterial compliance. No sex-specific differences in responses were observed. During phase 2, the high-protein, intermittent fasting group demonstrated a trend for less regain in BMI, low-density lipoprotein (LDL), and aortic pulse wave velocity than the heart healthy group. Our results suggest that a high-protein, intermittent fasting and low-calorie diet is associated with similar reductions in BMI and blood lipids in obese men and women. This diet also demonstrated an advantage in minimizing weight regain as well as enhancing arterial compliance as compared to a heart healthy diet after 1 year.

Comparison of High-Protein, Intermittent Fasting Low-Calorie Diet and Heart Healthy Diet for Vascular Health of the Obese

PubMed Central

Zuo, Li; He, Feng; Tinsley, Grant M.; Pannell, Benjamin K.; Ward, Emery; Arciero, Paul J.

2016-01-01

Aim: It has been debated whether different diets are more or less effective in long-term weight loss success and cardiovascular disease prevention among men and women. To further explore these questions, the present study evaluated the combined effects of a high-protein, intermittent fasting, low-calorie diet plan compared with a heart healthy diet plan during weight loss, and weight loss maintenance on blood lipids and vascular compliance of obese individuals. Methods: The experiment involved 40 obese adults (men, n = 21; women, n = 19) and was divided into two phases: (a) 12-week high-protein, intermittent fasting, low-calorie weight loss diet comparing men and women (Phase 1) and (b) a 1-year weight maintenance phase comparing high-protein, intermittent fasting with a heart healthy diet (Phase 2). Body weight, body mass index (BMI), blood lipids, and arterial compliance outcomes were assessed at weeks 1 (baseline control), 12 (weight loss), and 64 (12 + 52 week; weight loss maintenance). Results: At the end of weight loss intervention, concomitant reductions in body weight, BMI and blood lipids were observed, as well as enhanced arterial compliance. No sex-specific differences in responses were observed. During phase 2, the high-protein, intermittent fasting group demonstrated a trend for less regain in BMI, low-density lipoprotein (LDL), and aortic pulse wave velocity than the heart healthy group. Conclusion: Our results suggest that a high-protein, intermittent fasting and low-calorie diet is associated with similar reductions in BMI and blood lipids in obese men and women. This diet also demonstrated an advantage in minimizing weight regain as well as enhancing arterial compliance as compared to a heart healthy diet after 1 year. PMID:27621707

Sensor-based auto-focusing system using multi-scale feature extraction and phase correlation matching.

PubMed

Jang, Jinbeum; Yoo, Yoonjong; Kim, Jongheon; Paik, Joonki

2015-03-10

This paper presents a novel auto-focusing system based on a CMOS sensor containing pixels with different phases. Robust extraction of features in a severely defocused image is the fundamental problem of a phase-difference auto-focusing system. In order to solve this problem, a multi-resolution feature extraction algorithm is proposed. Given the extracted features, the proposed auto-focusing system can provide the ideal focusing position using phase correlation matching. The proposed auto-focusing (AF) algorithm consists of four steps: (i) acquisition of left and right images using AF points in the region-of-interest; (ii) feature extraction in the left image under low illumination and out-of-focus blur; (iii) the generation of two feature images using the phase difference between the left and right images; and (iv) estimation of the phase shifting vector using phase correlation matching. Since the proposed system accurately estimates the phase difference in the out-of-focus blurred image under low illumination, it can provide faster, more robust auto focusing than existing systems.

Sensor-Based Auto-Focusing System Using Multi-Scale Feature Extraction and Phase Correlation Matching

PubMed Central

Jang, Jinbeum; Yoo, Yoonjong; Kim, Jongheon; Paik, Joonki

2015-01-01

This paper presents a novel auto-focusing system based on a CMOS sensor containing pixels with different phases. Robust extraction of features in a severely defocused image is the fundamental problem of a phase-difference auto-focusing system. In order to solve this problem, a multi-resolution feature extraction algorithm is proposed. Given the extracted features, the proposed auto-focusing system can provide the ideal focusing position using phase correlation matching. The proposed auto-focusing (AF) algorithm consists of four steps: (i) acquisition of left and right images using AF points in the region-of-interest; (ii) feature extraction in the left image under low illumination and out-of-focus blur; (iii) the generation of two feature images using the phase difference between the left and right images; and (iv) estimation of the phase shifting vector using phase correlation matching. Since the proposed system accurately estimates the phase difference in the out-of-focus blurred image under low illumination, it can provide faster, more robust auto focusing than existing systems. PMID:25763645

Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry.

PubMed

Zhang, Caixiang; Eganhouse, Robert P; Pontolillo, James; Cozzarelli, Isabelle M; Wang, Yanxin

2012-03-23

4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid-liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC×GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment. Copyright © 2012 Elsevier B.V. All rights reserved.

RNA isolation from mammalian cells using porous polymer monoliths: an approach for high-throughput automation.

PubMed

Chatterjee, Anirban; Mirer, Paul L; Zaldivar Santamaria, Elvira; Klapperich, Catherine; Sharon, Andre; Sauer-Budge, Alexis F

2010-06-01

The life science and healthcare communities have been redefining the importance of ribonucleic acid (RNA) through the study of small molecule RNA (in RNAi/siRNA technologies), micro RNA (in cancer research and stem cell research), and mRNA (gene expression analysis for biologic drug targets). Research in this field increasingly requires efficient and high-throughput isolation techniques for RNA. Currently, several commercial kits are available for isolating RNA from cells. Although the quality and quantity of RNA yielded from these kits is sufficiently good for many purposes, limitations exist in terms of extraction efficiency from small cell populations and the ability to automate the extraction process. Traditionally, automating a process decreases the cost and personnel time while simultaneously increasing the throughput and reproducibility. As the RNA field matures, new methods for automating its extraction, especially from low cell numbers and in high throughput, are needed to achieve these improvements. The technology presented in this article is a step toward this goal. The method is based on a solid-phase extraction technology using a porous polymer monolith (PPM). A novel cell lysis approach and a larger binding surface throughout the PPM extraction column ensure a high yield from small starting samples, increasing sensitivity and reducing indirect costs in cell culture and sample storage. The method ensures a fast and simple procedure for RNA isolation from eukaryotic cells, with a high yield both in terms of quality and quantity. The technique is amenable to automation and streamlined workflow integration, with possible miniaturization of the sample handling process making it suitable for high-throughput applications.

Untargeted UPLC-MS Profiling Pipeline to Expand Tissue Metabolome Coverage: Application to Cardiovascular Disease

PubMed Central

2015-01-01

Metabolic profiling studies aim to achieve broad metabolome coverage in specific biological samples. However, wide metabolome coverage has proven difficult to achieve, mostly because of the diverse physicochemical properties of small molecules, obligating analysts to seek multiplatform and multimethod approaches. Challenges are even greater when it comes to applications to tissue samples, where tissue lysis and metabolite extraction can induce significant systematic variation in composition. We have developed a pipeline for obtaining the aqueous and organic compounds from diseased arterial tissue using two consecutive extractions, followed by a different untargeted UPLC-MS analysis method for each extract. Methods were rationally chosen and optimized to address the different physicochemical properties of each extract: hydrophilic interaction liquid chromatography (HILIC) for the aqueous extract and reversed-phase chromatography for the organic. This pipeline can be generic for tissue analysis as demonstrated by applications to different tissue types. The experimental setup and fast turnaround time of the two methods contributed toward obtaining highly reproducible features with exceptional chromatographic performance (CV % < 0.5%), making this pipeline suitable for metabolic profiling applications. We structurally assigned 226 metabolites from a range of chemical classes (e.g., carnitines, α-amino acids, purines, pyrimidines, phospholipids, sphingolipids, free fatty acids, and glycerolipids) which were mapped to their corresponding pathways, biological functions and known disease mechanisms. The combination of the two untargeted UPLC-MS methods showed high metabolite complementarity. We demonstrate the application of this pipeline to cardiovascular disease, where we show that the analyzed diseased groups (n = 120) of arterial tissue could be distinguished based on their metabolic profiles. PMID:25664760

Insight into the time-resolved extraction of aroma compounds during espresso coffee preparation: online monitoring by PTR-ToF-MS.

PubMed

Sánchez-López, José A; Zimmermann, Ralf; Yeretzian, Chahan

2014-12-02

Using proton-transfer-reaction time-of-flight mass-spectrometry (PTR-ToF-MS), we investigated the extraction dynamic of 95 ion traces in real time (time resolution = 1 s) during espresso coffee preparation. Fifty-two of these ions were tentatively identified. This was achieved by online sampling of the volatile organic compounds (VOCs) in close vicinity to the coffee flow, at the exit of the extraction hose of the espresso machine (single serve capsules). Ten replicates of six different single serve coffee types were extracted to a final weight between 20-120 g, according to the recommended cup size of the respective coffee capsule (Ristretto, Espresso, and Lungo), and analyzed. The results revealed considerable differences in the extraction kinetics between compounds, which led to a fast evolution of the volatile profiles in the extract flow and consequently to an evolution of the final aroma balance in the cup. Besides exploring the time-resolved extraction dynamics of VOCs, the dynamic data also allowed the coffees types (capsules) to be distinguished from one another. Both hierarchical cluster analysis (HCA) and principal component analysis (PCA) showed full separation between the coffees types. The methodology developed provides a fast and simple means of studying the extraction dynamics of VOCs and differentiating between different coffee types.

Disorder trapping by rapidly moving phase interface in an undercooled liquid

NASA Astrophysics Data System (ADS)

Galenko, Peter; Danilov, Denis; Nizovtseva, Irina; Reuther, Klemens; Rettenmayr, Markus

2017-08-01

Non-equilibrium phenomena such as the disappearance of solute drag, the origin of solute trapping and evolution of disorder trapping occur during fast transformations with originating metastable phases [D.M. Herlach, P.K. Galenko, D. Holland-Moritz, Metastable solids from undrercooled melts (Elsevier, Amsterdam, 2007)]. In the present work, a theoretical investigation of disorder trapping by a rapidly moving phase interface is presented. Using a model of fast phase transformations, a system of governing equations for the diffusion of atoms, and the evolution of both long-range order parameter and phase field variable is formulated. First numerical solutions are carried out for a congruently melting binary alloy system.

Fast method for simultaneous quantification of tamoxifen and metabolites in dried blood spots using an entry level LC-MS/MS system.

PubMed

Tré-Hardy, Marie; Capron, Arnaud; Antunes, Marina Venzon; Linden, Rafael; Wallemacq, Pierre

2016-11-01

The purpose of this study was to develop and validate a new liquid chromatography-tandem mass spectrometric (LC-MSMS) assay for the simultaneous quantification of tamoxifen (TAM) and its main therapeutically active metabolites, N-desmethyltamoxifen (NDT), 4-hydroxytamoxifen (4HT) and endoxifen (END) in dried blood spots. Ultrasound assisted methanolic extraction was used for TAM and metabolites extraction from dried blood spot. After evaporation and methanol reconstitution, the extract was injected into a LC-MSMS system. Reversed phase chromatography was performed on a C18 grafted column in gradient mode. TAM, metabolites, and internal standard (diazepam-d 5 ; IS) were identified in positive electrospray ionization mode using m/z transition of 372.5>72.1 (TAM); 374.23>58.10 (END); 358.27>58.10 (NDT); 388.23>44.80 (4HT) and 290.00>198.00 (IS). Total analytical run time was 6.5min. Assay was linear from 1 to 500ng/mL for all substances and presented intra and inter-assay precision and accuracy <15%. TAM, NDT, 4HT and END limits of quantification and detection were of 1 and 0.5ng/mL; 1 and 3ng/mL; 1.7 and 3ng/mL; 0.6 and 2ng/mL, respectively. Recovery ranged from 83.8 to 96.3% with matrix effect ranged from 4.3 to 29.8% for TAM and its metabolites. Hematocrit value ≤40% appeared to negatively influence accuracy of the method. In conclusion, the method described here is somewhat accessible, relatively fast, sensitive and selective with no interference. This assay might be used to investigate the level of TAM and its metabolites in DBS for therapeutic drug monitoring purposes. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

A fast learning method for large scale and multi-class samples of SVM

NASA Astrophysics Data System (ADS)

Fan, Yu; Guo, Huiming

2017-06-01

A multi-class classification SVM(Support Vector Machine) fast learning method based on binary tree is presented to solve its low learning efficiency when SVM processing large scale multi-class samples. This paper adopts bottom-up method to set up binary tree hierarchy structure, according to achieved hierarchy structure, sub-classifier learns from corresponding samples of each node. During the learning, several class clusters are generated after the first clustering of the training samples. Firstly, central points are extracted from those class clusters which just have one type of samples. For those which have two types of samples, cluster numbers of their positive and negative samples are set respectively according to their mixture degree, secondary clustering undertaken afterwards, after which, central points are extracted from achieved sub-class clusters. By learning from the reduced samples formed by the integration of extracted central points above, sub-classifiers are obtained. Simulation experiment shows that, this fast learning method, which is based on multi-level clustering, can guarantee higher classification accuracy, greatly reduce sample numbers and effectively improve learning efficiency.

The impact of soil organic matter and soil sterilisation on the bioaccessibility of 14C-azoxystrobin determined by desorption kinetics.

PubMed

Clegg, Helen; Riding, Matthew J; Oliver, Robin; Jones, Kevin C; Semple, Kirk T

2014-08-15

As soils represent a major sink for most pesticides, factors influencing pesticide degradation are essential in identifying their potential environmental risk. Desorption of (14)C-azoxystrobin was investigated over time in two soils under sterile and non-sterile conditions using exhaustive (solvent) and non-exhaustive (aqueous) methods. Desorption data were fitted to a two-compartment model, differentiating between fast and slow desorbing fractions. With increased ageing, rapid desorption (Frap) (bioaccessibility) decreased with corresponding increases in slowly desorbing fractions (F(slow)). The rapid desorption rate constant (k(fast)) was not affected by ageing, sterility or extraction solvent. The non-exhaustive extractions had similar desorption profiles; whereas exhaustive extractions in aged soils had the highest F(rap). In non-sterile soil, F(rap) was lower resulting in higher F(slow), while desorption rates remained unaffected. Organic matter (OM) reduces F(rap); but not desorption rates. Microorganisms and OM enhanced ageing effects, reducing the fraction of fast desorbing chemicals and potentially the bioaccessibility of pesticides in soil. Copyright © 2014 Elsevier B.V. All rights reserved.

Fast detection and characterization of organic and inorganic gunshot residues on the hands of suspects by CMV-GC-MS and LIBS.

PubMed

Tarifa, Anamary; Almirall, José R

2015-05-01

A rapid method for the characterization of both organic and inorganic components of gunshot residues (GSR) is proposed as an alternative tool to facilitate the identification of a suspected shooter. In this study, two fast screening methods were developed and optimized for the detection of organic compounds and inorganic components indicative of GSR presence on the hands of shooters and non-shooters. The proposed methods consist of headspace extraction of volatile organic compounds using a capillary microextraction of volatiles (CMV) device previously reported as a high-efficiency sampler followed by detection by GC-MS. This novel sampling technique has the potential to yield fast results (<2min sampling) and high sensitivity capable of detecting 3ng of diphenylamine (DPA) and 8ng of nitroglycerine (NG). Direct analysis of the headspace of over 50 swabs collected from the hands of suspected shooters (and non-shooters) provides information regarding VOCs present on their hands. In addition, a fast laser induced breakdown spectroscopy (LIBS) screening method for the detection of the inorganic components indicative of the presence of GSR (Sb, Pb and Ba) is described. The sampling method for the inorganics consists of liquid extraction of the target elements from the same cotton swabs (previously analyzed for VOCs) and an additional 30 swab samples followed by spiking 1μL of the extract solution onto a Teflon disk and then analyzed by LIBS. Advantages of LIBS include fast analysis (~12s per sample) and high selectivity and sensitivity, with expected LODs 0.1-18ng for each of the target elements after sampling. The analytical performance of the LIBS method is also compared to previously reported methods (inductively coupled plasma-optical emission spectroscopy). The combination of fast CMV sampling, unambiguous organic compound identification with GC-MS and fast LIBS analysis provides the basis for a new comprehensive screening method for GSR. Copyright © 2015 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

Effect of the hydroalcoholic extract and juice of Prunus divaricata fruit on blood glucose and serum lipids of normal and streptozotocin-induced diabetic rats

PubMed Central

Minaiyan, M.; Ghannadi, A.; Movahedian, A.; Ramezanlou, P.; Osooli, F.S.

2014-01-01

Prunus divaricata (Alloocheh) is a small tree cultivating in Iran, Middle East and central Asia. Prunus genus has many species with anti-oxidant, anti-hyperlipidemia and anti-hyperglycemia effects. In the present study the anti-diabetic and anti-hyperlipidemic effects of P. divaricata fruits were examined in normal and streptozotocin (STZ)-induced diabetic rats. Both groups, control and reference rats received normal saline and glibenclamide respectively. Test groups were treated with Prunus freeze dried juice (PFDJ, 200, 400, 800 mg/kg) and Prunus freeze dried extract (PFDE, 100, 200, 400 mg/kg) started at the 3rd day of the experiment and continued for 27 days thereafter. Weight changes of animals were checked periodically. Fasting blood glucose (FBG) level as well as serum triglyceride (TG), total cholesterol (TC), high density lipoprotein (HDL) and low density lipoprotein (LDL) cholesterol were determined. Different treatments had no significant effect on body weight increments of normal rats, while in diabetic rats, PFDJ (800 mg/kg) and PFDE (400 mg/kg) opposed with weight loss. In acute phase of experiment (0-8 h of 3rd day), none of tested fractions were effective in reducing FBG and serum lipids of normal rats. During the sub-acute phase (13th and 30th days) however, the greatest test doses of PFDJ (800 mg/kg) and PFDE (400 mg/kg) induced hypoglycema. In diabetic groups, PFDJ and PFDE, at all test doses, could diminish FBG during sub-acute phase of the experiment. In addition, PFDJ and PFDE at most examined doses could diminish TG significantly and they were also effective on cholesterol derivatives in different magnitude. PMID:26339257

Large-volume injection of sample diluents not miscible with the mobile phase as an alternative approach in sample preparation for bioanalysis: an application for fenspiride bioequivalence.

PubMed

Medvedovici, Andrei; Udrescu, Stefan; Albu, Florin; Tache, Florentin; David, Victor

2011-09-01

Liquid-liquid extraction of target compounds from biological matrices followed by the injection of a large volume from the organic layer into the chromatographic column operated under reversed-phase (RP) conditions would successfully combine the selectivity and the straightforward character of the procedure in order to enhance sensitivity, compared with the usual approach of involving solvent evaporation and residue re-dissolution. Large-volume injection of samples in diluents that are not miscible with the mobile phase was recently introduced in chromatographic practice. The risk of random errors produced during the manipulation of samples is also substantially reduced. A bioanalytical method designed for the bioequivalence of fenspiride containing pharmaceutical formulations was based on a sample preparation procedure involving extraction of the target analyte and the internal standard (trimetazidine) from alkalinized plasma samples in 1-octanol. A volume of 75 µl from the octanol layer was directly injected on a Zorbax SB C18 Rapid Resolution, 50 mm length × 4.6 mm internal diameter × 1.8 µm particle size column, with the RP separation being carried out under gradient elution conditions. Detection was made through positive ESI and MS/MS. Aspects related to method development and validation are discussed. The bioanalytical method was successfully applied to assess bioequivalence of a modified release pharmaceutical formulation containing 80 mg fenspiride hydrochloride during two different studies carried out as single-dose administration under fasting and fed conditions (four arms), and multiple doses administration, respectively. The quality attributes assigned to the bioanalytical method, as resulting from its application to the bioequivalence studies, are highlighted and fully demonstrate that sample preparation based on large-volume injection of immiscible diluents has an increased potential for application in bioanalysis.

Aqueous two-phase assisted by ultrasound for the extraction of anthocyanins from Lycium ruthenicum Murr.

PubMed

Qin, Benlin; Liu, Xuecong; Cui, Haiming; Ma, Yue; Wang, Zimin; Han, Jing

2017-10-21

In this study, an efficient ultrasound-assisted aqueous two-phase extraction method was used for the extraction of anthocyanins from Lycium ruthenicum Murr. An ethanol/ammonium sulfate system was chosen for the aqueous two-phase system due to its fine partitioning and recycling behaviors. Single-factor experiments were conducted to determine the optimized composition of the system, and the response surface methodology was used for the further optimization of the ultrasound-assisted aqueous two-phase extraction. The optimal conditions were as follows: a salt concentration of 20%, an ethanol concentration of 25%, an extraction time of 33.7 min, an extraction temperature of 25°C, a liquid/solid ratio of 50:1 w/w, pH value of 3.98, and an ultrasound power of 600 W. Under the above conditions, the yields of anthocyanins reached 4.71 mg/g dry sample. For the further purification, D-101 resin was used, and the purity of anthocyanins reached 25.3%. In conclusion, ultrasound-assisted aqueous two-phase extraction was an efficient, ecofriendly, and economical method, and it may be a promising technique for extracting bioactive components from plants.

Antitumor activity of ethanol extract from Hippophae rhamnoides L. leaves towards human acute myeloid leukemia cells in vitro.

PubMed

Zhamanbaeva, G T; Murzakhmetova, M K; Tuleukhanov, S T; Danilenko, M P

2014-12-01

We studied the effects of ethanol extract from Hippophae rhamnoides L. leaves on the growth and differentiation of human acute myeloid leukemia cells (KG-1a, HL60, and U937). The extract of Hippophae rhamnoides L. leaves inhibited cell growth depending on the cell strain and extract dose. In a high concentration (100 μg/ml), the extract also exhibited a cytotoxic effect on HL60 cells. Hippophae rhamnoides L. leaves extract did not affect cell differentiation and did not modify the differentiating effect of calcitriol, active vitamin D metabolite. Inhibition of cell proliferation was paralleled by paradoxical accumulation of phase S cells (synthetic phase) with a reciprocal decrease in the count of G1 cells (presynthetic phase). The extract in a concentration of 100 μg/ml induced the appearance of cells with a subdiploid DNA content (sub-G1 phase cells), which indicated induction of apoptosis. The antiproliferative effect of Hippophae rhamnoides L. extract on acute myeloid leukemia cells was at least partially determined by activation of the S phase checkpoint, which probably led to deceleration of the cell cycle and apoptosis induction.

Key experimental information on intermediate-range atomic structures in amorphous Ge2Sb2Te5 phase change material

NASA Astrophysics Data System (ADS)

Hosokawa, Shinya; Pilgrim, Wolf-Christian; Höhle, Astrid; Szubrin, Daniel; Boudet, Nathalie; Bérar, Jean-François; Maruyama, Kenji

2012-04-01

Laser-induced crystalline-amorphous phase change of Ge-Sb-Te alloys is the key mechanism enabling the fast and stable writing/erasing processes in rewritable optical storage devices, such as digital versatile disk (DVD) or blu-ray disk. Although the structural information in the amorphous phase is essential for clarifying this fast process, as well as long lasting stabilities of both the phases, experimental works were mostly limited to the short-range order by x ray absorption fine structure. Here we show both the short and intermediate-range atomic structures of amorphous DVD material, Ge2Sb2Te5 (GST), investigated by a combination of anomalous x ray scattering and reverse Monte Carlo modeling. From the obtained atomic configurations of amorphous GST, we have found that the Sb atoms and half of the Ge atoms play roles in the fast phase change process of order-disorder transition, while the remaining Ge atoms act for the proper activation energy of barriers between the amorphous and crystalline phases.

Proline 54 trans-cis isomerization is responsible for the kinetic partitioning at the last-step photocycle of photoactive yellow protein

PubMed Central

Lee, Byoung-Chul; Hoff, Wouter D.

2008-01-01

Photoactive yellow protein (PYP), a blue-light photoreceptor for Ectothiorhodospira halophila, has provided a unique system for studying protein folding that is coupled with a photocycle. Upon receptor activation by blue light, PYP proceeds through a photocycle that includes a partially folded signaling state. The last-step photocycle is a thermal recovery reaction from the signaling state to the native state. Bi-exponential kinetics had been observed for the last-step photocycle; however, the slow phase of the bi-exponential kinetics has not been extensively studied. Here we analyzed both fast and slow phases of the last-step photocycle in PYP. From the analysis of the denaturant dependence of the fast and slow phases, we found that the last-step photocycle proceeds through parallel channels of the folding pathway. The burial of the solvent-accessible area was responsible for the transition state of the fast phase, while structural rearrangement from the compact state to the native state was responsible for the transition state of the slow phase. The photocycle of PYP was linked to the thermodynamic cycle that includes both unfolding and refolding of the fast- and slow-phase intermediates. In order to test the hypothesis of proline-limited folding for the slow phase, we constructed two proline mutants: P54A and P68A. We found that only a single phase of the last-step photocycle was observed in P54A. This suggests that there is a low energy barrier between trans to cis conformation in P54 in the light-induced state of PYP, and the resulting cis conformation of P54 generates a slow-phase kinetic trap during the photocycle-coupled folding pathway of PYP. PMID:18794212

Direct online extraction and determination by supercritical fluid extraction with chromatography and mass spectrometry of targeted carotenoids from red Habanero peppers (Capsicum chinense Jacq.).

PubMed

Zoccali, Mariosimone; Giuffrida, Daniele; Dugo, Paola; Mondello, Luigi

2017-10-01

Recently, supercritical fluid chromatography coupled to mass spectrometry has gained attention as a fast and useful technology applied to the carotenoids analysis. However, no reports are available in the literature on the direct online extraction and determination by supercritical fluid extraction with chromatography and mass spectrometry. The aim of this research was the development of an online method coupling supercritical fluid extraction and supercritical fluid chromatography for a detailed targeted native carotenoids characterization in red habanero peppers. The online nature of the system, compared to offline approaches, improves run-to-run precision, enables the setting of batch-type applications, and reduces the risks of sample contamination. The extraction has been optimized using different temperatures, starting from 40°C up to 80°C. Multiple extractions, until depletion, were performed on the same sample to evaluate the extraction yield. The range of the first extraction yield, carried out at 80°C, which was the best extraction temperature, was 37.4-65.4%, with a %CV range of 2-12. Twenty-one targeted analytes were extracted and identified by the developed methodology in less than 17 min, including free, monoesters, and diesters carotenoids, in a very fast and efficient way. Quantification of the β-carotene was carried out by using the optimized conditions. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preconcentration of aqueous dyes through phase-transfer liquid-phase microextraction with a room-temperature ionic liquid.

PubMed

Chen, Hsiu-Liang; Chang, Shuo-Kai; Lee, Chia-Ying; Chuang, Li-Lin; Wei, Guor-Tzo

2012-09-12

In this study, we employed the room-temperature ionic liquid [bmim][PF(6)] as both ion-pair agent and an extractant in the phase-transfer liquid-phase microextraction (PTLPME) of aqueous dyes. In the PTLPME method, a dye solution was added to the extraction solution, comprising a small amount of [bmim][PF(6)] in a relatively large amount of CH(2)Cl(2), which serves as the disperser solvent to an extraction solution. Following extraction, CH(2)Cl(2) was evaporated from the extractant, resulting in the extracted dyes being concentrated in a small volume of the ionic liquid phase to increase the enrichment factor. The enrichment factors of for the dye Methylene Blue, Neutral Red, and Methyl Red were approximately 500, 550 and 400, respectively; their detection limits were 0.014, 0.43, and 0.02 μg L(-1), respectively, with relative standard deviations of 4.72%, 4.20%, and 6.10%, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Precision and fast wavelength tuning of a dynamically phase-locked widely-tunable laser.

PubMed

Numata, Kenji; Chen, Jeffrey R; Wu, Stewart T

2012-06-18

We report a precision and fast wavelength tuning technique demonstrated for a digital-supermode distributed Bragg reflector laser. The laser was dynamically offset-locked to a frequency-stabilized master laser using an optical phase-locked loop, enabling precision fast tuning to and from any frequencies within a ~40-GHz tuning range. The offset frequency noise was suppressed to the statically offset-locked level in less than ~40 μs upon each frequency switch, allowing the laser to retain the absolute frequency stability of the master laser. This technique satisfies stringent requirements for gas sensing lidars and enables other applications that require such well-controlled precision fast tuning.

Structural analysis of pyrolytic lignins isolated from switchgrass fast pyrolysis oil

USDA-ARS?s Scientific Manuscript database

Structural characterization of lignin extracted from the bio-oil produced by fast pyrolysis of switchgrass (Panicum virgatum) is reported. This new information is important to understanding the utility of lignin as a chemical feedstock in a pyrolysis based biorefinery. Pyrolysis induces a variety of...

Interactions of cervico-ocular and vestibulo-ocular fast-phase signals in the control of eye position in rabbits.

PubMed Central

Barmack, N H; Errico, P; Ferraresi, A; Pettorossi, V E

1989-01-01

1. Eye movements in unanaesthetized rabbits were studied during horizontal neck-proprioceptive stimulation (movement of the body with respect to the fixed head), when this stimulation was given alone and when it was given simultaneously with vestibular stimulation (rotation of the head-body). The effect of neck-proprioceptive stimulation on modifying the anticompensatory fast-phase eye movements (AFPs) evoked by vestibular stimulation was studied with a 'conditioning-test' protocol; the 'conditioning' stimulus was a neck-proprioceptive signal evoked by a step-like change in body position with respect to the head and the 'test' stimulus was a vestibular signal evoked by a step rotation of the head-body. 2. The influence of eye position and direction of slow eye movements on the occurrence of compensatory fast-phase eye movements (CFPs) evoked by neck-proprioceptive stimulation was also examined. 3. The anticompensatory fast phase (AFP) evoked by vestibular stimulation was attenuated by a preceding neck-proprioceptive stimulus which when delivered alone evoked compensatory slow-phase eye movements (CSP) in the same direction as the CSP evoked by vestibular stimulation. Conversely, the vestibularly evoked AFP was potentiated by a neck-proprioceptive stimulus which evoked CSPs opposite to that of vestibularly evoked CSPs. 4. Eccentric initial eye positions increased the probability of occurrence of midline-directed compensatory fast-phase eye movements (CFPs) evoked by appropriate neck-proprioceptive stimulation. 5. The gain of the horizontal cervico-ocular reflex (GHCOR) was measured from the combined changes in eye position resulting from AFPs and CSPs. GHCOR was potentiated during simultaneous vestibular stimulation. This enhancement of GHCOR occurred at neck-proprioceptive stimulus frequencies which, in the absence of conjoint vestibular stimulation, do not evoke CSPs. PMID:2795479

Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

PubMed

Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

2016-04-01

Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

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

PubMed

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

2017-02-01

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

Experimental and computational studies on molecularly imprinted solid-phase extraction for gonyautoxins 2,3 from dinoflagellate Alexandrium minutum.

PubMed

Lian, Ziru; Li, Hai-Bei; Wang, Jiangtao

2016-08-01

An innovative and effective extraction procedure based on molecularly imprinted solid-phase extraction (MISPE) was developed for the isolation of gonyautoxins 2,3 (GTX2,3) from Alexandrium minutum sample. Molecularly imprinted polymer microspheres were prepared by suspension polymerization and and were employed as sorbents for the solid-phase extraction of GTX2,3. An off-line MISPE protocol was optimized. Subsequently, the extract samples from A. minutum were analyzed. The results showed that the interference matrices in the extract were obviously cleaned up by MISPE procedures. This outcome enabled the direct extraction of GTX2,3 in A. minutum samples with extraction efficiency as high as 83 %, rather significantly, without any need for a cleanup step prior to the extraction. Furthermore, computational approach also provided direct evidences of the high selective isolation of GTX2,3 from the microalgal extracts.

Fast optimization method of designing a wideband metasurface without using the Pancharatnam-Berry phase.

PubMed

Sui, Sai; Ma, Hua; Lv, Yueguang; Wang, Jiafu; Li, Zhiqiang; Zhang, Jieqiu; Xu, Zhuo; Qu, Shaobo

2018-01-22

Arbitrary control of electromagnetic waves remains a significant challenge although it promises many important applications. Here, we proposed a fast optimization method of designing a wideband metasurface without using the Pancharatnam-Berry (PB) phase, of which the elements are non-absorptive and capable of predicting the wideband and smooth phase-shift. In our design method, the metasurface is composed of low-Q-factor resonant elements without using the PB phase, and is optimized by the genetic algorithm and nonlinear fitting method, having the advantages that the far field scattering patterns can be quickly synthesized by the hybrid array patterns. To validate the design method, a wideband low radar cross section metasurface is demonstrated, showing good feasibility and performance of wideband RCS reduction. This work reveals an opportunity arising from a metasurface in effective manipulation of microwave and flexible fast optimal design method.

Apparatus and Method to Enable Precision and Fast Laser Frequency Tuning

NASA Technical Reports Server (NTRS)

Chen, Jeffrey R. (Inventor); Numata, Kenji (Inventor); Wu, Stewart T. (Inventor); Yang, Guangning (Inventor)

2015-01-01

An apparatus and method is provided to enable precision and fast laser frequency tuning. For instance, a fast tunable slave laser may be dynamically offset-locked to a reference laser line using an optical phase-locked loop. The slave laser is heterodyned against a reference laser line to generate a beatnote that is subsequently frequency divided. The phase difference between the divided beatnote and a reference signal may be detected to generate an error signal proportional to the phase difference. The error signal is converted into appropriate feedback signals to phase lock the divided beatnote to the reference signal. The slave laser frequency target may be rapidly changed based on a combination of a dynamically changing frequency of the reference signal, the frequency dividing factor, and an effective polarity of the error signal. Feed-forward signals may be generated to accelerate the slave laser frequency switching through laser tuning ports.

The Chemistry of Separations Ligand Degradation by Organic Radical Cations

DOE PAGES

Mezyk, Stephen P.; Horne, Gregory P.; Mincher, Bruce J.; ...

2016-12-01

Solvent based extractions of used nuclear fuel use designer ligands in an organic phase extracting ligand complexed metal ions from an acidic aqueous phase. These extractions will be performed in highly radioactive environments, and the radiation chemistry of all these complexants and their diluents will play a major role in determining extraction efficiency, separation factors, and solvent-recycle longevity. Although there has been considerable effort in investigating ligand damage occurring in acidic water radiolysis conditions, only minimal fundamental kinetic and mechanistic data has been reported for the degradation of extraction ligands in the organic phase. Extraction solvent phases typically use normalmore » alkanes such as dodecane, TPH, and kerosene as diluents. The radiolysis of such diluents produce a mixture of radical cations (R •+), carbon-centered radicals (R •), solvated electrons, and molecular products such as hydrogen. Typically, the radical species will preferentially react with the dissolved oxygen present to produce relatively inert peroxyl radicals. This isolates the alkane radical cation species, R •+ as the major radiolytically-induced organic species that can react with, and degrade, extraction agents in this phase. Here we report on our recent studies of organic radical cation reactions with various ligands. Elucidating these parameters, and combining them with the known acidic aqueous phase chemistry, will allow a full, fundamental, understanding of the impact of radiation on solvent extraction based separation processes to be achieved.« less

Three phases hollow fiber LPME combined with HPLC-UV for extraction, preconcentration and determination of valerenic acid in Valeriana officinalis.

PubMed

Mirzaei, Mohamad; Dinpanah, Hossein

2011-07-01

In the present work, the applicability of hollow fiber-based liquid phase microextraction (HF-LPME) was evaluated for the extraction and preconcentration of valerenic acid prior to its determination by reversed-phase HPLC/UV. The target drug was extracted from 5.0 mL of aqueous solution with pH 3.5 into an organic extracting solvent (dihexyl ether) impregnated in the pores of a hollow fiber and finally back extracted into 10 μ L of aqueous solution with pH 9.5 located inside the lumen of the hollow fiber. In order to obtain high extraction efficiency, the parameters affecting the HF-LPME, including pH of the donor and acceptor phases, type of organic phase, ionic strength, the volume ratio of donor to acceptor phase, stirring rate and extraction time were studied and optimized. Under the optimized conditions, enrichment factor up to 446 was achieved and the relative standard deviation (RSD) of the method was 4.36% (n = 9). The linear range was 7.5-850 μg L⁻¹ with correlation coefficient (r²=0.999), detection limits was 2.5 μg L⁻¹ and the LOQ was 7.5 μg L⁻¹. The proposed method was evaluated by extraction and determination of valerenic acid in some Iranian wild species of Valerianaceae. Copyright © 2011 Elsevier B.V. All rights reserved.

The Chemistry of Separations Ligand Degradation by Organic Radical Cations

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

Mezyk, Stephen P.; Horne, Gregory P.; Mincher, Bruce J.

Solvent based extractions of used nuclear fuel use designer ligands in an organic phase extracting ligand complexed metal ions from an acidic aqueous phase. These extractions will be performed in highly radioactive environments, and the radiation chemistry of all these complexants and their diluents will play a major role in determining extraction efficiency, separation factors, and solvent-recycle longevity. Although there has been considerable effort in investigating ligand damage occurring in acidic water radiolysis conditions, only minimal fundamental kinetic and mechanistic data has been reported for the degradation of extraction ligands in the organic phase. Extraction solvent phases typically use normalmore » alkanes such as dodecane, TPH, and kerosene as diluents. The radiolysis of such diluents produce a mixture of radical cations (R •+), carbon-centered radicals (R •), solvated electrons, and molecular products such as hydrogen. Typically, the radical species will preferentially react with the dissolved oxygen present to produce relatively inert peroxyl radicals. This isolates the alkane radical cation species, R •+ as the major radiolytically-induced organic species that can react with, and degrade, extraction agents in this phase. Here we report on our recent studies of organic radical cation reactions with various ligands. Elucidating these parameters, and combining them with the known acidic aqueous phase chemistry, will allow a full, fundamental, understanding of the impact of radiation on solvent extraction based separation processes to be achieved.« less

Intense steady state electron beam generator

DOEpatents

Hershcovitch, A.; Kovarik, V.J.; Prelec, K.

1990-07-17

An intense, steady state, low emittance electron beam generator is formed by operating a hollow cathode discharge plasma source at critical levels in combination with an extraction electrode and a target electrode that are operable to extract a beam of fast primary electrons from the plasma source through a negatively biased grid that is critically operated to repel bulk electrons toward the plasma source while allowing the fast primary electrons to move toward the target in the desired beam that can be successfully transported for relatively large distances, such as one or more meters away from the plasma source. 2 figs.

Intense steady state electron beam generator

DOEpatents

Hershcovitch, Ady; Kovarik, Vincent J.; Prelec, Krsto

1990-01-01

An intense, steady state, low emittance electron beam generator is formed by operating a hollow cathode discharge plasma source at critical levels in combination with an extraction electrode and a target electrode that are operable to extract a beam of fast primary electrons from the plasma source through a negatively biased grid that is critically operated to repel bulk electrons toward the plasma source while allowing the fast primary electrons to move toward the target in the desired beam that can be successfully transported for relatively large distances, such as one or more meters away from the plasma source.

Method for separating water soluble organics from a process stream by aqueous biphasic extraction

DOEpatents

Chaiko, David J.; Mego, William A.

1999-01-01

A method for separating water-miscible organic species from a process stream by aqueous biphasic extraction is provided. An aqueous biphase system is generated by contacting a process stream comprised of water, salt, and organic species with an aqueous polymer solution. The organic species transfer from the salt-rich phase to the polymer-rich phase, and the phases are separated. Next, the polymer is recovered from the loaded polymer phase by selectively extracting the polymer into an organic phase at an elevated temperature, while the organic species remain in a substantially salt-free aqueous solution. Alternatively, the polymer is recovered from the loaded polymer by a temperature induced phase separation (cloud point extraction), whereby the polymer and the organic species separate into two distinct solutions. The method for separating water-miscible organic species is applicable to the treatment of industrial wastewater streams, including the extraction and recovery of complexed metal ions from salt solutions, organic contaminants from mineral processing streams, and colorants from spent dye baths.

Isolation and recovery of selected polybrominated diphenyl ethers from human serum and sheep serum: coupling reversed-phase solid-phase disk extraction and liquid-liquid extraction techniques with a capillary gas chromatographic electron capture negative ion mass spectrometric determinative technique.

PubMed

Loconto, Paul R; Isenga, David; O'Keefe, Michael; Knottnerus, Mark

2008-01-01

Polybrominated diphenyl ethers (PBDEs) are isolated and recovered with acceptable percent recoveries from human serum via liquid-liquid extraction and column chromatographic cleanup and fractionation with quantitation using capillary gas chromatography-mass spectrometry with electron capture negative ion and selected ion monitoring. PBDEs are found in unspiked serum. An alternative sample preparation approach is developed using sheep serum that utilizes a formic acid pre-treatment followed by reversed-phase solid-phase disk extraction and normal-phase solid-phase cleanup using acidified silica gel that yields>50% recoveries. When these percent recoveries are combined with a minimized phase ratio for human serum and very low instrument detection limits, method detection limits below 500 parts-per-trillion are realized.

Phase stabilization for mode locked lasers

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

Baer, M.T.

A method is described for stabilizing a phase relationship between two mode locked lasers, comprising: driving through a power splitter the mode lockers of both lasers from a single stable radio frequency source; monitoring the phase of pulses from each laser utilizing a fast photodiode output of each laser; feeding the output of the fast photodiodes to a phase detector and comparator; measuring a relative phase difference between the lasers with a phase detector and comparator, producing a voltage output signal or phase error signal representing the phase difference; amplifying and filtering the voltage output signal with an amplifier andmore » loop filter; feeding the resulting output signal to a voltage controlled phase delay between the power splitter and one of the lasers; and delaying the RF drive to the one laser to achieve a desired phase relationship, between the two lasers.« less

Ultra fast polymer network blue phase liquid crystals

NASA Astrophysics Data System (ADS)

Hussain, Zakir; Masutani, Akira; Danner, David; Pleis, Frank; Hollfelder, Nadine; Nelles, Gabriele; Kilickiran, Pinar

2011-06-01

Polymer-stabilization of blue phase liquid crystal systems within a host polymer network are reported, which enables ultrafast switching flexible displays. Our newly developed method to stabilize the blue phase in an existing polymer network (e.g., that of a polymer network liquid crystal; PNLC) has shown wide temperature stability and fast response speeds. Systems where the blue phase is stabilized in an already existing polymer network are attractive candidates for ultrafast LCDs. The technology also promises to be applied to flexible PNLC and/or polymer dispersed liquid crystal (PDLC) displays using plastic substrate such as polyethylene terephthalate (PET).

Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets.

PubMed

Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Rashidi, Ali Morad; Shirkhanloo, Hamid; Rahighi, Reza

2016-01-01

A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL(-1)), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL(-1)). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L(-1) for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24-15.6, 0.015-0.95 and 0.039-2.33 µg L(-1) for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned metal ions in river water, human urine and saliva sample with good recoveries in range of 94.2-103.0%. The accuracy of the method was underpinned by correct analysis of a standard reference material (SRM: 2668 level I, Urine). Copyright © 2015 Elsevier B.V. All rights reserved.

A rapid solid-phase extraction method for measurement of non-metabolised peripheral benzodiazepine receptor ligands, [(18)F]PBR102 and [(18)F]PBR111, in rat and primate plasma.

PubMed

Katsifis, Andrew; Loc'h, Christian; Henderson, David; Bourdier, Thomas; Pham, Tien; Greguric, Ivan; Lam, Peter; Callaghan, Paul; Mattner, Filomena; Eberl, Stefan; Fulham, Michael

2011-01-01

To develop a rapid and reliable method for estimating non-metabolised PBR ligands fluoroethoxy ([(18)F]PBR102)- and fluoropropoxy ([(18)F]PBR111)-substituted 2-(6-chloro-2-phenyl)imidazo[1,2-a]pyridine-3-yl)-N,N-diethylacetamides in plasma. Rats and baboons were imaged with PET up to 2 h postinjection of [(18)F]PBR102 and [(18)F]PBR111 under baseline conditions, after pre-blocking or displacement with PK11195. Arterial plasma samples were directly analysed by reverse-phase solid-phase extraction (RP-SPE) and RP-HPLC and by normal-phase TLC. SPE cartridges were successively washed with acetonitrile/water mixtures. SPE eluant radioactivity was measured in a γ-counter to determine the parent compound fraction and then analysed by HPLC and TLC for validation. In SPE, hydrophilic and lipophilic radiolabelled metabolites were eluted in water and 20% acetonitrile/water. All non-metabolised [(18)F]PBR102 and [(18)F]PBR111 were in SPE acetonitrile fraction as confirmed by HPLC and TLC analysis. Unchanged (%) [(18)F]PBR102 and [(18)F]PBR111 from SPE analysis in rat and baboon plasma agreed with those from HPLC and TLC analysis. In rats and baboons, the fraction of unchanged tracer followed a bi-exponential decrease, with half-lives of 7 to 10 min for the fast component and >80 min for the slow component for both tracers. Direct plasma SPE analysis of [(18)F]PBR102 and [(18)F]PBR111 can reliably estimate parent compound fraction. SPE was superior to HPLC for samples with low activity; it allows rapid and accurate metabolite analysis of a large number of plasma samples for improved estimation of metabolite-corrected input function during quantitative PET imaging studies. Crown Copyright © 2011. Published by Elsevier Inc. All rights reserved.

Physically incorporated extraction phase of solid-phase microextraction by sol-gel technology.

PubMed

Liu, Wenmin; Hu, Yuan; Zhao, Jinghong; Xu, Yuan; Guan, Yafeng

2006-01-13

A sol-gel method for the preparation of solid-phase microextraction (SPME) fiber was described and evaluated. The extraction phase of poly(dimethysiloxane) (PDMS) containing 3% vinyl group was physically incorporated into the sol-gel network without chemical bonding. The extraction phase itself is then partly crosslinked at 320 degrees C, forming an independent polymer network and can withstand desorption temperature of 290 degrees C. The headspace extraction of BTX by the fiber SPME was evaluated and the detection limit of o-xylene was down to 0.26 ng/l. Extraction and determination of organophosphorus pesticides (OPPs) in water, orange juice and red wine by the SPME-GC thermionic specified detector (TSD) was validated. Limits of detection of the method for OPPs were below 10 ng/l except methidathion. Relative standard deviations (RSDs) were in the range of 1-20% for pesticides being tested.

High-performance liquid chromatography with fast-scanning fluorescence detection and multivariate curve resolution for the efficient determination of galantamine and its main metabolites in serum.

PubMed

Culzoni, María J; Aucelio, Ricardo Q; Escandar, Graciela M

2012-08-31

Based on green analytical chemistry principles, an efficient approach was applied for the simultaneous determination of galantamine, a widely used cholinesterase inhibitor for the treatment of Alzheimer's disease, and its major metabolites in serum samples. After a simple serum deproteinization step, second-order data were rapidly obtained (less than 6 min) with a chromatographic system operating in the isocratic regime using ammonium acetate/acetonitrile (94:6) as mobile phase. Detection was made with a fast-scanning spectrofluorimeter, which allowed the efficient collection of data to obtain matrices of fluorescence intensity as a function of retention time and emission wavelength. Successful resolution was achieved in the presence of matrix interferences in serum samples using multivariate curve resolution-alternating least-squares (MCR-ALS). The developed approach allows the quantification of the analytes at levels found in treated patients, without the need of applying either preconcentration or extraction steps. Limits of detection in the range between 8 and 11 ng mL(-1), relative prediction errors from 7 to 12% and coefficients of variation from 4 to 7% were achieved. Copyright © 2012 Elsevier B.V. All rights reserved.

PAH detection in Quercus robur leaves and Pinus pinaster needles: A fast method for biomonitoring purpose.

PubMed

De Nicola, F; Concha Graña, E; Aboal, J R; Carballeira, A; Fernández, J Á; López Mahía, P; Prada Rodríguez, D; Muniategui Lorenzo, S

2016-06-01

Due to the complexity and heterogeneity of plant matrices, new procedure should be standardized for each single biomonitor. Thus, here is described a matrix solid-phase dispersion extraction method, previously used for moss samples, improved and modified for the analyses of PAHs in Quercus robur leaves and Pinus pinaster needles, species widely used in biomonitoring studies across Europe. The improvements compared to the previous procedure are the use of Florisil added with further clean-up sorbents, 10% deactivated silica for pine needles and PSA for oak leaves, being these matrices rich in interfering compounds, as shown by the gas chromatography-mass spectrometry analyses acquired in full scan mode. Good trueness, with values in the range 90-120% for the most of compounds, high precision (intermediate precision between 2% and 12%) and good sensitivity using only 250mg of samples (limits of quantification lower than 3 and 1.5ngg(-1), respectively for pine and oak) were achieved by the selected procedures. These methods proved to be reliable for PAH analyses and, having advantage of fastness, can be used in biomonitoring studies of PAH air contamination. Copyright © 2016 Elsevier B.V. All rights reserved.

A simple, fast and sensitive screening LC-ESI-MS/MS method for antibiotics in fish.

PubMed

Guidi, Letícia Rocha; Santos, Flávio Alves; Ribeiro, Ana Cláudia S R; Fernandes, Christian; Silva, Luiza H M; Gloria, Maria Beatriz A

2017-01-15

The objective of this study was to develop and validate a fast, sensitive and simple liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method for the screening of six classes of antibiotics (aminoglycosides, beta-lactams, macrolides, quinolones, sulfonamides and tetracyclines) in fish. Samples were extracted with trichloroacetic acid. LC separation was achieved on a Zorbax Eclipse XDB C18 column and gradient elution using 0.1% heptafluorobutyric acid in water and acetonitrile as mobile phase. Analysis was carried out in multiple reaction monitoring mode via electrospray interface operated in the positive ionization mode, with sulfaphenazole as internal standard. The method was suitable for routine screening purposes of 40 antibiotics, according to EC Guidelines for the Validation of Screening Methods for Residues of Veterinary Medicines, taking into consideration threshold value, cut-off factor, detection capability, limit of detection, sensitivity and specificity. Real fish samples (n=193) from aquaculture were analyzed and 15% were positive for enrofloxacin (quinolone), one of them at a higher concentration than the level of interest (50µgkg -1 ), suggesting possible contamination or illegal use of that antibiotic. Copyright © 2016 Elsevier B.V. All rights reserved.

One-step electrochemical deposition of a graphene-ZrO 2 nanocomposite: Preparation, characterization and application for detection of organophosphorus agents

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

Du, Dan; Liu, Juan; Zhang, Xiao-Yan

2011-04-27

This paper described the preparation, characterization, and electrochemical properties of a graphene-ZrO 2 nanocomposite (GZN) and its application for both the enrichment and detection of methyl parathion (MP). GZN was fabricated using electrochemical deposition and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), which showed the successful formation of nanocomposites. Due to the strong affinity to the phosphoric group and the fast electron-transfer kinetics of GZN, both the extraction and electrochemical detection of organophosphorus (OP) agents at the same GZN modified electrochemical sensor was possible. The combination of solid-phase extractionmore » and stripping voltammetric analysis allowed fast, sensitive, and selective determination of MP in garlic samples. The stripping response was highly linear over the MP concentrations ranging from 0.5 ng mL -1 to 100 ng mL -1, with a detection limit of 0.1 ng mL -1. This new nanocomposite-based electrochemical sensor provides an opportunity to develop a field-deployable, sensitive, and quantitative method for monitoring exposure to OPs.« less

Validation of a fast and accurate chromatographic method for detailed quantification of vitamin E in green leafy vegetables.

PubMed

Cruz, Rebeca; Casal, Susana

2013-11-15

Vitamin E analysis in green vegetables is performed by an array of different methods, making it difficult to compare published data or choosing the adequate one for a particular sample. Aiming to achieve a consistent method with wide applicability, the current study reports the development and validation of a fast micro-method for quantification of vitamin E in green leafy vegetables. The methodology uses solid-liquid extraction based on the Folch method, with tocol as internal standard, and normal-phase HPLC with fluorescence detection. A large linear working range was confirmed, being highly reproducible, with inter-day precisions below 5% (RSD). Method sensitivity was established (below 0.02 μg/g fresh weight), and accuracy was assessed by recovery tests (>96%). The method was tested in different green leafy vegetables, evidencing diverse tocochromanol profiles, with variable ratios and amounts of α- and γ-tocopherol, and other minor compounds. The methodology is adequate for routine analyses, with a reduced chromatographic run (<7 min) and organic solvent consumption, and requires only standard chromatographic equipment available in most laboratories. Copyright © 2013 Elsevier Ltd. All rights reserved.

Polyamines and inorganic ions extracted from woody tissues by freeze-thawing

Treesearch

Rakesh Minocha; Walter C. Shortle

1994-01-01

A simple and fast method for extraction of major inorganic ions (Ca, Mg, Mn, K, and P) and cellular polyamines from small quantities of wood and woody plant tissues is described. The method involves repeated freezing and thawing of samples instead of homogenization or wet ash digestion. The efficiency of extraction of both polyamines and inorganic ions by these methods...

Instantaneous phase estimation to measure weak velocity variations: application to noise correlation on seismic data at the exploration scale

NASA Astrophysics Data System (ADS)

Corciulo, M.; Roux, P.; Campillo, M.; Dubucq, D.

2010-12-01

Passive imaging from noise cross-correlation is a consolidated analysis applied at continental and regional scale whereas its use at local scale for seismic exploration purposes is still uncertain. The development of passive imaging by cross-correlation analysis is based on the extraction of the Green’s function from seismic noise data. In a completely random field in time and space, the cross-correlation permits to retrieve the complete Green’s function whatever the complexity of the medium. At the exploration scale and at frequency above 2 Hz, the noise sources are not ideally distributed around the stations which strongly affect the extraction of the direct arrivals from the noise cross-correlation process. In order to overcome this problem, the coda waves extracted from noise correlation could be useful. Coda waves describe long and scattered paths sampling the medium in different ways such that they become sensitive to weak velocity variations without being dependent on the noise source distribution. Indeed, scatters in the medium behave as a set of secondary noise sources which randomize the spatial distribution of noise sources contributing to the coda waves in the correlation process. We developed a new technique to measure weak velocity changes based on the computation of the local phase variations (instantaneous phase variation or IPV) of the cross-correlated signals. This newly-developed technique takes advantage from the doublet and stretching techniques classically used to monitor weak velocity variation from coda waves. We apply IPV to data acquired in Northern America (Canada) on a 1-km side square seismic network laid out by 397 stations. Data used to study temporal variations are cross-correlated signals computed on 10-minutes ambient noise in the frequency band 2-5 Hz. As the data set was acquired over five days, about 660 files are processed to perform a complete temporal analysis for each stations pair. The IPV permits to estimate the phase shift all over the signal length without any assumption on the medium velocity. The instantaneous phase is computed using the Hilbert transform of the signal. For each stations pair, we measure the phase difference between successive correlation functions calculated for 10 minutes of ambient noise. We then fit the instantaneous phase shift using a first-order polynomial function. The measure of the velocity variation corresponds to the slope of this fit. Compared to other techniques, the advantage of IPV is a very fast procedure which efficiently provides the measure of velocity variation on large data sets. Both experimental results and numerical tests on synthetic signals will be presented to assess the reliability of the IPV technique, with comparison to the doublet and stretching methods.

Fast ferroelectric phase shifters for energy recovery linacs

DOE PAGES

Kazakov, S. Yu; Shchelkunov, S. V.; Yakovlev, V. P.; ...

2010-11-24

Fast phase shifters are described that use a novel barium strontium titanate ceramic that can rapidly change its dielectric constant as an external bias voltage is changed. These phase shifters promise to reduce by ~10 times the power requirements for the rf source needed to drive an energy recovery linac (ERL). Such phase shifters will be coupled with superconducting radiofrequency cavities so as to tune them to compensate for phase instabilities, whether beam-driven or those caused by microphonics. The most promising design is presented, which was successfully cold tested and demonstrated a switching speed of ~30 ns for 77 deg, correspondingmore » to < 0.5 ns per deg of rf phase. As a result, other crucial issues (losses, phase shift values, etc.) are discussed.« less

Solvent Extraction of Furfural From Biomass

NASA Technical Reports Server (NTRS)

Humphrey, M. F.

1984-01-01

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

Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples.

PubMed

Gerace, E; Salomone, A; Abbadessa, G; Racca, S; Vincenti, M

2012-02-01

A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid-liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration.

Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples

PubMed Central

Gerace, E.; Salomone, A.; Abbadessa, G.; Racca, S.; Vincenti, M.

2011-01-01

A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid–liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration. PMID:29403714

Changes Caused by Fruit Extracts in the Lipid Phase of Biological and Model Membranes

PubMed Central

Pruchnik, Hanna; Oszmiański, Jan; Sarapuk, Janusz; Kleszczyńska, Halina

2010-01-01

The aim of the study was to determine changes incurred by polyphenolic compounds from selected fruits in the lipid phase of the erythrocyte membrane, in liposomes formed of erythrocyte lipids and phosphatidylcholine liposomes. In particular, the effect of extracts from apple, chokeberry, and strawberry on the red blood cell morphology, on packing order in the lipid hydrophilic phase, on fluidity of the hydrophobic phase, as well as on the temperature of phase transition in DPPC liposomes was studied. In the erythrocyte population, the proportions of echinocytes increased due to incorporation of polyphenolic compounds. Fluorimetry with a laurdan probe indicated increased packing density in the hydrophilic phase of the membrane in presence of polyphenolic extracts, the highest effect being observed for the apple extract. Using the fluorescence probes DPH and TMA-DPH, no effect was noted inside the hydrophobic phase of the membrane, as the lipid bilayer fluidity was not modified. The polyphenolic extracts slightly lowered the phase transition temperature of phosphatidylcholine liposomes. The studies have shown that the phenolic compounds contained in the extracts incorporate into the outer region of the erythrocyte membrane, affecting its shape and lipid packing order, which is reflected in the increasing number of echinocytes. The compounds also penetrate the outer part of the external lipid layer of liposomes formed of natural and DPPC lipids, changing its packing order. PMID:21423329

Qualitative screening of veterinary anti-microbial agents in tissues, milk, and eggs of food-producing animals using liquid chromatography coupled with tandem mass spectrometry.

PubMed

Chen, Dongmei; Yu, Jie; Tao, Yanfei; Pan, Yuanhu; Xie, Shuyu; Huang, Lingli; Peng, Dapeng; Wang, Xu; Wang, Yulian; Liu, Zhenli; Yuan, Zonghui

2016-04-01

A method for the analysis of 120 drugs in animal derived food was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). These analytes belong to 12 families of veterinary anti-microbial agents (quinolones, macrolides, β-lactams, nitroimidazoles, sulfonamides, lincomycines, chloramphenicols, quinoxalines, tetracyclines, polypeptides, and antibacterial synergists) as well as other compounds not assigned to a particular drug family. The animal derived food samples include muscle and liver of swine, bovine, sheep, and chicken, as well as hen eggs and dairy milk. The sample preparation included ultrasound-assisted extraction (UAE) with acetonitrile-water and a final clean-up with auto solid-phase extraction (SPE) on HLB cartridges. The detection and quantification of 120 anti-microbial agents was performed using LC-MS/MS in positive and negative ion mode. The chromatographic separation was performed on a C18 column using acetonitrile and 0.1% formic acid as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) of all drugs in food-producing animals were 0.5-3.0μg/kg and 1.5-10.0μg/kg, respectively. The developed method was successfully utilized to monitor real samples, which demonstrated that it is a simple, fast, and robust method, and could be used as a regulatory to screen for the presence of residues from veterinary anti-microbial drugs in animal-derived foods. Copyright © 2016 Elsevier B.V. All rights reserved.

Fast arsenic speciation in water by on-site solid phase extraction and high-resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Mihucz, Victor G.; Bencs, László; Koncz, Kornél; Tatár, Enikő; Weiszburg, Tamás; Záray, Gyula

2017-02-01

A method of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS), combined with on-site separation/solid phase extraction (SPE) has been developed for the speciation of inorganic As (iAs) in geothermal and drinking water samples. The HR-CS-GFAAS calibration curves were linear up to 200 μg/L As, but using second order polynomial fitting, accurate calibration could be performed up to 500 μg/L. It has been demonstrated that sample pH should not be higher than 8 for an accurate speciation of As(V) with a recovery of ≈ 95%. Geothermal water had fairly high salt content (≈ 2200 mg/L) due to the presence of chlorides and sulfates at mg/L levels. Therefore, a two-fold dilution of these types of samples before SPE is recommended, especially, for total As determinations, when the As concentration is as high as 400 μg/L. For drinking water, sampled from public wells with records of As concentrations higher than the 10 μg/L in the past, the reduction of As contamination below the WHO's health limit value could be observed. However, the electrical conductivity was close to 2500 μS/cm, i.e., the guideline limit for drinking water, which was due to their higher chloride content. The proposed fit-for-purpose SPE-HR-CS-GFAAS method could be a candidate for screening drinking water quality.

Bioanalytical LC-MS/MS method validation for plasma determination of topiramate in healthy Indian volunteers.

PubMed

Goswami, Dipanjan; Kumar, Ajay; Khuroo, Arshad H; Monif, Tausif; Rab, Shamsur

2009-11-01

A LC-MS/MS method for plasma topiramate analysis is delineated involving least number of healthy volunteers. Topiramate and amlodipine internal standard (IS) were extracted by simple centrifuge-coupled solid-phase extraction and reverse-phase chromatographic separation was performed on an Ascentis C(18) column. Turbo-spray negative-ion mode multiple-reaction monitoring was selected for mass pair detection at m/z 338.3 --> 78.0 and m/z 407.3 --> 295.5 for analyte and IS respectively. The method showed a dynamic linearity range from 10.4 to 2045.0 ng/mL, lower limit of quantitation achieved at 10.4 ng/mL and finally a mass spectrometric total run time of within 2.5 min for human sample analysis. Bioequivalence was assessed successfully using this fully validated method on 16 fasted Indian male subjects with 25 mg topiramate tablet administration. An appropriate study design describes plasma samples collection up to 216 h post dose in two periods, separated by a 28 day washout period. The challenge of half-life matching for test and reference drug was achieved with 73.43 +/- 9.68 and 73.06 +/- 14.03 h, respectively, and intra-subject coefficient of variation achieved within 11% for AUCs and C(max) evaluated by non-compartmental pharmacokinetic analysis. The results of LCMS topiramate complete method validation supported by pharmacokinetic study have not been published before, and are presented and discussed for the first time in this article. Copyright (c) 2009 John Wiley & Sons, Ltd.

Functionalized metal-organic framework nanocomposites for dispersive solid phase extraction and enantioselective capture of chiral drug intermediates.

PubMed

Ma, Xue; Zhou, Xiaohua; Yu, Ajuan; Zhao, Wuduo; Zhang, Wenfen; Zhang, Shusheng; Wei, Linlin; Cook, Debra J; Roy, Anirban

2018-02-16

The facile preparation, characterization and application of a novel magnetic graphene oxide- metal organic framework [Zn 2 (d-Cam) 2 (4, 4'-bpy)] n (MGO-ZnCB) as a sorbent for fast, simple and enantioselective capture of chiral drug intermediates are presented in this paper. The MGO-ZnCB nanocomposite, developed by encapsulating MGO nanoparticles into the homochiral metal organic framework of ZnCB, can integrate the advantages from each component endowing the hybrids with improved synergystic effects. The enantioselective performance of MGO-ZnCB was evaluated by dispersive magnetic nanoparticle solid phase extraction (d-MNSPE) of 1, 1'-bi-2-naphthol (BN) and 2, 2'-furoin (Furoin) racemic solutions. Due to the excellent dispersive capability, high stability, relatively larger saturation magnetization and distinct enrichment capacity of MGO-ZnCB, the d-MNSPE method provids good enantioselective separation of these compounds with enantiomeric excess (ee) values as high as 74.8% and 57.4%, respectively. The entire process with BN or Furoin can be completed within 3 min or less. After washing with methanol, the host MGO-ZnCB can be easily recycled and reused six times without any apparent loss of performance. Furthermore, the adsorbed BN and Furoin in nanodomains of the MGO-ZnCB composite were directly investigated for the first time by atomic force microscopy-infrared (AFM-IR) technique. Copyright © 2017 Elsevier B.V. All rights reserved.

pH-resistant titania hybrid organic-inorganic sol-gel coating for solid-phase microextraction of polar compounds.

PubMed

Li, Xiujuan; Gao, Jie; Zeng, Zhaorui

2007-05-02

A novel titania-hydroxy-terminated silicone oil (titania-OH-TSO) sol-gel coating was developed for solid-phase microextraction of polar compounds. In general, titania-based sol-gel reaction is very fast and need to be decelerated by the use of suitable chelating agents. But in the present work, a judiciously designed sol solution ingredients was used to create the titania-OH-TSO coating without the addition of any chelating agent, which simplified the sol-gel procedure. Thanks to the variety of titania's adsorption sites and their acid-base characteristics, aromatic amines, phenols and polycyclic aromatic hydrocarbons were efficiently extracted and preconcentrated from aqueous samples followed by thermal desorption and GC analysis. The newly developed sol-gel hybrid titania coating demonstrated excellent pH stability, and retained its extraction characteristics intact even after continuous rinsing with a 3 M HCl or NaOH solution for 12 h. Furthermore, it could withstand temperatures as high as 320 degrees C. Practical application was demonstrated through the analysis of six aromatic amines in dye process wastewater. A linearity of four orders of magnitude was obtained with correlation coefficient better than 0.9982. The detection limits ranged from 0.22 to 0.84 microg L(-1) and the repeatability of the measurements was <7.0%. The recoveries of these compounds studied in the wastewater were in the ranges 83.6-101.4%, indicating the method accuracy.

Identification of Marchfeld asparagus using Sr isotope ratio measurements by MC-ICP-MS.

PubMed

Swoboda, S; Brunner, M; Boulyga, S F; Galler, P; Horacek, M; Prohaska, T

2008-01-01

This work focuses on testing and application of Sr isotope signatures for the fast and reliable authentication and traceability of Asparagus officinalis originating from Marchfeld, Austria, using multicollector inductively coupled plasma mass spectrometry after optimised Rb/Sr separation. The major sample pool comprises freeze-dried and microwave-digested asparagus samples from Hungary and Slovakia which are compared with Austrian asparagus originating from the Marchfeld region, which is a protected geographical indication. Additional samples from Peru, The Netherlands and Germany were limited in number and allowed therefore only restricted statistical evaluation. Asparagus samples from Marchfeld were harvested within two subsequent years in order to investigate the annual variation. The results show that the Sr isotope ratio is consistent within these 2 years of investigation. Moreover, the Sr isotope ratio of total Sr in soil was found to be significantly higher than in an NH4NO3 extract, reflecting the mobile (bioavailable) phase. The isotope composition in the latter extract corresponds well to the range found in the asparagus samples in Marchfeld, even though the concentration of Sr in asparagus shows no direct correlation to the concentration of Sr in the mobile phase of the soil. The major question was whether the 'Marchfelder Spargel' can be distinguished from samples from the neighbouring countries of Hungary and Slovakia. According to our findings, they can be clearly (100%) singled out from the Hungarian samples and can be distinguished from the Slovakian asparagus samples with a probability of more than 80%.

Effects of Intermittent Fasting on Experimental Autoimune Encephalomyelitis in C57BL/6 Mice.

PubMed

Razeghi Jahromi, Soodeh; Ghaemi, Amir; Alizadeh, Akram; Sabetghadam, Fatemeh; Moradi Tabriz, Hedieh; Togha, Mansoureh

2016-06-01

Several religions recommend periods of fasting. One of the most frequently asked questions of MS patients before the holy month of Ramadan is weather fasting might have an unfavorable effect on their disease course. This debate became more challenging after the publication of experimental studies suggesting that calorie restriction prior to disease induction attenuates disease severity. We conducted this study to assess early and late effects of fasting on the animal model of MS, known as autoimmune encephalomyelitis. EAE was induced in the C57BL/6 mice, using Myelin Oligodendrocyte Glycopeptide  (MOG) 35-55 and they fasted every other day either after the appearance of the first clinical sign or 30 days after disease induction for ten days. Thereafter, the mice were sacrificed for further histological and immunological evaluations. Intermittent fasting after the establishment of EAE did not have any unfavorable effect on the course of disease. Moreover, fasting at the early phase of disease alleviated EAE severity by ameliorating spinal cord demyelination. Fasting suppressed the secretion of IFN-γ, TNF-α and raised IL-10 production in splenocytes. Fasting was also associated with a lower percent of cytotoxicity. Intermittent fasting not only had no unfavorable effect on EAE but also reduced EAE severity if started at early phase of disease.

Extraction equilibrium of indium(III) from nitric acid solutions by di(2-ethylhexyl)phosphoric acid dissolved in kerosene.

PubMed

Tsai, Hung-Sheng; Tsai, Teh-Hua

2012-01-04

The extraction equilibrium of indium(III) from a nitric acid solution using di(2-ethylhexyl) phosphoric acid (D2EHPA) as an acidic extractant of organophosphorus compounds dissolved in kerosene was studied. By graphical and numerical analysis, the compositions of indium-D2EHPA complexes in organic phase and stoichiometry of the extraction reaction were examined. Nitric acid solutions with various indium concentrations at 25 °C were used to obtain the equilibrium constant of InR₃ in the organic phase. The experimental results showed that the extraction distribution ratios of indium(III) between the organic phase and the aqueous solution increased when either the pH value of the aqueous solution and/or the concentration of the organic phase extractant increased. Finally, the recovery efficiency of indium(III) in nitric acid was measured.

Extraction of Oil from Flaxseed (Linum usitatissimum L.) Using Enzyme-Assisted Three-Phase Partitioning.

PubMed

Tan, Zhi-Jian; Yang, Zi-Zhen; Yi, Yong-Jian; Wang, Hong-Ying; Zhou, Wan-Lai; Li, Fen-Fang; Wang, Chao-Yun

2016-08-01

In this study, enzyme-assisted three-phase partitioning (EATPP) was used to extract oil from flaxseed. The whole procedure is composed of two parts: the enzymolysis procedure in which the flaxseed was hydrolyzed using an enzyme solution (the influencing parameters such as the type and concentration of enzyme, temperature, and pH were optimized) and three-phase partitioning (TPP), which was conducted by adding salt and t-butanol to the crude flaxseed slurry, resulting in the extraction of flaxseed oil into alcohol-rich upper phase. The concentration of t-butanol, concentration of salt, and the temperature were optimized to maximize the extraction yield. Under optimized conditions of a 49.29 % t-butanol concentration, 30.43 % ammonium sulfate concentration, and 35 °C extraction temperature, a maximum extraction yield of 71.68 % was obtained. This simple and effective EATPP can be used to achieve high extraction yields and oil quality, and thus, it is potential for large-scale oil production.

Structure of Bordetella pertussis peptidoglycan

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

Folkening, W.J.; Nogami, W.; Martin, S.A.

1987-09-01

Bordetella pertussis Tohama phases I and III were grown to the late-exponential phase in liquid medium containing (/sup 3/H)diaminopimelic acid and treated by a hot (96/sup 0/C) sodium dodecyl sulfate extraction procedure. Washed sodium dodecyl sulfate-insoluble residue from phases I and III consisted of complexes containing protein (ca. 40%) and peptidoglycan (60/sup 6/). Subsequent treatment with proteinase K yielded purified peptidoglycan which contained N-acetylglucosamine, N-acetylmuramic acid, alanine, glutamic acid, and diaminopimelic acid in molar ratios of 1:1:2:1:1 and <2% protein. Radiochemical analyses indicated that /sup 3/H added in diaminopimelic acid was present in peptidoglycan-protein complexes and purified peptidoglycan as diaminopimelicmore » acid exclusively and that pertussis peptidoglycan was not O acetylated, consistent with it being degraded completely by hen egg white lysozyme. Muramidase-derived disaccharide peptide monomers and peptide-cross-linked dimers and higher oligomers were isolated by molecular-sieve chromatography; from the distribution of these peptidoglycan fragments, the extent of peptide cross-linking of both phase I and III peptidoglycan was calculated to be ca. 48%. Unambiguous determination of the structure of muramidase-derived pepidoglycan fragments by fast atom bombardment-mass spectrometry and tandem mass spectrometry indicated that the pertussis peptidoglycan monomer fraction was surprisingly homogeneous, consisting of >95% N-acetylglucosaminyl-N-acetylmuramyl-alanyl-glutamyl-diaminopimelyl-alanine.« less

Primary and submovement control of aiming in C6 tetraplegics following posterior deltoid transfer

PubMed Central

2014-01-01

Background Upper limb motor control in fast, goal-directed aiming is altered in tetraplegics following posterior-deltoid musculotendinous transfer. Specifically, movements have similar end-point accuracy but longer duration and lower peak velocity than those of age-matched, neurotypical controls. Here, we examine in detail the interplay between primary movement and submovement phases in five C6 tetraplegic and five control participants. Methods Aiming movements were performed in two directions (20 cm away or toward), with or without vision. Trials that contained a submovement phase (i.e., discontinuity in velocity, acceleration or jerk) were identified. Discrete kinematic variables were then extracted on the primary and submovements phases. Results The presence of submovements did not differ between the tetraplegic (68%) and control (57%) groups, and almost all submovements resulted from acceleration and jerk discontinuities. Tetraplegics tended to make a smaller amplitude primary movement, which had lower peak velocity and greater spatial variability at peak velocity. This was followed by a larger amplitude and longer duration secondary submovement. Peak velocity of primary movement was not related to submovement incidence. Together, the primary and submovement phases of both groups were equally effective in reducing end-point error. Conclusions C6 tetraplegic participants exhibit some subtle differences in measures of motor behaviour compared to control participants, but importantly feedforward and feedback processes work effectively in combination to achieve accurate goal-directed aiming. PMID:25055852

Quantitative holographic interferometry applied to combustion and compressible flow research

NASA Astrophysics Data System (ADS)

Bryanston-Cross, Peter J.; Towers, D. P.

1993-03-01

The application of holographic interferometry to phase object analysis is described. Emphasis has been given to a method of extracting quantitative information automatically from the interferometric fringe data. To achieve this a carrier frequency has been added to the holographic data. This has made it possible, firstly to form a phase map using a fast Fourier transform (FFT) algorithm. Then to `solve,' or unwrap, this image to give a contiguous density map using a minimum weight spanning tree (MST) noise immune algorithm, known as fringe analysis (FRAN). Applications of this work to a burner flame and a compressible flow are presented. In both cases the spatial frequency of the fringes exceed the resolvable limit of conventional digital framestores. Therefore, a flatbed scanner with a resolution of 3200 X 2400 pixels has been used to produce very high resolution digital images from photographs. This approach has allowed the processing of data despite the presence of caustics, generated by strong thermal gradients at the edge of the combustion field. A similar example is presented from the analysis of a compressible transonic flow in the shock wave and trailing edge regions.

Separation and quantitation of debrisoquine and 4-hydroxydebrisoquine in human urine by capillary electrophoresis and high-performance liquid chromatography.

PubMed

Cifuentes, A; Valencia, J; Sanz, E; Sánchez, M J; Rodríguez-Delgado, M A

1997-08-22

A comparative study on the use of reversed-phase high-performance liquid chromatography (RP-HPLC) and capillary electrophoresis (CE) for the determination of debrisoquine (D) and its metabolite, 4-hydroxydebrisoquine (4-HD), in human urine is presented. Four different urine pre-treatments are compared for purification of samples prior to their injection in HPLC and CE. The use of a solid-phase extraction with a C18 cartridge provides the best results for the urine sample treatment, with good recoveries, i.e., 94.5% for D and 93.4% for 4-HD, and high reproducibility, i.e., R.S.D. N = 10 values of 1.7% and 1.2%, respectively. Under our separation conditions it is shown that CE is twice as fast and provides slightly better analysis time reproducibility than HPLC for this type of sample. Both the sensitivity and peak area reproducibility are better when HPLC is used. The two techniques show good agreement when employed for determination of phenotypes for hydroxylation, which seems to corroborate the usefulness of CE for this type of study.

Fast analysis of capsaicinoids in Naga Jolokia extracts (Capsicum chinense) by high-performance liquid chromatography using fused core columns.

PubMed

Stipcovich, Tea; Barbero, Gerardo F; Ferreiro-González, Marta; Palma, Miguel; Barroso, Carmelo G

2018-01-15

A rapid high-performance liquid chromatography method with a C18 reverse-phase fused-core column has been developed for the determination and quantification of the main capsaicinoids (nornordihydrocapsaicin, nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin and homodihydrocapsaicin) present in Naga Jolokia peppers. A fused-core Kinetex™ C18 column (50×2.1mm i.d.; 2.6μm) was used for the analysis. The chromatographic separation was obtained with a gradient method in which the mobile phase was water (0.1% acetic acid) as solvent A and acetonitrile (0.1% acetic acid) as solvent B. The separation of all compounds was achieved in less than 3min with a total analysis time (sample-to-sample) of 10min. The robustness of the method was evaluated. The method showed excellent repeatability and intermediate precision expressed as coefficient of variance of less than 2%. The developed method was employed for the quantification of the major capsaicinoids present in different peppers and commercial products containing chilli peppers. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optical Fluoride Sensor Based on Monomer-Dimer Equilibrium of Scandium(III)-Octaethylporphyrin in a Plasticized Polymeric Film

PubMed Central

Kang, Youngjea; Kampf, Jeff W.; Meyerhoff, Mark E.

2007-01-01

A fluoride-selective optical sensor based on scandium(III) octaethylporphyrin (Sc(III)OEP) as an ionophore within a plasticized PVC film is described. The presence of fluoride ion in the aqueous sample phase increases the formation of a difluoro-bridged Sc(III)OEP dimer species in the polymer film. The ability of the Sc(III) porphyrin to form the dimeric structure in the presence of fluoride is confirmed by UV-Vis spectroscopy and X-ray crystallography. For more practical sensing applications, a pH chromoionophore (ETH 7075) is added to the plasticized PVC film along with Sc(III)OEP and the observed optical response is based on co-extraction of protons with sample phase fluoride to create the dimeric porphyrin and a protonated chromoionophore species. The selectivity pattern observed is F-≫ClO4-, SCN-, NO3->Br-, Cl-. Only organic salicylate is a significant interferent. Fast and reversible fluoride response is observed over the range of 10-4 ~10-2 M fluoride, allowing use of the sensing film in a waveguide configuration for flow-injection measurements. PMID:17719905

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improvement of Insulin Secretion and Pancreatic β-cell Function in Streptozotocin-induced Diabetic Rats Treated with Aloe vera Extract

PubMed Central

Noor, Ayesha; Gunasekaran, S.; Vijayalakshmi, M. A.

2017-01-01

Background: Diabetes mellitus is a metabolic disorder characterized by chronic hyperglycemia. Plant extracts and their products are being used as an alternative system of medicine for the treatment of diabetes. Aloe vera has been traditionally used to treat several diseases and it exhibits antioxidant, anti-inflammatory, and wound-healing effects. Streptozotocin (STZ)-induced Wistar diabetic rats were used in this study to understand the potential protective effect of A. vera extract on the pancreatic islets. Objective: The aim of the present study was to evaluate the A. vera extract on improvement of insulin secretion and pancreatic β-cell function by morphometric analysis of pancreatic islets in STZ-induced diabetic Wistar rats. Materials and Methods: After acclimatization, male Wistar rats, maintained as per the Committee for the Purpose of Control and Supervision of Experiments on Animals guidelines, were randomly divided into four groups of six rats each. Fasting plasma glucose and insulin levels were assessed. The effect of A. vera extract in STZ-induced diabetic rats on the pancreatic islets by morphometric analysis was evaluated. Results: Oral administration of A. vera extract (300 mg/kg) daily to diabetic rats for 3 weeks showed restoration of blood glucose levels to normal levels with a concomitant increase in insulin levels upon feeding with A. vera extract in STZ-induced diabetic rats. Morphometric analysis of pancreatic sections revealed quantitative and qualitative gain in terms of number, diameter, volume, and area of the pancreatic islets of diabetic rats treated with A. vera extract when compared to the untreated diabetic rats. Conclusion: A. vera extract exerts antidiabetic effects by improving insulin secretion and pancreatic β-cell function by restoring pancreatic islet mass in STZ-induced diabetic Wistar rats. SUMMARY Fasting plasma glucose (FPG) and insulin levels were restored to normal levels in diabetic rats treated with Aloe vera extractIslets of pancreas were qualitatively and quantitatively restored to normalcy leading to restoration of FPG and insulin levels of diabetic rats treated with Aloe vera extractMorphometric analysis of pancreatic sections revealed quantitative and qualitative gain in terms of number, diameter, volume, and area of the pancreatic islets of diabetic rats treated with Aloe vera extract when compared to the untreated diabetic rats. Abbreviations Used: A. vera, FPG: Fasting plasma glucose, STZ: Streptozotocin, BW: Body weight PMID:29333050

Fast correction approach for wavefront sensorless adaptive optics based on a linear phase diversity technique.

PubMed

Yue, Dan; Nie, Haitao; Li, Ye; Ying, Changsheng

2018-03-01

Wavefront sensorless (WFSless) adaptive optics (AO) systems have been widely studied in recent years. To reach optimum results, such systems require an efficient correction method. This paper presents a fast wavefront correction approach for a WFSless AO system mainly based on the linear phase diversity (PD) technique. The fast closed-loop control algorithm is set up based on the linear relationship between the drive voltage of the deformable mirror (DM) and the far-field images of the system, which is obtained through the linear PD algorithm combined with the influence function of the DM. A large number of phase screens under different turbulence strengths are simulated to test the performance of the proposed method. The numerical simulation results show that the method has fast convergence rate and strong correction ability, a few correction times can achieve good correction results, and can effectively improve the imaging quality of the system while needing fewer measurements of CCD data.

Observation of a Rare Earth Ion–Extractant Complex Arrested at the Oil–Water Interface During Solvent Extraction

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

Bu, Wei; Yu, Hao; Luo, Guangming

2014-09-11

Selective extraction of metal ions from a complex aqueous mixture into an organic phase is used to separate toxic or radioactive metals from polluted environments and nuclear waste, as well as to produce industrially relevant metals, such as rare earth ions. Selectivity arises from the choice of an extractant amphiphile, dissolved in the organic phase, which interacts preferentially with the target metal ion. The extractant-mediated process of ion transport from an aqueous to an organic phase takes place at the aqueous–organic interface; nevertheless, little is known about the molecular mechanism of this process despite its importance. Although state-of-the-art X-ray scatteringmore » is uniquely capable of probing molecular ordering at a liquid–liquid interface with subnanometer spatial resolution, utilizing this capability to investigate interfacial dynamical processes of short temporal duration remains a challenge. We show that a temperature-driven adsorption transition can be used to turn the extraction on and off by controlling adsorption and desorption of extractants at the oil–water interface. Lowering the temperature through this transition immobilizes a supramolecular ion–extractant complex at the interface during the extraction of rare earth erbium ions. Under the conditions of these experiments, the ion–extractant complexes condense into a two-dimensional inverted bilayer, which is characterized on the molecular scale with synchrotron X-ray reflectivity and fluorescence measurements. Raising the temperature above the transition leads to Er ion extraction as a result of desorption of ion–extractant complexes from the interface into the bulk organic phase. XAFS measurements of the ion–extractant complexes in the bulk organic phase demonstrate that they are similar to the interfacial complexes.« less

Optimization of Ultrasonic-Assisted Aqueous Two-Phase Extraction of Phloridzin from Malus Micromalus Makino with Ethanol/Ammonia Sulfate System.

PubMed

Zhang, Zhen; Liu, Fang; He, Caian; Yu, Yueli; Wang, Min

2017-12-01

Application of an aqueous two-phase system (ATPS) coupled with ultrasonic technology for the extraction of phloridzin from Malus micromalus Makino was evaluated and optimized by response surface methodology (RSM). The ethanol/ammonium sulfate ATPS was selected for detailed investigation, including the phase diagram, effect of phase composition and extract conditions on the partition of phloridzin, and the recycling of ammonium sulfate. In addition, the evaluation of extraction efficiency and the identification of phloridzin were investigated. The optimal partition coefficient (6.55) and recovery (92.86%) of phloridzin were obtained in a system composed of 35% ethanol (w/w) and 16% (NH 4 ) 2 SO 4 (w/w), 51:1 liquid-to-solid ratio, and extraction temperature of 36 °C. Comparing with the traditional solvent extraction with respective 35% and 80% ethanol, ultrasonic-assisted aqueous two-phase extraction (UAATPE) strategy had significant advantages with lower ethanol consumption, less impurity of sugar and protein, and higher extracting efficiency of phloridzin. Our result indicated that UAATPE was a valuable method for the extraction and preliminary purification of phloridzin from the fruit of Malus micromalus Makino, which has great potential in the deep processing of Malus micromalus Makino industry to increase these fruits' additional value and drive the local economic development. © 2017 Institute of Food Technologists®.

Separation of chemical groups from bio-oil aqueous phase via sequential organic solvent extraction

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

Ren, Shoujie; Ye, Philip; Borole, Abhijeet P

Bio-oil aqueous phase contains a considerable amount of furans, alcohols, ketones, aldehydes and phenolics besides the major components of organic acids and anhydrosugars. The complexity of bio-oil aqueous phase limits its efficient utilization. To improve the efficiency of bio-oil biorefinery, this study focused on the separation of chemical groups from bio-oil aqueous phase via sequential organic solvent extractions. Due to their high recoverability and low solubility in water, four solvents (hexane, petroleum ether, chloroform, and ethyl acetate) with different polarities were evaluated, and the optimum process conditions for chemical extraction were determined. Chloroform had high extraction efficiency for furans, phenolics,more » and ketones. In addition to these chemical groups, ethyl acetate had high extraction efficiency for organic acids. The sequential extraction by using chloroform followed by ethyl acetate rendered that 62.2 wt.% of original furans, ketones, alcohols, and phenolics were extracted to chloroform, over 62 wt.% acetic acid was extracted to ethyl acetate, resulting in a high concentration of levoglucosan (~53.0 wt.%) in the final aqueous phase. Chemicals separated via the sequential extraction could be used as feedstocks in biorefinery using processes such as catalytic upgrading of furans and phenolics to hydrocarbons, fermentation of levoglucosan to produce alcohols and diols, and hydrogen production from organic acids via microbial electrolysis.« less

Separation of chemical groups from bio-oil aqueous phase via sequential organic solvent extraction

DOE PAGES

Ren, Shoujie; Ye, Philip; Borole, Abhijeet P

2017-01-05

Bio-oil aqueous phase contains a considerable amount of furans, alcohols, ketones, aldehydes and phenolics besides the major components of organic acids and anhydrosugars. The complexity of bio-oil aqueous phase limits its efficient utilization. To improve the efficiency of bio-oil biorefinery, this study focused on the separation of chemical groups from bio-oil aqueous phase via sequential organic solvent extractions. Due to their high recoverability and low solubility in water, four solvents (hexane, petroleum ether, chloroform, and ethyl acetate) with different polarities were evaluated, and the optimum process conditions for chemical extraction were determined. Chloroform had high extraction efficiency for furans, phenolics,more » and ketones. In addition to these chemical groups, ethyl acetate had high extraction efficiency for organic acids. The sequential extraction by using chloroform followed by ethyl acetate rendered that 62.2 wt.% of original furans, ketones, alcohols, and phenolics were extracted to chloroform, over 62 wt.% acetic acid was extracted to ethyl acetate, resulting in a high concentration of levoglucosan (~53.0 wt.%) in the final aqueous phase. Chemicals separated via the sequential extraction could be used as feedstocks in biorefinery using processes such as catalytic upgrading of furans and phenolics to hydrocarbons, fermentation of levoglucosan to produce alcohols and diols, and hydrogen production from organic acids via microbial electrolysis.« less

Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

PubMed

Teixeira, Leonel Silva; Vieira, Heulla Pereira; Windmöller, Cláudia Carvalhinho; Nascentes, Clésia Cristina

2014-02-01

A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants. © 2013 Published by Elsevier B.V.

Phase-space dependent critical gradient behavior of fast-ion transport due to Alfvén eigenmodes

DOE PAGES

Collins, C. S.; Heidbrink, W. W.; Podestà, M.; ...

2017-06-09

Experiments in the DIII-D tokamak show that many overlapping small-amplitude Alfv en eigenmodes (AEs) cause fast-ion transport to sharply increase above a critical threshold, leading to fast-ion density profile resilience and reduced fusion performance. The threshold is above the AE linear stability limit and varies between diagnostics that are sensitive to different parts of fast-ion phase-space. A comparison with theoretical analysis using the nova and orbit codes shows that, for the neutral particle diagnostic, the threshold corresponds to the onset of stochastic particle orbits due to wave-particle resonances with AEs in the measured region of phase space. We manipulated themore » bulk fast-ion distribution and instability behavior through variations in beam deposition geometry, and no significant differences in the onset threshold outside of measurement uncertainties were found, in agreement with the theoretical stochastic threshold analysis. Simulations using the `kick model' produce beam ion density gradients consistent with the empirically measured radial critical gradient and highlight the importance of including the energy and pitch dependence of the fast-ion distribution function in critical gradient models. The addition of electron cyclotron heating changes the types of AEs present in the experiment, comparatively increasing the measured fast-ion density and radial gradient. Our studies provide the basis for understanding how to avoid AE transport that can undesirably redistribute current and cause fast-ion losses, and the measurements are being used to validate AE-induced transport models that use the critical gradient paradigm, giving greater confidence when applied to ITER.« less

Phase-space dependent critical gradient behavior of fast-ion transport due to Alfvén eigenmodes

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

Collins, C. S.; Heidbrink, W. W.; Podestà, M.

Experiments in the DIII-D tokamak show that many overlapping small-amplitude Alfv en eigenmodes (AEs) cause fast-ion transport to sharply increase above a critical threshold, leading to fast-ion density profile resilience and reduced fusion performance. The threshold is above the AE linear stability limit and varies between diagnostics that are sensitive to different parts of fast-ion phase-space. A comparison with theoretical analysis using the nova and orbit codes shows that, for the neutral particle diagnostic, the threshold corresponds to the onset of stochastic particle orbits due to wave-particle resonances with AEs in the measured region of phase space. We manipulated themore » bulk fast-ion distribution and instability behavior through variations in beam deposition geometry, and no significant differences in the onset threshold outside of measurement uncertainties were found, in agreement with the theoretical stochastic threshold analysis. Simulations using the `kick model' produce beam ion density gradients consistent with the empirically measured radial critical gradient and highlight the importance of including the energy and pitch dependence of the fast-ion distribution function in critical gradient models. The addition of electron cyclotron heating changes the types of AEs present in the experiment, comparatively increasing the measured fast-ion density and radial gradient. Our studies provide the basis for understanding how to avoid AE transport that can undesirably redistribute current and cause fast-ion losses, and the measurements are being used to validate AE-induced transport models that use the critical gradient paradigm, giving greater confidence when applied to ITER.« less

POLONIUM SEPARATION PROCESS

DOEpatents

Karraker, D.G.

1959-07-14

A liquid-liquid extraction process is presented for the recovery of polonium from lead and bismuth. According to the invention an acidic aqueous chloride phase containing the polonium, lead, and bismuth values is contacted with a tributyl phosphate ether phase. The polonium preferentially enters the organic phase which is then separated and washed with an aqueous hydrochloric solution to remove any lead or bismuth which may also have been extracted. The now highly purified polonium in the organic phase may be transferred to an aqueous solution by extraction with aqueous nitric acid.

Fast correspondences search in anatomical trees

NASA Astrophysics Data System (ADS)

dos Santos, Thiago R.; Gergel, Ingmar; Meinzer, Hans-Peter; Maier-Hein, Lena

2010-03-01

Registration of multiple medical images commonly comprises the steps feature extraction, correspondences search and transformation computation. In this paper, we present a new method for a fast and pose independent search of correspondences using as features anatomical trees such as the bronchial system in the lungs or the vessel system in the liver. Our approach scores the similarities between the trees' nodes (bifurcations) taking into account both, topological properties extracted from their graph representations and anatomical properties extracted from the trees themselves. The node assignment maximizes the global similarity (sum of the scores of each pair of assigned nodes), assuring that the matches are distributed throughout the trees. Furthermore, the proposed method is able to deal with distortions in the data, such as noise, motion, artifacts, and problems associated with the extraction method, such as missing or false branches. According to an evaluation on swine lung data sets, the method requires less than one second on average to compute the matching and yields a high rate of correct matches compared to state of the art work.

Fast modal extraction in NASTRAN via the FEER computer program. [based on automatic matrix reduction method for lower modes of structures with many degrees of freedom

NASA Technical Reports Server (NTRS)

Newman, M. B.; Pipano, A.

1973-01-01

A new eigensolution routine, FEER (Fast Eigensolution Extraction Routine), used in conjunction with NASTRAN at Israel Aircraft Industries is described. The FEER program is based on an automatic matrix reduction scheme whereby the lower modes of structures with many degrees of freedom can be accurately extracted from a tridiagonal eigenvalue problem whose size is of the same order of magnitude as the number of required modes. The process is effected without arbitrary lumping of masses at selected node points or selection of nodes to be retained in the analysis set. The results of computational efficiency studies are presented, showing major arithmetic operation counts and actual computer run times of FEER as compared to other methods of eigenvalue extraction, including those available in the NASTRAN READ module. It is concluded that the tridiagonal reduction method used in FEER would serve as a valuable addition to NASTRAN for highly increased efficiency in obtaining structural vibration modes.

Simultaneous fast scanning XRF, dark field, phase-, and absorption contrast tomography

NASA Astrophysics Data System (ADS)

Medjoubi, Kadda; Bonissent, Alain; Leclercq, Nicolas; Langlois, Florent; Mercère, Pascal; Somogyi, Andrea

2013-09-01

Scanning hard X-ray nanoprobe imaging provides a unique tool for probing specimens with high sensitivity and large penetration depth. Moreover, the combination of complementary techniques such as X-ray fluorescence, absorption, phase contrast and dark field imaging gives complete quantitative information on the sample structure, composition and chemistry. The multi-technique "FLYSCAN" data acquisition scheme developed at Synchrotron SOLEIL permits to perform fast continuous scanning imaging and as such makes scanning tomography techniques feasible in a time-frame well-adapted to typical user experiments. Here we present the recent results of simultaneous fast scanning multi-technique tomography performed at Soleil. This fast scanning scheme will be implemented at the Nanoscopium beamline for large field of view 2D and 3D multimodal imaging.

Purification of nattokinase by reverse micelles extraction from fermentation broth: effect of temperature and phase volume ratio.

PubMed

Liu, Jun-Guo; Xing, Jian-Min; Chang, Tian-Shi; Liu, Hui-Zhou

2006-03-01

Nattokinase is a novel fibrinolytic enzyme that is considered to be a promising agent for thrombosis therapy. In this study, reverse micelles extraction was applied to purify and concentrate nattokinase from fermentation broth. The effects of temperature and phase volume ratio used for the forward and backward extraction on the extraction process were examined. The optimal temperature for forward and backward extraction were 25 degrees C and 35 degrees C respectively. Nattokinase became more thermosensitive during reverse micelles extraction. And it could be enriched in the stripping phase eight times during backward extraction. It was found that nattokinase could be purified by AOT reverse micelles with up to 80% activity recovery and with a purification factor of 3.9.

Interpretation of fast-ion signals during beam modulation experiments

DOE PAGES

Heidbrink, W. W.; Collins, C. S.; Stagner, L.; ...

2016-07-22

Fast-ion signals produced by a modulated neutral beam are used to infer fast-ion transport. The measured quantity is the divergence of perturbed fast-ion flux from the phase-space volume measured by the diagnostic, ∇•more » $$\\bar{Γ}$$. Since velocity-space transport often contributes to this divergence, the phase-space sensitivity of the diagnostic (or “weight function”) plays a crucial role in the interpretation of the signal. The source and sink make major contributions to the signal but their effects are accurately modeled by calculations that employ an exponential decay term for the sink. Recommendations for optimal design of a fast-ion transport experiment are given, illustrated by results from DIII-D measurements of fast-ion transport by Alfv´en eigenmodes. Finally, the signal-to-noise ratio of the diagnostic, systematic uncertainties in the modeling of the source and sink, and the non-linearity of the perturbation all contribute to the error in ∇•$$\\bar{Γ}$$.« less

Probing Photoinduced Structural Phase Transitions by Fast or Ultra-Fast Time-Resolved X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Cailleau, Hervé Collet, Eric; Buron-Le Cointe, Marylise; Lemée-Cailleau, Marie-Hélène Koshihara, Shin-Ya

A new frontier in the field of structural science is the emergence of the fast and ultra-fast X-ray science. Recent developments in time-resolved X-ray diffraction promise direct access to the dynamics of electronic, atomic and molecular motions in condensed matter triggered by a pulsed laser irradiation, i.e. to record "molecular movies" during the transformation of matter initiated by light pulse. These laser pump and X-ray probe techniques now provide an outstanding opportunity for the direct observation of a photoinduced structural phase transition as it takes place. The use of X-ray short-pulse of about 100ps around third-generation synchrotron sources allows structural investigations of fast photoinduced processes. Other new X-ray sources, such as laser-produced plasma ones, generate ultra-short pulses down to 100 fs. This opens the way to femtosecond X-ray crystallography, but with rather low X-ray intensities and more limited experimental possibilities at present. However this new ultra-fast science rapidly progresses around these sources and new large-scale projects exist. It is the aim of this contribution to overview the state of art and the perspectives of fast and ultra-fast X-ray scattering techniques to study photoinduced phase transitions (here, the word ultra-fast is used for sub-picosecond time resolution). In particular we would like to largely present the contribution of crystallographic methods in comparison with optical methods, such as pump-probe reflectivity measurements, the reader being not necessary familiar with X-ray scattering. Thus we want to present which type of physical information can be obtained from the positions of the Bragg peaks, their intensity and their shape, as well as from the diffuse scattering beyond Bragg peaks. An important physical feature is to take into consideration the difference in nature between a photoinduced phase transition and conventional homogeneous photoinduced chemical or biochemical processes where molecules transform in an independent way each other. Actually the photoinduced phase transition with the establishment of the new electronic and structural oscopic order is preceded by precursor co-operative phenomena due to the formation of nano-scale correlated objects. These are the counterpart of pre-transitional fluctuations at thermal equilibrium which take place above the transition temperature (short range order preceding long range one). Moreover ultra-fast X-ray scattering will play a central role within the fascinating field of manipulating coherence, for instance to directly observe coherent atomic motions induced by a light pulse, such as optical phonons. In the first part of this contribution we present what experimental features are accessible by X-ray scattering to describe the physical picture for a photoinduced structural phase transition. The second part shows how a time-resolved X-ray scattering experiment can be performed with regards to the different pulsed X-ray sources. The first time-resolved X-ray diffraction experiments on photoinduced phase transitions are described and discussed in the third part. Finally some challenges for future are briefly indicated in the conclusion.

Cytotoxicity and apoptotic inducibility of Vitex agnus-castus fruit extract in cultured human normal and cancer cells and effect on growth.

PubMed

Ohyama, Kunio; Akaike, Takenori; Hirobe, Chieko; Yamakawa, Toshio

2003-01-01

A crude extract was prepared with ethanol from dried ripened Vitex agnus-castus fruits growing in Israel (Vitex extract). Cytotoxicity of the extract against human uterine cervical canal fibroblast (HCF), human embryo fibroblast (HE-21), ovarian cancer (MCF-7), cervical carcinoma (SKG-3a), breast carcinoma (SKOV-3), gastric signet ring carcinoma (KATO-III), colon carcinoma (COLO 201), and small cell lung carcinoma (Lu-134-A-H) cells was examined. After culture for 24 h (logarithmic growth phase) or 72 h (stationary growth phase), the cells were treated with various concentrations of Vitex extract. In both growth phases, higher growth activity of cells and more cytotoxic activity of Vitex extract were seen. The cytotoxic activity against stationary growth-phase cells was less than that against logarithmic growth-phase cells. DNA fragmentation of Vitex extract-treated cells was seen in SKOV-3, KATO-III, COLO 201, and Lu-134-A-H cells. The DNA fragmentation in Vitex extract-treated KATO-III cells was inhibited by the presence of the antioxidative reagent pyrrolidine dithiocarbamate or N-acetyl-L-cysteine (NAC). Western blotting analysis showed that in Vitex extract-treated KATO-III cells, the presence of NAC also inhibited the expression of heme oxygenase-1 and the active forms of caspases-3, -8 and -9. It is concluded that the cytotoxic activity of Vitex extract may be attributed to the effect on cell growth, that cell death occurs through apoptosis, and that this apoptotic cell death may be attributed to increased intracellular oxidation by Vitex extract treatment.

Extraction of steroidal glucosiduronic acids from aqueous solutions by anionic liquid ion-exchangers

PubMed Central

Mattox, Vernon R.; Litwiller, Robert D.; Goodrich, June E.

1972-01-01

A pilot study on the extraction of three steroidal glucosiduronic acids from water into organic solutions of liquid ion-exchangers is reported. A single extraction of a 0.5mm aqueous solution of either 11-deoxycorticosterone 21-glucosiduronic acid or cortisone 21-glucosiduronic acid with 0.1m-tetraheptylammonium chloride in chloroform took more than 99% of the conjugate into the organic phase; under the same conditions, the very polar conjugate, β-cortol 3-glucosiduronic acid, was extracted to the extent of 43%. The presence of a small amount of chloride, acetate, or sulphate ion in the aqueous phase inhibited extraction, but making the aqueous phase 4.0m with ammonium sulphate promoted extraction strongly. An increase in the concentration of ion-exchanger in the organic phase also promoted extraction. The amount of cortisone 21-glucosiduronic acid extracted by tetraheptylammonium chloride over the pH range of 3.9 to 10.7 was essentially constant. Chloroform solutions of a tertiary, a secondary, or a primary amine hydrochloride also will extract cortisone 21-glucosiduronic acid from water. The various liquid ion exchangers will extract steroidal glucosiduronic acid methyl esters from water into chloroform, although less completely than the corresponding free acids. The extraction of the glucosiduronic acids from water by tetraheptylammonium chloride occurs by an ion-exchange process; extraction of the esters does not involve ion exchange. PMID:5075264

A new license plate extraction framework based on fast mean shift

NASA Astrophysics Data System (ADS)

Pan, Luning; Li, Shuguang

2010-08-01

License plate extraction is considered to be the most crucial step of Automatic license plate recognition (ALPR) system. In this paper, a region-based license plate hybrid detection method is proposed to solve practical problems under complex background in which existing large quantity of disturbing information. In this method, coarse license plate location is carried out firstly to get the head part of a vehicle. Then a new Fast Mean Shift method based on random sampling of Kernel Density Estimate (KDE) is adopted to segment the color vehicle images, in order to get candidate license plate regions. The remarkable speed-up it brings makes Mean Shift segmentation more suitable for this application. Feature extraction and classification is used to accurately separate license plate from other candidate regions. At last, tilted license plate regulation is used for future recognition steps.

Automated Design Tools for Integrated Mixed-Signal Microsystems (NeoCAD)

DTIC Science & Technology

2005-02-01

method, Model Order Reduction (MOR) tools, system-level, mixed-signal circuit synthesis and optimization tools, and parsitic extraction tools. A unique...Mission Area: Command and Control mixed signal circuit simulation parasitic extraction time-domain simulation IC design flow model order reduction... Extraction 1.2 Overall Program Milestones CHAPTER 2 FAST TIME DOMAIN MIXED-SIGNAL CIRCUIT SIMULATION 2.1 HAARSPICE Algorithms 2.1.1 Mathematical Background

A rapid and reliable procedure for extraction of cellular polyamines and inorganic ions from plant tissues

Treesearch

Rakesh Minocha; Walter C. Shortle; Stephanie L. Long; Subhash C. Minocha

1994-01-01

A fast and reliable method for the extraction of cellular polyamines and major inorganic ions (Ca, Mg, Mn, K, and P) from several plant tissues is described. The method involves repeated freezing and thawing of samples instead of homogenization. The efficiency of extraction of both the polyamines and inorganic ions by these two methods was compared for 10 different...

Adiabatic description of long range frequency sweeping

NASA Astrophysics Data System (ADS)

Breizman, Boris; Nyqvist, Robert; Lilley, Matthew

2012-10-01

A theoretical framework is developed to describe long range frequency sweeping events in the 1D electrostatic bump-on-tail model with fast particle sources and collisions. The model includes three collision operators (Krook, drag (dynamical friction) and velocity space diffusion), and allows for a general shape of the fast particle distribution function. The behavior of phase space holes and clumps is analyzed, and the effect of particle trapping due to separatrix expansion is discussed. With a fast particle distribution function whose slope decays above the resonant phase velocity, hooked frequency sweeping is found for holes in the presence of drag collisions alone.

[Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

PubMed

Lü, Weichao; Shen, Shuchang; Wang, Chao

2017-11-08

With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy.

PubMed

Kazemi, Elahe; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

2016-01-28

This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4-60.0 μg L(-1), a detection limit of 0.21 μg L(-1), an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L(-1) level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05-300 μg L(-1), a detection limit of 0.016 μg L(-1) and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L(-1) level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Chemical composition of Juniperus communis L. fruits supercritical CO2 extracts: dependence on pressure and extraction time.

PubMed

Barjaktarović, Branislava; Sovilj, Milan; Knez, Zeljko

2005-04-06

Ground fruits of the common juniper (Juniperus communis L.), with a particle size range from 0.250-0.400 mm, forming a bed of around 20.00 +/- 0.05 g, were extracted with supercritical CO(2) at pressures of 80, 90, and 100 bars and at a temperature of 40 degrees C. The total amount of extractable substances or global yield (mass of extract/mass of raw material) for the supercritical fluid extraction process varied from 0.65 to 4.00% (wt). At each investigated pressure, supercritical CO(2) extract fractions collected in successive time intervals over the course of the extraction were analyzed by capillary gas chromatography, using flame ionization (GC-FID) and mass spectrometric detection (GC-MS). More than 200 constituents were detected in the extracts, and the contents of 50 compounds were reported in the work. Dependence of the percentage yields of monoterpene, sesquiterpene, oxygenated monoterpene, and oxygenated sesquiterpene hydrocarbon groups on the extraction time was investigated, and conditions that favored the yielding of each terpene groups were emphasized. At all pressures, monoterpene hydrocarbons were almost completely extracted from the berries in the first 0.6 h. It was possible to extract oxygenated monoterpenes at 100 bar in 0.5 h and at 90 bar in 1.2 h. Contrary to that, during an extraction period of 4 h at 80 bar, it was possible to extract only 75% of the maximum yielded value of oxygenated monoterpene at 100 bar. Intensive extraction of sesquiterpenes could be by no means avoided at any pressure, but at the beginning of the process (the first 0.5 h) at 80 bar, they were extracted about 8 and 3 times slower than at 100 and 90 bar, respectively. Oxygenated sesquiterpenes were yielded at fast, constant extraction rates at 100 and 90 bar in 1.2 and 3 h, respectively. This initial fast extraction period was consequently followed by much slower extraction of oxygenated sesquiterpenes.