Membrane assisted solvent extraction for rare earth element recovery

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

Bhave, Ramesh R.; Kim, Daejin; Peterson, Eric S.

Systems and methods for the recovery of rare earth elements are provided. The systems and methods generally include membrane assisted solvent extraction using permeable hollow fibers having an immobilized organic phase within the pores of the hollow fibers. The permeable hollow fibers are generally in contact with an acidic aqueous feed on one side thereof and a strip solution on another side thereof. The systems and methods generally include the simultaneous extraction and stripping of rare earth elements as a continuous recovery process that is well suited for post-consumer products, end-of-life products, and other recovery sources of rare earth elements.

Quantitative differential phase contrast imaging at high resolution with radially asymmetric illumination.

PubMed

Lin, Yu-Zi; Huang, Kuang-Yuh; Luo, Yuan

2018-06-15

Half-circle illumination-based differential phase contrast (DPC) microscopy has been utilized to recover phase images through a pair of images along multiple axes. Recently, the half-circle based DPC using 12-axis measurements significantly provides a circularly symmetric phase transfer function to improve accuracy for more stable phase recovery. Instead of using half-circle-based DPC, we propose a new scheme of DPC under radially asymmetric illumination to achieve circularly symmetric phase transfer function and enhance the accuracy of phase recovery in a more stable and efficient fashion. We present the design, implementation, and experimental image data demonstrating the ability of our method to obtain quantitative phase images of microspheres, as well as live fibroblast cell samples.

Comparative analysis of the alveolar macrophage proteome in ALI/ARDS patients between the exudative phase and recovery phase

PubMed Central

2013-01-01

Background Despite decades of extensive studies, the morbidity and mortality for acute lung injury/acute respiratory distress syndrome (ALI/ARDS) remained high. Particularly, biomarkers essential for its early diagnosis and prognosis are lacking. Methods Recent studies suggest that alveolar macrophages (AMs) at the exudative phase of ALI/ARDS initiate, amplify and perpetuate inflammatory responses, while they resolve inflammation in the recovery phase to prevent further tissue injury and perpetuated inflammation in the lung. Therefore, proteins relevant to this functional switch could be valuable biomarkers for ALI/ARDS diagnosis and prognosis. We thus conducted comparative analysis of the AM proteome to assess its dynamic proteomic changes during ALI/ARDS progression and recovery. Results 135 proteins were characterized to be differentially expressed between AMs at the exudative and recovery phase. MALDI-TOF-MS and peptide mass fingerprint (PMF) analysis characterized 27 informative proteins, in which 17 proteins were found with a marked increase at the recovery phase, while the rest of 10 proteins were manifested by the significantly higher levels of expression at the exudative phase. Conclusions Given the role of above identified proteins played in the regulation of inflammatory responses, cell skeleton organization, oxidative stress, apoptosis and metabolism, they have the potential to serve as biomarkers for early diagnosis and prognosis in the setting of patients with ALI/ARDS. PMID:23773529

In-depth analysis of the substorm recovery phase using electron and proton induced emissions from satellite observations

NASA Astrophysics Data System (ADS)

Bryant, Chad Richard

The aurora is a well known phenomenon in the night sky. The observer of the ground can only see part of what is truly happening. The active aurora observed from the ground relates in many cases to what is termed a magnetospheric substorm. Recent research has been involved in determining the cause of these events while other parts of the substorm have been little studied. While additional progress will be made through conventional analysis and observations of the substorm onset, new approaches are advantageous to clarify different aspects of magnetospheric substorms. Very little quantitative analysis has been completed on what is called the recovery phase. This dissertation represents an attempt to achieve the first in-depth quantitative study of the recovery phase. It will use conventional electron auroral observations as well as an exceptional new dataset courtesy of global images of proton aurora. To effectively exploit the observations, new analysis tools were developed to expand our understanding of the recovery phase. In this dissertation the use of the auroral substorm power was determined to be a good analytical method in working with magnetospheric substorms. The start and end of the recovery phase and the decay of the recovery phase were all analysed using this methodology. It was found that the decay of the recovery phase is exponential but can be interrupted by enhancements that are related to flows in the magnetotail and that the region from where the flow comes determines the optical signature that is seen in the ionosphere. An example shows how the unique proton dataset provides new possibilities for observations when compared to conventional electron auroral observations. All of these results provide valuable new insights into current magnetospheric substorm models.

Rotavirus-like particles primary recovery from insect cells in aqueous two-phase systems.

PubMed

Benavides, Jorge; Mena, Jimmy A; Cisneros-Ruiz, Mayra; Ramírez, Octavio T; Palomares, Laura A; Rito-Palomares, Marco

2006-09-14

Virus-like particles have a wide range of applications, including vaccination, gene therapy, and even as nanomaterials. Their successful utilization depends on the availability of selective and scalable methods of product recovery and purification that integrate effectively with upstream operations. In this work, a strategy based on aqueous two phase system (ATPS) was developed for the recovery of double-layered rotavirus-like particles (dlRLP) produced by the insect cell-baculovirus expression system. Polyethylene glycol (PEG) molecular mass, PEG and salt concentrations, and volume ratio (Vr, volume of top phase/volume of bottom phase) were evaluated in order to determine the conditions where dlRLP and contaminants concentrated to opposite phases. Two-stage ATPS consisting of PEG 400-phosphate with a Vr of 13.0 and a tie-line length (TLL) of 35% (w/w) at pH 7.0 provided the best conditions for processing highly concentrated crude extract from disrupted cells (dlRLP concentration of 5 microg/mL). In such conditions intracellular dlRLP accumulated in the top phase (recovery of 90%), whereas cell debris remained in the interface. Furthermore, dlRLP from culture supernatants accumulated preferentially in the interface (recovery of 82%) using ATPS with a Vr of 1.0, pH of 7.0, PEG 3350 (10.1%, w/w) and phosphate (10.9%, w/w). The purity of dlRLP from culture supernatant increased up to 55 times after ATPS. The use of ATPS resulted in a recovery process that produced dlRLP with a purity between 6 and 11% and an overall product yield of 85% (w/w), considering purification from intracellular and extracellular dlRLP. Overall, the strategy proposed in this study is simpler than traditional methods for recovering dlRLP, and represents a scalable and economically viable alternative for production processes of vaccines against rotavirus infection with significant scope for generic commercial application.

Single image super-resolution based on compressive sensing and improved TV minimization sparse recovery

NASA Astrophysics Data System (ADS)

Vishnukumar, S.; Wilscy, M.

2017-12-01

In this paper, we propose a single image Super-Resolution (SR) method based on Compressive Sensing (CS) and Improved Total Variation (TV) Minimization Sparse Recovery. In the CS framework, low-resolution (LR) image is treated as the compressed version of high-resolution (HR) image. Dictionary Training and Sparse Recovery are the two phases of the method. K-Singular Value Decomposition (K-SVD) method is used for dictionary training and the dictionary represents HR image patches in a sparse manner. Here, only the interpolated version of the LR image is used for training purpose and thereby the structural self similarity inherent in the LR image is exploited. In the sparse recovery phase the sparse representation coefficients with respect to the trained dictionary for LR image patches are derived using Improved TV Minimization method. HR image can be reconstructed by the linear combination of the dictionary and the sparse coefficients. The experimental results show that the proposed method gives better results quantitatively as well as qualitatively on both natural and remote sensing images. The reconstructed images have better visual quality since edges and other sharp details are preserved.

Modelling of Imbibition Phenomena in Fluid Flow through Heterogeneous Inclined Porous Media with different porous materials

NASA Astrophysics Data System (ADS)

Patel, Hardik S.; Meher, Ramakanta

2017-12-01

In this paper, the counter - current imbibition phenomenon is discussed in an inclined heterogeneous porous media with the consideration of two types of porous materials like volcanic sand and fine sand. Adomian decomposition method is applied to find the saturation of wetting phase and the recovery rate of the reservoir. Finally, a simulation result is developed to study the saturation of wetting phase and the optimum recovery rate of reservoir with the choices of some interesting parametric values. This problem has a great importance in the field of oil recovery process.

Development of a comprehensive screening method for more than 300 organic chemicals in water samples using a combination of solid-phase extraction and liquid chromatography-time-of-flight-mass spectrometry.

PubMed

Chau, Hong Thi Cam; Kadokami, Kiwao; Ifuku, Tomomi; Yoshida, Yusuke

2017-12-01

A comprehensive screening method for 311 organic compounds with a wide range of physicochemical properties (log Pow -2.2-8.53) in water samples was developed by combining solid-phase extraction with liquid chromatography-high-resolution time-of-flight mass spectrometry. Method optimization using 128 pesticides revealed that tandem extraction with styrene-divinylbenzene polymer and activated carbon solid-phase extraction cartridges at pH 7.0 was optimal. The developed screening method was able to extract 190 model compounds with average recovery of 80.8% and average relative standard deviations (RSD) of 13.5% from spiked reagent water at 0.20 μg L -1 , and 87.1% recovery and 10.8% RSD at 0.05 μg L -1 . Spike-recovery testing (0.20 μg L -1 ) using real sewage treatment plant effluents resulted in an average recovery and average RSD of 190 model compounds of 77.4 and 13.1%, respectively. The method was applied to the influent and effluent of five sewage treatment plants in Kitakyushu, Japan, with 29 out of 311 analytes being observed at least once. The results showed that this method can screen for a large number of chemicals with a wide range of physicochemical properties quickly and at low operational cost, something that is difficult to achieve using conventional analytical methods. This method will find utility in target screening of hazardous chemicals with a high risk in environmental waters, and for confirming the safety of water after environmental incidents.

Determination of bentazone, dichlorprop, and MCPA in different soils by sodium hydroxide extraction in combination with solid-phase preconcentration.

PubMed

Thorstensen, C W; Christiansen, A

2001-09-01

A method for the extraction of bentazone, dichlorprop, and MCPA in three selected Norwegian soils of different textures is described. Initially three different extraction methods were tested on one soil type. All methods gave recoveries >80% for the pesticide mixture, but extraction with sodium hydroxide in combination with solid-phase preconcentration was used for further recovery tests with soils of different properties spiked at four herbicide concentration levels (0.001-10 microg/g of wet soil). The method was rapid and easy and required a minimum of organic solvents. The recoveries were in the range of 82-109, 80-123, and 45-91% for the soils containing 1.4 (Hole), 2.5 (Kroer), and 37.8% (Froland) organic carbon, respectively. Limits of quantification using GC-MS were 0.0003 microg/g of wet soil for bentazone and 0.0001 microg/g of wet soil for both dichlorprop and MCPA.

Integration of Gas Enhanced Oil Recovery in Multiphase Fermentations for the Microbial Production of Fuels and Chemicals.

PubMed

Pedraza-de la Cuesta, Susana; Keijzers, Lore; van der Wielen, Luuk A M; Cuellar, Maria C

2018-04-01

In multiphase fermentations where the product forms a second liquid phase or where solvents are added for product extraction, turbulent conditions disperse the oil phase as droplets. Surface-active components (SACs) present in the fermentation broth can stabilize the product droplets thus forming an emulsion. Breaking this emulsion increases process complexity and consequently the production cost. In previous works, it has been proposed to promote demulsification of oil/supernatant emulsions in an off-line batch bubble column operating at low gas flow rate. The aim of this study is to test the performance of this recovery method integrated to a fermentation, allowing for continuous removal of the oil phase. A 500 mL bubble column is successfully integrated with a 2 L reactor during 24 h without affecting cell growth or cell viability. However, higher levels of surfactants and emulsion stability are measured in the integrated system compared to a base case, reducing its capacity for oil recovery. This is related to release of SACs due to cellular stress when circulating through the recovery column. Therefore, it is concluded that the gas bubble-induced oil recovery method allows for oil separation and cell recycling without compromising fermentation performance; however, tuning of the column parameters considering increased levels of SACs due to cellular stress is required for improving oil recovery. © 2018 The Authors. Biotechnology Journal Published by Wiley-VCHVerlag GmbH & Co. KGaA, Weinheim.

Recovery Of Chromium Metal (VI) Using Supported Liquid Membrane (SLM) Method, A study of Influence of NaCl and pH in Receiving Phase on Transport

NASA Astrophysics Data System (ADS)

Cholid Djunaidi, Muhammad; Lusiana, Retno A.; Rahayu, Maya D.

2017-06-01

Chromium metal(VI) is a valuable metal but in contrary has high toxicity, so the separation and recovery from waste are very important. One method that can be used for the separation and recovery of chromium (VI) is a Supported Liquid Membrane (SLM). SLM system contains of three main components: a supporting membrane, organic solvents and carrier compounds. The supported Membrane used in this research is Polytetrafluoroethylene (PTFE), organic solvent is kerosene, and the carrier compound used is aliquat 336. The supported liquid membrane is placed between two phases, namely, feed phase as the source of analyte (Cr(VI)) and the receiving phase as the result of separation. Feed phase is the electroplating waste which contains of chromium metal with pH variation about 4, 6 and 9. Whereas the receiving phase are the solution of HCl, NaOH, HCl-NaCl and NaOH-NaCl with pH variation about 1, 3, 5 and 7. The efficiency separation is determined by measurement of chromium in the feed and the receiving phase using AAS (Atomic Absorption Spectrophotometry). The experiment results show that transport of Chrom (VI) by Supported Liquid membrane (SLM) is influenced by pH solution in feed phase and receiving phase as well as NaCl in receiving phase. The highest chromium metal is transported from feed phase about 97,78%, whereas in receiving phase shows about 58,09%. The highest chromium metal transport happens on pH 6 in feed phase, pH 7 in receiving phase with the mixture of NaOH and NaCl using carrier compound aliquat 336.

[Optimization of solid-phase extraction for enrichment of toxic organic compounds in water samples].

PubMed

Zhang, Ming-quan; Li, Feng-min; Wu, Qian-yuan; Hu, Hong-ying

2013-05-01

A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.

Concentration of organic compounds in natural waters with solid-phase dispersion based on advesicle modified silica prior to liquid chromatography.

PubMed

Parisis, Nikolaos A; Giokas, Dimosthenis L; Vlessidis, Athanasios G; Evmiridis, Nicholaos P

2005-12-02

The ability of vesicle-coated silica to aid the extraction of organic compounds from water prior to liquid chromatographic analysis is presented for the first time. The method is based on the formation of silica supported cationic multi-lamellar vesicles of gemini surfactants inherently ensuring the presence of hydrophilic and hydrophobic sites for the partitioning of analytes bearing different properties. Method development is illustrated by studying the adsolubilization of UV absorbing chemicals from swimming pool water. Due to the requirement for external energy input (intense shearing) a method based on solid-phase dispersion (SPD) was applied producing better results than off-line solid-phase extraction (SPE). Meticulous investigation of the experimental parameters was conducted in order to elucidate the mechanisms behind the proposed extraction pattern. Analyte recoveries were quantitative under the optimum experimental conditions offering recoveries higher than 96% with RSD values below 5%.

Variable Structure Control of a Hand-Launched Glider

NASA Technical Reports Server (NTRS)

Anderson, Mark R.; Waszak, Martin R.

2005-01-01

Variable structure control system design methods are applied to the problem of aircraft spin recovery. A variable structure control law typically has two phases of operation. The reaching mode phase uses a nonlinear relay control strategy to drive the system trajectory to a pre-defined switching surface within the motion state space. The sliding mode phase involves motion along the surface as the system moves toward an equilibrium or critical point. Analysis results presented in this paper reveal that the conventional method for spin recovery can be interpreted as a variable structure controller with a switching surface defined at zero yaw rate. Application of Lyapunov stability methods show that deflecting the ailerons in the direction of the spin helps to insure that this switching surface is stable. Flight test results, obtained using an instrumented hand-launched glider, are used to verify stability of the reaching mode dynamics.

Hydraulic Failure Defines the Recovery and Point of Death in Water-Stressed Conifers[OA

PubMed Central

Brodribb, Tim J.; Cochard, Hervé

2009-01-01

This study combines existing hydraulic principles with recently developed methods for probing leaf hydraulic function to determine whether xylem physiology can explain the dynamic response of gas exchange both during drought and in the recovery phase after rewatering. Four conifer species from wet and dry forests were exposed to a range of water stresses by withholding water and then rewatering to observe the recovery process. During both phases midday transpiration and leaf water potential (Ψleaf) were monitored. Stomatal responses to Ψleaf were established for each species and these relationships used to evaluate whether the recovery of gas exchange after drought was limited by postembolism hydraulic repair in leaves. Furthermore, the timing of gas-exchange recovery was used to determine the maximum survivable water stress for each species and this index compared with data for both leaf and stem vulnerability to water-stress-induced dysfunction measured for each species. Recovery of gas exchange after water stress took between 1 and >100 d and during this period all species showed strong 1:1 conformity to a combined hydraulic-stomatal limitation model (r2 = 0.70 across all plants). Gas-exchange recovery time showed two distinct phases, a rapid overnight recovery in plants stressed to <50% loss of leaf hydraulic conductance (Kleaf) and a highly Ψleaf-dependent phase in plants stressed to >50% loss of Kleaf. Maximum recoverable water stress (Ψmin) corresponded to a 95% loss of Kleaf. Thus, we conclude that xylem hydraulics represents a direct limit to the drought tolerance of these conifer species. PMID:19011001

Hydraulic failure defines the recovery and point of death in water-stressed conifers.

PubMed

Brodribb, Tim J; Cochard, Hervé

2009-01-01

This study combines existing hydraulic principles with recently developed methods for probing leaf hydraulic function to determine whether xylem physiology can explain the dynamic response of gas exchange both during drought and in the recovery phase after rewatering. Four conifer species from wet and dry forests were exposed to a range of water stresses by withholding water and then rewatering to observe the recovery process. During both phases midday transpiration and leaf water potential (Psileaf) were monitored. Stomatal responses to Psileaf were established for each species and these relationships used to evaluate whether the recovery of gas exchange after drought was limited by postembolism hydraulic repair in leaves. Furthermore, the timing of gas-exchange recovery was used to determine the maximum survivable water stress for each species and this index compared with data for both leaf and stem vulnerability to water-stress-induced dysfunction measured for each species. Recovery of gas exchange after water stress took between 1 and >100 d and during this period all species showed strong 1:1 conformity to a combined hydraulic-stomatal limitation model (r2 = 0.70 across all plants). Gas-exchange recovery time showed two distinct phases, a rapid overnight recovery in plants stressed to <50% loss of leaf hydraulic conductance (Kleaf) and a highly Psileaf-dependent phase in plants stressed to >50% loss of Kleaf. Maximum recoverable water stress (Psimin) corresponded to a 95% loss of Kleaf. Thus, we conclude that xylem hydraulics represents a direct limit to the drought tolerance of these conifer species.

A Novel Aqueous Two Phase System Composed of Surfactant and Xylitol for the Purification of Lipase from Pumpkin (Cucurbita moschata) Seeds and Recycling of Phase Components.

PubMed

Amid, Mehrnoush; Manap, Mohd Yazid; Hussin, Muhaini; Mustafa, Shuhaimi

2015-06-17

Lipase is one of the more important enzymes used in various industries such as the food, detergent, pharmaceutical, textile, and pulp and paper sectors. A novel aqueous two-phase system composed of surfactant and xylitol was employed for the first time to purify lipase from Cucurbita moschata. The influence of different parameters such as type and concentration of surfactants, and the composition of the surfactant/xylitol mixtures on the partitioning behavior and recovery of lipase was investigated. Moreover, the effect of system pH and crude load on the degree of purification and yield of the purified lipase were studied. The results indicated that the lipase was partitioned into the top surfactant rich phase while the impurities partitioned into the bottom xylitol-rich phase using an aqueous two phase system composed of 24% (w/w) Triton X-100 and 20% (w/w) xylitol, at 56.2% of tie line length (TLL), (TTL is one of the important parameters in this study and it is determined from a bimodal curve in which the tie-line connects two nodes on the bimodal, that represent concentration of phase components in the top and bottom phases) and a crude load of 25% (w/w) at pH 8.0. Recovery and recycling of components was also measured in each successive step process. The enzyme was successfully recovered by the proposed method with a high purification factor of 16.4 and yield of 97.4% while over 97% of the phase components were also recovered and recycled. This study demonstrated that the proposed novel aqueous two phase system method is more efficient and economical than the traditional aqueous two phase system method for the purification and recovery of the valuable enzyme lipase.

A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extraction and gas chromatography-ion trap mass spectrometry

USGS Publications Warehouse

Hladik, M.L.; Smalling, K.L.; Kuivila, K.M.

2008-01-01

A method was developed for the analysis of over 60 pesticides and degradates in water by HLB solid-phase extraction and gas-chromatography/mass spectrometry. Method recoveries and detection limits were determined using two surface waters with different dissolved organic carbon (DOC) concentrations. In the lower DOC water, recoveries and detection limits were 80%-108% and 1-12 ng/L, respectively. In the higher DOC water, the detection limits were slightly higher (1-15 ng/L). Additionally, surface water samples from four sites were analyzed and 14 pesticides were detected with concentrations ranging from 4 to 1,200 ng/L. ?? 2008 Springer Science+Business Media, LLC.

pH Triggered Recovery and Reuse of Thiolated Poly(acrylic acid) Functionalized Gold Nanoparticles with Applications in Colloidal Catalysis.

PubMed

Ansar, Siyam M; Fellows, Benjamin; Mispireta, Patrick; Mefford, O Thompson; Kitchens, Christopher L

2017-08-08

Thiolated poly(acrylic acid) (PAA-SH) functionalized gold nanoparticles were explored as a colloidal catalyst with potential application as a recoverable catalyst where the PAA provides pH-responsive dispersibility and phase transfer capability between aqueous and organic media. This system demonstrates complete nanoparticle recovery and redispersion over multiple reaction cycles without changes in nanoparticle morphology or reduction in conversion. The catalytic activity (rate constant) was reduced in subsequent reactions when recovery by aggregation was employed, despite unobservable changes in morphology or dispersibility. When colloidal catalyst recovery employed a pH induced phase transfer between two immiscible solvents, the catalytic activity of the recovered nanoparticles was unchanged over four cycles, maintaining the original rate constant and 100% conversion. The ability to recover and reuse colloidal catalysts by aggregation/redispersion and phase transfer methods that occur at low and high pH, respectively, could be used for different gold nanoparticle catalyzed reactions that occur at different pH conditions.

Hydrometallurgical recovery of germanium from coal gasification fly ash: pilot plant scale evaluation

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

Arroyo, F.; Fernandez-Pereira, C.; Olivares, J.

2009-04-15

In this article, a hydrometallurgical method for the selective recovery of germanium from fly ash (FA) has been tested at pilot plant scale. The pilot plant flowsheet comprised a first stage of water leaching of FA, and a subsequent selective recovery of the germanium from the leachate by solvent extraction method. The solvent extraction method was based on Ge complexation with catechol in an aqueous solution followed by the extraction of the Ge-catechol complex (Ge(C{sub 6}H{sub 4}O{sub 2}){sub 3}{sup 2-}) with an extracting organic reagent (trioctylamine) diluted in an organic solvent (kerosene), followed by the subsequent stripping of the organicmore » extract. The process has been tested on a FA generated in an integrated gasification with combined cycle (IGCC) process. The paper describes the designed 5 kg/h pilot plant and the tests performed on it. Under the operational conditions tested, approximately 50% of germanium could be recovered from FA after a water extraction at room temperature. Regarding the solvent extraction method, the best operational conditions for obtaining a concentrated germanium-bearing solution practically free of impurities were as follows: extraction time equal to 20 min; aqueous phase/organic phase volumetric ratio equal to 5; stripping with 1 M NaOH, stripping time equal to 30 min, and stripping phase/organic phase volumetric ratio equal to 5. 95% of germanium were recovered from water leachates using those conditions.« less

A new phase correction method in NMR imaging based on autocorrelation and histogram analysis.

PubMed

Ahn, C B; Cho, Z H

1987-01-01

A new statistical approach to phase correction in NMR imaging is proposed. The proposed scheme consists of first-and zero-order phase corrections each by the inverse multiplication of estimated phase error. The first-order error is estimated by the phase of autocorrelation calculated from the complex valued phase distorted image while the zero-order correction factor is extracted from the histogram of phase distribution of the first-order corrected image. Since all the correction procedures are performed on the spatial domain after completion of data acquisition, no prior adjustments or additional measurements are required. The algorithm can be applicable to most of the phase-involved NMR imaging techniques including inversion recovery imaging, quadrature modulated imaging, spectroscopic imaging, and flow imaging, etc. Some experimental results with inversion recovery imaging as well as quadrature spectroscopic imaging are shown to demonstrate the usefulness of the algorithm.

METHOD OF SEPARATING URANIUM FROM ALLOYS

DOEpatents

Chiotti, P.; Shoemaker, H.E.

1960-06-28

Uranium can be recovered from metallic uraniumthorium mixtures containing uranium in comparatively small amounts. The method of recovery comprises adding a quantity of magnesium to a mass to obtain a content of from 48 to 85% by weight; melting and forming a magnesium-thorium alloy at a temperature of between 585 and 800 deg C; agitating the mixture, allowing the mixture to settle whereby two phases, a thorium-containing magnesium-rich liquid phase and a solid uranium-rich phase, are formed; and separating the two phases.

Use of incomplete energy recovery for the energy compression of large energy spread charged particle beams

DOEpatents

Douglas, David R [Newport News, VA; Benson, Stephen V [Yorktown, VA

2007-01-23

A method of energy recovery for RF-base linear charged particle accelerators that allows energy recovery without large relative momentum spread of the particle beam involving first accelerating a waveform particle beam having a crest and a centroid with an injection energy E.sub.o with the centroid of the particle beam at a phase offset f.sub.o from the crest of the accelerating waveform to an energy E.sub.full and then recovering the beam energy centroid a phase f.sub.o+Df relative to the crest of the waveform particle beam such that (E.sub.full-E.sub.o)(1+cos(f.sub.o+Df))>dE/2 wherein dE=the full energy spread, dE/2=the full energy half spread and Df=the wave form phase distance.

Determination of organochlorine pesticide and polychlorinated biphenyl residues in fatty fish by tandem solid-phase extraction cleanup.

PubMed

Schenck, F J; Calderon, L; Podhorniak, L V

1996-01-01

A rapid, multiresidue solid-phase extraction (SPE) technique for determination of organochlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish was modified for use with fatty fish. In the modified procedures, samples are extracted with acetonitrile, and the extract is cleaned up with both C18 and Florisil SPE columns. Residues are determined by gas chromatography with electron capture detection. The original method was modified for use with fatty fish by reducing the amount of tissue extracted and by using an improved Florisil SPE cleanup. Recovery data are presented for 24 fortified organochlorine pesticide residues (0.12 ppm) and 3 fortified PCB residues (0.80 ppm) from flounder, bluefish, and shad samples, which contained 0.8, 5.4, and 22.6% fat, respectively. For the 3 types of fish, recoveries of 23 of 24 fortified organochlorine pesticide residues ranged from 55 to 129%, and recoveries of 3 fortified PCB residues ranged from 55 to 104%. There were no significant differences in recovery based on fish species and/or fat content for the majority of residues studied. This SPE method and the official AOAC method yielded comparable results for fish containing incurred organochlorine residues.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by graphitized carbon-based solid-phase extraction and high-performance liquid chromatography/mass spectrometry

USGS Publications Warehouse

Furlong, Edward T.; Anderson, Bruce D.; Werner, Stephen L.; Soliven, Paul P.; Coffey, Laura J.; Burkhardt, Mark R.

2001-01-01

In 1996, the U.S. Geological Survey National Water Quality Laboratory (NWQL) developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method to determine polar pesticide concentrations in surface- and ground-water samples. Subsequently, the NWQL developed a complementary analysis that uses high-performance liquid chromatography/mass spectrometry to detect, identify, and quantify polar pesticides and pesticide metabolites in filtered water at concentrations as low as 10 nanograms per liter. This new method was designed to improve sensitivity and selectivity over the prior method, and to reduce known interferences from natural organic matter.In this new method, pesticides are extracted from filtered water samples by useing a 0.5-gram graphitized carbon-based solid-phase extraction cartridge, eluted from the cartridge, and concentrations determined by using high-performance liquid chromatography with electrospray ionization-mass spectrometry. The upper concentration limit is 1.000 microgram per liter (μg/L) for most compounds. Single-operator method detection limits in organic-free water samples fortified with pesticides at a concentration of 0.025 μg/L ranged from 0.0019 to 0.022 μg/L for all compounds in the method. The grand mean (mean of mean recoveries for individual compounds) recoveries in organic-free water samples ranged from 72 to 89 percent, fortified with pesticides at three concentrations between 0.025 and 0.5 μg/L. Grand mean recoveries in ground- and surface-water samples ranged from 46 to 119 percent, also fortified with pesticides at three concentrations between 0.025 and 0.5 μg/L. Long-term recoveries from reagent water spikes were used to demonstrate that 38 of 65 compounds can be reported without qualification of the quantitative result across the analytical range of the method. The remaining 27 are reported with qualified estimates of concentration because of greater variability of recovery.

Matrix solid-phase dispersion technique for the determination of a new antiallergic drug, bilastine, in rat faeces.

PubMed

Berrueta, L A; Fernández-Armentia, M; Bakkali, A; Gonzalo, A; Lucero, M L; Orjales, A

2001-08-25

A matrix solid-phase dispersion (MSPD) procedure for the isolation and HPLC determination of a new antiallergic agent, bilastine, in rat faeces is presented. The effect on recovery of empirical variables such as nature, pH and volume of the washing and elution liquids and nature of the adsorbent has been tested. The best recoveries were attained using an octadecylsilyl sorbent, 10 ml of a 0.1 M NaHCO3-Na2CO3 aqueous buffer of pH 10.0 as washing solvent and 10 ml of methanol as elution solvent. The extracts were evaporated to dryness and reconstituted in mobile phase before their injection into a HPLC system, equipped with a Discovery RP-amide C16 column and a fluorescence detector. The method allows one to reach recoveries of 95.0% within the concentration range 0.05-10 microg/g, with within-day repeatabilities of less than 5% and between-day repeatabilities of less than 9% within this range. This method has been successfully applied to the excretion studies of bilastine in the rat.

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

PubMed

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

2014-01-01

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

An Exploration on the Suitability of Airborne Carbonyl Compounds Analysis in relation to Differences in Instrumentation (GC-MS versus HPLC-UV) and Standard Phases (Gas versus Liquid)

PubMed Central

Kim, Ki-Hyun; Szulejko, Jan E.; Kim, Yong-Hyun; Lee, Min-Hee

2014-01-01

The relative performance figure of merits was investigated for the two most common analytical methods employed for carbonyl compounds (CC), for example, between high performance liquid chromatography (HPLC)-UV detector (with 2,4-dinitrophenylhydrazine (DNPH) derivatization) and thermal desorption (TD)-gas chromatography (GC)-mass spectrometry (MS) (without derivatization). To this end, the suitability of each method is assessed by computing the relative recovery (RR) between the gas- and liquid-phase standards containing a suite of CC such as formaldehyde (FA), acetaldehyde (AA), propionaldehyde (PA), butyraldehyde (BA), isovaleraldehyde (IA), and valeraldehyde (VA) along with benzene (B) as a recovery reference for the GC method. The results confirm that a TD-GC-MS is advantageous to attain the maximum recovery for the heavier CCs (i.e., with molecular weights (MW) above BA−MW ≥ 74). On the other hand, the HPLC-UV is favorable for the lighter CCs (like FA and AA) with the least bias. Such compound-specific responses for each platform are validated by relative ordering of CCs as a function of response factor (RF), method detection limit (MDL), and recovery pattern. It is thus desirable to understand the advantages and limitations of each method to attain the CC data with the least experimental bias. PMID:24719571

[A Simultaneous Determination Method with Acetonitrile-n-Hexane Partitioning and Solid-Phase Extraction for Pesticide Residues in Livestock and Marine Products by GC-MS].

PubMed

Yoshizaki, Mayuko; Kobayashi, Yukari; Shimizu, Masanori; Maruyama, Kouichi

2015-01-01

A simultaneous determination method was examined for 312 pesticides (including isomers) in muscle of livestock and marine products by GC-MS. The pesticide residues extracted from samples with acetone and n-hexane were purified by acetonitrile-n-hexane partitioning, and C18 and SAX/PSA solid-phase extraction without using GPC. Matrix components such as cholesterol were effectively removed. In recovery tests performed by this method using pork, beef, chicken and shrimp, 237-257 pesticides showed recoveries within the range of 70-120% in each sample. Validity was confirmed for 214 of the target pesticides by means of a validation test using pork. In comparison with the Japanese official method using GPC, the treatment time of samples and the quantity of solvent were reduced substantially.

Correlation between Cyclin Dependent Kinases and Artemisinin-Induced Dormancy in Plasmodium falciparum In Vitro

PubMed Central

Gray, Karen-Ann; Gresty, Karryn J.; Chen, Nanhua; Zhang, Veronica; Gutteridge, Clare E.; Peatey, Christopher L.; Chavchich, Marina; Waters, Norman C.; Cheng, Qin

2016-01-01

Background Artemisinin-induced dormancy provides a plausible explanation for recrudescence following artemisinin monotherapy. This phenomenon shares similarities with cell cycle arrest where cyclin dependent kinases (CDKs) and cyclins play an important role. Methods Transcription profiles of Plasmodium falciparum CDKs and cyclins before and after dihydroartemisinin (DHA) treatment in three parasite lines, and the effect of CDK inhibitors on parasite recovery from DHA-induced dormancy were investigated. Results After DHA treatment, parasites enter a dormancy phase followed by a recovery phase. During the dormancy phase parasites up-regulate pfcrk1, pfcrk4, pfcyc2 and pfcyc4, and down-regulate pfmrk, pfpk5, pfpk6, pfcrk3, pfcyc1 and pfcyc3. When entering the recovery phase parasites immediately up-regulate all CDK and cyclin genes. Three CDK inhibitors, olomoucine, WR636638 and roscovitine, produced distinct effects on different phases of DHA-induced dormancy, blocking parasites recovery. Conclusions The up-regulation of PfCRK1 and PfCRK4, and down regulation of other CDKs and cyclins correlate with parasite survival in the dormant state. Changes in CDK expression are likely to negatively regulate parasite progression from G1 to S phase. These findings provide new insights into the mechanism of artemisinin-induced dormancy and cell cycle regulation of P. falciparum, opening new opportunities for preventing recrudescence following artemisinin treatment. PMID:27326764

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

NASA Astrophysics Data System (ADS)

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

2016-06-01

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

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

NASA Astrophysics Data System (ADS)

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-12-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34-80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics.

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

PubMed Central

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-01-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34–80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics. PMID:28000704

Optimization of cloud point extraction and solid phase extraction methods for speciation of arsenic in natural water using multivariate technique.

PubMed

Baig, Jameel A; Kazi, Tasneem G; Shah, Abdul Q; Arain, Mohammad B; Afridi, Hassan I; Kandhro, Ghulam A; Khan, Sumaira

2009-09-28

The simple and rapid pre-concentration techniques viz. cloud point extraction (CPE) and solid phase extraction (SPE) were applied for the determination of As(3+) and total inorganic arsenic (iAs) in surface and ground water samples. The As(3+) was formed complex with ammonium pyrrolidinedithiocarbamate (APDC) and extracted by surfactant-rich phases in the non-ionic surfactant Triton X-114, after centrifugation the surfactant-rich phase was diluted with 0.1 mol L(-1) HNO(3) in methanol. While total iAs in water samples was adsorbed on titanium dioxide (TiO(2)); after centrifugation, the solid phase was prepared to be slurry for determination. The extracted As species were determined by electrothermal atomic absorption spectrometry. The multivariate strategy was applied to estimate the optimum values of experimental factors for the recovery of As(3+) and total iAs by CPE and SPE. The standard addition method was used to validate the optimized methods. The obtained result showed sufficient recoveries for As(3+) and iAs (>98.0%). The concentration factor in both cases was found to be 40.

General introduction and recovery factors

USGS Publications Warehouse

Verma, Mahendra K.

2017-07-17

IntroductionThe U.S. Geological Survey (USGS) compared methods for estimating an incremental recovery factor (RF) for the carbon dioxide enhanced oil recovery (CO2-EOR) process involving the injection of CO2 into oil reservoirs. This chapter first provides some basic information on the RF, including its dependence on various reservoir and operational parameters, and then discusses the three development phases of oil recovery—primary, second­ary, and tertiary (EOR). It ends with a brief discussion of the three approaches for estimating recovery factors, which are detailed in subsequent chapters.

A novel aqueous micellar two-phase system composed of surfactant and sorbitol for purification of pectinase enzyme from Psidium guajava and recycling phase components.

PubMed

Amid, Mehrnoush; Murshid, Fara Syazana; Manap, Mohd Yazid; Hussin, Muhaini

2015-01-01

A novel aqueous two-phase system composed of a surfactant and sorbitol was employed for the first time to purify pectinase from Psidium guajava. The influences of different parameters, including the type and concentration of the surfactant and the concentration and composition of the surfactant/sorbitol ratio, on the partitioning behavior and recovery of pectinase were investigated. Moreover, the effects of system pH and the crude load on purification fold and the yield of purified pectinase were studied. The experimental results indicated that the pectinase was partitioned into surfactant-rich top phase, and the impurities were partitioned into the sorbitol-rich bottom phase with the novel method involving an ATPS composed of 26% (w/w) Triton X-100 and 23% (w/w) sorbitol at 54.2% of the TLL crude load of 20% (w/w) at pH 6.0. The enzyme was successfully recovered by this method with a high purification factor of 15.2 and a yield of 98.3%, whereas the phase components were also recovered and recycled at rates above 96%. This study demonstrated that this novel ATPS method can be used as an efficient and economical alternative to the traditional ATPS for the purification and recovery of the valuable enzyme.

Remission and Recovery in the Treatment for Adolescents with Depression Study (TADS): Acute and Long-term Outcomes

PubMed Central

Kennard, Betsy D.; Silva, Susan G.; Tonev, Simon; Rohde, Paul; Hughes, Jennifer L.; Vitiello, Benedetto; Kratochvil, Christopher J.; Curry, John F.; Emslie, Graham J.; Reinecke, Mark; March, John

2010-01-01

Objective We examine remission rate probabilities, recovery rates, and residual symptoms across 36 weeks in the Treatment for Adolescents with Depression Study (TADS). Method TADS, a multisite clinical trial, randomized 439 adolescents with major depressive disorder (MDD) to 12 weeks of treatment to fluoxetine (FLX), cognitive behavioral therapy (CBT), their combination (COMB), or pill placebo (PBO). The PBO group, treated openly after week 12, was not included in the subsequent analyses. Treatment differences in remission rates and probabilities of remission over time are compared. Recovery rates in remitters at week 12 (acute phase remitters) and week 18 (continuation phase remitters) are summarized. We also examined whether residual symptoms at the end of 12 weeks of acute treatment predicted later remission. Results At Week 36, the estimated remission rates for intention-to-treat cases were: COMB: 60%, FLX: 55%; CBT: 64%; overall: 60%. Paired comparisons reveal that at week 24 all active treatments converge on remission outcomes. The recovery rate at Week 36 was 65% for acute phase remitters and 71% for continuation phase remitters, with no significant between-treatment differences in recovery rates. Residual symptoms at the end of acute treatment predicted failure to achieve remission at weeks 18 and 36. Conclusions The majority of depressed adolescents in all three treatment modalities achieved remission at the end of nine months of treatment. PMID:19127172

ENVIRONMENTALLY CONSCIOUS ELECTROCHEMICAL MACHINING FOR ZERO DISCHARGE AND METAL RECYCLING - PHASE I

EPA Science Inventory

Magnetic resonance separation imaging using a divided inversion recovery technique (DIRT).

PubMed

Goldfarb, James W

2010-04-01

The divided inversion recovery technique is an MRI separation method based on tissue T(1) relaxation differences. When tissue T(1) relaxation times are longer than the time between inversion pulses in a segmented inversion recovery pulse sequence, longitudinal magnetization does not pass through the null point. Prior to additional inversion pulses, longitudinal magnetization may have an opposite polarity. Spatial displacement of tissues in inversion recovery balanced steady-state free-precession imaging has been shown to be due to this magnetization phase change resulting from incomplete magnetization recovery. In this paper, it is shown how this phase change can be used to provide image separation. A pulse sequence parameter, the time between inversion pulses (T180), can be adjusted to provide water-fat or fluid separation. Example water-fat and fluid separation images of the head, heart, and abdomen are presented. The water-fat separation performance was investigated by comparing image intensities in short-axis divided inversion recovery technique images of the heart. Fat, blood, and fluid signal was suppressed to the background noise level. Additionally, the separation performance was not affected by main magnetic field inhomogeneities.

Automated product recovery in a HG-196 photochemical isotope separation process

DOEpatents

Grossman, Mark W.; Speer, Richard

1992-01-01

A method of removing deposited product from a photochemical reactor used in the enrichment of .sup.196 Hg has been developed and shown to be effective for rapid re-cycling of the reactor system. Unlike previous methods relatively low temperatures are used in a gas and vapor phase process of removal. Importantly, the recovery process is understood in a quantitative manner so that scaling design to larger capacity systems can be easily carried out.

Automated product recovery in a Hg-196 photochemical isotope separation process

DOEpatents

Grossman, M.W.; Speer, R.

1992-07-21

A method of removing deposited product from a photochemical reactor used in the enrichment of [sup 196]Hg has been developed and shown to be effective for rapid re-cycling of the reactor system. Unlike previous methods relatively low temperatures are used in a gas and vapor phase process of removal. Importantly, the recovery process is understood in a quantitative manner so that scaling design to larger capacity systems can be easily carried out. 2 figs.

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.

Method development for the analysis of N-nitrosodimethylamine and other N-nitrosamines in drinking water at low nanogram/liter concentrations using solid-phase extraction and gas chromatography with chemical ionization tandem mass spectrometry.

PubMed

Munch, Jean W; Bassett, Margarita V

2006-01-01

N-nitrosodimethylamine (NDMA) is a probable human carcinogen of concern that has been identified as a drinking water contaminant. U.S. Environmental Protection Agency Method 521 has been developed for the analysis of NDMA and 6 additional N-nitrosamines in drinking water at low ng/L concentrations. The method uses solid-phase extraction with coconut charcoal as the sorbent and dichloromethane as the eluent to concentrate 0.50 L water samples to 1 mL. The extracts are analyzed by gas chromatography-chemical ionization tandem mass spectrometry using large-volume injection. Method performance was evaluated in 2 laboratories. Typical analyte recoveries of 87-104% were demonstrated for fortified reagent water samples, and recoveries of 77-106% were demonstrated for fortified drinking water samples. All relative standard deviations on replicate analyses were < 11%.

An investigation of the thermal shock resistance of lunar regolith and the recovery of hydrogen from lunar soil heated using microwave radiation

NASA Technical Reports Server (NTRS)

Meek, T. T.

1991-01-01

The objective is to develop a better understanding of the thermal shock properties of lunar regolith sintered using 2.45 GHz electromagnetic radiation and to do a preliminary study into the recovery of bound hydrogen in lunar soil heated using 2.45 GHz radiation. During the first phase of this work, lunar simulant material was used to test whether or not microhardness data could be used to infer thermal shock resistance and later actual lunar regolith was used. Results are included on the lunar regolith since this is of primary concern and not the simulant results. They were similar, however. The second phase investigated the recovery of hydrogen from lunar regolith and results indicate that microwave heating of lunar regolith may be a good method for recovery of bound gases in the regolith.

Development and validation of an LC-UV method for the determination of sulfonamides in animal feeds.

PubMed

Kumar, P; Companyó, R

2012-05-01

A simple LC-UV method was developed for the determination of residues of eight sulfonamides (sulfachloropyridazine, sulfadiazine, sulfadimidine, sulfadoxine, sulfamethoxypyridazine, sulfaquinoxaline, sulfamethoxazole, and sulfadimethoxine) in six types of animal feed. C18, Oasis HLB, Plexa and Plexa PCX stationary phases were assessed for the clean-up step and the latter was chosen as it showed greater efficiency in the clean-up of interferences. Feed samples spiked with sulfonamides at 2 mg/kg were used to assess the trueness (recovery %) and precision of the method. Mean recovery values ranged from 47% to 66%, intra-day precision (RSD %) from 4% to 15% and inter-day precision (RSD %) from 7% to 18% in pig feed. Recoveries and intra-day precisions were also evaluated in rabbit, hen, cow, chicken and piglet feed matrices. Calibration curves with standards prepared in mobile phase and matrix-matched calibration curves were compared and the matrix effects were ascertained. The limits of detection and quantification in the feeds ranged from 74 to 265 µg/kg and from 265 to 868 µg/kg, respectively. Copyright © 2011 John Wiley & Sons, Ltd.

Evaluation of Lipid Profile Changes in Pediatric Patients with Acute Mononucleosis

PubMed Central

2017-01-01

Background Acute Epstein-Barr virus (EBV) infection could lead to atherogenic lipid profile changes in adults; while there is no evidence about the children with Infectious mononucleosis (IM). The aim of this study was to evaluate the lipid profile of the children in acute phase of mononucleosis and two months after the recovery. Materials and Methods From 2010 through 2012, 36 children with IM aged 1-10 years were enrolled in a prospective cross-sectional study. Fasting serum total cholesterol, high density lipoprotein (HDL), low density lipoprotein (LDL), and triglyceride level were measured during acute phase of the disease and after 2 months of the recovery. Results From 36 patients enrolled, 25 (69.4%) cases were male and the mean age of the patients was 4.1 ± 2.0 years. The mean of the total cholesterol level in the acute phase and 2 months after the recovery were149.5 ± 35.3 mg/dL and 145.7±30.6, respectively (P = 0.38). However, the serum level of HDL cholesterol in patients after 2 months of recovery was significantly increased (37.9 ± 9.3 mg/dL vs. 28.5 ± 10.6 mg/dL, P <0.001). The mean value of serum LDL cholesterol was significantly reduced, two months after recovery (81.4 ± 19.5 mg/dL, vs. 92.6 ± 28.8 mg/dL, P = 0.009). Furthermore, the serum triglyceride level was significantly reduced after the recovery (108.7 ± 36.9 mg/dL) compared with the acute phase (163.8 ± 114.3 mg/dL) (P = 0.004). Conclusion EBV infection in children could change lipid profile which is partially restored 2 months after the recovery. PMID:28332346

Determination of Bile Acids in Piglet Bile by Solid Phase Extraction and Liquid Chromatography-Electrospray Tandem Mass Spectrometry.

PubMed

Mi, Si; Lim, David W; Turner, Justine M; Wales, Paul W; Curtis, Jonathan M

2016-03-01

An LC/MS/MS-based method was developed for the determination of individual bile acids (BA) and their conjugates in porcine bile samples. The C18-based solid-phase extraction (SPE) procedure was optimized so that all 19 target BA and their glycine and taurine conjugates were collected with high recoveries for standards (89.1-100.2%). Following this, all 19 compounds were separated and quantified in a single 12 min chromatographic run. The method was validated in terms of linearity, sensitivity, accuracy, precision, and recovery. An LOD in the low ppb range with measured precisions in the range of 0.5-9.3% was achieved. The recoveries for all of the 19 analytes in bile samples were all >80%. The validated method was successfully applied to the profiling of BA and their conjugates in the bile from piglets treated with exogenous glucagon-like peptide-2 (GLP-2) in a preclinical model of neonatal parenteral nutrition-associated liver disease (PNALD). The method developed is rapid and could be easily implemented for routine analysis of BA and their conjugates in other biofluids or tissues.

Phase Recovery Acceleration of Quantum-Dot Semiconductor Optical Amplifiers by Optical Pumping to Quantum-Well Wetting Layer

NASA Astrophysics Data System (ADS)

Kim, Jungho

2013-11-01

We theoretically investigate the phase recovery acceleration of quantum-dot (QD) semiconductor optical amplifiers (SOAs) by means of the optical pump injection to the quantum-well (QW) wetting layer (WL). We compare the ultrafast gain and phase recovery responses of QD SOAs in either the electrical or the optical pumping scheme by numerically solving 1088 coupled rate equations. The ultrafast gain recovery responses on the order of sub-picosecond are nearly the same for the two pumping schemes. The ultrafast phase recovery is not significantly accelerated by increasing the electrical current density, but greatly improved by increasing the optical pumping power to the QW WL. Because the phase recovery time of QD SOAs with the optical pumping scheme can be reduced down to several picoseconds, the complete phase recovery can be achieved when consecutive pulse signals with a repetition rate of 100 GHz is injected.

Impact of CT attenuation correction method on quantitative respiratory-correlated (4D) PET/CT imaging

PubMed Central

Lee, Tzu-Cheng; Alessio, Adam M.; Wollenweber, Scott D.; Stearns, Charles W.; Bowen, Stephen R.; Kinahan, Paul E.

2015-01-01

Purpose: Respiratory-correlated positron emission tomography (PET/CT) 4D PET/CT is used to mitigate errors from respiratory motion; however, the optimal CT attenuation correction (CTAC) method for 4D PET/CT is unknown. The authors performed a phantom study to evaluate the quantitative performance of CTAC methods for 4D PET/CT in the ground truth setting. Methods: A programmable respiratory motion phantom with a custom movable insert designed to emulate a lung lesion and lung tissue was used for this study. The insert was driven by one of five waveforms: two sinusoidal waveforms or three patient-specific respiratory waveforms. 3DPET and 4DPET images of the phantom under motion were acquired and reconstructed with six CTAC methods: helical breath-hold (3DHEL), helical free-breathing (3DMOT), 4D phase-averaged (4DAVG), 4D maximum intensity projection (4DMIP), 4D phase-matched (4DMATCH), and 4D end-exhale (4DEXH) CTAC. Recovery of SUVmax, SUVmean, SUVpeak, and segmented tumor volume was evaluated as RCmax, RCmean, RCpeak, and RCvol, representing percent difference relative to the static ground truth case. Paired Wilcoxon tests and Kruskal–Wallis ANOVA were used to test for significant differences. Results: For 4DPET imaging, the maximum intensity projection CTAC produced significantly more accurate recovery coefficients than all other CTAC methods (p < 0.0001 over all metrics). Over all motion waveforms, ratios of 4DMIP CTAC recovery were 0.2 ± 5.4, −1.8 ± 6.5, −3.2 ± 5.0, and 3.0 ± 5.9 for RCmax, RCpeak, RCmean, and RCvol. In comparison, recovery coefficients for phase-matched CTAC were −8.4 ± 5.3, −10.5 ± 6.2, −7.6 ± 5.0, and −13.0 ± 7.7 for RCmax, RCpeak, RCmean, and RCvol. When testing differences between phases over all CTAC methods and waveforms, end-exhale phases were significantly more accurate (p = 0.005). However, these differences were driven by the patient-specific respiratory waveforms; when testing patient and sinusoidal waveforms separately, patient waveforms were significantly different between phases (p < 0.0001) while the sinusoidal waveforms were not significantly different (p = 0.98). When considering only the subset of 4DMATCH images that corresponded to the end-exhale image phase, 4DEXH, mean and interquartile range were similar to 4DMATCH but variability was considerably reduced. Conclusions: Comparative advantages in accuracy and precision of SUV metrics and segmented volumes were demonstrated with the use of the maximum intensity projection and end-exhale CT attenuation correction. While respiratory phase-matched CTAC should in theory provide optimal corrections, image artifacts and differences in implementation of 4DCT and 4DPET sorting can degrade the benefit of this approach. These results may be useful to guide the implementation, analysis, and development of respiratory-correlated thoracic PET/CT in the radiation oncology and diagnostic settings. PMID:25563252

Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group?Determination of acetamide herbicides and their degradation products in water using online solid-phase extraction and liquid chromatography/mass spectrometry

USGS Publications Warehouse

Lee, E.A.; Strahan, A.P.

2003-01-01

An analytical method for the determination of 6 acetamide herbicides (acetochlor, alachlor, dimethenamid, flufenacet, metolachlor, and propachlor) and 16 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is described in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using octadecylsilane as the solid-phase extraction media on online automated equipment followed by liquid chromatography/mass spectrometry. The method uses only 10 milliliters of sample per injection. Three different water-sample matrices, a reagent-water, a ground-water, and a surface-water sample spiked at 0.10 and 1.0 microgram per liter, were analyzed to determine method performance. Method detection limits ranged from 0.004 to 0.051 microgram per liter for the parent acetamide herbicides and their degradation products. Mean recoveries for the acetamide compounds in the ground- and surface-water samples ranged from 62.3 to 117.4 percent. The secondary amide of acetochlor/metolachlor ethanesulfonic acid (ESA) was recovered at an average rate of 43.5 percent. The mean recoveries for propachlor and propachlor oxanilic acid (OXA) were next lowest, ranging from 62.3 to 95.5 percent. Mean recoveries from reagent-water samples ranged from 90.3 to 118.3 percent for all compounds. Overall the mean of the mean recoveries of all compounds in the three matrices spiked at 0.10 and 1.0 microgram per liter ranged from 89.9 to 100.7 percent, including the secondary amide of acetochlor/metolachlor ESA and the propachlor compounds. The acetamide herbicides and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter. The upper concentration limit is 2.0 micrograms per liter for all compounds without dilution. With the exception of the secondary amide of acetochlor/metolachlor ESA, good precision and accuracy for the chloroacetanalide herbicides and their degradation compounds were demonstrated for the method in buffered reagent water, ground water, and surface water. The extraction method as used did not optimize the recovery of the secondary amide of acetochlor/metolachlor ESA.

Statistical study of auroral omega bands

NASA Astrophysics Data System (ADS)

Partamies, Noora; Weygand, James M.; Juusola, Liisa

2017-09-01

The presence of very few statistical studies on auroral omega bands motivated us to test-use a semi-automatic method for identifying large-scale undulations of the diffuse aurora boundary and to investigate their occurrence. Five identical all-sky cameras with overlapping fields of view provided data for 438 auroral omega-like structures over Fennoscandian Lapland from 1996 to 2007. The results from this set of omega band events agree remarkably well with previous observations of omega band occurrence in magnetic local time (MLT), lifetime, location between the region 1 and 2 field-aligned currents, as well as current density estimates. The average peak emission height of omega forms corresponds to the estimated precipitation energies of a few keV, which experienced no significant change during the events. Analysis of both local and global magnetic indices demonstrates that omega bands are observed during substorm expansion and recovery phases that are more intense than average substorm expansion and recovery phases in the same region. The omega occurrence with respect to the substorm expansion and recovery phases is in a very good agreement with an earlier observed distribution of fast earthward flows in the plasma sheet during expansion and recovery phases. These findings support the theory that omegas are produced by fast earthward flows and auroral streamers, despite the rarity of good conjugate observations.

Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry.

PubMed

Kruve, Anneli; Künnapas, Allan; Herodes, Koit; Leito, Ivo

2008-04-11

Three sample preparation methods: Luke method (AOAC 985.22), QuEChERS (quick, easy, cheap, effective, rugged and safe) and matrix solid-phase dispersion (MSPD) were applied to different fruits and vegetables for analysis of 14 pesticide residues by high-performance liquid chromatography with electrospray ionization-mass spectrometry (HPLC/ESI/MS). Matrix effect, recovery and process efficiency of the sample preparation methods applied to different fruits and vegetables were compared. The Luke method was found to produce least matrix effect. On an average the best recoveries were obtained with the QuEChERS method. MSPD gave unsatisfactory recoveries for some basic pesticide residues. Comparison of matrix effects for different apple varieties showed high variability for some residues. It was demonstrated that the amount of co-extracting compounds that cause ionization suppression of aldicarb depends on the apple variety as well as on the sample preparation method employed.

LC-method development for the quantification of neuromedin-like peptides. Emphasis on column choice and mobile phase composition.

PubMed

Van Wanseele, Yannick; Viaene, Johan; Van den Borre, Leslie; Dewachter, Kathleen; Vander Heyden, Yvan; Smolders, Ilse; Van Eeckhaut, Ann

2017-04-15

In this study, the separation of four neuromedin-like peptides is investigated on four different core-shell stationary phases. Moreover, the effect of the mobile phase composition, i.e. organic modifier (acetonitrile and methanol) and additive (trifluoroacetic acid, formic acid, acetic acid, ammonium formate and ammonium acetate) on the chromatographic performance is studied. An improvement in chromatographic performance is observed when using the ammonium salt instead of its corresponding acid as additive, except for the column containing a positively charged surface (C18+). In general, the RP-Amide column provided the highest separation power with different mobile phases. However, for the neuromedin-like peptides of interest, the C18+ column in combination with a mobile phase containing methanol as organic modifier and acetic acid as additive provided narrower and higher peaks. A three-factor, three-level design is applied to further optimize the method in terms of increased peak height and reduced solvent consumption, without loss in resolution. The optimized method was subsequently used to assess the in vitro microdialysis recovery of the peptides of interest. Recovery values between 4 and 8% were obtained using a perfusion flow rate of 2μL/min. Copyright © 2017 Elsevier B.V. All rights reserved.

Recovery of organic acids

DOEpatents

Verser, Dan W.; Eggeman, Timothy J.

2009-10-13

A method is disclosed for the recovery of an organic acid from a dilute salt solution in which the cation of the salt forms an insoluble carbonate salt. A tertiary amine and CO.sub.2 are introduced to the solution to form the insoluble carbonate salt and a complex between the acid and an amine. A water immiscible solvent, such as an alcohol, is added to extract the acid/amine complex from the dilute salt solution to a reaction phase. The reaction phase is continuously dried and a product between the acid and the solvent, such as an ester, is formed.

Recovery of organic acids

DOEpatents

Verser, Dan W [Menlo Park, CA; Eggeman, Timothy J [Lakewood, CO

2011-11-01

A method is disclosed for the recovery of an organic acid from a dilute salt solution in which the cation of the salt forms an insoluble carbonate salt. A tertiary amine and CO.sub.2 are introduced to the solution to form the insoluble carbonate salt and a complex between the acid and an amine. A water immiscible solvent, such as an alcohol, is added to extract the acid/amine complex from the dilute salt solution to a reaction phase. The reaction phase is continuously dried and a product between the acid and the solvent, such as an ester, is formed.

Digital Mirror Device Application in Reduction of Wave-front Phase Errors

PubMed Central

Zhang, Yaping; Liu, Yan; Wang, Shuxue

2009-01-01

In order to correct the image distortion created by the mixing/shear layer, creative and effectual correction methods are necessary. First, a method combining adaptive optics (AO) correction with a digital micro-mirror device (DMD) is presented. Second, performance of an AO system using the Phase Diverse Speckle (PDS) principle is characterized in detail. Through combining the DMD method with PDS, a significant reduction in wavefront phase error is achieved in simulations and experiments. This kind of complex correction principle can be used to recovery the degraded images caused by unforeseen error sources. PMID:22574016

Psychosis, creativity and recovery: exploring the relationship in a patient.

PubMed

Kar, Nilamadhab; Barreto, Socorro

2018-04-26

Relation between mental illness and creativity is intricate. While many creative people show signs of mental illness, persons with severe mental illness occasionally have creative output beyond the ordinary. We are presenting a patient with psychotic illness whose creative potential took a positive turn during the illness phase and grew further following symptomatic improvement and helped in her recovery process. Observing the contrast related to creative productivity pre and post psychotic phase raises the probability of whether psychotic illness or process might enhance creative potential. The case additionally illustrates how creativity can be a useful method supporting recovery from severe mental illnesses. © BMJ Publishing Group Ltd (unless otherwise stated in the text of the article) 2018. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

Remedial options for creosote-contaminated sites

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

Wu, W.J.; Delshad, M.; Oolman, T.

2000-03-31

Free-phase DNAPL recovery operations are becoming increasingly prevalent at creosote-contaminated aquifer sites. This paper illustrates the potential of both classical and innovative recovery methods. The UTCHEM multiphase flow and transport numerical simulator was used to predict the migration of creosote DNAPL during a hypothetical spill event, during a long-term redistribution after the spill, and for a variety of subsequent free-phase DNAPL recovery operations. The physical parameters used for the DNAPL and the aquifer in the model are estimates for the DNAPL and the aquifer in the model are estimates for a specific creosote DNAPL site. Other simulations were also conductedmore » using physical parameters that are typical of a trichloroethene (TCE) DNAPL. Dramatic differences in DNAPL migration were observed between these simulations.« less

Reverse phase HPLC method for detection and quantification of lupin seed γ-conglutin.

PubMed

Mane, Sharmilee; Bringans, Scott; Johnson, Stuart; Pareek, Vishnu; Utikar, Ranjeet

2017-09-15

A simple, selective and accurate reverse phase HPLC method was developed for detection and quantitation of γ-conglutin from lupin seed extract. A linear gradient of water and acetonitrile containing trifluoroacetic acid (TFA) on a reverse phase column (Agilent Zorbax 300SB C-18), with a flow rate of 0.8ml/min was able to produce a sharp and symmetric peak of γ-conglutin with a retention time at 29.16min. The identity of γ-conglutin in the peak was confirmed by mass spectrometry (MS/MS identification) and sodium dodecyl sulphate polyacrylamide gel electrophoresis (SDS-PAGE) analysis. The data obtained from MS/MS analysis was matched against the specified database to obtain the exact match for the protein of interest. The proposed method was validated in terms of specificity, linearity, sensitivity, precision, recovery and accuracy. The analytical parameters revealed that the validated method was capable of selectively performing a good chromatographic separation of γ-conglutin from the lupin seed extract with no interference of the matrix. The detection and quantitation limit of γ-conglutin were found to be 2.68μg/ml and 8.12μg/ml respectively. The accuracy (precision and recovery) analysis of the method was conducted under repeatable conditions on different days. Intra-day and inter-day precision values less than 0.5% and recovery greater than 97% indicated high precision and accuracy of the method for analysis of γ-conglutin. The method validation findings were reproducible and can be successfully applied for routine analysis of γ-conglutin from lupin seed extract. Copyright © 2017 Elsevier B.V. All rights reserved.

A Novel Aqueous Micellar Two-Phase System Composed of Surfactant and Sorbitol for Purification of Pectinase Enzyme from Psidium guajava and Recycling Phase Components

PubMed Central

Murshid, Fara Syazana; Manap, Mohd Yazid; Hussin, Muhaini

2015-01-01

A novel aqueous two-phase system composed of a surfactant and sorbitol was employed for the first time to purify pectinase from Psidium guajava. The influences of different parameters, including the type and concentration of the surfactant and the concentration and composition of the surfactant/sorbitol ratio, on the partitioning behavior and recovery of pectinase were investigated. Moreover, the effects of system pH and the crude load on purification fold and the yield of purified pectinase were studied. The experimental results indicated that the pectinase was partitioned into surfactant-rich top phase, and the impurities were partitioned into the sorbitol-rich bottom phase with the novel method involving an ATPS composed of 26% (w/w) Triton X-100 and 23% (w/w) sorbitol at 54.2% of the TLL crude load of 20% (w/w) at pH 6.0. The enzyme was successfully recovered by this method with a high purification factor of 15.2 and a yield of 98.3%, whereas the phase components were also recovered and recycled at rates above 96%. This study demonstrated that this novel ATPS method can be used as an efficient and economical alternative to the traditional ATPS for the purification and recovery of the valuable enzyme. PMID:25756051

A novel liquid/liquid extraction process composed of surfactant and acetonitrile for purification of polygalacturonase enzyme from Durio zibethinus.

PubMed

Amid, Mehrnoush; Manap, Yazid; Azmira, Farhana; Hussin, Muhaini; Sarker, Zaidul Islam

2015-07-01

Polygalacturonase is one of the important enzymes used in various industries such as food, detergent, pharmaceutical, textile, pulp and paper. A novel liquid/liquid extraction process composed of surfactant and acetonitrile was employed for the first time to purify polygalacturonase from Durio zibethinus. The influences of different parameters such as type and concentration of surfactants, concentrations of acetonitrile and composition of surfactant/acetonitrile on partitioning behavior and recovery of polygalacturonase was investigated. Moreover, the effect of pH of system and crude load on purification fold and yield of purified polygalacturonase were studied. The results of the experiment indicated the polygalacturonase was partitioned into surfactant top rich phase with impurities being partitioned into acetonitrile bottom rich phase in the novel method of liquid/liquid process composed of 23% (w/w) Triton X-100 and 19% (w/w) acetonitrile, at 55.6% of TLL (tie line length) crude load of 25% (w/w) at pH 6.0. Recovery and recycling of components also was measured in each successive step of liquid/liquid extraction process. The enzyme was successfully recovered by the method with a high purification factor of 14.3 and yield of 97.3% while phase components were also recovered and recycled above 95%. This study demonstrated that the novel method of liquid/liquid extraction process can be used as an efficient and economical extraction method rather than the traditional methods of extraction for the purification and recovery of the valuable enzyme. Copyright © 2015 Elsevier B.V. All rights reserved.

Automated solid-phase extraction workstations combined with quantitative bioanalytical LC/MS.

PubMed

Huang, N H; Kagel, J R; Rossi, D T

1999-03-01

An automated solid-phase extraction workstation was used to develop, characterize and validate an LC/MS/MS method for quantifying a novel lipid-regulating drug in dog plasma. Method development was facilitated by workstation functions that allowed wash solvents of varying organic composition to be mixed and tested automatically. Precision estimates for this approach were within 9.8% relative standard deviation (RSD) across the calibration range. Accuracy for replicate determinations of quality controls was between -7.2 and +6.2% relative error (RE) over 5-1,000 ng/ml(-1). Recoveries were evaluated for a wide variety of wash solvents, elution solvents and sorbents. Optimized recoveries were generally > 95%. A sample throughput benchmark for the method was approximately equal 8 min per sample. Because of parallel sample processing, 100 samples were extracted in less than 120 min. The approach has proven useful for use with LC/MS/MS, using a multiple reaction monitoring (MRM) approach.

Method development for the analysis of 1,4-dioxane in drinking water using solid-phase extraction and gas chromatography-mass spectrometry.

PubMed

Grimmett, Paul E; Munch, Jean W

2009-01-01

1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The United States Environmental Protection Agency's (U.S. EPA) National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of an activated carbon solid-phase extraction of 500-mL or 100-mL water samples using dichloromethane as the elution solvent. The extracts are analyzed by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. In the NERL laboratory, recovery of 1,4-dioxane ranged from 94-110% in fortified laboratory reagent water and recoveries of 96-102% were demonstrated for fortified drinking water samples. The relative standard deviations for replicate analyses were less than 6% at concentrations exceeding the minimum reporting level.

A new method for concentration analysis of bacterial endotoxins in perfluorocarbon

NASA Astrophysics Data System (ADS)

Chen, Dan-Dan; Feng, Xiao-Ming; Wang, Chun-Ren; Huang, Qing-Quan; Yang, Zhao-Peng; Meng, Qing-Yuan

2014-12-01

This communication demonstrates the feasibility of the gel-clot method for the analysis of bacterial endotoxins in water extracts of perfluorocarbon which is a water insoluble liquid medical device. Perfluorocarbon (10 mL) was shaken with 10mL water for 15 min at 2000 r/min and the endotoxin present was extracted to the aqueous phase without interference inhibition/enhancement of the product and the recovery of endotoxin added to perfluorocarbon was determined. A validation study confirmed that endotoxins presented in perfluorocarbon pass over into the aqueous phase at concentrations of 20, 10 and 5 EU/mL with recoveries from 86.8% to 96.8%. Therefore, the gel-clot test is suitable for detecting bacterial endotoxins in perfluorocarbon which is a water insoluble medical device.

Monitoring training load, recovery-stress state, immune-endocrine responses, and physical performance in elite female basketball players during a periodized training program.

PubMed

Nunes, João A; Moreira, Alexandre; Crewther, Blair T; Nosaka, Ken; Viveiros, Luis; Aoki, Marcelo S

2014-10-01

This study investigated the effect of a periodized training program on internal training load (ITL), recovery-stress state, immune-endocrine responses, and physical performance in 19 elite female basketball players. The participants were monitored across a 12-week period before an international championship, which included 2 overloading and tapering phases. The first overloading phase (fourth to sixth week) was followed by a 1-week tapering, and the second overloading phase (eighth to 10th week) was followed by a 2-week tapering. ITL (session rating of perceived exertion method) and recovery-stress state (RESTQ-76 Sport questionnaire) were assessed weekly and bi-weekly, respectively. Pretraining and posttraining assessments included measures of salivary IgA, testosterone and cortisol concentrations, strength, jumping power, running endurance, and agility. Internal training load increased across all weeks from 2 to 11 (p ≤ 0.05). After the first tapering period (week 7), a further increase in ITL was observed during the second overloading phase (p ≤ 0.05). After the second tapering period, a decrease in ITL was detected (p ≤ 0.05). A disturbance in athlete stress-recovery state was noted during the second overloading period (p ≤ 0.05), before returning to baseline level in end of the second tapering period. The training program led to significant improvements in the physical performance parameters evaluated. The salivary measures did not change despite the fluctuations in ITL. In conclusion, a periodized training program evoked changes in ITL in elite female basketball players, which appeared to influence their recovery-stress state. The training plan was effective in preparing participants for competition, as indicated by improvements in recovery-stress state and physical performance after tapering.

Field-scale multi-phase LNAPL remediation: Validating a new computational framework against sequential field pilot trials.

PubMed

Sookhak Lari, Kaveh; Johnston, Colin D; Rayner, John L; Davis, Greg B

2018-03-05

Remediation of subsurface systems, including groundwater, soil and soil gas, contaminated with light non-aqueous phase liquids (LNAPLs) is challenging. Field-scale pilot trials of multi-phase remediation were undertaken at a site to determine the effectiveness of recovery options. Sequential LNAPL skimming and vacuum-enhanced skimming, with and without water table drawdown were trialled over 78days; in total extracting over 5m 3 of LNAPL. For the first time, a multi-component simulation framework (including the multi-phase multi-component code TMVOC-MP and processing codes) was developed and applied to simulate the broad range of multi-phase remediation and recovery methods used in the field trials. This framework was validated against the sequential pilot trials by comparing predicted and measured LNAPL mass removal rates and compositional changes. The framework was tested on both a Cray supercomputer and a cluster. Simulations mimicked trends in LNAPL recovery rates (from 0.14 to 3mL/s) across all remediation techniques each operating over periods of 4-14days over the 78day trial. The code also approximated order of magnitude compositional changes of hazardous chemical concentrations in extracted gas during vacuum-enhanced recovery. The verified framework enables longer term prediction of the effectiveness of remediation approaches allowing better determination of remediation endpoints and long-term risks. Copyright © 2017 Commonwealth Scientific and Industrial Research Organisation. Published by Elsevier B.V. All rights reserved.

Ionospheric behaviour during storm recovery phase

NASA Astrophysics Data System (ADS)

Buresova, D.; Lastovicka, J.; Boska, J.; Sindelarova, T.; Chum, J.

2012-04-01

Intensive ionospheric research, numerous multi-instrumental observations and large-scale numerical simulations of ionospheric F region response to magnetic storm-induced disturbances during the last several decades were primarily focused on the storm main phase, in most cases covering only a few hours of the recovery phase following after storm culmination. Ionospheric behaviour during entire recovery phase still belongs to not sufficiently explored and hardly predictable features. In general, the recovery phase is characterized by an abatement of perturbations and a gradual return to the "ground state" of ionosphere. However, observations of stormy ionosphere show significant departures from the climatology also within this phase. This paper deals with the quantitative and qualitative analysis of the ionospheric behaviour during the entire recovery phase of strong-to-severe magnetic storms at middle latitudes for nowadays and future modelling and forecasting purposes.

Simultaneous determination of emamectin and ivermectin residues in Atlantic salmon muscle by liquid chromatography with fluorescence detection.

PubMed

van de Riet, J M; Brothers, N N; Pearce, J N; Burns, B G

2001-01-01

A liquid chromatographic (LC) method for determining residues of the antiparasitic drugs emamectin (EMA) and ivermectin (IVR) in fish tissues has been developed. EMA and IVR residues are extracted with acetonitrile and cleaned up on a C18 solid-phase extraction column. Extracts are derivatized with 1-methylimidazole and trifluoroacetic anhydride and the components are determined by LC on a C18 reversed-phase column with fluorescence detection (excitation: 365 nm, emission: 470 nm). The mobile phase is 94% acetonitrile-water run isocratically. Calibration curves were linear between 1 and 32 ng injected for both EMA and IVR. The limit of detection for both analytes was 0.5 ng/g, with a limit of quantitation of 1.5 ng/g. Recoveries of EMA and IVR added to salmon muscle averaged 96 +/- 9% and 86 +/- 6%, respectively, at levels between 5 and 80 ng/g. The percent relative standard deviation for the described method was less than 7% over the range of concentrations studied. The operational errors, interferences, and recoveries for fortified samples compare favorably with an established IVR method. The recommended method is simple, rapid, and specific for monitoring residues of EMA and IVR in Atlantic salmon muscle.

Application of spectrophotometric, densitometric, and HPLC techniques as stability indicating methods for determination of Zaleplon in pharmaceutical preparations

NASA Astrophysics Data System (ADS)

Metwally, Fadia H.; Abdelkawy, M.; Abdelwahab, Nada S.

2007-12-01

Spectrophotometric, spectrodensitometric and HPLC are stability indicating methods described for determination of Zaleplon in pure and dosage forms. As Zaleplon is easily degradable, the proposed techniques in this manuscript are adopted for its determination in presence of its alkaline degradation product, namely N-[4-(3-cyano-pyrazolo[1,5a]pyridin-7-yl)-phenyl]- N-ethyl-acetamide. These approaches are successfully applied to quantify Zaleplon using the information included in the absorption spectra of appropriate solutions. The second derivative (D 2) spectrophotometric method, allows determination of Zaleplon without interference of its degradate at 235.2 nm using 0.01N HCl as a solvent with obedience to Beer's law over a concentration range of 1-10 μg ml -1 with mean percentage recovery 100.24 ± 0.86%. The first derivative of the ratio spectra ( 1DD) based on the simultaneous use of ( 1DD) and measurement at 241.8 nm using the same solvent and over the same concentration range as (D 2) spectrophotometric method, with mean percentage recovery 99.9 ± 1.07%. The spectrodensitometric analysis allows the separation and quantitation of Zaleplon from its degradate on silica gel plates using chloroform:acetone:ammonia solution (9:1:0.2 by volume) as a mobile phase. This method depends on quantitave densitometric evaluation of thin layer chromatogram of Zaleplon at 338 nm over a concentration range of 0.2-1 μg band -1, with mean percentage recovery 99.73 ± 1.35. Also a reversed-phase liquid chromatographic method using 5-C8 (22 cm × 4.6 mm i.d. 5 μm particle size) column was described and validated for quantitation of Zaleplon using acetonitrile:deionised water (35:65, v/v) as a mobile phase using Paracetamol as internal standard and a flow rate of 1.5 ml min -1 with UV detection of the effluent at 232 nm at ambient temperature over a concentration range of 2-20 μg ml -1 with mean percentage recovery 100.19 ± 1.15%. The insignificance difference of the proposed methods results with those of the reference one proved their accuracy and precision.

Dysprosium sorption by polymeric composite bead: robust parametric optimization using Taguchi method.

PubMed

Yadav, Kartikey K; Dasgupta, Kinshuk; Singh, Dhruva K; Varshney, Lalit; Singh, Harvinderpal

2015-03-06

Polyethersulfone-based beads encapsulating di-2-ethylhexyl phosphoric acid have been synthesized and evaluated for the recovery of rare earth values from the aqueous media. Percentage recovery and the sorption behavior of Dy(III) have been investigated under wide range of experimental parameters using these beads. Taguchi method utilizing L-18 orthogonal array has been adopted to identify the most influential process parameters responsible for higher degree of recovery with enhanced sorption of Dy(III) from chloride medium. Analysis of variance indicated that the feed concentration of Dy(III) is the most influential factor for equilibrium sorption capacity, whereas aqueous phase acidity influences the percentage recovery most. The presence of polyvinyl alcohol and multiwalled carbon nanotube modified the internal structure of the composite beads and resulted in uniform distribution of organic extractant inside polymeric matrix. The experiment performed under optimum process conditions as predicted by Taguchi method resulted in enhanced Dy(III) recovery and sorption capacity by polymeric beads with minimum standard deviation. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of ultrasound-assisted emulsification microextraction based on solidification of a floating organic droplet for determination of organochlorine pesticides in water samples.

PubMed

Shu, Bin; Yang, Zhaoguang; Lee, Hsiaowan; Qiu, Bo; Li, Haipu

2016-02-01

An ultrasound-assisted emulsification microextraction based on the solidification of a floating organic droplet followed by gas chromatography with electron capture detection was developed for the simultaneous determination of 13 organochlorine pesticides in water samples. In the proposed method, ultrasound was applied to achieve the emulsification without addition of any dispersive solvent. In consequence, the volume of extraction phase remained unaffected by the ion strength of aqueous phase and high extraction recoveries were obtained. It was also found that dilution of the floating phase with acetone was necessary for preventing peak splitting in chromatogram. Under optimal conditions, the proposed method provided good sensitivity (the detection limits of organochlorine pesticides ranged from 1.3 to 3.9 ng/L) and good repeatability of extraction (below 6.5%, n = 5). The recoveries in reservoir and river water samples were between 75.8% and 96.9%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A contradictory phenomenon of deshelving pulses in a dilute medium used for lengthened photon storage time.

PubMed

Ham, Byoung S

2010-08-16

Lengthening of photon storage time has been an important issue in quantum memories for long distance quantum communications utilizing quantum repeaters. Atom population transfer into an auxiliary spin state has been adapted to increase photon storage time of photon echoes. In this population transfer process phase shift to the collective atoms is inevitable, where the phase recovery condition must be multiple of 2pi to satisfy rephasing mechanism. Recent adaptation of the population transfer method to atomic frequency comb (AFC) echoes [Afzelius et al., Phys. Rev. Lett. 104, 040503 (2010)], where the population transfer method is originated in a controlled reversible inhomogeneous broadening technique [Moiseev and Kroll, Phys. Rev. Lett. 87, 173601 (2001)], however, shows contradictory phenomenon violating the phase recovery condition. This contradiction in AFC is reviewed as a general case of optical locking applied to a dilute medium for an optical depth-dependent coherence leakage resulting in partial retrieval efficiency.

Analysis and comparison of different phase shifters for Stirling pulse tube cryocooler

NASA Astrophysics Data System (ADS)

Lei, Tian; Pfotenhauer, John M.; Zhou, Wenjie

2016-12-01

Investigations of phase shifters and power recovery mechanisms are of sustainable interest for developing Stirling pulse tube cryocoolers (SPTC) with higher power density, more compact design and higher efficiency. This paper investigates the phase shifting capacity and the applications of four different phase shifters, including conventional inertance tube, gas-liquid and spring-oscillator phase shifters, as well as a power recovery displacer. Distributed models based on the electro-acoustic analogy are developed to estimate the phase shifting capacity and the acoustic power dissipation of the three phase shifters without power recovery. The results show that both gas-liquid and spring-oscillator phase shifters have the distinctive capacity of phase shifting with a significant reduction in the inertial component length. Furthermore, full distributed models of SPTCs connected with different phase shifters are developed. The cooling performance of SPTCs using all four phase shifters are presented and typical phase relations are analyzed. The comparison reveals that the power recovery displacer with a more complicated configuration provides the highest efficiency. The gas-liquid and spring-oscillator phase shifters show equivalent efficiency compared with the inertance tube phase shifter. Approximately 10-20% of the acoustic power is dissipated by the phase shifters without power recovery, while 15-20% of the acoustic power can be recovered by the power recovery displacer, leading to a maximum coefficient of performance (COP) above 0.14 at 80 K. A merit analysis is also done by presenting the pros and cons of different phase shifters.

Application of molecularly imprinted polymer based matrix solid phase dispersion for determination of fluoroquinolones, tetracyclines and sulfonamides in meat.

PubMed

Wang, Geng Nan; Zhang, Lei; Song, Yi Ping; Liu, Ju Xiang; Wang, Jian Ping

2017-10-15

In this study, a type of novel mixed-template molecularly imprinted polymer was synthesized that was able to recognize 8 fluoroquinolones, 8 sulfonamides and 4 tetracyclines simultaneously with recoveries higher than 92%. Then the polymer was used to develop a matrix solid phase dispersion method for simultaneous extraction of the 20 drugs in pork followed by determination with ultra performance liquid chromatography. During the experiments, the MMIP amount, washing solvent and elution solvent were optimized respectively. The limits of detection of this method for the 20 drugs in pork were in the range of 0.5-3.0ngg -1 , and the intra-day and inter-day recoveries from the fortified blank samples were in the range of 74.5%-102.7%. Therefore, this method could be used as a rapid, simple, specific and sensitive method for multi-determination of the residues of the three classes of drugs in meat. Copyright © 2017 Elsevier B.V. All rights reserved.

pH-Responsive Mercaptoundecanoic Acid Functionalized Gold Nanoparticles and Applications in Catalysis

PubMed Central

Ansar, Siyam M.; Chakraborty, Saptarshi

2018-01-01

Mercaptoundecanoic acid (MUA) functionalized gold nanoparticles (AuNP-MUA) were synthesized and demonstrated to possess pH-triggered aggregation and re-dispersion, as well as the capability of phase transfer between aqueous and organic phases in response to changes in pH. The pH of aggregation for AuNP-MUA is consistent with the pKa of MUA (pH ~4) in solution, while AuNP-MUA phase transition between aqueous and organic phases occurs at pH ~9. The ion pair formation between the amine group in octadecylamine (ODA), the carboxylate group in MUA, and the hydrophobic alkyl chain of ODA facilitates the phase transfer of AuNP-MUA into an organic medium. The AuNP-MUA were investigated as a reusable catalyst in the catalytic reduction of 4-nitrophenol by borohydride—a model reaction for AuNPs. It was determined that 100% MUA surface coverage completely inhibits the catalytic activity of AuNPs. Decreasing the surface coverage was shown to increase catalytic activity, but this decrease also leads to decreased colloidal stability, recoverability, and reusability in subsequent reactions. At 60% MUA surface coverage, colloidal stability and catalytic activity were achieved, but the surface coverage was insufficient to enable redispersion following pH-induced recovery. A balance between AuNP colloidal stability, recoverability, and catalytic activity with reusability was achieved at 90% MUA surface coverage. The AuNP-MUA catalyst can also be recovered at different pH ranges depending on the recovery method employed. At pH ~4, protonation of the MUA results in reduced surface charge and aggregation. At pH ~9, ODA will form an ion-pair with the MUA and induce phase transfer into an immiscible organic phase. Both the pH-triggered aggregation/re-dispersion and aqueous/organic phase transfer methods were employed for catalyst recovery and reuse in subsequent reactions. The ability to recover and reuse the AuNP-MUA catalyst by two different methods and different pH regimes is significant, based on the fact that nanoparticle-catalyzed reactions may occur under different pH conditions. PMID:29772775

Impact of CT attenuation correction method on quantitative respiratory-correlated (4D) PET/CT imaging

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

Nyflot, Matthew J., E-mail: nyflot@uw.edu; Lee, Tzu-Cheng; Alessio, Adam M.

Purpose: Respiratory-correlated positron emission tomography (PET/CT) 4D PET/CT is used to mitigate errors from respiratory motion; however, the optimal CT attenuation correction (CTAC) method for 4D PET/CT is unknown. The authors performed a phantom study to evaluate the quantitative performance of CTAC methods for 4D PET/CT in the ground truth setting. Methods: A programmable respiratory motion phantom with a custom movable insert designed to emulate a lung lesion and lung tissue was used for this study. The insert was driven by one of five waveforms: two sinusoidal waveforms or three patient-specific respiratory waveforms. 3DPET and 4DPET images of the phantommore » under motion were acquired and reconstructed with six CTAC methods: helical breath-hold (3DHEL), helical free-breathing (3DMOT), 4D phase-averaged (4DAVG), 4D maximum intensity projection (4DMIP), 4D phase-matched (4DMATCH), and 4D end-exhale (4DEXH) CTAC. Recovery of SUV{sub max}, SUV{sub mean}, SUV{sub peak}, and segmented tumor volume was evaluated as RC{sub max}, RC{sub mean}, RC{sub peak}, and RC{sub vol}, representing percent difference relative to the static ground truth case. Paired Wilcoxon tests and Kruskal–Wallis ANOVA were used to test for significant differences. Results: For 4DPET imaging, the maximum intensity projection CTAC produced significantly more accurate recovery coefficients than all other CTAC methods (p < 0.0001 over all metrics). Over all motion waveforms, ratios of 4DMIP CTAC recovery were 0.2 ± 5.4, −1.8 ± 6.5, −3.2 ± 5.0, and 3.0 ± 5.9 for RC{sub max}, RC{sub peak}, RC{sub mean}, and RC{sub vol}. In comparison, recovery coefficients for phase-matched CTAC were −8.4 ± 5.3, −10.5 ± 6.2, −7.6 ± 5.0, and −13.0 ± 7.7 for RC{sub max}, RC{sub peak}, RC{sub mean}, and RC{sub vol}. When testing differences between phases over all CTAC methods and waveforms, end-exhale phases were significantly more accurate (p = 0.005). However, these differences were driven by the patient-specific respiratory waveforms; when testing patient and sinusoidal waveforms separately, patient waveforms were significantly different between phases (p < 0.0001) while the sinusoidal waveforms were not significantly different (p = 0.98). When considering only the subset of 4DMATCH images that corresponded to the end-exhale image phase, 4DEXH, mean and interquartile range were similar to 4DMATCH but variability was considerably reduced. Conclusions: Comparative advantages in accuracy and precision of SUV metrics and segmented volumes were demonstrated with the use of the maximum intensity projection and end-exhale CT attenuation correction. While respiratory phase-matched CTAC should in theory provide optimal corrections, image artifacts and differences in implementation of 4DCT and 4DPET sorting can degrade the benefit of this approach. These results may be useful to guide the implementation, analysis, and development of respiratory-correlated thoracic PET/CT in the radiation oncology and diagnostic settings.« less

Polarization-insensitive techniques for optical signal processing

NASA Astrophysics Data System (ADS)

Salem, Reza

2006-12-01

This thesis investigates polarization-insensitive methods for optical signal processing. Two signal processing techniques are studied: clock recovery based on two-photon absorption in silicon and demultiplexing based on cross-phase modulation in highly nonlinear fiber. The clock recovery system is tested at an 80 Gb/s data rate for both back-to-back and transmission experiments. The demultiplexer is tested at a 160 Gb/s data rate in a back-to-back experiment. We experimentally demonstrate methods for eliminating polarization dependence in both systems. Our experimental results are confirmed by theoretical and numerical analysis.

40 CFR 300.315 - Phase IV-Documentation and cost recovery.

Code of Federal Regulations, 2010 CFR

2010-07-01

... scientific understanding of the environment and for research and development of improved response methods and...) SUPERFUND, EMERGENCY PLANNING, AND COMMUNITY RIGHT-TO-KNOW PROGRAMS NATIONAL OIL AND HAZARDOUS SUBSTANCES...

40 CFR 300.315 - Phase IV-Documentation and cost recovery.

Code of Federal Regulations, 2011 CFR

2011-07-01

...) SUPERFUND, EMERGENCY PLANNING, AND COMMUNITY RIGHT-TO-KNOW PROGRAMS NATIONAL OIL AND HAZARDOUS SUBSTANCES... scientific understanding of the environment and for research and development of improved response methods and...

Multi-phased anaerobic baffled reactor treating food waste.

PubMed

Ahamed, A; Chen, C-L; Rajagopal, R; Wu, D; Mao, Y; Ho, I J R; Lim, J W; Wang, J-Y

2015-04-01

This study was conducted to identify the performance of a multi-phased anaerobic baffled reactor (MP-ABR) with food waste (FW) as the substrate for biogas production and thereby to promote an efficient energy recovery and treatment method for the wastes with high organic solid content through phase separation. A four-chambered ABR was operated at an HRT of 30 days with an OLR of 0.5-1.0 g-VS/Ld for a period of 175 days at 35 ± 1°C. Consistent overall removal efficiencies of 85.3% (CODt), 94.5% (CODs), 89.6% (VFA) and 86.4% (VS) were observed throughout the experiment displaying a great potential to treat FW. Biogas generated was 215.57 mL/g-VS removed d. Phase separation was observed and supported by the COD and VFA trends, and an efficient recovery of bioenergy from FW was achieved. Copyright © 2015 Elsevier Ltd. All rights reserved.

Joint Carrier-Phase Synchronization and LDPC Decoding

NASA Technical Reports Server (NTRS)

Simon, Marvin; Valles, Esteban

2009-01-01

A method has been proposed to increase the degree of synchronization of a radio receiver with the phase of a suppressed carrier signal modulated with a binary- phase-shift-keying (BPSK) or quaternary- phase-shift-keying (QPSK) signal representing a low-density parity-check (LDPC) code. This method is an extended version of the method described in Using LDPC Code Constraints to Aid Recovery of Symbol Timing (NPO-43112), NASA Tech Briefs, Vol. 32, No. 10 (October 2008), page 54. Both methods and the receiver architectures in which they would be implemented belong to a class of timing- recovery methods and corresponding receiver architectures characterized as pilotless in that they do not require transmission and reception of pilot signals. The proposed method calls for the use of what is known in the art as soft decision feedback to remove the modulation from a replica of the incoming signal prior to feeding this replica to a phase-locked loop (PLL) or other carrier-tracking stage in the receiver. Soft decision feedback refers to suitably processed versions of intermediate results of iterative computations involved in the LDPC decoding process. Unlike a related prior method in which hard decision feedback (the final sequence of decoded symbols) is used to remove the modulation, the proposed method does not require estimation of the decoder error probability. In a basic digital implementation of the proposed method, the incoming signal (having carrier phase theta theta (sub c) plus noise would first be converted to inphase (I) and quadrature (Q) baseband signals by mixing it with I and Q signals at the carrier frequency [wc/(2 pi)] generated by a local oscillator. The resulting demodulated signals would be processed through one-symbol-period integrate and- dump filters, the outputs of which would be sampled and held, then multiplied by a soft-decision version of the baseband modulated signal. The resulting I and Q products consist of terms proportional to the cosine and sine of the carrier phase cc as well as correlated noise components. These products would be fed as inputs to a digital PLL that would include a number-controlled oscillator (NCO), which provides an estimate of the carrier phase, theta(sub c).

A digital clock recovery algorithm based on chromatic dispersion and polarization mode dispersion feedback dual phase detection for coherent optical transmission systems

NASA Astrophysics Data System (ADS)

Liu, Bo; Xin, Xiangjun; Zhang, Lijia; Wang, Fu; Zhang, Qi

2018-02-01

A new feedback symbol timing recovery technique using timing estimation joint equalization is proposed for digital receivers with two samples/symbol or higher sampling rate. Different from traditional methods, the clock recovery algorithm in this paper adopts another algorithm distinguishing the phases of adjacent symbols, so as to accurately estimate the timing offset based on the adjacent signals with the same phase. The addition of the module for eliminating phase modulation interference before timing estimation further reduce the variance, thus resulting in a smoothed timing estimate. The Mean Square Error (MSE) and Bit Error Rate (BER) of the resulting timing estimate are simulated to allow a satisfactory estimation performance. The obtained clock tone performance is satisfactory for MQAM modulation formats and the Roll-off Factor (ROF) close to 0. In the back-to-back system, when ROF= 0, the maximum of MSE obtained with the proposed approach reaches 0 . 0125. After 100-km fiber transmission, BER decreases to 10-3 with ROF= 0 and OSNR = 11 dB. With the increase in ROF, the performances of MSE and BER become better.

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

PubMed

Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improved Heat-of-Fusion Energy Storage

NASA Technical Reports Server (NTRS)

Chen, K. H.; Manvi, R.

1982-01-01

Alkali metal/alkali-halide mixtures proposed for preventing solid buildup during energy recovery. When mixture melts (by absorption of heat of fusion), it forms two immiscible liquids. Salt-rich phase is heavier and has higher melting/recrysallization temperature; so during energy recovery salt crystallizes in this phase first. Since heat exchanger for energy recovery is in lighter metal-rich phase, solids do not form and there is no reduction of heat-recovery efficiency.

A new separation and preconcentration method for selenium in some foods using modified silica gel with 2,6-diamino-4-phenil-1,3,5-triazine.

PubMed

Mendil, Durali; Demirci, Zafer; Uluozlu, Ozgur Dogan; Tuzen, Mustafa; Soylak, Mustafa

2017-04-15

A novel and simple solid phase extraction method was improved and recommended for selenium. Silica gel was modified with 2,6-diamino-4-phenil-1,3,5-triazine and characterized by FTIR, SEM and elemental analysis and used adsorbent for column solid phase extraction of selenium ions. The experimental parameters (pH, flow rates, amounts of the modified silica gel, concentration and type of eluent, volume of sample, etc.) on the recoveries of selenium were optimized. Standard reference materials were analyzed for validation of method. The present method was successfully applied to the detection of total selenium in water and microwave digested some food samples with quantitative recoveries (> 95%). The relative standard deviations were<8%. Matrix influences were not observed. The adsorption capacity of modified silica gel was 5.90mgg -1 . The LOD was 0.015μgL -1 . Enrichment factor was obtained as 50 for the introduced method. Copyright © 2016 Elsevier Ltd. All rights reserved.

What time does the recovery phase of geomagnetic storms start: A superposed epoch analysis

NASA Astrophysics Data System (ADS)

Du, A.; Zhang, Y.; Ou, J.; Luo, H.

2015-12-01

It is well known that the recovery phase of the geomagnetic storms start during Dst reaches a minimum. This present paper is a discussion of recovery phase onset of a superposed epoch analysis of 247 storm events (-450 < Dst < -50 nT). The data of the solar wind parameters, the geomagnetic index AE and Dst are by means of 1 hour OMNI database. The energy budget for the driver and decay terms introduced by Burton et al. (1975) are checked. As might be expected, the recovery phase of geomagnetic storms starts when the decay term is greater than the driver term. The balance of the decay and driver terms is also dependent on the solar wind energy input during the initial phase. In general, at the onset of the recovery phase, EK-L decreases to 70% of a maximum of EK-L.

Recovery Based on Spirituality in Substance Abusers in Iran

PubMed Central

Shamsalinia, Abbas; Norouzi, Kiyan; Khoshknab, Masoud Fallahi; Farhoudian, Ali

2014-01-01

Background and Purpose: Spirituality is an important factor influencing the decrease of substance abuse severity and maintenance of the recovery phase. This research, investigates the effect of spiritual experiences in the recovery of substance abusers. Material and Methods: Qualitative data was collected from 16 men and 6 women, selected through purposeful sampling to ensure an equilibrated gender representation and data from different recovery periods. Data were collected via semi-structured interviews. Results: Data showed two main categories: “Mutual relationship between spirituality and recovery,” divided into four subcategories: religious background, religious teachings, experience exchange, and support of family and society; and “A new perspective toward life” subdivided into access to calmness and spiritual development. A factor “spirituality meaning religion” arose repeatedly throughout the study. Conclusion: The results of this study can be useful for policy makers, care providers, families, and drug addicts. The promotion of spirituality in substance abusers can help in their struggle with temptation. Effective strategies to ensure drug abstinence and maintenance of the recovery phase are encouraging substance abusers and their families to participate in spirituality-based psychotherapy sessions held in addiction treatment centers, multi-disciplinary cooperation among the organizations involved in the addiction phenomenon, and training the families regarding the importance of spirituality in the mental health of their children through mass media. PMID:25363097

Catalytic distillation water recovery subsystem

NASA Technical Reports Server (NTRS)

Budininkas, P.; Rasouli, F.

1985-01-01

An integrated engineering breadboard subsystem for the recovery of potable water from untreated urine based on the vapor phase catalytic ammonia removal was designed, fabricated and tested. Unlike other evaporative methods, this process catalytically oxidizes ammonia and volatile hydrocarbons vaporizing with water to innocuous products; therefore, no pretreatment of urine is required. Since the subsystem is fabricated from commercially available components, its volume, weight and power requirements are not optimized; however, it is suitable for zero-g operation. The testing program consists of parametric tests, one month of daily tests and a continuous test of 168 hours duration. The recovered water is clear, odorless, low in ammonia and organic carbon, and requires only an adjustment of its pH to meet potable water standards. The obtained data indicate that the vapor phase catalytic ammonia removal process, if further developed, would also be competitive with other water recovery systems in weight, volume and power requirements.

Recovery of biotechnological products using aqueous two phase systems.

PubMed

Phong, Win Nee; Show, Pau Loke; Chow, Yin Hui; Ling, Tau Chuan

2018-04-16

Aqueous two-phase system (ATPS) has been suggested as a promising separation tool in the biotechnological industry. This liquid-liquid extraction technique represents an interesting advance in downstream processing due to several advantages such as simplicity, rapid separation, efficiency, economy, flexibility and biocompatibility. Up to date, a range of biotechnological products have been successfully recovered from different sources with high yield using ATPS-based strategy. In view of the important potential contribution of the ATPS in downstream processing, this review article aims to provide latest information about the application of ATPS in the recovery of various biotechnological products in the past 7 years (2010-2017). Apart from that, the challenges as well as the possible future work and outlook of the ATPS-based recovery method have also been presented in this review article. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Determination of highly protein bound drugs in plasma using high-performance liquid chromatography and column switching, exemplified by the retinoids.

PubMed

Wyss, R; Bucheli, F

1988-12-02

During method development for the determination of either isotretinoin, tretinoin and their 4-oxo-metabolites, or etretinate, acitretin and 13-cis-acitretin in plasma using high-performance liquid chromatography and column switching, recovery problems arose, when undiluted plasma samples were injected directly onto the precolumn. These recovery problems may be due to the strong binding of the retinoids to different plasma proteins. Measures to overcome this strong protein binding, such as variation of the injection solution composition and the purge mobile phase, were systematically investigated. Best recoveries were obtained by diluting of plasma with 9 mM sodium hydroxide-acetonitrile (8:2, v/v) and protein precipitation with ethanol for the isotretinoin and etretinate series, respectively, in combination with the use of a purge mobile phase containing ammonium acetate and 10-20% acetonitrile. Less effective was the use of a longer precolumn or heating of the precolumn.

Deproteinizing methods evaluated for determination of uric acid in serum by reversed-phase liquid chromatography with ultraviolet detection.

PubMed

Sakuma, R; Nishina, T; Kitamura, M

1987-08-01

We evaluated six deproteinizing methods for determination of uric acid in serum by "high-performance" liquid chromatography with ultraviolet detection: those involving zinc hydroxide, sodium tungstate, trichloroacetic acid, perchloric acid, acetonitrile, and centrifugal ultrafiltration (with Amicon MPS-1 devices). We used a Toyosoda ODS-120A reversed-phase column. The mobile phase was sodium phosphate buffer (40 mmol/L, pH 2.2) containing 20 mL of methanol per liter. Absorbance of the eluate was monitored at 284 nm. The precipitation method with perchloric acid gave high recoveries of uric acid and good precision, and results agreed with those by the uricase-catalase method of Kageyama (Clin Chim Acta 1971;31:421-6).

Optical ptychographic microscopy for quantitative anisotropic phase imaging

NASA Astrophysics Data System (ADS)

Anthony, N.; Cadenazzi, G.; Nugent, K. A.; Abbey, B.

2016-12-01

Ptychography has recently been adapted for the recovery of the complete Jones matrix of an anisotropic specimen, using a vectorial form of the Ptychographic Iterative Engine (vPIE) for a set of linearly polarized probes. Here we show that this method can be applied to the recovery of the in-plane components of the elastic strain tensor in a diametrically compressed disc. The advantages and disadvantages of vPIE for the recovery of strain information from `real-world' samples is discussed as well as the potential for this approach to be applied to the characterization of the mechanical properties of optically transparent materials

Chemical enhanced oil recovery (EOR) activities in Indonesia: How it's future

NASA Astrophysics Data System (ADS)

Abdurrahman, Muslim

2017-05-01

Enhanced oil recovery (EOR) is a proven method for increasing oil production in many oil fields in the world. Huge oil remaining in the reservoir after primary and secondary recovery stage are the main reason for developing EOR methods. Approximately of 49.50 billion barrels oil as a candidate for EOR activities in Indonesia. This present study focuses on the chemical EOR activities involved surfactant and polymer. This research based on pertinent information from various resources such as journal papers, conference papers, and report from the government. Based on this information, this paper explain in detail the progress of each project and it shows the potential oil field employ chemical EOR in the near future. Generally, the EOR activities can be categorized into two phases such as preliminary study phase and field implementation phase. In the preliminary study, the activities simply involve experimental and/or simulation works. Following the preliminary is the field implementation phase which can be categorized into three phases such as field trial, pilot project, and full-scale. In fact, several activities have been conducted by Lemigas (government oil and gas research center), Institut Teknologi Bandung, Institut Pertanian Bogor. These activities focused on laboratory and simulation work. Those institutions have been developing the chemical formula collaborating with oil companies for applying the EOR method in their oil fields. Currently, status of chemical EOR activities include 5 oil fields under pilot project and 12 oil fields under field trial. There are 7 oil fields applying surfactant, 4 oil fields by alkaline-surfactant-polymer (ASP), 2 oil fields by polymer, 1 oil field by surfactant polymer (SP), and 1 oil field by caustic. According to this information, we will have insight knowledge about the EOR current activities, the main issues, future activities on chemical EOR in Indonesia. Moreover, this study can became the preliminary information for researchers who interested conducting further research and development on the chemical EOR activities in the near future.

Getting by, getting back, and getting on: Matching mental health services to consumers' recovery goals.

PubMed

Yarborough, Bobbi Jo H; Yarborough, Micah T; Janoff, Shannon L; Green, Carla A

2016-06-01

The goal of this study was to better understand mental health recovery from the point of view of mental health consumers to identify opportunities for practice improvements that closely align services with consumer goals and consumer-preferred outcomes. As part of an exploratory study of recovery, semistructured interviews were conducted with 177 integrated health plan members diagnosed with schizophrenia, schizoaffective disorder, bipolar disorder, or affective psychosis. Transcripts of in-depth interviews were coded using Atlas.ti, and definitions of recovery were further subcoded. A qualitative analysis using a modified grounded theory approach and constant comparative method identified common themes and less common but potentially important recovery-related experiences and perspectives. Three primary and 2 cross-cutting themes emerged. "Getting by" meant coping and meeting basic needs. "Getting back" meant learning to live with mental illness. "Getting on" meant living a life where mental illness was no longer prominent. Regaining control and recouping losses were cross-cutting themes. Mental health recovery is complex and dynamic; individuals' recovery goals can be expected to change over time. Person-centered care must accommodate changing consumer priorities, services must be flexible and responsive, and outcomes need to match consumers' objectives. Clinicians can assist in (a) identifying recovery goals, (b) monitoring progress toward and recognizing movement away from goals, (c) tailoring support to different phases/stages, and (d) supporting transitions between phases/stages. (PsycINFO Database Record (c) 2016 APA, all rights reserved).

Simultaneous determination of piracetam and vincamine by spectrophotometric and high-performance liquid chromatographic methods.

PubMed

El-Saharty, Yasser Shaker Ibrahim

2008-01-01

A mixture of piracetam and vincamine was determined by 3 different methods. The first was the determination of piracetam and vincamine using the ratio-spectra first-derivative (DD1) spectrophotometric technique at 209 and 293 nm in concentration ranges of 10-45 and 2-14 microg/mL with mean recoveries of 99.22 +/- 0.72 and 99.67 +/- 0.79%, respectively. The second method was based on the resolution of the 2 components by bivariate calibration depending on a mathematic algorithm that provides simplicity and rapidity. The method depended on quantitative evaluation of the absorbencies at 210 and 225 nm in concentration ranges of 5-45 and 2-14 microg/mL, with mean recoveries of 100.33 +/- 0.54 and 100.44 +/- 0.98% for piracetam and vincamine, respectively. The third method was reversed-phase liquid chromatography using 0.05 M potassium dihydrogen phosphate-methanol (50 + 50, v/v) as the mobile phase, with the pH adjusted to 3.5 with phosphoric acid. The eluent was monitored at 215 nm in concentration ranges of 5-100 and 2-200 microg/mL, with mean recoveries of 99.62 +/- 0.67 and 99.32 +/- 0.85% for piracetam and vincamine, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparation. The methods retained their accuracy and precision when applying the standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

Solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery mine, near Edgemont, South Dakota

USGS Publications Warehouse

Johnson, Raymond H.; Diehl, Sharon F.; Benzel, William M.

2013-01-01

This report releases solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery site near Edgemont, South Dakota. These cores were collected by Powertech Uranium Corporation, and material not used for their analyses were given to the U.S. Geological Survey for additional sampling and analyses. These additional analyses included total carbon and sulfur, whole rock acid digestion for major and trace elements, 234U/238U activity ratios, X-ray diffraction, thin sections, scanning electron microscopy analyses, and cathodoluminescence. This report provides the methods and data results from these analyses along with a short summary of observations.

Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

PubMed

Srivastava, Alpuna; Pandey, Richa; Verma, Ram K; Gupta, Madan M

2006-01-01

A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanol-water (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 microm, 125 x 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 microg/mL). Detection limits were 10 microg/mL for sennoside B and 35 microg/mL for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 microg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by Carbopak-B solid-phase extraction and high-preformance liquid chromatography

USGS Publications Warehouse

Werner, Stephen L.; Burkhardt, Mark R.; DeRusseau, Sabrina N.

1996-01-01

In accordance with the needs of the National Water-Quality Assessment Program (NAWQA), the U.S. Geological Survey has developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method. The method is used to determine 41 pesticides and pesticide metabolites that are not readily amenable to gas chromatography or other high-temperature analytical techniques. Pesticides are extracted from filtered environmental water samples using a 0.5-gram graphitized carbon-based solid-phase cartridge, eluted from the cartridge into two analytical fractions, and analyzed using high-performance liquid chromatography with photodiode-array detection. The upper concentration limit is 1.6 micrograms per liter (=B5g/L) for most compounds. Single-operator method detection limits in organic-free water samples ranged from 0.006 to 0.032 =B5g/L= Recoveries in organic-free water samples ranged from 37 to 88 percent. Recoveries in ground- and surface-water samples ranged from 29 to 94 percent. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time of 7 days.

Application of a novel cold activated carbon fiber-solid phase microextraction for analysis of organochlorine pesticides in soil.

PubMed

Chai, Xiaolan; Jia, Jinping; Sun, Tonghua; Wang, Yalin; Liao, Liyan

2007-08-01

A novel and simple analytical procedure using cold activated carbon fiber-solid phase microextraction (CACF-SPME) was applied to determine organochlorine pesticides (OCs) in soil samples. The pesticides in this study consist of alpha -, beta -, gamma -, and delta -hexachlorocyclohexane (HCH). By heating the sample while cooling the fiber, the developed method not only provides better performance in terms of sensitivity, linearity and recovery but also offers shorter adsorption procedure than that of traditional headspace-solid phase microextraction (HS-SPME). The experimental conditions such as the amount of water, adsorption time and adsorption temperature were optimized. Matrix effects were investigated with different types of soils. We concluded that using the standard addition method was required for quantification purposes. The limits of detection obtained using the proposed method range from 0.01 to 0.05 ng/g, and the recoveries for CACF-SPME are in the range of 80.01% to 89.68% with relative standard deviation (RSDs) better than 8.60%. The proposed method was further applied to determine OCs in real agricultural soil. The results are in good agreement with those obtained using traditional ultrasonic extraction. The research demonstrates the suitability of the CACF-SPME for the analysis of OCs in soil.

Mixed hemimicelles solid-phase extraction based on sodium dodecyl sulfate (SDS)-coated nano-magnets for the spectrophotometric determination of Fingolomid in biological fluids

NASA Astrophysics Data System (ADS)

Azari, Zhila; Pourbasheer, Eslam; Beheshti, Abolghasem

2016-01-01

In this study, mixed hemimicelles solid-phase extraction (SPE) based on sodium dodecyl sulfate (SDS)-coated nano-magnets Fe3O4 was investigated as a novel method for the separation and determination of Fingolimod (FLM) in water, urine and plasma samples prior to spectrophotometeric determination. Due to the high surface area of these new sorbents and the excellent adsorption capacity after surface modification by SDS, satisfactory extraction recoveries can be produced. The main factors affecting the adsolubilization of analysts, such as pH, surfactant and adsorbent amounts, ionic strength, extraction time and desorption conditions were studied and optimized. Under the selected conditions, FLM has been quantitatively extracted. The accuracy of the method was evaluated by recovery measurements on spiked samples, and good recoveries of 96%, 95% and 88% were observed for water, urine and plasma respectively. Proper linear behaviors over the investigated concentration ranges of 2-26, 2-17 and 2-13 mg/L with good coefficients of determination, 0.998, 0.997 and 0.995 were achieved for water, urine and plasma samples, respectively. To the best of our knowledge, this is the first time that a mixed hemimicelles SPE method based on magnetic separation and nanoparticles has been used as a simple and sensitive method for monitoring of FLM in water and biological samples.

Effect of wetting-layer density of states on the gain and phase recovery dynamics of quantum-dot semiconductor optical amplifiers

NASA Astrophysics Data System (ADS)

Kim, Jungho; Yu, Bong-Ahn

2015-03-01

We numerically investigate the effect of the wetting-layer (WL) density of states on the gain and phase recovery dynamics of quantum-dot semiconductor optical amplifiers in both electrical and optical pumping schemes by solving 1088 coupled rate equations. The temporal variations of the ultrafast gain and phase recovery responses at the ground state (GS) are calculated as a function of the WL density of states. The ultrafast gain recovery responses do not significantly depend on the WL density of states in the electrical pumping scheme and the three optical pumping schemes such as the optical pumping to the WL, the optical pumping to the excited state ensemble, and the optical pumping to the GS ensemble. The ultrafast phase recovery responses are also not significantly affected by the WL density of states except the optical pumping to the WL, where the phase recovery component caused by the WL becomes slowed down as the WL density of states increases.

Estimation of three-phase relative permeability by simulating fluid dynamics directly on rock-microstructure images

NASA Astrophysics Data System (ADS)

Jiang, F.; Tsuji, T.

2017-01-01

Given the world's growing demand for energy, a combination of geological CO2 sequestration and enhanced oil recovery (EOR) technologies is currently regarded as a promising solution, as it would provide a means of reducing carbon emissions into the atmosphere while also leading to the economic benefit of simultaneously recovering oil. The optimization of injection strategies to maximize CO2 storage and increase the oil recovery factors requires complicated pore-scale flow information within a reservoir system consisting of coexisting oil, water, and CO2 phases. In this study, an immiscible three-phase lattice-Boltzmann (LB) model was developed to investigate the complicated flow state with interaction between water, oil, and CO2 systems in porous media. The two main mechanisms of oil remobilization, namely, double-drainage and film flow, can be captured by our model. The estimation of three-phase relative permeability is proposed using the digital rock physics (DRP) simulations. The results indicate that the relative permeability of CO2 as calculated using our steady state method is not sensitive to the initial oil fraction if the oil distribution is originally uniform. Baker's (1988) empirical model was tested and found to be able to provide a good prediction of the three-phase relative permeability data. Our numerical method provides a new tool for accurately predicting three-phase relative permeability data directly based on micro-CT rock images.

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.

Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of triazine and phenylurea herbicides and their degradation products in water using solid-phase extraction and liquid chromatography/mass spectrometry

USGS Publications Warehouse

Lee, Edward Alan; Strahan, Alex P.; Thurman, Earl Michael

2002-01-01

An analytical method for the determination of 7 triazine and phenylurea herbicides and 12 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is presented in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using 0.5 gram graphitized carbon as the solid-phase extraction media followed by liquid chromatography/mass spectrometry. Three different water-sample matrices?ground-water, surface-water, and reagent-water samples?spiked at 0.2 and 2.0 micrograms per liter were analyzed. Method detection limits ranged from 0.013 to 0.168 microgram per liter for the parent triazine herbicides and the triazine degradation products. Method detection limits ranged from 0.042 to 0.141 microgram per liter for the parent phenylurea herbicides and their degradation products. Mean recoveries for the triazine compounds in the ground- and surface-water samples generally ranged from 72.6 to 117.5 percent, but deethyl-cyanazine amide was recovered at 140.5 percent. Mean recoveries from the ground- and surface-water samples for the phenylurea compounds spiked at the 2.0-micrograms-per-liter level ranged from 82.1 to 114.4 percent. The mean recoveries for the phenylureas spiked at 0.2-microgram per liter were less consistent, ranging from 87.0 to 136.0 percent. Mean recoveries from reagent-water samples ranged from 87.0 to 109.5 percent for all compounds. The triazine compounds and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter, with the exception of deethylcyanazine and deethylcyanazine amide which are reported at 0.20 to 2.0 micrograms per liter. The phenylurea compounds and their degradation products are reported in concentrations ranging from 0.20 to 2.0 micrograms per liter. The upper concentration limit was 2.0 micrograms per liter for all compounds without dilution.

Effect of additional optical pumping injection into the ground-state ensemble on the gain and the phase recovery acceleration of quantum-dot semiconductor optical amplifiers

NASA Astrophysics Data System (ADS)

Kim, Jungho

2014-02-01

The effect of additional optical pumping injection into the ground-state ensemble on the ultrafast gain and the phase recovery dynamics of electrically-driven quantum-dot semiconductor optical amplifiers is numerically investigated by solving 1088 coupled rate equations. The ultrafast gain and the phase recovery responses are calculated with respect to the additional optical pumping power. Increasing the additional optical pumping power can significantly accelerate the ultrafast phase recovery, which cannot be done by increasing the injection current density.

Nanofluid of graphene-based amphiphilic Janus nanosheets for tertiary or enhanced oil recovery: High performance at low concentration

PubMed Central

Luo, Dan; Wang, Feng; Zhu, Jingyi; Cao, Feng; Liu, Yuan; Li, Xiaogang; Willson, Richard C.; Yang, Zhaozhong; Chu, Ching-Wu; Ren, Zhifeng

2016-01-01

The current simple nanofluid flooding method for tertiary or enhanced oil recovery is inefficient, especially when used with low nanoparticle concentration. We have designed and produced a nanofluid of graphene-based amphiphilic nanosheets that is very effective at low concentration. Our nanosheets spontaneously approached the oil–water interface and reduced the interfacial tension in a saline environment (4 wt % NaCl and 1 wt % CaCl2), regardless of the solid surface wettability. A climbing film appeared and grew at moderate hydrodynamic condition to encapsulate the oil phase. With strong hydrodynamic power input, a solid-like interfacial film formed and was able to return to its original form even after being seriously disturbed. The film rapidly separated oil and water phases for slug-like oil displacement. The unique behavior of our nanosheet nanofluid tripled the best performance of conventional nanofluid flooding methods under similar conditions. PMID:27354529

Nanofluid of graphene-based amphiphilic Janus nanosheets for tertiary or enhanced oil recovery: High performance at low concentration.

PubMed

Luo, Dan; Wang, Feng; Zhu, Jingyi; Cao, Feng; Liu, Yuan; Li, Xiaogang; Willson, Richard C; Yang, Zhaozhong; Chu, Ching-Wu; Ren, Zhifeng

2016-07-12

The current simple nanofluid flooding method for tertiary or enhanced oil recovery is inefficient, especially when used with low nanoparticle concentration. We have designed and produced a nanofluid of graphene-based amphiphilic nanosheets that is very effective at low concentration. Our nanosheets spontaneously approached the oil-water interface and reduced the interfacial tension in a saline environment (4 wt % NaCl and 1 wt % CaCl2), regardless of the solid surface wettability. A climbing film appeared and grew at moderate hydrodynamic condition to encapsulate the oil phase. With strong hydrodynamic power input, a solid-like interfacial film formed and was able to return to its original form even after being seriously disturbed. The film rapidly separated oil and water phases for slug-like oil displacement. The unique behavior of our nanosheet nanofluid tripled the best performance of conventional nanofluid flooding methods under similar conditions.

Reshaping an enduring sense of self: the process of recovery from a first episode of schizophrenia.

PubMed

Romano, Donna M; McCay, Elizabeth; Goering, Paula; Boydell, Katherine; Zipursky, Robert

2010-08-01

Although advances in the treatment of schizophrenia have been made, little is known about the process of recovery from first episode of schizophrenia (FES). To date, the study of recovery in the field of mental health has focused on long-term mental illness. This qualitative study addresses ways in which individuals with FES describe their process of recovery and how identified individuals (e.g. family members) describe their perceptions of and roles in the participant's process of recovery. Charmaz's constructivist grounded theory methodology was used to interview 10 young adults twice who self-identified as recovering from FES. In addition, 10 individuals were identified who had influenced their recovery and were interviewed once, for a total of 30 interviews. Data collection sources included in-depth semi-structured interviews. Data analysis methods were consistent with Charmaz's methodology and included coding, and constant comparison of data. The results provide a substantive theory of the process of recovery from FES that is comprised of the following phases: 'Who they were prior to the illness', 'Lives interrupted: Encountering the illness', 'Engaging in services and supports', 'Re-engaging in life', 'Envisioning the future'; and the core category, 'Re-shaping an enduring sense of self', that occurred throughout all phases. A prominent feature of this model is that participants' enduring sense of self were reshaped rather than reconstructed throughout their recovery. This model of recovery from FES is unique, and as such, provides implications for clinical care, research and policy development for these young adults and their families.

Determination of a flame retardant hydrolysis product in human urine by SPE and LC-MS. Comparison of molecularly imprinted solid-phase extraction with a mixed-mode anion exchanger.

PubMed

Möller, Kristina; Crescenzi, Carlo; Nilsson, Ulrika

2004-01-01

Diphenyl phosphate is a hydrolysis product and possible metabolite of the flame retardant and plasticiser additive triphenyl phosphate. A molecularly imprinted polymer solid-phase extraction (MISPE) method for extracting diphenyl phosphate from aqueous solutions has been developed and compared with SPE using a commercially available mixed-mode anion exchanger. The imprinted polymer was prepared using 2-vinylpyridine (2-Vpy) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, and a structural analogue of the analyte as the template molecule. The imprinted polymer was evaluated for use as a SPE sorbent, in tests with both aqueous standards and spiked urine samples, by comparing recovery and breakthrough data obtained using the imprinted form of the polymer and a non-imprinted form (NIP). Extraction from aqueous solutions resulted in more than 80% recovery. Adsorption by the molecularly imprinted polymer (MIP) was non-selective, but selectivity was achieved by selective desorption in the wash steps. Diphenyl phosphate could also be selectively extracted from urine samples, although the urine matrix reduced the capacity of the MISPE cartridges. Recoveries from urine extraction were higher than 70%. It was important to control pH during sample loading. The MISPE method was found to yield a less complex LC-ESI-MS chromatogram of the urine extracts compared with the mixed-mode anion-exchanger method. An LC-ESI-MS method using a Hypercarb LC column with a graphitised carbon stationary phase was also evaluated for organophosphate diesters. LC-ESI-MS using negative-ion detection in selected ion monitoring (SIM) mode was shown to be linear for diphenyl phosphate in the range 0.08-20 ng microL(-1).

Sci-Fri AM: MRI and Diagnostic Imaging - 05: Comparison of Input Function Measurements from DCE and MOLLI

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

Majtenyi, Nicholas; Juma, Hanif; Klein, Ran

Dynamic contrast-enhanced (DCE)-MRI is a technique for obtaining tissue hemodynamic information (e.g. tumours). Despite widespread clinical application of DCE-MRI, the technique suffers from a lack of standardization and accuracy, especially with respect to the concentration-versus-time of gadolinium (Gd) in feeding arteries (the input function, IF). MR phase has a linear quantitative relationship with Gd concentration ([Gd]), making it ideal for measuring the first-pass of the IF, but is not considered accurate in the steady-state washout. Modified Look-Locker Inversion Recovery (MOLLI) is a fast and accurate method to measure T1 and has been validated to quantify typical [Gd] ranges experienced inmore » the washout of the IF. Two different methods to measure the IF for DCE-MRI were compared: 1) conventional phase-versus-time (“Phase-only”) and 2) phase-versus-time combined with pre- and post-DCE MOLLI T1 measurements (“Phase+MOLLI”). The IF obtained from Phase+MOLLI was calculated from MOLLI T1 values and known relaxivity, then added to the Phase-only acquisition with the washout IF subtracted. A significant difference was observed between IF values for [Gd] between the Phase-only and Phase+MOLLI acquisitions (P = 0.03). To ensure the IFs from MOLLI T1s were accurate, it was compared to [Gd] obtained from “gold-standard” inversion recovery (IR). MOLLI showed excellent agreement with IR when imaged in static phantoms (r{sup 2} = 0.997, P = 0.001). The Phase+MOLLI IF was more accurate than the Phase-only IF in measuring the washout. The Phase+MOLLI acquisition may therefore provide a DCE-MRI reference standard that could lead to better clinical diagnoses.« less

Development of a gas chromatography-mass spectrometry method for the determination of pesticides in gaseous and particulate phases in the atmosphere.

PubMed

Borrás, E; Sánchez, P; Muñoz, A; Tortajada-Genaro, L A

2011-08-05

A reliable multi-residue method for determining gaseous and particulate phase pesticides in atmospheric samples has been developed. This method, based on full scan gas chromatography-mass spectrometry (GC-MS), allowed the proper determination of sixteen relevant pesticides, in a wide range of concentrations and without the influence of interferences. The pesticides were benfluralin, bitertanol, buprofezin, chlorfenvinphos, chlorpyrifos, chlorpyrifos-methyl, ethalfluralin, fenthion, lindane, malathion, methidathion, propachlor, propanil, pyriproxifen, tebuconazol and trifluralin. Comparisons of two types of sampling filters (quartz and glass fibre) and four types of solid-phase cartridges (XAD-2, XAD-4, Florisil and Orbo-49P) showed that the most suitable supports were glass fibre filter for particulate pesticides and XAD-2 and XAD-4 cartridges for gaseous pesticides (>95% recovery). Evaluations of elution solvents for ultrasonic-assisted extraction demonstrated that isooctane is better than ethylacetate, dichloromethane, methanol or a mixture of acetone:hexane (1:1). Recovery assays and the standard addition method were performed to validate the proposed methodology. Moreover, large simulator chamber experiments allowed the best study of the gas-particle partitioning of pesticides for testing the sampling efficiency for the validation of an analytical multiresidue method for pesticides in air. Satisfactory analytical parameters were obtained, with a repeatability of 5±1%, a reproducibility of 13±3% and detection limits of 0.05-0.18 pg m(-3) for the particulate phase and 26-88 pg m(-3) for the gaseous phase. Finally, the methodology was successfully applied to rural and agricultural samples in the Mediterranean area. Copyright © 2011 Elsevier B.V. All rights reserved.

Analysis of cocoa flavanols and procyanidins (DP 1-10) in cocoa-containing ingredients and products by rapid resolution liquid chromatography: single-laboratory validation.

PubMed

Machonis, Philip R; Jones, Matthew A; Kwik-Uribe, Catherine

2014-01-01

Recently, a multilaboratory validation (MLV) of AOAC Official Method 2012.24 for the determination of cocoa flavanols and procyanidins (CF-CP) in cocoa-based ingredients and products determined that the method was robust, reliable, and transferrable. Due to the complexity of the CF-CP molecules, this method required a run time exceeding 1 h to achieve acceptable separations. To address this issue, a rapid resolution normal phase LC method was developed, and a single-laboratory validation (SLV) study conducted. Flavanols and procyanidins with a degree of polymerization (DP) up to 10 were eluted in 15 min using a binary gradient applied to a diol stationary phase, detected using fluorescence detection, and reported as a total sum of DP 1-10. Quantification was achieved using (-)-epicatechin-based relative response factors for DP 2-10. Spike recovery samples and seven different types of cocoa-based samples were analyzed to evaluate the accuracy, precision, LOD, LOQ, and linearity of the method. The within-day precision of the reported content for the samples was 1.15-5.08%, and overall precision was 3.97-13.61%. Spike-recovery experiments demonstrated recoveries of over 98%. The results of this SLV were compared to those previously obtained in the MLV and found to be consistent. The translation to rapid resolution LC allowed for an 80% reduction in analysis time and solvent usage, while retaining the accuracy and reliability of the original method. The savings in both cost and time of this rapid method make it well-suited for routine laboratory use.

Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

2015-09-30

A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

Improved method for the extraction and chromatographic analysis on a fused-core column of ellagitannins found in oak-aged wine.

PubMed

Navarro, María; Kontoudakis, Nikolaos; Canals, Joan Miquel; García-Romero, Esteban; Gómez-Alonso, Sergio; Zamora, Fernando; Hermosín-Gutiérrez, Isidro

2017-07-01

A new method for the analysis of ellagitannins observed in oak-aged wine is proposed, exhibiting interesting advantages with regard to previously reported analytical methods. The necessary extraction of ellagitannins from wine was simplified to a single step of solid phase extraction (SPE) using size exclusion chromatography with Sephadex LH-20 without the need for any previous SPE of phenolic compounds using reversed-phase materials. The quantitative recovery of wine ellagitannins requires a combined elution with methanol and ethyl acetate, especially for increasing the recovery of the less polar acutissimins. The chromatographic method was performed using a fused-core C18 column, thereby avoiding the coelution of main ellagitannins, such as vescalagin and roburin E. However, the very polar ellagitannins, namely, the roburins A, B and C, still partially coeluted, and their quantification was assisted by the MS detector. This methodology also enabled the analysis of free gallic and ellagic acids in the same chromatographic run. Copyright © 2017 Elsevier Ltd. All rights reserved.

Development and validation of a solid-phase extraction method coupled to liquid chromatography with fluorescence detection for the determination of fluoroquinolone residues in powdered infant formulae. Application to the analysis of samples from the Spanish and Latin American market.

PubMed

Rodriguez, E; Moreno-Bondi, M C; Marazuela, M D

2008-10-31

This paper describes a new method for the effective extraction, clean-up and chromatographic analysis of residues of four fluoroquinolones (ciprofloxacin, enrofloxacin, danofloxacin and sarafloxacin) in powdered infant formulae and follow-on preparations. Samples were reconstituted following the manufacturer's recommendations and treated with trichloroacetic acid in methanol 10% (w/v) for deproteinization. Two solid-phase extraction cartridges have been evaluated for sample clean-up and preconcentration, Strata Screen A and Strata X and the later provided the best recoveries for all the analytes tested. Chromatographic analysis has been carried out using a polar endcapped column (AQUA C(18)) and fluorescence detection, with lomefloxacin (LOME) as internal standard. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(alpha)) and detection capability (CC(beta)). Typical recoveries ranged between 70 and 110% at levels below and above the maximum residue limits of the target analytes in bovine milk, with an excellent intralab reproducibility (RSDs<7%). Matrix effects did not significantly affect method accuracy, as evidenced by analyzing different brands of milk. The method has been successfully applied to the analysis of 100 samples of infant and follow-on formulae of the Spanish and Latin American market, using LC-MS/MS as confirmatory technique.

Liquid chromatographic determination of the cyanobacterial toxin beta-n-methylamino-L-alanine in algae food supplements, freshwater fish, and bottled water.

PubMed

Scott, Peter M; Niedzwiadek, Barbara; Rawn, Dorothea F K; Lau, Ben P-Y

2009-08-01

Beta-N-Methylamino-L-alanine (BMAA) is a neurotoxin originally found in cycad seeds and now known to be produced by many species of freshwater and marine cyanobacteria. We developed a method for its determination in blue-green algae (BGA) food supplements, freshwater fish, and bottled water by using a strong cation-exchange, solid-phase extraction column for cleanup after 0.3 M trichloroacetic acid extraction of BGA supplements and fish. Bottled water was applied directly onto the solid-phase extraction column. For analysis of carbonated water, sonication and pH adjustment to 1.5 were needed. To determine protein-bound BMAA, the protein pellet left after extraction of the BGA supplement and fish was hydrolyzed by boiling with 6 M hydrochloric acid; BMAA was cleaned up on a C18 column and a strong cation-exchange, solid-phase extraction column. Determination of BMAA was by liquid chromatography of the fluorescent derivative formed with 9-fluorenylmethyl chloroformate. The method was validated by recovery experiments using spiking levels of 1.0 to 10 microg/g for BGA supplements, 0.5 to 5.0 microg/g for fish, and 0.002 microg/g for bottled water; mean recoveries were in the range of 67 to 89% for BGA supplements and fish, and 59 to 92% for bottled water. Recoveries of BMAA from spiked extracts of hydrolyzed protein from BGA supplements and fish ranged from 66 to 83%. The cleanup developed provides a useful method for surveying foods and supplements for BMAA and protein-bound BMAA.

Double-resolution electron holography with simple Fourier transform of fringe-shifted holograms.

PubMed

Volkov, V V; Han, M G; Zhu, Y

2013-11-01

We propose a fringe-shifting holographic method with an appropriate image wave recovery algorithm leading to exact solution of holographic equations. With this new method the complex object image wave recovered from holograms appears to have much less traditional artifacts caused by the autocorrelation band present practically in all Fourier transformed holograms. The new analytical solutions make possible a double-resolution electron holography free from autocorrelation band artifacts and thus push the limits for phase resolution. The new image wave recovery algorithm uses a popular Fourier solution of the side band-pass filter technique, while the fringe-shifting holographic method is simple to implement in practice. Published by Elsevier B.V.

Determination of osthol and its metabolites in a phase I reaction system and the Caco-2 cell model by HPLC-UV and LC-MS/MS

PubMed Central

Yuan, Zhenting; Xu, Haiyan; Wang, Ke; Zhao, Zhonghua; Hu, Ming

2012-01-01

A straightforward and sensitive reversed-phase high-performance liquid chromatography (HPLC) assay was developed and validated for the analysis of osthol and its phase I metabolites (internal standard: umbelliferone). The method was validated for the determination of osthol with respect to selectivity, precision, linearity, limit of detection, recovery, and stability. The linear response range was 0.47 ~ 60 μM, and the average recoveries ranged from 98 to 101%. The inter-day and intra-day relative standard deviations were both less than 5%. Using this method, we showed that more than 80% of osthol was metabolized in 20 min in a phase I metabolic reaction system. Transport experiments in the Caco-2 cell culture model indicated that osthol was easily absorbed with high absorptive permeability (>10×10-6 cm/sec). The permeability did not display concentration-dependence or vectorial-dependence and is mildly temperature sensitive (activation energy less than 10 Kcal/mole), indicating passive mechanism of transport. When analyzed by LC-MS/MS, five metabolites were detected in a phase I reaction system and in the receiver side of a modified Caco-2 cell model, which was supplemented with the phase I reaction system. The major metabolites appeared to be desmethyl-osthol and multiple isomers of dehydro-osthol. In conclusion, a likely cause of poor osthol bioavailability is rapid phase I metabolism via the cytochrome P-450 pathways. PMID:19304430

Free-product plume distribution and recovery modeling prediction in a diesel-contaminated volcanic aquifer

NASA Astrophysics Data System (ADS)

Hernández-Espriú, Antonio; Martínez-Santos, Pedro; Sánchez-León, Emilio; Marín, Luis E.

Light non-aqueous phase liquids (LNAPL) represent one of the most serious problems in aquifers contaminated with petroleum hydrocarbons liquids. To design an appropriate remediation strategy it is essential to understand the behavior of the plume. The aim of this paper is threefold: (1) to characterize the fluid distribution of an LNAPL plume detected in a volcanic low-conductivity aquifer (∼0.4 m/day from slug tests interpretation), (2) to simulate the recovery processes of the free-product contamination and (3) to evaluate the primary recovery efficiency of the following alternatives: skimming, dual-phase extraction, Bioslurping and multi-phase extraction wells. The API/Charbeneau analytical model was used to investigate the recovery feasibility based on the geological properties and hydrogeological conditions with a multi-phase (water, air, LNAPL) transport approach in the vadose zone. The modeling performed in this research, in terms of LNAPL distribution in the subsurface, show that oil saturation is 7% in the air-oil interface, with a maximum value of 70% in the capillary fringe. Equilibrium between water and LNAPL phases is reached at a depth of 1.80 m from the air-oil interface. On the other hand, the LNAPL recovery model results suggest a remarkable enhancement of the free-product recovery when simultaneous extra-phase extraction was simulated from wells, in addition to the LNAPL lens. Recovery efficiencies were 27%, 65%, 66% and 67% for skimming, dual-phase extraction, Bioslurping and multi-phase extraction, respectively. During a 3-year simulation, skimmer wells and multi-phase extraction showed the lowest and highest LNAPL recovery rates, with expected values from 207 to 163 and 2305 to 707 l-LNAPL/day, respectively. At a field level we are proposing a well distribution arrangement that alternates pairs of dual-phase well-Bioslurping well. This not only improves the recovery of the free-product plume, but also pumps the dissolve plume and enhances in situ biodegradation in the vadose zone. Thus, aquifer and soil remediation can be achieved at a shorter time. Rough calculations suggest that LNAPL can be recovered at an approximate cost of 6-10/l.

RECOVERY OF VOCS FROM SURFACTANT SOLUTION BY PERVAPORATION

EPA Science Inventory

Surfactant-based processes are emerging as promising technologies to enhance conventional pump-and-treat methods for remediating soils contaminated with nonaqueous phase liquids (NAPLs), primarily due to the potential to significantly reduce the remediation time. In order to reus...

A three-phase excess post-exercise oxygen consumption in Atlantic salmon Salmo salar and its response to exercise training.

PubMed

Zhang, Y; Claireaux, G; Takle, H; Jørgensen, S M; Farrell, A P

2018-03-09

The recovery of oxygen uptake to the standard metabolic rate (SMR) following exhaustive chasing exercise in Atlantic salmon Salmo salar parr occurred in three phases (rapid, plateau and slow). The initial recovery phase lasted 0·7 h and contributed 16% to the total excess post-exercise oxygen consumption (EPOC). It was followed by a longer plateau phase that contributed 53% to the total EPOC. The slow recovery phase that completed recovery of SMR, which has not been reported previously, made a 31% contribution to the total EPOC. The plasticity of EPOC was demonstrated in exercise-trained fish. Exercise training increased EPOC by 39% when compared with control fish (mean ± S.E., 877·7 ± 73·1 v. 629·2 ± 53·4 mg O 2 kg -1 , d.f. = 9, P < 0·05), with the duration of the plateau phase increasing by 38% (4·7 ± 0·58 v. 3·4 ± 0·16 h, d.f. = 9, P < 0·05) and the contribution of the slow phase to the total EPOC increasing by 80% (173·9 ± 23·9 v. 312·5 ± 50·4 mg O 2 kg -1 , d.f. = 9, P < 0·05). As a result, the combination of the plateau and slow phases of exercise-trained fish increased by 47% compared with control fish (756·6 ± 71·4 v. 513·6 ± 43·1 mg O 2 kg -1 ; d.f. = 9, P = 0·01). To substantiate the hypothesis that the plateau and slow recovery phase of EPOC was related to general metabolic recovery following exhaustive exercise, the time-course for recovery of SMR was compared with previously published metabolite recovery profiles. The final phase of metabolic recovery was temporally associated with the final phases of gluconeogenesis, lactate oxidation and muscle intracellular pH regulation. Therefore, the plasticity of the latter phase of EPOC agreed with the known effects of exercise training in fishes. © 2018 The Fisheries Society of the British Isles.

Evaluation of arm-leg coordination in flat breaststroke.

PubMed

Chollet, D; Seifert, L; Leblanc, H; Boulesteix, L; Carter, M

2004-10-01

This study proposes a new method to evaluate arm-leg coordination in flat breaststroke. Five arm and leg stroke phases were defined with a velocity-video system. Five time gaps quantified the time between arm and leg actions during three paces of a race (200 m, 100 m and 50 m) in 16 top level swimmers. Based on these time gaps, effective glide, effective propulsion, effective leg insweep and effective recovery were used to identify the different stroke phases of the body. A faster pace corresponded to increased stroke rate, decreased stroke length, increased propulsive phases, shorter glide phases, and a shorter T1 time gap, which measured the effective body glide. The top level swimmers showed short time gaps (T2, T3, T4, measuring the timing of arm-leg recoveries), which reflected the continuity in arm and leg actions. The measurement of these time gaps thus provides a pertinent evaluation of swimmers' skill in adapting their arm-leg coordination to biomechanical constraints.

Generalization of the Poincare sphere to process 2D displacement signals

NASA Astrophysics Data System (ADS)

Sciammarella, Cesar A.; Lamberti, Luciano

2017-06-01

Traditionally the multiple phase method has been considered as an essential tool for phase information recovery. The in-quadrature phase method that theoretically is an alternative pathway to achieve the same goal failed in actual applications. The authors in a previous paper dealing with 1D signals have shown that properly implemented the in-quadrature method yields phase values with the same accuracy than the multiple phase method. The present paper extends the methodology developed in 1D to 2D. This extension is not a straight forward process and requires the introduction of a number of additional concepts and developments. The concept of monogenic function provides the necessary tools required for the extension process. The monogenic function has a graphic representation through the Poincare sphere familiar in the field of Photoelasticity and through the developments introduced in this paper connected to the analysis of displacement fringe patterns. The paper is illustrated with examples of application that show that multiple phases method and the in-quadrature are two aspects of the same basic theoretical model.

Charge Exchange Contribution to the Decay of the Ring Current, Measured by Energetic Neutral Atoms (ENAs)

NASA Technical Reports Server (NTRS)

Jorgensen, A. M.; Henderson, M. G.; Roelof, E. C.; Reeves, G. D.; Spence, H. E.

2001-01-01

In this paper we calculate the contribution of charge exchange to the decay of the ring current. Past works have suggested that charge exchange of ring current protons is primarily responsible for the decay of the ring current during the late recovery phase, but there is still much debate about the fast decay of the early recovery phase. We use energetic neutral atom (ENA) measurements from Polar to calculate the total ENA energy escape. To get the total ENA escape we apply a forward modeling technique, and to estimate the total ring current energy escape we use the Dessler-Parker-Sckopke relationship. We find that during the late recovery phase of the March 10, 1998 storm ENAs with energies greater than 17.5 keV can account for 75% of the estimated energy loss from the ring current. During the fast recovery the measured ENAs can only account for a small portion of the total energy loss. We also find that the lifetime of the trapped ions is significantly shorter during the fast recovery phase than during the late recovery phase, suggesting that different processes are operating during the two phases.

Determination of tylosin and tilmicosin residues in animal tissues by reversed-phase liquid chromatography.

PubMed

Chan, W; Gerhardt, G C; Salisbury, C D

1994-01-01

A method for the simultaneous determination of tylosin and tilmicosin residues in animal tissues is reported. Solid-phase extraction columns are used to isolate the drugs from tissue extracts. Determination is accomplished by reversed-phase liquid chromatography with UV detection at 287 nm. Mean recoveries from spiked tissues were 79.9% (coefficient of variation [CV], 8.1%) for tylosin and 92.6% (CV, 8.7%) for tilmicosin. Detection limits for tylosin and tilmicosin were 0.020 and 0.010 ppm, respectively.

Accelerated wavefront determination technique for optical imaging through scattering medium

NASA Astrophysics Data System (ADS)

He, Hexiang; Wong, Kam Sing

2016-03-01

Wavefront shaping applied on scattering light is a promising optical imaging method in biological systems. Normally, optimized modulation can be obtained by a Liquid-Crystal Spatial Light Modulator (LC-SLM) and CCD hardware iteration. Here we introduce an improved method for this optimization process. The core of the proposed method is to firstly detect the disturbed wavefront, and then to calculate the modulation phase pattern by computer simulation. In particular, phase retrieval method together with phase conjugation is most effective. In this way, the LC-SLM based system can complete the wavefront optimization and imaging restoration within several seconds which is two orders of magnitude faster than the conventional technique. The experimental results show good imaging quality and may contribute to real time imaging recovery in scattering medium.

Scaling of counter-current imbibition recovery curves using artificial neural networks

NASA Astrophysics Data System (ADS)

Jafari, Iman; Masihi, Mohsen; Nasiri Zarandi, Masoud

2018-06-01

Scaling imbibition curves are of great importance in the characterization and simulation of oil production from naturally fractured reservoirs. Different parameters such as matrix porosity and permeability, oil and water viscosities, matrix dimensions, and oil/water interfacial tensions have an effective on the imbibition process. Studies on the scaling imbibition curves along with the consideration of different assumptions have resulted in various scaling equations. In this work, using an artificial neural network (ANN) method, a novel technique is presented for scaling imbibition recovery curves, which can be used for scaling the experimental and field-scale imbibition cases. The imbibition recovery curves for training and testing the neural network were gathered through the simulation of different scenarios using a commercial reservoir simulator. In this ANN-based method, six parameters were assumed to have an effect on the imbibition process and were considered as the inputs for training the network. Using the ‘Bayesian regularization’ training algorithm, the network was trained and tested. Training and testing phases showed superior results in comparison with the other scaling methods. It is concluded that using the new technique is useful for scaling imbibition recovery curves, especially for complex cases, for which the common scaling methods are not designed.

Test results on reuse of reclaimed shower water - A summary

NASA Technical Reports Server (NTRS)

Verostko, Charles E.; Garcia, Rafael; Sauer, Richard; Reysa, Richard P.; Linton, Arthur T.

1989-01-01

Results are presented from tests to evaluate a microgravity whole body shower and waste water recovery system design for possible use on the Space Station. Several water recovery methods were tested, including phase change distillation, a thermoelectric hollow fiber membrane evaporation subsystem, and a reverse osmosis dynamic membrane system. Consideration is given to the test hardware, the types of soaps evaluated, the human response to showering with reclaimed water, chemical treatment for microbial control, the procedures for providing hygienic water, and the quality of water produced by the systems. All three of the waste water recovery systems tested successfully produced reclaimed water for reuse.

Experiments on sparsity assisted phase retrieval of phase objects

NASA Astrophysics Data System (ADS)

Gaur, Charu; Lochab, Priyanka; Khare, Kedar

2017-05-01

Iterative phase retrieval algorithms such as the Gerchberg-Saxton method and the Fienup hybrid input-output method are known to suffer from the twin image stagnation problem, particularly when the solution to be recovered is complex valued and has centrosymmetric support. Recently we showed that the twin image stagnation problem can be addressed using image sparsity ideas (Gaur et al 2015 J. Opt. Soc. Am. A 32 1922). In this work we test this sparsity assisted phase retrieval method with experimental single shot Fourier transform intensity data frames corresponding to phase objects displayed on a spatial light modulator. The standard iterative phase retrieval algorithms are combined with an image sparsity based penalty in an adaptive manner. Illustrations for both binary and continuous phase objects are provided. It is observed that image sparsity constraint has an important role to play in obtaining meaningful phase recovery without encountering the well-known stagnation problems. The results are valuable for enabling single shot coherent diffraction imaging of phase objects for applications involving illumination wavelengths over a wide range of electromagnetic spectrum.

Thermal re-ignition processes of switching arcs with various gas-blast using voltage application highly controlled by powersemiconductors

NASA Astrophysics Data System (ADS)

Nakano, Tomoyuki; Tanaka, Yasunori; Murai, K.; Uesugi, Y.; Ishijima, T.; Tomita, K.; Suzuki, K.; Shinkai, T.

2018-05-01

This paper focuses on a fundamental experimental approach to thermal arc re-ignition processes in a variety of gas flows in a nozzle. Using power semiconductor switches in the experimental system, the arc current and the voltage applied to the arc were controlled with precise timing. With this system, residual arcs were created in decaying phase under free recovery conditions; arc re-ignition was then intentionally instigated by application of artificial voltage—i.e. quasi-transient recovery voltage—to study the arc behaviour in both decaying and re-ignition phases. In this study, SF6, CO2, N2, O2, air and Ar arcs were intentionally re-ignited by quasi-TRV application at 20 μs delay time from initiation of free recovery condition. Through these experiments, the electron density at the nozzle throat was measured using a laser Thomson scattering method together with high speed video camera observation during the re-ignition process. Temporal variations in the electron density from the arc decaying to re-ignition phases were successfully obtained for each gas-blast arc at the nozzle throat. In addition, initial dielectric recovery properties of SF6, CO2, air and Ar arcs were measured under the same conditions. These data will be useful in the fundamental elucidation of thermal arc re-ignition processes.

Dynamics of spacing adjustment and recovery mechanisms of ABAC-type growth pattern in ternary eutectic systems

NASA Astrophysics Data System (ADS)

Mohagheghi, Samira; Şerefoğlu, Melis

2017-07-01

In directionally solidified 2D samples at ternary eutectic compositions, the stable three-phase pattern is established to be lamellar structure with ABAC stacking, where A, B, and C are crystalline phases. Beyond the stability limits of the ABAC pattern, the system uses various spacing adjustment mechanisms to revert to the stable regime. In this study, the dynamics of spacing adjustment and recovery mechanisms of isotropic ABAC patterns were investigated using three-phase In-Bi-Sn alloy. Unidirectional solidification experiments were performed on 23.0 and 62.7 μm-thick samples, where solidification front was monitored in real-time from both sides of the sample using a particular microscopy system. At these thicknesses, the pattern was found to be 2D during steady-state growth, i.e. both top and bottom microstructures were the same. However, during spacing adjustment and recovery mechanisms, 3D features were observed. Dynamics of two major instabilities, lamellae branching and elimination, were quantified. After these instabilities, two key ABAC pattern recovery mechanisms, namely, phase invasion and phase exchange processes, were identified and analyzed. After elimination, ABAC pattern is recovered by either continuous eliminations of all phases or by phase exchange. After branching, the recovery mechanisms are established to be phase invasion and phase exchange.

Language features in the acute phase of poststroke severe aphasia could predict the outcome.

PubMed

Glize, Bertrand; Villain, Marie; Richert, Laura; Vellay, Maeva; de Gabory, Isabelle; Mazaux, Jean-Michel; Dehail, Patrick; Sibon, Igor; Laganaro, Marina; Joseph, Pierre-Alain

2017-04-01

Aphasia recovery remains difficult to predict initially in particular for the most severe cases. The features of impaired verbal communication which are the basis for cognitive-linguistic diagnosis and treatment could be part of prediction of recovery from aphasia. This study investigated whether some components of language screening in the acute phase of stroke are reliable prognostic factors for language recovery in the post-acute phase. Monocentric prospective study. University hospital stroke unit. Eighty-six patients aged between 21 and 92 years (mean=67.4, SD=15.3) were admitted after a first left hemisphere stroke with aphasia and were consecutively included. Language assessment was performed in the acute phase and 3 months post-stroke with the LAnguage Screening Test (LAST) and the Aphasia Severity Rating Scale (ASRS) of the Boston Diagnostic Aphasia Examination (BDAE). Severe aphasia was defined as ASRS<3. Good recovery was defined as an ASRS≥4. Language scores and other potential predictors of recovery were analysed by comparing groups of patients with good versus poor recovery and as predictors of change with multiple regression approaches. LAST Total score as well as all the individual items of LAST, NIHSS and ASRS measured in the acute phase significantly differentiated good and poor recovery from aphasia at three months for all aphasic patients and for the most severe cases. In multivariable analyses the repetition score of LAST at the acute phase was significantly associated with the delta of ASRS between the acute phase and 3 months after the stroke reflecting changes in symptom severity. For patients with initial severe aphasia, word repetition from a language screening task seems to be a more relevant predictor of recovery than initial severity to enrich the prognosis of poststroke aphasia recovery three month after a stroke. These findings show the importance of phonological perception and production as well as speech motor components in the recovery of language. These linguistic aspects of the assessment seem more relevant than severity for prediction in the acute phase. These findings could improve aphasia management pathway for people with severe aphasia and their families and minimize the evidence-practice gap for speech pathologists.

Known plaintext attack on double random phase encoding using fingerprint as key and a method for avoiding the attack.

PubMed

Tashima, Hideaki; Takeda, Masafumi; Suzuki, Hiroyuki; Obi, Takashi; Yamaguchi, Masahiro; Ohyama, Nagaaki

2010-06-21

We have shown that the application of double random phase encoding (DRPE) to biometrics enables the use of biometrics as cipher keys for binary data encryption. However, DRPE is reported to be vulnerable to known-plaintext attacks (KPAs) using a phase recovery algorithm. In this study, we investigated the vulnerability of DRPE using fingerprints as cipher keys to the KPAs. By means of computational experiments, we estimated the encryption key and restored the fingerprint image using the estimated key. Further, we propose a method for avoiding the KPA on the DRPE that employs the phase retrieval algorithm. The proposed method makes the amplitude component of the encrypted image constant in order to prevent the amplitude component of the encrypted image from being used as a clue for phase retrieval. Computational experiments showed that the proposed method not only avoids revealing the cipher key and the fingerprint but also serves as a sufficiently accurate verification system.

Psychological Interventions for Vaccine Injections in Young Children 0 to 3 Years

PubMed Central

Pillai Riddell, Rebecca; Taddio, Anna; McMurtry, C. Meghan; Chambers, Christine; Shah, Vibhuti; Noel, Melanie

2015-01-01

Background: This systematic review evaluated the effectiveness of distraction for reducing infant distress during vaccinations in young children aged 0 to 3 years. Design/Methods: Database searches identified relevant randomized and quasi-randomized controlled trials. Three separate clinical questions related to variants of the psychological strategy of distraction (directed video; directed toy; nondirected toy) were pursued. Distress was identified as the critical outcome to assess the benefits of distraction and extracted from relevant trials. Distress was analyzed by phase of procedure (distress preprocedure; distress acute; distress recovery; idiosyncratic phases based on some or all of the 3 aforementioned phases). Results: Ten studies were included in the review. Significant results are presented herein. For directed video distraction, moderate quality evidence suggested that distress was lowered in the treatment group standardized mean difference (SMD −0.68 lower [95% confidence interval (CI), −1.04 to −0.32]) for the acute+recovery phase as well as the preprocedure phase (SMD −0.49 lower [95% CI, −7.6 to −0.22]). For directed toy distraction, the analysis of low-quality evidence for a combined preprocedure+acute+recovery phase of distress (analysis n=81), suggested that distress was lowered in the treatment group (SMD −0.47 lower [95% CI, −0.91 to −0.02]). An effect for nondirected toy distraction was also seen, analyzing very–low-quality evidence, for the acute distress phase (n=290; SMD −0.93 lower [95% CI, −1.86 to 0.00]). Conclusion: Generally low-quality to very–low-quality evidence suggests that there may be an effect of directed (toy and video) and nondirected toy distraction for children aged 0 to 3 years, for certain phases of the vaccination. PMID:26201014

A quantitative headspace-solid-phase microextraction-gas chromatography-flame ionization detector method to analyze short chain free fatty acids in rat feces.

PubMed

Fiorini, Dennis; Boarelli, Maria Chiara; Gabbianelli, Rosita; Ballini, Roberto; Pacetti, Deborah

2016-09-01

This study sought to develop and validate a quantitative method to analyze short chain free fatty acids (SCFAs) in rat feces by solid-phase microextraction and gas chromatography (SPME-GC) using the salt mixture ammonium sulfate and sodium dihydrogen phosphate as salting out agent. Conditioning and extraction time, linearity, limits of detection and quantification, repeatability, and recovery were evaluated. The proposed method allows quantification with improved sensitivity as compared with other methods exploiting SPME-GC. The method has been applied to analyze rat fecal samples, quantifying acetic, propionic, isobutyric, butyric, isopentanoic, pentanoic, and hexanoic acids. Copyright © 2016 Elsevier Inc. All rights reserved.

Modelling mortality and discharge of hospitalized stroke patients using a phase-type recovery model.

PubMed

Jones, Bruce; McClean, Sally; Stanford, David

2018-05-01

We model the length of in-patient hospital stays due to stroke and the mode of discharge using a phase-type stroke recovery model. The model allows for three different types of stroke: haemorrhagic (the most severe, caused by ruptured blood vessels that cause brain bleeding), cerebral infarction (less severe, caused by blood clots) and transient ischemic attack or TIA (the least severe, a mini-stroke caused by a temporary blood clot). A four-phase recovery process is used, where the initial phase depends on the type of stroke, and transition from one phase to the next depends on the age of the patient. There are three differing modes of absorption for this phase-type model: from a typical recovery phase, a patient may die (mode 1), be transferred to a nursing home (mode 2) or be discharged to the individual's usual residence (mode 3). The first recovery phase is characterized by a very high rate of mortality and very low rates of discharge by the other two modes. The next two recovery phases have progressively lower mortality rates and higher mode 2 and 3 discharge rates. The fourth recovery phase is visited only by those who experience a very mild TIA, and they are discharged to home after a short stay. The novelty of our approach to phase representation is two-fold: first, it aligns the phases with labelled diagnosis states, representing stages of illness severity; second, the model allows us to obtain expressions for Key Performance Indicators that are of use to healthcare professionals. This allows us to use a backward estimation process where we leverage the fact that we know the phase of admission (the diagnosis), but not which phases are subsequently entered or when this happens; this strategy improves both computational efficiency and accuracy. The model has clear practical value as it yields length of stay distributions by age and type of stroke, which are useful in resource planning. Also, inclusion of the three modes of discharge permits analyses of outcomes.

Determination of steroid hormones and related compounds in filtered and unfiltered water by solid-phase extraction, derivatization, and gas chromatography with tandem mass spectrometry

USGS Publications Warehouse

Foreman, William T.; Gray, James L.; ReVello, Rhiannon C.; Lindley, Chris E.; Losche, Scott A.; Barber, Larry B.

2012-01-01

A new analytical method has been developed and implemented at the U.S. Geological Survey National Water Quality Laboratory that determines a suite of 20 steroid hormones and related compounds in filtered water (using laboratory schedule 2434) and in unfiltered water (using laboratory schedule 4434). This report documents the procedures and initial performance data for the method and provides guidance on application of the method and considerations of data quality in relation to data interpretation. The analytical method determines 6 natural and 3 synthetic estrogen compounds, 6 natural androgens, 1 natural and 1 synthetic progestin compound, and 2 sterols: cholesterol and 3--coprostanol. These two sterols have limited biological activity but typically are abundant in wastewater effluents and serve as useful tracers. Bisphenol A, an industrial chemical used primarily to produce polycarbonate plastic and epoxy resins and that has been shown to have estrogenic activity, also is determined by the method. A technique referred to as isotope-dilution quantification is used to improve quantitative accuracy by accounting for sample-specific procedural losses in the determined analyte concentration. Briefly, deuterium- or carbon-13-labeled isotope-dilution standards (IDSs), all of which are direct or chemically similar isotopic analogs of the method analytes, are added to all environmental and quality-control and quality-assurance samples before extraction. Method analytes and IDS compounds are isolated from filtered or unfiltered water by solid-phase extraction onto an octadecylsilyl disk, overlain with a graded glass-fiber filter to facilitate extraction of unfiltered sample matrices. The disks are eluted with methanol, and the extract is evaporated to dryness, reconstituted in solvent, passed through a Florisil solid-phase extraction column to remove polar organic interferences, and again evaporated to dryness in a reaction vial. The method compounds are reacted with activated -methyl--trimethylsilyl trifluoroacetamide at 65 degrees Celsius for 1 hour to form trimethylsilyl or trimethylsilyl-enol ether derivatives that are more amenable to gas chromatographic separation than the underivatized compounds. Analysis is carried out by gas chromatography with tandem mass spectrometry using calibration standards that are derivatized concurrently with the sample extracts. Analyte concentrations are quantified relative to specific IDS compounds in the sample, which directly compensate for procedural losses (incomplete recovery) in the determined and reported analyte concentrations. Thus, reported analyte concentrations (or analyte recoveries for spiked samples) are corrected based on recovery of the corresponding IDS compound during the quantification process. Recovery for each IDS compound is reported for each sample and represents an absolute recovery in a manner comparable to surrogate recoveries for other organic methods used by the National Water Quality Laboratory. Thus, IDS recoveries provide a useful tool for evaluating sample-specific analytical performance from an absolute mass recovery standpoint. IDS absolute recovery will differ and typically be lower than the corresponding analyte’s method recovery in spiked samples. However, additional correction of reported analyte concentrations is unnecessary and inappropriate because the analyte concentration (or recovery) already is compensated for by the isotope-dilution quantification procedure. Method analytes were spiked at 10 and 100 nanograms per liter (ng/L) for most analytes (10 times greater spike levels were used for bisphenol A and 100 times greater spike levels were used for 3--coprostanol and cholesterol) into the following validation-sample matrices: reagent water, wastewater-affected surface water, a secondary-treated wastewater effluent, and a primary (no biological treatment) wastewater effluent. Overall method recovery for all analytes in these matrices averaged 100 percent, with overall relative standard deviation of 28 percent. Mean recoveries of the 20 individual analytes for spiked reagent-water samples prepared along with field samples and analyzed in 2009–2010 ranged from 84–104 percent, with relative standard deviations of 6–36 percent. Concentrations for two analytes, equilin and progesterone, are reported as estimated because these analytes had excessive bias or variability, or both. Additional database coding is applied to other reported analyte data as needed, based on sample-specific IDS recovery performance. Detection levels were derived statistically by fortifying reagent water at six different levels (0.1 to 4 ng/L) and range from about 0.4 to 4 ng/L for 16 analytes. Interim reporting levels applied to analytes in this report range from 0.8 to 8 ng/L. Bisphenol A and the sterols (cholesterol and 3-beta-coprostanol) were consistently detected in laboratory and field blanks. The minimum reporting levels were set at 100 ng/L for bisphenol A and at 200 ng/L for the two sterols to prevent any bias associated with the presence of these compounds in the blanks. A minimum reporting level of 2 ng/L was set for 11-ketotestosterone to minimize false positive risk from an interfering siloxane compound emanating as chromatographic-column bleed, from vial septum material, or from other sources at no more than 1 ng/L.

Virtual Reality Cue Refusal Video Game for Alcohol and Cigarette Recovery Support: Summative Study

PubMed Central

Rossie, Karen; Stokes, Katie; Tallman, Christina; Tanner, Bradley

2018-01-01

Background New technologies such as virtual reality, augmented reality, and video games hold promise to support and enhance individuals in addiction treatment and recovery. Quitting or decreasing cigarette or alcohol use can lead to significant health improvements for individuals, decreasing heart disease risk and cancer risks (for both nicotine and alcohol use), among others. However, remaining in recovery from use is a significant challenge for most individuals. Objective We developed and assessed the Take Control game, a partially immersive Kinect for Windows platform game that allows users to counter substance cues through active movements (hitting, kicking, etc). Methods Formative analysis during phase I and phase II guided development. We conducted a small wait-list control trial using a quasi-random sampling technique (systematic) with 61 participants in recovery from addiction to alcohol or tobacco. Participants used the game 3 times and reported on substance use, cravings, satisfaction with the game experience, self-efficacy related to recovery, and side effects from exposure to a virtual reality intervention and substance cues. Results Participants found the game engaging and fun and felt playing the game would support recovery efforts. On average, reported substance use decreased for participants during the intervention period. Participants in recovery for alcohol use saw more benefit than those in recovery for tobacco use, with a statistically significant increase in self-efficacy, attitude, and behavior during the intervention. Side effects from the use of a virtual reality intervention were minor and decreased over time; cravings and side effects also decreased during the study. Conclusions The preliminary results suggest the intervention holds promise as an adjunct to standard treatment for those in recovery, particularly from alcohol use. PMID:29661748

Protocols for collection of streamflow, water-quality, streambed-sediment, periphyton, macroinvertebrate, fish, and habitat data to describe stream quality for the Hydrobiological Monitoring Program, Equus Beds Aquifer Storage and Recovery Program, city of Wichita, Kansas

USGS Publications Warehouse

Stone, Mandy L.; Rasmussen, Teresa J.; Bennett, Trudy J.; Poulton, Barry C.; Ziegler, Andrew C.

2012-01-01

The city of Wichita, Kansas uses the Equus Beds aquifer, one of two sources, for municipal water supply. To meet future water needs, plans for artificial recharge of the aquifer have been implemented in several phases. Phase I of the Equus Beds Aquifer Storage and Recovery (ASR) Program began with injection of water from the Little Arkansas River into the aquifer for storage and subsequent recovery in 2006. Construction of a river intake structure and surface-water treatment plant began as implementation of Phase II of the Equus Beds ASR Program in 2010. An important aspect of the ASR Program is the monitoring of water quality and the effects of recharge activities on stream conditions. Physical, chemical, and biological data provide the basis for an integrated assessment of stream quality. This report describes protocols for collecting streamflow, water-quality, streambed-sediment, periphyton, macroinvertebrate, fish, and habitat data as part of the city of Wichita's hydrobiological monitoring program (HBMP). Following consistent and reliable methods for data collection and processing is imperative for the long-term success of the monitoring program.

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.

Metabolic changes in concussed American football players during the acute and chronic post-injury phases

PubMed Central

2011-01-01

Background Despite negative neuroimaging findings many athletes display neurophysiological alterations and post-concussion symptoms that may be attributable to neurometabolic alterations. Methods The present study investigated the effects of sports concussion on brain metabolism using 1H-MR Spectroscopy by comparing a group of 10 non-concussed athletes with a group of 10 concussed athletes of the same age (mean: 22.5 years) and education (mean: 16 years) within both the acute and chronic post-injury phases. All athletes were scanned 1-6 days post-concussion and again 6-months later in a 3T Siemens MRI. Results Concussed athletes demonstrated neurometabolic impairment in prefrontal and motor (M1) cortices in the acute phase where NAA:Cr levels remained depressed relative to controls. There was some recovery observed in the chronic phase where Glu:Cr levels returned to those of control athletes; however, there was a pathological increase of m-I:Cr levels in M1 that was only present in the chronic phase. Conclusions These results confirm cortical neurometabolic changes in the acute post-concussion phase as well as recovery and continued metabolic abnormalities in the chronic phase. The results indicate that complex pathophysiological processes differ depending on the post-injury phase and the neurometabolite in question. PMID:21861906

Effects of active recovery on autonomic and haemodynamic responses after aerobic exercise.

PubMed

Soares, Antonio H G; Oliveira, Tiago P; Cavalcante, Bruno R; Farah, Breno Q; Lima, Aluísio H R A; Cucato, Gabriel G; Cardoso, Crivaldo G; Ritti-Dias, Raphael M

2017-01-01

The aim of this study was to examine the effect of active recovery on autonomic and haemodynamic responses after exercise in healthy adults. Nineteen healthy young male individuals underwent two experimental sessions: exercise with active recovery (AR) and exercise with passive recovery (PR). The exercise sessions comprised three phases: warm-up (5 min), exercise phase (cycle ergometer, 30 min, intensity between 60 and 70% of the heart rate reserve) and recovery (5 min). In the AR, the subjects remained cycling in the recovery phase at intensity between 30% and 35% of heart rate reserve, while in the PR, the subjects stopped the exercise after finishing the exercise phase. Blood pressure and heart rate were measured before and over the 30 min after the interventions. There were no differences for systolic and diastolic blood pressures, heart rate and rate pressure product between active and passive recovery sessions. Also, all heart rate variability parameters changed similarly after exercise with passive or active recovery sessions. In summary, exercise with active recovery does not affect the autonomic and haemodynamic responses after moderate-intensity aerobic exercise in healthy young male individuals. © 2015 Scandinavian Society of Clinical Physiology and Nuclear Medicine. Published by John Wiley & Sons Ltd.

Hydrophilic interaction liquid chromatography-solid phase extraction directly combined with protein precipitation for the determination of triptorelin in plasma.

PubMed

Wang, Jixia; Kong, Song; Yan, Jingyu; Jin, Gaowa; Guo, Zhimou; Shen, Aijin; Xu, Junyan; Zhang, Xiuli; Zou, Lijuan; Liang, Xinmiao

2014-06-01

Peptide drugs play a critical role in therapeutic treatment. However, as the complexity of plasma, determination of peptide drugs using liquid chromatography-tandem mass spectrometry (LC-MS/MS) is a daunting task. To solve this problem, hydrophilic interaction liquid chromatography-solid phase extraction (HILIC-SPE) directly combined with protein precipitation (PPT) was developed for the selective extraction of triptorelin from plasma. The extracts were analyzed by reversed-phase liquid chromatography (RPLC). Proteins, phospholipids and highly polar interferences could be removed from plasma by the efficient combination of PPT, HILIC-SPE and RPLC-MS/MS. This method was evaluated by matrix effect, recovery and process efficiency at different concentration levels (50, 500 and 5,000 ng/mL) of triptorelin. Furthermore, the performance of HILIC-SPE was compared with that of reversed-phase C18 SPE and hydrophilic lipophilic balance (Oasis HLB) SPE. Among them, HILIC-SPE provided the minimum matrix effect (ranging from 96.02% to 103.41%), the maximum recovery (ranging from 80.68% to 90.54%) and the satisfactory process efficiency (ranging from 82.83% to 92.95%). The validated method was successfully applied to determine triptorelin in rat plasma. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Analysis of trace levels of sulfonamide and tetracycline antimicrobials in groundwater and surface water using solid-phase extraction and liquid chromatography/mass spectrometry

USGS Publications Warehouse

Lindsey, M.E.; Meyer, M.; Thurman, E.M.

2001-01-01

A method has been developed for the trace analysis of two classes of antimicrobials consisting of six sulfonamides (SAs) and five tetracyclines (TCs), which commonly are used for veterinary purposes and agricultural feed additives and are suspected to leach into ground and surface water. The method used solid-phase extraction and liquid chromatography/mass spectrometry (LC/MS) with positive ion electrospray. The unique combination of a metal chelation agent (Na2EDTA) with a macroporous copolymer resulted in quantitative recoveries by solid-phase extraction (mean recovery, 98 ?? 12%) at submicrogram-per-liter concentrations. An ammonium formate/formic acid buffer with a methanol/water gradient was used to separate the antimicrobials and to optimize the signal intensity. Mass spectral fragmentation and ionization characteristics were determined for each class of compounds for unequivocal identification. For all SAs, a characteristic m/z 156 ion representing the sulfanilyl fragment was identified. TCs exhibited neutral losses of 17 amu resulting from the loss of ammonia and 35 amu from the subsequent loss of water. Unusual matrix effects were seen only for TCs in this first survey of groundwater and surface water samples from sites around the United States, requiring that TCs be quantitated using the method of standard additions.

Ion chromatographic methods for the detection of starch hydrolysis products in ruminal digesta.

PubMed

Barsuhn, K; Kotarski, S F

1991-06-21

Dionex high-performance ion chromatographic methods were evaluated for separation and quantitation of plant sugars and starch digestion products in the ruminal digesta of cattle. Mono- and disaccharides were eluted from a Dionex CarboPac PA1 column with sodium hydroxide used isocratically or as a pH gradient. Maltooligosaccharides which had a degree of polymerization (DP) less than 30 glucose residues were eluted in 60 min by a sodium hydroxide eluent containing a sodium acetate gradient. Carbohydrates were detected amperometrically. Responses were linear (r2 greater than 0.99) for glucose, disaccharides and maltooligosaccharides (DP less than 8). Precipitation and solid-phase extraction methods were evaluated for clean-up of samples of feedstuffs, ruminal contents, and bacterial culture fluids. Perchloric acid precipitation hydrolyzed sucrose but did not affect recoveries of cellobiose, isomaltose or maltose. Ethanol in concentrations of 79 and 86% precipitated maltooligosaccharides having chain lengths larger than 14 and 9 glucose residues, respectively. Maltooligosaccharide recoveries from solid-phase extraction columns varied with maltooligosaccharide size and column packing. Recoveries were greater than 94% for short chains (DP less than 6) eluted from phenyl-substituted columns and variable for all oligosaccharides eluted from C18 columns. Applications of these methods are presented and include: (1) detection of sugars in ruminant feed, (2) monitoring changes in ruminal sugars after feeding and (3) monitoring changes in extracellular sugars and oligosaccharides in the culture fluids of the ruminal bacterium, Bacteroides ruminicola.

Extraction and Liquid Chromatography-Tandem Mass Spectrometry Detection of 3-Monochloropropanediol Esters and Glycidyl Esters in Infant Formula.

PubMed

Leigh, Jessica K; MacMahon, Shaun

2016-12-14

A method was developed for the extraction of fatty acid esters of 3-chloro-1,2-propanediol (3-MCPD) and glycidol from infant formula, followed by quantitative analysis of the extracts using liquid chromatography-tandem mass spectrometry (LC-MS/MS). These process-induced chemical contaminants are found in refined vegetable oils, and studies have shown that they are potentially carcinogenic and/or genotoxic, making their presence in edible oils (and processed foods containing these oils) a potential health risk. The extraction procedure involves a liquid-liquid extraction, where powdered infant formula is dissolved in water and extracted with ethyl acetate. Following shaking, centrifugation, and drying of the organic phase, the resulting fat extract is cleaned-up using solid-phase extraction and analyzed by LC-MS/MS. Method performance was confirmed by verifying the percent recovery of each 3-MCPD and glycidyl ester in a homemade powdered infant formula reference material. Average ester recoveries in the reference material ranged from 84.9 to 109.0% (0.6-9.5% RSD). The method was also validated by fortifying three varieties of commercial infant formulas with a 3-MCPD and glycidyl ester solution. Average recoveries of the esters across all concentrations and varieties of infant formula ranged from 88.7 to 107.5% (1.0-9.5% RSD). Based on the validation results, this method is suitable for producing 3-MCPD and glycidyl ester occurrence data in all commercially available varieties of infant formula.

Fitting a single-phase model to the post-exercise changes in heart rate and oxygen uptake.

PubMed

Stupnicki, R; Gabryś, T; Szmatlan-Gabryś, U; Tomaszewski, P

2010-01-01

The kinetics of post-exercise heart rate (HR) and oxygen consumption (EPOC) was studied in 10 elite cyclists subjected to four laboratory cycle ergometer maximal exercises lasting 30, 90, 180 or 360 s. Heart rate and oxygen uptake (VO2) were recorded over a period of 6 min after the exercise. By applying the logit transformation to the recorded variables and relating them to the decimal logarithm of the recovery time, uniform single-phase courses of changes were shown for both variables in all subjects and exercises. This enabled computing half-recovery times (t(1/2)) for both variables. Half-time for VO2 negatively correlated with square root of exercise duration (within-subject r = -0.629, p < 0.001), the total post-exercise oxygen uptake till t(1/2) was thus constant irrespectively of exercise intensity. The method is simple and enables reliable comparisons of various modes of exercise with respect to the rate of recovery.

Development of sensitive determination method for fungicides from environmental water samples with Titanate nanotube array micro-solid phase extraction prior to high performance liquid chromatography.

PubMed

Huang, Yunrui; Zhou, Qingxiang; Xie, Guohong

2013-01-01

Fungicides have been widely used throughout the world, and the resulted pollution has absorbed great attention in recent years. Present study described an effective measurement technique for fungicides including thiram, metalaxyl, diethofencarb, myclobutanil and tebuconazole in environmental water samples. A micro-solid phase extraction (μSPE) was developed utilizing ordered TiO(2) nanotube array for determination of target fungicides prior to a high performance liquid chromatography (HPLC). The experimental results indicated that TiO(2) nanotube arrays demonstrated excellent merits on the preconcentration of fungicides, and excellent linear relationship between peak area and the concentration of fungicides was obtained in the range of 0.1-50 μg L(-1). The detection limits for the targeted fungicides were in the range of 0.016-0.086 μg L(-1) (S/N=3). Four real environmental water samples were used to validate the applicability of the proposed method, and good spiked recoveries in the range of 73.9-114% were achieved. A comparison of present method with conventional solid phase extraction was made and the results exhibited that proposed method resulted in better recoveries. The results demonstrated that this μ-SPE technique was a viable alternative for the analysis of fungicides in complex samples. Copyright © 2012 Elsevier Ltd. All rights reserved.

[Determination of 23 antibiotics and 3 β-agonists in livestock drinking water by ultra performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction].

PubMed

Shi, Ao

2016-02-01

A method has been developed for the simultaneous determination of 23 antibiotics (four categories) and 3 β-agonists in livestock drinking water using solid-phase extraction and ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI MS/MS). The samples were adjusted pH to 5. 0, added Na2EDTA, enriched and cleaned-up by an HLB solid-phase extraction cartridge. The target compounds were confirmed and quantified by UPLC-ESI MS/MS with external standard method for the anti- biotics and internal standard method for the β-agonists. The recoveries were assessed by using lab tap water as matrix. The average recoveries of the 23 antibiotics and the 3 β-agonists were in the range of 50. 7%-104. 6% and the relative standard deviations (RSDs) were 2. 6%-8. 8% (n= 3). Under the optimal conditions, the calibration curves of the 23 antibiotics and the 3 β-agonists showed good linearity with the correlation coefficients better than 0. 994. The limits of detection (LODs, S/N≥3) ranged from 0. 01-0. 20 ng/L. The developed method was applied to analyze the livestock drinking waters in 36 Beijing intensive livestock farms. The results showed that some antibiotics were detected.

Determination of catechins and catechin gallates in tissues by liquid chromatography with coulometric array detection and selective solid phase extraction.

PubMed

Chu, Kai On; Wang, Chi Chiu; Chu, Ching Yan; Rogers, Michael Scott; Choy, Kwong Wai; Pang, Chi Pui

2004-10-25

Catechins levels in organ tissues, particularly liver, determined by published methods are unexpectedly low, probably due to the release of oxidative enzymes, metal ions and reactive metabolites from tissue cells during homogenization and to the pro-oxidant effects of ascorbic acid during sample processing in the presence of metal ions. We describe a new method for simultaneous analysis of eight catechins in tissue: (+)-catechin (C), (-)-epicatechin (EC), (-)-gallocatechin (GC), (-)-epigallocatechin (EGC), (-)-catechin gallate (CG), (-)-epicatechin gallate (ECG), (-)-gallocatechin gallate (GCG) and (-)-epigallocatechin gallate (EGCG) (Fig. 1). The new extraction procedure utilized a methanol/ethylacetate/dithionite (2:1:3) mixture during homogenization for simultaneous enzyme precipitation and antioxidant protection. Selective solid phase extraction was used to remove most interfering bio-matrices. Reversed phase HPLC with CoulArray detection was used to determine the eight catechins simultaneously within 25 min. Good linearity (>0.9922) was obtained in the range 20-4000 ng/g. The coefficients of variance (CV) were less than 5%. Absolute recovery ranged from 62 to 96%, accuracy 92.5 +/- 4.5 to 104.9 +/- 6%. The detection limit was 5 ng/g. This method is capable for determining catechins in rat tissues of liver, brain, spleen, and kidney. The method is robust, reproducible, with high recovery, and has been validated for both in vitro and in vivo sample analysis.

A Validated Stability Indicating RP-HPLC Method for the Determination of Emtricitabine, Tenofovir Disoproxil Fumarate, Elvitegravir and Cobicistat in Pharmaceutical Dosage Form

PubMed Central

Runja, Chinnalalaiah; Ravi Kumar, Pigili; Avanapu, Srinivasa Rao

2016-01-01

A new simple, rapid stability indicating assay method has been developed and validated for the determination of emtricitabine, tenofovir disoproxil fumarate, elvitegravir and cobicistat using reverse-phase high-performance liquid chromatography in their pharmaceutical dosage form. The chromatographic separation was performed on an ODS column (250 × 4.6 mm, 5 µm) using mobile phase A (potassium dihydrogen orthophosphate, pH adjusted to 2.5) and mobile phase B (acetonitrile) in the ratio of 55:45% v/v at a flow rate of 1 mL/min. The analytes were detected at 250 nm. The method was found to be linear in the concentration range of 2–12 µg/mL for EMT, 3–18 µg/mL for TNDF, 1.5–9 µg/mL for ELV and COB, with the coefficient value (R2) of >0.9990. The accuracy was measured via recovery studies and found to be acceptable, and the percentage recoveries were found in the range of 99.93–100.08 ± 0.5%. Forced degradation studies were also conducted, and the drugs were subjected to various stress conditions such as acid hydrolysis, base hydrolysis, oxidative, photolytic and thermal degradation. The proposed method was successfully validated and applied for the quantitative estimation of these drugs in both bulk and tablet dosage forms. PMID:26865655

Close-form expression of one-tap normalized LMS carrier phase recovery in optical communication systems

NASA Astrophysics Data System (ADS)

Xu, Tianhua; Jacobsen, Gunnar; Popov, Sergei; Li, Jie; Liu, Tiegen; Zhang, Yimo

2016-10-01

The performance of long-haul high speed coherent optical fiber communication systems is significantly degraded by the laser phase noise and the equalization enhanced phase noise (EEPN). In this paper, the analysis of the one-tap normalized least-mean-square (LMS) carrier phase recovery (CPR) is carried out and the close-form expression is investigated for quadrature phase shift keying (QPSK) coherent optical fiber communication systems, in compensating both laser phase noise and equalization enhanced phase noise. Numerical simulations have also been implemented to verify the theoretical analysis. It is found that the one-tap normalized least-mean-square algorithm gives the same analytical expression for predicting CPR bit-error-rate (BER) floors as the traditional differential carrier phase recovery, when both the laser phase noise and the equalization enhanced phase noise are taken into account.

Claus sulfur recovery unit startups

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

Parnell, D.C.

1973-08-01

Because of the recent emphasis on reducing sulfur emissions to the atmosphere, Claus-type sulfur recovery units are becoming more prevalent throughout the industry. Many plants, including refinery, chemical, and natural gasoline units, are being required to install Claus sulfur recovery facilities to meet pollution requirements. Although Claus units in some cases cannot alone meet the most rigid air pollution codes currently being enforced, they are still the most economical and practical method for recovering about 94 to 97% of the sulfur from hydrogen sulfide rich gases. For best operation and longer service life, proper startup and shutdown procedures for thesemore » sulfur recovery units should be followed. On all startups and shutdowns, these units require considerable operator attention; improper operation during these critical phases can affect overall plant efficiency.« less

Analysis of imazaquin in soybeans by solid-phase extraction and high-performance liquid chromatography.

PubMed

Guo, C; Hu, J-Y; Chen, X-Y; Li, J-Z

2008-02-01

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.

Development and validation of reversed phase high performance liquid chromatography method for determination of dexpanthenol in pharmaceutical formulations.

PubMed

Kulikov, A U; Zinchenko, A A

2007-02-19

This paper describes the validation of an isocratic HPLC method for the assay of dexpanthenol in aerosol and gel. The method employs the Vydac Proteins C4 column with a mobile phase of aqueous solution of trifluoroacetic acid and UV detection at 206 nm. A linear response (r>0.9999) was observed in the range of 13.0-130 microg mL(-1). The method shows good recoveries and intra and inter-day relative standard deviations were less than 1.0%. Validation parameters as specificity, accuracy and robustness were also determined. The method can be used for dexpanthenol assay of panthenol aerosol and gel with dexpanthenol as the method separates dexpanthenol from aerosol or gel excipients.

Coarse-grained simulation of molecular mechanisms of recovery in thermally activated shape-memory polymers

NASA Astrophysics Data System (ADS)

Abberton, Brendan C.; Liu, Wing Kam; Keten, Sinan

2013-12-01

Thermally actuated shape-memory polymers (SMPs) are capable of being programmed into a temporary shape and then recovering their permanent reference shape upon exposure to heat, which facilitates a phase transition that allows dramatic increase in molecular mobility. Experimental, analytical, and computational studies have established empirical relations of the thermomechanical behavior of SMPs that have been instrumental in device design. However, the underlying mechanisms of the recovery behavior and dependence on polymer microstructure remain to be fully understood for copolymer systems. This presents an opportunity for bottom-up studies through molecular modeling; however, the limited time-scales of atomistic simulations prohibit the study of key performance metrics pertaining to recovery. In order to elucidate the effects of phase fraction, recovery temperature, and deformation temperature on shape recovery, here we investigate the shape-memory behavior in a copolymer model with coarse-grained potentials using a two-phase molecular model that reproduces physical crosslinking. Our simulation protocol allows observation of upwards of 90% strain recovery in some cases, at time-scales that are on the order of the timescale of the relevant relaxation mechanism (stress relaxation in the unentangled soft-phase). Partial disintegration of the glassy phase during mechanical deformation is found to contribute to irrecoverable strain. Temperature dependence of the recovery indicates nearly full elastic recovery above the trigger temperature, which is near the glass-transition temperature of the rubbery switching matrix. We find that the trigger temperature is also directly correlated with the deformation temperature, indicating that deformation temperature influences the recovery temperatures required to obtain a given amount of shape recovery, until the plateau regions overlap above the transition region. Increasing the fraction of glassy phase results in higher strain recovery at low to intermediate temperatures, a widening of the transition region, and an eventual crossover at high temperatures. Our results corroborate experimental findings on shape-memory behavior and provide new insight into factors governing deformation recovery that can be leveraged in biomaterials design. The established computational methodology can be extended in straightforward ways to investigate the effects of monomer chemistry, low-molecular-weight solvents, physical and chemical crosslinking, different phase-separation morphologies, and more complicated mechanical deformation toward predictive modeling capabilities for stimuli-responsive polymers.

Understanding the Phases of Recovery from Serious Mental Illness: The Roles of Referent and Expert Power in a Mutual-Help Setting

ERIC Educational Resources Information Center

Beeble, Marisa L.; Salem, Deborah A.

2009-01-01

This study explored an approach to studying recovery that is sensitive to the multiphase and contextual nature of the recovery process. The authors focused on the experience of recovery in a mutual-help group, Schizophrenics Anonymous (SA). Prior qualitative research conducted with SA revealed that SA participants experience four phases of…

Methods of analysis and quality-assurance practices of the U.S. Geological Survey organic laboratory, Sacramento, California; determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry

USGS Publications Warehouse

Crepeau, Kathryn L.; Domagalski, Joseph L.; Kuivila, Kathryn

1994-01-01

Analytical method and quality-assurance practices were developed for a study of the fate and transport of pesticides in the Sacramento-San Joaquin Delta and the Sacramento and San Joaquin River. Water samples were filtered to remove suspended parti- culate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide, and the pesticides were eluted with three 2-milliliter aliquots of hexane:diethyl ether (1:1). The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for analytes determined per 1,500-milliliter samples ranged from 0.006 to 0.047 microgram per liter. Recoveries ranged from 47 to 89 percent for 12 pesticides in organic-free, Sacramento River and San Joaquin River water samples fortified at 0.05 and 0.26 microgram per liter. The method was modified to improve the pesticide recovery by reducing the sample volume to 1,000 milliliters. Internal standards were added to improve quantitative precision and accuracy. The analysis also was expanded to include a total of 21 pesticides. The method detection limits for 1,000-milliliter samples ranged from 0.022 to 0.129 microgram per liter. Recoveries ranged from 38 to 128 percent for 21 pesticides in organic-free, Sacramento River and San Joaquin River water samples fortified at 0.10 and 0.75 microgram per liter.

[Determination of glycyrrhizinic acid in biotransformation system by reversed-phase high performance liquid chromatography].

PubMed

Li, Hui; Lu, Dingqiang; Liu, Weimin

2004-05-01

A method for determining glycyrrhizinic acid in the biotransformation system by reversed-phase high performance liquid chromatography (RP-HPLC) was developed. The HPLC conditions were as follows: Hypersil C18 column (4.6 mm i.d. x 250 mm, 5 microm) with a mixture of methanol-water-acetic acid (70:30:1, v/v) as the mobile phase; flow rate at 1.0 mL/min; and UV detection at 254 nm. The linear range of glycyrrhizinic acid was 0.2-20 microg. The recoveries were 98%-103% with relative standard deviations between 0.16% and 1.58% (n = 3). The method is simple, rapid and accurate for determining glycyrrhizinic acid.

High performance liquid chromatographic and thin layer densitometric methods for the determination of risperidone in the presence of its degradation products in bulk powder and in tablets.

PubMed

El-Sherif, Zeinab A; El-Zeany, Badr; El-Houssini, Ola M

2005-01-04

Two reproducible stability indicating methods were developed for the determination of risperidone (RISP) in presence of its degradation products in pure form and in tablets. The first method was based on reversed phase high performance liquid chromatography (HPLC), on Lichrosorb RP C 18 column (250 mm i.d., 4 mm, 10 microm), using methanol:0.05 M potassium dihydrogen phosphate pH 7 (65:35 (v/v)) as the mobile phase at a flow rate of 1 ml min(-1) at ambient temperature. Quantification was achieved with UV detection at 280 nm over a concentration range of 25-500 microg ml(-1) with mean percentage recovery of 99.87 +/- 1.049. The method retained its accuracy in the presence of up to 90% of RISP degradation products. The second method was based on TLC separation of RISP from its degradation products followed by densitometric measurement of the intact drug spot at 280 nm. The separation was carried out on aluminum sheet of silica gel 60F254 using acetonitrile:methanol:propanol:triethanolamine (8.5:1.2:0.6:0.2 (v/v/v/v)), as the mobile phase, over a concentration range of 2-10 microg per spot and mean percentage recovery of 100.1 +/- 1.18. The two methods were simple, precise, sensitive and could be successfully applied for the determination of pure, laboratory prepared mixtures and tablets. The results obtained were compared with the manufacturer's method.

Synthesis of thermo-responsive polymers recycling aqueous two-phase systems and phase formation mechanism with partition of ε-polylysine.

PubMed

Xu, Chengning; Dong, Wenying; Wan, Junfen; Cao, Xuejun

2016-11-11

Aqueous two-phase systems (ATPS) have the potential application in bioseparation and biocatalysis engineering. In this paper, a recyclable ATPS was developed by two thermo-responsive copolymers, P VBAm and P N . Copolymer P VBAm was copolymerized using N-vinylcaprolactam, Butyl methacrylate and Acrylamide as monomers, and P N was synthesized by N-isopropylacrylamide. The lower critical solution temperature (LCST) of P VBAm and P N were 45.0°C and 33.5°C, respectively. The recoveries of both polymers could achieve over 95.0%. The phase behavior and formation mechanism of P VBAm /P N ATPS was studied. Low-field nuclear magnetic resonance (LF-NMR) was applied in the phase-forming mechanism study in ATPS. In addition, combining the analysis results of surface tension, transmission electron microscopy and dynamic light scattering, the phase-forming of the P VBAm /P N ATPS was proved. The application was performed by partition of ε-polylysine in the 2% P VBAm /2% P N (w/w) ATPS. The results demonstrated that ε-polylysine was extracted into the P N -rich phase, the maximal partition coefficient (1/K) and extraction recovery of pure ε-polylysine were 6.87 and 96.36%, respectively, and 7.41 partition coefficient and 97.85% extraction recovery for ε-polylysine fermentation broth were obtained in the presence of 50mM (NH 4 ) 2 SO 4 at room temperature. And this method can effectively remove the most impurities from fermentation broth when (NH 4 ) 2 SO 4 exists in the ATPS. It is believed that the thermo-responsive recycling ATPS has a good application prospect in the field of bio-separation. Copyright © 2016 Elsevier B.V. All rights reserved.

An On-Line Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of Perfluoroalkyl Acids in Drinking and Surface Waters

PubMed Central

Mazzoni, Michela; Rusconi, Marianna; Valsecchi, Sara; Martins, Claudia P. B.; Polesello, Stefano

2015-01-01

An UHPLC-MS/MS multiresidue method based on an on-line solid phase extraction (SPE) procedure was developed for the simultaneous determination of 9 perfluorinated carboxylates (from 4 to 12 carbon atoms) and 3 perfluorinated sulphonates (from 4 to 8 carbon atoms). This work proposes using an on-line solid phase extraction before chromatographic separation and analysis to replace traditional methods of off-line SPE before direct injection to LC-MS/MS. Manual sample preparation was reduced to sample centrifugation and acidification, thus eliminating several procedural errors and significantly reducing time-consuming and costs. Ionization suppression between target perfluorinated analytes and their coeluting SIL-IS were detected for homologues with a number of carbon atoms less than 9, but the quantitation was not affected. Total matrix effect corrected by SIL-IS, inclusive of extraction efficacy, and of ionization efficiency, ranged between −34 and +39%. The percentage of recoveries, between 76 and 134%, calculated in different matrices (tap water and rivers impacted by different pollutions) was generally satisfactory. LODs and LOQs of this on-line SPE method, which also incorporate recovery losses, ranged from 0.2 to 5.0 ng/L and from 1 to 20 ng/L, respectively. Validated on-line SPE-LC/MS/MS method has been applied in a wide survey for the determination of perfluoroalkyl acids in Italian surface and ground waters. PMID:25834752

Determination of atrazine and its major degradation products in soil pore water by solid-phase extraction, chemical derivatization, and gas chromatography/mass spectrometry

USGS Publications Warehouse

Carter, D.S.

1996-01-01

This report describes a method for the determination of atrazine, desethylatrazine, deisopropylatrazine, didealkylatrazine, and hydroxyatrazine from soil pore waters by use of solid-phase extractionfollowed by chemical derivatization and gas chromatography/mass spectrometry. The analytes are isolated from the pore-water matrix byextraction onto a graphitized carbon-black cartridge. The cartridge is dried under vacuum, and adsorbed analytes are removed by elution with ethyl acetate followed by dichloromethane/methanol (7:3, volume/volume). Water is removed from the ethyl acetate fraction on an anhydrous sodium sulfate column. The combined fractions are solvent exchanged into acetonitrile, evaporated by use of a nitrogen stream, and derivatized by use of N- methyl-N-(tert-butyldimethylsilyl)- trifluoroacetamide. The derivatized extracts are analyzed by capillary-column gaschromatography/electron-impact mass spectrometry in the scan mode. Estimated method detection limits range from 0.03 to 0.07 micrograms per liter. The mean recoveries of all analytes and surrogates determined at 0.74 to 0.82 micrograms per liter in reagent water in soil pore water were 94 percent and 98 percent, respectively. The mean recoveries of all analytes and surrogates determined at 7.4 to 8.2 micrograms per liter in reagent water and in soil pore water were 96 percent and 97 percent,respectively. Recoveries were 90 percent or higher, regardless of analyte concentration or matrix composition, for all compounds excepthydroxyatrazine, whose recoveries were slightly lower (77 percent) at the low concentration.

Stochastical analysis of surfactant-enhanced remediation of denser-than-water nonaqueous phase liquid (DNAPL)-contaminated soils.

PubMed

Zhang, Renduo; Wood, A Lynn; Enfield, Carl G; Jeong, Seung-Woo

2003-01-01

Stochastical analysis was performed to assess the effect of soil spatial variability and heterogeneity on the recovery of denser-than-water nonaqueous phase liquids (DNAPL) during the process of surfactant-enhanced remediation. UTCHEM, a three-dimensional, multicomponent, multiphase, compositional model, was used to simulate water flow and chemical transport processes in heterogeneous soils. Soil spatial variability and heterogeneity were accounted for by considering the soil permeability as a spatial random variable and a geostatistical method was used to generate random distributions of the permeability. The randomly generated permeability fields were incorporated into UTCHEM to simulate DNAPL transport in heterogeneous media and stochastical analysis was conducted based on the simulated results. From the analysis, an exponential relationship between average DNAPL recovery and soil heterogeneity (defined as the standard deviation of log of permeability) was established with a coefficient of determination (r2) of 0.991, which indicated that DNAPL recovery decreased exponentially with increasing soil heterogeneity. Temporal and spatial distributions of relative saturations in the water phase, DNAPL, and microemulsion in heterogeneous soils were compared with those in homogeneous soils and related to soil heterogeneity. Cleanup time and uncertainty to determine DNAPL distributions in heterogeneous soils were also quantified. The study would provide useful information to design strategies for the characterization and remediation of nonaqueous phase liquid-contaminated soils with spatial variability and heterogeneity.

Syringe-cartridge solid-phase extraction method for patulin in apple juice.

PubMed

Eisele, Thomas A; Gibson, Midori Z

2003-01-01

A syringe-cartridge solid-phase extraction (SPE) method was developed for determination of patulin in apple juice. A 2.5 mL portion of test sample was passed through a conditioned macroporous SPE cartridge and washed with 2 mL 1% sodium bicarbonate followed by 2 mL 1% acetic acid. Patulin was eluted with 1 mL 10% ethyl acetate in ethyl ether and determined by reversed-phase liquid chromatography using a mobile phase consisting of 81% acetonitrile, 9% water, and 10% 0.05M potassium phosphate buffer, pH 2.4. Recoveries averaged 92% and the relative standard deviation was 8.0% in test samples spiked with 50 ng/mL patulin. The method appears to be applicable for monitoring apple juice samples to meet the U.S. Food and Drug Administration compliance action level of 50 microg/kg in an industrial quality assurance laboratory environment.

Phase-locked Optical Signal Recovery

DTIC Science & Technology

2009-01-01

detection . However, implementing an optical phase lock loop ( OPLL ) to generate the synchronised carrier for the homodyne technique requires... Loop (OIPLL) in which a narrow bandwidth optical phase lock loop ( OPLL ) is used to control the free -running frequency of an optically injection...receiver uses an Optical Injection Phase Lock Loop (OIPLL) for carrier recovery,

Efficient subtle motion detection from high-speed video for sound recovery and vibration analysis using singular value decomposition-based approach

NASA Astrophysics Data System (ADS)

Zhang, Dashan; Guo, Jie; Jin, Yi; Zhu, Chang'an

2017-09-01

High-speed cameras provide full field measurement of structure motions and have been applied in nondestructive testing and noncontact structure monitoring. Recently, a phase-based method has been proposed to extract sound-induced vibrations from phase variations in videos, and this method provides insights into the study of remote sound surveillance and material analysis. An efficient singular value decomposition (SVD)-based approach is introduced to detect sound-induced subtle motions from pixel intensities in silent high-speed videos. A high-speed camera is initially applied to capture a video of the vibrating objects stimulated by sound fluctuations. Then, subimages collected from a small region on the captured video are reshaped into vectors and reconstructed to form a matrix. Orthonormal image bases (OIBs) are obtained from the SVD of the matrix; available vibration signal can then be obtained by projecting subsequent subimages onto specific OIBs. A simulation test is initiated to validate the effectiveness and efficiency of the proposed method. Two experiments are conducted to demonstrate the potential applications in sound recovery and material analysis. Results show that the proposed method efficiently detects subtle motions from the video.

[Analysis of sulfonamids and their metabolites in drinking water by high Performance liquid chromatography tandem mass spectrometry].

PubMed

Wang, Shuo; Li, Shuming; Zhang, Xiangming; Wei, Yunfang; Zhang, Meiyun; Zhang, Jing

2015-07-01

To develop a comprehensive method for simultaneous analysis of sulfonamides and their metabolites in drinking water by high performance liquid chromatography tandem mass spectrometry (LC-MS/MS). Different solid-phase extraction columns were compared with respect to the recovery of target drugs from drinking water. The drinking water samples were adjusted to 3 by HCl and purified by a mix mode cation-ion exchange solid-phase extraction (SPE), following determination using LG-MS/MS. A total of 21 sulfonamides were separated by a C15 column (2.1 mm x 100 mm, 1.7 µm) and analyzed under positive ion mode with multi-reaction monitoring. The matrix-matched external standard calibration was used for quantification. The method quantification limits for 21 analytes were 0.03-0.63 ng/L with overall recoveries of 50.1%-114.9%, and the relative standard deviations less than 20%. The method was finally used to analyze sulfonamides in drinking water in Beijing, and 5 target compounds (sulfadiazine, sulfathiazole, sulfapyridine, trimethoprim and sulfamethazine) were detected at a concentration range of 0.08-32.54 ng/L. This method could be applied in simultaneous analysis of sulfonamides and their metabolites in drinking water samples.

Simultaneous determination of 29 pharmaceuticals in fish muscle and plasma by ultrasonic extraction followed by SPE-UHPLC-MS/MS.

PubMed

Liu, You-Yu; Hu, Xia-Lin; Bao, Yi-Fan; Yin, Da-Qiang

2018-02-12

A confirmatory method for the simultaneous detection of 29 pharmaceuticals in fish muscle and plasma was developed by using solid-phase extraction combined with ultra high performance liquid chromatography and tandem mass spectrometry. Fish samples were extracted with methanol and enriched using Oasis HLB solid-phase extraction columns in one step. Twenty-nine target pharmaceuticals were quantified by the internal standard method and the calibration curves showed good linearity in a wide range with determination coefficients of greater than 0.913. The detection limits of the pharmaceuticals ranged from 0.01 to 2.00 μg/kg (μg/L). The applicability of the method was checked by precision and recovery experiments. The average recoveries of the 29 pharmaceuticals were between 61 and 111%, and all the relative standard deviations were below 25%. Our reported method has been demonstrated to be sensitive, convenient, rapid and reliable for the simultaneous determination of 29 pharmaceuticals in fish muscle and plasma. Real sample determination showed that 25 and 9 of the 29 compounds were detected in fish muscle and plasma, respectively. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Quantitation of fumonisin B1 and B2 in feed using FMOC pre-column derivatization with HPLC and fluorescence detection.

PubMed

Smith, Lori L; Francis, Kyle A; Johnson, Joseph T; Gaskill, Cynthia L

2017-11-01

Pre-column derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) was determined to be effective for quantitation of fumonisins B 1 and B 2 in feed. Liquid-solid extraction, clean-up using immunoaffinity solid phase extraction chromatography, and FMOC-derivatization preceded analysis by reverse phase HPLC with fluorescence. Instrument response was unchanged in the presence of matrix, indicating no need to use matrix-matched calibrants. Furthermore, high method recoveries indicated calibrants do not need to undergo clean-up to account for analyte loss. Established method features include linear instrument response from 0.04-2.5µg/mL and stable derivatized calibrants over 7days. Fortified cornmeal method recoveries from 0.1-30.0μg/g were determined for FB 1 (75.1%-109%) and FB 2 (96.0%-115.2%). Inter-assay precision ranged from 1.0%-16.7%. Method accuracy was further confirmed using certified reference material. Inter-laboratory comparison with naturally-contaminated field corn demonstrated equivalent results with conventional derivatization. These results indicate FMOC derivatization is a suitable alternative for fumonisins B 1 and B 2 quantitation in corn-based feeds. Copyright © 2017 Elsevier Ltd. All rights reserved.

Multi-residue analysis method for analysis of pharmaceuticals using liquid chromatography-time of flight/mass spectrometry (LC-TOF/MS) in water sample

NASA Astrophysics Data System (ADS)

Al-Qaim, Fouad Fadhil; Abdullah, Md Pauzi; Othman, Mohamed Rozali

2013-11-01

In this work, a developed method using solid - phase extraction (SPE) followed by liquid chromatography - time of flight mass spectrometry (LC-ESI-TOF/MS) was developed and validated for quantification and confirmation of eleven pharmaceuticals with different therapeutic classes in water samples, Malaysia. These compounds are caffeine (CAF), prazosin (PRZ), enalapril (ENL), carbamazepine (CBZ), nifedipine (NFD), levonorgestrel (LNG), simvastatin (SMV), hydrochlorothiazide (HYD), gliclazide (GLIC), diclofenac-Na (DIC-Na) and mefenamic acid (MEF). LC was performed on a Dionex Ultimate 3000/LC 09115047 (USA) system. Chromatography was performed on a Thermo Scientific C18 (250 mm × 2.1 mm, i.d.: 5μm) column. Several parameters were optimised such as; mobile phase, gradient elution, collision energy and solvent elution for extraction of compounds from water. The recoveries obtained ranged from 30-148 % in river water. Five pharmaceutical compounds were detected in the surface water samples: caffeine, prazosin, enalpril, diclofenac-Na and mefenamic acid. The developed method is precise and accepted recoveries were got. In addition, this method is suitable to identify and quantify trace concentrations of pharmaceuticals in surface water.

Intensified fractionation of brewery yeast waste for the recovery of invertase using aqueous two-phase systems.

PubMed

De León-González, Grecia; González-Valdez, José; Mayolo-Deloisa, Karla; Rito-Palomares, Marco

2016-11-01

The potential recovery of high-value products from brewery yeast waste confers value to this industrial residue. Aqueous two-phase systems (ATPS) have demonstrated to be an attractive alternative for the primary recovery of biological products and are therefore suitable for the recovery of invertase from this residue. Sixteen different polyethylene glycol (PEG)-potassium phosphate ATPS were tested to evaluate the effects of PEG molecular weight (MW) and tie-line length (TLL) upon the partition behavior of invertase. Concentrations of crude extract from brewery yeast waste were then varied in the systems that presented the best behaviors to intensify the potential recovery of the enzyme. Results show that the use of a PEG MW 400 g mol -1 system with a TLL of 45.0% (w/w) resulted in an invertase bottom phase recovery with a purification factor of 29.5 and a recovery yield of up to 66.2% after scaling the system to a total weight of 15.0 g. This represents 15.1 mg of invertase per mL of processed bottom phase. With these results, a single-stage ATPS process for the recovery of invertase is proposed. © 2015 International Union of Biochemistry and Molecular Biology, Inc.

Mixed Matrix PVDF Membranes With in Situ Synthesized PAMAM Dendrimer-Like Particles: A New Class of Sorbents for Cu(II) Recovery from Aqueous Solutions by Ultrafiltration.

PubMed

Kotte, Madhusudhana Rao; Kuvarega, Alex T; Cho, Manki; Mamba, Bhekie B; Diallo, Mamadou S

2015-08-18

Advances in industrial ecology, desalination, and resource recovery have established that industrial wastewater, seawater, and brines are important and largely untapped sources of critical metals and elements. A Grand Challenge in metal recovery from industrial wastewater is to design and synthesize high capacity, recyclable and robust chelating ligands with tunable metal ion selectivity that can be efficiently processed into low-energy separation materials and modules. In our efforts to develop high capacity chelating membranes for metal recovery from impaired water, we report a one-pot method for the preparation of a new family of mixed matrix polyvinylidene fluoride (PVDF) membranes with in situ synthesized poly(amidoamine) [PAMAM] particles. The key feature of our new membrane preparation method is the in situ synthesis of PAMAM dendrimer-like particles in the dope solutions prior to membrane casting using low-generation dendrimers (G0 and G1-NH2) with terminal primary amine groups as precursors and epichlorohydrin (ECH) as cross-linker. By using a combined thermally induced phase separation (TIPS) and nonsolvent induced phase separation (NIPS) casting process, we successfully prepared a new family of asymmetric PVDF ultrafiltration membranes with (i) neutral and hydrophilic surface layers of average pore diameters of 22-45 nm, (ii) high loadings (∼48 wt %) of dendrimer-like PAMAM particles with average diameters of ∼1.3-2.4 μm, and (iii) matrices with sponge-like microstructures characteristics of membranes with strong mechanical integrity. Preliminary experiments show that these new mixed matrix PVDF membranes can serve as high capacity sorbents for Cu(II) recovery from aqueous solutions by ultrafiltration.

Modelling of Seismic and Resistivity Responses during the Injection of CO2 in Sandstone Reservoir

NASA Astrophysics Data System (ADS)

Omar, Muhamad Nizarul Idhafi Bin; Almanna Lubis, Luluan; Nur Arif Zanuri, Muhammad; Ghosh, Deva P.; Irawan, Sonny; Regassa Jufar, Shiferaw

2016-07-01

Enhanced oil recovery plays vital role in production phase in a producing oil field. Initially, in many cases hydrocarbon will naturally flow to the well as respect to the reservoir pressure. But over time, hydrocarbon flow to the well will decrease as the pressure decrease and require recovery method so called enhanced oil recovery (EOR) to recover the hydrocarbon flow. Generally, EOR works by injecting substances, such as carbon dioxide (CO2) to form a pressure difference to establish a constant productive flow of hydrocarbon to production well. Monitoring CO2 performance is crucial in ensuring the right trajectory and pressure differences are established to make sure the technique works in recovering hydrocarbon flow. In this paper, we work on computer simulation method in monitoring CO2 performance by seismic and resistivity model, enabling geoscientists and reservoir engineers to monitor production behaviour as respect to CO2 injection.

Acetonitrile extraction and dual-layer solid phase extraction clean-up for pesticide residue analysis in propolis.

PubMed

Oellig, Claudia

2016-05-06

Propolis is a very complex mixture of substances that is produced by honey bees and is known to be a rather challenging matrix for residue analysis. Besides resins, flavonoids and phenols, high amount of wax is co-extracted resulting in immense matrix effects. Therefore a suitable clean-up is crucial and indispensable. In this study, a reliable solid phase extraction (SPE) clean-up was developed for pesticide residue analysis in propolis. The clean-up success was quickly and easily monitored by high-performance thin-layer chromatography with different detection possibilities. The final method consists of the extraction of propolis with acetonitrile according to the QuEChERS method followed by an effective extract purification on dual-layer SPE cartridges with spherical hydrophobic polystyrene-divinylbenzene resin/primary secondary amine as sorbent and a mixture of toluene/acetone (95:5, v/v) for elution. Besides fat-soluble components like waxes, flavonoids, and terpenoids, more polar compounds like organic acids, fatty acids, sugars and anthocyanins were also removed to large extent. Method performance was assessed by recovery experiments at spiking levels of 0.5 and 1mg/kg (n=5) for fourteen pesticides that are relevant for propolis. Mean recoveries determined by HPLC-MS against solvent standards were between 40 and 101%, while calculation against matrix-matched standards provided recoveries of 79-104%. Precision of recovery, assessed by relative standard deviations, were below 9%. Thus, the developed dual-layer SPE clean-up enables the reliable pesticide residue analysis in propolis and provides a suitable alternative to time-consuming clean-up procedures proposed in literature. Copyright © 2016 Elsevier B.V. All rights reserved.

Exercise therapy and recovery after SCI: evidence that shows early intervention improves recovery of function

PubMed Central

Brown, AK; Woller, SA; Moreno, G; Grau, JW; Hook, MA

2011-01-01

Study design This was designed as an experimental study. Objectives Locomotor training is one of the most effective strategies currently available for facilitating recovery of function after an incomplete spinal cord injury (SCI). However, there is still controversy regarding the timing of treatment initiation for maximal recovery benefits. To address this issue, the present study compares the effects of exercise initiated in the acute and secondary phase of SCI. Setting Texas A&M University, College Station, TX, USA. Methods Rats received a moderate spinal contusion injury and began an exercise program 1 (D1-EX) or 8 days (D8-EX) later. They were individually placed into transparent exercise balls for 60 min per day, for 14 consecutive days. Control rats were placed in exercise balls that were rendered immobile. Motor and sensory recovery was assessed for 28 days after injury. Results The D1-EX rats recovered significantly more locomotor function (BBB scale) than controls and D8-EX rats. Moreover, analyses revealed that rats in the D8-EX group had significantly lower tactile reactivity thresholds compared with control and D1-EX rats, and symptoms of allodynia were not reversed by exercise. Rats in the D8-EX group also had significantly larger areas of damage across spinal sections caudal to the injury center compared with the D1-EX group. Conclusion These results indicate that implementing an exercise regimen in the acute phase of SCI maximizes the potential for recovery of function. PMID:21242998

Development and validation of high-performance liquid chromatography and high-performance thin-layer chromatography methods for the quantification of khellin in Ammi visnaga seed

PubMed Central

Kamal, Abid; Khan, Washim; Ahmad, Sayeed; Ahmad, F. J.; Saleem, Kishwar

2015-01-01

Objective: The present study was used to design simple, accurate and sensitive reversed phase-high-performance liquid chromatography RP-HPLC and high-performance thin-layer chromatography (HPTLC) methods for the development of quantification of khellin present in the seeds of Ammi visnaga. Materials and Methods: RP-HPLC analysis was performed on a C18 column with methanol: Water (75: 25, v/v) as a mobile phase. The HPTLC method involved densitometric evaluation of khellin after resolving it on silica gel plate using ethyl acetate: Toluene: Formic acid (5.5:4.0:0.5, v/v/v) as a mobile phase. Results: The developed HPLC and HPTLC methods were validated for precision (interday, intraday and intersystem), robustness and accuracy, limit of detection and limit of quantification. The relationship between the concentration of standard solutions and the peak response was linear in both HPLC and HPTLC methods with the concentration range of 10–80 μg/mL in HPLC and 25–1,000 ng/spot in HPTLC for khellin. The % relative standard deviation values for method precision was found to be 0.63–1.97%, 0.62–2.05% in HPLC and HPTLC for khellin respectively. Accuracy of the method was checked by recovery studies conducted at three different concentration levels and the average percentage recovery was found to be 100.53% in HPLC and 100.08% in HPTLC for khellin. Conclusions: The developed HPLC and HPTLC methods for the quantification of khellin were found simple, precise, specific, sensitive and accurate which can be used for routine analysis and quality control of A. visnaga and several formulations containing it as an ingredient. PMID:26681890

Exploring mechanisms of fatigue during repeated exercise and the dose dependent effects of carbohydrate and protein ingestion: study protocol for a randomised controlled trial

PubMed Central

2014-01-01

Background Muscle glycogen has been well established as the primary metabolic energy substrate during physical exercise of moderate- to high-intensity and has accordingly been implicated as a limiting factor when such activity is sustained for a prolonged duration. However, the role of this substrate during repeated exercise after limited recovery is less clear, with ongoing debate regarding how recovery processes can best be supported via nutritional intervention. The aim of this project is to examine the causes of fatigue during repeated exercise bouts via manipulation of glycogen availability through nutritional intervention, thus simultaneously informing aspects of the optimal feeding strategy for recovery from prolonged exercise. Methods/Design The project involves two phases with each involving two treatment arms administered in a repeated measures design. For each treatment, participants will be required to exercise to the point of volitional exhaustion on a motorised treadmill at 70% of previously determined maximal oxygen uptake, before a four hour recovery period in which participants will be prescribed solutions providing 1.2 grams of sucrose per kilogram of body mass per hour of recovery (g.kg-1.h-1) relative to either a lower rate of sucrose ingestion (that is, 0.3 g.kg-1. h-1; Phase I) or a moderate dose (that is, 0.8 g.kg-1.h-1) rendered isocaloric via the addition of 0.4 g.kg-1.h-1 whey protein hydrolysate (Phase II); the latter administered in a double blind manner as part of a randomised and counterbalanced design. Muscle biopsies will be sampled at the beginning and end of recovery for determination of muscle glycogen resynthesis rates, with further biopsies taken following a second bout of exhaustive exercise to determine differences in substrate availability relative to the initial sample taken following the first exercise bout. Discussion Phase I will inform whether a dose–response relationship exists between carbohydrate ingestion rate and muscle glycogen availability and/or the subsequent capacity for physical exercise. Phase II will determine whether such effects are dependent on glycogen availability per se or energy intake, potentially via protein mediated mechanisms. Trial registration ISRCTN87937960. PMID:24670140

Major Depressive Disorder in recovery and neuropsychological functioning: effects of selective serotonin reuptake inhibitor and dual inhibitor depression treatments on residual cognitive deficits in patients with Major Depressive Disorder in recovery.

PubMed

Herrera-Guzmán, Ixchel; Gudayol-Ferré, Esteve; Herrera-Abarca, Jorge E; Herrera-Guzmán, Daniel; Montelongo-Pedraza, Pedro; Padrós Blázquez, Ferran; Peró-Cebollero, Maribel; Guàrdia-Olmos, Joan

2010-06-01

Cognitive disturbances in Major Depressive Disorder (MDD) could persist beyond the symptomatic phase of the illness. However, the works addressing this topic did not usually account for the possible impact of medication on the cognitive functions of depressed patients. The present study aims to investigate whether MDD patients in remission treated with selective serotonin reuptake inhibitors (SSRI) or dual serotonergic-noradrenergic reuptake inhibitors (SNRI) show cognitive deficits, to study whether the same patients suffer neuropsychological disturbances when they are unmedicated and in recovery phase, and if the previous pharmacological treatment used to achieve the remission of MDD clinical symptoms had any effect in the profile of these patients' cognitive performance in the recovery phase. Thirty-six subjects with MDD treated with escitalopram and 37 depressed patients with duloxetine were compared both in remission phase and 24 weeks later, when they were unmedicated and in recovery phase. They were also compared, in both moments, to 37 healthy subjects. The control subjects showed a broader better cognitive performance than MDD patients in both measurement moments, but several cognitive functions improved over time. Also, the patients treated with SNRI performed better in memory tests than the SNRI-treated patients in remission phase, and in recovery phase. Our sample size is somewhat small, and we followed our patients only for 6months after treatment. Cognitive functions improve over time in patients with MDD beyond the remission phase, and the antidepressant treatment class used in acute depressive phase could influence his/her memory improvement. Copyright 2009 Elsevier B.V. All rights reserved.

Recovering from a stroke: a longitudinal, qualitative study of older Norwegian women.

PubMed

Eilertsen, Grethe; Kirkevold, Marit; Bjørk, Ida Torunn

2010-07-01

To illuminate older women's experiences and the characteristics of the recovery process following a stroke. Patients with stroke face serious challenges related to bodily changes, existential aspects and daily life after stroke. Few qualitative longitudinal studies have examined the recovery process from the perspective of the patient. Knowledge about older women's experiences in coping with life after a stroke is limited. Prospective, longitudinal, case-study design. Six women aged 68-83 suffering from first-time stroke were recruited from two stroke units. Each participant was interviewed in-depth 12-14 times during the first two years post stroke. The interviews addressed how they experienced their body, their self-understanding, daily life and how this had changed over time. Most interviews took place in the participants' homes. Gadamer's philosophical hermeneutics informed the analyses. Post stroke recovery was slow and complex and evolved through four distinct phases. In the first phase (0-2 months post stroke), the participants' main concerns were their bodily changes; in the second phase (2-6 months), activities of daily life; in the third phase (6-12 months), self-understanding and in the fourth phase (12-24 months), going on with life. The transition between phases was gradual. Recovery from stroke evolves over time through four distinct phases, which differ depending on significant experiences and associated meanings. Psychological and social resources are equally critical in the women's process of recovery. The four phases of rehabilitation suggest at what points various concerns require increased therapeutic attention. Psychological and social resources must be vitalised at an early phase similar to bodily resources. This knowledge may assist professionals in offering adequate help throughout the recovery process even beyond the established rehabilitation period. © 2010 Blackwell Publishing Ltd.

Application of decline curve analysis to estimate recovery factors for carbon dioxide enhanced oil recovery

USGS Publications Warehouse

Jahediesfanjani, Hossein

2017-07-17

IntroductionIn the decline curve analysis (DCA) method of estimating recoverable hydrocarbon volumes, the analyst uses historical production data from a well, lease, group of wells (or pattern), or reservoir and plots production rates against time or cumu­lative production for the analysis. The DCA of an individual well is founded on the same basis as the fluid-flow principles that are used for pressure-transient analysis of a single well in a reservoir domain and therefore can provide scientifically reasonable and accurate results. However, when used for a group of wells, a lease, or a reservoir, the DCA becomes more of an empirical method. Plots from the DCA reflect the reservoir response to the oil withdrawal (or production) under the prevailing operating and reservoir conditions, and they continue to be good tools for estimating recoverable hydrocarbon volumes and future production rates. For predicting the total recov­erable hydrocarbon volume, the DCA results can help the analyst to evaluate the reservoir performance under any of the three phases of reservoir productive life—primary, secondary (waterflood), or tertiary (enhanced oil recovery) phases—so long as the historical production data are sufficient to establish decline trends at the end of the three phases.

Unconventional slowing down of electronic recovery in photoexcited charge-ordered La 1/3Sr 2/3FeO 3

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

Zhu, Yi; Hoffman, Jason; Rowland, Clare E.

Ordered electronic phases are intimately related to emerging phenomena such as high Tc superconductivity and colossal magnetoresistance. The coupling of electronic charge with other degrees of freedom such as lattice and spin are of central interest in correlated systems. Their correlations have been intensively studied from femtosecond to picosecond time scales, while the dynamics of ordered electronic phases beyond nanoseconds are usually assumed to follow a trivia thermally driven recovery. Here, we report an unusual slowing down of electronic phases across a first-order phase transition, far beyond thermal relaxation time. Following optical excitation, the recovery time of both transient opticalmore » reflectivity and x-ray diffraction intensity from a charge-ordered superstructure in a La 1/3Sr 2/3FeO 3 thin film increases by orders of magnitude longer than the independently measured lattice cooling time when the sample temperature approaches the phase transition temperature. The combined experimental and theoretical investigations show that the slowing down of electronic recovery corresponds to the pseudo-critical dynamics that originates from magnetic interactions close to a weakly first-order phase transition. As a result, this extraordinary long electronic recovery time exemplifies an interplay of ordered electronic phases with magnetism beyond thermal processes in correlated systems.« less

Unconventional slowing down of electronic recovery in photoexcited charge-ordered La 1/3Sr 2/3FeO 3

DOE PAGES

Zhu, Yi; Hoffman, Jason; Rowland, Clare E.; ...

2018-05-04

Ordered electronic phases are intimately related to emerging phenomena such as high Tc superconductivity and colossal magnetoresistance. The coupling of electronic charge with other degrees of freedom such as lattice and spin are of central interest in correlated systems. Their correlations have been intensively studied from femtosecond to picosecond time scales, while the dynamics of ordered electronic phases beyond nanoseconds are usually assumed to follow a trivia thermally driven recovery. Here, we report an unusual slowing down of electronic phases across a first-order phase transition, far beyond thermal relaxation time. Following optical excitation, the recovery time of both transient opticalmore » reflectivity and x-ray diffraction intensity from a charge-ordered superstructure in a La 1/3Sr 2/3FeO 3 thin film increases by orders of magnitude longer than the independently measured lattice cooling time when the sample temperature approaches the phase transition temperature. The combined experimental and theoretical investigations show that the slowing down of electronic recovery corresponds to the pseudo-critical dynamics that originates from magnetic interactions close to a weakly first-order phase transition. As a result, this extraordinary long electronic recovery time exemplifies an interplay of ordered electronic phases with magnetism beyond thermal processes in correlated systems.« less

Single-shot quantitative phase microscopy with color-multiplexed differential phase contrast (cDPC).

PubMed

Phillips, Zachary F; Chen, Michael; Waller, Laura

2017-01-01

We present a new technique for quantitative phase and amplitude microscopy from a single color image with coded illumination. Our system consists of a commercial brightfield microscope with one hardware modification-an inexpensive 3D printed condenser insert. The method, color-multiplexed Differential Phase Contrast (cDPC), is a single-shot variant of Differential Phase Contrast (DPC), which recovers the phase of a sample from images with asymmetric illumination. We employ partially coherent illumination to achieve resolution corresponding to 2× the objective NA. Quantitative phase can then be used to synthesize DIC and phase contrast images or extract shape and density. We demonstrate amplitude and phase recovery at camera-limited frame rates (50 fps) for various in vitro cell samples and c. elegans in a micro-fluidic channel.

Space Station Freedom Water Recovery test total organic carbon accountability

NASA Technical Reports Server (NTRS)

Davidson, Michael W.; Slivon, Laurence; Sheldon, Linda; Traweek, Mary

1991-01-01

Marshall Space Flight Center's (MSFC) Water Recovery Test (WRT) addresses the concept of integrated hygiene and potable reuse water recovery systems baselined for Space Station Freedom (SSF). To assess the adequacy of water recovery system designs and the conformance of reclaimed water quality to established specifications, MSFC has initiated an extensive water characterization program. MSFC's goal is to quantitatively account for a large percentage of organic compounds present in waste and reclaimed hygiene and potable waters from the WRT and in humidity condensate from Spacelab missions. The program is coordinated into Phase A and B. Phase A's focus is qualitative and semi-quantitative. Precise quantitative analyses are not emphasized. Phase B's focus centers on a near complete quantitative characterization of all water types. Technical approaches along with Phase A and partial Phase B investigations on the compositional analysis of Total Organic Carbon (TOC) Accountability are presented.

Cost and Performance Report for LNAPL Recovery: Multi-Phase Extraction and Dual-Pump Recovery of LNAPL at the BP Former Amoco Refinery, Sugar Creek, MO

EPA Pesticide Factsheets

This case study was prepared to summarize the recovery of light non-aqueous phase liquid (LNAPL) at two locations at the BP Products of North America, Inc. Former Amoco Refinery (former refinery) in Sugar Creek, Missouri.

Solid phase extraction of 2,4-D from human urine.

PubMed

Thompson, T S; Treble, R G

1996-10-01

A method for determining urinary concentrations of 2,4-D in samples collected from non-occupationally, environmentally exposed individuals was developed. The 2,4-D was extracted from fortified human urine samples using octadecylsilane solid phase extraction cartridges. The average percent recovery for urine samples spiked at 2 and 20 ng/mL was 100% and 93%, respectively. The method detection limit was estimated to be 0.75 ng of 2,4-D per mL of urine based on a 10 mL sample size. The potential use of 2,4-dichlorophenylacetic acid as a surrogate standard was also investigated.

Extraction and determination of biogenic amines in fermented sausages and other meat products using reversed-phase-HPLC.

PubMed

Straub, B; Schollenberger, M; Kicherer, M; Luckas, B; Hammes, W P

1993-09-01

A convenient method is described for the analysis of biogenic amines (BA) by means of reversed-phase-HPLC. The method is characterized by multi-channel UV detection (diodearray), subsequent post-column derivatization with o-phthaldialdehyde and 3-mercaptopropionic acid, and fluorescence detection. For the analysis of meat products and especially fermented sausages an optimized perchloric acid extraction process was introduced to determine putrescine, cadaverine, histamine, tyramine and 2-phenylethylamine. BA recoveries from meat ranged between 96 and 113% with a detection limit for amines of 0.5 mg/kg.

Ultrahigh-speed clock recovery with optical phase lock loop based on four-wave-mixing in a semiconductor optical amplifier

NASA Astrophysics Data System (ADS)

Kim, Dong Hwan; Kim, Sang Hyuck; Jo, Jae Cheol; Choi, Sang Sam

2000-08-01

A new phase lock loop (PLL) is proposed and demonstrated for clock recovery from 40 Gbps time-division-multiplexed (TDM) optical signal using simple optical phase lock loop circuit. The proposed clock recovery scheme improves the jitter effect in PLL circuit from the clock pulse laser of harmonically-mode locked fiber laser. The cross-correlation component between the optical signal and an optical clock pulse train is detected as a four-wave-mixing (FWM) signal generated in SOA. The lock-in frequency range of the clock recovery is found to be within 10 KHz.

Coherent cavity-enhanced dual-comb spectroscopy

PubMed Central

Fleisher, Adam J.; Long, David A.; Reed, Zachary D.; Hodges, Joseph T.; Plusquellic, David F.

2016-01-01

Dual-comb spectroscopy allows for the rapid, multiplexed acquisition of high-resolution spectra without the need for moving parts or low-resolution dispersive optics. This method of broadband spectroscopy is most often accomplished via tight phase locking of two mode-locked lasers or via sophisticated signal processing algorithms, and therefore, long integration times of phase coherent signals are difficult to achieve. Here we demonstrate an alternative approach to dual-comb spectroscopy using two phase modulator combs originating from a single continuous-wave laser capable of > 2 hours of coherent real-time averaging. The dual combs were generated by driving the phase modulators with step-recovery diodes where each comb consisted of > 250 teeth with 203 MHz spacing and spanned > 50 GHz region in the near-infrared. The step-recovery diodes are passive devices that provide low-phase-noise harmonics for efficient coupling into an enhancement cavity at picowatt optical powers. With this approach, we demonstrate the sensitivity to simultaneously monitor ambient levels of CO2, CO, HDO, and H2O in a single spectral region at a maximum acquisition rate of 150 kHz. Robust, compact, low-cost and widely tunable dual-comb systems could enable a network of distributed multiplexed optical sensors. PMID:27409866

The electrum-tarnish method for the determination of the fugacity of sulfur in laboratory sulfide systems

USGS Publications Warehouse

Barton, P.B.; Toulmin, P.

1964-01-01

A new method for the determination of the fugacity of sulfur in laboratory systems consists of visual observation of the development and decomposition of a sulfide tarnish phase on silver-gold alloy (electrum) of precisely known composition. The alloy system is calibrated against pure sulfur. The method has the following advantages: simple apparatus; ability to cover a large range of fugacity of S2; ability to cover a large temperature range by permitting runs of long duration; ability to tolerate other components in the gas phase; and ease of recovery of the quenched charges for determinations of phases and compositions. Results obtained by the electrum-tarnish method are in satisfactory agreement with those obtained by other workers for the fs2 vs. T curves for the assemblage Ni(1-x)S + NiS2. The electrum-tarnish method shows promise for investigating many other reactions. Univariant reactions studied by this method can be represented as lines forming a genetic grid in terms of the environmental parameters fs2 and T, The slopes of such lines can yield valuable thermodynamic data for the phases involved, but activity coefficients must be known for phases of variable composition. ?? 1964.

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

Jenkins, T.F.; Thorne, P.G.; Myers, K.F.

Salting-out solvent extraction (SOE) was compared with cartridge and membrane solid-phase extraction (SPE) for preconcentration of nitroaromatics, nitramines, and aminonitroaromatics prior to determination by reversed-phase high-performance liquid chromatography. The solid phases used were manufacturer-cleaned materials, Porapak RDX for the cartridge method and Empore SDB-RPS for the membrane method. Thirty-three groundwater samples from the Naval Surface Warfare Center, Crane, Indiana, were analyzed using the direct analysis protocol specified in SW846 Method 8330, and the results were compared with analyses conducted after preconcentration using SOE with acetonitrile, cartridge-based SPE, and membrane-based SPE. For high-concentration samples, analytical results from the three preconcentration techniquesmore » were compared with results from the direct analysis protocol; good recovery of all target analytes was achieved by all three pre-concentration methods. For low-concentration samples, results from the two SPE methods were correlated with results from the SOE method; very similar data was obtained by the SOE and SPE methods, even at concentrations well below 1 microgram/L.« less

Phase Transformation and Shape Memory Effect of Ti-Pd-Pt-Zr High-Temperature Shape Memory Alloys

NASA Astrophysics Data System (ADS)

Yamabe-Mitarai, Yoko; Takebe, Wataru; Shimojo, Masayuki

2017-12-01

To understand the potential of high-temperature shape memory alloys, we have investigated the phase transformation and shape memory effect of Ti-(50 - x)Pt- xPd-5Zr alloys ( x = 0, 5, and 15 at.%), which present the B2 structure in the austenite phase and B19 structure in the martensite phase. Their phase transformation temperatures are very high; A f and M f of Ti-50Pt are 1066 and 1012 °C, respectively. By adding Zr and Pd, the phase transition temperatures decrease, ranging between 804 and 994 °C for A f and 590 and 865 °C for M f. Even at the high phase transformation temperature, a maximum recovery ratio of 70% was obtained for one cycle in a thermal cyclic test. A work output of 1.2 J/cm3 was also obtained. The recovery ratio obtained by the thermal cyclic test was less than 70% because the recovery strain was < 1% and a large irrecoverable strain was obtained. The shape recovery was explained by the austenite strength. The training effect was also investigated.

Determination of fluoroquinolones in cattle manure-based biogas residue by ultrasonic-enhanced microwave-assisted extraction followed by online solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Lu, Xue-Feng; Zhou, Yang; Zhang, Jian; Ren, Yu-Peng

2018-06-01

The present work describes the development and application of an ultrasonic-enhanced microwave-assisted extraction (UEMAE) followed by online solid phase extraction (SPE)-ultra-high performance liquid chromatography-tandem mass spectrometry method for the analysis of 14 fluoroquinolones in cattle manure-based biogas residue (CMBBR). The UEMAE was performed using the mixed solution of sodium dihydrogen phosphate and disodium ethylenediamine tetraacetic acid, avoiding use of any organic solvent. The online SPE system employed two solid phase extraction columns in a parallel manner, and the extraction was performed by passing 1 mL of the extract through the column. Quantification was performed using standard spiked samples and structural analogue internal standard, which were indispensable to reduce the matrix effects. Validation parameters were performed and good linearity (R 2  > 0.99 in all cases) and precision (inter- and intra-day relative standard deviations were lower than 12.8%) were obtained. Limits of detection were as low as 0.021 ng ∙ g -1 and lower limits of quantification were 0.5 ng ∙ g -1 for all fluoroquinolones. The overall extraction recovery, which was the product of the UEMAE recovery and the online SPE recovery, was assessed for three concentration levels (0.8, 40 and 400 ng ∙ g -1 ) and acceptable values (74.3-99.3%) were found. As a part of the method validation, the developed method has been used to analyze real CMBBR samples. Nine fluoroquinolones were found in the concentration range of 0.9-74.6 ng ∙ g -1 , while five were not detected in the samples. The results showed the method could be adapted for screening the presence or the final fate of fluoroquinolones during fermentation of animal waste. Copyright © 2018. Published by Elsevier B.V.

DOLPHIn—Dictionary Learning for Phase Retrieval

NASA Astrophysics Data System (ADS)

Tillmann, Andreas M.; Eldar, Yonina C.; Mairal, Julien

2016-12-01

We propose a new algorithm to learn a dictionary for reconstructing and sparsely encoding signals from measurements without phase. Specifically, we consider the task of estimating a two-dimensional image from squared-magnitude measurements of a complex-valued linear transformation of the original image. Several recent phase retrieval algorithms exploit underlying sparsity of the unknown signal in order to improve recovery performance. In this work, we consider such a sparse signal prior in the context of phase retrieval, when the sparsifying dictionary is not known in advance. Our algorithm jointly reconstructs the unknown signal - possibly corrupted by noise - and learns a dictionary such that each patch of the estimated image can be sparsely represented. Numerical experiments demonstrate that our approach can obtain significantly better reconstructions for phase retrieval problems with noise than methods that cannot exploit such "hidden" sparsity. Moreover, on the theoretical side, we provide a convergence result for our method.

Evaluation of alternative environmentally friendly matrix solid phase dispersion solid supports for the simultaneous extraction of 15 pesticides of different chemical classes from drinking water treatment sludge.

PubMed

Soares, Karina Lotz; Cerqueira, Maristela Barnes Rodrigues; Caldas, Sergiane Souza; Primel, Ednei Gilberto

2017-09-01

This study describes the development, optimization and validation of a method for the extraction of 15 pesticides of different chemical classes in drinking water treatment sludge (DWTS) by vortex-assisted Matrix Solid Phase Dispersion (MSPD) with determination by gas chromatography coupled to mass spectrometry. It focused on the application of alternative and different solid supports to the extraction step of the MSPD. The main parameters that influenced the extraction were studied in order to obtain better recovery responses. Recoveries ranged from 70 to 120% with RSD below 20% for all analytes. Limits of quantification (LOQ) of the method ranged from 5 to 500 μg kg -1 whereas the analytical curves showed correlation coefficients above 0.997. The method under investigation used low volume of solvent (5 mL), low sample mass (1.5 g) and low mass of chitin (0.5 g), an environmentally friendly support. It has advantages, such as speed, simplicity and low cost material, over other methods. When the method was applied, 4 out of 15 pesticides were detected in the DWTS samples in concentrations below the LOQ. Copyright © 2017 Elsevier Ltd. All rights reserved.

A validated high-performance liquid chromatography method with diode array detection for simultaneous determination of nine flavonoids in Senecio cannabifolius Less.

PubMed

Niu, Tian-Zeng; Zhang, Yu-Wei; Bao, Yong-Li; Wu, Yin; Yu, Chun-Lei; Sun, Lu-Guo; Yi, Jing-Wen; Huang, Yan-Xin; Li, Yu-Xin

2013-03-25

A reversed phase high performance liquid chromatography method coupled with a diode array detector (HPLC-DAD) was developed for the first time for the simultaneous determination of 9 flavonoids in Senecio cannabifolius, a traditional Chinese medicinal herb. Agilent Zorbax SB-C18 column was used at room temperature and the mobile phase was a mixture of acetonitrile and 0.5% formic acid (v/v) in water in the gradient elution mode at a flow-rate of 1.0mlmin(-1), detected at 360nm. Validation of this method was performed to verify the linearity, precision, limits of detection and quantification, intra- and inter-day variabilities, reproducibility and recovery. The calibration curves showed good linearities (R(2)>0.9995) within the test ranges. The relative standard deviation (RSD) of the method was less than 3.0% for intra- and inter-day assays. The samples were stable for at least 96h, and the average recoveries were between 90.6% and 102.5%. High sensitivity was demonstrated with detection limits of 0.028-0.085μg/ml for flavonoids. The newly established HPLC method represents a powerful technique for the quality assurance of S. cannabifolius. Copyright © 2012 Elsevier B.V. All rights reserved.

Development and Validation of RP-HPLC Method for the Estimation of Ivabradine Hydrochloride in Tablets

PubMed Central

Seerapu, Sunitha; Srinivasan, B. P.

2010-01-01

A simple, sensitive, precise and robust reverse–phase high-performance liquid chromatographic method for analysis of ivabradine hydrochloride in pharmaceutical formulations was developed and validated as per ICH guidelines. The separation was performed on SS Wakosil C18AR, 250×4.6 mm, 5 μm column with methanol:25 mM phosphate buffer (60:40 v/v), adjusted to pH 6.5 with orthophosphoric acid, added drop wise, as mobile phase. A well defined chromatographic peak of Ivabradine hydrochloride was exhibited with a retention time of 6.55±0.05 min and tailing factor of 1.14 at the flow rate of 0.8 ml/min and at ambient temperature, when monitored at 285 nm. The linear regression analysis data for calibration plots showed good linear relationship with R=0.9998 in the concentration range of 30-210 μg/ml. The method was validated for precision, recovery and robustness. Intra and Inter-day precision (% relative standard deviation) were always less than 2%. The method showed the mean % recovery of 99.00 and 98.55 % for Ivabrad and Inapure tablets, respectively. The proposed method has been successfully applied to the commercial tablets without any interference of excipients. PMID:21695008

Recovery of sugars from ionic liquid biomass liquor by solvent extraction

DOEpatents

Brennan, Timothy Charles R.; Holmes, Bradley M.; Simmons, Blake A.; Blanch, Harvey W.

2015-10-13

The present invention provides for a composition comprising a solution comprising (a) an ionic liquid (IL) or ionic liquid-aqueous (ILA) phase and (b) an organic phase, wherein the solution comprises a sugar and a boronic acid. The present invention also provides for a method of removing a sugar from a solution, comprising: (a) providing a solution comprising (i) an IL or ILA phase and (ii) an organic phase, wherein the solution comprises an IL, a sugar and a boronic acid; (b) contacting the sugar with the boronic acid to form a sugar-boronic acid complex, (c) separating the organic phase and the aqueous phase, wherein the organic phase contains the sugar-boronic acid complex, and optionally (d) separating the sugar from the organic phase.

Simultaneous determination of bromhexine hydrochloride and methyl and propyl p-hydroxybenzoate and determination of dextromethorphan hydrobromide in cough-cold syrup by high-performance liquid chromatography.

PubMed

Rauha, J P; Salomies, H; Aalto, M

1996-11-01

Liquid chromatographic methods were developed for the determination of bromhexine hydrochloride, methyl p-hydroxybenzoate and propyl p-hydroxybenzoate (method A) and dextromethorphan hydrobromide (method B) in cough-cold syrup formulations. Reversed-phase analytical columns (150 mm x 3.9 mm i.d.) were used with (A) C18 and (B) phenyl as stationary phases and mixtures of (A) acetonitrile and aqueous 15 mM triethylamine solution (43:57) and (B) methanol and aqueous 3% ammonium formate buffer solution (53:47) as mobile phases at a flow rate of 1.0 ml min-1. Both aqueous components were adjusted to pH 3.9. UV detection of analytes was at (A) 245 nm and (B) 278 nm. In both methods, the time required for an HPLC run giving good separations and recoveries was less than 8 min.

Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials

DOE PAGES

Gao, Jun; Manard, Benjamin Thomas; Castro, Alonso; ...

2017-02-02

Advances in sample nebulization and injection technology have significantly reduced the volume of solution required for trace impurity analysis in plutonium and uranium materials. Correspondingly, we have designed and tested a novel chip-based microfluidic platform, containing a 100-µL or 20-µL solid-phase microextraction column, packed by centrifugation, which supports nuclear material mass and solution volume reductions of 90% or more compared to standard methods. Quantitative recovery of 28 trace elements in uranium was demonstrated using a UTEVA chromatographic resin column, and trace element recovery from thorium (a surrogate for plutonium) was similarly demonstrated using anion exchange resin AG MP-1. Of ninemore » materials tested, compatibility of polyvinyl chloride (PVC), polypropylene (PP), and polytetrafluoroethylene (PTFE) chips with the strong nitric acid media was highest. Finally, the microcolumns can be incorporated into a variety of devices and systems, and can be loaded with other solid-phase resins for trace element assay in high-purity metals.« less

Polysaccharide-derived mesoporous materials (Starbon®) for sustainable separation of complex mixtures.

PubMed

Zuin, Vânia G; Budarin, Vitaliy L; De Bruyn, Mario; Shuttleworth, Peter S; Hunt, Andrew J; Pluciennik, Camille; Borisova, Aleksandra; Dodson, Jennifer; Parker, Helen L; Clark, James H

2017-09-21

The recovery and separation of high value and low volume extractives are a considerable challenge for the commercial realisation of zero-waste biorefineries. Using solid-phase extractions (SPE) based on sustainable sorbents is a promising method to enable efficient, green and selective separation of these complex extractive mixtures. Mesoporous carbonaceous solids derived from renewable polysaccharides are ideal stationary phases due to their tuneable functionality and surface structure. In this study, the structure-separation relationships of thirteen polysaccharide-derived mesoporous materials and two modified types as sorbents for ten naturally-occurring bioactive phenolic compounds were investigated. For the first time, a comprehensive statistical analysis of the key molecular and surface properties influencing the recovery of these species was carried out. The obtained results show the possibility of developing tailored materials for purification, separation or extraction, depending on the molecular composition of the analyte. The wide versatility and application span of these polysaccharide-derived mesoporous materials offer new sustainable and inexpensive alternatives to traditional silica-based stationary phases.

Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials

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

Gao, Jun; Manard, Benjamin Thomas; Castro, Alonso

Advances in sample nebulization and injection technology have significantly reduced the volume of solution required for trace impurity analysis in plutonium and uranium materials. Correspondingly, we have designed and tested a novel chip-based microfluidic platform, containing a 100-µL or 20-µL solid-phase microextraction column, packed by centrifugation, which supports nuclear material mass and solution volume reductions of 90% or more compared to standard methods. Quantitative recovery of 28 trace elements in uranium was demonstrated using a UTEVA chromatographic resin column, and trace element recovery from thorium (a surrogate for plutonium) was similarly demonstrated using anion exchange resin AG MP-1. Of ninemore » materials tested, compatibility of polyvinyl chloride (PVC), polypropylene (PP), and polytetrafluoroethylene (PTFE) chips with the strong nitric acid media was highest. Finally, the microcolumns can be incorporated into a variety of devices and systems, and can be loaded with other solid-phase resins for trace element assay in high-purity metals.« less

Phase-sensitive dual-inversion recovery for accelerated carotid vessel wall imaging.

PubMed

Bonanno, Gabriele; Brotman, David; Stuber, Matthias

2015-03-01

Dual-inversion recovery (DIR) is widely used for magnetic resonance vessel wall imaging. However, optimal contrast may be difficult to obtain and is subject to RR variability. Furthermore, DIR imaging is time-inefficient and multislice acquisitions may lead to prolonged scanning times. Therefore, an extension of phase-sensitive (PS) DIR is proposed for carotid vessel wall imaging. The statistical distribution of the phase signal after DIR is probed to segment carotid lumens and suppress their residual blood signal. The proposed PS-DIR technique was characterized over a broad range of inversion times. Multislice imaging was then implemented by interleaving the acquisition of 3 slices after DIR. Quantitative evaluation was then performed in healthy adult subjects and compared with conventional DIR imaging. Single-slice PS-DIR provided effective blood-signal suppression over a wide range of inversion times, enhancing wall-lumen contrast and vessel wall conspicuity for carotid arteries. Multislice PS-DIR imaging with effective blood-signal suppression is enabled. A variant of the PS-DIR method has successfully been implemented and tested for carotid vessel wall imaging. This technique removes timing constraints related to inversion recovery, enhances wall-lumen contrast, and enables a 3-fold increase in volumetric coverage at no extra cost in scanning time.

Practical and Secure Recovery of Disk Encryption Key Using Smart Cards

NASA Astrophysics Data System (ADS)

Omote, Kazumasa; Kato, Kazuhiko

In key-recovery methods using smart cards, a user can recover the disk encryption key in cooperation with the system administrator, even if the user has lost the smart card including the disk encryption key. However, the disk encryption key is known to the system administrator in advance in most key-recovery methods. Hence user's disk data may be read by the system administrator. Furthermore, if the disk encryption key is not known to the system administrator in advance, it is difficult to achieve a key authentication. In this paper, we propose a scheme which enables to recover the disk encryption key when the user's smart card is lost. In our scheme, the disk encryption key is not preserved anywhere and then the system administrator cannot know the key before key-recovery phase. Only someone who has a user's smart card and knows the user's password can decrypt that user's disk data. Furthermore, we measured the processing time required for user authentication in an experimental environment using a virtual machine monitor. As a result, we found that this processing time is short enough to be practical.

Optimized demineralization technique for the measurement of stable isotope ratios of nonexchangeable H in soil organic matter.

PubMed

Ruppenthal, Marc; Oelmann, Yvonne; Wilcke, Wolfgang

2013-01-15

To make use of the isotope ratio of nonexchangeable hydrogen (δ(2)H(n (nonexchangeable))) of bulk soil organic matter (SOM), the mineral matrix (containing structural water of clay minerals) must be separated from SOM and samples need to be analyzed after H isotope equilibration. We present a novel technique for demineralization of soil samples with HF and dilute HCl and recovery of the SOM fraction solubilized in the HF demineralization solution via solid-phase extraction. Compared with existing techniques, organic C (C(org)) and organic N (N(org)) recovery of demineralized SOM concentrates was significantly increased (C(org) recovery using existing techniques vs new demineralization method: 58% vs 78%; N(org) recovery: 60% vs 78%). Chemicals used for the demineralization treatment did not affect δ(2)H(n) values as revealed by spiking with deuterated water. The new demineralization method minimized organic matter losses and thus artificial H isotope fractionation, opening up the opportunity to use δ(2)H(n) analyses of SOM as a new tool in paleoclimatology or geospatial forensics.

Magnetic Field Observations of Partial Ring Current during Storm Recovery Phase

NASA Technical Reports Server (NTRS)

Le, G.; Russell, C. T.; Slavin, J. A.; Lucek, E. A.

2008-01-01

We present results of an extensive survey of the magnetic field observations in the inner magnetosphere using 30 years of magnetospheric magnetic field data from Polar, Cluster, ISEE, and AMPTE/CCE missions. The purpose of this study is to understand the magnetic field evolution during the recovery phase of geomagnetic storms, and its implication to the ring current recovery and loss mechanisms of ring current particles. It is now commonly believed that a strong partial ring current is formed during the storm main phase due to the enhanced earthward convection of energetic ions from nightside plasma sheet. But the presence of a strong partial ring current throughout the recovery phase remains controversial. The magnetic field generated by the ring current inflates the inner magnetosphere and causes magnetic field depressions in the equatorial magnetosphere. During the storm recovery phase, we find that the distribution of the equatorial magnetic field depression exhibits similar local time dependence as the ring current distribution obtained from the combined dataset in the earlier study. It shows that a strong partial ring current is a permanent feature throughout the recovery phase. In the early recovery phase, the partial ring current peaks near the dusk terminator as indicated by the peak of the magnetic field depression. As the recovery phase progresses, the partial ring current decays most quickly near the dusk and results in a dusk-to-midnight moving of the peak of the partial ring current. Thus the loss mechanisms work most effectively near the dusk. The magnetic field depression increases the gyroradius of ring current protons to a scale greater or comparable to the thickness of the magnetopause, which increases the chance of ion drift loss near the dusk magnetopause at larger L-shell (L greater than 5). But the drift loss mechanism alone cannot explain the loss of ring current ions especially in the smaller L-shell (L less than 5). The precipitation loss due to wave-particle interaction is most likely the dominant loss mechanism in the small L-shell as it works most effectively at the same local time.

Assessment of grammar optimizes language tasks for the intracarotid amobarbital procedure.

PubMed

Połczyńska, Monika; Kuhn, Taylor; You, S Christine; Walshaw, Patricia; Curtiss, Susan; Bookheimer, Susan

2017-11-01

A previous study showed that assessment of language laterality could be improved by adding grammar tests to the recovery phase of the intracarotid amobarbital procedure (IAP) (Połczyńska et al. 2014). The aim of this study was to further investigate the extent to which grammar tests lateralize language function during the recovery phase of the IAP in a larger patient sample. Forty patients with drug-resistant epilepsy (14 females, thirty-two right-handed, mean age 38.5years, SD=10.6) participated in this study. On EEG, 24 patients had seizures originating in the left hemisphere (LH), 13 in the right hemisphere (RH), and 4 demonstrated mixed seizure origin. Thirty participants (75%) had bilateral injections, and ten (25%) had unilateral injections (five RH and five LH). Based on results from the encoding phase, we segregated our study participants to a LH language dominant and a mixed dominance group. In the recovery phase of the IAP, the participants were administered a new grammar test (the CYCLE-N) and a standard language test. We analyzed the laterality index measure and effect sizes in the two tests. In the LH-dominant group, the CYCLE-N generated more profound language deficits in the recovery phase than the standard after injection to either hemisphere (p<0.001). At the same time, the laterality index for the grammar tasks was still higher than for the standard tests. Critically, the CYCLE-N administered in the recovery phase was nearly as effective as the standard tests given during the encoding phase. The results may be significant for individuals with epilepsy undergoing IAP. The grammar tests may be a highly efficient measure for lateralizing language function in the recovery phase. Copyright © 2017 Elsevier Inc. All rights reserved.

Selective solid-phase extraction using a molecularly imprinted polymer for the analysis of patulin in apple-based foods.

PubMed

Lucci, Paolo; Moret, Sabrina; Bettin, Sara; Conte, Lanfranco

2017-01-01

The aim of this work was to evaluate the use of a molecularly imprinted polymer as a selective solid-phase extraction sorbent for the clean-up and pre-concentration of patulin from apple-based food products. Ultra high pressure liquid chromatography coupled to ultraviolet absorbance detection was used for the analysis of patulin. The molecularly imprinted polymer was applied, for the first time, to the determination of patulin in apple juice, puree and jam samples spiked within the maximum levels specified by the European Commission No. 1881/2006. High recoveries (>77%) were obtained. The method was validated and found to be linear in the range 2-100 μg/kg with correlation coefficients greater than 0.965 and repeatability relative standard deviation below 11% in all cases. Compared with dispersive solid-phase extraction (QuEChERS method) and octadecyl sorbent, the molecularly imprinted polymer showed higher recoveries and selectivity for patulin. The application of Affinisep molecularly imprinted polymer as a selective sorbent material for detection of patulin fulfilled the method performance criteria required by the Commission Regulation No. 401/2006, demonstrating the suitability of the technique for the control of patulin at low ppb levels in different apple-based foods such as juice, puree and jam samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

TLC-Densitometric and RP-HPLC Methods for Simultaneous Determination of Dexamethasone and Chlorpheniramine Maleate in the Presence of Methylparaben and Propylparaben.

PubMed

Farid, Nehal F; Naguib, Ibrahim A; Moatamed, Radwa S; El Ghobashy, Mohamed R

2017-01-01

Validated simple, sensitive, and highly selective methods are applied for the quantitative determination of dexamethasone and chlorpheniramine maleate in the presence of their reported preservatives (methylparaben and propylparaben), whether in pure forms or in pharmaceutical formulation. TLC is the first method, in which dexamethasone, chlorpheniramine maleate, methylparaben, and propylparaben are separated on silica gel TLC F254 plates using hexane-acetone-ammonia (5.5 + 4.5 + 0.5, v/v/v) as the developing phase. Separated bands are scanned at 254 nm over a concentration range of 0.1-1.7 and 0.4-2.8 μg/band, with mean ± SD recoveries of 99.12 ± 0.964 and 100.14 ± 0.962%, for dexamethasone and chlorpheniramine maleate, respectively. Reversed-phase HPLC is the second method, in which a mixture of dexamethasone and chlorpheniramine maleate, methylparaben, and propylparaben is separated on a reversed-phase silica C18 (5 μm particle size, 250 mm, 4.6 mm id) column using 0.1 M ammonium acetate buffer-acetonitrile (60 + 40, v/v, pH 3) as the mobile phase. The drugs were detected at 220 nm over a concentration range of 5-50 μg/mL, 2-90 μg/mL, 4-100 μg/mL, and 7-50 μg/mL, with mean ± SD recoveries of 100.85 ± 0.905, 99.67 ± 1.281, 100.20 ± 0.906, and 99.81 ± 0.954%, for dexamethasone, chlorpheniramine maleate, methylparaben paraben, and propylparaben, respectively. The advantages of the suggested methods over previously reported methods are the ability to detect lower concentrations of the main drugs and to show better resolution of interfering preservatives; hence, these methods could be more reliable for routine QC analyses.

Method and apparatus for improved observation of in-situ combustion processes

DOEpatents

Lee, D.O.; Montoya, P.C.; Wayland, J.R. Jr.

Method and apparatus are provided for obtaining accurate dynamic measurements for passage of phase fronts through a core sample in a test fixture. Flow-through grid structures are provided for electrodes to permit data to be obtained before, during and after passage of a front there-through. Such electrodes are incorporated in a test apparatus for obtaining electrical characteristics of the core sample. With the inventive structure a method is provided for measurement of instabilities in a phase front progressing through the medium. Availability of accurate dynamic data representing parameters descriptive of material characteristics before, during and after passage of a front provides a more efficient method for enhanced recovery of oil using a fire flood technique. 6 figures, 2 tables.

Determination of tocopheryl acetate and ascorbyl tetraisopalmitate in cosmetic formulations by HPLC.

PubMed

Almeida, M M; Alves, J M P; Patto, D C S; Lima, C R R C; Quenca-Guillen, J S; Santoro, M I R M; Kedor-Hackmann, E R M

2009-12-01

A rapid HPLC method was developed for the assay of tocopheryl acetate and ascorbyl tetraisopalmitate in cosmetic formulations. The validated method was applied for quantitative determination of these vitamins in simulated emulsion formulation. Samples were analysed directly on a RP-18 reverse phase column with UV detection at 222 nm. A mixture of methanol and isopropanol (25 : 75 v/v) was used as mobile phase. The retention time of tocopheryl acetate and ascorbyl tetraisopalmitate were 3.0 min and 5.9 min, respectively. Recovery was between 95% and 104%. In addition, the excipients did not interfere in the analysis. The method is simple, reproducible, selective and is suitable for routine analyses of commercial products.

Extraction and LC determination of lysine clonixinate salt in water/oil microemulsions.

PubMed

Pineros, I; Ballesteros, P; Lastres, J L

2002-02-01

A new reversed-phase high performance liquid chromatography method has been developed and validated for the quantitative determination of lysine clonixinate salt in water/oil microemulsions. The mobile phase was acetonitrile-buffer phosphate pH 3.3. Detection was UV absorbance at 252 nm. The precision and accurately of the method were excellent. The established linearity range was 5-60 microg ml(-1) (r(2)=0.999). Microemulsions samples were dispersed with chloroform and extracted lysine clonixinate salt with water. This easy method employing chloroformic extraction has been done three times. The recovery of lysine clonixinate salt from spiked placebo and microemulsion were >90% over the linear range.

Polydopamine-coated magnetic nanoparticles for isolation and enrichment of estrogenic compounds from surface water samples followed by liquid chromatography-tandem mass spectrometry determination.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Piovesana, Susy; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2016-06-01

Estrogens, phytoestrogens, and mycoestrogens may enter into the surface waters from different sources, such as effluents of municipal wastewater treatment plants, industrial plants, and animal farms and runoff from agricultural areas. In this work, a multiresidue analytical method for the determination of 17 natural estrogenic compounds, including four steroid estrogens, six mycoestrogens, and seven phytoestrogens, in river water samples has been developed. (Fe3O4)-based magnetic nanoparticles coated by polydopamine (Fe3O4@pDA) were used for dispersive solid-phase extraction, and the final extract was analyzed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry. The Fe3O4 magnetic nanoparticles were prepared by a co-precipitation procedure, coated by pDA, and characterized by scanning electron microscopy, infrared spectroscopy, and elemental analysis. The sample preparation method was optimized in terms of extraction recovery, matrix effect, selectivity, trueness, precision, method limits of detection, and method limits of quantification (MLOQs). For all the 17 analytes, recoveries were >70 % and matrix effects were below 30 % when 25 mL of river water sample was treated with 90 mg of Fe3O4@pDA nanoparticles. Selectivity was tested by spiking river water samples with 50 other compounds (mycotoxins, antibacterials, conjugated hormones, UV filters, alkylphenols, etc.), and only aflatoxins and some benzophenones showed recoveries >60 %. This method proved to be simple and robust and allowed the determination of natural estrogenic compounds belonging to different classes in surface waters with MLOQs ranging between 0.003 and 0.1 μg L(-1). Graphical Abstract Determination of natural estrogenic compounds in water by magnetic solid phase extraction followed by liquid chromatography-tandem mass spectrometry analysis.

Processing of Phosphorus Slag with Recovery of Rare Earth Metals and Obtaining Silicon Containing Cake

NASA Astrophysics Data System (ADS)

Karshigina, Zaure; Abisheva, Zinesh; Bochevskaya, Yelena; Akcil, Ata; Sharipova, Aynash; Sargelova, Elmira

2016-10-01

The present research is devoted to the processing of slag generating during the yellow phosphorus production. In this paper are presented studies on leaching of phosphorus production slag by nitric acid with recovery of rare earth metals (REMs) into solution. REMs recovery into the solution achieved 98 % during the leaching process with using 7.5 mol/L of HNO3, liquid-to-solid ratio is 2.6:1, temperature is 60°C, process duration is 1 hour and stirrer speed is 500 rpm. Behaviour during the leaching of associated components such as calcium, aluminium, and iron was studied. After the leaching cake contains ∼⃒75-85 % of SiO2 and it might be useful for obtaining of precipitated silicon dioxide. With the purpose of separation from the impurities, recovery and concentrating of REMs, the obtained solution after leaching was subjected to extraction processing methods. The influence of ratio of organic and aqueous phases (O: A) on the extraction of rare earth metals by tributyl phosphate (TBP) with concentrations from 20 up to 100 % was studied. The REMs extraction with increasing TBP concentration under changes O:A ratio from 1:20 down to 1:1 into the organic phase from the solutions after nitric acid leaching increased from 22.2 up to 99.3%. The duration effect of REMs extraction process was studied by tributyl phosphate. It is revealed that with increasing of duration of the extraction process from 10 to 30 minutes REMs recovery into the organic phase almost did not changed. The behaviour of iron in the extraction process by TBP was studied. It was found that such accompanying components as calcium and aluminium by tributyl phosphate didn't extracted. To construct isotherm of REMs extraction of by tributyl phosphate was used variable volume method. It was calculated three-step extraction is needed for REMs recovery from the solutions after nitric acid leaching of phosphorus production slag. The process of the three-steps counter current extraction of rare earth metals was modelled from the solutions after slag leaching with using 50 % of TBP in kerosene at the ratios O:A = 1:6 and 1:20. So, REMs recovery into the extract achieved 97.0 and 76.5 %, respectively. It was offered flowsheet of processing of phosphorus slag production with extraction of rare earth metals and obtaining silicon containing cake.

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.

Influence of optical pumping wavelength on the ultrafast gain and phase recovery acceleration of quantum-dot semiconductor optical amplifiers

NASA Astrophysics Data System (ADS)

Kim, Jungho

2013-10-01

We numerically investigate the influence of the optical pumping wavelength on the ultrafast gain and phase recovery acceleration of quantum-dot (QD) semiconductor optical amplifiers (SOAs) by solving 1088 coupled rate equations. The temporal variations of the gain and phase recovery response at the ground state (GS) of QDs are calculated at various signal wavelengths when the optical pumping wavelengths at the excited state (ES) of QDs are varied. The phase recovery response is fastest when the wavelength of the signal and pumping beams corresponds to the respective emission wavelength of the GS and the ES in the same size of QDs. The absorption efficiency of the optical pumping beam at the ES is determined by the Lorentzian line shape function of the homogeneous broadening.

Single-shot quantitative phase microscopy with color-multiplexed differential phase contrast (cDPC)

PubMed Central

2017-01-01

We present a new technique for quantitative phase and amplitude microscopy from a single color image with coded illumination. Our system consists of a commercial brightfield microscope with one hardware modification—an inexpensive 3D printed condenser insert. The method, color-multiplexed Differential Phase Contrast (cDPC), is a single-shot variant of Differential Phase Contrast (DPC), which recovers the phase of a sample from images with asymmetric illumination. We employ partially coherent illumination to achieve resolution corresponding to 2× the objective NA. Quantitative phase can then be used to synthesize DIC and phase contrast images or extract shape and density. We demonstrate amplitude and phase recovery at camera-limited frame rates (50 fps) for various in vitro cell samples and c. elegans in a micro-fluidic channel. PMID:28152023

Field-Aligned Current at Plasma Sheet Boundary Layers During Storm Time: Cluster Observation

NASA Astrophysics Data System (ADS)

Shi, J.; Cheng, Z.; Zhang, T.; Dunlop, M.; Liu, Z.

2007-05-01

The magnetic field data from the FGM instruments on board the four Cluster spacecrafts were used to study Field Aligned Current (FAC) at the Plasma Sheet Boundary Layers (PSBLs) with the so called "curlometer technique". We analyzed the date obtained in 2001 in the magnetotail and only two cases were found in the storm time. One (August 17, 2001) occurred from sudden commencement to main phase, and the other (October 1, 2001) lay in the main phase and recovery phase. The relationship between the FAC density and the AE index was studied and the results are shown as follows. (1) In the sudden commencement and the main phase the density of the FAC increases obviously, in the recovery phase the density of the FAC increases slightly. (2) From the sudden commencement to the initial stage of the main phase the FAC increases with decreasing AE index and decreases with increasing AE index. From the late stage of the main phase to initial stage of the recovery phase, the FAC increases with increasing AE index and decreases with decreasing AE index. In the late stage of the recovery phase the disturbance of the FAC is not so violent, so that the FAC varying with the AE index is not very obvious.

Confirmatory and quantitative analysis of beta-lactam antibiotics in bovine kidney tissue by dispersive solid-phase extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Fagerquist, Clifton K; Lightfield, Alan R; Lehotay, Steven J

2005-03-01

A simple, rapid, rugged, sensitive, and specific method for the confirmation and quantitation of 10 beta-lactam antibiotics in fortified and incurred bovine kidney tissue has been developed. The method uses a simple solvent extraction, dispersive solid-phase extraction (dispersive-SPE) cleanup, and liquid chromatography-tandem mass spectrometry (LC/MS/MS) for confirmation and quantitation. Dispersive-SPE greatly simplifies and accelerates sample cleanup and improves overall recoveries compared with conventional SPE cleanup. The beta-lactam antibiotics tested were as follows: deacetylcephapirin (an antimicrobial metabolite of cephapirin), amoxicillin, desfuroylceftiofur cysteine disulfide (DCCD, an antimicrobial metabolite of ceftiofur), ampicillin, cefazolin, penicillin G, oxacillin, cloxacillin, naficillin, and dicloxacillin. Average recoveries of fortified samples were 70% or better for all beta-lactams except DCCD, which had an average recovery of 58%. The LC/MS/MS method was able to demonstrate quantitative recoveries at established tolerance levels and provide confirmatory data for unambiguous analyte identification. The method was also tested on 30 incurred bovine kidney samples obtained from the USDA Food Safety and Inspection Service, which had previously tested the samples using the approved semiquantitative microbial assay. The results from the quantitative LC/MS/MS analysis were in general agreement with the microbial assay for 23 samples although the LC/MS/MS method was superior in that it could specifically identify which beta-lactam was present and quantitate its concentration, whereas the microbial assay could only identify the type of beta-lactam present and report a concentration with respect to the microbial inhibition of a penicillin G standard. In addition, for 6 of the 23 samples, LC/MS/MS analysis detected a penicillin and a cephalosporin beta-lactam, whereas the microbial assay detected only a penicillin beta-lactam. For samples that do not fall into the "general agreement" category, the most serious discrepancy involves two samples where the LC/MS/MS method detected a violative level of a cephalosporin beta-lactam (deacetylcephapirin) in the first sample and a possibly violative level of desfuroylceftiofur in the second, whereas the microbial assay identified the two samples as having only violative levels of a penicillin beta-lactam.

Controlling the metal to semiconductor transition of MoS 2 and WS 2 in solution

DOE PAGES

Chou, Stanley Shihyao; Yi-Kai Huang; Kim, Jaemyung; ...

2015-01-22

Lithiation-exfoliation produces single to few-layered MoS 2 and WS 2 sheets dispersible in water. However, the process transforms them from the pristine semiconducting 2H phase to a distorted metallic phase. Recovery of the semiconducting properties typically involves heating of the chemically exfoliated sheets at elevated temperatures. Therefore, it has been largely limited to sheets deposited on solid substrates. We report the dispersion of chemically exfoliated MoS 2 sheets in high boiling point organic solvents enabled by surface functionalization and the controllable recovery of their semiconducting properties directly in solution. Ultimately, this process connects the scalability of chemical exfoliation with themore » simplicity of solution processing, enabling a facile method for tuning the metal to semiconductor transitions of MoS 2 and WS 2 within a liquid medium.« less

Extension of the QuEChERS method for pesticide residues in cereals to flaxseeds, peanuts, and doughs.

PubMed

Koesukwiwat, Urairat; Lehotay, Steven J; Mastovska, Katerina; Dorweiler, Kelly J; Leepipatpiboon, Natchanun

2010-05-26

A simple method was evaluated for the determination of pesticide residues in flaxseeds, doughs, and peanuts using gas chromatography-time-of-flight mass spectrometry (GC-TOF) for analysis. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which was previously optimized for cereal grain samples, was evaluated in these fatty matrices. This extraction method involves first mixing the sample with 1:1 water/acetonitrile for an hour to swell the matrix and permit the salt-out liquid-liquid partitioning step using anhydrous MgSO(4) and NaCl. After shaking and centrifugation, cleanup is done by dispersive solid-phase extraction (d-SPE) using 150 mg of anhydrous MgSO(4), 150 mg of PSA, and 50 mg of C-18 per milliliter of extract. This method gave efficient separation of pesticides from fat and removal of coextracted substances better than gel permeation chromatography or use of a freeze-out step, which involved excessive use of solvent and/or time. The optimized analytical conditions were evaluated in terms of recoveries, reproducibilities, limits of detection, and matrix effects for 34 representative pesticides using different types of flaxseeds, peanuts, and doughs. Use of matrix-matched standards provided acceptable results for most pesticides with overall average recoveries between 70 and 120% and consistent RSDs <20% for semipolar pesticides and <26% for lipophilic pesticides. The recoveries of these latter types of pesticides depended on the fat content in the matrices and partitioning factor between the lipids and acetonitrile. We believe that the consistency of the pesticide recoveries for different samples in multiple experiments and the physicochemical partitioning explanation for <70% recoveries of lipophilic pesticides justify compensation of results for the empirically determined recovery values. In any case, this method still meets 10 ng/g detection limit needs for lipophilic pesticides and may be used for qualitative screening applications, in which any identified pesticides can be quantified and confirmed by a more intensive method that achieves >70% recoveries for lipophilic pesticides.

Analytical method for the evaluation of the outdoor air contamination by emerging pollutants using tree leaves as bioindicators.

PubMed

Barroso, Pedro José; Martín, Julia; Santos, Juan Luis; Aparicio, Irene; Alonso, Esteban

2018-01-01

In this work, an analytical method, based on sonication-assisted extraction, clean-up by dispersive solid-phase extraction and determination by liquid chromatography-tandem mass spectrometry, has been developed and validated for the simultaneous determination of 15 emerging pollutants in leaves from four ornamental tree species. Target compounds include perfluorinated organic compounds, plasticizers, surfactants, brominated flame retardant, and preservatives. The method was optimized using Box-Behnken statistical experimental design with response surface methodology and validated in terms of recovery, accuracy, precision, and method detection and quantification limits. Quantification of target compounds was carried out using matrix-matched calibration curves. The highest recoveries were achieved for the perfluorinated organic compounds (mean values up to 87%) and preservatives (up to 88%). The lowest recoveries were achieved for plasticizers (51%) and brominated flame retardant (63%). Method detection and quantification limits were in the ranges 0.01-0.09 ng/g dry matter (dm) and 0.02-0.30 ng/g dm, respectively, for most of the target compounds. The method was successfully applied to the determination of the target compounds on leaves from four tree species used as urban ornamental trees (Citrus aurantium, Celtis australis, Platanus hispanica, and Jacaranda mimosifolia). Graphical abstract Analytical method for the biomonitorization of emerging pollutants in outdoor air.

Effects of the different frequencies of whole-body vibration during the recovery phase after exhaustive exercise.

PubMed

Cheng, C F; Hsu, W C; Lee, C L; Chung, P K

2010-12-01

This study was to investigate the effects of vibration exercise on the oxygen consumption (VO2) and heart rate variability (HRV) during the recovery phase after exhaustive exercise. Twenty male college students volunteered as subjects to participate in the study. The subjects were randomly crossover assigned to perform three 10 min vibration exercises, namely non-vibration (CON, 0 Hz, 0 mm), low-frequency (LFT, 20 Hz, 0.4 mm) and high-frequency (HFT, 36 Hz, 0.4 mm) treatments immediately after an incremental exhaustive cycling exercise in separated days. The beat-to-beat HRV, blood lactate concentration and VO2 were measured during the 1-hour recovery phase. The time- and frequency-domain indices of HRV were analyzed to confirm the effects of vibration exercises on the cardiac autonomic modulation. There were no significant differences on the VO2, HRV and blood lactate concentrations at 30th minute (post-30 min) or 60th minute (post-60 min) during the recovery phase among the three treatments. There were also no significant differences on the excess post-exercise oxygen consumption (EPOC) during the recovery phase among the treatments. However, the VO2 at post-30 min in CON and LFT were significantly higher than the baseline values, whereas the VO2 in HFT returned to resting condition at the post-30 min. The results indicate that both low and high frequency vibration exercises could not improve the physiological recovery after exhaustive cycling exercise. However, the high frequency vibration exercise probably has a potential to facilitate the VO2 to return to the resting level during the recovery phase.

Steroid hormones in environmental matrices: extraction method comparison.

PubMed

Andaluri, Gangadhar; Suri, Rominder P S; Graham, Kendon

2017-11-09

The U.S. Environmental Protection Agency (EPA) has developed methods for the analysis of steroid hormones in water, soil, sediment, and municipal biosolids by HRGC/HRMS (EPA Method 1698). Following the guidelines provided in US-EPA Method 1698, the extraction methods were validated with reagent water and applied to municipal wastewater, surface water, and municipal biosolids using GC/MS/MS for the analysis of nine most commonly detected steroid hormones. This is the first reported comparison of the separatory funnel extraction (SFE), continuous liquid-liquid extraction (CLLE), and Soxhlet extraction methods developed by the U.S. EPA. Furthermore, a solid phase extraction (SPE) method was also developed in-house for the extraction of steroid hormones from aquatic environmental samples. This study provides valuable information regarding the robustness of the different extraction methods. Statistical analysis of the data showed that SPE-based methods provided better recovery efficiencies and lower variability of the steroid hormones followed by SFE. The analytical methods developed in-house for extraction of biosolids showed a wide recovery range; however, the variability was low (≤ 7% RSD). Soxhlet extraction and CLLE are lengthy procedures and have been shown to provide highly variably recovery efficiencies. The results of this study are guidance for better sample preparation strategies in analytical methods for steroid hormone analysis, and SPE adds to the choice in environmental sample analysis.

Gas phase recovery of hydrogen sulfide contaminated polymer electrolyte membrane fuel cells

NASA Astrophysics Data System (ADS)

Kakati, Biraj Kumar; Kucernak, Anthony R. J.

2014-04-01

The effect of hydrogen sulfide (H2S) on the anode of a polymer electrolyte membrane fuel cell (PEMFC) and the gas phase recovery of the contaminated PEMFC using ozone (O3) were studied. Experiments were performed on fuel cell electrodes both in an aqueous electrolyte and within an operating fuel cell. The ex-situ analyses of a fresh electrode; a H2S contaminated electrode (23 μmolH2S cm-2); and the contaminated electrode cleaned with O3 shows that all sulfide can be removed within 900 s at room temperature. Online gas analysis of the recovery process confirms the recovery time required as around 720 s. Similarly, performance studies of an H2S contaminated PEMFC shows that complete rejuvenation occurs following 600-900 s O3 treatment at room temperature. The cleaning process involves both electrochemical oxidation (facilitated by the high equilibrium potential of the O3 reduction process) and direct chemical oxidation of the contaminant. The O3 cleaning process is more efficient than the external polarization of the single cell at 1.6 V. Application of O3 at room temperature limits the amount of carbon corrosion. Room temperature O3 treatment of poisoned fuel cell stacks may offer an efficient and quick remediation method to recover otherwise inoperable systems.

A Sugar-Based Gelator for Marine Oil-Spill Recovery.

PubMed

Vibhute, Amol M; Muvvala, Venkatanarayana; Sureshan, Kana M

2016-06-27

Marine oil spills constitute an environmental disaster with severe adverse effects on the economy and ecosystem. Phase-selective organogelators (PSOGs), molecules that can congeal oil selectively from oil-water mixtures, have been proposed to be useful for oil-spill recovery. However, a major drawback lies in the mode of application of the PSOG to an oil spill spread over a large area. The proposed method of using carrier solvents is impractical for various reasons. Direct application of the PSOG as a solid, although it would be ideal, is unknown, presumably owing to poor dispersion of the solid through the oil. We have designed five cheap and easy-to-make glucose-derived PSOGs that disperse in the oil phase uniformly when applied as a fine powder. These gelators were shown to selectively congeal many oils, including crude oil, from oil-water mixtures to form stable gels, which is an essential property for efficient oil-spill recovery. We have demonstrated that these PSOGs can be applied aerially as a solid powder onto a mixture of crude oil and sea water and the congealed oil can then be scooped out. Our innovative mode of application and low cost of the PSOG offers a practical solution to oil-spill recovery. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Zero valent Fe-reduced graphene oxide quantum dots as a novel magnetic dispersive solid phase microextraction sorbent for extraction of organophosphorus pesticides in real water and fruit juice samples prior to analysis by gas chromatography-mass spectrometry.

PubMed

Akbarzade, Samaneh; Chamsaz, Mahmoud; Rounaghi, Gholam Hossein; Ghorbani, Mahdi

2018-01-01

A selective and sensitive magnetic dispersive solid-phase microextraction (MDSPME) coupled with gas chromatography-mass spectrometry was developed for extraction and determination of organophosphorus pesticides (Sevin, Fenitrothion, Malathion, Parathion, and Diazinon) in fruit juice and real water samples. Zero valent Fe-reduced graphene oxide quantum dots (rGOQDs@ Fe) as a new and effective sorbent were prepared and applied for extraction of organophosphorus pesticides using MDSPME method. In order to study the performance of this new sorbent, the ability of rGOQDs@ Fe was compared with graphene oxide and magnetic graphene oxide nanocomposite by recovery experiments of the organophosphorus pesticides. Several affecting parameters in the microextraction procedure, including pH of donor phase, donor phase volume, stirring rate, extraction time, and desorption conditions such as the type and volume of solvents and desorption time were thoroughly investigated and optimized. Under the optimal conditions, the method showed a wide linear dynamic range with R-square between 0.9959 and 0.9991. The limit of detections, the intraday and interday relative standard deviations (n = 5) were less than 0.07 ngmL -1 , 4.7, and 8.6%, respectively. The method was successfully applied for extraction and determination of organophosphorus pesticides in real water samples (well, river and tap water) and fruit juice samples (apple and grape juice). The obtained relative recoveries were in the range of 82.9%-113.2% with RSD percentages of less than 5.8% for all the real samples.

Spectrally resolved digital holography using a white light LED

NASA Astrophysics Data System (ADS)

Claus, D.; Pedrini, G.; Buchta, D.; Osten, W.

2017-06-01

This paper introduces the concept of spectrally resolved digital holography. The measurement principle and the analysis of the data will be discussed in detail. The usefulness of spectrally resolved digital holography is demonstrated for colour imaging and optical metrology with regards to the recovery of modulus information and phase information, respectively. The phase information will be used to measure the shape of an object via the application of the dual wavelength method. Based on the large degree of data available, multiple speckle de-correlated dual wavelength phase maps can be obtained, which when averaged result in a signal to noise ratio improvement.

Influence of relative permeabilities on chemical enhanced oil recovery

NASA Astrophysics Data System (ADS)

Destefanis, M. F.; Savioli, G. B.

2011-05-01

The main objective of chemical flooding is to mobilize the trapped oil remaining after a secondary recovery by waterflooding. This purpose is achieved by lowering the oil-water interfacial tension and producing partial miscibility between both phases. The chemical partition among phases (phase behavior) influences all other physical properties. In particular, it affects residual saturations determining relative permeability curves. Relative permeabilities rule the flow of each phase through the porous medium, so they play an essential role in oil recovery. Therefore, in this work we study the influence of relative permeabilities on the behavior of a surfactant-polymer flooding for the three different types of phase behavior. This analysis is performed applying the 3D compositional numerical simulator UTCHEM developed at the University of Texas at Austin. From the examples studied, we conclude that the influence of relative permeabilities depends on the type of phase behavior, i.e., as microemulsion relative permeability decreases, oil recovery increases for Types II(+) and III while slightly decreases for Type II(-). Moreover, a better displacement efficiency is observed for Types II(+) and III, because they behave similarly to a miscible displacement.

Determination of some metal ions in various meat and baby food samples by atomic spectrometry.

PubMed

Daşbaşı, Teslima; Saçmacı, Şerife; Ülgen, Ahmet; Kartal, Şenol

2016-04-15

In this paper, we report a simple and rapid solid phase extraction system for the separation/preconcentration and determination of Cd(II), Co(II), Cu(II), Fe(III), Cr(III), Pb(II), and Zn(II) ions by flame atomic absorption spectrometry (FAAS). This method is based upon the retention of metal ions on a column packed with poly[N-(3-methyl-1H-indole-1-yl)]-2-methacrylamide-co-2-acrylamido-2-methyl-1-propane sulphonic acid-co divinylbenzene] (MMAD) resin as a solid-phase extraction (SPE) sorbent at pH 8. At the optimized conditions, the limits of detection (3 s/b) between 0.12 and 1.6 μg L(-1), preconcentration factor of 100, and the relative standard deviation of ⩽1.8% were achieved (n=10). The accuracy of the method was verified by analyzing certified reference materials (CRMs) and performing recovery experiments. The developed method was successfully applied to the various natural water, meat products and baby food samples. The recoveries of analyte ions were found in added real samples and CRMs from 95% to 102%. Copyright © 2015 Elsevier Ltd. All rights reserved.

Contribution to the rheological testing of pharmaceutical semisolids.

PubMed

Siska, B; Snejdrova, E; Machac, I; Dolecek, P; Martiska, J

2018-01-22

Rheological behaviour of pharmaceutical semisolid preparations significantly affects manufacturing process, administration, stability, homogeneity of incorporated drug, accuracy of dosing, adhesion in the place of application, drug release, and resulting therapeutic effect of the product. We performed test of consistency by penetrometry, rotational, oscillation and creep tests, and squeeze and tack tests of model samples to introduce methods suitable for characterization and comparison of semisolids in practice. Penetrometry is a simple method allowing sorting the semisolids to low and high stress-resistant materials but deficient for rheological characterization of semisolids. Value of yield stress, generally considered to be appropriate feature of semisolids, is significantly influenced by the method of testing and the way of evaluation. The hysteresis loops of model semisolids revealed incomplete thixotropy, therefore, three-step thixotropy test was employed. Semisolids showed nonlinear response in the creep phase of tests and partial recovery of structure by storing energy in the recovery phase. Squeeze and tack tests seem to be convenient ways for comparison of semisolids. Our study can contribute to a better understanding of different flow behaviour of semisolids given by different physicochemical properties of excipients and can bring useful approaches to evaluation and comparison of semisolids in practice.

The Utilization of the Microflora Indigenous to and Present in Oil-Bearing Formations to Selectively Plug the More Porous Zones Thereby Increasing Oil Recovery During Waterflooding

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

Brown, Lewis R.; Byrnes, Martin J.; Stephens, James O.

This project was designed to demonstrate that a microbially enhanced oil recovery process (MEOR), developed in part under DOE Contract No. DE-AC22-90BC14665, will increase oil recovery from fluvial dominated deltaic oil reservoirs. The process involves stimulating the in-situ indigenous microbial population in the reservoir to grow in the more permeable zones, thus diverting flow to other areas of the reservoir, thereby increasing the effectiveness of the waterflood. This five and a half year project is divided into three phases, Phase I, Planning and Analysis (9 months), Phase II, Implementation (45 months), and Phase III, Technology Transfer (12 months). Phase Imore » was completed and reported in the first annual report. This fifth annual report covers the completion of Phase II and the first six months of Phase III.« less

Could aspiration of the Graafian follicle cause luteal phase deficiency?

PubMed

Feichtinger, W; Kemeter, P; Szalay, S; Beck, A; Janisch, H

1982-02-01

Luteal phase quality was evaluated in 32 patients wih nonstimulated cycles after laparoscopic oocyte recovery for in vitro fertilization. A luteal phase deficiency occurred in two cases (6.2%), the mean duration of the luteal phase was 13.5 +/- 1.3 days in 30 patients, and two patients developed amenorrhea of 23 and 43 days respectively after laparoscopy in spite of normal progesterone values 7 and 9 days after oocyte recovery. Six embryo transfers were performed after fertilization and regular cleavage of the obtained oocytes. No pregnancy resulted from the embryo transfers, although the patients had apparently normal luteal phases. In one patient there was a transient beta-subunit human chorionic gonadotropin (beta-hCG) elevation in serum. Luteal phase deficiency should not be main cause of a nonsuccessful embryo transfer. However, a prophylactic luteal phase support after oocyte recovery and embryo transfer in nonstimulated cycles is proposed.

Determination of pharmaceutical compounds in surface- and ground-water samples by solid-phase extraction and high-performance liquid chromatography-electrospray ionization mass spectrometry

USGS Publications Warehouse

Cahill, J.D.; Furlong, E.T.; Burkhardt, M.R.; Kolpin, D.; Anderson, L.G.

2004-01-01

Commonly used prescription and over-the-counter pharmaceuticals are possibly present in surface- and ground-water samples at ambient concentrations less than 1 μg/L. In this report, the performance characteristics of a combined solid-phase extraction isolation and high-performance liquid chromatography–electrospray ionization mass spectrometry (HPLC–ESI-MS) analytical procedure for routine determination of the presence and concentration of human-health pharmaceuticals are described. This method was developed and used in a recent national reconnaissance of pharmaceuticals in USA surface waters. The selection of pharmaceuticals evaluated for this method was based on usage estimates, resulting in a method that contains compounds from diverse chemical classes, which presents challenges and compromises when applied as a single routine analysis. The method performed well for the majority of the 22 pharmaceuticals evaluated, with recoveries greater than 60% for 12 pharmaceuticals. The recoveries of angiotensin-converting enzyme inhibitors, a histamine (H2) receptor antagonist, and antihypoglycemic compound classes were less than 50%, but were retained in the method to provide information describing the potential presence of these compounds in environmental samples and to indicate evidence of possible matrix enhancing effects. Long-term recoveries, evaluated from reagent-water fortifications processed over 2 years, were similar to initial method performance. Method detection limits averaged 0.022 μg/L, sufficient for expected ambient concentrations. Compound-dependent matrix effects on HPLC/ESI-MS analysis, including enhancement and suppression of ionization, were observed as a 20–30% increase in measured concentrations for three compounds and greater than 50% increase for two compounds. Changing internal standard and more frequent ESI source maintenance minimized matrix effects. Application of the method in the national survey demonstrates that several pharmaceuticals are routinely detected at 0.010–0.100 μg/L concentrations.

A HPLC-DAD method for the simultaneous determination of five marker components in the traditional herbal medicine Bangpungtongsung-san

PubMed Central

Weon, Jin Bae; Yang, Hye Jin; Ma, Jin Yeul; Ma, Choong Je

2011-01-01

Background: Bangpungtongsung-san, one of the traditional herbal medicines, was known to be a prescription for obesity. Objective: For the simultaneous determination of five components (paeoniflorin, 6-gingerol, decursin, geniposide, and glycyrrhizin) in Bangpungtongsung-san, a high-performance liquid chromatography with diode-array detector method was established. Materials and Methods: To develop the method, a reverse phase column, DIONEX C 18 (5 μm, 120 µ, 4.6 mm × 150 mm) was used. The mobile phase consisted of methanol and water using a gradient elution. The UV wavelength was set at 230, 240, and 254 nm. Method validation was accomplished by linearity, precision test, and recovery test. Results: All calibration curves of components showed good linearity (R 2 > 0.9959). The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.01 to 0.17 μg/ml and 0.04 to 0.53 μg/ml, respectively. The relative standard deviations (RSD) value of precision test, intraday and interday tests were less than 0.43% and 1.26%. In the recovery test, results of accuracy ranged from 95.27% to 107.70% with RSD values less than 2.21%. Conclusion: This developed method was applied to the commercial Bangpungtongsung-san sample and the five marker components were separated effectively without interference of any peaks of components. PMID:21472081

Improved method for the on-line metal chelate affinity chromatography-high-performance liquid chromatographic determination of tetracycline antibiotics in animal products.

PubMed

Cooper, A D; Stubbings, G W; Kelly, M; Tarbin, J A; Farrington, W H; Shearer, G

1998-07-03

An improved on-line metal chelate affinity chromatography-high-performance liquid chromatography (MCAC-HPLC) method for the determination of tetracycline antibiotics in animal tissues and egg has been developed. Extraction was carried out with ethyl acetate. The extract was then evaporated to dryness and reconstituted in methanol prior to on-line MCAC clean-up and HPLC-UV determination. Recoveries of tetracycline, oxytetracycline, demeclocycline and chlortetracycline in the range 42% to 101% were obtained from egg, poultry, fish and venison tissues spiked at 25 micrograms kg-1. Limits of detection less than 10 microgram kg-1 were estimated for all four analytes. This method has higher throughput, higher recovery and lower limits of detection than a previously reported on-line MCAC-HPLC method which involved aqueous extraction and solid-phase extraction clean-up.

Effects of sonication radiation on oil recovery by ultrasonic waves stimulated water-flooding.

PubMed

Mohammadian, Erfan; Junin, Radzuan; Rahmani, Omeid; Idris, Ahmad Kamal

2013-02-01

Due to partial understanding of mechanisms involved in application of ultrasonic waves as enhanced oil recovery method, series of straight (normal), and ultrasonic stimulated water-flooding experiments were conducted on a long unconsolidated sand pack using ultrasonic transducers. Kerosene, vaseline, and SAE-10 (engine oil) were used as non-wet phase in the system. In addition, a series of fluid flow and temperature rise experiments were conducted using ultrasonic bath in order to enhance the understanding about contributing mechanisms. 3-16% increase in the recovery of water-flooding was observed. Emulsification, viscosity reduction, and cavitation were identified as contributing mechanisms. The findings of this study are expected to increase the insight to involving mechanisms which lead to improving the recovery of oil as a result of application of ultrasound waves. Copyright © 2012 Elsevier B.V. All rights reserved.

Beneficiation and leaching study of a muti-Au carrier and low grade refractory gold ore

NASA Astrophysics Data System (ADS)

Li, W. J.; Song, Y. S.; Chen, Y.; Cai, L. L.; Zhou, G. Y.

2017-09-01

Detailed mineralogy and beneficiation and leaching study of a muti-Au carrier, low grade refractory gold ore from a beneficiation plant in Henan Province, China, was investigated. Mineral liberation analysis, scanning electron microscopy, element phase analysis and etc. by a mineral liberation analyser were used for mineralogical characterization study of this ore. The present work describes an experimental study on the effect of traditional parameters (such as grinding fineness and reagent regimes), middling processing method and flowsheet construction on the total recovery and the assay of the floatation concentrate. Two-step floatation and part of middling combined to the floatation tailing for gold leaching process resulted in high gold grade (g.t-1) and gold recovery (%) for this refractory gold ore. This process opens the possibilities of maximizing Au grade and recoveries in a muti-Au carrier and low grade refractory gold ore where low recoveries are common.

TOGA: A TOUGH code for modeling three-phase, multi-component, and non-isothermal processes involved in CO 2-based Enhanced Oil Recovery

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

Pan, Lehua; Oldenburg, Curtis M.

TOGA is a numerical reservoir simulator for modeling non-isothermal flow and transport of water, CO 2, multicomponent oil, and related gas components for applications including CO 2-enhanced oil recovery (CO 2-EOR) and geologic carbon sequestration in depleted oil and gas reservoirs. TOGA uses an approach based on the Peng-Robinson equation of state (PR-EOS) to calculate the thermophysical properties of the gas and oil phases including the gas/oil components dissolved in the aqueous phase, and uses a mixing model to estimate the thermophysical properties of the aqueous phase. The phase behavior (e.g., occurrence and disappearance of the three phases, gas +more » oil + aqueous) and the partitioning of non-aqueous components (e.g., CO 2, CH 4, and n-oil components) between coexisting phases are modeled using K-values derived from assumptions of equal-fugacity that have been demonstrated to be very accurate as shown by comparison to measured data. Models for saturated (water) vapor pressure and water solubility (in the oil phase) are used to calculate the partitioning of the water (H 2O) component between the gas and oil phases. All components (e.g., CO 2, H 2O, and n hydrocarbon components) are allowed to be present in all phases (aqueous, gaseous, and oil). TOGA uses a multiphase version of Darcy’s Law to model flow and transport through porous media of mixtures with up to three phases over a range of pressures and temperatures appropriate to hydrocarbon recovery and geologic carbon sequestration systems. Transport of the gaseous and dissolved components is by advection and Fickian molecular diffusion. New methods for phase partitioning and thermophysical property modeling in TOGA have been validated against experimental data published in the literature for describing phase partitioning and phase behavior. Flow and transport has been verified by testing against related TOUGH2 EOS modules and CMG. The code has also been validated against a CO 2-EOR experimental core flood involving flow of three phases and 12 components. Results of simulations of a hypothetical 3D CO 2-EOR problem involving three phases and multiple components are presented to demonstrate the field-scale capabilities of the new code. This user guide provides instructions for use and sample problems for verification and demonstration.« less

Method selection for sustainability assessments: The case of recovery of resources from waste water.

PubMed

Zijp, M C; Waaijers-van der Loop, S L; Heijungs, R; Broeren, M L M; Peeters, R; Van Nieuwenhuijzen, A; Shen, L; Heugens, E H W; Posthuma, L

2017-07-15

Sustainability assessments provide scientific support in decision procedures towards sustainable solutions. However, in order to contribute in identifying and choosing sustainable solutions, the sustainability assessment has to fit the decision context. Two complicating factors exist. First, different stakeholders tend to have different views on what a sustainability assessment should encompass. Second, a plethora of sustainability assessment methods exist, due to the multi-dimensional characteristic of the concept. Different methods provide other representations of sustainability. Based on a literature review, we present a protocol to facilitate method selection together with stakeholders. The protocol guides the exploration of i) the decision context, ii) the different views of stakeholders and iii) the selection of pertinent assessment methods. In addition, we present an online tool for method selection. This tool identifies assessment methods that meet the specifications obtained with the protocol, and currently contains characteristics of 30 sustainability assessment methods. The utility of the protocol and the tool are tested in a case study on the recovery of resources from domestic waste water. In several iterations, a combination of methods was selected, followed by execution of the selected sustainability assessment methods. The assessment results can be used in the first phase of the decision procedure that leads to a strategic choice for sustainable resource recovery from waste water in the Netherlands. Copyright © 2017 Elsevier Ltd. All rights reserved.

Simple Criteria to Determine the Set of Key Parameters of the DRPE Method by a Brute-force Attack

NASA Astrophysics Data System (ADS)

Nalegaev, S. S.; Petrov, N. V.

Known techniques of breaking Double Random Phase Encoding (DRPE), which bypass the resource-intensive brute-force method, require at least two conditions: the attacker knows the encryption algorithm; there is an access to the pairs of source and encoded images. Our numerical results show that for the accurate recovery by numerical brute-force attack, someone needs only some a priori information about the source images, which can be quite general. From the results of our numerical experiments with optical data encryption DRPE with digital holography, we have proposed four simple criteria for guaranteed and accurate data recovery. These criteria can be applied, if the grayscale, binary (including QR-codes) or color images are used as a source.

Task-related increases in fatigue predict recovery time after academic stress.

PubMed

Blasche, Gerhard; Zilic, Jelena; Frischenschlager, Oskar

2016-01-01

The aim of this study was to investigate the time course of recovery after an academic exam as a model of high workload and its association with stress-related fatigue. Thirty-six medical students (17 females, 19 males) filled out diaries during an exam phase, starting 2 days prior to the exam, and a control phase 4 weeks after the exam for 14 days, respectively. Fatigue, distress, quality of sleep, and health complaints were assessed. Recovery time was determined for each individual and variable by comparing the 3-day average with the confidence interval of the control phase. Recovery time was predicted by Cox regression analyses. Recovery times of all variables except health complaints were predicted by stress-related fatigue. Half of the individuals had recovered after 6 days, and 80% of the individuals had recovered after 8 days. The time necessary for recovery from work demands is determined by fatigue as a measure of resource depletion.

Recovery of uranium values

DOEpatents

Brown, K. B.; Crouse, Jr., D. J.; Moore, J. G.

1959-03-10

A liquid-liquid extraction method is presented for recovering uranium values from an aqueous acidic solution by means of certain high molecular weight amine fn the amine classes of primary, secondary, heterocyclic secondary, tertiary, or heterocyclic tertiary. The uranium bearing aqueous acidic solution is contacted with the selected anine dissolved in a nonpolar waterimmiscible organfc solvent such as kerosene. The uranium which is substantially completely extracted by the organic phase may be stripped therefrom by water, and recovered from the aqueous phase by treatment into ammonia to precipitate ammonium diuranate.

RECOVERY OF URANIUM VALUES

DOEpatents

Brown, K.B.; Crouse, D.J. Jr.; Moore, J.G.

1959-03-10

A liquid-liquid extraction method is presented for recovering uranium values from an aqueous acidic solution by means of certain high molecular weight amine in the amine classes of primary, secondary, heterocyclic secondary, tertiary, or heterocyclic tertiary. The uranium bearing aqueous acidic solution is contacted with the selected amine dissolved in a nonpolar water-immiscible organic solvent such as kerosene. The uranium which is substantially completely exiracted by the organic phase may be stripped therefrom by waters and recovered from the aqueous phase by treatment into ammonia to precipitate ammonium diuranate.

Development and Validation of HPLC Method for Determination of Crocetin, a constituent of Saffron, in Human Serum Samples

PubMed Central

Mohammadpour, Amir Hooshang; Ramezani, Mohammad; Tavakoli Anaraki, Nasim; Malaekeh-Nikouei, Bizhan; Amel Farzad, Sara; Hosseinzadeh, Hossein

2013-01-01

Objective(s): The present study reports the development and validation of a sensitive and rapid extraction method beside high performance liquid chromatographic method for the determination of crocetin in human serum. Materials and Methods: The HPLC method was carried out by using a C18 reversed-phase column and a mobile phase composed of methanol/water/acetic acid (85:14.5:0.5 v/v/v) at the flow rate of 0.8 ml/min. The UV detector was set at 423 nm and 13-cis retinoic acid was used as the internal standard. Serum samples were pretreated with solid-phase extraction using Bond Elut C18 (200mg) cartridges or with direct precipitation using acetonitrile. Results: The calibration curves were linear over the range of 0.05-1.25 µg/ml for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction. The mean recoveries of crocetin over a concentration range of 0.05-5 µg/ml serum for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction were above 70 % and 60 %, respectively. The intraday coefficients of variation were 0.37- 2.6% for direct precipitation method and 0.64 - 5.43% for solid-phase extraction. The inter day coefficients of variation were 1.69 – 6.03% for direct precipitation method and 5.13-12.74% for solid-phase extraction, respectively. The lower limit of quantification for crocetin was 0.05 µg/ml for direct precipitation method and 0.5 µg/ml for solid-phase extraction. Conclusion: The validated direct precipitation method for HPLC satisfied all of the criteria that were necessary for a bioanalytical method and could reliably quantitate crocetin in human serum for future clinical pharmacokinetic study. PMID:23638292

Sewage sludge as a fuel and raw material for phosphorus recovery: Combined process of gasification and P extraction.

PubMed

Gorazda, K; Tarko, B; Werle, S; Wzorek, Z

2018-03-01

Increasing problems associated with sewage sludge disposal are observed nowadays. As the thermal conversion of sewage sludge (combustion, co-combustion, gasification and pyrolysis) appears to be the most promising alternative for its management, the solid residues left after gasification were examined. The present study evaluates the potential of this waste as an alternative phosphorus source in the context of phosphorus recovery. The obtained solid gasification residues were characterised (chemical and phase composition, thermal properties, surface properties and technological parameters used for phosphorus raw materials) and compared to commercial phosphate raw materials. It was revealed that gasification residue is a valuable source of phosphorus and microelements, comparable to sewage sludge ash (SSA) considered nowadays as secondary phosphorus raw materials. Chemical properties as well as technological parameters characteristic for natural phosphate ores are different. Solid gasification residue was leached with mineral acids (phosphoric and nitric) according to the patented method of phosphorus recovery - PolFerAsh, developed by Cracow University of Technology. It was revealed that phosphorus can be selectively leached from solid gasification residue with high efficiency (73-82%); moreover, most of the iron and heavy metals stay in the solid phase due to the low concentration of acids and proper solid to liquid phase ratio. The obtained leachates are valuable products that can be considered for the production of fertilisers. Combining the gasification process with nutrient recovery provides the opportunity for more environmentally efficient technologies driven by sustainable development rules. Copyright © 2017 Elsevier Ltd. All rights reserved.

[HPLC method to determine DEHP released into blood from a disposable extracorporeal circulation tube].

PubMed

Liu, Xi; Yu, Jingjing; Li, Shen; Wang, Hong; Liu, Jiaxin

2013-08-01

We used blood as leaching medium, simulating clinical operation under maximum condition, to develop Liquid-phase extraction- High Performance Liquid Chromatography (HPLC) method for determination of plasticizer Di-(2-ethylhexyl)phthalate (DEHP) released from Disposable Extracorporeal Circulation Tube in order to lay the foundation of risk analysis of this product. The characteristic wavelength of DEHP in methanol was detected. Acetonitrile was added to the leaching blood in proportion and extracted DEHP from blood. The methodology for HPLC to quantify DEHP was established and the DEHP amount released from this disposable extracorporeal circulation tube was measured. The experiments showed good results as follows. The characteristic wavelength of DEHP was 272nm. The concentration of DEHP (5-250 microg/mL) kept good linear relationship with peak area (r=0.9999). Method sensitivity was 1 microg/mL. Precisions showed RSD<5%. The adding standard extraction Recovery Rates of 25, 100 and 250 microg DEHP standard were 61.91 +/- 3.32)%, (69.38 +/- 0.55)% and (68.47 +/- 1.15)%. The DEHP maximum amounts released from 3 sets of this disposable extracorporeal circulation tube were 204.14, 106.30 and 165.34 mg/set. Our Liquid-phase Extraction-HPLC method showed high accuracy and precision, and relatively stable recovery rate. Its operation was also convenient.

[Simultaneous determination of six fluorescent whitening agents in plastic and paper packaging materials by high performance liquid chromatography].

PubMed

Zhang, Juzhou; Ji, Shuilin; Cai, Huimei; Li, Jing; Wang, Yongxin; Wang, Jingqiu

2017-11-08

A novel analytical method was developed for the simultaneous determination of six fluorescent whitening agents (FWAs:FWA 135, FWA 184, FWA 185, FWA 199, FWA 378 and FWA 393) in paper and plastic food packaging materials by high performance liquid chromatography with fluorescence detection (HPLC-FLD). The sample was extracted with mixed solution of chloroform and acetonitrile (3:7, v/v), then cleaned up by HLB solid phase extraction column. Qualitative and quantitative analyses were carried out by HPLC. The sample was separated on a Phenomenex C18 column using acetonitrile and 5 mmol/L ammonium acetate aqueous solution as mobile phases. The results indicated that the linear range of FWA393 was 15-1500 μg/L and the linear ranges of the other five FWAs were 5-500 μg/L with correlation coefficients greater than 0.999. The recoveries in spiked samples were between 80.4% and 125.0% with RSDs ( n =6) of 1%-13%. Furthermore, this method was applied to analyze 12 samples in the market to verify the practicality of the method. The method showed the advantages of simplicity, high recovery and good precision, and is suitable for the detection of the six fluorescent whitening agents in food packaging materials.

Selective enrichment and determination of monoamine neurotransmitters by CU(II) immobilized magnetic solid phase extraction coupled with high-performance liquid chromatography-fluorescence detection.

PubMed

He, Maofang; Wang, Chaozhan; Wei, Yinmao

2016-01-15

In this paper, iminodiacetic acid-Cu(II) functionalized Fe3O4@SiO2 magnetic nanoparticles were prepared and used as new adsorbents for magnetic solid phase extraction (MSPE) of six monoamine neurotransmitters (MNTs) from rabbit plasma. The selective enrichment of MNTs at pH 5.0 was motivated by the specific coordination interaction between amino groups of MNTs and the immobilized Cu(II). The employed weak acidic extraction condition avoided the oxidation of MNTs, and thus facilitated operation and ensured higher recoveries. Under optimal conditions, the recoveries of six MNTs from rabbit plasma were in the range of 83.9-109.4%, with RSD of 2.0-10.0%. When coupled the Cu(II) immobilized MSPE with high-performance liquid chromatography-fluorescence detection, the method exhibited relatively lower detection limits than the previously reported methods, and the method was successfully used to determine the endogenous MNTs in rabbit plasma. The proposed method has potential application for the determination of MNTs in biological samples. Also, the utilization of coordination interaction to improve the selectivity might open another way to selectively enrich small alkaloids from complex samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of a solid-phase extraction method coupled with HPLC-UV detection for the determination of biogenic amines in Chinese rice wine.

PubMed

Zhang, Ying; Li, Yan; Zhu, Xiao-Juan; Li, Min; Chen, Hao-Yu; Lv, Xiao-Ling; Zhang, Jian

2017-07-01

A reliable and accurate method for the determination of seven biogenic amines (BAs) was developed and validated with Chinese rice wine samples. The BAs were derivatised with dansyl chloride, cleaned up using solid-phase extraction (SPE) and separated by high-performance liquid chromatography (HPLC) coupled with ultraviolet (UV) detection. The optimised derivatisation reaction, conducted at pH 9.6 and 60°C for 30 min, ensured baseline separation and peak symmetry for each BA. SPE clean-up using Oasis MCX cartridges yielded good recovery rates for all BAs and effectively reduced matrix effects. The developed method shows good linearity with determination coefficients of more than 0.9989 over a concentration range of 0.1-100 mg l -1 . The limits of detection (LODs) for the investigated BAs ranged from 2.07 to 5.56 µg l -1 . The intra- and inter-day relative standard deviations (RSDs) ranged from 0.86% to 3.81% and from 2.13% to 3.82%, respectively. Spiking experiments showed that the overall recovery rates ranged from 85% to 113%. Thus, the proposed method was demonstrated as being suitable for simultaneous detection, with accurate and precise quantification, of BAs in Chinese rice wine.

A sensitive and rapid determination of ranitidine in human plasma by HPLC with fluorescence detection and its application for a pharmacokinetic study.

PubMed

Ulu, Sevgi Tatar; Tuncel, Muzaffer

2012-04-01

A novel precolumn derivatization reversed-phase high-performance liquid chromatography method with fluorescence detection is described for the determination of ranitidine in human plasma. The method was based on the reaction of ranitidine with 4-fluoro-7-nitrobenzo-2-oxa-1,3-diazole forming yellow colored fluorescent product. The separation was achieved on a C(18) column using methanol-water (60:40, v/v) mobile phase. Fluorescence detection was used at the excitation and emission of 458 and 521 nm, respectively. Lisinopril was utilized as an internal standard. The flow rate was 1.2 mL/min. Ranitidine and lisinopril appeared at 3.24 and 2.25 min, respectively. The method was validated for system suitability, precision, accuracy, linearity, limit of detection, limit of quantification, recovery and robustness. Intra- and inter-day precisions of the assays were in the range of 0.01-0.44%. The assay was linear over the concentration range of 50-2000 ng/mL. The mean recovery was determined to be 96.40 ± 0.02%. This method was successfully applied to a pharmacokinetic study after oral administration of a dose (150 mg) of ranitidine. © The Author [2012]. Published by Oxford University Press. All rights reserved.

Sparse recovery of undersampled intensity patterns for coherent diffraction imaging at high X-ray energies

DOE PAGES

Maddali, S.; Calvo-Almazan, I.; Almer, J.; ...

2018-03-21

Coherent X-ray photons with energies higher than 50 keV offer new possibilities for imaging nanoscale lattice distortions in bulk crystalline materials using Bragg peak phase retrieval methods. However, the compression of reciprocal space at high energies typically results in poorly resolved fringes on an area detector, rendering the diffraction data unsuitable for the three-dimensional reconstruction of compact crystals. To address this problem, we propose a method by which to recover fine fringe detail in the scattered intensity. This recovery is achieved in two steps: multiple undersampled measurements are made by in-plane sub-pixel motion of the area detector, then this datamore » set is passed to a sparsity-based numerical solver that recovers fringe detail suitable for standard Bragg coherent diffraction imaging (BCDI) reconstruction methods of compact single crystals. The key insight of this paper is that sparsity in a BCDI data set can be enforced by recognising that the signal in the detector, though poorly resolved, is band-limited. This requires fewer in-plane detector translations for complete signal recovery, while adhering to information theory limits. Lastly, we use simulated BCDI data sets to demonstrate the approach, outline our sparse recovery strategy, and comment on future opportunities.« less

Sparse recovery of undersampled intensity patterns for coherent diffraction imaging at high X-ray energies

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

Maddali, S.; Calvo-Almazan, I.; Almer, J.

Coherent X-ray photons with energies higher than 50 keV offer new possibilities for imaging nanoscale lattice distortions in bulk crystalline materials using Bragg peak phase retrieval methods. However, the compression of reciprocal space at high energies typically results in poorly resolved fringes on an area detector, rendering the diffraction data unsuitable for the three-dimensional reconstruction of compact crystals. To address this problem, we propose a method by which to recover fine fringe detail in the scattered intensity. This recovery is achieved in two steps: multiple undersampled measurements are made by in-plane sub-pixel motion of the area detector, then this datamore » set is passed to a sparsity-based numerical solver that recovers fringe detail suitable for standard Bragg coherent diffraction imaging (BCDI) reconstruction methods of compact single crystals. The key insight of this paper is that sparsity in a BCDI data set can be enforced by recognising that the signal in the detector, though poorly resolved, is band-limited. This requires fewer in-plane detector translations for complete signal recovery, while adhering to information theory limits. Lastly, we use simulated BCDI data sets to demonstrate the approach, outline our sparse recovery strategy, and comment on future opportunities.« less

Sparse recovery of undersampled intensity patterns for coherent diffraction imaging at high X-ray energies.

PubMed

Maddali, S; Calvo-Almazan, I; Almer, J; Kenesei, P; Park, J-S; Harder, R; Nashed, Y; Hruszkewycz, S O

2018-03-21

Coherent X-ray photons with energies higher than 50 keV offer new possibilities for imaging nanoscale lattice distortions in bulk crystalline materials using Bragg peak phase retrieval methods. However, the compression of reciprocal space at high energies typically results in poorly resolved fringes on an area detector, rendering the diffraction data unsuitable for the three-dimensional reconstruction of compact crystals. To address this problem, we propose a method by which to recover fine fringe detail in the scattered intensity. This recovery is achieved in two steps: multiple undersampled measurements are made by in-plane sub-pixel motion of the area detector, then this data set is passed to a sparsity-based numerical solver that recovers fringe detail suitable for standard Bragg coherent diffraction imaging (BCDI) reconstruction methods of compact single crystals. The key insight of this paper is that sparsity in a BCDI data set can be enforced by recognising that the signal in the detector, though poorly resolved, is band-limited. This requires fewer in-plane detector translations for complete signal recovery, while adhering to information theory limits. We use simulated BCDI data sets to demonstrate the approach, outline our sparse recovery strategy, and comment on future opportunities.

Synthesis of g-C3N4/Fe3O4 nanocomposites and application as a new sorbent for solid phase extraction of polycyclic aromatic hydrocarbons in water samples.

PubMed

Wang, Man; Cui, Shihai; Yang, Xiaodi; Bi, Wentao

2015-01-01

An easy preparation of g-C3N4/Fe3O4 nanocomposites by chemical co-precipitation has been demonstrated. The as-prepared materials were characterized by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy and thermogravimetric analysis. The high affinity of g-C3N4 toward polycyclic aromatic hydrocarbons and the magnetic behavior of Fe3O4 were combined to provide an efficient and simple magnetic solid phase extraction (MSPE). The adsorption and desorption of polycyclic aromatic hydrocarbons on g-C3N4/Fe3O4 were examined. Different factors affecting the magnetic solid phase extraction of polycyclic aromatic hydrocarbons were assessed in terms of adsorption, desorption, and recovery. Under the optimized conditions, the proposed method showed good limits of detection (LOD, S/N=3) in the range of 0.05-0.1 ng mL(-1) and precision in the range of 1.8-5.3% (RSDs, n=3). This method was also successfully applied to the analysis of real water samples; good spiked recoveries over the range of 80.0-99.8% were obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

[Simultaneous determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography].

PubMed

Liu, Min; Li, Xiaolin; Bie, Wei; Wang, Minglin; Feng, Qian

2011-02-01

A new method was established for the determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol-water (1:1, v/v) and purified by a solid phase extraction column. Then, the chromatographic separation was achieved on a Luna C18 column by linear gradient elution. The mobile phase was 10 mmol/L ammonium acetate-acetonitrile (containing 1% acetic acid). The results showed that the 15 industrial synthetic dyes can be separated efficiently. The recoveries of the 15 industrial synthetic dyes spiked in condiment were between 84.6% and 114.2% with the relative standard deviations of 0.9% - 10.3%. The limits of detection of this method was 0.05 - 0.18 mg/kg for the 15 industrial synthetic dyes. The method is simple, sensitive, accurate, repeatable and can be used for simultaneous determination of the 15 illegally added industrial synthetic dyes.

Determination of 4-nonylphenol and 4-octylphenol in human blood samples by high-performance liquid chromatography with multi-electrode electrochemical coulometric-array detection.

PubMed

Inoue, K; Yoshimura, Y; Makino, T; Nakazawa, H

2000-11-01

Alkylphenols can affect human health because they disrupt the endocrine system. In this study, an analytical method for determining trace amounts of 4-nonylphenol (NP) and 4-octylphenol (OP) in human blood samples was developed. Reversed-phase HPLC with multi-electrode electrochemical coulometric-array detection was used for the determination of NP and OP in plasma and serum samples prepared with a solid-phase extraction method. The separation was achieved using an isocratic mobile phase of 0.7% phosphoric acid-acetonitrile with a C18 reversed phase column. The detection limits of NP and OP were 1.0 and 0.5 ng ml-1, respectively. The recoveries of NP and OP added to human plasma samples were above 70.0% with a relative standard deviation of less than 15.5%. The method was found to be applicable to the determination of NP and OP in various human blood samples such as serum and plasma.

Quantitative understanding of Forbush decrease drivers based on shock-only and CME-only models using global signature of February 14, 1978 event

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

Raghav, Anil; Lotekar, Ajay; Bhaskar, Ankush

We have studied the Forbush decrease (FD) event that occurred on February 14, 1978 using 43 neutron monitor observatories to understand the global signature of FD. We have studied rigidity dependence of shock amplitude and total FD amplitude. We have found almost the same power law index for both shock phase amplitude and total FD amplitude. Local time variation of shock phase amplitude and maximum depression time of FD have been investigated which indicate possible effect of shock/CME orientation. We have analyzed rigidity dependence of time constants of two phase recovery. Time constants of slow component of recovery phase showmore » rigidity dependence and imply possible effect of diffusion. Solar wind speed was observed to be well correlated with slow component of FD recovery phase. This indicates solar wind speed as possible driver of recovery phase. To investigate the contribution of interplanetary drivers, shock and CME in FD, we have used shock-only and CME-only models. We have applied these models separately to shock phase and main phase amplitudes respectively. This confirms presently accepted physical scenario that the first step of FD is due to propagating shock barrier and second step is due to flux rope of CME/magnetic cloud.« less

Determination of polychlorinated biphenyls in transformer oil using various adsorbents for solid phase extraction.

PubMed

Na, Yun-Cheol; Kim, Kang-Jin; Hong, Jongki; Seo, Jung-Ju

2008-08-01

Various adsorbents for a solid phase extraction (SPE) method were used to study their ability to separate PCBs from transformer oil to rapidly determine their sub-ppm concentration in the transformer oil. Approximately 90% of the transformer oil could be removed from the PCBs by using a hydrophilic-lipophilic balanced copolymer (HLB) adsorbent, but the recovery of deca-chlorobiphenyl (deca-CB) used as a surrogate was only 24.5% due to lose during this cleanup process. The use of a silica adsorbent gave good results with 89.9% recovery of the deca-CB. The recovery of Aroclor 1242 and 1260 were 95.4 and 90.3% on silica, and 98.9 and 83.5% on HLB, respectively. Acid treatment was an essential step in removing the ambiguous interference peaks to help identify the PCBs. A decreased sensitivity of the electron capture detection (ECD) for PCBs was observed due to the presence of the remaining trace oil after the workup procedure. This loss in sensitivity was allowed for by using tetrachloroxylene as an internal standard, and this was found to be reliable for the criteria of quality control by employing an experiment in which LCS was spiked with 2mg/l of Aroclor 1260 and analyzed each day over a 25 day period. The MDL for the analytical method established in this study is 0.05 mg/l.

Development and Validation of HPLC Method for Determination of Crocetin, a constituent of Saffron, in Human Serum Samples.

PubMed

Mohammadpour, Amir Hooshang; Ramezani, Mohammad; Tavakoli Anaraki, Nasim; Malaekeh-Nikouei, Bizhan; Amel Farzad, Sara; Hosseinzadeh, Hossein

2013-01-01

The present study reports the development and validation of a sensitive and rapid extraction method beside high performance liquid chromatographic method for the determination of crocetin in human serum. The HPLC method was carried out by using a C18 reversed-phase column and a mobile phase composed of methanol/water/acetic acid (85:14.5:0.5 v/v/v) at the flow rate of 0.8 ml/min. The UV detector was set at 423 nm and 13-cis retinoic acid was used as the internal standard. Serum samples were pretreated with solid-phase extraction using Bond Elut C18 (200mg) cartridges or with direct precipitation using acetonitrile. The calibration curves were linear over the range of 0.05-1.25 µg/ml for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction. The mean recoveries of crocetin over a concentration range of 0.05-5 µg/ml serum for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction were above 70 % and 60 %, respectively. The intraday coefficients of variation were 0.37- 2.6% for direct precipitation method and 0.64 - 5.43% for solid-phase extraction. The inter day coefficients of variation were 1.69 - 6.03% for direct precipitation method and 5.13-12.74% for solid-phase extraction, respectively. The lower limit of quantification for crocetin was 0.05 µg/ml for direct precipitation method and 0.5 µg/ml for solid-phase extraction. The validated direct precipitation method for HPLC satisfied all of the criteria that were necessary for a bioanalytical method and could reliably quantitate crocetin in human serum for future clinical pharmacokinetic study.

Examination of a modified cell cycle synchronization method and bovine nuclear transfer using synchronized early G1 phase fibroblast cells.

PubMed

Urakawa, Manami; Ideta, Atsushi; Sawada, Tokihiko; Aoyagi, Yoshito

2004-08-01

Somatic cell nuclear transfer has a low success rate, due to a high incidence of fetal loss and increased perinatal morbidity/mortality. One factor that may affect the successful development of nuclear transfer embryos is the cell cycle stage of the donor cell. In order to establish a cell cycle synchronization method that can consistently produce cloned embryos and offspring, we examined the effects of different combinations of three cell treatments on the recovery rate of mitotic phase cells using bovine fetal fibroblasts. In the first experiment, we examined the recovery rate of mitotic phase cells by a combination of treatment with a metaphase arrestant (1 microM 2-methoxyestradiol), shaking the plate and selecting cells with a diameter of 20 microns. As a result, 99% of mitotic phase cells were recovered by repeating the combined treatment of metaphase arrestant and shaking, and collection of cells with a specific diameter. In the second experiment, nuclear transfer was carried out using early G1 phase cells by choosing pairs of bridged cells derived from mitotic phase cells recovered by the combined treatment of 1 microM 2-methoxyestradiol and shaking, and collection of cells with a diameter of 20 microns. The reconstructed embryos were transferred to recipient heifers to determine post-implantation development. Development of embryos reconstructed from early G1 phase cells from the >/=6 cells stage on Day 3 to the morula-blastocyst stage on Day 6 was 100%. Ten blastocysts constructed from two cell lines were transferred into 10 recipient heifers. Nine of the 10 recipients delivered single live calves. In conclusion, mitotic phase bovine fibroblast cells were easily recovered by the combined treatments of 1 microM 2-methoxyestradiol, shaking, and selecting cells of the appropriate diameter. Furthermore, nuclear transfer using cells in the early G1 phase as donor cells gave a high rate of offspring production.

Quantitative estimation of itopride hydrochloride and rabeprazole sodium from capsule formulation.

PubMed

Pillai, S; Singhvi, I

2008-09-01

Two simple, accurate, economical and reproducible UV spectrophotometric methods and one HPLC method for simultaneous estimation of two component drug mixture of itopride hydrochloride and rabeprazole sodium from combined capsule dosage form have been developed. First developed method involves formation and solving of simultaneous equations using 265.2 nm and 290.8 nm as two wavelengths. Second method is based on two wavelength calculation, wavelengths selected for estimation of itopride hydrochloride was 278.0 nm and 298.8 nm and for rabeprazole sodium 253.6 nm and 275.2 nm. Developed HPLC method is a reverse phase chromatographic method using phenomenex C(18) column and acetonitrile: phosphate buffer (35:65 v/v) pH 7.0 as mobile phase. All developed methods obey Beer's law in concentration range employed for respective methods. Results of analysis were validated statistically and by recovery studies.

Quantitative Estimation of Itopride Hydrochloride and Rabeprazole Sodium from Capsule Formulation

PubMed Central

Pillai, S.; Singhvi, I.

2008-01-01

Two simple, accurate, economical and reproducible UV spectrophotometric methods and one HPLC method for simultaneous estimation of two component drug mixture of itopride hydrochloride and rabeprazole sodium from combined capsule dosage form have been developed. First developed method involves formation and solving of simultaneous equations using 265.2 nm and 290.8 nm as two wavelengths. Second method is based on two wavelength calculation, wavelengths selected for estimation of itopride hydrochloride was 278.0 nm and 298.8 nm and for rabeprazole sodium 253.6 nm and 275.2 nm. Developed HPLC method is a reverse phase chromatographic method using phenomenex C18 column and acetonitrile: phosphate buffer (35:65 v/v) pH 7.0 as mobile phase. All developed methods obey Beer's law in concentration range employed for respective methods. Results of analysis were validated statistically and by recovery studies. PMID:21394269

Are corticosteroids useful in all degrees of severity and rapid recovery of Bell's palsy?

PubMed

Ferreira, Margarida; Firmino, Machado J; Marques, Elisa A; Santos, Paula C; Duarte, José A

2016-07-01

Conclusions The results provide preliminary evidence that corticosteroids were not effective in all grades of dysfunction and for achieving a rapid remission in the early phase of BP, highlighting the need to define standard and rigorous criteria to prescribe corticosteroids in these patients. Objectives The main aim of this study was to investigate whether the use of corticosteroids better associated than paralleled with neuromuscular training (C + FNT) is more effective than facial neuromuscular training (FNT) applied alone, in terms of recovery degree and facial symmetry during the early phase of Bell's palsy (BP). Patients and methods A prospective single-blinded study involved 73 patients: the C + FNT group (n = 42; median age = 37.5 years) and FNT group (n = 31; median age = 49.0 years). Patients were assessed before and 6 weeks after treatment by House-Brackmann (HB-FGS) and Sunnybrook Facial Grading System (SB-FGS). Results Recovery degree and facial symmetry improved significantly in both groups (p < 0.001), without differences between groups (p > 0.05). However, the C + FNT group displayed better outcomes for cheek (p = 0.004) and mouth (p = 0.022) resting symmetry at SB-FGS, instead of compared to the FNT group. The corticosteroids had no significant effect on all recovery degrees (p = 0.992) and rapid remission (p = 0.952). Multiple linear regression analysis showed that the type of intervention was not a significant predictor for recovery degree (p = 0.917).

Tyrosine requirement during the rapid catch-up growth phase of recovery from severe childhood undernutrition

USDA-ARS?s Scientific Manuscript database

The requirement for aromatic amino acids, during the rapid catch-up in weight phase of recovery from severe childhood under nutrition (SCU) is not clearly established. As a first step, the present study aimed to estimate the tyrosine requirement of children with SCU during the catch-up growth phase ...

Continuation-Phase Cognitive Therapy's Effects on Remission and Recovery from Depression

ERIC Educational Resources Information Center

Vittengl, Jeffrey R.; Clark, Lee Anna; Jarrett, Robin B.

2009-01-01

The authors tested the effects of continuation-phase cognitive therapy (C-CT) on remission and recovery from recurrent major depressive disorder, defined as 6 weeks and 8 months, respectively, of continuously absent or minimal symptoms. Responders to acute-phase cognitive therapy were randomized to 8 months of C-CT (n = 41) or assessment control…

[Simultaneous determination of 22 typical pharmaceuticals and personal care products in environmental water using ultra performance liquid chromatography- triple quadrupole mass spectrometry].

PubMed

Wu, Chunying; Gu, Feng; Bai, Lu; Lu, Wenlong

2015-08-01

An analytical method for simultaneous determination of 22 typical pharmaceuticals and personal care products (PPCPs) in environmental water samples was developed by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). An Oasis HLB solid phase extraction cartridge, methanol as washing solution, water containing 0. 1% formic acid-methanol (7:3, v/v) as the mobile phases were selected for sample pretreatment and chromatographic separation. Based on the optimized sample pretreatment procedures and separation condition, the target recoveries ranged from 73% to 125% in water with the relative standard deviations ( RSDs) from 8.8% to 17.5%, and the linear ranges were from 2 to 2 000 µg/L with correlation coefficients (R2) not less than 0.997. The method can be applied to simultaneous determination of the 22 typical PPCPs in environmental water samples because of its low detection limits and high recoveries. It can provide support and help for the related research on water environmental risk assessment and control of the micro-organic pollutants.

Optimization of Analytical Conditions for a Rapid Determination of Aniline in Environmental Water by Liquid Chromatography/Tandem Mass Spectrometry.

PubMed

Furukawa, Koji; Hashimoto, Makoto; Kaneco, Satoshi

2017-01-01

A rapid determination of aniline in environmental water was examined based on liquid chromatography/tandem mass spectrometry (LC/MS/MS). Environmental water samples were diluted 20-fold with Mill-Q water and measured by LC/MS/MS after adding a surrogate substance (aniline-d 5 ). In the results of the present study, the calibration curve of aniline showed good linearity in the range of 0.05 - 2.0 μg/L. Since the RSD (repeatability) by measuring repeatedly an aniline standard solution (0.05 μg/L, n = 7) was 3.2%, the repeatability of this work was very excellent. In addition, the recovery rate of aniline in environmental water was in the range of 99.0 - 102% with RSD 3.4 - 7.7%, and very good recovery test results were obtained. From these results, this analytical method was confirmed to be effective for aniline measurements of environmental water samples. Also, it is possible to conduct rapid analyses of aniline in environmental water without any solid-phase extraction process, compared to the solid-phase extraction-GC/MS method.

Determination of acidic herbicides in surface water by solid-phase extraction followed by capillary zone electrophoresis.

PubMed

Qin, Weidong; Wei, Hongping; Li, Sam Fong Yau

2002-08-01

A rapid solid-phase extraction-capillary zone electrophoresis (CZE) method for determining 2,4-dichlorophenoxyacetic acid, 4-(2,4-dichlorophenoxy) butyric acid, and 2,4,5-trichlorophenoxyacetic acid in real water samples is described. Factors affecting the recoveries and detection of the targets are investigated. With samples being acidified to pH 2 and salted by sodium sulfate to 2% (w/w), an average recovery of greater than 85% is obtained using ethyl acetate as the eluent on an octadecylsilane-bonded silica cartridge. A running buffer of 5 mM sodium tetraborate in a water-acetonitrile mixture (70:30, v/v) adjusted to pH 9 is employed in the CZE analysis, and the targets can be analyzed within 7 min with good reproducibility and acceptable sensitivity. The method is suitable for detecting herbicide residues of sub-parts-per-billion levels in surface water. A local pond water is analyzed, and the concentrations of 2,4-dichlorophenoxyacetic acid and 4-(2,4-dichlorophenoxy) butyric acid are detected to be 0.27 +/- 0.03 ppb and 0.61 +/- 0.08 ppb, respectively.

Determination of sulfonamides in selected Malaysian swine wastewater by high-performance liquid chromatography.

PubMed

Malintan, Nancy T; Mohd, Mustafa Ali

2006-09-15

An analytical HPLC method for the simultaneous determination of eight sulfonamides in swine wastewater was developed. The samples were collected from three states in Malaysia. Sample clean up was carried out by employing solid-phase extraction using a 60 mg Oasis HLB (Waters) cartridge with 3 ml reservoir. The HPLC column used was Supelcosil C18 (250 mm x 4.6mm I.D.) and elution was carried out using gradient mode. The mobile phases used were acetonitrile and 0.5% acetic acid in purified water. Antibiotics were detected using UV absorbance at 272 nm. Recoveries obtained for sulphanilamide ranged from 31.9+/-5.1% to 36.2+/-1.0%, while recoveries for other sulfa drugs studied were from 91.9+/-5.0% to 106.0+/-1.1%. The limit of quantitation (LOQ) for sulfamerazine, sulfamethazine and sulfamethoxypyridazine was 7.5 ng/L, while the LOQ for the other studied antibiotics was 5.0 ng/L. The method was used to analyse sulfonamides in wastewater collected from selected Malaysian swine facilities.

Simultaneous determination of the HIV nucleoside analogue reverse transcriptase inhibitors lamivudine, didanosine, stavudine, zidovudine and abacavir in human plasma by reversed phase high performance liquid chromatography.

PubMed

Verweij-van Wissen, C P W G M; Aarnoutse, R E; Burger, D M

2005-02-25

A reversed phase high performance liquid chromatography method was developed for the simultaneous quantitative determination of the nucleoside reverse transcriptase inhibitors (NRTIs) lamivudine, didanosine, stavudine, zidovudine and abacavir in plasma. The method involved solid-phase extraction with Oasis MAX cartridges from plasma, followed by high performance liquid chromatography with a SymmetryShield RP 18 column and ultraviolet detection set at a wavelength of 260 nm. The assay was validated over the concentration range of 0.015-5 mg/l for all five NRTIs. The average accuracies for the assay were 92-102%, inter- and intra-day coefficients of variation (CV) were <2.5% and extraction recoveries were higher than 97%. This method proved to be simple, accurate and precise, and is currently in use in our laboratory for the quantitative analysis of NRTIs in plasma.

Allantoin as a solid phase adsorbent for removing endotoxins.

PubMed

Vagenende, Vincent; Ching, Tim-Jang; Chua, Rui-Jing; Gagnon, Pete

2013-10-04

In this study we present a simple and robust method for removing endotoxins from protein solutions by using crystals of the small-molecule compound 2,5-dioxo-4-imidazolidinyl urea (allantoin) as a solid phase adsorbent. Allantoin crystalline powder is added to a protein solution at supersaturated concentrations, endotoxins bind and undissolved allantoin crystals with bound endotoxins are removed by filtration or centrifugation. This method removes an average of 99.98% endotoxin for 20 test proteins. The average protein recovery is ∼80%. Endotoxin binding is largely independent of pH, conductivity, reducing agent and various organic solvents. This is consistent with a hydrogen-bond based binding mechanism. Allantoin does not affect protein activity and stability, and the use of allantoin as a solid phase adsorbent provides better endotoxin removal than anion exchange, polymixin affinity and biological affinity methods for endotoxin clearance. Copyright © 2013 Elsevier B.V. All rights reserved.

Differential carrier phase recovery for QPSK optical coherent systems with integrated tunable lasers.

PubMed

Fatadin, Irshaad; Ives, David; Savory, Seb J

2013-04-22

The performance of a differential carrier phase recovery algorithm is investigated for the quadrature phase shift keying (QPSK) modulation format with an integrated tunable laser. The phase noise of the widely-tunable laser measured using a digital coherent receiver is shown to exhibit significant drift compared to a standard distributed feedback (DFB) laser due to enhanced low frequency noise component. The simulated performance of the differential algorithm is compared to the Viterbi-Viterbi phase estimation at different baud rates using the measured phase noise for the integrated tunable laser.

Magnetic ionic liquid aqueous two-phase system coupled with high performance liquid chromatography: A rapid approach for determination of chloramphenicol in water environment.

PubMed

Yao, Tian; Yao, Shun

2017-01-20

A novel organic magnetic ionic liquid based on guanidinium cation was synthesized and characterized. A new method of magnetic ionic liquid aqueous two-phase system (MILATPs) coupled with high-performance liquid chromatography (HPLC) was established to preconcentrate and determine trace amount of chloramphenicol (CAP) in water environment for the first time. In the absence of volatile organic solvents, MILATPs not only has the excellent properties of rapid extraction, but also exhibits a response to an external magnetic field which can be applied to assist phase separation. The phase behavior of MILATPs was investigated and phase equilibrium data were correlated by Merchuk equation. Various influencing factors on CAP recovery were systematically investigated and optimized. Under the optimal conditions, the preconcentration factor was 147.2 with the precision values (RSD%) of 2.42% and 4.45% for intra-day (n=6) and inter-day (n=6), respectively. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.14ngmL -1 and 0.42ngmL -1 , respectively. Fine linear range of 12.25ngmL -1 -2200ngmL -1 was obtained. Finally, the validated method was successfully applied for the analysis of CAP in some environmental waters with the recoveries for the spiked samples in the acceptable range of 94.6%-99.72%. Hopefully, MILATPs is showing great potential to promote new development in the field of extraction, separation and pretreatment of various biochemical samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Sulfonated poly(styrene-divinylbenzene) modified with amines and the application for pipette-tip solid-phase extraction of carbendazim in apples.

PubMed

Ma, Yuxin; Liu, Lingling; Tang, Weiyang; Zhu, Tao

2017-10-01

Sulfonated poly(styrene-divinylbenzene) modified with five kinds of amine functional groups was applied to the determination of carbendazim in apple samples with a pipette-tip solid-phase extraction method. The structures of the polymers were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Five different modifications of the solid-phase extraction sorbent based on sulfonated poly(styrene-divinylbenzene) were tested under static and pipette-tip solid-phase extraction conditions. The polymer modified with p-methoxyaniline showed the best recognition capacity and adsorption amount for carbendazim. Under the optimum conditions, 3.00 mg of the adsorbent, 1.00 mL of ethyl acetate as washing solvent, and 1.00 mL of ammonia/acetonitrile (5:95, v/v) as elution solvent were used in the pretreatment procedure of apple samples. The calibration graphs of carbendazim in methanol were linear over 5.00-200.00 μg/mL, and the limits of detection and quantification were 0.01 and 0.03 μg/mL, respectively. The method recoveries of carbendazim were in the range of 91.31-98.13% with associated intraday relative standard deviations of 0.76-2.13% and interday relative standard deviations of 1.10-1.85%. Sulfonated poly(styrene-divinylbenzene) modified with p-methoxyaniline showed satisfactory results (recovery: 97.96%) and potential for the rapid purification of carbendazim in apple samples combined with the pipette-tip solid-phase extraction. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phase-and-amplitude recovery from a single phase-contrast image using partially spatially coherent x-ray radiation

NASA Astrophysics Data System (ADS)

Beltran, Mario A.; Paganin, David M.; Pelliccia, Daniele

2018-05-01

A simple method of phase-and-amplitude extraction is derived that corrects for image blurring induced by partially spatially coherent incident illumination using only a single intensity image as input. The method is based on Fresnel diffraction theory for the case of high Fresnel number, merged with the space-frequency description formalism used to quantify partially coherent fields and assumes the object under study is composed of a single-material. A priori knowledge of the object’s complex refractive index and information obtained by characterizing the spatial coherence of the source is required. The algorithm was applied to propagation-based phase-contrast data measured with a laboratory-based micro-focus x-ray source. The blurring due to the finite spatial extent of the source is embedded within the algorithm as a simple correction term to the so-called Paganin algorithm and is also numerically stable in the presence of noise.

Dissolved air flotation and centrifugation as methods for oil recovery from ruptured microalgal cells.

PubMed

Ghasemi Naghdi, Forough; Schenk, Peer M

2016-10-01

Solvent-free microalgal lipid recovery is highly desirable for safer, more sustainable and more economical microalgal oil production. Dispersed air flotation and centrifugation were evaluated for the ability to separate oil and debris from a slurry mixture of osmotically fractured Chaetoceros muelleri cells with and without utilizing collectors. Microalgal oil partially phase-separated as a top layer and partially formed an oil-in-water emulsion. Although collectors, such as sodium dodecyl sulphate enhanced selective flotation, by just adjusting the pH and cell concentration of the mixture, up to 78% of the lipids were recovered in the froth. Using centrifugation of fractured microalgal slurry resulted in removal of 60% cell debris and up to 68.5% of microalgal oil was present in the supernatant. Both methods, centrifugation and flotation provided options for separation of microalgal oil from C. muelleri slurry with similar fatty acid recoveries of 57% and 60%, respectively. Copyright © 2016. Published by Elsevier Ltd.

Extraction of anionic dye from aqueous solutions by emulsion liquid membrane.

PubMed

Dâas, Attef; Hamdaoui, Oualid

2010-06-15

In this work, the extraction of Congo red (CR), an anionic disazo direct dye, from aqueous solutions by emulsion liquid membrane (ELM) was investigated. The important operational parameters governing emulsion stability and extraction behavior of dye were studied. The extraction of CR was influenced by a number of variables such as surfactant concentration, stirring speed, acid concentration in the feed solution and volume ratios of internal phase to organic phase and of emulsion to feed solution. Under most favorable conditions, practically all the CR molecules present in the feed phase were extracted even in the presence of salt (NaCl). At the optimum experimental conditions, total removal of antharaquinonic dye Acid Blue 25 was attained after only 10 min. Influence of sodium carbonate concentration as internal receiving phase on the stripping efficiency of CR was examined. The best sodium carbonate concentration in the internal phase that conducted to excellent stripping efficiency (>99%) and emulsion stability was 0.1N. The membrane recovery was total and the permeation of CR was not decreased up to seven runs. ELM process is a promising alternative to conventional methods and should increase awareness of the potential for recovery of anionic dyes. Copyright 2010 Elsevier B.V. All rights reserved.

Coherent cavity-enhanced dual-comb spectroscopy.

PubMed

Fleisher, Adam J; Long, David A; Reed, Zachary D; Hodges, Joseph T; Plusquellic, David F

2016-05-16

Dual-comb spectroscopy allows for the rapid, multiplexed acquisition of high-resolution spectra without the need for moving parts or low-resolution dispersive optics. This method of broadband spectroscopy is most often accomplished via tight phase locking of two mode-locked lasers or via sophisticated signal processing algorithms, and therefore, long integration times of phase coherent signals are difficult to achieve. Here we demonstrate an alternative approach to dual-comb spectroscopy using two phase modulator combs originating from a single continuous-wave laser capable of > 2 hours of coherent real-time averaging. The dual combs were generated by driving the phase modulators with step-recovery diodes where each comb consisted of > 250 teeth with 203 MHz spacing and spanned > 50 GHz region in the near-infrared. The step-recovery diodes are passive devices that provide low-phase-noise harmonics for efficient coupling into an enhancement cavity at picowatt optical powers. With this approach, we demonstrate the sensitivity to simultaneously monitor ambient levels of CO₂, CO, HDO, and H₂O in a single spectral region at a maximum acquisition rate of 150 kHz. Robust, compact, low-cost and widely tunable dual-comb systems could enable a network of distributed multiplexed optical sensors.

Optimization of the freezing process for hematopoietic progenitor cells: effect of precooling, initial dimethyl sulfoxide concentration, freezing program, and storage in vapor-phase or liquid nitrogen on in vitro white blood cell quality.

PubMed

Dijkstra-Tiekstra, Margriet J; Setroikromo, Airies C; Kraan, Marcha; Gkoumassi, Effimia; de Wildt-Eggen, Janny

2014-12-01

Adding dimethyl sulfoxide (DMSO) to hematopoietic progenitor cells (HPCs) causes an exothermic reaction, potentially affecting their viability. The freezing method might also influence this. The aim was to investigate the effect of 1) precooling of DMSO and plasma (D/P) and white blood cell (WBC)-enriched product, 2) DMSO concentration of D/P, 3) freezing program, and 4) storage method on WBC quality. WBC-enriched product without CD34+ cells was used instead of HPCs. This was divided into six or eight portions. D/P (20 or 50%; precooled or room temperature [RT]) was added to the WBC-enriched product (precooled or RT), resulting in 10% DMSO, while monitoring temperature. The product was frozen using controlled-rate freezing ("fast-rate" or "slow-rate") and placed in vapor-phase or liquid nitrogen. After thawing, WBC recovery and viability were determined. Temperature increased most for precooled D/P to precooled WBC-enriched product, without influence of 20 or 50% D/P, but remained for all variations below 30°C. WBC recovery for both freezing programs was more than 95%. Recovery of WBC viability was higher for slow-rate freezing compared to fast-rate freezing (74% vs. 61%; p < 0.05) and also for 50% compared to 20% D/P (two test variations). Effect of precooling D/P or WBC-enriched product and of storage in vapor-phase or liquid nitrogen was marginal. Based on these results, precooling is not necessary. Fifty percent D/P is preferred over 20% D/P. Slow-rate freezing is preferred over fast-rate freezing. For safety reasons storage in vapor-phase nitrogen is preferred over storage in liquid nitrogen. Additional testing using real HPCs might be necessary. © 2014 AABB.

Development and validation of a solid phase extraction sample cleanup procedure for the recovery of trace levels of nitro-organic explosives in soil.

PubMed

Thomas, Jennifer L; Donnelly, Christopher C; Lloyd, Erin W; Mothershead, Robert F; Miller, Mark L

2018-03-01

An improved cleanup method has been developed for the recovery of trace levels of 12 nitro-organic explosives in soil, which is important not only for the forensic community, but also has environmental implications. A wide variety of explosives or explosive-related compounds were evaluated, including nitramines, nitrate esters, nitroaromatics, and a nitroalkane. Fortified soil samples were extracted with acetone, processed via solid phase extraction (SPE), and then analyzed by gas chromatography with electron capture detection. The following three SPE sorbents in cartridge format were compared: Empore™ SDB-XC, Oasis ® HLB, and Bond Elut NEXUS cartridges. The NEXUS cartridges provided the best overall recoveries for the 12 explosives in potting soil (average 48%) and the fastest processing times (<30min). It also rejected matrix components from spent motor oil on potting soil. The SPE method was validated by assessing limit of detection (LOD), processed sample stability, and interferences. All 12 compounds were detectable at 0.02μg explosive/gram of soil or lower in the three matrices tested (potting soil, sand, and loam) over three days. Seven explosives were stable up to seven days at 2μg/g and three were stable at 0.2μg/g, both in processed loam, which was the most challenging matrix. In the interference study, five interferences above the determined LOD for soil were detected in matrices collected across the United States and in purchased all-purpose sand, potting soil, and loam. This represented a 3.2% false positive rate for the 13 matrices processed by the screening method for interferences. The reported SPE cleanup method provides a fast and simple extraction process for separating organic explosives from matrix components, facilitating sample throughput and reducing instrument maintenance. In addition, a comparison study of the validated SPE method versus conventional syringe filtration was completed and highlighted the benefits of sample cleanup for removing matrix interferences, while also providing lower supply cost, order of magnitude lower LODs for most explosives, higher percent recoveries for complex matrices, and fewer instrument maintenance issues. Published by Elsevier B.V.

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

USGS Publications Warehouse

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

1984-01-01

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

Multi-residue method for the determination of 450 pesticide residues in honey, fruit juice and wine by double-cartridge solid-phase extraction/gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry.

PubMed

Pang, G-F; Fan, C-L; Liu, Y-M; Cao, Y-Z; Zhang, J-J; Fu, B-L; Li, X-M; Li, Z-Y; Wu, Y-P

2006-08-01

A multi-residue method was developed for the determination of 450 pesticide residues in honey, fruit juice and wine using double-cartridge solid-phase extraction (SPE), gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS). The method development was based on an appraisal of the characteristics of GC-MS and LC-MS-MS for 654 pesticides as well as the efficiency of extraction and purification from honey, fruit juice and wine. Samples were first diluted with water plus acetone, then extracted with portions of dichloromethane. The extracts were concentrated and cleaned up with graphitized carbon black and aminopropyl cartridges stacked in tandem. Pesticides were eluted with acetonitrile + toluene, and the eluates were concentrated. For 383 pesticides, the eluate was extracted with hexane twice and internal standard solution was added prior to GC-MS determination. For 67 pesticides, extraction was with methanol prior to LC-MS-MS determination. The limit of detection for the method was between 1.0 and 300 ng g(-1) depending on each pesticide analyte. At the three fortification levels of 2.0-3000 ng g(-1), the average recovery rates were between 59 and 123%, among which 413 pesticides (92% of the 450) had recovery rates of 70-120% and 35 pesticides (8% of the 450) had recovery rates of 59-70%. There were 437 pesticides (97% of the 450) with a relative standard deviation below 25%; there were 13 varieties (3% of the 450) between 25.0 and 30.4%.

[Determination of acacetin in Xiangjuganmao Keli (no sweet) by HPLC].

PubMed

Bian, Jia-Hong; Qian, Kun; Xu, Xiang; Shen, Jun

2006-11-01

To establish a method for the determination of acacetin in Xiangjuganmao Keli (no sweet). Acacetin in powdered herb was extracted by ultrasonator with methanol and was hydrolyzed with hydrochloric acid. Separation was accomplished on an ODS reversed phase column (5 microm, 4.6 x 250 mm) with a mobile phase of methanol-water-acetic acid(350: 150: 2). The detective wavelength was at 340 nm. The method was accurate, the results were stable and reproducible. The linear range of calibration cure was within the concentration of 2.00 - 10.00 microg/ml (r = 0.9998). The average extraction recovery was 99.9% (n = 6), RSD = 0.41% (n = 6). The method is simple, convenient, sensitive, and reproducible for quality control of Xiangjuganmao Keli (no sweet).

Determination of pyrazole and pyrrole pesticides in environmental water samples by solid-phase extraction using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography.

PubMed

Ma, Jiping; Lu, Xi; Xia, Yan; Yan, Fengli

2015-02-01

A solid-phase extraction (SPE) method using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography was developed for the determination of four pyrazole and pyrrole pesticides (fenpyroximate, chlorfenapyr, fipronil and flusilazole) in environmental water samples. Several parameters, such as extraction adsorbent, elution solvent and volume and sample loading flow rate were optimized to obtain high SPE recoveries and extraction efficiency. The calibration curves for the pesticides extracted were linear in the range of 0.05-10 μg L(-1) for chlorfenapyr and fenpyroximate and 0.05-20 μg L(-1) for fipronil and flusilazole, with the correlation coefficients (r(2)) between 0.9966 and 0.9990. The method gave good precisions (relative standard deviation %) from 2.9 to 10.1% for real spiked samples from reservoir water and seawater; method recoveries ranged 92.2-105.9 and 98.5-103.9% for real spiked samples from reservoir water and seawater, respectively. Limits of detection (S/N = 3) for the method were determined to be 8-19 ng L(-1). The optimized method was successfully applied to the determination of four pesticides of pyrazoles and pyrroles in real environmental water samples. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

PubMed

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

2018-03-01

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

[Multi-residue method for screening of pesticides in crops by liquid chromatography with tandem mass spectrometry].

PubMed

Tanizawa, Haruna; Shima, Mikie; Ikehara, Chieko; Kobata, Masakazu; Sato, Motoaki

2005-10-01

A simple and rapid method was developed for the screening of 82 pesticides/metabolites in a wide variety of crops, using solid-phase extraction and liquid chromatography with tandem mass spectrometry (LC/MS/MS). After extraction with methanol, the filtered extracts were made up to 100 mL and a 2 mL aliquot was subjected to solid-phase extraction. Co-extractives were removed with a C18 mini-column, while pesticides were retained on 3 kinds of mini-columns (HLB, SAX, activated carbon), and then eluted with acetonitrile. Analysis was performed by LC/MS/MS, and MS acquisition parameters were established in positive and negative ESI modes. The utility of the method was demonstrated by the analysis of 6 crops (carrot, cabbage, onion, spinach, lemon, brown rice) and one mixed vegetable juice. Of 82 compounds tested, 75 in carrot and 62 in lemon were obtained with recoveries ranging from 70-120%. For all samples tested, 75 compounds could be obtained with recoveries of over 50%, and the detection limits of most compounds were lower than 0.01 microg/g. This method provides acceptable performance for analysis of these 75 compounds. Further, by using aliquots of the extracts with small-scale mini-columns, purified samples could be obtained. This proposed method with small matrix effects, is effective and suitable for screening of multiple residual pesticides by using LC/MS/MS.

Dual-domain lateral shearing interferometer

DOEpatents

Naulleau, Patrick P.; Goldberg, Kenneth Alan

2004-03-16

The phase-shifting point diffraction interferometer (PS/PDI) was developed to address the problem of at-wavelength metrology of extreme ultraviolet (EUV) optical systems. Although extremely accurate, the fact that the PS/PDI is limited to use with coherent EUV sources, such as undulator radiation, is a drawback for its widespread use. An alternative to the PS/PDI, with relaxed coherence requirements, is lateral shearing interferometry (LSI). The use of a cross-grating, carrier-frequency configuration to characterize a large-field 4.times.-reduction EUV lithography optic is demonstrated. The results obtained are directly compared with PS/PDI measurements. A defocused implementation of the lateral shearing interferometer in which an image-plane filter allows both phase-shifting and Fourier wavefront recovery. The two wavefront recovery methods can be combined in a dual-domain technique providing suppression of noise added by self-interference of high-frequency components in the test-optic wavefront.

Diaion HP-2MG modified with 2-(2,6-dichlorobenzylideneamino) benzenethiol as new adsorbent for solid phase extraction and flame atomic absorption spectrometric determination of metal ions.

PubMed

Ghaedi, M; Montazerozohori, M; Haghdoust, S; Zaare, F; Soylak, M

2013-04-01

A solid phase extraction method for enrichment-separation and the determination of cobalt (Co(2+)), copper (Cu(2+)), nickel (Ni(2+)), zinc (Zn(2+)) and lead (Pb(2+)) ions in real samples has been proposed. The influences of some analytical parameters like pH, flow rate, eluent type and interference of matrix ions on recoveries of analytes were optimized. The limits of detection were found in the range of 1.6-3.9 µg L(-1), while preconcentration factor for all understudy metal ions were found to be 166 with loading half time (t 1/2) less than 10 min. The procedure was applied for the enrichment-separation of analyte ions in environmental samples with recoveries higher than 94.8% and relative SD <4.9% (N = 5).

Solid-phase extraction of heavy metal ions on bucky tubes disc in natural water and herbal plant samples.

PubMed

Soylak, Mustafa; Unsal, Yunus Emre

2011-10-01

A preconcentration-separation procedure has been established based on solid-phase extraction of Fe(III) and Pb(II) on bucky tubes (BTs) disc. Fe(III) and Pb(II) ions were quantitatively recovered at pH 6. The influences of the analytical parameters like sample volume, flow rates on the recoveries of analytes on BT disc were investigated. The effects of co-existing ions on the recoveries were also studied. The detection limits for iron and lead were found 1.6 and 4.9 μg L⁻¹, respectively. The validation of the presented method was checked by the analysis of TMDA-51.3 fortified water certified reference material. The presented procedure was successfully applied to the separation-preconcentration and determination of iron and lead content of some natural water and herbal plant samples from Kayseri, Turkey.

Flow in porous media, phase and ultralow interfacial tensions: Mechanisms of enhanced petroleum recovery

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

Davis, H.T.; Scriven, L.E.

1991-07-01

A major program of university research, longer-ranged and more fundamental in approach than industrial research, into basic mechanisms of enhancing petroleum recovery and into underlying physics, chemistry, geology, applied mathematics, computation, and engineering science has been built at Minnesota. The original focus was surfactant-based chemical flooding, but the approach taken was sufficiently fundamental that the research, longer-ranged than industrial efforts, has become quite multidirectional. Topics discussed are volume controlled porosimetry; fluid distribution and transport in porous media at low wetting phase saturation; molecular dynamics of fluids in ultranarrow pores; molecular dynamics and molecular theory of wetting and adsorption; new numericalmore » methods to handle initial and boundary conditions in immiscible displacement; electron microscopy of surfactant fluid microstructure; low cost system for animating liquid crystallites viewed with polarized light; surfaces of constant mean curvature with prescribed contact angle.« less

Determination of chlorinated acid herbicides in vegetation and soil by liquid chromatography/electrospray-tandem mass spectrometry.

PubMed

Schaner, Angela; Konecny, Jaclyn; Luckey, Laura; Hickes, Heidi

2007-01-01

The method presented uses reversed-phase liquid chromatography with negative electrospray ionization and tandem mass spectrometry to analyze 9 chlorinated acid herbicides in soil and vegetation matrixes: clopyralid, dicamba, MCPP, MCPA, 2,4-DP, 2,4-D, triclopyr, 2,4-DB, and picloram. A 20 g portion is extracted with a basic solution and an aliquot acidified and micropartitioned with 3 mL chloroform. Vegetation samples are subjected to an additional cleanup with a mixed-mode anion exchange solid-phase extraction cartridge. Two precursor product ion transitions per analyte are measured and evaluated to provide the maximum degree of confidence in results. Average recoveries for 3 different soil types tested ranged from 72 to 107% for all compounds with the exception of 2,4-DB at 56-99%. Average recoveries for the 3 different vegetation types studied were lower and ranged from 53 to 80% for all compounds.

Resilient distributed control in the presence of misbehaving agents in networked control systems.

PubMed

Zeng, Wente; Chow, Mo-Yuen

2014-11-01

In this paper, we study the problem of reaching a consensus among all the agents in the networked control systems (NCS) in the presence of misbehaving agents. A reputation-based resilient distributed control algorithm is first proposed for the leader-follower consensus network. The proposed algorithm embeds a resilience mechanism that includes four phases (detection, mitigation, identification, and update), into the control process in a distributed manner. At each phase, every agent only uses local and one-hop neighbors' information to identify and isolate the misbehaving agents, and even compensate their effect on the system. We then extend the proposed algorithm to the leaderless consensus network by introducing and adding two recovery schemes (rollback and excitation recovery) into the current framework to guarantee the accurate convergence of the well-behaving agents in NCS. The effectiveness of the proposed method is demonstrated through case studies in multirobot formation control and wireless sensor networks.

Determination of malachite green and its leuco form in water

USGS Publications Warehouse

Allen, J.L.; Meinertz, J.R.; Gofus, J.E.

1992-01-01

Liquid chromatographic (lc) analysis can detect malachite green residues in water at less than 10 mu-g/l. Water samples were concentrated on disposable diol columns, eluted with 0.05m P-toluene-sulfonic acid in methanol, and determined by reversed-phase lc. When combined with a lead oxide postcolumn reactor, the lc method can simultaneously determine both leuco and chromatic forms of malachite green. Recoveries averaged 95.4% For the chromatic form and 57.3% For the leuco form of malachite green oxalate and leuco malachite green in spiked pond water samples. Recoveries of the carbinol form of malachite green (an equilibrium product of the dye in water) from spiked tap water samples averaged 98.6%. Recoveries of leuco malachite green were low and ph-dependent.

RP-LC and TLC Densitometric Determination of Paracetamol and Pamabrom in Presence of Hazardous Impurity of Paracetamol and Application to Pharmaceuticals

PubMed Central

El-Houssini, Ola Mohamed

2013-01-01

Two simple, accurate and reproducible methods were developed and validated for the simultaneous determination of paracetamol (PARA) and pamabrom (PAMB) in pure form and in tablets. The first method was based on reserved-phase high-performance liquid chromatography, on a Thermo Hypersil ODS column using methanol:0.01 M sodium hexane sulfonate:formic acid (67.5:212.5:1 v/v/v) as the mobile phase. The flow rate was 2 mL/min and the column temperature was adjusted to 35 °C. Quantification was achieved with UV detection at 277 nm over concentration range of 100–600 and 4–24 μg/mL, with mean percentage recoveries were found to be 99.90 ± 0.586 and 99.26 ± 0.901 for PARA and PAMB, respectively. The second method was based on thin-layer chromatography separation of PARA and PAMB followed by densitometric measurement of the spots at 254 nm and 277 nm for PARA and PAMB respectively. Separation was carried out on aluminum sheet of silica gel 60F254 using dichloromethane:methanol:glacial acetic acid (7.5:1:0.5 v/v/v) as the mobile phase over concentration range of 1–10 and 0.32–3.20 μg per spot, with mean percentage recovery of 100.52 ± 1.332 and 99.71 ± 1.478 for PARA and PAMB, respectively. The methods retained their accuracy in presence of up to 50% of P-aminophenol and could be successfully applied in tablets. PMID:24046511

Exploring the Use of Thermal Infrared Imaging in Human Stress Research

PubMed Central

Grant, Joshua A.; Cardone, Daniela; Tusche, Anita; Singer, Tania

2014-01-01

High resolution thermal infrared imaging is a pioneering method giving indices of sympathetic activity via the contact-free recording of facial tissues (thermal imprints). Compared to established stress markers, the great advantage of this method is its non-invasiveness. The goal of our study was to pilot the use of thermal infrared imaging in the classical setting of human stress research. Thermal imprints were compared to established stress markers (heart rate, heart rate variability, finger temperature, alpha-amylase and cortisol) in 15 participants undergoing anticipation, stress and recovery phases of two laboratory stress tests, the Cold Pressor Test and the Trier Social Stress Test. The majority of the thermal imprints proved to be change-sensitive in both tests. While correlations between the thermal imprints and established stress markers were mostly non-significant, the thermal imprints (but not the established stress makers) did correlate with stress-induced mood changes. Multivariate pattern analysis revealed that in contrast to the established stress markers the thermal imprints could not disambiguate anticipation, stress and recovery phases of both tests. Overall, these results suggest that thermal infrared imaging is a valuable method for the estimation of sympathetic activity in the stress laboratory setting. The use of this non-invasive method may be particularly beneficial for covert recordings, in the study of special populations showing difficulties in complying with the standard instruments of data collection and in the domain of psychophysiological covariance research. Meanwhile, the established stress markers seem to be superior when it comes to the characterization of complex physiological states during the different phases of the stress cycle. PMID:24675709

Exploring the use of thermal infrared imaging in human stress research.

PubMed

Engert, Veronika; Merla, Arcangelo; Grant, Joshua A; Cardone, Daniela; Tusche, Anita; Singer, Tania

2014-01-01

High resolution thermal infrared imaging is a pioneering method giving indices of sympathetic activity via the contact-free recording of facial tissues (thermal imprints). Compared to established stress markers, the great advantage of this method is its non-invasiveness. The goal of our study was to pilot the use of thermal infrared imaging in the classical setting of human stress research. Thermal imprints were compared to established stress markers (heart rate, heart rate variability, finger temperature, alpha-amylase and cortisol) in 15 participants undergoing anticipation, stress and recovery phases of two laboratory stress tests, the Cold Pressor Test and the Trier Social Stress Test. The majority of the thermal imprints proved to be change-sensitive in both tests. While correlations between the thermal imprints and established stress markers were mostly non-significant, the thermal imprints (but not the established stress makers) did correlate with stress-induced mood changes. Multivariate pattern analysis revealed that in contrast to the established stress markers the thermal imprints could not disambiguate anticipation, stress and recovery phases of both tests. Overall, these results suggest that thermal infrared imaging is a valuable method for the estimation of sympathetic activity in the stress laboratory setting. The use of this non-invasive method may be particularly beneficial for covert recordings, in the study of special populations showing difficulties in complying with the standard instruments of data collection and in the domain of psychophysiological covariance research. Meanwhile, the established stress markers seem to be superior when it comes to the characterization of complex physiological states during the different phases of the stress cycle.

Trace analysis of endocrine disrupting compounds in environmental water samples by use of solid-phase extraction and gas chromatography with mass spectrometry detection.

PubMed

Azzouz, Abdelmonaim; Ballesteros, Evaristo

2014-09-19

A novel analytical method using a continuous solid-phase extraction system in combination with gas chromatography-mass spectrometry for the simultaneous separation and determination of endocrine disrupting compounds (EDCs) is reported. The method was applied to major EDCs of various types including parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in water. Samples were preconcentrated by using an automatic solid-phase extraction module containing a sorbent column, and retained analytes eluted with acetonitrile for derivatization with a mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane. A number of variables potentially influencing recovery of the target compounds such as the type of SPE sorbent (Silica gel, Florisil, RP-C18, Amberlite XAD-2 and XAD-4, Oasis HLB and LiChrolut EN), eluent and properties of the water including pH and ionic strength, were examined. LiChrolut EN was found to be the most efficient sorbent for retaining the analytes, with ∼100% efficiency. The ensuing method was validated with good analytical results including low limits of detection (0.01-0.08ng/L for 100mL of sample) and good linearity (r(2)>0.997) throughout the studied concentration ranges. The method exhibited good accuracy (recoveries of 90-101%) and precision (relative standard deviations less than 7%) in the determination of EDCs in drinking, river, pond, well, swimming pool and waste water. Waste water samples were found to contain the largest number and highest concentrations of analytes (3.2-390ng/L). Copyright © 2014 Elsevier B.V. All rights reserved.

Large-scale pesticide testing in olives by liquid chromatography-electrospray tandem mass spectrometry using two sample preparation methods based on matrix solid-phase dispersion and QuEChERS.

PubMed

Gilbert-López, Bienvenida; García-Reyes, Juan F; Lozano, Ana; Fernández-Alba, Amadeo R; Molina-Díaz, Antonio

2010-09-24

In this work we have evaluated the performance of two sample preparation methodologies for the large-scale multiresidue analysis of pesticides in olives using liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS). The tested sample treatment methodologies were: (1) liquid-liquid partitioning with acetonitrile followed by dispersive solid-phase extraction clean-up using GCB, PSA and C18 sorbents (QuEChERS method - modified for fatty vegetables) and (2) matrix solid-phase dispersion (MSPD) using aminopropyl as sorbent material and a final clean-up performed in the elution step using Florisil. An LC-MS/MS method covering 104 multiclass pesticides was developed to examine the performance of these two protocols. The separation of the compounds from the olive extracts was achieved using a short C18 column (50 mm x 4.6 mm i.d.) with 1.8 microm particle size. The identification and confirmation of the compounds was based on retention time matching along with the presence (and ratio) of two typical MRM transitions. Limits of detection obtained were lower than 10 microgkg(-1) for 89% analytes using both sample treatment protocols. Recoveries studies performed on olives samples spiked at two concentration levels (10 and 100 microgkg(-1)) yielded average recoveries in the range 70-120% for most analytes when QuEChERS procedure is employed. When MSPD was the choice for sample extraction, recoveries obtained were in the range 50-70% for most of target compounds. The proposed methods were successfully applied to the analysis of real olives samples, revealing the presence of some of the target species in the microgkg(-1) range. Besides the evaluation of the sample preparation approaches, we also discuss the use of advanced software features associated to MRM method development that overcome several limitations and drawbacks associated to MS/MS methods (time segments boundaries, tedious method development/manual scheduling and acquisition limitations). This software feature recently offered by different vendors is based on an algorithm that associates retention time data for each individual MS/MS transition, so that the number of simultaneously traced transitions throughout the entire chromatographic run (dwell times and sensitivity) is maximized. Copyright 2010 Elsevier B.V. All rights reserved.

"To See With My Own Eyes": Experiences of Family Visits During Phase 1 Recovery.

PubMed

Wendler, M Cecilia; Smith, Katherine; Ellenburg, Wanda; Gill, Rita; Anderson, Lea; Spiegel-Thayer, Kim

2017-02-01

Long separations are a characteristic of the day of surgery, keeping patients and their family members waiting and apart. At a time of high vulnerability, these separations can cause anxiety and worry. The purpose of this study was to identify the outcomes and experiences of patients and family members who engaged in a 5- to 10-minute supervised family visit during phase I postanesthesia recovery. This was a descriptive, single-group, mixed-methods study. Quantitative data, gathered on the day of surgery, was obtained from patients (vital signs, state anxiety scores) and their designated family members (state anxiety scores); satisfaction with the visit was also measured. An optional second, qualitative phase included a semi-structured interview examining the remembered experiences of patients and family members. A statistically significant drop in state anxiety was discovered after the visit, and satisfaction with the visit was exceedingly high. Qualitatively, patients and family members described their overwhelming relief to be able "to see with my own eyes" how well each was doing. This study supports that family visits in the postanesthesia care unit are safe and profoundly important as an independent nursing intervention. Recommendations include implementation of family visits during postanesthesia care unit recovery for all patients and family members who desire them. Copyright © 2016 American Society of PeriAnesthesia Nurses. Published by Elsevier Inc. All rights reserved.

Magnetic Field Observations of Partial Ring Current during Storm Recovery Phase

NASA Technical Reports Server (NTRS)

Le, Guan; Russell, C. T.; Slavin, J. A.; Lucek, E. A.

2007-01-01

We present results of an extensive survey of the magnetic field observations in the inner magnetosphere using 30 years of magnetospheric magnetic field data from Polar, Cluster, ISEE, and AMPTE/CCE missions. The purpose of this study is to understand the magnetic field evolution during the recovery phase of geomagnetic storms, and its implication to the ring current recovery and loss mechanisms of ring current particles. Our previous work on global ring current distribution [Le et al., 2004] has shown that a significant partial ring current is always present at all Dst levels (regardless of storm phases) even for quiet time ring current. The total current carried by the partial ring current is much stronger than (during stormtime) or at least comparable to (during quiet time) the symmetric ring current. It is now commonly believed that a strong partial ring current is formed during the storm main phase due to the enhanced earthward convection of energetic ions from nightside plasma sheet. But the presence of a strong partial ring current throughout the recovery phase remains controversial. The magnetic field generated by the ring current inflates the inner magnetosphere and causes magnetic field depressions in the equatorial magnetosphere. During the storm recovery phase, we find that the distribution of the equatorial magnetic field depression exhibits similar local time dependence as the ring current distribution obtained from the combined dataset in the earlier study. It shows that a strong partial ring current is a permanent feature throughout the recovery phase. In the early recovery phase, the partial ring current peaks near the dusk terminator as indicated by the peak of the magnetic field depression. As the recovery phase progresses, the partial ring current decays most quickly near the dusk and results in a dusk-to-midnight moving of the peak of the partial ring current. Thus the loss mechanisms work most effectively near the dusk. The magnetic field depression increases the gyroradius of ring current protons to a scale greater or comparable to the thickness of the magnetopause, which increases the chance of ion drift loss near the dusk magnetopause at larger L-shell (L>5). But the drift loss mechanism alone cannot explain the loss of ring current ions especially in the smaller L-shell (L<5). The precipitation loss due to wave-particle interaction is most likely the dominant loss mechanism in the small L-shell as it works most effectively at the same local time.

Characterization and recovery of copper values from discarded slag.

PubMed

Das, Bisweswar; Mishra, Barada Kanta; Angadi, Shivakumar; Pradhan, Siddharth Kumar; Prakash, Sandur; Mohanty, Jayakrushna

2010-06-01

In any copper smelter large quantities of copper slag are discarded as waste material causing space and environmental problems. This discarded slag contains important amounts of metallic values such as copper and iron. The recovery of copper values from an Indian smelter slag that contains 1.53% Cu, 39.8% Fe and 34.65% SiO(2) was the focus of the present study. A complete investigation of the different phases present in the slag has been carried out by means of optical microscopy, Raman spectroscopy, scanning electron microscopy (SEM), and X-ray diffraction (XRD) techniques. It is observed that iron and silica are mostly associated with the fayalite phase whereas copper is present in both oxide and sulfide phases. These oxide and sulfide phases of copper are mostly present within the slag phase and to some extent the slag is also embedded inside the oxide and sulfide phases. The recovery of copper values from the discarded slag has been explored by applying a flotation technique using conventional sodium isopropyl xanthate (SIX) as the collector. The effects of flotation parameters such as pH and collector concentration are investigated. Under optimum flotation conditions, it is possible to achieve 21% Cu with more than 80% recovery.

RF power recovery feedback circulator

DOEpatents

Sharamentov, Sergey I [Bolingbrook, IL

2011-03-29

A device and method for improving the efficiency of RF systems having a Reflective Load. In the preferred embodiment, Reflected Energy from a superconducting resonator of a particle accelerator is reintroduced to the resonator after the phase of the Reflected Energy is aligned with the phase of the Supply Energy from a RF Energy Source. In one embodiment, a Circulator is used to transfer Reflected Energy from the Reflective Load into a Phase Adjuster which aligns the phase of the Reflected Energy with that of the Supply Energy. The phase-aligned energy is then combined with the Supply Energy, and reintroduced into the Reflective Load. In systems having a constant phase shift, the Phase Adjuster may be designed to shift the phase of the Reflected Energy by a constant amount using a Phase Shifter. In systems having a variety (variable) phase shifts, a Phase Shifter controlled by a phase feedback loop comprising a Phase Detector and a Feedback Controller to account for the various phase shifts is preferable.

Method for the Determination of Aconitum Alkaloids in Dietary Supplements and Raw Materials by Reversed-Phase Liquid Chromatography with Ultraviolet Detection and Confirmation by Tandem Mass Spectrometry: Single-Laboratory Validation

PubMed Central

Tang, Wai-Tong; Wong, Sui-Kay; Law, Tin-Yau; Pang, Kwok-Chu; Sin, Della; Tam, Yin-King

2008-01-01

A study of single-laboratory validation (SLV) of a reversed-phase liquid Chromatography (RP-LC) method was conducted for the determination of diester-diterpene Aconitum alkaloids, viz., aconitine, mesaconitine, and hypaconitine, in a variety of dietary supplements, including single-arid multiple-ingredient dry powder extracts, pills, capsules, and raw materials. The Aconitum alkaloids in the samples were extracted by diethyl ether in the presence of ammonia. After cleanup with solid-phase extraction to remove the matrix interferences, the alkaloids were determined by RP-LC with UV detection at 235 nm, and the results were confirmed by tandem mass Spectrometry. The linear responses for aconitine, mesaconitine, and hypaconitine based on the present LC system ranged from 0.5 to 200 μg/mL. Relative standard deviations of 2.0 to 6.9% were obtained from duplicate analysis of 6 test materials of different matrixes for the 3 Aconitum alkaloids performed by 2 analysts on 5 different days. The recoveries determined for supplements and raw materials spiked with 3 Aconitum alkaloids at levels of 2.5–10 μg/g were in the range of 86–99%. In view of the attainment of satisfactory results for accuracy, precision, and recovery in the SLV study, it is recommended that the method validation process proceed to a collaborative study. PMID:17225594

Recovery of high-purity silver directly from dilute effluents by an emulsion liquid membrane-crystallization process.

PubMed

Tang, Bing; Yu, Guojun; Fang, Jianzhang; Shi, Taihong

2010-05-15

An emulsion liquid membrane (ELM)-crystallization process, using hypophosphorous acid as a reducing agent in the internal aqueous phase, has been developed for the purpose of recovering high-purity silver directly from dilute industrial effluents (waste rinse water). After pretreatment with HNO(3), silver in waste rinse water can be reliably recovered with high efficiency through the established process. The main parameters in the process of ELM-crystallization include the concentration of carrier in the membrane phase, the concentration of reducing agent in the internal aqueous phase, and the treatment ratio, which influence the recovery efficiency to various extents and must be controlled carefully. The results indicated that more than 99.5% (wt.) of the silver ions in the external aqueous phase were extracted by the ELM-crystallization process, with an average efficiency of recovery of 99.24% (wt.) and a purity of 99.92% (wt.). The membrane phase can be used repeatedly without loss of the efficiency of recovery. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Evaluation of analytical methodology for the detection of hormones and their attenuation during aquifer recharge and recovery cycles.

PubMed

de Lima Stebbins, Daniela; Docs, Jon; Lowe, Paula; Cohen, Jason; Lei, Hongxia

2016-05-18

The hormones listed in the screening survey list 2 of the Unregulated Contaminant Monitoring Rule 3 (estrone, 17-β-estradiol, 17-α-ethynylestradiol, 16-α-hydroxyestradiol (estriol), equilin, testosterone and 4-androstene-3,17-dione) were analyzed by liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Two analytical methods were compared: EPA method 539 and the isotope dilution method. EPA method 539 was successfully utilized in river and drinking water matrices with fortified recoveries of 98.9 to 108.5%. Samples from the Hillsborough River reflected levels below the method detection limit (MDL) for the majority of the analytes, except estrone (E1), which was detected at very low concentrations (<0.5 to 1 ng L(-1)) in the majority of samples. No hormones were detected in drinking water samples. The isotope dilution method was used to analyze reclaimed and aquifer storage and recovery (ASR) water samples as a result of strong matrix/solid phase extraction (SPE) losses observed in these more complex matrices. Most of the compounds were not detected or found at relatively low concentrations in the ASR samples. Attenuation of 50 to 99.1% was observed as a result of the ASR recharge/recovery cycles for most of the hormones, except for estriol (E3). Relatively stable concentrations of E3 were found, with only 10% attenuation at one of the sites and no measureable attenuation at another location. These results have substantiated that while EPA method 539 works well for most environmental samples, the isotope dilution method is more robust when dealing with complex matrices such as reclaimed and ASR samples.

Comparison of UV spectrophotometry and high performance liquid chromatography methods for the determination of repaglinide in tablets

PubMed Central

Dhole, Seema M.; Khedekar, Pramod B.; Amnerkar, Nikhil D.

2012-01-01

Background: Repaglinide is a miglitinide class of antidiabetic drug used for the treatment of type 2 diabetes mellitus. A fast and reliable method for the determination of repaglinide was highly desirable to support formulation screening and quality control. Objective: UV spectrophotometric and reversed-phase high performance liquid chromatography (RP-HPLC) methods were developed for determination of repaglinide in the tablet dosage form. Materials and Methods: The UV spectrum recorded between 200 400 nm using methanol as solvent and the wavelength 241 nm was selected for the determination of repaglinide. RP-HPLC analysis was carried out using Agilent TC-C18 (2) column and mobile phase composed of methanol and water (80:20 v/v, pH adjusted to 3.5 with orthophosphoric acid) at a flow rate of 1.0 ml/min. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the International Conference on Harmonization (ICH) guidelines. Results: The developed methods illustrated excellent linearity (r2 > 0.999) in the concentration range of 5-30 μg/ml and 5-50 μg/ml for UV spectrophotometric and HPLC methods, respectively. Precision (%R.S.D < 1.50) and mean recoveries were found in the range of 99.63-100.45% for UV spectrophotometric method and 99.71-100.25% for HPLC method which shows accuracy of the methods. Conclusion: The developed methods were found to be reliable, simple, fast, accurate and successfully used for the quality control of repaglinide as a bulk drug and in pharmaceutical formulations. PMID:23781481

Bonded-phase extraction column isolation of organic compounds in groundwater at a hazardous waste site

USGS Publications Warehouse

Rostad, C.E.; Pereira, W.E.; Ratcliff, S.M.

1984-01-01

A procedure for isolation of hazardous organic compounds from water for gas chromatography/mass spectrometry analysis Is presented and applied to creosote- and pentachlorophenol-contaminated groundwater resulting from wood-treatment processes. This simple procedure involved passing a 50-100-mL sample through a bonded-phase extraction column, eluting the trapped organic compounds from the column with 2-4 mL of solvent, and evaporating the sample to 100 ??L with a stream of dry nitrogen, after which the sample was ready for gas chromatography/mass spectrometry analysis. Representative compounds indicative of creosote contamination were used for recovery and precision studies from the cyclohexyl-bonded phase. Recovery of these compounds from n-octyl-, n-octadecyl-, cyclohexyl-, and phenyl-bonded phases was compared. The bonded phase that exhibited the best recovery and least bias toward acidic or basic cmpounds was the n-octadecyl phase. Detailed compound Identification Is given for compounds Isolated from creosote- and pentachlorophenol-contaminated groundwater using the cyclohexyl-bonded phase.

Characterization of free thiol variants of an IgG1 by reversed phase ultra high pressure liquid chromatography coupled with mass spectrometry.

PubMed

Liu, Hongbin; Jeong, Justin; Kao, Yung-Hsiang; Zhang, Yonghua Taylor

2015-05-10

RP-HPLC has been demonstrated as a powerful tool to study antibody free thiol and disulfide variants. Recently, the introduction of UHPLC columns with wide pore size (300Å) and small particle size (1.7μm) offered the opportunity to further improve the separation of such variants. This paper describes a systematic evaluation of stationary phases, operating parameters, and mobile phases for a UHPLC based method to separate free thiol variants of a recombinant monoclonal antibody (referred as mAb A), targeting high resolution, high throughput and improved recovery. Among the four different stationary phases evaluated, UHPLC diphenyl columns were found to provide the best separation. Using an optimized UHPLC method, free thiol variants of mAb A were separated in 5min. Importantly, the UHPLC method revealed minor variants that had coeluted in an HPLC based method, and the UHPLC method is also applicable as a platform method for characterization of other mAbs as well. Furthermore, an on-line UHPLC-MS method was developed to characterize the separated variants, and this method can streamline the characterization of fully assembled monoclonal and bispecific therapeutic antibodies. Copyright © 2015 Elsevier B.V. All rights reserved.

Purification of pectinase from mango (Mangifera indica L. cv. Chokanan) waste using an aqueous organic phase system: a potential low cost source of the enzyme.

PubMed

Amid, Mehrnoush; Abdul Manap, Mohd Yazid; Mustafa, Shuhaimi

2013-07-15

As a novel method of purification, an aqueous organic phase system (AOPS) was employed to purify pectinase from mango waste. The effect of different parameters, such as the alcohol concentration (ethanol, 1-propanol, and 2-propanol), the salt type and concentration (ammonium sulfate, potassium phosphate and sodium citrate), the feed stock crude load, the aqueous phase pH and NaCl concentration, were investigated in the recovery of pectinase from mango peel. The partition coefficient (K), selectivity (S), purification factor (PF) and yield (Y, %) were investigated in this study as important parameters for the evaluation of enzyme recovery. The desirable partition efficiency for pectinase purification was achieved in an AOPS of 19% (w/w) ethanol and 22% (w/w) potassium phosphate in the presence of 5% (w/w) NaCl at pH 7.0. Based on the system, the purification factor of pectinase was enhanced 11.7, with a high yield of 97.1%. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Optimization and application of parallel solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of 11 aminoglycoside residues in honey and royal jelly.

PubMed

Wang, Xinran; Yang, Shupeng; Li, Yi; Zhang, Jinzhen; Jin, Yue; Zhao, Wen; Zhang, Yongxin; Huang, Jingping; Wang, Peng; Wu, Cuiling; Zhou, Jinhui

2018-03-23

A robust and sensitive method of solid-phase extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established and performed for the simultaneous determination of eleven aminoglycosides (AGs) in royal jelly and honey. After sample extraction by a phosphate buffer containing trichloroacetic acid (TCA) and ethylenediaminetetracetic acid disodium salt (Na 2 EDTA), the extraction solution was subjected to a parallel solid-phase extraction for clean-up prior to the LC-MS/MS analysis. The same method was applied to analyze two completely different matrices, honey and royal jelly. Good sensitivity, repeatability, and recovery were obtained by using the mobile phase without an ion-pairing reagent such as heptafluorobutyric acid (HFBA) or sodium heptanesulfonate. The calibration curves of the honey and royal jelly samples exhibited a good linear response (R 2  > 0.99) at six concentrations in the range of 10-1000 μg/mL. The limit of quantification (LOQ) of the AGs ranged from 10 to 25 μg/kg in the honey and from 12.5 to 25 μg/kg in the royal jelly. The recoveries of the AGs for the honey and royal jelly samples were in the range of 79.48% to 108.95% and 74.61% to 113.70% respectively and the relative standard deviations (RSDs) were between 1.23% and 9.59%, and between 1.51% and 9.98%, respectively. The proposed approach has been allowed in China as a reference method for the simultaneous determination of eleven AGs in honey and royal jelly. Copyright © 2018 Elsevier B.V. All rights reserved.

[Analysis of the preferred conformations and determination of the concentrations of ephedrine and pseudoephedrine based on hollow fiber liquid-phase microextraction].

PubMed

Chen, Xuan; Bai, Xiaohong; Wang, Xiao; Wang, Jing; Bu, Wei

2010-12-01

The preferred conformations of the ephedrine and pseudoephedrine in Ephedra sinica Stapf and rat urine were analyzed by the hollow fiber liquid-phase microextraction (HF-LPME) and their extraction mechanisms were illuminated. The method of the separation of the ephedrine and pseudoephedrine and the determination of their concentrations with high performance liquid chromatography (HPLC) were established. The optimal experimental conditions were as follows: the organic phase carrier was the hollow fiber of polyvinylidene fluoride (MOF-503), organic solvent was n-hexanol, the extraction time was 35 min, the stirring rate was 1200 r/min, the sample phase was the NaOH solution (5 mol/L) of the analyte, the acceptor was 0.01 mol/L H2SO4 solution. The extracts were analyzed by HPLC. Under the optimal conditions, the method is convenient and highly sensitive. In Ephedra sinica Stapf, the linear ranges of ephedrine and pseudoephedrine were 5-100 microg/L, the detection limits were 1.9 microg/L and 1.2 microg/L and the enrichment factors were 38 and 61, respectively. The average recoveries of ephedrine and pseudoephedrine were 100.6% +/- 1.2% and 103.2% +/- 3.5%, respectively. In rat urine, their linear ranges were 100 - 5 x 10(4) microg/L, the detection limits were 30 microg/L and 42 microg/L and the enrichment factors were 20 and 17, respectively. In rat urine, their average recoveries were 108.4% +/- 4.4% and 106. 1% +/- 5.4%, respectively. The obtained results indicated that the method can be successfully applied for the extraction and determination of the ephedrine and pseudoephedrine in Ephedra sinica Stapf and rat urine.

High Fidelity Computational Analysis of CO2 Trapping at Pore Scales

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

Kumar, Vinod

2013-07-13

With an alarming rise in carbon dioxide (CO2) emission from anthropogenic sources, CO2 sequestration has become an attractive choice to mitigate the emission. Some popular storage media for CO{sub 2} are oil reservoirs, deep coal-bed, and deep oceanic-beds. These have been used for the long term CO{sub 2} storage. Due to special lowering viscosity and surface tension property of CO{sub 2}, it has been widely used for enhanced oil recovery. The sites for CO{sub 2} sequestration or enhanced oil recovery mostly consist of porous rocks. Lack of knowledge of molecular mobility under confinement and molecule-surface interactions between CO2 and naturalmore » porous media results in generally governed by unpredictable absorption kinetics and total absorption capacity for injected fluids, and therefore, constitutes barriers to the deployment of this technology. Therefore, it is important to understand the flow dynamics of CO{sub 2} through the porous microstructures at the finest scale (pore-scale) to accurately predict the storage potential and long-term dynamics of the sequestered CO{sub 2}. This report discusses about pore-network flow modeling approach using variational method and analyzes simulated results this method simulations at pore-scales for idealized network and using Berea Sandstone CT scanned images. Variational method provides a promising way to study the kinetic behavior and storage potential at the pore scale in the presence of other phases. The current study validates variational solutions for single and two-phase Newtonian and single phase non-Newtonian flow through angular pores for special geometries whose analytical and/or empirical solutions are known. The hydraulic conductance for single phase flow through a triangular duct was also validated against empirical results derived from lubricant theory.« less

Chemical systems for improved oil recovery: Phase behavior, oil recovery, and mobility control studies

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

Llave, F.; Gall, B.; Gao, H., Scott, L., Cook, I.

Selected surfactant systems containing a series of ethoxylated nonionic surfactants in combination with an anionic surfactant system have been studied to evaluate phase behavior as well as oil recovery potential. These experiments were conducted to evaluate possible improved phase behavior and overall oil recovery potential of mixed surfactant systems over a broad range of conditions. Both polyacrylamide polymers and Xanthan biopolymers were evaluated. Studies were initiated to use a chemical flooding simulation program, UTCHEM, to simulate oil recovery for laboratory and field applications and evaluate its use to simulate oil saturation distributions obtained in CT-monitoring of oil recovery experiments. Themore » phase behavior studies focused on evaluating the effect of anionic-nonionic surfactant proportion on overall phase behavior. Two distinct transition behaviors were observed, depending on the dominant surfactant in the overall system. The first type of transition corresponded to more conventional behavior attributed to nonionic-dominant surfactant systems. This behavior is manifested by an oil-water-surfactant system that inverts from a water-external (highly conducting) microemulsion to an oil-external (nonconducting) one, as a function of temperature. The latter type which inverts in an opposite manner can be attributed to the separation of the anionic-nonionic mixtures into water- and oil-soluble surfactants. Both types of transition behavior can still be used to identify relative proximity to optimal areas. Determining these transition ranges provided more insight on how the behavior of these surfactant mixtures was affected by altering component proportions. Efforts to optimize the chemical system for oil displacement experiments were also undertaken. Phase behavior studies with systems formulated with biopolymer in solution were conducted.« less

The Exploration Water Recovery System

NASA Technical Reports Server (NTRS)

ORourke, Mary Jane E.; Carter, Layne; Holder, Donald W.; Tomes, Kristin M.

2006-01-01

The Exploration Water Recovery System is designed towards fulfillment of NASA s Vision for Space Exploration, which will require elevation of existing technologies to higher levels of optimization. This new system, designed for application to the Exploration infrastructure, presents a novel combination of proven air and water purification technologies. The integration of unit operations is modified from that of the current state-of-the-art water recovery system so as to optimize treatment of the various waste water streams, contaminant loads, and flow rates. Optimization is achieved primarily through the removal of volatile organic contaminants from the vapor phase prior to their absorption into the liquid phase. In the current state-of-the-art system, the water vapor in the cabin atmosphere is condensed, and the volatile organic contaminants present in that atmosphere are absorbed into the aqueous phase. Removal of contaminants the5 occurs via catalytic oxidation in the liquid phase. Oxidation kinetics, however, dictate that removal of volatile organic contaminants from the vapor phase can inherently be more efficient than their removal from the aqueous phase. Taking advantage of this efficiency reduces the complexity of the water recovery system. This reduction in system complexity is accompanied by reductions in the weight, volume, power, and resupply requirements of the system. Vapor compression distillation technology is used to treat the urine, condensate, and hygiene waste streams. This contributes to the reduction in resupply, as incorporation of vapor compression distillation technology at this point in the process reduces reliance on the expendable ion exchange and adsorption media used in the current state-of-the-art water recovery system. Other proven technologies that are incorporated into the Exploration Water Recovery System include the Trace Contaminant Control System and the Volatile Removal Assembly.

Off-flavor related volatiles in soymilk as affected by soybean variety, grinding, and heat-processing methods.

PubMed

Zhang, Yan; Guo, Shuntang; Liu, Zhisheng; Chang, Sam K C

2012-08-01

Off-flavor of soymilk is a barrier to the acceptance of consumers. The objectionable soy odor can be reduced through inhibition of their formation or through removal after being formed. In this study, soymilk was prepared by three grinding methods (ambient, cold, and hot grinding) from two varieties (yellow Prosoy and a black soybean) before undergoing three heating processes: stove cooking, one-phase UHT (ultrahigh temperature), and two-phase UHT process using a Microthermics direct injection processor, which was equipped with a vacuuming step to remove injected water and volatiles. Eight typical soy odor compounds, generated from lipid oxidation, were extracted by a solid-phase microextraction method and analyzed by gas chromatography. The results showed that hot grinding and cold grinding significantly reduced off-flavor as compared with ambient grinding, and hot grinding achieved the best result. The UHT methods, especially the two-phase UHT method, were effective to reduce soy odor. Different odor compounds showed distinct concentration patterns because of different formation mechanisms. The two varieties behaved differently in odor formation during the soymilk-making process. Most odor compounds could be reduced to below the detection limit through a combination of hot grinding and two-phase UHT processing. However, hot grinding gave lower solid and protein recoveries in soymilk.

Determination of selected azaarenes in water by bonded-phase extraction and liquid chromatography

USGS Publications Warehouse

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

1986-01-01

A method for the rapid and simple quantitative determination of quinoline, isoquinoline, and five selected three-ring azaarenes in water has been developed. The azaarene fraction is separated from its carbon analogues on n-octadecyl packing material by edition with acidified water/acetonitrile. Concentration as great as 1000-fold is achieved readily. Instrumental analysis involves high-speed liquid chromatography on flexible-walled, wide-bore columns with fluorescence and ultraviolet detection at several wavelengths employing filter photometers in series. Method-validation data is provided as azaarene recovery efficiency from fortified samples. Distilled water, river water, contaminated ground water, and secondary-treatment effluent have been tested. Recoveries at part-per-billion levels are nearly quantitative for the three-ring compounds, but they decrease for quinoline and isoquinoline. ?? 1986 American Chemical Society.

Aerodynamic characterisation and trajectory simulations for the Ariane-5 booster recovery system

NASA Astrophysics Data System (ADS)

Meiboom, F. P.

One of the most critical aspects of the early phases of the development of the Ariane-5 booster recovery system was the determination of the behavior of the booster during its atmospheric reentry, since this behavior determines the start conditions for the parachute system elements. A combination of wind-tunnel tests (subsonic and supersonic) and analytical methods was applied to define the aerodynamic characteristics of the booster. This aerodynamic characterization in combination with information of the ascent trajectory, atmospheric properties and booster mass and inertia were used as input for the 6-DOF trajectory simulations of the vehicle. Uncertainties in aerodynamic properties and deviations in atmospheric and booster properties were incorporated to define the range of initial conditions for the parachute system, utilizing stochastic (Monte-Carlo) methods.

Simple saponification method for the quantitative determination of carotenoids in green vegetables.

PubMed

Larsen, Erik; Christensen, Lars P

2005-08-24

A simple, reliable, and gentle saponification method for the quantitative determination of carotenoids in green vegetables was developed. The method involves an extraction procedure with acetone and the selective removal of the chlorophylls and esterified fatty acids from the organic phase using a strongly basic resin (Ambersep 900 OH). Extracts from common green vegetables (beans, broccoli, green bell pepper, chive, lettuce, parsley, peas, and spinach) were analyzed by high-performance liquid chromatography (HPLC) for their content of major carotenoids before and after action of Ambersep 900 OH. The mean recovery percentages for most carotenoids [(all-E)-violaxanthin, (all-E)-lutein epoxide, (all-E)-lutein, neolutein A, and (all-E)-beta-carotene] after saponification of the vegetable extracts with Ambersep 900 OH were close to 100% (99-104%), while the mean recovery percentages of (9'Z)-neoxanthin increased to 119% and that of (all-E)-neoxanthin and neolutein B decreased to 90% and 72%, respectively.

Liquid chromatographic determination of 4,4'-dinitrocarbanilide, the active component of the infertility agent nicarbazin, in chicken, duck, goose, and snake eggs.

PubMed

Primus, Thomas M; Kohler, Dennis J; Goodall, Margaret A; Yoder, Christi; Mathies, Thomas; Miller, Lowell; Johnston, John J; Vercauteren, Kurt

2003-01-01

4,4'-Dinitrocarbanilide (DNC) was extracted from chicken, duck, goose, and snake eggs and isolated by reversed-phase liquid chromatography. DNC was detected by ultraviolet absorbance at 347 nm and quantitated by comparison with a calibration standard. Recoveries of DNC from fortified control chicken, duck, goose, and snake egg samples were determined for DNC levels of 0.16, 10, and 16 microg/g. The mean recoveries from chicken, duck, goose, and snake eggs were 92 +/- 4, 88 +/- 9, 87 +/- 7, and 95 +/- 6%, respectively. The method limits of detection for DNC in chicken, duck, goose, and snake eggs ranged from 0.015 to 0.035 microg/g. The reported method is much simpler than and equally efficient as previous methods developed for the determination of DNC residues in egg contents.

Micro-CT Pore Scale Study Of Flow In Porous Media: Effect Of Voxel Resolution

NASA Astrophysics Data System (ADS)

Shah, S.; Gray, F.; Crawshaw, J.; Boek, E.

2014-12-01

In the last few years, pore scale studies have become the key to understanding the complex fluid flow processes in the fields of groundwater remediation, hydrocarbon recovery and environmental issues related to carbon storage and capture. A pore scale study is often comprised of two key procedures: 3D pore scale imaging and numerical modelling techniques. The essence of a pore scale study is to test the physics implemented in a model of complicated fluid flow processes at one scale (microscopic) and then apply the model to solve the problems associated with water resources and oil recovery at other scales (macroscopic and field). However, the process of up-scaling from the pore scale to the macroscopic scale has encountered many challenges due to both pore scale imaging and modelling techniques. Due to the technical limitations in the imaging method, there is always a compromise between the spatial (voxel) resolution and the physical volume of the sample (field of view, FOV) to be scanned by the imaging methods, specifically X-ray micro-CT (XMT) in our case In this study, a careful analysis was done to understand the effect of voxel size, using XMT to image the 3D pore space of a variety of porous media from sandstones to carbonates scanned at different voxel resolution (4.5 μm, 6.2 μm, 8.3 μm and 10.2 μm) but keeping the scanned FOV constant for all the samples. We systematically segment the micro-CT images into three phases, the macro-pore phase, an intermediate phase (unresolved micro-pores + grains) and the grain phase and then study the effect of voxel size on the structure of the macro-pore and the intermediate phases and the fluid flow properties using lattice-Boltzmann (LB) and pore network (PN) modelling methods. We have also applied a numerical coarsening algorithm (up-scale method) to reduce the computational power and time required to accurately predict the flow properties using the LB and PN method.

A Comprehensive Examination of Delayed Emotional Recovery in Borderline Personality Disorder

PubMed Central

Fitzpatrick, Skye; Kuo, Janice R.

2014-01-01

Background and Objectives Despite growing attention to emotion processes in borderline personality disorder (BPD), little research has examined delayed emotional recovery (i.e., long-lasting emotions after the termination of an emotionally evocative stimulus) in this population. The extant data on delayed emotional recovery in BPD are limited by a lack of assessment across a range of indices and emotions. The present study addresses these gaps by comparing emotional recovery between individuals with BPD, social anxiety disorder (SAD), and healthy controls (HCs) using a multi-modal assessment approach. Methods Participants underwent fear, anger, and sadness inductions followed by a 5-minute “washout” phase wherein emotional recovery was assessed via self-report, respiratory sinus arrhythmia (RSA), and skin conductance responses (SCR). Results After controlling for state dissociation, the BPD and SAD group exhibited decreases in RSA, while the HC group showed no changes in RSA after the anger induction only. Groups did not differ in rate of emotional recovery across self-report, RSA, or SCR after fear and sadness inductions. Limitations The present study is limited by a solely female and small sample, and the short time frame in which emotional recovery was assessed. Conclusions Findings indicate that individuals with BPD generally do not exhibit delayed emotional recovery, but may show decreases in parasympathetic activity during the recovery period after experiencing anger. However, this pattern may not be specific to this disorder. PMID:25482953

Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

PubMed

Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Goud, D Raghavender; Dubey, D K; Pardasani, Deepak

2015-05-15

Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative determination of ambroxol in tablets by derivative UV spectrophotometric method and HPLC.

PubMed

Dinçer, Zafer; Basan, Hasan; Göger, Nilgün Günden

2003-04-01

A derivative UV spectrophotometric method for the determination of ambroxol in tablets was developed. Determination of ambroxol in tablets was conducted by using first-order derivative UV spectrophotometric method at 255 nm (n = 5). Standards for the calibration graph ranging from 5.0 to 35.0 microg/ml were prepared from stock solution. The proposed method was accurate with 98.6+/-0.4% recovery value and precise with coefficient of variation (CV) of 1.22. These results were compared with those obtained by reference methods, zero-order UV spectrophotometric method and reversed-phase high-performance liquid chromatography (HPLC) method. A reversed-phase C(18) column with aqueous phosphate (0.01 M)-acetonitrile-glacial acetic acid (59:40:1, v/v/v) (pH 3.12) mobile phase was used and UV detector was set to 252 nm. Calibration solutions used in HPLC were ranging from 5.0 to 20.0 microg/ml. Results obtained by derivative UV spectrophotometric method was comparable to those obtained by reference methods, zero-order UV spectrophotometric method and HPLC, as far as ANOVA test, F(calculated) = 0.762 and F(theoretical) = 3.89, was concerned. Copyright 2003 Elsevier Science B.V.

Enhanced phasic GABA inhibition during the repair phase of stroke: a novel therapeutic target.

PubMed

Hiu, Takeshi; Farzampour, Zoya; Paz, Jeanne T; Wang, Eric Hou Jen; Badgely, Corrine; Olson, Andrew; Micheva, Kristina D; Wang, Gordon; Lemmens, Robin; Tran, Kevin V; Nishiyama, Yasuhiro; Liang, Xibin; Hamilton, Scott A; O'Rourke, Nancy; Smith, Stephen J; Huguenard, John R; Bliss, Tonya M; Steinberg, Gary K

2016-02-01

Ischaemic stroke is the leading cause of severe long-term disability yet lacks drug therapies that promote the repair phase of recovery. This repair phase of stroke occurs days to months after stroke onset and involves brain remapping and plasticity within the peri-infarct zone. Elucidating mechanisms that promote this plasticity is critical for the development of new therapeutics with a broad treatment window. Inhibiting tonic (extrasynaptic) GABA signalling during the repair phase was reported to enhance functional recovery in mice suggesting that GABA plays an important function in modulating brain repair. While tonic GABA appears to suppress brain repair after stroke, less is known about the role of phasic (synaptic) GABA during the repair phase. We observed an increase in postsynaptic phasic GABA signalling in mice within the peri-infarct cortex specific to layer 5; we found increased numbers of α1 receptor subunit-containing GABAergic synapses detected using array tomography, and an associated increased efficacy of spontaneous and miniature inhibitory postsynaptic currents in pyramidal neurons. Furthermore, we demonstrate that enhancing phasic GABA signalling using zolpidem, a Food and Drug Administration (FDA)-approved GABA-positive allosteric modulator, during the repair phase improved behavioural recovery. These data identify potentiation of phasic GABA signalling as a novel therapeutic strategy, indicate zolpidem's potential to improve recovery, and underscore the necessity to distinguish the role of tonic and phasic GABA signalling in stroke recovery. © The Author (2015). Published by Oxford University Press on behalf of the Guarantors of Brain.

Enhanced phasic GABA inhibition during the repair phase of stroke: a novel therapeutic target

PubMed Central

Paz, Jeanne T.; Wang, Eric Hou Jen; Badgely, Corrine; Olson, Andrew; Micheva, Kristina D.; Wang, Gordon; Lemmens, Robin; Tran, Kevin V.; Nishiyama, Yasuhiro; Liang, Xibin; Hamilton, Scott A.; O’Rourke, Nancy; Smith, Stephen J.; Huguenard, John R.; Bliss, Tonya M.

2016-01-01

Abstract Ischaemic stroke is the leading cause of severe long-term disability yet lacks drug therapies that promote the repair phase of recovery. This repair phase of stroke occurs days to months after stroke onset and involves brain remapping and plasticity within the peri-infarct zone. Elucidating mechanisms that promote this plasticity is critical for the development of new therapeutics with a broad treatment window. Inhibiting tonic (extrasynaptic) GABA signalling during the repair phase was reported to enhance functional recovery in mice suggesting that GABA plays an important function in modulating brain repair. While tonic GABA appears to suppress brain repair after stroke, less is known about the role of phasic (synaptic) GABA during the repair phase. We observed an increase in postsynaptic phasic GABA signalling in mice within the peri-infarct cortex specific to layer 5; we found increased numbers of α1 receptor subunit-containing GABAergic synapses detected using array tomography, and an associated increased efficacy of spontaneous and miniature inhibitory postsynaptic currents in pyramidal neurons. Furthermore, we demonstrate that enhancing phasic GABA signalling using zolpidem, a Food and Drug Administration (FDA)-approved GABA-positive allosteric modulator, during the repair phase improved behavioural recovery. These data identify potentiation of phasic GABA signalling as a novel therapeutic strategy, indicate zolpidem’s potential to improve recovery, and underscore the necessity to distinguish the role of tonic and phasic GABA signalling in stroke recovery. PMID:26685158

Comparison of UV spectrophotometry and high performance liquid chromatography methods for the determination of repaglinide in tablets.

PubMed

Dhole, Seema M; Khedekar, Pramod B; Amnerkar, Nikhil D

2012-07-01

Repaglinide is a miglitinide class of antidiabetic drug used for the treatment of type 2 diabetes mellitus. A fast and reliable method for the determination of repaglinide was highly desirable to support formulation screening and quality control. UV spectrophotometric and reversed-phase high performance liquid chromatography (RP-HPLC) methods were developed for determination of repaglinide in the tablet dosage form. The UV spectrum recorded between 200 400 nm using methanol as solvent and the wavelength 241 nm was selected for the determination of repaglinide. RP-HPLC analysis was carried out using Agilent TC-C18 (2) column and mobile phase composed of methanol and water (80:20 v/v, pH adjusted to 3.5 with orthophosphoric acid) at a flow rate of 1.0 ml/min. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the International Conference on Harmonization (ICH) guidelines. The developed methods illustrated excellent linearity (r(2) > 0.999) in the concentration range of 5-30 μg/ml and 5-50 μg/ml for UV spectrophotometric and HPLC methods, respectively. Precision (%R.S.D < 1.50) and mean recoveries were found in the range of 99.63-100.45% for UV spectrophotometric method and 99.71-100.25% for HPLC method which shows accuracy of the methods. The developed methods were found to be reliable, simple, fast, accurate and successfully used for the quality control of repaglinide as a bulk drug and in pharmaceutical formulations.

Effect of sample preparation and preenrichment media on the recovery of Salmonella from cantaloupes, mangoes, and tomatoes.

PubMed

Hammack, Thomas S; Johnson, Mildred L; Jacobson, Andrew P; Andrews, Wallace H

2006-01-01

Studies were conducted to determine the relative effectiveness of buffered peptone water (BPW), lactose (LAC) broth, and Universal Preenrichment (UP) broth for the recovery of Salmonella organisms from fruit rinses, whole fruit, and comminuted fruit. In the first phase, the relative effectiveness of the rinse and soak methods for the recovery of Salmonella from surface-contaminated mangoes and tomatoes was examined. Fruits were spot inoculated with single Salmonella serovars and held for 4 days at 2-6 degrees C before analysis was initiated. The contaminated fruit was rinsed in portions of BPW, LAC broth, or UP broth. Portions from each rinse were added to its respective broth (e.g., BPW to BPW). Individual whole fruit, in their remaining broth rinses (soak method), and the fruit rinse/broths (rinse method) were incubated for 24 h at 35 degrees C. The Bacteriological Analytical Manual (BAM) Salmonella culture method was followed thereafter. The soak method produced significantly greater numbers (P < 0.05) of positive test portions than did the rinse method for the analysis of mangoes (93 versus 12) and tomatoes (85 versus 34). The 3 broths were comparable for the recovery of Salmonella for both the soak and the rinse methods for mangoes. For tomatoes, there were no significant differences among the broths for the soak method, but BPW and UP broth were significantly more productive (P < 0.05) than LAC broth by the rinse method. In the second phase, the relative effectiveness of LAC broth, BPW, and UP broth for the recovery of Salmonella from comminuted fruit was examined. Fruits were contaminated with single Salmonella serovars and aged for 4 days at 2-6 degrees C. Twenty 25 g test portions were preenriched in each of the following broths: BPW, LAC broth, and UP broth. The BAM Salmonella culture method was followed thereafter. For cantaloupes, significantly more (P < 0.05) Salmonella-positive test portions were recovered with UP broth (96 Salmonella-positive test portions) and BPW (87 Salmonella-positive test portions) than with LAC broth (57 Salmonella-positive test portions). For mangoes, BPW recovered an arithmetically larger number of Salmonella-positive test portions (27 Salmonella-positive test portions) than did either LAC broth (14 Salmonella-positive test portions) or UP broth (18 Salmonella-positive test portions). For tomatoes, there were no significant differences among the broths: BPW recovered 65 Salmonella-positive test portions, UP broth recovered 62 Salmonella-positive test portions, and LAC broth recovered 60 Salmonella-positive test portions. For the analysis of whole fruit, it is recommended that the soak method be used. For whole fruit analyzed with the soak method, UP broth should be used for tomatoes and BPW should be used for mangoes. It is further recommended that UP broth be used for the analysis of comminuted cantaloupes and that BPW be used for the analysis of comminuted mangoes and tomatoes.

Positive and negative ionospheric responses to the March 2015 geomagnetic storm from BDS observations

NASA Astrophysics Data System (ADS)

Jin, Shuanggen; Jin, Rui; Kutoglu, H.

2017-06-01

The most intense geomagnetic storm in solar cycle 24 occurred on March 17, 2015, and the detailed ionospheric storm morphologies are difficultly obtained from traditional observations. In this paper, the Geostationary Earth Orbit (GEO) observations of BeiDou Navigation Satellite System (BDS) are for the first time used to investigate the ionospheric responses to the geomagnetic storm. Using BDS GEO and GIMs TEC series, negative and positive responses to the March 2015 storm are found at local and global scales. During the main phase, positive ionospheric storm is the main response to the geomagnetic storm, while in the recovery phase, negative phases are pronounced at all latitudes. Maximum amplitudes of negative and positive phases appear in the afternoon and post-dusk sectors during both main and recovery phases. Furthermore, dual-peak positive phases in main phase and repeated negative phase during the recovery are found from BDS GEO observations. The geomagnetic latitudes corresponding to the maximum disturbances during the main and recovery phases show large differences, but they are quasi-symmetrical between southern and northern hemispheres. No clear zonal propagation of traveling ionospheric disturbances is detected in the GNSS TEC disturbances at high and low latitudes. The thermospheric composition variations could be the dominant source of the observed ionospheric storm effect from GUVI [O]/[N2] ratio data as well as storm-time electric fields. Our study demonstrates that the BDS (especially the GEO) observations are an important data source to observe ionospheric responses to the geomagnetic storm.

Radiation effects on the resting and proliferating cells in normal tissue of mouse (in Japanese)

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

Hayashi, S.

1972-10-01

The investigation was planned to compare the radiosensitivity of callus- forming cells in resting phase with that in proliferating phase and to compare the recovery of sublethal damage of callusforming cells in resting phase with that in proliferating phase. Experimental animals were 8-week-old female I.C.R./ J.C.L. mice. The maximum sizes of callus were nearly constant among control mice without irradiation after fracture. They, however, were inhibited with administered doses and seemed to be reflected by the Proliferating ability of callus-forming cells after irradiation. The analysis was performed by C.I.D. 50 (callus inhibition dose 50) or dose that produced a specifiedmore » inhibition of callus size in half of the subjects. The callus-forming cells in adult mice were in resting phase without any stimulations, but they extensively entered into proliferating phase after fracture. The labeling index rose around 6 hrs after fracture and reached 9% of the maximum value at 72 are after fracture. Mice were followed by x-ray projection until 60 days after irradiation to observe the callus sizes, and the maximum sizes of callus for each mouse were examined by planimetry to calculate the C.I.D. 50. The callus-forming cell was more radioresistant in resting phase by a factor of 1.5 to 2.0 than in proliferating phase. The cell in resting phase demonstrated a marked recovery of sublethal damage in 4 hrs after administration of 1.000 rads, and it showed essentially no more changes in recovery with the increased time interval to 24 hrs, while the cell in proliferating phase demonstrated almost full recovery of sublethal damage is 2 hrs after administration of 300 rads and showed a fluctuated pattern of recovery with a dip at 4 hrs of the time interval in two fractions. (auth)« less

Spontaneous splenic rupture during the recovery phase of dengue fever.

PubMed

de Silva, W T T; Gunasekera, M

2015-07-02

Spontaneous splenic rupture is a rare but known complication of dengue fever. Previously reported cases have occurred early during the course of the disease and most cases have led to a fatal outcome. Here we report a case of spontaneous splenic rupture in a patient with dengue fever, which occurred during the recovery phase of the illness. A 28-year-old Sinhalese, Sri Lankan man presented with a history of fever, myalgia and vomiting of 4 days duration. Investigations revealed a diagnosis of dengue fever with no signs of plasma leakage. He was managed in the ward as per local protocol. During the recovery phase the patient developed severe abdominal distention with circulatory failure. Radiology revealed splenic rupture with massive amounts of abdominal free fluid. The patient was resuscitated and Emergency laparotomy with splenectomy was performed. The outcome was excellent with the patient making a complete recovery. Although splenic rupture is a known complication of dengue fever it may be manifested late in the disease process. A high degree of suspicion should be maintained and patients must be monitored even during the recovery phase of dengue fever. Early diagnosis and intervention can prevent mortality.

Coalescent Theory Analysis of Population Collapse and Recovery in a Neutral Evolution Model

NASA Astrophysics Data System (ADS)

King, Dawn; Bahar, Sonya

As we move through the Anthropocene Epoch, human-driven climate change is predicted to accelerate extinction risk in the near future. Therefore, understanding basic underlying mechanisms of population loss and recovery could be paramount to saving key species in changing ecosystems. Here, we present an evolutionary model that investigates the dynamics of population collapse and recovery following a simulated mass extinction. Previously, we have shown that nonequilibrium, continuous phase transitions of the directed percolation universality class occur as a function of two different control parameters: the mutability, μ, which dictates how phenotypically different an offspring can be from its parent, and the death probability, δ, which probabilistically removes organisms within each generation. Here, we characterize the phylogenetic tree structures at two levels of biological organization--the organism and species level. Using methods from coalescent theory, we examine the phylogenetic tree structures at, and above, criticality, by considering common descent. The times to most recent common ancestor show phase transition behavior, as well as scale-free branching behavior at both levels of organization. We further examine these genealogical structures pre- and post-extinction. This research was supported by funding from the James S. McDonnell Foundation.

Optimization and application of octadecyl-modified monolithic silica for solid-phase extraction of drugs in whole blood samples.

PubMed

Namera, Akira; Saito, Takeshi; Ota, Shigenori; Miyazaki, Shota; Oikawa, Hiroshi; Murata, Kazuhiro; Nagao, Masataka

2017-09-29

Monolithic silica in MonoSpin for solid-phase extraction of drugs from whole blood samples was developed to facilitate high-throughput analysis. Monolithic silica of various pore sizes and octadecyl contents were synthesized, and their effects on recovery rates were evaluated. The silica monolith M18-200 (20μm through-pore size, 10.4nm mesopore size, and 17.3% carbon content) achieved the best recovery of the target analytes in whole blood samples. The extraction proceeded with centrifugal force at 1000rpm for 2min, and the eluate was directly injected into the liquid chromatography-mass spectrometry system without any tedious steps such as evaporation of extraction solvents. Under the optimized condition, low detection limits of 0.5-2.0ngmL -1 and calibration ranges up to 1000ngmL -1 were obtained. The recoveries of the target drugs in the whole blood were 76-108% with relative standard deviation of less than 14.3%. These results indicate that the developed method based on monolithic silica is convenient, highly efficient, and applicable for detecting drugs in whole blood samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Phased Array Approach To Retrieve Gases, Liquids, Or Solids From Subsurface And Subaqueous Geologic Or Man-Made Formations

DOEpatents

Rynne, Timothy M.; Spadaro, John F.; Iovenitti, Joe L.; Dering, John P.; Hill, Donald G.

1998-10-27

A method of enhancing the remediation of contaminated soils and ground water, production of oil and gas, and production of any solid, gas, and/or liquid from subsurface geologic and man-made formations including the steps of estimating the geometric boundaries of the region containing the material to be recovered, drilling a recovery well(s) into subsurface in a strategic location to recover the material of interest, establishing multiple sources of acoustical power in an array about and spaced-apart from the surface or at various depths below the surface in a borehole(s) and/or well(s), directing a volume of acoustical excitation from the sources into the region containing the material to be recovered, the excitation in the form of either controllable sinusoidal, square, pulsed, or various combinations of these three waveforms, and controlling the phasing, frequency, power, duration, and direction of these waveforms from the sources to increase and control the intensity of acoustical excitation in the region of the material to be recovered to enhance. the recovery of said material from the recovery well(s). The invention will augment any technology affecting the removal of materials from the subsurface.

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.

Determination of total phthalate in cosmetics using a simple three-phase sample preparation method.

PubMed

Liu, Laping; Wang, Zhengmeng; Zhao, Sihan; Duan, Jiahui; Tao, Hu; Wang, Wenji; Liu, Shuhui

2018-02-01

A simple sample preparation method requiring minimal organic solvents is proposed for the determination of the total phthalate content in cosmetics by high-performance liquid chromatography-tandem mass spectrometry. The hydrolysis of phthalates and purification of interfering substances were performed in a three-phase system that included an upper n-hexane phase, a middle ethanol phase, and a lower aqueous alkali solution. This three-phase system utilized an incremental purification strategy. The apolar ingredients were extracted with n-hexane, the polar pigments accumulated in the ethanol phase, and the hydrolysis product, phthalic acid, remained in the hydrolysate. Under the optimized conditions, the correlation coefficients (r) for the calibration curves were 0.998-0.999 in the range 0.60-12 mol L -1 . The limit of detection was 5.1 μmol kg -1 , and the limit of quantification was 9.2 μmol kg -1 . The recoveries varied from 84 to 97% with RSDs equal to or lower than 11%. The intra-day and inter-day repeatability values, expressed as the relative standard deviation, were less than 8.7 and 9.8, respectively. No obvious matrix effect existed in the different cosmetics matrices. The validated method was applied for the analysis of 57 commercial cosmetic samples. Graphical abstract Analysis of phthalates in cosmetics using a three-phase preparation method.

First recovery in anorexia nervosa patients in the long-term course: a discrete-time survival analysis.

PubMed

Herzog, W; Schellberg, D; Deter, H C

1997-02-01

The results of a 12-year follow-up study of occurrence and timing of first recovery in 69 hospitalized patients with severe anorexia nervosa (AN) are presented. For the first time discrete-time survival analysis methods were used to determine the likelihood of recovery in AN patients. Furthermore, predictors gleaned from pretreatment-posttreatment studies of long-term outcome in AN could be evaluated as to their effect on a change in the time course structure of the likelihood of first recovery. Results show that AN condition did not improve until after 6 years after the first inpatient treatment in 50% of patients. However, a restricter-type AN and low serum creatinine levels were predictors for earlier recovery. One specific effect was that AN patients who show purging behavior in combination with additional social disturbances have a lower chance of recovering. The use of discrete-time survival analysis methodology in further prospective studies will contribute to the development of more tailored treatment of AN, which also takes the individual phase of illness and specific aspects of the symptomatology into account.

COORDINATION COMPOUND-SOLVENT EXTRACTION PROCESS FOR URANIUM RECOVERY

DOEpatents

Reas, W.H.

1959-03-10

A method is presented for the separation of uranium from aqueous solutions containing a uranyl salt and thorium. Thc separation is effected by adding to such solutions an organic complexing agent, and then contacting the solution with an organic solvent in which the organic complexing agent is soluble. By use of the proper complexing agent in the proper concentrations uranium will be complexed and subsequently removed in the organic solvent phase, while the thorium remains in the aqueous phase. Mentioned as suitable organic complexing agents are antipyrine, bromoantipyrine, and pyramidon.

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

PubMed

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

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

Spectroscopic characterization of bone tissue of experimental animals after glucocorticoid treatment and recovery period

NASA Astrophysics Data System (ADS)

Mitić, Žarko J.; Najman, Stevo J.; Cakić, Milorad D.; Ajduković, Zorica R.; Ignjatović, Nenad L.; Nikolić, Ružica S.; Nikolić, Goran M.; Stojanović, Sanja T.; Vukelić, Marija Đ.; Trajanović, Miroslav D.

2014-09-01

The influence of glucocorticoids on the composition and mineral/organic content of the mandible in tested animals after recovery and healing phase was investigated in this work. The results of FTIR analysis demonstrated that bone tissue composition was changed after glucocorticoid treatment. The increase of calcium, magnesium, phosphorus content and mineral part of bones was statistically significant in recovery phase and in treatment phase that included calcitonin and thymus extract. Some changes also happened in the organic part of the matrix, as indicated by intensity changes for already present IR bands and the appearance of new IR bands in the region 3500-1300 cm-1.

Food availability promotes rapid recovery from thermal stress in a scleractinian coral

NASA Astrophysics Data System (ADS)

Connolly, S. R.; Lopez-Yglesias, M. A.; Anthony, K. R. N.

2012-12-01

Bleaching in corals due to environmental stress represents a loss of energy intake often leading to an increase in mortality risk. Successful coral recovery from severe bleaching events may depend on the rate of replenishment of algal symbiont populations following the period of thermal stress, the supply of an alternative food source, or both. Here, we explore the role of food availability in promoting the survival and recovery of a common coral ( Acropora intermedia) following acute experimentally induced thermal stress. Fed corals were provided with live rotifers daily, to maintain densities of zooplankton in tanks that are typical of coral reefs. After a 6-week acclimation phase, heated corals were subjected to a +4 °C thermal anomaly for a 7-day period (bleaching phase) then temperatures were returned to normal for a further 2 weeks (recovery phase). Results demonstrated that heated corals had higher survival when they were provided with heterotrophic food. Fed corals experienced reduced loss of chlorophyll a, relative to unfed corals. During the recovery phase, both fed and unfed corals recovered within a few days; however, fed corals recovered to pre-bleaching phase levels of chlorophyll a, whereas unfed corals stabilized approximately one-third below this level. Protein levels of fed corals declined markedly during the bleaching phase, but recovered all of their losses by the end of the recovery phase. In contrast, unfed corals had low protein levels that were maintained throughout the experiment. To the extent that these results are representative of corals' responses to thermal anomalies in nature, the findings imply that availability of particulate food matter has the potential to increase corals' capacity to survive thermally induced bleaching and to ameliorate its sub-lethal effects. They also support the hypothesis that different rates of heterotrophy are an important determinant of variation in resilience to thermal stress among reef environments.

A novel optimised and validated method for analysis of multi-residues of pesticides in fruits and vegetables by microwave-assisted extraction (MAE)-dispersive solid-phase extraction (d-SPE)-retention time locked (RTL)-gas chromatography-mass spectrometry with Deconvolution reporting software (DRS).

PubMed

Satpathy, Gouri; Tyagi, Yogesh Kumar; Gupta, Rajinder Kumar

2011-08-01

A rapid, effective and ecofriendly method for sensitive screening and quantification of 72 pesticides residue in fruits and vegetables, by microwave-assisted extraction (MAE) followed by dispersive solid-phase extraction (d-SPE), retention time locked (RTL) capillary gas-chromatographic separation in trace ion mode mass spectrometric determination has been validated as per ISO/IEC: 17025:2005. Identification and reporting with total and extracted ion chromatograms were facilitated to a great extent by Deconvolution reporting software (DRS). For all compounds LOD were 0.002-0.02mg/kg and LOQ were 0.025-0.100mg/kg. Correlation coefficients of the calibration curves in the range of 0.025-0.50mg/kg were >0.993. To validate matrix effects repeatability, reproducibility, recovery and overall uncertainty were calculated for the 35 matrices at 0.025, 0.050 and 0.100mg/kg. Recovery ranged between 72% and 114% with RSD of <20% for repeatability and intermediate precision. The reproducibility of the method was evaluated by an inter laboratory participation and Z score obtained within ±2. Copyright © 2011 Elsevier Ltd. All rights reserved.

40 CFR 300.315 - Phase IV-Documentation and cost recovery.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 28 2014-07-01 2014-07-01 false Phase IV-Documentation and cost recovery. 300.315 Section 300.315 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SUPERFUND, EMERGENCY PLANNING, AND COMMUNITY RIGHT-TO-KNOW PROGRAMS NATIONAL OIL AND HAZARDOUS SUBSTANCES...

40 CFR 300.315 - Phase IV-Documentation and cost recovery.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 29 2013-07-01 2013-07-01 false Phase IV-Documentation and cost recovery. 300.315 Section 300.315 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SUPERFUND, EMERGENCY PLANNING, AND COMMUNITY RIGHT-TO-KNOW PROGRAMS NATIONAL OIL AND HAZARDOUS SUBSTANCES...

40 CFR 300.315 - Phase IV-Documentation and cost recovery.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 29 2012-07-01 2012-07-01 false Phase IV-Documentation and cost recovery. 300.315 Section 300.315 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SUPERFUND, EMERGENCY PLANNING, AND COMMUNITY RIGHT-TO-KNOW PROGRAMS NATIONAL OIL AND HAZARDOUS SUBSTANCES...

Optimizing separate phase light hydrocarbon recovery from contaminated unconfined aquifers

NASA Astrophysics Data System (ADS)

Cooper, Grant S.; Peralta, Richard C.; Kaluarachchi, Jagath J.

A modeling approach is presented that optimizes separate phase recovery of light non-aqueous phase liquids (LNAPL) for a single dual-extraction well in a homogeneous, isotropic unconfined aquifer. A simulation/regression/optimization (S/R/O) model is developed to predict, analyze, and optimize the oil recovery process. The approach combines detailed simulation, nonlinear regression, and optimization. The S/R/O model utilizes nonlinear regression equations describing system response to time-varying water pumping and oil skimming. Regression equations are developed for residual oil volume and free oil volume. The S/R/O model determines optimized time-varying (stepwise) pumping rates which minimize residual oil volume and maximize free oil recovery while causing free oil volume to decrease a specified amount. This S/R/O modeling approach implicitly immobilizes the free product plume by reversing the water table gradient while achieving containment. Application to a simple representative problem illustrates the S/R/O model utility for problem analysis and remediation design. When compared with the best steady pumping strategies, the optimal stepwise pumping strategy improves free oil recovery by 11.5% and reduces the amount of residual oil left in the system due to pumping by 15%. The S/R/O model approach offers promise for enhancing the design of free phase LNAPL recovery systems and to help in making cost-effective operation and management decisions for hydrogeologists, engineers, and regulators.

High-speed clock recovery unit based on a phase aligner

NASA Astrophysics Data System (ADS)

Tejera, Efrain; Esper-Chain, Roberto; Tobajas, Felix; De Armas, Valentin; Sarmiento, Roberto

2003-04-01

Nowadays clock recovery units are key elements in high speed digital communication systems. For an efficient operation, this units should generate a low jitter clock based on the NRZ received data, and be tolerant to long absence of transitions. Architectures based on Hogge phase detectors have been widely used, nevertheless, they are very sensitive to jitter of the received data and they have a limited tolerance to the absence of transitions. This paper shows a novel high speed clock recovery unit based on a phase aligner. The system allows a very fast clock recovery with a low jitter, moreover, it is very resistant to absence of transitions. The design is based on eight phases obtained from a reference clock running at the nominal frequency of the received signal. This high speed reference clock is generated using a crystal and a clock multiplier unit. The phase alignment system chooses, as starting point, the two phases closest to the data phase. This allows a maximum error of 45 degrees between the clock and data signal phases. Furthermore, the system includes a feed-back loop that interpolates the chosen phases to reduce the phase error to zero. Due to the high stability and reduced tolerance of the local reference clock, the jitter obtained is highly reduced and the system becomes able to operate under long absence of transitions. This performances make this design suitable for systems such as high speed serial link technologies. This system has been designed for CMOS 0.25μm at 1.25GHz and has been verified through HSpice simulations.

Monitoring the recovery of Juncus roemerianus marsh burns with the normalized difference vegetation index and Landsat Thematic Mapper data

USGS Publications Warehouse

Ramsey, Elijah W.; Sapkota, S.K.; Barnes, F.G.; Nelson, G.A.

2002-01-01

Nine atmospherically corrected Landsat Thematic Mapper images were used to generate mean normalized difference vegetation indices (NDVI) at 11 burn sites throughout a coastal Juncus roemerianus marsh in St. Marks National Wildlife Refuge, Florida. Time-since-burn, the time lapse from the date of burn to the date of image collection, was related to variation in mean NDVI over time. Regression analysis showed that NDVI increased for about 300 to 400 days immediately after the burn, overshooting the typical mean NDVI of a nonburned marsh. For about another 500 to 600 days NDVI decreased until reaching a nearly constant NDVI of about 0.40. During the phase of increasing NDVI the ability to predict time-since-burn was within about ??60 days. Within the decreasing phase this dropped to about ??88 days. Examination of each burn site revealed some nonburn related influences on NDVI (e.g., seasonality). Normalization of burn NDVI by site-specific nonburn control NDVI eliminated most influences. However, differential responses at the site-specific level remained related to either storm impacts or secondary burning. At these sites, collateral data helped clarify the abnormal changes in NDVI. Accounting for these abnormalities, site-specific burn recovery trends could be broadly standardized into four general phases: Phase 1-preburn, Phase 2-initial recovery (increasing NDVI), Phase 3-late recovery (decreasing NDVI), and Phase 4-final coalescence (unchanging NDVI). Phase 2 tended to last about 300 to 500 days, Phase 3 an additional 500 to 600 days, and finally reaching Phase 4, 900 to 1,000 days after burn.

SOLVENT EXTRACTION PROCESS FOR THE RECOVERY OF METALS FROM PHOSPHORIC ACID

DOEpatents

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

1958-11-01

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

High performance liquid chromatographic determination of caffeine in decaffeinated coffee, tea, and beverage products.

PubMed

Ashoor, S H; Seperich, G J; Monte, W C; Welty, J

1983-05-01

A method was developed for determining caffeine in decaffeinated coffee, tea, and beverage products by high performance liquid chromatography (HPLC). The HPLC system consisted of a Bio-Sil ODS-5S C18 column, methanol-water (25 + 75) mobile phase at 1 mL/min, and a UV detector. The method is simple and specific. Caffeine recoveries were 93.8-98.3% and coefficients of variation were 0.90-2.25%.

Method for the determination of catechin and epicatechin enantiomers in cocoa-based ingredients and products by high-performance liquid chromatography: single-laboratory validation.

PubMed

Machonis, Philip R; Jones, Matthew A; Schaneberg, Brian T; Kwik-Uribe, Catherine L

2012-01-01

A single-laboratory validation study was performed for an HPLC method to identify and quantify the flavanol enantiomers (+)- and (-)-epicatechin and (+)- and (-)-catechin in cocoa-based ingredients and products. These compounds were eluted isocratically with an ammonium acetate-methanol mobile phase applied to a modified beta-cyclodextrin chiral stationary phase and detected using fluorescence. Spike recovery experiments using appropriate matrix blanks, along with cocoa extract, cocoa powder, and dark chocolate, were used to evaluate accuracy, repeatability, specificity, LOD, LOQ, and linearity of the method as performed by a single analyst on multiple days. In all samples analyzed, (-)-epicatechin was the predominant flavanol and represented 68-91% of the total monomeric flavanols detected. For the cocoa-based products, within-day (intraday) precision for (-)-epicatechin was between 1.46-3.22%, for (+)-catechin between 3.66-6.90%, and for (-)-catechin between 1.69-6.89%; (+)-epicatechin was not detected in these samples. Recoveries for the three sample types investigated ranged from 82.2 to 102.1% at the 50% spiking level, 83.7 to 102.0% at the 100% spiking level, and 80.4 to 101.1% at the 200% spiking level. Based on performance results, this method may be suitable for routine laboratory use in analysis of cocoa-based ingredients and products.

Development and validation of an HPLC-method for determination of free and bound phenolic acids in cereals after solid-phase extraction.

PubMed

Irakli, Maria N; Samanidou, Victoria F; Biliaderis, Costas G; Papadoyannis, Ioannis N

2012-10-01

Whole cereal grains are a good source of phenolic acids associated with reduced risk of chronic diseases. This paper reports the development and validation of a high-performance liquid chromatography-diode array detection (HPLC-DAD) method for the determination of phenolic acids in cereals in either free or bound form. Extraction of free phenolic acids and clean-up was performed by an optimised solid-phase extraction (SPE) protocol on Oasis HLB cartridges using aqueous methanol as eluant. The mean recovery of analytes ranged between 84% and 106%. Bound phenolic acids were extracted using alkaline hydrolysis with mean recoveries of 80-95%, except for gallic acid, caffeic acid and protocatechuic acid. Both free and bound phenolic extracts were separated on a Nucleosil 100 C18 column, 5 μm (250 mm × 4.6 mm) thermostated at 30 °C, using a linear gradient elution system consisting of 1% (v/v) acetic acid in methanol. Method validation was performed by means of linearity, accuracy, intra-day and inter-day precision and sensitivity. Detection limits ranged between 0.13 and 0.18 μg/g. The method was applied to the analysis of free and bound phenolic acids contents in durum wheat, bread wheat, barley, oat, rice, rye, corn and triticale. Copyright © 2012 Elsevier Ltd. All rights reserved.

Comparison of two methods for purification of enterocin B, a bacteriocin produced by Enterococcus faecium W3.

PubMed

Dündar, Halil; Atakay, Mehmet; Çelikbıçak, Ömür; Salih, Bekir; Bozoğlu, Faruk

2015-01-01

This study aimed to compare two different approaches for the purification of enterocin B from Enterococcus faecium strain W3 based on the observation that the bacteriocin was found both in cell associated form and in culture supernatant. The first approach employed ammonium sulfate precipitation, cation-exchange chromatography, and sequential reverse-phase high-performance liquid chromatography. The latter approach exploited a pH-mediated cell adsorption-desorption method to extract cell-bound bacteriocin, and one run of reverse-phase chromatography. The first method resulted in purification of enterocin B with a recovery of 4% of the initial bacteriocin activity found in culture supernatant. MALDI-TOF MS analysis and de novo peptide sequencing of the purified bacteriocin confirmed that the active peptide was enterocin B. The second method achieved the purification of enterocin B with a higher recovery (16%) and enabled us to achieve pure bacteriocin within a shorter period of time by avoiding time consuming purification protocols. The purity and identity of the active peptide were confirmed again by matrix-assisted laser desorption/ionization time-of flight (MALDI-TOF) mass spectrometry (MS) analysis. Although both approaches were satisfactory to obtain a sufficient amount of enterocin B for use in MS and amino acid sequence analysis, the latter was proved to be applicable in large-scale and rapid purification of enterocin B.

Quantitative determination of steroids in the fruiting bodies and submerged-cultured mycelia of Inonotus obliquus.

PubMed

Gao, Yuan; Xu, Hongyu; Lu, Zhenming; Xu, Zhenghong

2009-11-01

This study describes the method of quantitative determination of betulin, ergosterol, cholesterol, lanosterol, stigmasterol and sitosterol in the fruiting bodies and submerged-cultured mycelia of Inonotus obliquus. A high performance liquid chromatographic (HPLC) method was applied to separate these steroids. The procedure was carried out on a reversed-phase C, column, using a stepwise gradient of water-methanol as mobile phase with the following profile: 0-10 min, 10% water, 90% methanol; 10-40 min, 3% water, 97% methanol. The flow rate was 1.4 mL/min and the detection wavelength was 202 nm. The analysis was completed within 40 min. The results showed that this method has good reproducibility and satisfactory recoveries for the determination of steroids. The relative standard deviations of the peak areas were less than 2.94% (n = 5) for intraday assays. A good linear correlation was obtained in a range of 0.4-4.8 microg. The recoveries of betulin, ergosterol, cholesterol, lanosterol, stigmasterol, and sitosterol were 100.05%-100.72%, 99.31%-101.04%, 97.52%-101.63%, 96.61%-100.08%, 96.21%-100.76% and 100.04%-100.51%, respectively. This method can be applied to evaluate real samples, and it is rapid, accurate and suitable for the quantitative determination of steroids in the fruiting bodies and submerged-cultured mycelia of Inonotus obliquus.

Development of a simple one-pot extraction method for various drugs and metabolites of forensic interest in blood by modifying the QuEChERS method.

PubMed

Matsuta, Shuntaro; Nakanishi, Keiko; Miki, Akihiro; Zaitsu, Kei; Shima, Noriaki; Kamata, Tooru; Nishioka, Hiroshi; Katagi, Munehiro; Tatsuno, Michiaki; Tsuboi, Kento; Tsuchihashi, Hitoshi; Suzuki, Koichi

2013-10-10

A rapid and convenient extraction method has been developed for the determination of various drugs and metabolites of forensic interest in blood by modifying the dispersive solid-phase extraction method "QuEChERS". The following 13 analytes with various chemical properties were used for the method development and its validation: amphetamine, methamphetamine, zolpidem, the carboxylate-form major metabolite of zolpidem M-1, flunitrazepam, 7-aminoflunitrazepam, phenobarbital, triazolam, α-hydroxytriazolam, brotizolam, α-hydroxybrotizolam, chlorpromazine, and promethazine. The modification of the QuEChERS method includes the use of relatively large amounts of inorganic salts in order to coagulate blood, which allows easy isolation of the organic extract phase. A combination of 100 mg anhydrous magnesium sulfate as a dehydrating agent, 50mg sodium chloride as a salting-out agent, and 500 μL acetonitrile containing 0.2% acetic acid as the organic solvent provided the optimum conditions for processing a 100 μL whole blood sample. The recoveries of the analytes spiked into whole blood at 0.5 μg/mL ranged between 59% and 93%. Although the addition of the graphitized carbon Envi-carb for cleanup decreased the recoveries of zolpidem and its carboxylate-form metabolite M-1, it was very effective in avoiding interferences by cholesterol. The present method can provide a rapid, effective, user-friendly, and relatively hygienic method for the simultaneous extraction of a wide range of drugs and metabolites in whole blood specimens. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Measuring of electrical changes induced by in situ combustion through flow-through electrodes in a laboratory sample of core material

DOEpatents

Lee, D.O.; Montoya, P.C.; Wayland, J.R. Jr.

1986-12-09

Method and apparatus are provided for obtaining accurate dynamic measurements for passage of phase fronts through a core sample in a test fixture. Flow-through grid structures are provided for electrodes to permit data to be obtained before, during and after passage of a front there through. Such electrodes are incorporated in a test apparatus for obtaining electrical characteristics of the core sample. With the inventive structure a method is provided for measurement of instabilities in a phase front progressing through the medium. Availability of accurate dynamic data representing parameters descriptive of material characteristics before, during and after passage of a front provides a more efficient method for enhanced recovery of oil using a fire flood technique. 12 figs.

Measuring of electrical changes induced by in situ combustion through flow-through electrodes in a laboratory sample of core material

DOEpatents

Lee, David O.; Montoya, Paul C.; Wayland, Jr., James R.

1986-01-01

Method and apparatus are provided for obtaining accurate dynamic measurements for passage of phase fronts through a core sample in a test fixture. Flow-through grid structures are provided for electrodes to permit data to be obtained before, during and after passage of a front therethrough. Such electrodes are incorporated in a test apparatus for obtaining electrical characteristics of the core sample. With the inventive structure a method is provided for measurement of instabilities in a phase front progressing through the medium. Availability of accurate dynamic data representing parameters descriptive of material characteristics before, during and after passage of a front provides a more efficient method for enhanced recovery of oil using a fire flood technique.

Quantitative determination of reserpine, ajmaline, and ajmalicine in Rauvolfia serpentina by reversed-phase high-performance liquid chromatography.

PubMed

Srivastava, A; Tripathi, A K; Pandey, R; Verma, R K; Gupta, M M

2006-10-01

A sensitive and reproducible reversed-phase high-performance liquid chromatography (HPLC) method using photodiode array detection is established for the simultaneous quantitation of important root alkaloids of Rauvolfia serpentina, namely, reserpine, ajmaline, and ajmalicine. A Chromolith Performance RP-18e column (100 x 4.6-mm i.d.) and a binary gradient mobile phase composed of 0.01 M (pH 3.5) phosphate buffer (NaH(2)PO(4)) containing 0.5% glacial acetic acid and acetonitrile are used. Analysis is run at a flow rate of 1.0 mL/min with the detector operated at a wavelength of 254 nm. The calibration curves are linear over a concentration range of 1-20 microg/mL (r = 1.000) for all the alkaloids. The various other aspects of analysis (i.e., peak purity, similarity, recovery, and repeatability) are also validated. For the three components, the recoveries are found to be 98.27%, 97.03%, and 98.38%, respectively. The limits of detection are 6, 4, and 8 microg/mL for ajmaline, ajmalicine, and reserpine, respectively, and the limits of quantitation are 19, 12, and 23 microg/mL for ajmaline, ajmalicine, and reserpine, respectively. The developed method is simple, reproducible, and easy to operate. It is useful for the evaluation of R. serpentina.

Sol-gel-graphene-based fabric-phase sorptive extraction for cow and human breast milk sample cleanup for screening bisphenol A and residual dental restorative material before analysis by HPLC with diode array detection.

PubMed

Samanidou, Victoria; Filippou, Olga; Marinou, Eirini; Kabir, Abuzar; Furton, Kenneth G

2017-06-01

Fabric-phase sorptive extraction has already been recognized as a simple and green alternative to the conventional sorbent-based sorptive microextraction techniques, using hybrid organic-inorganic sorbent coatings chemically bonded to a flexible fabric surface. Herein, we have investigated the synergistic combination of the advanced material properties offered by sol-gel graphene sorbent and the simplicity of Fabric phase sorptive extraction approach in selectively extracting bisphenol A and residual monomers including bisphenol A glycerolatedimethacrylate, urethane dimethacrylate, and triethylene glycol dimethacrylate derived dental restorative materials from cow and human breast milk samples. Different coatings were evaluated. Final method development employed sol-gel graphene coated media. The main experimental parameters influencing extraction of the compounds, such as sorbent chemistry used, sample loading conditions, elution solvent, sorption stirring time, elution time, impact of protein precipitation, amount of sample, and matrix effect, were investigated and optimized. Absolute recovery values from standard solutions were 50% for bisphenol A, 78% for T triethylene glycol dimethacrylate, 110% for urethane dimethacrylate, and 103% for bisphenol A glycerolatedimethacrylate, while respective absolute recovery values from milk were 30, 52, 104, and 42%. Method validation was performed according to European Decision 657/2002/EC in terms of selectivity, sensitivity, linearity, accuracy, and precision. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Out-of-equilibrium pH transients in the guinea-pig ventricular myocyte

PubMed Central

Leem, Chae-Hun; Vaughan-Jones, Richard D

1998-01-01

Following an intracellular alkali load (imposed by acetate prepulsing in CO2/HCO3− buffer), intracellular pH (pHi) of the guinea-pig ventricular myocyte (recorded from intracellular SNARF fluorescence) recovers to control levels. Recovery has two phases. An initial rapid phase (lasting up to 2 min) is followed by a later slow phase (several minutes). Inhibition of sarcolemmal acid-loading carriers (by removal of extracellular Cl−) inhibits the later, slow phase but the initial rapid recovery phase persists. It also persists in the absence of extracellular Na+ and in the presence of the HCO3− transport inhibitor DIDS (4,4-di-isothiocyanatostilbene-2,2-disulphonic acid). The rapid recovery phase is not evident if the alkali load has been induced by reducing PCO2 (from 10 to 5 %), and it is inhibited in the absence of CO2/HCO3− buffer (i.e. Hepes buffer). It is also slowed by the carbonic anhydrase (CA) inhibitor acetazolamide (ATZ). We conclude that it is caused by buffering of the alkali load through the hydration of intracellular CO2 (CO2-dependent buffering). The time course of rapid recovery is consistent with an intracellular CO2 hydration rate constant (k1) of 0.36 s−1 in the presence of CA activity, and 0.14 s−1 in the absence of CA activity. This latter k1 value matches the literature value for uncatalysed CO2 hydration in free solution. Natural CO2 hydration is accelerated 2.6-fold in the ventricular myocyte by endogenous CA. The rapid recovery phase represents a period when the intracellular CO2/HCO3− buffer is out of equilibrium (OOE). Modelling of the recovery phase using our k1 value, indicates that OOE conditions will normally extend for at least 2 min following a step rise in pHi (at constant PCO2). If CA is inactive, this period can be as long as 5 min. During normal pHi regulation, the recovery rate during these periods cannot be used as a measure of sarcolemmal acid loading since it is a mixture of slow CO2-dependent buffering and transmembrane acid loading. The implication of this finding for quantification of pHi regulation during alkalosis is discussed. PMID:9575296

Determination of acetanilide herbicides in cereal crops using accelerated solvent extraction, solid-phase extraction and gas chromatography-electron capture detector.

PubMed

Zhang, Yaping; Yang, Jun; Shi, Ronghua; Su, Qingde; Yao, Li; Li, Panpan

2011-07-01

A method was developed to determine eight acetanilide herbicides from cereal crops based on accelerated solvent extraction (ASE) and solid-phase extraction (SPE) followed by gas chromatography-electron capture detector (GC-ECD) analysis. During the ASE process, the effect of four parameters (temperature, static time, static cycles and solvent) on the extraction efficiency was considered and compared with shake-flask extraction method. After extraction with ASE, four SPE tubes (graphitic carbon black/primary secondary amine (GCB/PSA), GCB, Florisil and alumina-N) were assayed for comparison to obtain the best clean-up efficiency. The results show that GCB/PSA cartridge gave the best recoveries and cleanest chromatograms. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and recovery were studied. At 0.05 mg/kg spiked level, recoveries and precision values for rice, wheat and maize were 82.3-115.8 and 1.1-13.6%, respectively. For all the herbicides, LOD and LOQ ranged from 0.8 to 1.7 μg/kg and from 2.4 to 5.3 μg/kg, respectively. The proposed analytical methodology was applied for the analysis of the targets in samples; only three herbicides, propyzamid, metolachlor and diflufenican, were detected in two samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hydrophilic interaction liquid chromatographic analysis of aminohydroxyphenylalanines from melanin pigments.

PubMed

Nezirević, Dzeneta; Arstrand, Kerstin; Kågedal, Bertil

2007-09-07

Malignant melanomas are more often seen in subjects with light colored skin who tan poorly than in persons who tan more rapidly. This has been attributed to the structure of their pigment, pheomelanin, which differs markedly from the eumelanin of persons with darker skin. To study the hydrolysis products of pheomelanin pigments a new method was developed for analysis of 4-amino-3-hydroxyphenylalanine (4-AHP) and 3-amino-4-hydroxyphenylalanine (3-AHP). Pheomelanin samples were hydrolyzed and extracted with solid-phase extraction columns using strong cation-exchange (SCX) cartridges. Separation of 4-AHP and 3-AHP was achieved on a ZIC-HILIC column (150 mm x 2.1mm I.D.) with a mobile phase consisting of acetonitrile: 0.1 M ammonium acetate buffer, pH 4.5 (82:18, v/v). Detection was performed with an electrochemical detector at +400 mV. Run time was 30 min. The limits of detection were 73 pg and 51 pg for 4-AHP and 3-AHP respectively, using 2 microl injections. Good linearity was found within the range 0.05-5.0 microg/ml. Absolute recovery was 70% and relative recovery was 100%. The AHPs were stable for 1 year in the hydrolyzed samples, for 4 days in the eluates from solid-phase sorbents stored in the refrigerator, and for 2 days diluted with mobile phase and stored in the autosampler at 10 degrees C. The within-day imprecision was <5% and the between-day imprecision was <7% for the two analytes. The method, applied to the analysis of pheomelanin in urine from human melanoma patients, allows the analysis of 30 samples in one set and is suitable for routine work with human hair and melanoma cells. By using the ZIC-HILIC stationary phase, ion-pairing reagents could be avoided, which makes the method suitable to further analysis of degradation products from pheomelanins using mass spectrometric detection.

Translational MR Neuroimaging of Stroke and Recovery

PubMed Central

Mandeville, Emiri T.; Ayata, Cenk; Zheng, Yi; Mandeville, Joseph B.

2016-01-01

Multiparametric magnetic resonance imaging (MRI) has become a critical clinical tool for diagnosing focal ischemic stroke severity, staging treatment, and predicting outcome. Imaging during the acute phase focuses on tissue viability in the stroke vicinity, while imaging during recovery requires the evaluation of distributed structural and functional connectivity. Preclinical MRI of experimental stroke models provides validation of non-invasive biomarkers in terms of cellular and molecular mechanisms, while also providing a translational platform for evaluation of prospective therapies. This brief review of translational stroke imaging discusses the acute to chronic imaging transition, the principles underlying common MRI methods employed in stroke research, and experimental results obtained by clinical and preclinical imaging to determine tissue viability, vascular remodeling, structural connectivity of major white matter tracts, and functional connectivity using task-based and resting-state fMRI during the stroke recovery process. PMID:27578048

Resolving Phase Ambiguities In OQPSK

NASA Technical Reports Server (NTRS)

Nguyen, Tien M.

1991-01-01

Improved design for modulator and demodulator in offset-quaternary-phase-key-shifting (OQPSK) communication system enables receiver to resolve ambiguity in estimated phase of received signal. Features include unique-code-word modulation and detection and digital implementation of Costas loop in carrier-recovery subsystem. Enchances performance of carrier-recovery subsystem, reduces complexity of receiver by removing redundant circuits from previous design, and eliminates dependence of timing in receiver upon parallel-to-serial-conversion clock.

Aqueous enzymatic extraction of Moringa oleifera oil.

PubMed

Mat Yusoff, Masni; Gordon, Michael H; Ezeh, Onyinye; Niranjan, Keshavan

2016-11-15

This paper reports on the extraction of Moringa oleifera (MO) oil by using aqueous enzymatic extraction (AEE) method. The effect of different process parameters on the oil recovery was discovered by using statistical optimization, besides the effect of selected parameters on the formation of its oil-in-water cream emulsions. Within the pre-determined ranges, the use of pH 4.5, moisture/kernel ratio of 8:1 (w/w), and 300stroke/min shaking speed at 40°C for 1h incubation time resulted in highest oil recovery of approximately 70% (goil/g solvent-extracted oil). These optimized parameters also result in a very thin emulsion layer, indicating minute amount of emulsion formed. Zero oil recovery with thick emulsion were observed when the used aqueous phase was re-utilized for another AEE process. The findings suggest that the critical selection of AEE parameters is key to high oil recovery with minimum emulsion formation thereby lowering the load on the de-emulsification step. Copyright © 2016 Elsevier Ltd. All rights reserved.

The Recovery Process When Participating in Cancer Support and Rehabilitation Programs in Sweden

PubMed Central

Melin-Johansson, Christina; Öhlén, Joakim; Koinberg, Ingalill; Berg, Linda; Nolbris, Margaretha Jenholt

2015-01-01

The aim was to illuminate the meaning of participating in support and rehabilitation programs described by people diagnosed with cancer. Nineteen persons were interviewed in focus groups and face-to-face. Data were analyzed with a qualitative phenomenological hermeneutical method for researching lived experiences. Interpretation proceeded through three phases: naïve reading, structural analysis, and comprehensive understanding. Three themes were disclosed: receiving support for recovery when being most vulnerable, recapturing capabilities through supportive activities, and searching to find stability and well-being in a changed life situation. Participating in the programs was an existential transition from living in an unpredictable situation that was turned into something meaningful. Recovery did not mean the return to a state of normality; rather, it meant a continuing recovery from cancer treatments and symptoms involving recapturing capabilities and searching for a balance in a forever changed life. This study provides new insights about the experiences of participating in cancer support and rehabilitation programs. PMID:28462312

Getting More Ecologically Relevant Information from Laboratory Tests: Recovery of Lemna minor After Exposure to Herbicides and Their Mixtures.

PubMed

Knežević, Varja; Tunić, Tanja; Gajić, Pero; Marjan, Patricija; Savić, Danko; Tenji, Dina; Teodorović, Ivana

2016-11-01

Recovery after exposure to herbicides-atrazine, isoproturon, and trifluralin-their binary and ternary mixtures, was studied under laboratory conditions using a slightly adapted standard protocol for Lemna minor. The objectives of the present study were (1) to compare empirical to predicted toxicity of selected herbicide mixtures; (2) to assess L. minor recovery potential after exposure to selected individual herbicides and their mixtures; and (3) to suggest an appropriate recovery potential assessment approach and endpoint in a modified laboratory growth inhibition test. The deviation of empirical from predicted toxicity was highest in binary mixtures of dissimilarly acting herbicides. The concentration addition model slightly underestimated mixture effects, indicating potential synergistic interactions between photosynthetic inhibitors (atrazine and isoproturon) and a cell mitosis inhibitor (trifluralin). Recovery after exposure to the binary mixture of atrazine and isoproturon was fast and concentration-independent: no significant differences between relative growth rates (RGRs) in any of the mixtures (IC10 Mix , 25 Mix , and 50 Mix ) versus control level were recorded in the last interval of the recovery phase. The recovery of the plants exposed to binary and ternary mixtures of dissimilarly acting herbicides was strictly concentration-dependent. Only plants exposed to IC10 Mix , regardless of the herbicides, recovered RGRs close to control level in the last interval of the recovery phase. The inhibition of the RGRs in the last interval of the recovery phase compared with the control level is a proposed endpoint that could inform on reversibility of the effects and indicate possible mixture effects on plant population recovery potential.

Determination of three steroidal saponins from Ophiopogon japonicus (Liliaceae) via high-performance liquid chromatography with mass spectrometry.

PubMed

Wang, Yongyi; Xu, Jinzhong; Qu, Haibin

2013-01-01

A simple and accurate analytical method was developed for simultaneous quantification of three steroidal saponins in the roots of Ophiopogon japonicus via high-performance liquid chromatography (HPLC) with mass spectrometry (MS) in this study. Separation was performed on a Tigerkin C(18) column and detection was performed by mass spectrometry. A mobile phase consisted of 0.02% formic acid in water (v/v) and 0.02% formic acid in acetonitrile (v/v) was used with a flow rate of 0.5 mL min(-1). The quantitative HPLC-MS method was validated for linearity, precision, repeatability, stability, recovery, limits of detection and quantification. This developed method provides good linearity (r >0.9993), intra- and inter-day precisions (RSD <4.18%), repeatability (RSD <5.05%), stability (RSD <2.08%) and recovery (93.82-102.84%) for three steroidal saponins. It could be considered as a suitable quality control method for O. japonicus.

Standardized measurement of recovery from nonspecific back pain.

PubMed

Hush, Julia M; Kamper, Steven J; Stanton, Tasha R; Ostelo, Raymond; Refshauge, Kathryn M

2012-05-01

To propose standardized, patient-centered measures of recovery from nonspecific low back pain (LBP) in research, underpinned by an empirically derived concept of recovery and informed by expert opinion. Synthesis of literature reviews and expert panel opinion. Primary care centers for the management of nonspecific LBP. Persons with nonspecific LBP. Conservative treatments for nonspecific LBP. Three phases of research were conducted. First, qualitative research that explored patients' perspectives of recovery from nonspecific LBP was reviewed. Second, measures of recovery used in LBP clinical trials during the past decade were investigated in a systematic review. Third, opinion was sought from an expert panel of clinicians and researchers about how to measure recovery from nonspecific LBP, in a workshop at the 10th International Forum for Primary Care Research in Low Back Pain. An empirically derived and patient-centered concept of recovery from nonspecific LBP was developed from the qualitative research phase. The systematic review conducted in the second study phase revealed that researchers have used vastly heterogeneous measures of LBP recovery in clinical trials during the past decade. Finally, the key conclusions of the LBP Forum workshop were (1) that appropriate patient-centered instruments to measure recovery include global measures and patient-specific measures; and (2) that the benefits of implementing the same recovery measures for acute and chronic LBP outweigh the disadvantages of using different measures. The results were synthesized to inform our recommendation that researchers consider adopting 2 instruments as standardized measures of recovery from nonspecific LBP, as an adjunct to the existing core set of LBP outcome measures. These instruments are an 11-point Global Back Recovery Scale, for a simple measure of global recovery, and the Patient-Generated Index of Quality of Life-Back Pain, to evaluate specific relevant dimensions of recovery. This recommendation has majority endorsement by members of the Australian National Health and Medical Research Council Acute Low Back Pain Review Group. Copyright © 2012 American Congress of Rehabilitation Medicine. Published by Elsevier Inc. All rights reserved.

Advanced Natural Gas Reciprocating Engine(s)

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

Pike, Edward

The objective of the Cummins ARES program, in partnership with the US Department of Energy (DOE), is to develop advanced natural gas engine technologies that increase engine system efficiency at lower emissions levels while attaining lower cost of ownership. The goals of the project are to demonstrate engine system achieving 50% Brake Thermal Efficiency (BTE) in three phases, 44%, 47% and 50% (starting baseline efficiency at 36% BTE) and 0.1 g/bhp-hr NOx system out emissions (starting baseline NOx emissions at 2 – 4 g/bhp-hr NOx). Primary path towards above goals include high Brake Mean Effective Pressure (BMEP), improved closed cyclemore » efficiency, increased air handling efficiency and optimized engine subsystems. Cummins has successfully demonstrated each of the phases of this program. All targets have been achieved through application of a combined set of advanced base engine technologies and Waste Heat Recovery from Charge Air and Exhaust streams, optimized and validated on the demonstration engine and other large engines. The following architectures were selected for each Phase: Phase 1: Lean Burn Spark Ignited (SI) Key Technologies: High Efficiency Turbocharging, Higher Efficiency Combustion System. In production on the 60/91L engines. Over 500MW of ARES Phase 1 technology has been sold. Phase 2: Lean Burn Technology with Exhaust Waste Heat Recovery (WHR) System Key Technologies: Advanced Ignition System, Combustion Improvement, Integrated Waste Heat Recovery System. Base engine technologies intended for production within 2 to 3 years Phase 3: Lean Burn Technology with Exhaust and Charge Air Waste Heat Recovery System Key Technologies: Lower Friction, New Cylinder Head Designs, Improved Integrated Waste Heat Recovery System. Intended for production within 5 to 6 years Cummins is committed to the launch of next generation of large advanced NG engines based on ARES technology to be commercialized worldwide.« less

Gas chromatographic-mass spectrometric determination of alkylphosphonic acids from aqueous samples by ion-pair solid-phase extraction on activated charcoal and methylation.

PubMed

Vijaya Saradhi, U V R; Prabhakar, S; Jagadeshwar Reddy, T; Murty, M R V S

2007-07-20

In the present paper, we report an improved ion-pair solid-phase extraction (IP-SPE) method for the analysis of alkylphosphonic acids, namely, methyl, ethyl and propylphosphonic acids, present in the aqueous sample. The aqueous sample was mixed with an ion-pair reagent, phenyltrimethylammonium hydroxide (PTMAH) and passed through activated charcoal SPE cartridge. The retained chemicals in the cartridge were extracted with methanol and analysed by gas chromatography-mass spectrometry (GC-MS) under the electron impact ionization (EI) mode. The analytes were converted to their methyl esters by pyrolytic methylation in the hot GC injection port. The recoveries of alkylphosphonic acids were above 95% and the minimum detection limits were as low as 10 ng/mL. The recovery of the test chemicals was tested with solvents, dichloromethane, n-hexane, ethyl acetate, acetone, acetonitrile and methanol. The chemicals could be efficiently extracted by the hydrophilic solvents. The method did not work at the highly acidic pH (when acidified with dilute HCl) but worked well from pH 4.0 to 14.0. The present method was also tested with other tetra-(methyl, ethyl, propyl and n-butyl)ammonium hydroxides. The test chemicals were not converted to their methyl and ethyl esters with tetramethyl and tetraethylammonium hydroxides, whereas they were converted to their corresponding propyl and n-butyl esters with tetrapropyl and tetra(n-butyl)ammonium hydroxides. The method was also applied to two highly cross-linked polymeric sorbents DSC-6S and Oasis HLB. The recovery of the chemicals on these sorbents was observed to be poor. Methylation using phenyltrimethylammonium hydroxide is non-hazardous and advantageous over methylation using diazomethane. The method was applied to the analysis of aqueous samples given in one of the official proficiency tests conducted by the Organization for the Prohibition of Chemical Weapons and all the spiked chemicals were identified as methyl esters.

[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.

Wavefront reconstruction for multi-lateral shearing interferometry using difference Zernike polynomials fitting

NASA Astrophysics Data System (ADS)

Liu, Ke; Wang, Jiannian; Wang, Hai; Li, Yanqiu

2018-07-01

For the multi-lateral shearing interferometers (multi-LSIs), the measurement accuracy can be enhanced by estimating the wavefront under test with the multidirectional phase information encoded in the shearing interferogram. Usually the multi-LSIs reconstruct the test wavefront from the phase derivatives in multiple directions using the discrete Fourier transforms (DFT) method, which is only suitable to small shear ratios and relatively sensitive to noise. To improve the accuracy of multi-LSIs, wavefront reconstruction from the multidirectional phase differences using the difference Zernike polynomials fitting (DZPF) method is proposed in this paper. For the DZPF method applied in the quadriwave LSI, difference Zernike polynomials in only two orthogonal shear directions are required to represent the phase differences in multiple shear directions. In this way, the test wavefront can be reconstructed from the phase differences in multiple shear directions using a noise-variance weighted least-squares method with almost no extra computational burden, compared with the usual recovery from the phase differences in two orthogonal directions. Numerical simulation results show that the DZPF method can maintain high reconstruction accuracy in a wider range of shear ratios and has much better anti-noise performance than the DFT method. A null test experiment of the quadriwave LSI has been conducted and the experimental results show that the measurement accuracy of the quadriwave LSI can be improved from 0.0054 λ rms to 0.0029 λ rms (λ = 632.8 nm) by substituting the DFT method with the proposed DZPF method in the wavefront reconstruction process.

Social support in the post-abortion recovery room: evidence from patients, support persons and nurses in a Vancouver clinic.

PubMed

Veiga, Mariana B; Lam, Melanie; Gemeinhardt, Carla; Houlihan, Edwina; Fitzsimmons, Brian P; Hodgson, Zoë G

2011-03-01

The benefits of social support in post-surgical recovery are well documented; social support decreases preoperative stress and postoperative recovery time. However, a paucity of studies have examined the effect of social support in the context of pregnancy termination. This study is the first to examine the effect of postoperative accompaniment from the patient, support person and nurses' perspective. This study was carried out in two phases. In Phase I, no accompaniment was allowed in the post-anesthesia recovery room (PAR); in Phase II, accompaniment was permitted. All participants completed pre- and postoperative questionnaires. The perception of accompaniment was overwhelmingly positive in patients and support people. Patients in Phase II demonstrated a high (over 95%) acceptance of accompaniment in the recovery room. It was found that 96.8% reported they would choose to be accompanied in the recovery room again if they had to have another abortion. Support persons felt very strongly that their presence was helpful to the patient. The decrease in pre- to postoperative anxiety levels was significantly greater in those women who were accompanied. However, overall, nurses demonstrated a negative attitude towards accompaniment in the recovery room. In summary, the presence of a support person in the PAR was perceived in a positive manner by patients and support people. However, the reasoning behind the negative opinion of nurses requires further study before PAR accompaniment can be considered a possibility in the context of pregnancy termination. Copyright © 2011 Elsevier Inc. All rights reserved.

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.

Fate of Neutrophils during the Recovery Phase of Ischemia/Reperfusion Induced Acute Kidney Injury

PubMed Central

2017-01-01

Effective clearance of inflammatory cells is required for resolution of inflammation. Here, we show in vivo evidence that apoptosis and reverse transendothelial migration (rTEM) are important mechanisms in eliminating neutrophils and facilitating recovery following ischemia/reperfusion injury (IRI) of the kidney. The clearance of neutrophils was delayed in the Bax knockout (KO)BM → wild-type (WT) chimera in which bone marrow derived cells are partially resistant to apoptosis, compared to WTBM → WT mice. These mice also showed delayed functional, histological recovery, increased tissue cytokines, and accelerated fibrosis. The circulating intercellular adhesion molecule-1 (ICAM-1)+ Gr-1+ neutrophils displaying rTEM phenotype increased during the recovery phase and blockade of junctional adhesion molecule-C (JAM-C), a negative regulator of rTEM, resulted in an increase in circulating ICAM-1+ neutrophils, faster resolution of inflammation and recovery. The presence of Tamm-Horsfall protein (THP) in circulating ICAM-1+ neutrophils could suggest that they are derived from injured kidneys. In conclusion, we suggest that apoptosis and rTEM are critically involved in the clearance mechanisms of neutrophils during the recovery phase of IRI. PMID:28875605

Electro-assisted solid-phase microextraction based on poly(3,4-ethylenedioxythiophen) combined with GC for the quantification of tricyclic antidepressants.

PubMed

Davarani, Saied Saeed Hosseiny; Nojavan, Saeed; Asadi, Roghayeh; Banitaba, Mohammad Hossein

2013-07-01

In this study, a platinum wire coated with poly(3,4-ethylenedioxythiophen) was used as an electro-assisted solid-phase microextraction fiber for the quantification of tricyclic antidepressant drugs in biological samples by coupling to GC employing a flame ionization detector. In this study, an electric field increased the extraction rate and recovery. The fiber used as a solid phase was synthesized by the electropolymerization of 3,4-ethylenedioxythiophen monomers onto a platinum wire. The ability of this fiber to extract imipramine, desipramine, and clomipramine by using the electro-assisted solid-phase microextraction technique was evaluated. The effect of various parameters that influence the extraction efficiency, which include solution temperature, extraction time, stirring rate, ionic strength, time and temperature of desorption, and thickness of the fiber, was optimized. Under optimized conditions, the linear ranges and regression coefficients of calibration curves were in the range of 0.5-250 and 0.990-0.998 ng/mL, respectively. Detection limits were in the range of 0.15-0.45 ng/mL. Finally, this method was applied to the determination of drugs in urine and wastewater samples and recoveries were 4.8-108.9%. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Molecularly imprinted solid phase extraction for simultaneous determination of Δ9-tetrahydrocannabinol and its main metabolites by gas chromatography-mass spectrometry in urine samples.

PubMed

Nestić, Marina; Babić, Sandra; Pavlović, Dragana Mutavdžić; Sutlović, Davorka

2013-09-10

In presented paper analytical method based on solid-phase extraction using molecularly imprinted polymer and gas chromatography-mass spectrometry has been developed and validated for the confirmation of THC, THC-OH and THC-COOH in urine samples. Non-covalent molecularly imprinted polymers of THC-OH were prepared using different functional monomers (methacrylic acid, 4-vinylpyridine, and 2-hydroxyethyl methacrylate), ethylene glycol dimethacrylate as a cross-linker and 2,2'-azobis-isobutyronitrile as an initiator of radical polymerization. Analytes were extracted from urine samples using prepared polymer sorbent with highest binding selectivity and capability. Before extraction, urine samples were hydrolyzed with alkaline. Elution was performed with chloroform:ethyl acetate (60:40, v/v). Dry extracts were silylated with BSTFA+1% TMCS. Detection and quantification were performed using gas chromatography-mass spectrometry in single ion recording mode. The developed method was linear over the range from LOQ to 150 ng mL(-1) for all three analytes. For THC, THC-OH and THC-COOH LOD was 2.5, 1 and 1 ng mL(-1), and LOQ was 3, 2 and 2 ng mL(-1), respectively. The precision, accuracy, recovery and matrix effect were investigated at 5, 25 and 50 ng mL(-1). In the investigated concentration range recoveries were 71.9% for THC, 78.6% for THC-OH and 75.2% for THC-COOH. Matrix effect was not significant (<10%) for all analytes in the concentration range from 5 ng mL(-1) to 50 ng mL(-1). Extraction recovery on non-imprinted polymer was relatively high indicating high non-specific binding. Optimized and validated method was applied to 15 post-mortem urine samples. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Periodic mesoporous organosilica materials as sorbents for solid-phase extraction of drugs prior to simultaneous enantiomeric separation by capillary electrophoresis.

PubMed

Valimaña-Traverso, Jesús; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; García, María Ángeles; Sierra, Isabel; Marina, María Luisa

2018-06-19

Two novel periodic mesoporous organosilica materials were synthesized with a neutral phenylene-bridged ligand, 1,4-bis(trimethoxysilylethyl)benzene, one of them using tetraethyl orthosilicate as additional silica source (PMO-TMSEB-1 and PMO-TMSEB-2). A third material was also synthesized with 1,4-bis(triethoxysilyl)benzene ligand (PMO-TESB-1) which use has scarcely been reported. The three materials were evaluated as solid-phase extraction (SPE) sorbents for the off-line extraction of a mixture of seven drugs of different nature (duloxetine, terbutaline, econazole, propranolol, verapamil, metoprolol, and betaxolol) from water samples. Subsequent simultaneous enantiomeric analysis by CE, using sulfated-β-cyclodextrin (2% w/v) dissolved in a 25 mM phosphate buffer (pH 3.0) and a voltage of -20 kV (negative polarity) was carried out. Enantiomeric resolutions ranging from 2.4 to 8.5 were obtained in an analysis time of 16 min. After optimization of SPE parameters, it was shown that using just 100 mg of PMO-TESB-1 as sorbent, a preconcentration factor of 400 with 200 mL solution was achieved, allowing recoveries between 80.5 and 103.1% (except for terbutaline), with good repeatability (% RSD = 2-8 %, n = 5). Analytical characteristics of the method were evaluated in terms of precision, linearity and accuracy with method quantitation limits between 5.6 and 21.9 μg/L. The developed method was applied to the analysis of spiked wastewater samples collected in different treatment plants, with recoveries between 73.9 and 102.9% except for econazole with recovery values ranging between 58.5 and 72.4%. Copyright © 2018 Elsevier B.V. All rights reserved.

Micro versus macro solid phase extraction for monitoring water contaminants: a preliminary study using trihalomethanes.

PubMed

Alexandrou, Lydon D; Spencer, Michelle J S; Morrison, Paul D; Meehan, Barry J; Jones, Oliver A H

2015-04-15

Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental science. However, traditional methods need electrically powered pumps, can use large volumes of solvent (if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and provides comparable concentration factors to established methods. It is also an enclosed system so volatile components are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required. However, the technology is new and has not been much used for environmental analysis. In this study we compare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile trihalomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane). The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with similar recovery rates for the target compounds. This method shows potential for further development in a range of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

[Performance evaluation of a fluorescamine-HPLC method for determination of histamine in fish and fish products].

PubMed

Kikuchi, Hiroyuki; Tsutsumi, Tomoaki; Matsuda, Rieko

2012-01-01

A method for the quantification of histamine in fish and fish products using tandem solid-phase extraction and fluorescence derivatization with fluorescamine was previously developed. In this study, we improved this analytical method to develop an official test method for quantification of histamine in fish and fish products, and performed a single laboratory study to validate it. Recovery tests of histamine from fillet (Thunnus obesus), and two fish products (fish sauce and salted and dried whole big-eye sardine) that were spiked at the level of 25 and 50 µg/g for T. obesus, and 50 and 100 µg/g for the two fish products, were carried out. The recoveries of histamine from the three samples tested were 88.8-99.6% with good repeatability (1.3-2.1%) and reproducibility (2.1-4.7%). Therefore, this method is acceptable for the quantification of histamine in fish and fish products. Moreover, surveillance of histamine content in food on the market was conducted using this method, and high levels of histamine were detected in some fish products.

Simultaneous determination of aliskiren and hydrochlorothiazide in tablets and spiked human urine by ion-pair liquid chromatography.

PubMed

Belal, F; Walash, M; El-Enany, N; Zayed, S

2013-12-01

An alternative method for analysis of aliskiren (ALI) and hydrochlorothiazde (HCT) in combined dosage forms by ion-pair reversed phase high performance liquid chromatography was developed and validated. The pharmaceutical preparations were analyzed using a C18 column (250 mm x 4.6 mm, 3 microm) with a mobile phase consisting of 25% methanol, 50% sodium monobasic phosphate aqueous solution containing 6 mM tetrabutylammonium bromide and 25% water at pH 7.2. Isocratic analysis was performed at a flow rate of 1 mL/min and a column temperature of 30 degrees C under direct UV detection at 210 nm. Paracetamol was used as internal standard. The validation was performed according to the ICH guidelines. The proposed method was linear over the concentration range of 0.250 to 60 and 0.1 to 10 microg/mL for ALI and HCT, respectively. The limits of detection and quantitation (LOD and LOQ) were 0.075 and 0.198 microg/mL, respectively, for ALI and 0.04 and 0.062 microg/mL, respectively, for HCT. The method proved to be specific, sensitive, precise and accurate with mean recovery values of 101.1 +/- 0.32% and 100.9 +/- 0.41% for ALI and HCT, respectively. The method robustness was evaluated by means of an experimental design. The proposed method was applied successfully to spiked human urine samples with mean recoveries of 98.8 +/- 0.36% and 98.1 +/- 0.21% for ALI and HCT, respectively.

QbD-oriented development and validation of a bioanalytical method for nevirapine with enhanced liquid-liquid extraction and chromatographic separation.

PubMed

Beg, Sarwar; Chaudhary, Vandna; Sharma, Gajanand; Garg, Babita; Panda, Sagar Suman; Singh, Bhupinder

2016-06-01

The present studies describe the systematic quality by design (QbD)-oriented development and validation of a simple, rapid, sensitive and cost-effective reversed-phase HPLC bioanalytical method for nevirapine in rat plasma. Chromatographic separation was carried out on a C18 column using isocratic 68:9:23% v/v elution of methanol, acetonitrile and water (pH 3, adjusted by orthophosphoric acid) at a flow rate of 1.0 mL/min using UV detection at 230 nm. A Box-Behnken design was applied for chromatographic method optimization taking mobile phase ratio, pH and flow rate as the critical method parameters (CMPs) from screening studies. Peak area, retention time, theoretical plates and peak tailing were measured as the critical analytical attributes (CAAs). Further, the bioanalytical liquid-liquid extraction process was optimized using an optimal design by selecting extraction time, centrifugation speed and temperature as the CMPs for percentage recovery of nevirapine as the CAA. The search for an optimum chromatographic solution was conducted through numerical desirability function. Validation studies performed as per the US Food and Drug Administration requirements revealed results within the acceptance limit. In a nutshell, the studies successfully demonstrate the utility of analytical QbD approach for the rational development of a bioanalytical method with enhanced chromatographic separation and recovery of nevirapine in rat plasma. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Development, validation, and application of a method for selected avermectin determination in rural waters using high performance liquid chromatography and fluorescence detection.

PubMed

Lemos, Maria Augusta Travassos; Matos, Camila Alves; de Resende, Michele Fabri; Prado, Rachel Bardy; Donagemma, Raquel Andrade; Netto, Annibal Duarte Pereira

2016-11-01

Avermectins (AVM) are macrocyclic lactones used in livestock and agriculture. A quantitative method of high performance liquid chromatography with fluorescence detection for the determination of eprinomectin, abamectin, doramectin and ivermectin in rural water samples was developed and validated. The method was employed to study samples collected in the Pito Aceso River microbasin, located in the Bom Jardim municipality, Rio de Janeiro State, Brazil. Samples were extracted by solid phase extraction using a polymeric stationary phase, the eluted fraction was re-concentrated under a gentle N2 flow and derivatized to allow AVM determination using liquid chromatography with fluorescence detection. The excitation and emission wavelengths of the derivatives were 365 and 470nm, respectively, and a total chromatographic run of 12min was achieved. Very low limits of quantification (22-58ngL(-1)) were found after re-concentration using N2. Recovery values varied from 85.7% to 119.2% with standard deviations between 1.2% and 10.2%. The validated method was applied in the determination of AVM in 15 water samples collected in the Pito Aceso River microbasin, but most of them were free of AVM or showed only trace levels of these compounds, except for a sample that contained doramectin (9.11µgL(-1)). The method is suitable for routine analysis with satisfactory recovery, sensitivity, and selectivity. Copyright © 2016 Elsevier Inc. All rights reserved.

[Determination of genkwanin in flos Genkwa by HPLC].

PubMed

Zhang, B; Yuan, S; Xia, K

1996-04-01

In this paper, the method for determining genkwanin in Flos Genkwa was established by HPLC. Detected at 332nm on a Lichrosorb 5 RP-18 column with a mobile phase of methanol-water-acetic acid (65:35:5), the content of genkwanin in Flos Genkwa was determined to be 0.16%. The recovery rate was 95.46% and RSD 1.15%.

Mixed-mode isolation of triazine metabolites from soil and aquifer sediments using automated solid-phase extraction

USGS Publications Warehouse

Mills, M.S.; Thurman, E.M.

1992-01-01

Reversed-phase isolation and ion-exchange purification were combined in the automated solid-phase extraction of two polar s-triazine metabolites, 2-amino-4-chloro-6-(isopropylamino)-s-triazine (deethylatrazine) and 2-amino-4-chloro-6-(ethylamino)-s-triazine (deisopropylatrazine) from clay-loam and slit-loam soils and sandy aquifer sediments. First, methanol/ water (4/1, v/v) soil extracts were transferred to an automated workstation following evaporation of the methanol phase for the rapid reversed-phase isolation of the metabolites on an octadecylresin (C18). The retention of the triazine metabolites on C18 decreased substantially when trace methanol concentrations (1%) remained. Furthermore, the retention on C18 increased with decreasing aqueous solubility and increasing alkyl-chain length of the metabolites and parent herbicides, indicating a reversed-phase interaction. The analytes were eluted with ethyl acetate, which left much of the soil organic-matter impurities on the resin. Second, the small-volume organic eluate was purified on an anion-exchange resin (0.5 mL/min) to extract the remaining soil pigments that could foul the ion source of the GC/MS system. Recoveries of the analytes were 75%, using deuterated atrazine as a surrogate, and were comparable to recoveries by soxhlet extraction. The detection limit was 0.1 ??g/kg with a coefficient of variation of 15%. The ease and efficiency of this automated method makes it viable, practical technique for studying triazine metabolites in the environment.

Facile synthesis of poly(ionic liquid)-bonded magnetic nanospheres as a high-performance sorbent for the pretreatment and determination of phenolic compounds in water samples.

PubMed

Bi, Wentao; Wang, Man; Yang, Xiaodi; Row, Kyung Ho

2014-07-01

Poly(ionic liquid)-bonded magnetic nanospheres were easily synthesized and applied to the pretreatment and determination of phenolic compounds in water samples, which have detrimental effects on water quality and the health of living beings. The high affinity of poly(ionic liquid)s toward the target compounds as well as the magnetic behavior of Fe3 O4 were combined in this material to provide an efficient and simple magnetic solid-phase extraction approach. The adsorption behavior of the poly(ionic liquid)-bonded magnetic nanospheres was examined to optimize the synthesis. Different parameters affecting the magnetic solid-phase extraction of phenolic compounds were assessed in terms of adsorption and recovery. Under the optimal conditions, the proposed method showed excellent detection sensitivity with limits of detection in the range of 0.3-0.8 ng/mL and precision in the range of 1.2-3.3%. This method was also applied successfully to the analysis of real water samples; good spiked recoveries over the range of 82.5-99.2% were obtained. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Isotope dilution gas chromatography with mass spectrometry for the analysis of 4-octyl phenol, 4-nonylphenol, and bisphenol A in vegetable oils.

PubMed

Wu, Pinggu; Zhang, Liqun; Yang, Dajin; Zhang, Jing; Hu, Zhengyan; Wang, Liyuan; Ma, Bingjie

2016-03-01

By the combination of solid-phase extraction as well as isotope dilution gas chromatography with mass spectrometry, a sensitive and reliable method for the determination of endocrine-disrupting chemicals including bisphenol A, 4-octylphenol, and 4-nonylphenol in vegetable oils was established. The application of a silica/N-(n-propyl)ethylenediamine mixed solid-phase extraction cartridge achieved relatively low matrix effects for bisphenol A, 4-octylphenol, and 4-nonylphenol in vegetable oils. Experiments were designed to evaluate the effects of derivatization, and the extraction parameters were optimized. The estimated limits of detection and quantification for bisphenol A, 4-octylphenol, and 4-nonylphenol were 0.83 and 2.5 μg/kg, respectively. In a spiked experiment in vegetable oils, the recovery of the added bisphenol A was 97.5-110.3%, recovery of the added 4-octylphenol was 64.4-87.4%, and that of 4-nonylphenol was 68.2-89.3%. This sensitive method was then applied to real vegetable oil samples from Zhejiang Province of China, and none of the target compounds were detected. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of phthalic acid esters in water samples by hollow fiber liquid-phase microextraction prior to gas chromatography tandem mass spectrometry.

PubMed

González-Sálamo, Javier; González-Curbelo, Miguel Ángel; Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel

2018-06-01

A new hollow fiber liquid-phase microextraction (HF-LPME) method has been developed for the extraction of a group of phthalic acid esters (PAEs) of interest from different water samples prior to gas chromatography tandem mass spectrometry analysis. HF-LPME was carried out using 1-octanol as extraction solvent followed by a back extraction step with cyclohexane. The different parameters that affect HF-LPME such as sample pH, ionic strength, extraction time, stirring rate, extraction temperature and back extraction conditions were investigated. The optimized conditions involved the extraction of 10 mL of sample without pH adjustment or addition of salt during 75 min under a stirring of 850 rpm at 60 °C and subsequent desorption with 200 μL of cyclohexane for 10 min in an ultrasonic bath. The method was validated in terms of calibration and recovery studies using dibutyl phthalate-d 4 as internal standard. The developed procedure gave satisfactory recovery (74-120%) and relative standard deviation values (<20%) for the studied PAEs in mineral, tap, pond and waste water samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Determination of 10 sulfonamide residues in meat samples by liquid chromatography with ultraviolet detection.

PubMed

Di Sabatino, Marcello; Di Pietra, Anna Maria; Benfenati, Luigi; Di Simone, Bruno

2007-01-01

A liquid chromatography (LC) method is described for the simultaneous determination of 10 commonly used sulfonamide drug residues in meat. The 10 sulfonamide drugs of interest were sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamethizole, sulfamonomethoxine, sulfachloropyridazine, sulfadoxine, sulfadimethoxine, and sulfaquinoxaline. The residues were extracted with acetone-chloroform (1 + 1). Sulfonamides were quantitatively retained in the extracting solution and afterwards eluted from a cation-exchanger solid-phase extraction cartridge with a solution of methanol-aqueous ammonia. The solution was dried, reconstituted with 5 mL methanol and filtered before analysis by LC-ultraviolet using a C18 column with a mobile phase gradient of potassium dihydrogen phosphate buffer, pH 2.5, and methanol-acetonitrile (30 + 70, v/v). The method was applied to cattle, swine, chicken, and sheep muscle tissues. The validation was performed with a fortified cattle meat sample at level of 100 ppb, which is the administrative maximum residue limit for sulfonamides in the European Union. The limit of quantitation for all sulfonamides was between 3 and 14 ppb. Recovery was evaluated for different meat matrixes. The mean recovery values were between 66.3% for pork meat samples and 71.5% for cattle meat samples.

Ringer tablet-based ionic liquid phase microextraction: Application in extraction and preconcentration of neonicotinoid insecticides from fruit juice and vegetable samples.

PubMed

Farajzadeh, Mir Ali; Bamorowat, Mahdi; Mogaddam, Mohammad Reza Afshar

2016-11-01

An efficient, reliable, sensitive, rapid, and green analytical method for the extraction and determination of neonicotinoid insecticides in aqueous samples has been developed using ionic liquid phase microextraction coupled with high performance liquid chromatography-diode array detector. In this method, a few microliters of 1-hexyl-3-methylimidazolium hexafluorophosphate (as an extractant) is added onto a ringer tablet and it is transferred into a conical test tube containing aqueous phase of the analytes. By manually shaking, the ringer tablet is dissolved and the extractant is released into the aqueous phase as very tiny droplets to provide a cloudy solution. After centrifuging the extracted analytes into ionic liquid are collected at the bottom of a conical test tube. Under the optimum extraction conditions, the method showed low limits of detection and quantification between 0.12 and 0.33 and 0.41 and 1.11ngmL(-1), respectively. Extraction recoveries and enrichment factors were from 66% to 84% and 655% to 843%, respectively. Finally different aqueous samples were successfully analyzed using the proposed method. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of six pesticides in the medicinal herb Cordia salicifolia by matrix solid-phase dispersion and gas chromatography/mass spectrometry.

PubMed

de Carvalho, Pedro Henrique Viana; Prata, Vanessa de Menezes; Alves, Péricles Barreto; Navickiene, Sandro

2009-01-01

A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selected-ion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexane-dichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9%, with relative standard deviations between 6.3 and 26%. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.

Development and validation of a rapid reversed-phase HPLC method for the determination of the non-nucleoside reverse transcriptase inhibitor dapivirine from polymeric nanoparticles.

PubMed

das Neves, José; Sarmento, Bruno; Amiji, Mansoor M; Bahia, Maria Fernanda

2010-06-05

The objective of this work was to develop and validate a rapid reversed-phase (RP) high-performance liquid chromatography (HPLC) method for the in vitro pharmaceutical characterization of dapivirine-loaded polymeric nanoparticles. Chromatographic runs were performed on a RP C18 column with a mobile phase comprising acetonitrile-0.5% (w/v) triethanolamine solution in isocratic mode (80:20, v/v) at a flow rate of 1 ml/min. Dapivirine was detected at a wavelength of 290 nm. The method was shown to be specific, linear in the range of 1-50 microg/ml (R(2)=0.9998), precise at the intra-day and inter-day levels as reflected by the relative standard deviation values (less than 0.85%), accurate (recovery rate of 100.17+/-0.35%), and robust to changes in the mobile phase and column brand. The detection and quantitation limits were 0.08 and 0.24 microg/ml, respectively. The method was successfully used to determine the loading capacity and association efficiency of dapivirine in poly(lactic-co-glycolic acid)-based nanoparticles and its in vitro release. Copyright (c) 2010 Elsevier B.V. All rights reserved.

EEG patterns from acute to chronic stroke phases in focal cerebral ischemic rats: correlations with functional recovery.

PubMed

Zhang, Shao-jie; Ke, Zheng; Li, Le; Yip, Shea-ping; Tong, Kai-yu

2013-04-01

Monitoring the neural activities from the ischemic penumbra provides critical information on neurological recovery after stroke. The purpose of this study is to evaluate the temporal alterations of neural activities using electroencephalography (EEG) from the acute phase to the chronic phase, and to compare EEG with the degree of post-stroke motor function recovery in a rat model of focal ischemic stroke. Male Sprague-Dawley rats were subjected to 90 min transient middle cerebral artery occlusion surgery followed by reperfusion for seven days (n = 58). The EEG signals were recorded at the pre-stroke phase (0 h), acute phase (3, 6 h), subacute phase (12, 24, 48, 72 h) and chronic phase (96, 120, 144, 168 h) (n = 8). This study analyzed post-stroke seizures and polymorphic delta activities (PDAs) and calculated quantitative EEG parameters such as the alpha-to-delta ratio (ADR). The ADR represented the ratio between alpha power and delta power, which indicated how fast the EEG activities were. Forelimb and hindlimb motor functions were measured by De Ryck's test and the beam walking test, respectively. In the acute phase, delta power increased fourfold with the occurrence of PDAs, and the histological staining showed that the infarct was limited to the striatum and secondary sensory cortex. In the subacute phase, the alpha power reduced to 50% of the baseline, and the infarct progressed to the forelimb cortical region. ADRs reduced from 0.23 ± 0.09 to 0.04 ± 0.01 at 3 h in the acute phase and gradually recovered to 0.22 ± 0.08 at 168 h in the chronic phase. In the comparison of correlations between the EEG parameters and the limb motor function from the acute phase to the chronic phase, ADRs were found to have the highest correlation coefficients with the beam walking test (r = 0.9524, p < 0.05) and De Ryck's test (r = 0.8077, p < 0.05). This study measured EEG activities after focal cerebral ischemia and showed that functional recovery was closely correlated with the neural activities in the penumbra. Longitudinal EEG monitoring at different phases after a stroke can provide information on the neural activities, which are well correlated with the motor function recovery.

Optoelectrical clock recovery with dispersion monitoring for high speed transmission

NASA Astrophysics Data System (ADS)

Wen, He; Liao, Jinxin; Zheng, Xiaoping; Zhang, Hanyi; Guo, Yili

2010-12-01

The proposed clock recovery scheme introduces electrooptical modulation to down convert the clock frequency facilitating succeeding narrow band filtering by a phase locked loop (PLL) with ordinary radio frequency (RF) devices, further, employs a quadrature phase detector in the PLL to provide an indication signal for monitoring residual dispersion. It was demonstrated in a polarization multiplexed 160-Gbit/s optical non-return to zero quadrature phase shift keying (NRZ-QPSK) transmission system.

Content determination of aniracetam in aniracetam inclusion complex by HPLC.

PubMed

Li, Yongjian; Hu, Dejian; Sun, Yong

2009-01-01

We established a HPLC method for content determination of aniracetam in aniracetam inclusion complex. The chromato column was Agilent ODS (4.6mm x 150mm, 5 microm), the mobile phase was methanol-0.01 mol/L Potassium dihydrogen phosphate buffer solution (25:75, pH 3.0), with the flow rate of 1.0 ml/min, column temperature of 30 degrees and the detection wave at 280 nm, the sample size was 20microL. A good linear relationship was obtained between the peak areas and the concentrations of aniracetam in the range from 5- 80microg/ml (r=0.9998), the mean recovery was 100.1% (n=15), RSD=0.19%. This method is convenient, rapid, accurate, and brings about good recovery; it can be used for content determination of aniracetam in aniracetam inclusion complex.

Applicability of multisyringe chromatography coupled to on-line solid-phase extraction to the simultaneous determination of dicamba, 2,4-D, and atrazine.

PubMed

Chávez-Moreno, C A; Guzmán-Mar, J L; Hinojosa-Reyes, L; Hernández-Ramírez, A; Ferrer, L; Cerdà, V

2012-07-01

Simultaneous determination of three herbicides (dicamba, 2,4-D, and atrazine) has been achieved by on-line solid-phase extraction (SPE) coupled to multisyringe chromatography (MSC) with UV detection. The preconcentration conditions were optimized; a preconcentration flow rate of 0.5 mL min(-1) and elution at 0.8 mL min(-1) were the optimum conditions. A C(18) (8 mm i.d.) membrane extraction disk conditioned with 0.3 mol L(-1) HCl in 0.5% MeOH was used. A 3-mL sample was preconcentrated, then eluted with 0.43 mL 40:60 water-MeOH. A C(18) monolithic column (25 mm × 4.6 mm) was used for chromatographic separation. Separation of the three compounds was achieved in 10 min by use of 0.01% aqueous acetic acid-MeOH (60:40) as mobile phase at a flow rate of 0.8 mL min(-1). The limits of detection (LOD) were 13, 57, and 22 μg L(-1) for dicamba, 2,4-D, and atrazine, respectively. The sampling frequency was three analyses per hour, and each analysis consumed only 7.3 mL solvent. The method was applied to spiked water samples, and recovery between 85 and 112% was obtained. Recovery was significantly better than in the conventional HPLC-UV method. These results indicated the reliability and accuracy of this flow-based method. This is the first time this family of herbicides has been simultaneously analyzed by on-line SPE-MSC using a monolithic column.

Isotropic differential phase contrast microscopy for quantitative phase bio-imaging.

PubMed

Chen, Hsi-Hsun; Lin, Yu-Zi; Luo, Yuan

2018-05-16

Quantitative phase imaging (QPI) has been investigated to retrieve optical phase information of an object and applied to biological microscopy and related medical studies. In recent examples, differential phase contrast (DPC) microscopy can recover phase image of thin sample under multi-axis intensity measurements in wide-field scheme. Unlike conventional DPC, based on theoretical approach under partially coherent condition, we propose a new method to achieve isotropic differential phase contrast (iDPC) with high accuracy and stability for phase recovery in simple and high-speed fashion. The iDPC is simply implemented with a partially coherent microscopy and a programmable thin-film transistor (TFT) shield to digitally modulate structured illumination patterns for QPI. In this article, simulation results show consistency of our theoretical approach for iDPC under partial coherence. In addition, we further demonstrate experiments of quantitative phase images of a standard micro-lens array, as well as label-free live human cell samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Learning disordered topological phases by statistical recovery of symmetry

NASA Astrophysics Data System (ADS)

Yoshioka, Nobuyuki; Akagi, Yutaka; Katsura, Hosho

2018-05-01

We apply the artificial neural network in a supervised manner to map out the quantum phase diagram of disordered topological superconductors in class DIII. Given the disorder that keeps the discrete symmetries of the ensemble as a whole, translational symmetry which is broken in the quasiparticle distribution individually is recovered statistically by taking an ensemble average. By using this, we classify the phases by the artificial neural network that learned the quasiparticle distribution in the clean limit and show that the result is totally consistent with the calculation by the transfer matrix method or noncommutative geometry approach. If all three phases, namely the Z2, trivial, and thermal metal phases, appear in the clean limit, the machine can classify them with high confidence over the entire phase diagram. If only the former two phases are present, we find that the machine remains confused in a certain region, leading us to conclude the detection of the unknown phase which is eventually identified as the thermal metal phase.

Development of sandwich ELISA for testing bovine β-lactoglobulin allergenic residues by specific polyclonal antibody against human IgE binding epitopes.

PubMed

He, Shengfa; Li, Xin; Gao, Jinyan; Tong, Ping; Chen, Hongbing

2017-07-15

Bovine β-lactoglobulin (BLG) is the main allergen in cows' milk, and the most commonly used method for detecting BLG is enzyme-linked immunosorbent assay (ELISA). However, antibodies used in commercial ELISA kits do not recognize specifically BLG IgE epitopes. Here, an antibody specific to IgE linear epitopes for BLG was used to develop a sandwich ELISA using a rabbit anti-BLG polyclonal antibody. The linear range for BLG detection was 31.25-8000ng/mL and limit of detection was 1.96ng/mL. BLG content in dairy samples was determined, and there was a good agreement between this immunoassay and reversed-phase high-performance liquid chromatography with high recovery. Additionally, BLG content in food samples had an average recovery of 104.25%. Allergenic residues were also detected in hydrolyzed infant formulas. The method developed could be a practical approach to determine BLG and its allergenic residues in food with a high degree of sensitivity, reliability and recovery. Copyright © 2017 Elsevier Ltd. All rights reserved.

Validated LC–MS-MS Method for Multiresidual Analysis of 13 Illicit Phenethylamines in Amniotic Fluid

PubMed Central

Burrai, Lucia; Nieddu, Maria; Carta, Antonio; Trignano, Claudia; Sanna, Raimonda; Boatto, Gianpiero

2016-01-01

A multi-residue analytical method was developed for the determination in amniotic fluid (AF) of 13 illicit phenethylamines, including 12 compounds never investigated in this matrix before. Samples were subject to solid-phase extraction using; hydrophilic–lipophilic balance cartridges which gave good recoveries and low matrix effects on analysis of the extracts. The quantification was performed by liquid chromatography electrospray tandem mass spectrometry. The water–acetonitrile mobile phase containing 0.1% formic acid, used with a C18 reversed phase column, provided adequate separation, resolution and signal-to-noise ratio for the analytes and the internal standard. The final optimized method was validated according to international guidelines. A monitoring campaign to assess fetal exposure to these 13 substances of abuse has been performed on AF test samples obtained from pregnant women. All mothers (n = 194) reported no use of drugs of abuse during pregnancy, and this was confirmed by the analytical data. PMID:26755540

Solid-phase microextraction and chiral HPLC analysis of ibuprofen in urine.

PubMed

de Oliveira, Anderson Rodrigo Moraes; Cesarino, Evandro José; Bonato, Pierina Sueli

2005-04-25

A simple and rapid solid-phase microextraction method was developed for the enantioselective analysis of ibuprofen in urine. The sampling was made with a polydimethylsiloxane-divinylbenzene coated fiber immersed in the liquid sample. After desorptioning from the fiber, ibuprofen enantiomers were analyzed by HPLC using a Chiralpak AD-RH column and UV detection. The mobile phase was made of methanol-pH 3.0 phosphoric acid solution (75:25, v/v), at a flow rate of 0.45 mL/min. The mean recoveries of SPME were 19.8 and 19.1% for (-)-R-ibuprofen and (+)-(S)-ibuprofen, respectively. The method was linear at the range of 0.25-25 microg/mL. Within-day and between-day assay precision and accuracy were below 15% for both ibuprofen enantiomers at concentrations of 0.75, 7.5 and 20 microg/mL. The method was tested with urine quality control samples and human urine fractions after administration of 200 mg rac-ibuprofen.

Determination of some aldehydes by using solid-phase microextraction and high-performance liquid chromatography with UV detection.

PubMed

Kumar, Ashwini; Singh, Baldev; Malik, Ashok Kumar; Tiwary, Dhananjay K

2007-01-01

A new approach has been developed for the extraction and determination of aldehydes such as veratraldehyde, m-nitrobenzaldehyde, cinnamaldehyde, benzaldehyde, and p-chlorobenzaldehyde by using solid-phase microextraction (SPME) and high-performance liquid chromatography with UV detection (HPLC/UV). The method involves adsorption of the aldehydes on polydimethylsiloxane/divinylbenzene-coated fiber, followed by desorption in the desorption chamber of the SPME-HPLC interface, using acetonitrile-water (70 + 30) as the mobile phase; UV detection was at 254 nm. A good separation of 5 aldehydes was obtained on a C18 column. The detection limits of veratraldehyde, m-nitrobenzaldehyde, cinnamaldehyde, benzaldehyde, and p-chlorobenzaldehyde are 25, 41, 13, 12, and 11 pg/mL, respectively, which are about 100 times better than the detection limits for other SPME methods using gas chromatography. The proposed method was validated by determining benzaldehyde in bitter almonds and cinnamaldehyde in cinnamon bark. The recoveries of the 5 analytes were determined by analysis of spiked drinking water.

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.

A method to simulate motor control strategies to recover from perturbations: application to a stumble recovery during gait.

PubMed

Forner-Cordero, Arturo; Ackermann, Marko; de Lima Freitas, Mateus

2011-01-01

Perturbations during human gait such as a trip or a slip can result in a fall, especially among frail populations such as the elderly. In order to recover from a trip or a stumble during gait, humans perform different types of recovery strategies. It is very useful to uncover the mechanisms of the recovery to improve training methods for populations at risk of falling. Moreover, human recovery strategies could be applied to implement controllers for bipedal robot walker, as an application of biomimetic design. A biomechanical model of the response to a trip during gait might uncover the control mechanisms underlying the different recovery strategies and the adaptation of the responses found during the execution of successive perturbation trials. This paper introduces a model of stumble in the multibody system framework. This model is used to assess different feedforward strategies to recover from a trip. First of all, normal gait patterns for the musculoskeletal system model are obtained by solving an optimal control problem. Secondly, the reference gait is perturbed by the application of forces on the swinging foot in different ways: as an instantaneous inelastic collision of the foot with an obstacle, as an impulsive horizontal force or using a force curve measured experimentally during gait perturbation experiments. The influence of the type of perturbation, the timing of the collision with respect to the gait cycle, as well as of the coefficient of restitution was investigated previously. Finally, in order to test the effects of different muscle excitation levels on the initial phases of the recovery response, several muscle excitations were added to selected muscles of the legs, thus providing a simulation of the recovery reactions. These results pave the way for future analysis and modeling of the control mechanisms of gait.

UV-visible spectroscopy as an alternative to liquid chromatography for determination of everolimus in surfactant-containing dissolution media: a useful approach based on solid-phase extraction.

PubMed

Kamberi, Marika; Tran, Thu-Ngoc

2012-11-01

High-throughput 96-well solid phase extraction (SPE) plate with C-18 reversed phase sorbent followed by UV-visible (UV-Vis) microplate reader was applied to the analysis of hydrophobic drugs in surfactant-containing dissolution media, which are often used to evaluate the in-vitro drug release of drug eluting stents (DES). Everolimus and dissolution medium containing Triton X-405 were selected as representatives, and the appropriate SPE conditions (adsorption, washing and elution) were investigated to obtain a practical and reliable sample clean-up. It was shown that the developed SPE procedure was capable of removing interfering components (Triton X-405 and its impurities), allowing for an accurate automated spectrophotometric analysis to be performed. The proposed UV-Vis spectrophotometric method yielded equivalent results compared to a classical LC analysis method. Linear regression analysis indicated that both methods have the ability to obtain test results that are directly proportional to the concentration of analyte in the sample within the selected range of 1.0-10 μg/ml for everolimus, with a coefficient of correlation (r(2)) value of >0.998 and standard deviation of the residuals (Syx) of <2%. The individual recoveries of everolimus ranged from 97 to 104% for the UV-Vis spectrophotometric method and from 98 to 102 for the HPLC method, respectively. The 95% CI of the mean recovery for the UV-Vis spectrophotometric method was 99-102% and for the HPLC method was 99-101%. No statistical difference was found between the mean recoveries of the methods (p=0.42). Hence the methods are free from interference due to Triton and other chemicals present in the dissolution medium. The variation in the amount of everolimus estimated by UV-Vis spectrophotometric and HPLC methods was ≤3.5%, and the drug release profiles obtained by both methods were found to be equivalent by evaluation with two-one-sided t-test (two-tailed, p=0.62; mean of differences, 0.17; 95% CI, 0.62-0.96) and similarity factor f2 (f2 value, 87). The excellent conformity of the results makes UV-Vis spectrophotometer an ideal tool for analyzing the drugs in the media containing surfactants, after SPE. The 96-well SPE plates in combination with UV-Vis microplate reader provide a high throughput method for the determination of in-vitro drug release profile of DES. Switching from HPLC to UV-Vis spectrophotometer microplate reader assay reduces the solvent consumption and labor required for the sample analyses. This directly impacts the profitability of the laboratory. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of Aging Treatment on the Compressibility and Recovery of NiTi Shape Memory Alloys as Static Seals

NASA Astrophysics Data System (ADS)

Lu, Xiaofeng; Li, Gang; Liu, Luwei; Zhu, Xiaolei; Tu, Shan-Tung

2017-07-01

The improvement of the compressibility and recovery of the gaskets can decrease the leakage occurrence in bolted flange connections. In this study, the effect of aging treatment on the compressibility and recovery of NiTi shape memory alloys is investigated as static seals together with thermal analysis. The experimental results indicate that different phase transformations of NiTi alloys are exhibited in the DSC curves during aging treatment. The recovery coefficient of NiTi alloys aged at 500 °C for 2 h is quite low accompanied with a large residual strain. With increasing aging time at the aging temperature of 400 °C, the residual strain and area of hysteresis loop of NiTi alloys are both increased, whereas the recovery coefficient is decreased. Since the deformation associates the phase transformation behavior, aging treatment could improve the compressibility and recovery of NiTi alloys as static seals.

Development of a solid-phase extraction method for determination of pheophorbide a and pyropheophorbide a in health foods by liquid chromatography.

PubMed

Oshima, Harumi; Ueno, Eiji; Saito, Isao; Matsumoto, Hiroshi

2004-01-01

A simple solid-phase extraction (SPE) method was developed for the liquid chromatography (LC) determination of pheophorbide (Phor) a and pyropheophorbide (Pyro) a in health foods such as chlorella, spirulina, etc. The food sample was extracted with 85% (v/v) acetone. The extract was acidified with hydrochloric acid and loaded on a C18 cartridge. After washing with water, Phor a and Pyro a were eluted with the LC mobile phase. Phor a and Pyro a were separated by isocratic reversed-phase LC and quantitated by fluorescence detection. The recoveries for spiked samples of chlorella and the extract were 87.1-102.0%. Commercial health foods (chlorella, spirulina, aloe, kale, Jews mallow, and green tea leaves) were analyzed using the SPE method. The values found for Phor a and Pyro a ranged from 2 to 788 microg/g and from <1 to 24 microg/g, respectively. There was no significant difference between the SPE method and the official method in Japan (spectrophotometry after liquid-liquid extraction). The advantages of the SPE method are the short extraction times, lack of emulsions, and reduced consumption of organic solvents compared with the official method in Japan. The SPE method is considered to be useful for the screening of Phor a and Pyro a in health foods.

Perceptions of Chronicity and Recovery among Youth in Treatment for Substance Use Problems

PubMed Central

Gonzales, Rachel; Anglin, M. Douglas; Beattie, Rebecca; Ong, Chris Angelo; Glik, Deborah C.

2012-01-01

Purpose To explore how youth contextualize substance use problems and recovery, in general and for themselves, in relation to the commonly accepted chronicity framework. Methods Fourteen focus groups were conducted with 118 youth in substance abuse treatment settings (aged 12-24; 78.3% male; 66.1% Latino) located throughout diverse areas of Los Angeles County. Transcribed qualitative focus group data were analyzed for major substance use and recovery themes. Results Most (80%) youth do not accept a chronicity framework that conceptualizes substance use problems as recurring and constituting a life-long illness. Most (65%) view substance use problems as a function of poor behavioral choices or a developmental/social lifestyle phase. Youth perceptions of recovery tend to parallel this view, as most define recovery to mean having an improved or changed lifestyle that is achieved through making better behavioral choices (67%) and exerting personal control over one's behavior (57%) through willpower, confidence, or discipline. Other recovery themes identified by youth were substance use related (47%), wellness or well-being related (43%) and therapeutic or treatment related (14%). Conclusions Findings highlight the importance of considering youth perceptions about substance use chronicity and recovery in making improvements and promoting new developments in clinical and recovery support approaches to better meet the needs of youth with substance use problems. Findings are discussed under a theoretical context of behavior change to provide insights for the treatment and recovery communities. PMID:22824444

Natural history of frozen shoulder: fact or fiction? A systematic review.

PubMed

Wong, C K; Levine, W N; Deo, K; Kesting, R S; Mercer, E A; Schram, G A; Strang, B L

2017-03-01

In 1940s, it was proposed that frozen shoulder progresses through a self-limiting natural history of painful, stiff and recovery phases, leading to full recovery without treatment. However, clinical evidence of persistent limitations lasting for years contradicts this assumption. To assess evidence for the natural history theory of frozen shoulder by examining: (1) progression through recovery phases, and (2) full resolution without treatment. MEDLINE, PubMed, EBSCO CINAHL and PEDro database searches augmented by hand searching. Cohort or randomised controlled trials with no-treatment comparison groups including adults with frozen shoulder who received no treatment and reporting range of motion, pain or function for ≥6 months. Reviewers assessed study eligibility and quality, and extracted data before reaching consensus. Limited early range-of-motion improvements and greater late improvements defined progression through recovery phases. Restoration of normal range of motion and previous function defined full resolution. Of 508 citations, 13 articles were reviewed and seven were included in this review. Low-quality evidence suggested that no treatment yielded some, but not complete, improvement in range of motion after 1 to 4 years of follow-up. No evidence supported the theory of progression through recovery phases to full resolution without treatment. On the contrary, moderate-quality evidence from three randomised controlled trials with longitudinal data demonstrated that most improvement occurred early, not late. Low-quality evidence revealed the weakness of longstanding assumptions about frozen shoulder. Contradictory evidence and a lack of supporting evidence shows that the theory of recovery phases leading to complete resolution without treatment for frozen shoulder is unfounded. Copyright © 2016 Chartered Society of Physiotherapy. Published by Elsevier Ltd. All rights reserved.

Compaction managed mirror bend achromat

DOEpatents

Douglas, David [Yorktown, VA

2005-10-18

A method for controlling the momentum compaction in a beam of charged particles. The method includes a compaction-managed mirror bend achromat (CMMBA) that provides a beamline design that retains the large momentum acceptance of a conventional mirror bend achromat. The CMMBA also provides the ability to tailor the system momentum compaction spectrum as desired for specific applications. The CMMBA enables magnetostatic management of the longitudinal phase space in Energy Recovery Linacs (ERLs) thereby alleviating the need for harmonic linearization of the RF waveform.

Quantitative analysis of phylloquinone (vitamin K1) in soy bean oils by high-performance liquid chromatography.

PubMed

Zonta, F; Stancher, B

1985-07-19

A high-performance liquid chromatographic method for determining phylloquinone (vitamin K1) in soy bean oils is described. Resolution of vitamin K1 from interfering peaks of the matrix was obtained after enzymatic digestion, extraction and liquid-solid chromatography on alumina. An isocratic reversed-phase chromatography with UV detection was used in the final stage. The quantitation was carried out by the standard addition method, and the recovery of the whole procedure was 88.2%.

Separation and Enrichment of Gold in Water, Geological and Environmental Samples by Solid Phase Extraction on Multiwalled Carbon Nanotubes Prior to its Determination by Flame Atomic Absorption Spectrometry.

PubMed

Duran, Ali; Tuzen, Mustafa; Soylak, Mustafa

2015-01-01

This study proposes the application of multi-walled carbon nanotubes as a solid sorbent for the preconcentration of gold prior to its flame atomic absorption spectrometry determination. Extraction was achieved by using a glass column (15.0 cm in length and 1.0 cm in diameter). Quantitative recoveries were obtained in the pH range of 2.5-4.0; the elution step was carried out with 5.0 ml of 1.0 mol/L HNO3 in acetone. In the ligand-free study, variables such as pH, eluent type, sample volume, flow rates, and matrix effect were examined for the optimum recovery of gold ions. The gold ions were able to be pre-concentrated by a factor of 150 and their LOD was determined to be 1.71 μg/L. In order to evaluate the accuracy of the developed method, addition-recovery tests were applied for the tap water, mineral water, and sea water samples. Gold recovery studies were implemented using a wet digestion technique for mine and soil samples taken from various media, and this method was also applied for anodic slime samples taken from the factories located in the Kayseri Industrial Zone of Turkey.

Simultaneous determination of water-soluble vitamins in selected food matrices by liquid chromatography/electrospray ionization tandem mass spectrometry.

PubMed

Gentili, Alessandra; Caretti, Fulvia; D'Ascenzo, Giuseppe; Marchese, Stefano; Perret, Daniela; Di Corcia, Daniele; Rocca, Lucia Mainero

2008-07-01

A rapid, simple and sensitive method based on liquid chromatography/tandem mass spectrometry (LC/MS/MS) with an electrospray ionization (ESI) source for the simultaneous analysis of fourteen water-soluble vitamins (B1, B2, two B3 vitamers, B5, five B6 vitamers, B8, B9, B12 and C) in various food matrices, i.e. maize flour, green and golden kiwi and tomato pulp, is presented here. Analytes were separated by ion-suppression reversed-phase liquid chromatography in less than 10 min and detected in positive ion mode. Sensitivity and specificity of this method allowed two important results to be achieved: (i) limits of detection of the analytes at ng g(-1) levels (except for vitamin C); (ii) development of a rapid sample treatment that minimizes analyte exposition to light, air and heat, eliminating any step of extract concentration. Analyte recovery depended on the type of matrix. In particular, recovery of the analytes in maize flour was > or =70%, with the exception of vitamin C, pyridoxal-5'-phosphate and vitamin B9 (ca 40%); with tomato pulp, recovery was > or =64%, except for vitamin C (41%); with kiwi, recovery was > or =73%, except for nicotinamide (ca. 30%).

A multi-residue method for pesticides analysis in green coffee beans using gas chromatography-negative chemical ionization mass spectrometry in selective ion monitoring mode.

PubMed

Pizzutti, Ionara R; de Kok, Andre; Dickow Cardoso, Carmem; Reichert, Bárbara; de Kroon, Marijke; Wind, Wouter; Weber Righi, Laís; Caiel da Silva, Rosselei

2012-08-17

In this study, a new gas chromatography-mass spectrometry (GC-MS) method, using the very selective negative chemical ionization (NCI) mode, was developed and applied in combination with a modified acetonitrile-based extraction method (QuEChERS) for the analysis of a large number of pesticide residues (51 pesticides, including isomers and degradation products) in green coffee beans. A previously developed integrated sample homogenization and extraction method for both pesticides and mycotoxins analysis was used. An homogeneous slurry of green milled coffee beans and water (ratio 1:4, w/w) was prepared and extracted with acetonitrile/acetic acid (1%), followed by magnesium sulfate addition for phase separation. Aliquots from this extract could be used directly for LC-MS/MS analysis of mycotoxins and LC-amenable pesticides. For GC-MS analysis, a further clean-up was necessary. C18- and PSA-bonded silica were tested as dispersive solid-phase extraction (d-SPE) sorbents, separate and as a mixture, and the best results were obtained using C18-bonded silica. For the optimal sensitivity and selectivity, GC-MS detection in the NCI-selected ion monitoring (SIM) mode had to be used to allow the fast analysis of the difficult coffee bean matrix. The validation was performed by analyzing recovery samples at three different spike concentrations, 10, 20 and 50 μg kg(-1), with 6 replicates (n=6) at each concentration. Linearity (r(2)) of calibration curves, estimated instrument and method limits of detection and limits of quantification (LOD(i), LOD(m), LOQ(i) and LOQ(m), respectively), accuracy (as recovery %), precision (as RSD%) and matrix effects (%) were determined for each individual pesticide. From the 51 analytes (42 parent pesticides, 4 isomers and 5 degradation products) determined by GC-MS (NCI-SIM), approximately 76% showed average recoveries between 70-120% and 75% and RSD ≤ 20% at the lowest spike concentration of 10 μg kg(-1), the target method LOQ. For the spike concentrations of 20 and 50 μg kg(-1), the recoveries and RSDs were even better. The validated LOQ(m) was 10, 20 and 50 μg kg(-1) for respectively 33, 3 and 6 of the analytes studied. For five compounds, the European Union method performance requirements for the validation of a quantitative method (average recoveries between 70-120% and repeatability RSD ≤ 20%) were not achieved and 4 problematic pesticides (captan, captafol, folpet and dicofol) could not be detected as their parent compound, but only via their degradation products. Although the matrix effect (matrix-enhanced detector response) was high for all pesticides studied, the matrix interference was minimal, due to the high selectivity obtained with the GC-NCI-MS detection. Matrix-matched calibration for applying the method in routine analysis is recommended for reliable quantitative results. Copyright © 2012 Elsevier B.V. All rights reserved.

Sarcolemmal mechanisms for pHi recovery from alkalosis in the guinea-pig ventricular myocyte

PubMed Central

Leem, Chae-Hun; Vaughan-Jones, Richard D

1998-01-01

The mechanism of pHi recovery from an intracellular alkali load (induced by acetate prepulse or by reduction/removal of ambient PCO2) was investigated using intracellular SNARF fluorescence in the guinea-pig ventricular myocyte. In Hepes buffer (pHo 7.40), pHi recovery was inhibited by removal of extracellular Cl−, but not by removal of Na+o or elevation of K+o. Recovery was unaffected by the stilbene drug DIDS (4,4-diisothiocyanatostilbene-disulphonic acid), but was slowed dose dependently by the stilbene drug DBDS (dibenzamidostilbene-disulphonic acid). In 5 % CO2/HCO3− buffer (pHo 7.40), pHi recovery was faster than in Hepes buffer. It consisted of an initial rapid recovery phase followed by a slow phase. Much of the rapid phase has been attributed to CO2-dependent buffering. The slow phase was inhibited completely by Cl− removal but not by Na+o removal or K+o elevation. At a test pHi of 7.30 in CO2/HCO3− buffer, the slow phase was inhibited 70 % by DIDS. The mean DIDS-inhibitable acid influx was equivalent in magnitude to the HCO3−-stimulated acid influx. Similarly, the DIDS-insensitive influx was equivalent to that estimated in Hepes buffer. We conclude that two independent sarcolemmal acid-loading carriers are stimulated by a rise of pHi and account for the slow phase of recovery from an alkali load. The results are consistent with activation of a DIDS-sensitive Cl−-HCO3− anion exchanger (AE) to produce HCO3− efflux, and a DIDS-insensitive Cl−-OH− exchanger (CHE) to produce OH− efflux. H+-Cl− co-influx as the alternative configuration for CHE is not, however, excluded. The dual acid-loading system (AE plus CHE), previously shown to be activated by a fall of extracellular pH, is thus activated by a rise of intracellular pH. Activity of the dual-loading system is therefore controlled by pH on both sides of the cardiac sarcolemma. PMID:9575297

Using ecological function to develop recovery criteria for depleted species: Sea otters and kelp forests in the Aleutian archipelago

USGS Publications Warehouse

Estes, James A.; Tinker, M. Tim; Bodkin, James L.

2010-01-01

Recovery criteria for depleted species or populations normally are based on demographic measures, the goal being to maintain enough individuals over a sufficiently large area to assure a socially tolerable risk of future extinction. Such demographically based recovery criteria may be insufficient to restore the functional roles of strongly interacting species. We explored the idea of developing a recovery criterion for sea otters (Enhydra lutris) in the Aleutian archipelago on the basis of their keystone role in kelp forest ecosystems. We surveyed sea otters and rocky reef habitats at 34 island-time combinations. The system nearly always existed in either a kelp-dominated or deforested phase state, which was predictable from sea otter density. We used a resampling analysis of these data to show that the phase state at any particular island can be determined at 95% probability of correct classification with information from as few as six sites. When sea otter population status (and thus the phase state of the kelp forest) was allowed to vary randomly among islands, just 15 islands had to be sampled to estimate the true proportion that were kelp dominated (within 10%) with 90% confidence. We conclude that kelp forest phase state is a more appropriate, sensitive, and cost-effective measure of sea otter recovery than the more traditional demographically based metrics, and we suggest that similar approaches have broad potential utility in establishing recovery criteria for depleted populations of other functionally important species.

Persistent gut motor dysfunction in a murine model of T-cell-induced enteropathy.

PubMed

Mizutani, T; Akiho, H; Khan, W I; Murao, H; Ogino, H; Kanayama, K; Nakamura, K; Takayanagi, R

2010-02-01

Inflammatory bowel disease (IBD) patients in remission often experience irritable bowel syndrome (IBS)-like symptoms. We investigated the mechanism for intestinal muscle hypercontractility seen in T-cell-induced enteropathy in recovery phase. BALB/c mice were treated with an anti-CD3 antibody (100 microg per mouse) and euthanized at varying days post-treatment to investigate the histological changes, longitudinal smooth muscle cell contraction, cytokines (Th1, Th2 cytokines, TNF-alpha) and serotonin (5-HT)-expressing enterochromaffin cell numbers in the small intestine. The role of 5-HT in anti-CD3 antibody-induced intestinal muscle function in recovery phase was assessed by inhibiting 5-HT synthesis using 4-chloro-DL-phenylalanine (PCPA). Small intestinal tissue damage was observed from 24 h after the anti-CD3 antibody injection, but had resolved by day 5. Carbachol-induced smooth muscle cell contractility was significantly increased from 4 h after injection, and this muscle hypercontractility was evident in recovery phase (at day 7). Th2 cytokines (IL-4, IL-13) were significantly increased from 4 h to day 7. 5-HT-expressing cells in the intestine were increased from day 1 to day 7. The 5-HT synthesis inhibitor PCPA decreased the anti-CD3 antibody-induced muscle hypercontractility in recovery phase. Intestinal muscle hypercontractility in remission is maintained at the smooth muscle cell level. Th2 cytokines and 5-HT in the small intestine contribute to the maintenance of the altered muscle function in recovery phase.

A rapid space-resolved solid-phase microextraction method as a powerful tool to determine contaminants in wine based on their volatility.

PubMed

Liu, Min; Peng, Qing-Qing; Chen, Yu-Feng; Tang, Qian; Feng, Qing

2015-06-01

A novel space-resolved solid phase microextraction (SR-SPME) technique was developed to facilitate simultaneously analyte monitoring within heterogeneous samples. Graphene (G) and graphene oxide (GO) were coated separately to the segmented fibers which were successfully used for the solid-phase microextraction of two contaminants with dramatically different volatility: 2,4,6-trichloroanisole (TCA) and dibutyl phthalate (DBP). The space-resolved fiber showed good precision (5.4%, 6.8%), low detection limits (0.3ng/L, 0.3ng/L), and wide linearity (1.0-250.0ng/L, 1.0-250.0ng/L) under the optimized conditions for TCA and DBP, respectively. The method was applied to simultaneous analysis of the two contaminates with satisfactory recoveries, which were 96.96% and 98.20% for wine samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Online solid-phase extraction with high-performance liquid chromatography and mass spectrometry for the determination of five tannins in traditional Chinese medicine injections.

PubMed

Sun, Meng; Lin, Yuanyuan; Zhang, Jie; Zheng, Shaohua; Wang, Sicen

2016-03-01

A rapid analytical method based on online solid-phase extraction with high-performance liquid chromatography and mass spectrometry has been established and applied to the determination of tannin compounds that may cause adverse effects in traditional Chinese medicine injections. Different solid-phase extraction sorbents have been compared and the elution buffer was optimized. The performance of the method was verified by evaluation of recovery (≥40%), repeatability (RSD ≤ 6%), linearity (r(2) ≥ 0.993), and limit of quantification (≤0.35 μg/mL). Five tannin compounds, gallic acid, cianidanol, gallocatechin gallate, ellagic acid, and penta-O-galloylglucose, were identified with concentrations ranging from 3.1-37.4 μg/mL in the analyzed traditional Chinese medicine injections. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simple, sensitive determination of ganciclovir in infant plasma by high-performance liquid chromatography with fluorescence detection.

PubMed

Yoshida, Terumitsu; Takahashi, Ryohei; Imai, Koichi; Uchida, Hiroshi; Arai, Yasutoshi; Oh-ishi, Tsutomu

2010-03-01

This study developed a simple and sensitive method using reversed-phase high-performance liquid chromatography (HPLC) for ganciclovir (GCV) plasma concentrations in cytomegalovirus infectious infants with hearing loss. The method involves a simple protein precipitation procedure that uses no solid-phase or liquid-liquid extraction. The HPLC separation was carried out on a Cadenza CD-C(18) column (3 microm, 4.6 mm x 150 mm) with phosphate buffer (pH 2.5, 25 mM) containing 1% methanol-acetonitrile mixture (4:3, v/v) as a mobile phase at a 0.7 mL/min flow rate. GCV was detected using a fluorescence detection (lambdaex/em: 265/380 nm). The quantification limit was 0.025 microg/mL for 100 microL of plasma sample at which good intra- and inter-assay coefficient of variation values (< 4.96%) and recoveries (94.9-96.5%) were established.

Potential application of aqueous two-phase systems and three-phase partitioning for the recovery of superoxide dismutase from a clarified homogenate of Kluyveromyces marxianus.

PubMed

Simental-Martínez, Jesús; Rito-Palomares, Marco; Benavides, Jorge

2014-01-01

Superoxide dismutase (SOD; EC 1.15.1.1) is an antioxidant enzyme that represents the primary cellular defense against superoxide radicals and has interesting applications in the medical and cosmetic industries. In the present work, the partition behavior of SOD in aqueous two-phase systems (ATPS) (using a standard solution and a complex extract from Kluyveromyces marxianus as sample) was characterized on different types of ATPS (polymer-polymer, polymer-salt, alcohol-salt, and ionic liquid (IL)-salt). The systems composed of PEG 3350-potassium phosphate, 45% TLL, 0.5 M NaCl (315 U/mg, 87% recovery, and 15.1-fold purification) and t-butanol-20% ammonium sulfate (205.8 U/mg, 80% recovery and 9.8-fold purification), coupled with a subsequent 100 kDa ultrafiltration stage, allowed the design of a prototype process for the recovery and partial purification of the product of interest. The findings reported herein demonstrate the potential of PEG-salt ATPS for the potential recovery of SOD. © 2014 American Institute of Chemical Engineers.

Analytical Method Development and Validation for the Simultaneous Estimation of Abacavir and Lamivudine by Reversed-phase High-performance Liquid Chromatography in Bulk and Tablet Dosage Forms.

PubMed

Raees Ahmad, Sufiyan Ahmad; Patil, Lalit; Mohammed Usman, Mohammed Rageeb; Imran, Mohammad; Akhtar, Rashid

2018-01-01

A simple rapid, accurate, precise, and reproducible validated reverse phase high performance liquid chromatography (HPLC) method was developed for the determination of Abacavir (ABAC) and Lamivudine (LAMI) in bulk and tablet dosage forms. The quantification was carried out using Symmetry Premsil C18 (250 mm × 4.6 mm, 5 μm) column run in isocratic way using mobile phase comprising methanol: water (0.05% orthophosphoric acid with pH 3) 83:17 v/v and a detection wavelength of 245 nm and injection volume of 20 μl, with a flow rate of 1 ml/min. In the developed method, the retention times of ABAC and LAMI were found to be 3.5 min and 7.4 min, respectively. The method was validated in terms of linearity, precision, accuracy, limits of detection, limits of quantitation, and robustness in accordance with the International Conference on Harmonization guidelines. The assay of the proposed method was found to be 99% - 101%. The recovery studies were also carried out and mean % recovery was found to be 99% - 101%. The % relative standard deviation from reproducibility was found to be <2%. The proposed method was statistically evaluated and can be applied for routine quality control analysis of ABAC and LAMI in bulk and in tablet dosage form. Attempts were made to develop RP-HPLC method for simultaneous estimation of Abacavir and Lamivudine for the RP-HPLC method. The developed method was validated according to the ICH guidelines. The linearity, precision, range, robustness were within the limits as specified by the ICH guidelines. Hence the method was found to be simple, accurate, precise, economic and reproducible. So the proposed methods can be used for the routine quality control analysis of Abacavir and Lamivudine in bulk drug as well as in formulations. Abbreviations Used: HPLC: High-performance liquid chromatography, UV: Ultraviolet, ICH: International Conference on Harmonization, ABAC: Abacavir, LAMI: Lamivudine, HIV: Human immunodeficiency virus, AIDS: Acquired immunodeficiency syndrome, NRTI: Nucleoside reverse transcriptase inhibitors, ARV: Antiretroviral, RSD: Relative standard deviation, RT: Retention time, SD: Standard deviation.

Simultaneous determination of gaseous and particulate carbonyls in air by coupling micellar electrokinetic capillary chromatography with molecular imprinting solid-phase extraction.

PubMed

Sun, Hui; Lai, Jia-Ping; Fung, Ying Sing

2014-09-05

A novel method coupling molecular imprinting solid-phase extraction (MISPE) and micellar electrokinetic capillary chromatography (MEKC) was developed to enable the hourly determination of low level of ambient carbonyls, and study their partition between gaseous phase and particulate phase. With 2,4-dinitroaniline (DNAN) as dummy imprinting template, the unreacted 2,4-Dinitrophenylhydrazine (DNPH) in sampling solution could be removed effectively using MISPE, and an average recovery of 97±5.3% (n=5) for the carbonyl-DNPH derivatives was achieved. Owing to the high enrichment due to sample clean-up, and the improvement of MEKC separation efficiency, many low abundant carbonyls could be detected by hourly in the field study. Copyright © 2014 Elsevier B.V. All rights reserved.

Characterization of Rare Earth Elements in in Clay Deposits Associated with Central Appalachian Coal Seams

NASA Astrophysics Data System (ADS)

Scott, M.; Verba, C.; Falcon, A.; Poston, J.; McKoy, M.

2017-12-01

Because of their multiple uses in clean energy technologies, rare earth elements (REE) are critical for national economic and energy security. With no current domestic source, supply remains a major concern for domestic security. Underclay - specifically the layer of stratum beneath a coal bed - is a potentially rich source of REE. This study focuses on the characterization and ion exchange recovery of REE from underclay samples from the Lower Freeport, Middle Kittanning, and Pittsburgh coal seams in West Virginia. Multimodal techniques provided quantitative assessments of REE-bearing mineral phases in select underclays and the influence of organic acid rock treatment on the recovery of REE from both exchangeable and crystalline mineral phases present. All samples are from extensively weathered horizons that contain abundant kaolinite and illite. Total REE concentrations range from 250-450 ppm and all samples have a HREE/LEEE ratio >20%. Rare earth element bearing minerals identified in the clay are monazite, xenotime, florencite, and crandallite. Our selective recovery approach is designed to isolate and recover REE through partial dissolution of the clay matrix and ion exchange rather than dissolution/recovery of phosphate or aluminosilicate bound REE. These results provide a better understanding of coal seam underclay, the affinity of REEs for specific ligands and colloids, and how the rock and ligands respond to different chemical treatments. These processes are important to the development and commercialization of efficient and cost effective methods to extract REE from domestic geologic deposits and recover into salable forms.

Three-phase compositional modeling of CO2 injection by higher-order finite element methods with CPA equation of state for aqueous phase

NASA Astrophysics Data System (ADS)

Moortgat, Joachim; Li, Zhidong; Firoozabadi, Abbas

2012-12-01

Most simulators for subsurface flow of water, gas, and oil phases use empirical correlations, such as Henry's law, for the CO2 composition in the aqueous phase, and equations of state (EOS) that do not represent the polar interactions between CO2and water. Widely used simulators are also based on lowest-order finite difference methods and suffer from numerical dispersion and grid sensitivity. They may not capture the viscous and gravitational fingering that can negatively affect hydrocarbon (HC) recovery, or aid carbon sequestration in aquifers. We present a three-phase compositional model based on higher-order finite element methods and incorporate rigorous and efficient three-phase-split computations for either three HC phases or water-oil-gas systems. For HC phases, we use the Peng-Robinson EOS. We allow solubility of CO2in water and adopt a new cubic-plus-association (CPA) EOS, which accounts for cross association between H2O and CO2 molecules, and association between H2O molecules. The CPA-EOS is highly accurate over a broad range of pressures and temperatures. The main novelty of this work is the formulation of a reservoir simulator with new EOS-based unique three-phase-split computations, which satisfy both the equalities of fugacities in all three phases and the global minimum of Gibbs free energy. We provide five examples that demonstrate twice the convergence rate of our method compared with a finite difference approach, and compare with experimental data and other simulators. The examples consider gravitational fingering during CO2sequestration in aquifers, viscous fingering in water-alternating-gas injection, and full compositional modeling of three HC phases.

Determination of artificial sweeteners in water samples by solid-phase extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Ordóñez, Edgar Y; Quintana, José Benito; Rodil, Rosario; Cela, Rafael

2012-09-21

The development and performance evaluation of an analytical method for the determination of six artificial sweeteners in environmental waters using solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry are presented. To this end, different SPE alternatives have been evaluated: polymeric reversed-phase (Oasis HLB, Env+, Plexa and Strata X), and mixed-mode with either weak (Oasis WAX) or strong anionic-exchange (Oasis MAX and Plexa PAX) sorbents. Among them, reversed-phase sorbents, particularly Oasis HLB and Strata X, showed the best performance. Oasis HLB provided good trueness (recoveries: 73-112%), precision (RSD<10%) and limits of quantification (LOQ: 0.01-0.5 μg/L). Moreover, two LC separation mechanisms were evaluated: reversed-phase (RPLC) and hydrophilic interaction (HILIC), with RPLC providing better performance than HILIC. The final application of the method showed the presence of acesulfame, cyclamate, saccharin and sucralose in the wastewater and surface water samples analyzed at concentrations up to 54 μg/L. Copyright © 2012 Elsevier B.V. All rights reserved.

A single chip 2 Gbit/s clock recovery subsystem for digital communications

NASA Astrophysics Data System (ADS)

Hickling, Ronald M.

A self-contained clock recovery/data resynchronizer phase locked loop (PLL) for use in microwave and fiber optic digital communications has been fabricated using GaAs integrated circuit technology. The IC contains the analog and digital components for the PLL: an edge-triggered phase detector based on a 1.2 GHz phase/frequency comparator, an op amp for creating the loop filter, and a VCO based on a differential source-coupled pair amplifier.

Advanced Exploration Systems Water Architecture Study Interim Results

NASA Technical Reports Server (NTRS)

Sargusingh, Miriam J.

2013-01-01

The mission of the Advanced Exploration System (AES) Water Recovery Project (WRP) is to develop advanced water recovery systems that enable NASA human exploration missions beyond low Earth orbit (LEO). The primary objective of the AES WRP is to develop water recovery technologies critical to near-term missions beyond LEO. The secondary objective is to continue to advance mid-readiness-level technologies to support future NASA missions. An effort is being undertaken to establish the architecture for the AES Water Recovery System (WRS) that meets both near- and long-term objectives. The resultant architecture will be used to guide future technical planning, establish a baseline development roadmap for technology infusion, and establish baseline assumptions for integrated ground and on-orbit Environmental Control and Life Support Systems definition. This study is being performed in three phases. Phase I established the scope of the study through definition of the mission requirements and constraints, as well as identifying all possible WRS configurations that meet the mission requirements. Phase II focused on the near-term space exploration objectives by establishing an International Space Station-derived reference schematic for long-duration (>180 day) in-space habitation. Phase III will focus on the long-term space exploration objectives, trading the viable WRS configurations identified in Phase I to identify the ideal exploration WRS. The results of Phases I and II are discussed in this paper.

AES Water Architecture Study Interim Results

NASA Technical Reports Server (NTRS)

Sarguisingh, Miriam J.

2012-01-01

The mission of the Advanced Exploration System (AES) Water Recovery Project (WRP) is to develop advanced water recovery systems in order to enable NASA human exploration missions beyond low earth orbit (LEO). The primary objective of the AES WRP is to develop water recovery technologies critical to near term missions beyond LEO. The secondary objective is to continue to advance mid-readiness level technologies to support future NASA missions. An effort is being undertaken to establish the architecture for the AES Water Recovery System (WRS) that meets both near and long term objectives. The resultant architecture will be used to guide future technical planning, establish a baseline development roadmap for technology infusion, and establish baseline assumptions for integrated ground and on-orbit environmental control and life support systems (ECLSS) definition. This study is being performed in three phases. Phase I of this study established the scope of the study through definition of the mission requirements and constraints, as well as indentifying all possible WRS configurations that meet the mission requirements. Phase II of this study focused on the near term space exploration objectives by establishing an ISS-derived reference schematic for long-duration (>180 day) in-space habitation. Phase III will focus on the long term space exploration objectives, trading the viable WRS configurations identified in Phase I to identify the ideal exploration WRS. The results of Phases I and II are discussed in this paper.

A matrix solid-phase dispersion method for the extraction of seven pesticides from mango and papaya.

PubMed

Navickiene, Sandro; Aquino, Adriano; Bezerra, Débora Santos Silva

2010-10-01

A simple and effective extraction method based on matrix solid-phase dispersion was developed to determine trichlorfon, pyrimethanil, methyl parathion, tetraconazole, thiabendazole, imazalil, and tebuconazole in papaya and mango using gas chromatography-mass spectrometry with selected ion monitoring. Different parameters of the method were evaluated, such as type of solid-phase (silica-gel, neutral alumina, and Florisil), the amount of solid-phase, and eluent [dichloromethane, ethyl acetate-dichloromethane (4:1, 1:4, 1:1, 2:3, v/v)]. The best results were obtained using 2.0 g of mango or papaya, 3.0 g of silica as dispersant sorbent, and ethyl acetate-dichloromethane (1:1, v/v) as eluting solvent. The method was validated using mango and papaya samples fortified with pesticides at different concentration levels (0.05, 0.10, and 1.0 mg/kg). Average recoveries (4 replicates) ranged from 80% to 146%, with relative standard deviations between 1.0% and 28%. Detection and quantification limits for mango and papaya ranged from 0.01 to 0.03 mg/kg and 0.05 to 0.10 mg/kg, respectively. The proposed method was applied to the analysis of these compounds in commercial fruit samples from a local market (Aracaju/SE, Brazil), and residues of the pesticides were not detected on the samples.

Effective Use of Household Water Treatment and Safe Storage in Response to the 2010 Haiti Earthquake

PubMed Central

Lantagne, Daniele; Clasen, Thomas

2013-01-01

When water supplies are compromised during an emergency, responders often recommend household water treatment and safe storage (HWTS) methods, such as boiling or chlorination. We evaluated the near- and longer-term impact of chlorine and filter products distributed shortly after the 2010 earthquake in Haiti. HWTS products were deemed as effective to use if they actually improved unsafe household drinking water to internationally accepted microbiological water quality standards. The acute emergency survey (442 households) was conducted within 8 weeks of emergency onset; the recovery survey (218 households) was conducted 10 months after onset. Effective use varied by HWTS product (from 8% to 63% of recipients in the acute phase and from 0% to 46% of recipients in the recovery phase). Higher rates of effective use were associated with programs that were underway in Haiti before the emergency, had a plan at initial distribution for program continuation, and distributed products with community health worker support and a safe storage container. PMID:23836571

Poly(methyloctylsiloxane) immobilized on silica as a sorbent for solid-phase extraction of some pesticides.

PubMed

Vigna, Camila R M; Morais, Lais S R; Collins, Carol H; Jardim, Isabel C S F

2006-05-12

A laboratory-made sorbent for solid-phase extraction (SPE) was obtained by thermal immobilization of poly(methyloctylsiloxane) (PMOS) onto silica. Cartridges packed with the new sorbent were used for the simultaneous determination of imazethapyr, nicosulfuron, diuron, linuron and chlorimuron-ethyl in water. These pesticides were separated and quantified using high-performance liquid chromatography with diode array detection (HPLC-DAD). The recoveries achieved with the laboratory-made PMOS cartridges were compared with those of some commercially available silica-based and polymer-based cartridges having C18, C8 and NH(2) pendant groups. Method validation using the laboratory-made sorbent was performed for the five pesticides at three fortifications levels (1x, 2x and 10x the limit of quantification of each pesticide). The laboratory-made PMOS cartridge has low cost preparation and showed good recoveries (72-111%) for all pesticides. Repeatability and intermediate precision were lower than 15%. Its performance was similar or even better, in some cases, than those of the commercial cartridges.

Phase and Pupil Amplitude Recovery for JWST Space-Optics Control

NASA Technical Reports Server (NTRS)

Dean, B. H.; Zielinski, T. P.; Smith, J. S.; Bolcar, M. R.; Aronstein, D. L.; Fienup, J. R.

2010-01-01

This slide presentation reviews the phase and pupil amplitude recovery for the James Webb Space Telescope (JWST) Near Infrared Camera (NIRCam). It includes views of the Integrated Science Instrument Module (ISIM), the NIRCam, examples of Phase Retrieval Data, Ghost Irradiance, Pupil Amplitude Estimation, Amplitude Retrieval, Initial Plate Scale Estimation using the Modulation Transfer Function (MTF), Pupil Amplitude Estimation vs lambda, Pupil Amplitude Estimation vs. number of Images, Pupil Amplitude Estimation vs Rotation (clocking), and Typical Phase Retrieval Results Also included is information about the phase retrieval approach, Non-Linear Optimization (NLO) Optimized Diversity Functions, and Least Square Error vs. Starting Pupil Amplitude.

Operation of emergency operating centers during mass casualty incidents in taiwan: a disaster management perspective.

PubMed

Wen, Jet-Chau; Tsai, Chia-Chou; Chen, Mei-Hsuan; Chang, Wei-Ta

2014-10-01

On April 27, 2011, a train derailed and crashed in Taiwan, causing a mass casualty incident (MCI) that was similar to a previous event and with similar consequences. In both disasters, the emergency operating centers (EOCs) could not effectively integrate associated agencies to deal with the incident. The coordination and utilization of resources were inefficient, which caused difficulty in command structure operation and casualty evacuation. This study was designed to create a survey questionnaire with problem items using disaster management phases mandated by Taiwan's Emergency Medical Care Law (EMCL), use statistical methods (t test) to analyze the results and issues the EOCs encountered during the operation, and propose solutions for those problems. Findings showed that EOCs lacked authority to intervene or coordinate with associated agencies. Also, placing emphasis on the recovery phase should improve future prevention and response mechanisms. To improve the response to MCIs, the EMCL needs to be amended to give EOCs the lead during disasters; use feedback from the recovery phase to improve future disaster management and operation coordination; and establish an information-sharing platform across agencies to address all aspects of relief work.(Disaster Med Public Health Preparedness. 2014;0:1-6).

Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples.

PubMed

Ghaedi, M; Ahmadi, F; Soylak, M

2007-08-17

A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni2+, Cu2+ and Co2+ ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 microg L(-1) for copper, 0.75 microg L(-1) for nickel and 0.80 microg L(-1) for cobalt. The loading capacity was 0.56 mg g(-1) for Ni2+, 0.50 mg g(-1) for Cu2+ and 0.47 mg g(-1) for Co2+. The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n=3).

Determination of Triazine Herbicides in Drinking Water by Dispersive Micro Solid Phase Extraction with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometric Detection.

PubMed

Chen, Dawei; Zhang, Yiping; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

2015-11-11

A novel dispersive micro solid phase extraction (DMSPE) method based on a polymer cation exchange material (PCX) was applied to the simultaneous determination of the 30 triazine herbicides in drinking water with ultrahigh-performance liquid chromatography-high-resolution mass spectrometric detection. Drinking water samples were acidified with formic acid, and then triazines were adsorbed by the PCX sorbent. Subsequently, the analytes were eluted with ammonium hydroxide/acetonitrile. The chromatographic separation was performed on an HSS T3 column using water (4 mM ammonium formate and 0.1% formic acid) and acetonitrile (0.1% formic acid) as the mobile phase. The method achieved LODs of 0.2-30.0 ng/L for the 30 triazines, with recoveries in the range of 70.5-112.1%, and the precision of the method was better than 12.7%. These results indicated that the proposed method had the advantages of convenience and high efficiency when applied to the analysis of the 30 triazines in drinking water.

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

PubMed

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

2016-06-01

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

Stability Indicating HPLC Method for the Determination of Chiral Purity of R-(-)-5-[2-aminopropyl]-2-methoxybenzene Sulfonamide.

PubMed

Kasawar, G B; Farooqui, M N

2009-09-01

A chiral reverse phase liquid chromatographic method was developed for the enantiomeric resolution of racemic mixture of (-)-5-[2-aminopropyl]-2-methoxybenzene sulfonamide in bulk drug. The enantiomeric separation of sulfonamide was resolved on a Crownpak CR (+) column using perchloric acid buffer of pH 1.0 as mobile phase and with UV detection at 226 nm. The method is validated and proved to be robust. The limit of detection and quantification of S (-)-(5)-[2-aminopropyl]-2-methoxybenzene sulfonamide] was found to be 0.084 and 0.159 mug/ml, respectively for 20 mul injection volume. The percentage recovery of S (-)-(5)-[2-aminopropyl]-2-methoxybenzene sulfonamide] ranged from 99.57 to 101.88 in bulk drug samples of R (-)-(5)-[2- aminopropyl]-2-methoxybenzene sulfonamide].

Stability Indicating HPLC Method for the Determination of Chiral Purity of R-(-)-5-[2-aminopropyl]-2-methoxybenzene Sulfonamide

PubMed Central

Kasawar, G. B.; Farooqui, M. N.

2009-01-01

A chiral reverse phase liquid chromatographic method was developed for the enantiomeric resolution of racemic mixture of (-)-5-[2-aminopropyl]-2-methoxybenzene sulfonamide in bulk drug. The enantiomeric separation of sulfonamide was resolved on a Crownpak CR (+) column using perchloric acid buffer of pH 1.0 as mobile phase and with UV detection at 226 nm. The method is validated and proved to be robust. The limit of detection and quantification of S (-)-(5)-[2-aminopropyl]-2-methoxybenzene sulfonamide] was found to be 0.084 and 0.159 μg/ml, respectively for 20 μl injection volume. The percentage recovery of S (-)-(5)-[2-aminopropyl]-2-methoxybenzene sulfonamide] ranged from 99.57 to 101.88 in bulk drug samples of R (-)-(5)-[2- aminopropyl]-2-methoxybenzene sulfonamide]. PMID:20502572

Quantitative analysis of matrine in liquid crystalline nanoparticles by HPLC.

PubMed

Peng, Xinsheng; Li, Baohong; Hu, Min; Ling, Yahao; Tian, Yuan; Zhou, Yanxing; Zhou, Yanfang

2014-01-01

A reversed-phase high-performance liquid chromatographic method has been developed to quantitatively determine matrine in liquid crystal nanoparticles. The chromatographic method is carried out using an isocratic system. The mobile phase was composed of methanol-PBS(pH6.8)-triethylamine (50 : 50 : 0.1%) with a flow rate of 1 mL/min with SPD-20A UV/vis detector and the detection wavelength was at 220 nm. The linearity of matrine is in the range of 1.6 to 200.0  μ g/mL. The regression equation is y = 10706x - 2959 (R (2) = 1.0). The average recovery is 101.7%; RSD = 2.22%  (n = 9). This method provides a simple and accurate strategy to determine matrine in liquid crystalline nanoparticle.

Determination of Low Concentrations of Acetochlor in Water by Automated Solid-Phase Extraction and Gas Chromatography with Mass-Selective Detection

USGS Publications Warehouse

Lindley, C.E.; Stewart, J.T.; Sandstrom, M.W.

1996-01-01

A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 ??g/L. Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 ??g/L. Average single-operator precision, over the course of 1 week, was better than 5%.

Electron density increases due to Lightning activity as deduced from LWPC code and VLF signal perturbations.

NASA Astrophysics Data System (ADS)

Samir, Nait Amor; Bouderba, Yasmina

VLF signal perturbations in association with thunderstorm activity appear as changes in the signal amplitude and phase. Several papers reported on the characteristics of thus perturbations and their connection to the lightning strokes amplitude and polarity. In this contribution, we quantified the electrons density increases due to lightning activity by the use of the LWPC code and VLF signal perturbations parameters. The method is similar to what people did in studying the solar eruptions effect. the results showed that the reference height (h') decreased to lower altitudes (between 70 and 80 km). From the LWPC code results the maximum of the electron density was then deduced. Therefore, a numerical simulation of the atmospheric species times dependences was performed to study the recovery times of the electrons density at different heights. The results showed that the recovery time last for several minutes and explain the observation of long recovery Early signal perturbations.

Factors influencing recovery and restoration following a chemical incident.

PubMed

Peña-Fernández, A; Wyke, S; Brooke, N; Duarte-Davidson, R

2014-11-01

Chemicals are an important part of our society. A wide range of chemicals are discharged into the environment every day from residential, commercial and industrial sources. Many of these discharges do not pose a threat to public health or the environment. However, global events have shown that chemical incidents or accidents can have severe consequences on human health, the environment and society. It is important that appropriate tools and technical guidance are available to ensure that a robust and efficient approach to developing a remediation strategy is adopted. The purpose of remediation is to protect human health from future exposure and to return the affected area back to normal as soon as possible. There are a range of recovery options (techniques or methods for remediation) that are applicable to a broad range of chemicals and incidents. Recovery options should be evaluated according to their appropriateness and efficacy for removing contaminants from the environment; however economic drivers and social and political considerations often influence decision makers on which remedial actions are implemented during the recovery phase of a chemical incident. To date, there is limited information in the literature on remediation strategies and recovery options that have been implemented following a chemical incident, or how successful they have been. Additional factors that can affect the approach taken for recovery are not well assessed or understood by decision makers involved in the remediation and restoration of the environment following a chemical incident. The identification of this gap has led to the development of the UK Recovery Handbook for Chemical Incidents to provide a framework for choosing an effective recovery strategy. A compendium of practical evidence-based recovery options (techniques or methods for remediation) for inhabited areas, food production systems and water environments has also been developed and is included in the chemical handbook. This paper presents the key factors that should be considered when developing a recovery strategy with respect to how these may impact on its effectiveness. The paper also highlights the importance of these factors through an evaluation of recovery strategies implemented following real chemical incidents that have been reported in the literature. Copyright © 2014 Elsevier Ltd. All rights reserved.

An improved adaptive interpolation clock recovery loop based on phase splitting algorithm for coherent optical communication system

NASA Astrophysics Data System (ADS)

Liu, Xuan; Liu, Bo; Zhang, Li-jia; Xin, Xiang-jun; Zhang, Qi; Wang, Yong-jun; Tian, Qing-hua; Tian, Feng; Mao, Ya-ya

2018-01-01

Traditional clock recovery scheme achieves timing adjustment by digital interpolation, thus recovering the sampling sequence. Based on this, an improved clock recovery architecture joint channel equalization for coherent optical communication system is presented in this paper. The loop is different from the traditional clock recovery. In order to reduce the interpolation error caused by the distortion in the frequency domain of the interpolator and to suppress the spectral mirroring generated by the sampling rate change, the proposed algorithm joint equalization, improves the original interpolator in the loop, along with adaptive filtering, and makes error compensation for the original signals according to the balanced pre-filtering signals. Then the signals are adaptive interpolated through the feedback loop. Furthermore, the phase splitting timing recovery algorithm is adopted in this paper. The time error is calculated according to the improved algorithm when there is no transition between the adjacent symbols, making calculated timing error more accurate. Meanwhile, Carrier coarse synchronization module is placed before the beginning of timing recovery to eliminate the larger frequency offset interference, which effectively adjust the sampling clock phase. In this paper, the simulation results show that the timing error is greatly reduced after the loop is changed. Based on the phase splitting algorithm, the BER and MSE are better than those in the unvaried architecture. In the fiber channel, using MQAM modulation format, after 100 km-transmission of single-mode fiber, especially when ROF(roll-off factor) values tends to 0, the algorithm shows a better clock performance under different ROFs. When SNR values are less than 8, the BER could achieve 10-2 to 10-1 magnitude. Furthermore, the proposed timing recovery is more suitable for the situation with low SNR values.

Apollo experience report: Postflight testing of command modules

NASA Technical Reports Server (NTRS)

Hamilton, D. T.

1973-01-01

Various phases of the postflight testing of the command modules used in the Apollo Program are presented. The specific tasks to be accomplished by the task force recovery teams, the National Aeronautics and Space Administration Lyndon B. Johnson Space Center, (formerly the Manned Spacecraft Center) and the cognizant contractors/subcontractors are outlined. The means and methods used in postflight testing and how such activities evolved during the Apollo Program and were tailored to meet specific test requirements are described. Action taken to resolve or minimize problems or anomalies discovered during the flight, the postflight test phase, or mission evaluation is discussed.

SEPARATION OF THORIUM FROM URANIUM BY EXTRACTION

DOEpatents

Bohlmann, E.G.

1959-07-28

A method is presented for the recovery and separation of uranium and thorium values contained in an aqueous nitric acid solution which is more than 3 M in nitric acid. The uranium and thorium containing solution preferable about 7 M in nitric acid is contacted with tributyl phosphatekerosene mixture. Both U and Th are extracted by the immiscible organic. After phase separation the Th is selectively back extracted by contacting with an aqueous nitric acid solution preferably between 0.1 to 1.5 M in nitric acid. The uranium which is still in the organic extractant phase may be recovered by contacting with water.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

PubMed

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

High-speed clock recovery with phase-locked-loop-based on LiNbO3 modulators

NASA Astrophysics Data System (ADS)

Zhu, Guanghao; Chen, Hongmin; Wang, Qiang; Dutta, Niloy K.

2003-08-01

In this paper, we present a scheme for recovering 10 GHz clock from 40 Gb/s and 80 Gb/s time division multiplexed (TDM) return to zero (RZ) data stream. The proposed clock recovery is successfully demonstrated using an electrical phase locked loop (PLL). The jitter of the recovered clock is estimated to be around 50 fs. The key part in the proposed clock recovery circuit is a LiNbO3 Mach-Zehnder modulator which is shown to be highly effective in optical to electrical down conversion.

Sparsity-based multi-height phase recovery in holographic microscopy

NASA Astrophysics Data System (ADS)

Rivenson, Yair; Wu, Yichen; Wang, Hongda; Zhang, Yibo; Feizi, Alborz; Ozcan, Aydogan

2016-11-01

High-resolution imaging of densely connected samples such as pathology slides using digital in-line holographic microscopy requires the acquisition of several holograms, e.g., at >6-8 different sample-to-sensor distances, to achieve robust phase recovery and coherent imaging of specimen. Reducing the number of these holographic measurements would normally result in reconstruction artifacts and loss of image quality, which would be detrimental especially for biomedical and diagnostics-related applications. Inspired by the fact that most natural images are sparse in some domain, here we introduce a sparsity-based phase reconstruction technique implemented in wavelet domain to achieve at least 2-fold reduction in the number of holographic measurements for coherent imaging of densely connected samples with minimal impact on the reconstructed image quality, quantified using a structural similarity index. We demonstrated the success of this approach by imaging Papanicolaou smears and breast cancer tissue slides over a large field-of-view of ~20 mm2 using 2 in-line holograms that are acquired at different sample-to-sensor distances and processed using sparsity-based multi-height phase recovery. This new phase recovery approach that makes use of sparsity can also be extended to other coherent imaging schemes, involving e.g., multiple illumination angles or wavelengths to increase the throughput and speed of coherent imaging.

Biscalix[4]arene derivative as a very efficient phase selective gelator for oil spill recovery.

PubMed

Tsai, Chia-Chen; Cheng, Ying-Tsai; Shen, Li-Ching; Chang, Kai-Chi; Ho, I-Ting; Chu, Jean-Ho; Chung, Wen-Sheng

2013-11-15

A biscalixarene framework, without long alkyl chains, has been readily synthesized in three steps starting from the parent calix[4]arene. The biscalix[4]arene 1 was able to form organogels in various alcoholic solvents; furthermore, it exhibited an excellent phase selective gelation property that is potentially useful in oil spill recovery.

Characterization of adsorption on the stationary phase using high-performance immunoaffinity chromatography.

PubMed

Nielsen, R G; Wilson, G S

1987-12-25

Low-level adsorption on the stationary phase has been studied using immunochemical reagents. An immunoaffinity column has been evaluated using affinity-purified radioisotope-labeled monoclonal antibodies. Recovery experiments including continuous immunosorbent monitoring have been performed. Proper characterization of an immunoaffinity separation can result in the recovery of immunologically active material in high yield.

Determination of benzodiazepines in beverages using green extraction methods and capillary HPLC-UV detection.

PubMed

Piergiovanni, Maurizio; Cappiello, Achille; Famiglini, Giorgio; Termopoli, Veronica; Palma, Pierangela

2018-05-30

Dispersive liquid-liquid microextraction with and without ultrasound assistance (DLLME, UA-DLLME) and microextraction with packed sorbent (MEPS) methods for the extraction and determination of eight different benzodiazepines (BDZ) (chlordiazepoxide, flurazepam, bromazepam, oxazepam, lorazepam, clobazam, clonazepam, and flunitrazepam) in three commercial non-alcoholic and light alcoholic beverages were optimized and compared. Benzodiazepines are frequently used for their extensive diffusion and strong numbing effect in drug-facilitated crimes (DFC). The tiny small amount of sample required for DLLME and MEPS extraction makes them very suitable for specimens collected at the crime scene of DFCs. Microextraction techniques are of increasing interest thanks to their accordance to green analytical chemistry (GAC) guidelines providing good recovery values. Ultrasound assistance (UA-DLLME) was used to investigate whether this type of energy can improve the recoveries of the analytes. Analyses of the extracts were performed with reverse-phase capillary high-performance liquid chromatography with UV detection (HPLC - UV), thanks to low environmental impact, robustness, diffusion, and affordability. Recovery percentages at three different concentrations in the three beverages were between 14.30% and 103.28% with intraday and interday RSD lower than ±2.78%. The same samples were extracted using a MEPS protocol, and the results were compared with those obtained with DLLME. MEPS gave recoveries between 20.90% and 101.88% for all matrices showing a better performance than DLLME at higher concentrations, though lower recoveries were observed with diluted samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous quantification of acetanilide herbicides and their oxanilic and sulfonic acid metabolites in natural waters.

PubMed

Heberle, S A; Aga, D S; Hany, R; Müller, S R

2000-02-15

This paper describes a procedure for simultaneous enrichment, separation, and quantification of acetanilide herbicides and their major ionic oxanilic acid (OXA) and ethanesulfonic acid (ESA) metabolites in groundwater and surface water using Carbopack B as a solid-phase extraction (SPE) material. The analytes adsorbed on Carbopack B were eluted selectively from the solid phase in three fractions containing the parent compounds (PCs), their OXA metabolites, and their ESA metabolites, respectively. The complete separation of the three compound classes allowed the analysis of the neutral PCs (acetochlor, alachlor, and metolachlor) and their methylated OXA metabolites by gas chromatography/mass spectrometry. The ESA compounds were analyzed by high-performance liquid chromatography with UV detection. The use of Carbopack B resulted in good recoveries of the polar metabolites even from large sample volumes (1 L). Absolute recoveries from spiked surface and groundwater samples ranged between 76 and 100% for the PCs, between 41 and 91% for the OXAs, and between 47 and 96% for the ESAs. The maximum standard deviation of the absolute recoveries was 12%. The method detection limits are between 1 and 8 ng/L for the PCs, between 1 and 7 ng/L for the OXAs, and between 10 and 90 ng/L for the ESAs.

Validated reversed phase LC method for quantitative analysis of polymethoxyflavones in citrus peel extracts.

PubMed

Wang, Zhenyu; Li, Shiming; Ferguson, Stephen; Goodnow, Robert; Ho, Chi-Tang

2008-01-01

Polymethoxyflavones (PMFs), which exist exclusively in the citrus genus, have biological activities including anti-inflammatory, anticarcinogenic, and antiatherogenic properties. A validated RPLC method was developed for quantitative analysis of six major PMFs, namely nobiletin, tangeretin, sinensetin, 5,6,7,4'-tetramethoxyflavone, 3,5,6,7,3',4'-hexamethoxyflavone, and 3,5,6,7,8,3',4'-heptamethoxyflavone. The polar embedded LC stationary phase was able to fully resolve the six analogues. The developed method was fully validated in terms of linearity, accuracy, precision, sensitivity, and system suitability. The LOD of the method was calculated as 0.15 microg/mL and the recovery rate was between 97.0 and 105.1%. This analytical method was successfully applied to quantify the individual PMFs in four commercially available citrus peel extracts (CPEs). Each extract shows significant difference in the PMF composition and concentration. This method may provide a simple, rapid, and reliable tool to help reveal the correlation between the bioactivity of the PMF extracts and the individual PMF content.

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

PubMed

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

2016-11-01

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

Semi-permeable surface analytical reversed-phase column for the improved trace analysis of acidic pesticides in water with coupled-column reversed-phase liquid chromatography with UV detection. Determination of bromoxynil and bentazone in surface water.

PubMed

Hogendoorn, E A; Westhuis, K; Dijkman, E; Heusinkveld, H A; den Boer, A C; Evers, E A; Baumann, R A

1999-10-08

The coupled-column (LC-LC) configuration consisting of a 3 microm C18 column (50 x 4.6 mm I.D.) as the first column and a 5 microm C18 semi-permeable-surface (SPS) column (150 x 4.6 mm I.D.) as the second column appeared to be successful for the screening of acidic pesticides in surface water samples. In comparison to LC-LC employing two C18 columns, the combination of C18/SPS-C18 significantly decreased the baseline deviation caused by the hump of the co-extracted humic substances when using UV detection (217 nm). The developed LC-LC procedure allowed the simultaneous determination of the target analytes bentazone and bromoxynil in uncleaned extracts of surface water samples to a level of 0.05 microg/l in less than 15 min. In combination with a simple solid-phase extraction step (200 ml of water on a 500 mg C18-bonded silica) the analytical procedure provides a high sample throughput. During a period of about five months more than 200 ditch-water samples originating from agricultural locations were analyzed with the developed procedure. Validation of the method was performed by randomly analyzing recoveries of water samples spiked at levels of 0.1 microg/l (n=10), 0.5 microg/l (n=7) and 2.5 microg/l (n=4). Weighted regression of the recovery data showed that the method provides overall recoveries of 95 and 100% for bentazone and bromoxynil, respectively, with corresponding intra-laboratory reproducibilities of 10 and 11%, respectively. Confirmation of the analytes in part of the samples extracts was carried out with GC-negative ion chemical ionization MS involving a derivatization step with bis(trifluoromethyl)benzyl bromide. No false negatives or positives were observed.

Critical periods after stroke study: translating animal stroke recovery experiments into a clinical trial

PubMed Central

Dromerick, Alexander W.; Edwardson, Matthew A.; Edwards, Dorothy F.; Giannetti, Margot L.; Barth, Jessica; Brady, Kathaleen P.; Chan, Evan; Tan, Ming T.; Tamboli, Irfan; Chia, Ruth; Orquiza, Michael; Padilla, Robert M.; Cheema, Amrita K.; Mapstone, Mark E.; Fiandaca, Massimo S.; Federoff, Howard J.; Newport, Elissa L.

2015-01-01

Introduction: Seven hundred ninety-five thousand Americans will have a stroke this year, and half will have a chronic hemiparesis. Substantial animal literature suggests that the mammalian brain has much potential to recover from acute injury using mechanisms of neuroplasticity, and that these mechanisms can be accessed using training paradigms and neurotransmitter manipulation. However, most of these findings have not been tested or confirmed in the rehabilitation setting, in large part because of the challenges in translating a conceptually straightforward laboratory experiment into a meaningful and rigorous clinical trial in humans. Through presentation of methods for a Phase II trial, we discuss these issues and describe our approach. Methods: In rodents there is compelling evidence for timing effects in rehabilitation; motor training delivered at certain times after stroke may be more effective than the same training delivered earlier or later, suggesting that there is a critical or sensitive period for strongest rehabilitation training effects. If analogous critical/sensitive periods can be identified after human stroke, then existing clinical resources can be better utilized to promote recovery. The Critical Periods after Stroke Study (CPASS) is a phase II randomized, controlled trial designed to explore whether such a sensitive period exists. We will randomize 64 persons to receive an additional 20 h of upper extremity therapy either immediately upon rehab admission, 2–3 months after stroke onset, 6 months after onset, or to an observation-only control group. The primary outcome measure will be the Action Research Arm Test (ARAT) at 1 year. Blood will be drawn at up to 3 time points for later biomarker studies. Conclusion: CPASS is an example of the translation of rodent motor recovery experiments into the clinical setting; data obtained from this single site randomized controlled trial will be used to finalize the design of a Phase III trial. PMID:25972803

RCRA Facility investigation report for Waste Area Grouping 6 at Oak Ridge National Laboratory, Oak Ridge, Tennessee. Volume 5, Technical Memorandums 06-09A, 06-10A, and 06-12A

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

None

This report provides a detailed summary of the activities carried out to sample groundwater at Waste Area Grouping (WAG) 6. The analytical results for samples collected during Phase 1, Activity 2 of the WAG 6 Resource Conservation and Recovery Act Facility Investigation (RFI) are also presented. In addition, analytical results for Phase 1, activity sampling events for which data were not previously reported are included in this TM. A summary of the groundwater sampling activities of WAG 6, to date, are given in the Introduction. The Methodology section describes the sampling procedures and analytical parameters. Six attachments are included. Attachmentsmore » 1 and 2 provide analytical results for selected RFI groundwater samples and ORNL sampling event. Attachment 3 provides a summary of the contaminants detected in each well sampled for all sampling events conducted at WAG 6. Bechtel National Inc. (BNI)/IT Corporation Contract Laboratory (IT) RFI analytical methods and detection limits are given in Attachment 4. Attachment 5 provides the Oak Ridge National Laboratory (ORNL)/Analytical Chemistry Division (ACD) analytical methods and detection limits and Resource Conservation and Recovery Act (RCRA) quarterly compliance monitoring (1988--1989). Attachment 6 provides ORNL/ACD groundwater analytical methods and detection limits (for the 1990 RCRA semi-annual compliance monitoring).« less

Determination of parabens and endocrine-disrupting alkylphenols in soil by gas chromatography-mass spectrometry following matrix solid-phase dispersion or in-column microwave-assisted extraction: a comparative study.

PubMed

Pérez, R A; Albero, B; Miguel, E; Sánchez-Brunete, C

2012-03-01

Two rapid methods were evaluated for the simultaneous extraction of seven parabens and two alkylphenols from soil based on matrix solid-phase dispersion (MSPD) and microwave-assisted extraction (MAE). Soil extracts were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide and analyzed by gas chromatography with mass spectrometry. Extraction and clean-up of samples were carried out by both methods in a single step. A glass sample holder, inside the microwave cell, was used in MAE to allow the simultaneous extraction and clean-up of samples and shorten the MAE procedure. The detection limits achieved by MSPD were lower than those obtained by MAE because the presence of matrix interferences increased with this extraction method. The extraction yields obtained by MSPD and MAE for three different types of soils were compared. Both procedures showed good recoveries and sensitivity for the determination of parabens and alkylphenols in two of the soils assayed, however, only MSPD yielded good recoveries with the other soil. Finally, MSPD was applied to the analysis of soils collected in different sites of Spain. In most of the samples analyzed, methylparaben and butylparaben were detected at levels ranging from 1.21 to 8.04 ng g(-1) dry weight and 0.48 to 1.02 ng g(-1) dry weight, respectively.

Sample Enrichment for Bioanalytical Assessment of Disinfected Drinking Water: Concentrating the Polar, the Volatiles, and the Unknowns.

PubMed

Stalter, Daniel; Peters, Leon I; O'Malley, Elissa; Tang, Janet Yat-Man; Revalor, Marion; Farré, Maria José; Watson, Kalinda; von Gunten, Urs; Escher, Beate I

2016-06-21

Enrichment methods used in sample preparation for the bioanalytical assessment of disinfected drinking water result in the loss of volatile and hydrophilic disinfection byproducts (DBPs) and hence likely tend to underestimate biological effects. We developed and evaluated methods that are compatible with bioassays, for extracting nonvolatile and volatile DBPs from chlorinated and chloraminated drinking water to minimize the loss of analytes. For nonvolatile DBPs, solid-phase extraction (SPE) with TELOS ENV as solid phase performed superior compared to ten other sorbents. SPE yielded >70% recovery of nonpurgeable adsorbable organic halogens (AOX). For volatile DBPs, cryogenic vacuum distillation performed unsatisfactorily. Purge and cold-trap with crushed ice serving as condensation nuclei achieved recoveries of 50-100% for trihalomethanes and haloacetonitriles and approximately 60-90% for purged AOX from tap water. We compared the purgeable versus the nonpurgeable fraction by combining purge-and-trap extraction with SPE. The purgeable DBP fraction enriched with the purge-and-trap method exerted a lower oxidative stress response in mammalian cells than the nonpurgeable DBPs enriched with SPE after purging, while contributions of both fractions to bacterial cytotoxicity was more variable. 37 quantified DBPs explained almost the entire AOX in the purge-and-trap extracts, but <16% in the SPE extracts demonstrating that the nonpurgeable fraction is dominated by unknown DBPs.

[Determination of perfluoroalkyl acids in lamb liver by high performance liquid chromatography- tandem mass spectrometry combined with dispersive solid phase extraction].

PubMed

Zhu, Pingping; Yue, Zhenfeng; Zheng, Zongkun; Zhang, Yi; Li, Wenyin; Zhao, Fengjuan; Xiao Chengui; Bai, Runye; Lin, Wei

2015-05-01

A method was developed for the determination of 19 perfluoroalkyl acids (PFAs) in lamb liver by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS) combined with dispersive solid phase extraction. The sample was extracted with acidified acetonitrile, and then cleaned-up by a mixture of N-propylethylenediamine (PSA), C18 and graphitized carbon black (GCB) sorbents. The 19 PFAs were analyzed by HPLC-MS/MS with a C18 chromatographic column, adopting the multiple reaction monitoring (MRM) mode with negative electrospray ionization. The effects of the dosages of hydrochloric acid and the sorbents on the recoveries of the 19 PFAs were studied. For accurate quantitative analysis, the isotope internal standard method was used. The calibration curves were linear with the correlation coefficients over 0.998 in the range of 0.05-20 µg/kg for the 19 PFAs. The limits of detection were 0.004-0.111 µg/kg. The limits of quantification were 0.012-0.370 µg/kg. The mean recoveries of the 19 PFAs at spiked levels of 0.5, 1.0, 2.0 µg/kg were in the range from 80% to 128% with the relative standard deviations of 0.31%-11.1%. The developed method is rapid, simple, accurate. It is suitable for the determination of the 19 PFAs in large quantities of lamb liver samples.

Influence of cell density and phase variants of bacterial symbionts (Xenorhabdus spp.) on dauer juvenile recovery and development of biocontrol nematodes Steinernema carpocapsae and S. feltiae (Nematoda: Rhabditida).

PubMed

Hirao, A; Ehlers, R-U

2009-08-01

The rhabditid nematodes Steinernema carpocapsae and Steinernema feltiae are used in biological control of insect pests. Mass production is done in liquid culture media pre-incubated with their bacterial symbionts Xenorhabdus nematophila and Xenorhabdus bovienii, respectively, before nematode dauer juveniles (DJs) are inoculated. As a response to food signals produced by the bacterial symbionts, the DJs exit from the developmentally arrested dauer stage (they recover development) and grow to adults, which produce DJ offspring. Variable DJ recovery after inoculation often causes process failure due to non-synchronous population development and low numbers of adult nematodes. This contribution investigated the influence of the bacterial cell density on DJ recovery and development to adults. At higher density of 10(10) bacterial cells ml(-1), a higher percentage of DJ recovery was induced, and adults occurred earlier in both Steinernema spp. than at lower density of 10(9) and 10(8) cells ml(-1). Xenorhabdus symbionts produce phase variants. Recovery in bacteria-free supernatants was lower than in supernatants containing bacterial cells for both primary and secondary phase Xenorhabdus spp. and lower in secondary than in primary phase supernatants or cell suspensions. In general, recovery was lower for Steinernema feltiae and the time at which 50% of the population had recovered after exposure to the food signal was longer (RT(50) = 17.1 h) than for Steinernema carpocapsae (RT(50) = 6.6 h). Whereas >90% S. carpocapsae DJs recovered in hemolymph serum of the lepidopteran insect Galleria mellonella, recovery of S. feltiae only reached 31%. Penetration into a host insect prior to exposure to the insect's food signal did not enhance DJ recovery. Consequences for liquid culture mass production of the nematodes and differences between species of the genera Steinernema and Heterorhabditis are discussed.

Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil.

PubMed

Drzymala, Sarah S; Weiz, Stefan; Heinze, Julia; Marten, Silvia; Prinz, Carsten; Zimathies, Annett; Garbe, Leif-Alexander; Koch, Matthias

2015-05-01

Established maximum levels for the mycotoxin zearalenone (ZEN) in edible oil require monitoring by reliable analytical methods. Therefore, an automated SPE-HPLC online system based on dynamic covalent hydrazine chemistry has been developed. The SPE step comprises a reversible hydrazone formation by ZEN and a hydrazine moiety covalently attached to a solid phase. Seven hydrazine materials with different properties regarding the resin backbone, pore size, particle size, specific surface area, and loading have been evaluated. As a result, a hydrazine-functionalized silica gel was chosen. The final automated online method was validated and applied to the analysis of three maize germ oil samples including a provisionally certified reference material. Important performance criteria for the recovery (70-120 %) and precision (RSDr <25 %) as set by the Commission Regulation EC 401/2006 were fulfilled: The mean recovery was 78 % and RSDr did not exceed 8 %. The results of the SPE-HPLC online method were further compared to results obtained by liquid-liquid extraction with stable isotope dilution analysis LC-MS/MS and found to be in good agreement. The developed SPE-HPLC online system with fluorescence detection allows a reliable, accurate, and sensitive quantification (limit of quantification, 30 μg/kg) of ZEN in edible oils while significantly reducing the workload. To our knowledge, this is the first report on an automated SPE-HPLC method based on a covalent SPE approach.

validated microbiological and HPLC methods for the determination of moxifloxacin in pharmaceutical preparations and human plasma.

PubMed

Abdelaziz, Ahmed A; Elbanna, Tarek E; Gamaleldeen, Noha M

2012-10-01

The article presents a comparison between microbiological and high performance liquid chromatographic (HPLC) assays for quantification of moxifloxacin in tablets, ophthalmic solutions and human plasma. The microbiological method employed a cylinder-plate agar diffusion assay using a strain of Esherichia coli ATCC 25922 as the test organism and phosphate buffer (pH8) as the diluent. The calibration curves were linear (R(2) > 0.98) over a concentration range of 0.125 to 16 µgml(-1). The within day and between days precisions were ≤ 4.47% and ≤ 6.39% respectively. Recovery values were between 89.4 and 110.2%. The HPLC assay used Hypersil(®) BDS C18 reversed phase column (250×4.6 mm, 5µm) with a mobile phase comprising 20 mM ammonium dihydrogen orthophosphate (pH3) and acetonitrile (75:25) and flowing at 1.5 ml/min. The detection was at 295nm. The calibration curves were linear (R(2) > 0.999) over the range of 0.125 to 16 µg ml(-1). The within day and between days precisions were ≤ 4.07% and ≤ 5.09% respectively. Recovery values were between 97.7 and 107.6%. Similar potencies were obtained after the analysis of moxifloxacin tablets and ophthalmic solutions by both methods. Also pharmacokinetic parameters were calculated after the analysis of plasma samples of six male healthhy volunteers by both validated methods.

Simultaneous determination of methocarbamol and aspirin by RP-HPLC using fluorescence detection with time programming: its application to pharmaceutical dosage form.

PubMed

El-Din, M Sharaf; Eid, M; Zeid, A M

2013-01-01

A new simple, rapid and sensitive reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of methocarbamol (MET) and aspirin (ASP) in their combined dosage form. The separation of these compounds was achieved within 6.0 min on a CLC Shim-pack C8 column (250 × 4.6 mm, 5 µm particle size) using isocratic mobile phase consisting of acetonitrile and 0.02 M dihydrogenphosphate buffer (30:70, v/v) at pH = 5.0. The analysis was performed at a flow rate of 1.0 mL/min with fluorescence detection at 277/313 nm for MET and 298/410 nm for ASP using real-time programming. The selectivity, linearity of calibration, accuracy, inter- and intra-day precision and recovery were examined as parts of the method validation. The concentration-response relationship was linear over concentration ranges of 0.02-0.20 and 0.02-0.40 µg/mL for MET and ASP, respectively, with a limit of detection of 6 and 32 ng/mL for MET and ASP, respectively. The proposed method was successfully applied for the analysis of both MET and ASP in prepared tablets with average recoveries of 99.88 ± 0.65% for MET and 100.44 ± 0.78% for ASP. The results were favourably compared to those obtained by a reference method. Copyright © 2012 John Wiley & Sons, Ltd.

One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion.

PubMed

Tu, Xijuan; Ma, Shuangqin; Gao, Zhaosheng; Wang, Jing; Huang, Shaokang; Chen, Wenbin

2017-11-01

Flavonoids are frequently found as glycosylated derivatives in plant materials. To determine contents of flavonoid aglycones in these matrices, procedures for the extraction and hydrolysis of flavonoid glycosides are required. The current sample preparation method is both labour and time consuming. Develop a modified matrix solid phase dispersion (MSPD) procedure as an alternative methodology for the one-step extraction and hydrolysis of flavonoid glycosides. HPLC-DAD was applied for demonstrating the one-step extraction and hydrolysis of flavonoids in rape bee pollen. The obtained contents of flavonoid aglycones (quercetin, kaempferol, isorhamnetin) were used for the optimisation and validation of the method. The extraction and hydrolysis were accomplished in one step. The procedure completes in 2 h with silica gel as dispersant, a 1:2 ratio of sample to dispersant, and 60% aqueous ethanol with 0.3 M hydrochloric acid as the extraction solution. The relative standard deviations (RSDs) of repeatability were less than 5%, and the recoveries at two fortified levels were between 88.3 and 104.8%. The proposed methodology is simple and highly efficient, with good repeatability and recovery. Compared with currently available methods, the present work has advantages of using less time and labour, higher extraction efficiency, and less consumption of the acid catalyst. This method may have applications for the one-step extraction and hydrolysis of bioactive compounds from plant materials. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Liquid chromatographic-diode-array detection multiresidue determination of rice herbicides in drinking and paddy-field water.

PubMed

Roehrs, Rafael; Zanella, Renato; Pizzuti, Ionara; Adaime, Martha B; Pareja, Lucía; Niell, Silvina; Cesio, María V; Heinzen, Horacio

2009-01-01

A sensitive, rapid, and simple multiresidue method for the simultaneous determination of six postemergence herbicides currently used in rice cultivation--metsulfuron methyl, bensulfuron methyl, pyrazosulfuron ethyl, bentazone, bispyribac sodium, and cyhalofop butyl--in drinking and paddy-field water is presented. Water samples were extracted with solid-phase extraction cartridges. Final determination was made by LC with diode-array detection. The extraction efficiencies of C18 and HLB cartridges were compared. The average recovery obtained for these compounds for the lowest spiked level (0.1 microg/L) varied from 70 to 122% for C18 and 75-119% for HLB, with RSDs of 11 and 8.3%, respectively. The method had good linearity, and the lower detection limit for the pesticides studied varied from 0.03 to 0.04 microg/L. The proposed method was also tested in paddy-field water, with recovery studies giving good results with low RSDs at 1.0 microg/L.

[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.

Capillary electrophoresis for analyzing pesticides in fruits and vegetables using solid-phase extraction and stir-bar sorptive extraction.

PubMed

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

2005-05-06

Two procedures based on solid-phase extraction (SPE) and stir-bar sorptive extraction (SBSE) in combination with micellar electrokinetic chromatography (MEKC)--diode array detection (DAD) were compared for the simultaneous extraction of acrinathrin, bitertanol, cyproconazole, fludioxonil, flutriafol, myclobutanil, pyriproxyfen, and tebuconazole in lettuce, tomato, grape, and strawberry. Selectivity and resolution of the MEKC procedure were studied changing the pH and the molarity of the buffer, the type and the concentration of surfactant, and the methanol content in the mobile phase. A buffer consisting of 6 mM sodium tetraborate decahydrate with 75 mM of cholic acid sodium solution (pH 9.2) gave the best results. Linearity, extraction efficiencies and limits of quantitation (LOQs) of both extraction methods were compared. The recoveries obtained by SPE ranged from 40 to 106% with relative standard deviations (R.S.D.s) from 10 to 19% whereas by the SBSE method, the recoveries were 12-47% and the R.S.D.s 3-17%. The LOQs were much better by SPE (0.2-0.5 mg kg(-1) depending on the processed sample amount) than those obtained by SBSE (1 mg kg(-1) for each compound). Advantages and disadvantages of both procedures are also discussed. As SPE is more robust, rapid, and sensitive than SBSE, its application in combination with MEKC is recommended because provided LOQs below the MRLs established, which is not always attained by SBSE.

Determination of the clean-up efficiency of the solid-phase extraction of rosemary extracts: Application of full-factorial design in hyphenation with Gaussian peak fit function.

PubMed

Meischl, Florian; Kirchler, Christian Günter; Jäger, Michael Andreas; Huck, Christian Wolfgang; Rainer, Matthias

2018-02-01

We present a novel method for the quantitative determination of the clean-up efficiency to provide a calculated parameter for peak purity through iterative fitting in conjunction with design of experiments. Rosemary extracts were used and analyzed before and after solid-phase extraction using a self-fabricated mixed-mode sorbent based on poly(N-vinylimidazole/ethylene glycol dimethacrylate). Optimization was performed by variation of washing steps using a full three-level factorial design and response surface methodology. Separation efficiency of rosmarinic acid from interfering compounds was calculated using an iterative fit of Gaussian-like signals and quantifications were performed by the separate integration of the two interfering peak areas. Results and recoveries were analyzed using Design-Expert® software and revealed significant differences between the washing steps. Optimized parameters were considered and used for all further experiments. Furthermore, the solid-phase extraction procedure was tested and compared with commercial available sorbents. In contrast to generic protocols of the manufacturers, the optimized procedure showed excellent recoveries and clean-up rates for the polymer with ion exchange properties. Finally, rosemary extracts from different manufacturing areas and application types were studied to verify the developed method for its applicability. The cleaned-up extracts were analyzed by liquid chromatography with tandem mass spectrometry for detailed compound evaluation to exclude any interference from coeluting molecules. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

National validation study of a swab protocol for the recovery of Bacillus anthracis spores from surfaces.

PubMed

Hodges, Lisa R; Rose, Laura J; O'Connell, Heather; Arduino, Matthew J

2010-05-01

Twelve Laboratory Response Network (LRN) affiliated laboratories participated in a validation study of a macrofoam swab protocol for the recovery, detection, and quantification of viable B. anthracis (BA) Sterne spores from steel surfaces. CDC personnel inoculated steel coupons (26cm(2)) with 1-4 log(10) BA spores and recovered them by sampling with pre-moistened macrofoam swabs. Phase 1 (P1) of the study evaluated swabs containing BA only, while dust and background organisms were added to swabs in Phase 2 (P2) to mimic environmental conditions. Laboratories processed swabs and enumerated spores by culturing eluted swab suspensions and counting colonies with morphology consistent with BA. Processed swabs were placed in enrichment broth, incubated 24h, and cultured by streaking for isolation. Real-time PCR was performed on selected colonies from P2 samples to confirm the identity of BA. Mean percent recovery (%R) of spores from the surface ranged from 15.8 to 31.0% (P1) and from 27.9 to 55.0% (P2). The highest mean percent recovery was 31.0% (sd 10.9%) for P1 (4 log(10) inoculum) and 55.0% (sd 27.6%) for P2 (1 log(10) inoculum). The overall %R was higher for P2 (44.6%) than P1 (24.1%), but the overall reproducibility (between-lab variability) was lower in P2 than in P1 (25.0 vs 16.5%CV, respectively). The overall precision (within-lab variability) was close to identical for P1 and P2 (44.0 and 44.1, respectively), but varied greatly between inoculum levels. The protocol demonstrated linearity in %R over the three inoculum levels and is able to detect between 26 and 5x10(6)spores/26cm(2). Sensitivity as determined by culture was >98.3% for both phases and all inocula, suggesting that the culture method maintains sensitivity in the presence of contaminants. The enrichment broth method alone was less sensitive for sampled swabs (66.4%) during P2, suggesting that the presence of background organisms inhibited growth or isolation of BA from the broth. The addition of real-time PCR testing to the assay increased specificity from >85.4% to >95.0% in P2. Although the precision was low at the 1 log(10) inoculum level in both phases (59.0 and 50.2%), this swab processing protocol, was sensitive, specific, precise, and reproducible at 2-4 log(10)/26cm(2) spore concentrations. Published by Elsevier B.V.

Polycyclic aromatic hydrocarbons (PAHs) in yogurt samples.

PubMed

Battisti, Chiara; Girelli, Anna Maria; Tarola, Anna Maria

2015-01-01

The concentrations and distributions of major polycyclic aromatic hydrocarbons (PAHs) were determined in 20 kinds of yogurt specimens collected from Italian supermarkets using reversed phase high-performance liquid chromatography equipped with fluorescence detection. The method was validated by determination of recovery percentages, precision (repeatability) and sensitivity (limits of detection) with yogurt samples fortified at 0.25, 0.5 and 1 µg/kg concentration levels. The recovery of 13 PAHs, with the exception of naphthalene and acenaphthene, ranged from 61% to 130% and from 60% to 97% at all the levels for yogurts with low (0.1%) and high (3.9%) fat content, respectively. The method is repeatable with relative standard deviation values <20% for all analytes. The results obtained demonstrate that acenaphthene, fluorantene, phenanthrene, anthracene, fluoranthene and pyrene were found in all samples with a similar distribution, but different content when yogurts with low and high fats were compared.

Highly efficient catalytic systems based on Pd-coated microbeads

NASA Astrophysics Data System (ADS)

Lim, Jin Hyun; Cho, Ahyoung; Lee, Seung Hwan; Park, Bumkyo; Kang, Dong Woo; Koo, Chong Min; Yu, Taekyung; Park, Bum Jun

2018-01-01

The efficiency of two prototype catalysis systems using palladium (Pd)-coated microparticles was investigated with regard to the recovery and recyclability of the catalytic particles. One such system was the interface-adsorption method, in which polymer particles coated with Pd nanoparticles strongly and irreversibly attach to the oil-water interface. Due to the irreversible adsorption of the catalytic particles to the interface, particle loss was completely prevented while mixing the aqueous solution and while collecting the products. The other system was based on the magnetic field-associated particle recovery method. The use of polymeric microparticles containing Pd nanoparticles and magnetite nanoparticles accelerated the sedimentation of the particles in the aqueous phase by applying a strong magnetic field, consequently suppressing drainage of the particles from the reactor along the product stream. Upon multiple runs of the catalytic reactions, it was found that conversion does not change significantly, demonstrating the excellent recyclability and performance efficiency in the catalytic processes.

Effect of Caffeine on near Maximal Blood Pressure and Blood Pressure Recovery in Physically-Active, College-Aged Females

PubMed Central

CONNAHAN, LAURA E.; OTT, CHRISTOPHER A.; BARRY, VAUGHN W.

2017-01-01

The purpose of this study is to determine how caffeine affects exercise blood pressure (BP) and active and passive recovery BP after vigorous intensity exercise in physically active college-aged females. Fifteen physically active, ACSM stratified low-risk females (age (y): 23.53 ± 4.07, weight (kg): 60.34 ± 3.67, height (cm): 165.14 ± 7.20, BMI (kg/m2): 22.18 ± 1.55) participated in two Bruce protocol exercise tests. Before each test participants consumed 1) a placebo or 2) 3.3 mg·kg−1 of caffeine at least one hour before exercise in a counterbalanced double-blinded fashion. After reaching 85% of their age-predicted maximum heart rate, BP was taken and participants began an active (i.e. walking) recovery phase for 6 minutes followed by a passive (i.e. sitting) recovery phase. BP was assessed every two minutes in each phase. Recovery times were assessed until active and passive BP equaled 20 mmHg and 10 mmHg above resting, respectively. Participants completed each test 1–2 weeks a part. Maximal systolic and diastolic blood pressures were not significantly different between the two trials. Active recovery, passive recovery, and total recovery times were all significantly longer during the caffeine trial than the placebo trial. Furthermore, the time to reach age-predicted maximum heart rate was significantly shorter in the placebo trial than the caffeine trial. While caffeine consumption did not significantly affect maximal blood pressure, it did affect active and passive recovery time following vigorous intensity exercise in physically active females. Exercise endurance also improved after consuming caffeine in this population. PMID:28344739

Effect of Caffeine on near Maximal Blood Pressure and Blood Pressure Recovery in Physically-Active, College-Aged Females.

PubMed

Connahan, Laura E; Ott, Christopher A; Barry, Vaughn W

2017-01-01

The purpose of this study is to determine how caffeine affects exercise blood pressure (BP) and active and passive recovery BP after vigorous intensity exercise in physically active college-aged females. Fifteen physically active, ACSM stratified low-risk females (age (y): 23.53 ± 4.07, weight (kg): 60.34 ± 3.67, height (cm): 165.14 ± 7.20, BMI (kg/m 2 ): 22.18 ± 1.55) participated in two Bruce protocol exercise tests. Before each test participants consumed 1) a placebo or 2) 3.3 mg·kg -1 of caffeine at least one hour before exercise in a counterbalanced double-blinded fashion. After reaching 85% of their age-predicted maximum heart rate, BP was taken and participants began an active (i.e. walking) recovery phase for 6 minutes followed by a passive (i.e. sitting) recovery phase. BP was assessed every two minutes in each phase. Recovery times were assessed until active and passive BP equaled 20 mmHg and 10 mmHg above resting, respectively. Participants completed each test 1-2 weeks a part. Maximal systolic and diastolic blood pressures were not significantly different between the two trials. Active recovery, passive recovery, and total recovery times were all significantly longer during the caffeine trial than the placebo trial. Furthermore, the time to reach age-predicted maximum heart rate was significantly shorter in the placebo trial than the caffeine trial. While caffeine consumption did not significantly affect maximal blood pressure, it did affect active and passive recovery time following vigorous intensity exercise in physically active females. Exercise endurance also improved after consuming caffeine in this population.