Investigation into Generation of Micro Features by Localised Electrochemical Deposition

NASA Astrophysics Data System (ADS)

Debnath, Subhrajit; Laskar, Hanimur Rahaman; Bhattacharyya, B.

2017-11-01

With the fast advancement of technology, localised electrochemical deposition (LECD) is becoming very advantageous in generating high aspect ratio micro features to meet the steep demand in modern precision industries of the present world. Except many other advantages, this technology is highly uncomplicated and economical for fabricating metal micro-parts with in micron ranges. In the present study, copper micro-columns have been fabricated utilizing LECD process. Different process parameters such as voltage, frequency, duty ratio and electrolyte concentration, which affect the deposition performance have been identified and their effects on deposition performances such as deposition rate, height and diameter of the micro-columns have been experimentally investigated. Taguchi's methodology has been used to study the effects as well as to obtain the optimum values of process parameters so that localised deposition with best performance can be achieved. Moreover, the generated micro-columns were carefully observed under optical and scanning electron microscope from where the surface quality of the deposited micro-columns has been studied qualitatively. Also, an array of copper micro-columns has been fabricated on stainless steel (SS-304) substrate for further exploration of LECD process capability.

Fabrication and characterization of microelectromechanical systems-based gas chromatography column with embedded micro-posts for separation of environmental carcinogens.

PubMed

Sun, Jianhai; Cui, Dafu; Chen, Xing; Zhang, Lulu; Cai, Haoyuan; Li, Hui

2013-05-24

In this paper, a micro gas chromatography (μGC) column with embedded micro-posts was developed for increasing overall surface area of the columns which is able to support more of the stationary phase and reducing the effective width of the column, leading to higher separation efficiency. The proposed columns have a higher sample capacity as the overall surface area is about 3 times larger than that of open columns with the same dimensions. In order to achieve an even flow velocity in the channels, the location of the micro-posts in the linear channels and the configuration of curved channels were optimized by numerical simulation. The results have indicated that the proposed column separated 5 environmental carcinogens in less than 50s, achieved a separation efficiency of about 9500plates/m and eluted highly symmetrical Gaussian peaks. Copyright © 2013 Elsevier B.V. All rights reserved.

Pushing quantitation limits in micro UHPLC-MS/MS analysis of steroid hormones by sample dilution using high volume injection.

PubMed

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tímea; Mészáros, Katalin Viola; Szabó, Pál Tamás

2016-09-10

Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LoQ). Micro UHPLC coupling with sensitive tandem mass spectrometry provides state of the art solutions for such analytical problems. Decreased column volume in micro LC limits the injectable sample volume. However, if analyte concentration is extremely low, it might be necessary to inject high sample volumes. This is particularly critical for strong sample solvents and weakly retained analytes, which are often the case when preparing biological samples (protein precipitation, sample extraction, etc.). In that case, high injection volumes may cause band broadening, peak distortion or even elution in dead volume. In this study, we evaluated possibilities of high volume injection onto microbore RP-LC columns, when sample solvent is diluted. The presented micro RP-LC-MS/MS method was optimized for the analysis of steroid hormones from human plasma after protein precipitation with organic solvents. A proper sample dilution procedure helps to increase the injection volume without compromising peak shapes. Finally, due to increased injection volume, the limit of quantitation can be decreased by a factor of 2-5, depending on the analytes and the experimental conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

PubMed

Washington, John W; Henderson, W Matthew; Ellington, J Jackson; Jenkins, Thomas M; Evans, John J

2008-02-15

With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorooctanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary phases, two different liquid chromatography-tandem mass spectrometry (LC/MS/MS) systems, and eight combinations of sample-extract pretreatments, extractions and cleanups on three test soils. For the columns and systems we tested, we achieved the greatest analytical sensitivity for PFCAs using a column with a C(18) stationary phase in a Waters LC/MS/MS. In this system we achieved an instrument detection limit for PFOA of 270 ag/microL, equating to about 14 fg of PFOA on-column. While an elementary acetonitrile/water extraction of soils recovers PFCAs effectively, natural soil organic matter also dissolved in the extracts commonly imparts significant noise that appears as broad, multi-nodal, asymmetric peaks that coelute with several PFCAs. The intensity and elution profile of this noise is highly variable among soils and it challenges detection of low concentrations of PFCAs by decreasing the signal-to-noise contrast. In an effort to decrease this background noise, we investigated several methods of pretreatment, extraction and cleanup, in a variety of combinations, that used alkaline and unbuffered water, acetonitrile, tetrabutylammonium hydrogen sulfate, methyl-tert-butyl ether, dispersed activated carbon and solid-phase extraction. For the combined objectives of complete recovery and minimization of background noise, we have chosen: (1) alkaline pretreatment; (2) extraction with acetonitrile/water; (3) evaporation to dryness; (4) reconstitution with tetrabutylammonium-hydrogen-sulfate ion-pairing solution; (5) ion-pair extraction to methyl-tert-butyl ether; (6) evaporation to dryness; (7) reconstitution with 60/40 acetonitrile/water (v/v); and (8) analysis by LC/MS/MS. Using this method, we detected in all three of our test soils, endogenous concentrations of all of our PFCA analytes, C(6) through C(10)-the lowest concentrations being roughly 30 pg/g of dry soil for perfluorinated hexanoic and decanoic acids in an agricultural soil.

Cu2+-imprinted cross-linked chitosan resin as micro-column packing materials for online chemiluminescence determination of trace copper.

PubMed

Nie, Feng; Hao, Liang; Gao, Mei; Wu, Yingchun; Li, Xinsheng; Yu, Sha

2011-01-01

The Cu(2+)-imprinted cross-linked chitosan resin was synthesized and the binding characteristic of the resin to Cu(2+) was evaluated. The prepared resin was packed into a micro-glass column and used as micro-separating column. The micro-separating column was connected into the chemiluminescence flow system and placed in front of the window of the photomultiplier tube. Based on the luminol-hydrogen peroxide chemiluminescence system, a flow injection online chemiluminescence method for determination of trace copper was developed and trace Cu(2+) in complex samples was successfully determined. The proposed method improved the shortcomings of chemiluminescence method's poor selectivity. Copyright © 2010 John Wiley & Sons, Ltd.

Micro-apparatus for rapid determinations of protein solubilities

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Munson, Sibyl

1991-01-01

We have developed a column-based micro-technique for rapid determinations of protein solubilities. While retaining a large crystal surface area, the column dead volume has been reduced to equal to or less than 5 micro liters. The technique was tested with tetragonal lysozyme (pH 4.5, 0.1 M acetate, 3.0 percent NaCl, 5-25 C) and column volumes of about 60, 300, and 900 micro liters. Identical solubility data were obtained, indicating that equilibration was obtained even in the smallest columns. In addition, solubility data for Br- and I- salts of lysozyme (pH 4.5, 0.1 M acetate buffer, 0.5 M salt concentrations) were obtained. It appears that the technique can be further miniaturized. The limit in further reducing the crystalline column volume is determined by the minimum solution sample size needed to determine the protein concentration.

Determination of phosphonoformate (foscarnet) in calf and human serum by automated solid-phase extraction and high-performance liquid chromatography with amperometric detection.

PubMed

Ba, B B; Corniot, A G; Ducint, D; Breilh, D; Grellet, J; Saux, M C

1999-03-05

An isocratic high-performance liquid chromatographic method with automated solid-phase extraction has been developed to determine foscarnet in calf and human serums. Extraction was performed with an anion exchanger, SAX, from which the analyte was eluted with a 50 mM potassium pyrophosphate buffer, pH 8.4. The mobile phase consisted of methanol-40 mM disodium hydrogenphosphate, pH 7.6 containing 0.25 mM tetrahexylammonium hydrogensulphate (25:75, v/v). The analyte was separated on a polyether ether ketone (PEEK) column 150x4.6 mm I.D. packed with Kromasil 100 C18, 5 microm. Amperometric detection allowed a quantification limit of 15 microM. The assay was linear from 15 to 240 microM. The recovery of foscarnet from calf serum ranged from 60.65+/-1.89% for 15 microM to 67.45+/-1.24% for 200 microM. The coefficient of variation was < or = 3.73% for intra-assay precision and < or =7.24% for inter-assay precision for calf serum concentrations ranged from 15 to 800 microM. For the same samples, the deviation from the nominal value ranged from -8.97% to +5.40% for same day accuracy and from -4.50% to +2.77% for day-to-day accuracy. Selectivity was satisfactory towards potential co-medications. Replacement of human serum by calf serum for calibration standards and quality control samples was validated. Automation brought more protection against biohazards and increase in productivity for routine monitoring and pharmacokinetic studies.

Blood cell mRNAs and microRNAs: optimized protocols for extraction and preservation.

PubMed

Eikmans, Michael; Rekers, Niels V; Anholts, Jacqueline D H; Heidt, Sebastiaan; Claas, Frans H J

2013-03-14

Assessing messenger RNA (mRNA) and microRNA levels in peripheral blood cells may complement conventional parameters in clinical practice. Working with small, precious samples requires optimal RNA yields and minimal RNA degradation. Several procedures for RNA extraction and complementary DNA (cDNA) synthesis were compared for their efficiency. The effect on RNA quality of freeze-thawing peripheral blood cells and storage in preserving reagents was investigated. In terms of RNA yield and convenience, quality quantitative polymerase chain reaction signals per nanogram of total RNA and using NucleoSpin and mirVana columns is preferable. The SuperScript III protocol results in the highest cDNA yields. During conventional procedures of storing peripheral blood cells at -180°C and thawing them thereafter, RNA integrity is maintained. TRIzol preserves RNA in cells stored at -20°C. Detection of mRNA levels significantly decreases in degraded RNA samples, whereas microRNA molecules remain relatively stable. When standardized to reference targets, mRNA transcripts and microRNAs can be reliably quantified in moderately degraded (quality index 4-7) and severely degraded (quality index <4) RNA samples, respectively. We describe a strategy for obtaining high-quality and quantity RNA from fresh and stored cells from blood. The results serve as a guideline for sensitive mRNA and microRNA expression assessment in clinical material.

Recent advances in micro-scale and nano-scale high-performance liquid-phase chromatography for proteome research.

PubMed

Tao, Dingyin; Zhang, Lihua; Shan, Yichu; Liang, Zhen; Zhang, Yukui

2011-01-01

High-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS-MS) is regarded as one of the most powerful techniques for separation and identification of proteins. Recently, much effort has been made to improve the separation capacity, detection sensitivity, and analysis throughput of micro- and nano-HPLC, by increasing column length, reducing column internal diameter, and using integrated techniques. Development of HPLC columns has also been rapid, as a result of the use of submicrometer packing materials and monolithic columns. All these innovations result in clearly improved performance of micro- and nano-HPLC for proteome research.

Sensitive and simultaneous determination of HIV protease inhibitors in rat biological samples by liquid chromatography-mass spectrometry.

PubMed

Gao, Weihua; Kishida, Tomoyuki; Kimura, Keisuke; Kageyama, Michiharu; Sumi, Masaki; Yoshikawa, Yukako; Shibata, Nobuhito; Takada, Kanji

2002-06-01

A sensitive and simultaneous liquid chromatographic-mass spectrometric (LC/MS) method for the determination of current four HIV protease inhibitors (PIs), indinavir (IDV), saquinavir (SQV), nelfinavir (NFV) and amprenavir (APV) in rat plasma and liver dialysate by a microdialysis method was described. An isocratic LC/MS method in combination with atmospheric pressure chemical ionization was developed for the determination of these four PIs in biological samples in the same run. The analytes including an internal standard were extracted from 100 microL of plasma or 150 microL of liver dialysate samples by salting-out with 100 microL of ice-cold 2 M K(3)PO(4) followed by ether extraction. The separation of analytes was carried out on a reversed-phase semi-micro column using 50% of acetonitrile containing 1% acetic acid as mobile phase at a flow rate of 0.2mL/min(-1). The separation was completed within 5 min. Precision, recovery and limits of detection indicated that the method was suitable for the quantitative determination of these PIs in rat plasma or liver dialysate. This simple, sensitive and highly specific LC/MS method is suitable for pharmacokinetic studies and therapeutic drug monitoring in AIDS patients who receive double protease therapy. Copyright 2002 John Wiley & Sons, Ltd.

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

PubMed

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

2011-11-01

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

Enantioseparation of racemic aminoglutethimide using asynchronous simulated moving bed chromatography.

PubMed

Lin, Xiaojian; Gong, Rujin; Li, Jiaxu; Li, Ping; Yu, Jianguo; Rodrigues, Alirio E

2016-10-07

The separation of aminoglutethimide enantiomers by the continuous multicolumn chromatographic processes were investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenyl-carbamate stationary phase (brand name Chiralcel OD) and mobile phase was a mixture of n-hexane and ethanol with monoethanolamine additive. The continuous enantioseparation processes included a synchronous shifting process (SMB) and an asynchronous shifting process (VARICOL), which allowed reducing the column number (here from six-column SMB to five-column VARICOL process). Transport-dispersive model with the consideration of both intraparticle mass transfer resistance and axial dispersion was adopted to design and optimize the operation conditions for the separation of aminoglutethimide enantiomers by SMB process and VARICOL process. According to the optimized operation conditions, experiments were carried out on VARICOL-Micro unit using five-column VARICOL process with 1/1.5/1.5/1 configuration and six-column SMB process with 1/2/2/1 configuration. Products of R-aminoglutethimide (R-AG) enantiomer and S-aminoglutethimide (S-AG) enantiomer with more than 99.0% purity were obtained continuously from extract stream and raffinate stream, respectively. Furthermore, the experiemntal data obtained from five-column VARICOL process were compared with that from six-column SMB process, the feasibility and efficiency for the separation of guaifenesin enantiomers by VARICOL processes were evaluated. Copyright © 2016 Elsevier B.V. All rights reserved.

Determining multifumigants in whole grains and legumes, milled and low-fat grain products, spices, citrus fruit, and beverages.

PubMed

Daft, J

1987-01-01

Whole grain and legumes, milled and low-fat products, spices, citrus fruit, and dry beverage ingredients are leached with purified, acidified acetone-water solutions. Portions of these leachates are then back-extracted with purified isooctane. Liquid beverages are directly extracted with the isooctane. Six to 10 microL of each isooctane extract is then screened for 11 fumigant residues by gas chromatography (GC) using electron-capture and Hall electroconductivity detectors, and dual 20% OV-101 columns. Further confirmation of residue identity is done on 20% OV-225/20% OV-17 (2.5 + 1 mixed-bed) and 10% SP-1000 columns. The analytes determined include methyl bromide, methylene chloride, carbon disulfide, chloroform, ethylene dichloride, methyl chloroform, carbon tetrachloride, trichloroethylene, chloropicrin, ethylene dibromide, and tetrachloroethylene, using mixed-component reference solutions. Average recoveries from fortified grain range from 25 to 85%; methyl bromide and chloropicrin were recovered the least. Recoveries from the other kinds of food samples range from 43 to 111%. Advantages of this procedure are (1) clean sample extracts, (2) ppb detection limits, (3) residue stability, (4) relative speed, quality control, and safety of the analysis, and (5) results which gave an accurate picture of residual fumigants in grain and food products.

Extraction of toxic compounds from saliva by magnetic-stirring-assisted micro-solid-phase extraction step followed by headspace-gas chromatography-ion mobility spectrometry.

PubMed

Criado-García, Laura; Arce, Lourdes

2016-09-01

A new sample extraction procedure based on micro-solid-phase extraction (μSPE) using a mixture of sorbents of different polarities (polymeric reversed-phase sorbent HLB, silica-based sorbent C18, and multiwalled carbon nanotubes) was applied to extract benzene, toluene, butyraldehyde, benzaldehyde, and tolualdehyde present in saliva to avoid interference from moisture and matrix components and enhance sensitivity and selectivity of the ion mobility spectrometry (IMS) methodology proposed. The extraction of target analytes from saliva samples by using μSPE were followed by the desorption step carried out in the headspace vials placed in the autosampler of the IMS device. Then, 200 μL of headspace was injected into the GC column coupled to the IMS for its analysis. The method was fully validated in terms of sensitivity, precision, and recovery. The LODs and LOQs obtained, when analytes were dissolved in saliva samples to consider the matrix effect, were within the range of 0.38-0.49 and 1.26-1.66 μg mL(-1), respectively. The relative standard deviations were <3.5 % for retention time and drift time values, which indicate that the method proposed can be applied to determine toxic compounds in saliva samples. Graphical abstract Summary of steps followed in the experimental set up of this work.

Citridones, new potentiators of antifungal miconazole activity, produced by Penicillium sp. FKI-1938. I. Taxonomy, fermentation, isolation and biological properties.

PubMed

Fukuda, Takashi; Yamaguchi, Yuichi; Masuma, Rokuro; Tomoda, Hiroshi; Omura, Satoshi

2005-05-01

New phenylfuropyridinones and related compounds, designated citridones A, B, B' and C, were isolated along with known CJ-16,173, from the culture broth of Penicillium sp. FKI-1938 by solvent extraction, silica gel column chromatography and HPLC. Citridones (75 microM) potentiate the miconazole activity against Candida albicans, decreasing the IC50 value of miconazole from 14.5 nM to 3.5 to approximately 6.3 nM.

Detection biomarkers of lung cancer using mini-GC-PID system integrated with micro GC column and micro pre-concentrator

PubMed Central

2014-01-01

The survival rate of lung cancer can be significantly improved by monitoring biomarkers in exhaled air that indicate diseases in early stage, so it is very important to develop micro analytical systems which can offer a fast, on-site, real-time detecting biomarkers in exhaled air. In this paper, a mini-gas chromatography (GC)-photo-ionization detector (PID) system integrated with a micro GC column and a micro pre-concentrator was developed for forming an inexpensive, fast, and non-invasive diagnostic tool for lung cancer. This system has very strong concentrate ability owing to its integrated micro pre-concentrator, which make the detection of trace components in exhaled air very easy. In addition, the integrated micro GC column can separate complex mixtures, which overcome low resolution and poor anti-interference ability of other instruments. The results indicated that the mini-GC-PID system can effectively separate and detect the biomarkers at parts-per-billion (ppb) level. PMID:25339856

Application of capillary gas chromatography mass spectrometry/computer techniques to synoptic survey of organic material in bed sediment

USGS Publications Warehouse

Steinheimer, T.R.; Pereira, W.E.; Johnson, S.M.

1981-01-01

A bed sediment sample taken from an area impacted by heavy industrial activity was analyzed for organic compounds of environmental significance. Extraction was effected on a Soxhlet apparatus using a freeze-dried sample. The Soxhlet extract was fractionated by silica gel micro-column adsorption chromatography. Separation and identification of the organic compounds was accomplished by capillary gas chromatography/mass spectrometry techniques. More than 50 compounds were identified; these include saturated hydrocarbons, olefins, aromatic hydrocarbons, alkylated polycyclic aromatic hydrocarbons, and oxygenated compounds such as aldehydes and ketones. The role of bed sediments as a source or sink for organic pollutants is discussed. ?? 1981.

Identification of kinetin and kinetin riboside in coconut (Cocos nucifera L.) water using a combined approach of liquid chromatography-tandem mass spectrometry, high performance liquid chromatography and capillary electrophoresis.

PubMed

Ge, Liya; Yong, Jean Wan Hong; Goh, Ngoh Khang; Chia, Lian Sai; Tan, Swee Ngin; Ong, Eng Shi

2005-12-27

Kinetin (free base and riboside), which was assumed by many scientists to be a synthetic cytokinin plant growth hormone, has been detected for the first time in the endosperm liquid of fresh young coconut fruits ("coconut water"). To facilitate the study, we developed a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the identification and quantification of kinetin and kinetin riboside in purified coconut water extract sample. Following a solid-phase extraction of cytokinins in coconut water using C18 columns, the samples were further purified by Oasis MCX columns and analyzed by LC-MS/MS for kinetin and kinetin riboside. Detection by mass spectrometry was carried out using selected reaction monitoring (SRM) mode, by identifying the putative kinetin and kinetin riboside based on their characteristic fragments. Based on a signal-to-noise ratio of 3, the limits of detection in SRM mode were 0.02 microM and 0.005 microM for kinetin and kinetin riboside, respectively. Furthermore, optimal conditions for a baseline chromatographic separation of 18 cytokinin standards by high performance liquid chromatography (HPLC) were developed. The HPLC method had been employed for the confirmation and further fractionation of kinetin in coconut water extracts. The confirmation and fractionation of kinetin riboside was carried out using a further modified HPLC program due to the presence of other interfering material(s) in the sample matrix. Finally, fractions of putative kinetin and kinetin riboside collected from HPLC eluate of coconut water sample were further authenticated by independent capillary zone electrophoresis (CZE) experiment.

Micro-fabricated packed gas chromatography column based on laser etching technology.

PubMed

Sun, J H; Guan, F Y; Zhu, X F; Ning, Z W; Ma, T J; Liu, J H; Deng, T

2016-01-15

In this work, a micro packed gas chromatograph column integrated with a micro heater was fabricated by using laser etching technology (LET) for analyzing environmental gases. LET is a powerful tool to etch deep well-shaped channels on the glass wafer, and it is the most effective way to increase depth of channels. The fabricated packed GC column with a length of over 1.6m, to our best knowledge, which is the longest so far. In addition, the fabricated column with a rectangular cross section of 1.2mm (depth) × 0.6mm (width) has a large aspect ratio of 2:1. The results show that the fabricated packed column had a large sample capacity, achieved a separation efficiency of about 5800 plates/m and eluted highly symmetrical Gaussian peaks. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous determination of quercetin, kaempferol and isorhamnetin accumulated human breast cancer cells, by high-performance liquid chromatography.

PubMed

Wang, Yi; Cao, Jiang; Weng, Jian-Hua; Zeng, Su

2005-09-01

Quercetin, kaempferol and isorhamnetin are the most important constituents in ginkgo flavonoids. A simple, rapid and sensitive high-performance liquid chromatography method was developed to simultaneously determine quercetin, kaempferol and isorhamnetin absorped by human breast cancer cells. Cells were treated with ginkgo flavonols and then lysed with Triton-X 100. The flavonols in the samples were measured by RP-HPLC with a C18 column after a simple extraction with a mixture of ether and acetone. The mobile phase contained phosphate buffer (pH 2.0; 10 mM) tetrahydrofuran, methanol and isopropanol (65:15:10:20, v/v/v/v). The ultraviolet detector was operated at 380 nm. The calibration curve was linear from 0.1 to 1.0 microM (r > 0.999) for each flavonol. The mean extraction efficiency was about 70%. The recovery of the assay was between 98.9 and 100.6%. The limit of detection was 0.01 microM for quercetin and kaempferol and 0.05 microM for isorhamnetin. The limit of quantitation was 0.1 microM (R.S.D.<10%) for each flavonol. The intra- and inter-day coefficients of variation were less than 10% (R.S.D.). The validated method was applied to quantify quercetin, kaempferol and isorhamnetin in human breast cancer Bcap37 and Bcap37/MDR1 cells.

Gas chromatography--inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental water samples.

PubMed

Heisterkamp, M; Adams, F C

2001-07-01

The application of inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental waters is described. Construction of the transfer line was achieved by means of a relatively simple and rapid coupling procedure. Derivatization of the ionic lead species was achieved by in-situ propylation with sodium tetrapropylborate; simultaneous extraction of the derivatized compounds in hexane was followed by separation and detection by capillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight mass spectrometry. Detection limits for the different organolead species ranged from 10 to 15 fg (as Pb), corresponding to procedural detection limits between 50 and 75 ng L(-1), on the basis of a 50 mL snow sample, extraction with 200 microL hexane, and subsequent injection of 1 microL of the organic extract on to the column. The accuracy of the system was confirmed by additional analysis of the water samples by capillary gas chromatography coupled with microwave-induced plasma-atomic-emission spectrometry and the analysis of a standard reference material CRM 605 (road dust) with a certified content of trimethyllead.

A high-pressure liquid chromatographic method for the determination of N-acetyl-p-aminophenol (acetaminophen) in serum or plasma using a direct injection technique.

PubMed

Manno, B R; Manno, J E; Dempsey, C A; Wood, M A

1981-01-01

N-Acetyl-p-aminophenol (acetaminophen) is becoming more prevalent as an intoxicant in accidental or intentional overdose, therefore, a direct injection ultra-micro high-pressure liquid chromatographic (HPLC) method has been developed for its quantitation. The HPLC analysis was performed using a Model 110 Solvent Metering Pump equipped with a Model 110-19 Pressure Filter (Altex Scientific, Berkeley, CA), a Model 7120 Rheodyne Injector (Rheodyne, Berkeley, CA) or a Model U6K Injector (Waters Associates, Milford, MA) a Model 440 Absorbance Detector (Water's Associates), and a Model 3380A Recorder Integrator (Hewlett Packard, Avondale, PA). A commercially prepared muBonapak C18 Column (Water's Associates) was used. Acetaminophen was eluted with a mixture of 0.01 mol/L aqueous sodium acetate, pH 4.0: acetonitrile (93:7) and the absorbance detector was operated wih a 254 nm filter. The method, which requires only 2 microL of serum or plasma for analysis, offers several distinct advantages to the analyst. No pre- or post-column extraction or other manipulation of the specimen is required to obtain a quantitative result. Rapid processing of the specimen is possible because both acetaminophen and the internal standard are eluted in less than 10 minutes. The small sample (2 microL) is ideal for use with pediatric patients.

Assessment of elemental mobility in soil using a fluidised bed approach with on-line ICP-MS analysis.

PubMed

Beeston, Michael Philip; Glass, Hylke Jan; van Elteren, Johannes Teun; Slejkovec, Zdenka

2007-09-19

A new method has been developed to analyse the mobility of elements within soils employing counter-current flow soil contacting in a fluidised bed (FB) column. This method alleviates the problem of irreproducible peaks suffered by state-of-the-art micro-column techniques as a result of particle compaction. Reproducible extraction profiles are produced through the leaching of soil with a linear gradient of 0.05 mol L(-1) ammonium sulphate to 0.11 mol L(-1) acetic acid using a high pressure liquid chromatography (HPLC) quaternary pump, and the continuous monitoring of the elements in the leachate with inductively coupled plasma mass spectrometry (ICP-MS). Quantification of the procedure is achieved with an external flow injection (FI) calibration method. Flow rate and FB column length were investigated as critical parameters to the efficiency of the extraction methodology. It was found that an increase in the column length from 10 to 20 cm using a flow rate of 0.15 mL min(-1) produced the same increase in extracted elemental concentration as an increase in flow rate from 0.15 to 0.30 mL min(-1). In both examples, the increase in the concentration of elements leached from the soil may be ascribed to the increase in the concentration gradient between the solid and liquid. The exhaustive nature of the technique defines the maximum leachable concentration within the operationally defined leaching parameters of the exchangeable phase, providing a more accurate assessment of the risk associated with the elements in the soil for the phase providing the greatest risk to the environment. The multi-elemental high sensitivity nature of the on-line detector provides an accurate determination of the associations present between the elements in the soil, and the identification of multiple phases within the exchangeable phase through the presence of multiple peaks in the extraction profiles. It is possible through the deconvolution of these extraction profiles that the concentration corresponding to the peaks identified can be defined.

Histological examination of the oral mucosa after fractional diode laser irradiation with different power and pulse duration

NASA Astrophysics Data System (ADS)

Belikov, Andrey V.; Ermolaeva, Ludmila A.; Korzhevsky, Dmitriy E.; Sergeeva, Elena S.; Semyashkina, Yulia V.; Antropova, Maria M.; Fedotov, Denis Y.; Zaitseva, Maria A.; Kashina, Tatiana V.

2018-04-01

Optical and histological methods were used to examination of influence the power and pulse duration of 980-nm diode laser to the dimensions and morphology of tissue around fractional micro injuries created by the radiation of that laser in the oral mucosa of rats in vivo. The power of laser radiation (P) varied in the range of 1÷21 W, and its pulse duration (tp) - in the range 50÷500 ms. Histological examination showed that in the mucosa of the oral cavity after the laser fractional irradiation, there following effects are found: a tissue defect, a transudate in the lumen of ablative micro injury, stretching and compacting effect of the nuclei of the basal epithelium, the disappearance of granules of the keratohialin, destroying the structure of the connective tissue, erythrocyte stasis in the vessels, the disappearance of transverse striation in the muscle fibers in muscle layer. It has been found that ablative micro injury begins to form up at P = 5 W, tp = 100 ms and affects only the epithelial layer of the mucosa. At P = 7 W, tp = 120 ms, the ratio of width to depth of ablative micro injury is 1 : 1, and at P = 10 W, tp = 100 ms, an ablative micro column with ratio of 1 : 1.5 is formed in the epithelial and submucosal layers of the mucosa. The laser effect with P = 15 W, tp = 200 ms leads to lengthening of the ablation micro-column to 1 : 2, with the bottom of the ablative micro column reaching the muscular layer. With a further growth of laser power or pulse duration, the width of the micro injury increases, and the growth of the micro injury depth is slowed down so that the micro column buildup is ceased.

Method for the determination of organophosphate insecticides in water, sediment and biota.

PubMed

Tse, Hung; Comba, Michael; Alaee, Mehran

2004-01-01

A procedure for the determination of 13 organophosphate insecticides (OPs) in water, sediment and biota at low ppb levels is described. Samples were extracted with dichloromethane or acetone/hexane and cleaned up with micro-column silica gel chromatography. Measurements were made by dual capillary column gas chromatography using both nitrogen-phosphorus (NPD) and electron capture (ECD) detection. Recoveries from fortified water samples ranged from 76% to 102% for all sample types. Practical detection limits ranged between 0.003 and 0.029 microg/l in natural water samples, 0.0004-0.005 microg/g w.w. for sediments, and 0.001-0.005 microg/g w.w for biota using the NPD and ECD method. Losses in sediments were experienced when sulphur was removed. Precision and accuracy were not affected in sediment samples where sulphur was not removed.

Countercurrent flow of supercritical anti-solvent in the production of pure xanthophylls from Nannochloropsis oculata.

PubMed

Cho, Yueh-Cheng; Wang, Yuan-Chuen; Shieh, Chwen-Jen; Lin, Justin Chun-Te; Chang, Chieh-Ming J; Han, Esther

2012-08-10

This study examined pilot scaled elution chromatography coupled with supercritical anti-solvent precipitation (using countercurrent flow) in generating zeaxanthin-rich particulates from a micro-algal species. Ultrasonic agitated acetone extract subjected to column fractionation successfully yielded a fraction containing 349.4 mg/g of zeaxanthin with a recovery of 85%. Subsequently, supercritical anti-solvent (SAS) precipitation of the column fraction at 150 bar and 343 K produced submicron-sized particulates with a concentration of 845.5mg/g of zeaxanthin with a recovery of 90%. Experimental results from a two-factor response surface method SAS precipitation indicated that purity, mean size and morphology of the precipitates were significantly affected by the flow type configuration, feed flow rate and injection time. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparison of several solid-phase extraction sorbents for continuous determination of amines in water by gas chromatography-mass spectrometry.

PubMed

Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

2009-08-15

A semiautomatic method has been proposed for the determination of different types of amines in water samples including anilines, chloroanilines, N-nitrosamines and aliphatic amines. The analytes were retained on a solid-phase extraction sorbent column and after elution, 1 microL of the extract was analysed by gas chromatography coupled with electron impact ionization mass spectrometry. A systematic overview is given of the advantages and disadvantages of several sorbents (LiChrolut EN, Oasis HLB, RP-C(18), graphitized carbon black, fullerenes and nanotubes) in the retention of amine compounds and based on sensitivity, selectivity and reliability. The retention efficiency for the studied amines was higher (ca. 100%) with LiChrolut EN and Oasis HLB than it was with RP-C(18) and fullerenes (53 and 62%, respectively, on average). Detection limits of 0.5-16 ng L(-1) for the 27 amines studied were obtained when using a sorbent column containing 75 mg of LiChrolut EN for 100mL of sample, the RSD being lower than 6.5%. The method was applied with good accuracy and precision in the determination of amines in various types of water including river, pond, tap, well, drinking, swimming pool and waste.

Demonstration of motionless Knudsen pump based micro-gas chromatography featuring micro-fabricated columns and on-column detectors.

PubMed

Liu, Jing; Gupta, Naveen K; Wise, Kensall D; Gianchandani, Yogesh B; Fan, Xudong

2011-10-21

This paper reports the investigation of a micro-gas chromatography (μGC) system that utilizes an array of miniaturized motionless Knudsen pumps (KPs) as well as microfabricated separation columns and optical detectors. A prototype system was built to achieve a flow rate of 1 mL min(-1) and 0.26 mL min(-1) for helium and dry air, respectively, when they were used as carrier gas. This system was then employed to evaluate GC performance compromises and demonstrate the ability to separate and detect gas mixtures containing analytes of different volatilities and polarities. Furthermore, the use of pressure programming of the KP array was demonstrated to significantly shorten the analysis time while maintaining a high detection resolution. Using this method, we obtained a high resolution detection of 5 alkanes of different volatilities within 5 min. Finally, we successfully detected gas mixtures of various polarities using a tandem-column μGC configuration by installing two on-column optical detectors to obtain complementary chromatograms.

Confirmation of diosmetin 3-O-glucuronide as major metabolite of diosmin in humans, using micro-liquid-chromatography-mass spectrometry and ion mobility mass spectrometry.

PubMed

Silvestro, Luigi; Tarcomnicu, Isabela; Dulea, Constanta; Attili, Nageswara Rao B N; Ciuca, Valentin; Peru, Dan; Rizea Savu, Simona

2013-10-01

Diosmin is a flavonoid often administered in the treatment of chronic venous insufficiency, hemorrhoids, and related affections. Diosmin is rapidly hydrolized in the intestine to its aglicone, diosmetin, which is further metabolized to conjugates. In this study, the development and validations of three new methods for the determination of diosmetin, free and after enzymatic deconjugation, and of its potential glucuronide metabolites, diosmetin-3-O-glucuronide, diosmetin-7-O-glucuronide, and diosmetin-3,7-O-glucuronide from human plasma and urine are presented. First, the quantification of diosmetin, free and after deconjugation, was carried out by high-performance liquid chromatography coupled with tandem mass spectrometry, on an Ascentis RP-Amide column (150 × 2.1 mm, 5 μm), in reversed-phase conditions, after enzymatic digestion. Then glucuronide metabolites from plasma were separated by micro-liquid chromatography coupled with tandem mass spectrometry on a HALO C18 (50 × 0.3 mm, 2.7 μm, 90 Å) column, after solid-phase extraction. Finally, glucuronides from urine were measured using a Discovery HSF5 (100 × 2.1 mm, 5 μm) column, after simple dilution with mobile phase. The methods were validated by assessing linearity, accuracy, precision, low limit of quantification, selectivity, extraction recovery, stability, and matrix effects; results in agreement with regulatory (Food and Drug Administration and European Medicines Agency) guidelines acceptance criteria were obtained in all cases. The methods were applied to a pharmacokinetic study with diosmin (450 mg orally administered tablets). The mean C max of diosmetin in plasma was 6,049.3 ± 5,548.6 pg/mL. A very good correlation between measured diosmetin and glucuronide metabolites concentrations was obtained. Diosmetin-3-O-glucuronide was identified as a major circulating metabolite of diosmetin in plasma and in urine, and this finding was confirmed by supplementary experiments with differential ion-mobility mass spectrometry.

Simultaneous determination of thirteen different steroid hormones using micro UHPLC-MS/MS with on-line SPE system.

PubMed

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tímea; Mészáros, Katalin Viola; Bálint, Mária; Szabó, Pál Tamás

2018-02-20

Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LOQ). Micro UHPLC coupled to sensitive tandem mass spectrometry provides state of the art solution for such analytical problems. Using on-line SPE with column switching on a micro UHPLC-MS/MS system allowed to decrease LOQ without any complex sample preparation protocol. The presented method is capable of reaching satisfactory low LOQ values for analysis of thirteen different steroid molecules from human plasma without the most commonly used off-line SPE or compound derivatization. Steroids were determined by using two simple sample preparation methods, based on lower and higher plasma steroid concentrations. In the first method, higher analyte concentrations were directly determined after protein precipitation with methanol. The organic phase obtained from the precipitation was diluted with water and directly injected into the LC-MS system. In the second method, low steroid levels were determined by concentrating the organic phase after steroid extraction. In this case, analytes were extracted with ethyl acetate and reconstituted in 90/10 water/acetonitrile following evaporation to dryness. This step provided much lower LOQs, outperforming previously published values. The method has been validated and subsequently applied to clinical laboratory measurement. Copyright © 2017 Elsevier B.V. All rights reserved.

Use of mesophilic and thermophilic bacteria for the improvement of copper extraction from a low-grade ore

NASA Astrophysics Data System (ADS)

Darezereshki, E.; Schaffie, M.; Lotfalian, M.; Seiedbaghery, S. A.; Ranjbar, M.

2011-04-01

Bioleaching was examined for copper extraction from a low grade ore using mesophilic and moderate thermophilic bacteria. Five equal size columns were used for the leaching of the ore. Sulfuric acid solution with a flow rate of 3.12 L·m-2·h-1 and pH 1.5 passed through each column continuously for 90 d. In the first and the second column, bioleaching was performed without agglomeration of the ore and on the agglomerated ore, respectively. 28wt% of the copper was extracted in the first column after 40 d, while this figure was 38wt% in the second column. After 90 d, however, the overall extractions were almost the same for both of them. Bioleaching with mesophilic bacteria was performed in the third column without agglomeration of the ore and in the fourth column on the agglomerated ore. After 40 d, copper extractions in the third and the fourth columns were 62wt% and 70wt%, respectively. Copper extractions were 75wt% for both the columns after 90 d. For the last column, bioleaching was performed with moderate thermophilic bacteria and agglomerated ore. Copper extractions were 80wt% and 85wt% after 40 and 90 d, respectively. It was concluded that crushing and agglomeration of the ore using bacteria could enhance the copper extraction considerably.

Automated in-tube solid-phase microextraction coupled with liquid chromatography/electrospray ionization mass spectrometry for the determination of beta-blockers and metabolites in urine and serum samples.

PubMed

Kataoka, H; Narimatsu, S; Lord, H L; Pawliszyn, J

1999-10-01

The technique of automated in-tube solid-phase microextraction (SPME) coupled with liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) was evaluated for the determination of beta-blockers in urine and serum samples. In-tube SPME is an extraction technique for organic compounds in aqueous samples, in which analytes are extracted from the sample directly into an open tubular capillary by repeated draw/eject cycles of sample solution. LC/MS analyses of beta-blockers were initially performed by liquid injection onto a LC column. Nine beta-blockers tested in this study gave very simple ESI mass spectra, and strong signals corresponding to [M + H]+ were observed for all beta-blockers. The beta-blockers were separated with a Hypersil BDS C18 column using acetonitrile/methanol/water/acetic acid (15:15:70:1) as a mobile phase. To optimize the extraction of beta-blockers, several in-tube SPME parameters were examined. The optimum extraction conditions were 15 draw/eject cycles of 30 microL of sample in 100 mM Tris-HCl (pH 8.5) at a flow rate of 100 microL/min using an Omegawax 250 capillary (Supelco, Bellefonte, PA). The beta-blockers extracted by the capillary were easily desorbed by mobile-phase flow, and carryover of beta-blockers was not observed. Using in-tube SPME/LC/ESI-MS with selected ion monitoring, the calibration curves of beta-blockers were linear in the range from 2 to 100 ng/mL with correlation coefficients above 0.9982 (n = 18) and detection limits (S/N = 3) of 0.1-1.2 ng/mL. This method was successfully applied to the analysis of biological samples without interference peaks. The recoveries of beta-blockers spiked into human urine and serum samples were above 84 and 71%, respectively. A serum sample from a patient administrated propranolol was analyzed using this method and both propranolol and its metabolites were detected.

Cyclodextrin based polymer sorbents for micro-solid phase extraction followed by liquid chromatography tandem mass spectrometry in determination of endogenous steroids.

PubMed

Manaf, Normaliza Abdul; Saad, Bahruddin; Mohamed, Mohamed H; Wilson, Lee D; Latiff, Aishah A

2018-03-30

Sorbents were prepared by cross-linking β-cyclodextrin (β-CD) using two different types of cross-linker units at variable reactant mole ratios. The resulting polymers containing β-CD were evaluated as sorbents in micro-solid phase extraction (μ-SPE) format for the extraction of the endogenous steroids testosterone (T), epitestosterone (E), androsterone (A), etiocholanolone (Etio), 5α-androstane-3α,17β-diol (5αAdiol) and 5β-androstane-3α,17β-diol (5βAdiol). The best sorbent (C1; cyclodextrin polymer) showed superior extraction characteristics compared with commercial sorbents (C18 and Bond Elut Plexa). Parameters influencing the extraction efficiency of the C1 sorbent such as extraction and desorption times, desorption solvent and volume of sample were investigated. The extracts were separated using a Hypersil Gold column (50 × 2.1 mm, 1.9 μm) under gradient elution coupled to a LC-MS/MS. The compounds were successfully separated within 8 min. The method offers good repeatability (RSD < 10%) and linearity (r 2  > 0.995) were within the range of 1-200 ng mL -1 for T and E, 250-4000 ng mL -1 for A and Etio and 25-500 ng mL -1 for 5αAdiol and 5βAdiol, respectively. The method was applied for the determination of steroid profile of urine from volunteers. Copyright © 2018 Elsevier B.V. All rights reserved.

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 comparison study of nanofiber, microfiber, and new composite nano/microfiber polymers used as sorbents for on-line solid phase extraction in chromatography system.

PubMed

Háková, Martina; Havlíková, Lucie Chocholoušová; Chvojka, Jiří; Erben, Jakub; Solich, Petr; Švec, František; Šatínský, Dalibor

2018-09-06

Three different approaches has been used to obtain nano/micro fibers and their diversity and extraction properties were examined. The effect of their structure on stability in an ultra-high-performance liquid chromatography (UHPLC) system during on-line SPE procedure was monitored. Five types of various nano/micro fiber polymers were used as sorbents: polyamide 6 nanofibers, polyvinylidene difluoride nanofibers, polyethylene microfibers, and two new polycaprolactone microfiber/nanofiber and polycaprolactone microfibers/polyvinylidene difluoride nanofibers composite polymers. The fiber polymers were filled in a cartridge directly connected to the UHPLC system and tested. For each polymer, the optimal conditions of the on-line extraction were found and potential applicability on real samples was tested. The determination of ochratoxin A (OTA) in beer matrix was chosen as a case study. Relevant factors such as the mechanical and chemical stability of the nano/microfibers, filling the cartridges, fiber reusability and the possibility and the repeatability of all processes were involved in the proposed study. A new nano/micro composite sorbent consisting of polycaprolactone microfibers/polyvinylidene difluoride nanofibers was chosen as the most suitable sorbent for the on-line extraction of OTA from a beer matrix. The tested validation parameters had the value of intra-day precision lower than 1.48%, linearity in the range from 0.5 to 100 μg L -1 with r 2  ≥ 0.9999 for standard and matrix calibration curve, and recovery in the range 99.1-103.9% at five concentration levels. Long-term precision evaluated for 31 analyses over the period of three months did not exceed 2.9% RSD. It confirmed the column reusability and perfect stability of nano/micro composite sorbent in the presence of organic solvents and after repeated injection of a complex beer matrix. Copyright © 2018 Elsevier B.V. All rights reserved.

Novel dispersive micro-solid-phase extraction combined with ultrahigh-performance liquid chromatography-high-resolution mass spectrometry to determine morpholine residues in citrus and apples.

PubMed

Chen, Dawei; Miao, Hong; Zou, Jianhong; Cao, Pei; Ma, Ning; Zhao, Yunfeng; Wu, Yongning

2015-01-21

This paper presents a new analytical method for the determination of morpholine residues in citrus and apples using a novel dispersive micro-solid-phase extraction (DMSPE), followed by ultrahigh-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS). Samples were extracted with 1% formic acid in acetonitrile/water (1:1, v/v) and then cleaned up using the DMSPE procedure. Morpholine from the extract was adsorbed to a polymer cation exchange sorbent and eluted with ammonium hydroxide/acetonitrile (3:97, v/v) through a 1 mL syringe with a 0.22 μm nylon syringe filter. All of the samples were analyzed by UHPLC-HRMS/MS on a Waters Acquity BEH hydrophilic interaction chromatography column using 0.1% formic acid and 4 mM ammonium formate in water/acetonitrile as the mobile phase with gradient elution. The method showed good linearity (R(2) > 0.999) in the range of 1-100 μg/L for the analyte. The limit of detection and limit of quantitation values of morpholine were 2 and 5 μg/kg, respectively. The average recoveries of morpholine from the citrus and apple samples spiked at three different concentrations (5, 20, and 100 μg/kg) were in a range from 78.4 to 102.7%.

Q Sepharose micro-column chromatography: A simple screening method for identifying beta thalassemia traits and hemoglobin E carriers.

PubMed

Wong, Peerapon; Sritippayawan, Suchila; Suwannakhon, Narutchala; Tapprom, Akamon; Deoisares, Rawisut; Sanguansermsri, Torpong

2016-11-01

For beta thalassemia control program in pregnancy, mass screening of the carrier state by determination of the hemoglobin (Hb) A 2 and Hb E proportions and mutation analysis is a preferred method for making prenatal diagnoses. Q Sepharose micro-column chromatography, developed for the determination of Hb A 2 and Hb E for screening purposes, was compared with high performance liquid chromatography (HPLC) to ascertain its relative accuracy and reliability. Results using Q Sepharose micro-column chromatography in 350 blood specimens, including 50 samples genetically proven to be beta thalassemia heterozygotes, were compared to HPLC for validation. An additional study was conducted to test a clinical application on a large-scale survey for beta thalassemia in 1581 pregnant women and their spouses. The mean (±SD) Hb A 2 proportions in the normal and genetically proven beta thalassemia heterozygotes were 2.70±0.40% and 6.30±1.23%, respectively, as determined by Q-Sepharose micro-column chromatography, and 2.65±0.31% and 5.37±0.96%, respectively, as determined by HPLC. The mean Hb E proportions in the Hb E heterozygotes were 23.25±4.13% and 24.72±3.5% as determined by Q Sepharose micro-column chromatography and HPLC, respectively. In the large-scale survey for beta thalassemia, 23 at risk couples were detected. Seven affected fetuses were identified by prenatal diagnosis. Q Sepharose micro-column chromatography was found to be reliable, reproducible and well-suited for large-scale surveys. Additionally, by being reusable and convenient, this simple and economical chromatography method may be an alternative means to screen for beta thalassemia and Hb E carriers in the mass population. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Secondary metabolites of ponderosa lemon (Citrus pyriformis) and their antioxidant, anti-inflammatory, and cytotoxic activities.

PubMed

Hamdan, Dalia; El-Readi, Mahmoud Zaki; Tahrani, Ahmad; Herrmann, Florian; Kaufmann, Dorothea; Farrag, Nawal; El-Shazly, Assem; Wink, Michael

2011-01-01

Column chromatography of the dichloromethane fraction from an aqueous methanolic extract of fruit peel of Citrus pyriformis Hassk. (Rutaceae) resulted in the isolation of seven compounds including one coumarin (citropten), two limonoids (limonin and deacetylnomilin), and four sterols (stigmasterol, ergosterol, sitosteryl-3-beta-D-glucoside, and sitosteryl-6'-O-acyl-3-beta-D-glucoside). From the ethyl acetate fraction naringin, hesperidin, and neohesperidin were isolated. The dichloromethane extract of the defatted seeds contained three additional compounds, nomilin, ichangin, and cholesterol. The isolated compounds were identified by MS (EI, CI, and ESI), 1H, 13C, and 2D-NMR spectral data. The limonoids were determined qualitatively by LC-ESI/MS resulting in the identification of 11 limonoid aglycones. The total methanolic extract of the peel and the petroleum ether, dichloromethane, and ethyl acetate fractions were screened for their antioxidant and anti-inflammatory activities. The ethyl acetate fraction exhibited a significant scavenging activity for DPPH free radicals (IC50 = 132.3 microg/mL). The petroleum ether fraction inhibited 5-lipoxygenase with IC50 = 30.6 microg/mL indicating potential anti-inflammatory properties. Limonin has a potent cytotoxic effect against COS7 cells [IC50 = (35.0 +/- 6.1) microM] compared with acteoside as a positive control [IC50 = (144.5 +/- 10.96) microM].

Determination of pesticides in waters by automatic on-line solid-phase extraction-capillary electrophoresis.

PubMed

Hinsmann, P; Arce, L; Ríos, A; Valcárcel, M

2000-01-07

The separation of seven pesticides by micellar electrokinetic capillary chromatography in spiked water samples is described, allowing the analysis of pesticides mixtures down to a concentration of 50 microg l(-1) in less than 13 min. Calibration, pre-concentration, elution and injection into the sample vial was carried out automatically by a continuous flow system (CFS) coupled to a capillary electrophoresis system via a programmable arm. The whole system was electronically coupled by a micro-processor and completely controlled by a computer. A C18 solid-phase mini-column was used for the pre-concentration, allowing a 12-fold enrichment (as an average value) of the pesticides from fortified water samples. Under the optimal extraction conditions, recoveries between 90 and 114% for most of the pesticides were obtained.

Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

NASA Technical Reports Server (NTRS)

Huz, Kateryna

2014-01-01

RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better detection via good peak separation with a longer run time is a better asset than moderate peak separation with a shorter run time. Even given that RESOLVE is highly interested in water and that mission timeline is of significant importance given the short seven-to-ten-day mission timeline, worse detection with an 8m column may lead to overlooking other substances existing on the moon that could advance planetary science. Thus, I recommend the 20m column. However, if mission timeline and water separation are deemed the highest priority, the 8m column should be selected due to its ability to separate water within a shorter run time than the 20m column.

Medication and volume delivery by gravity-driven micro-drip intravenous infusion: potential variations during "wide-open" flow.

PubMed

Pierce, Eric T; Kumar, Vikram; Zheng, Hui; Peterfreund, Robert A

2013-03-01

Gravity-driven micro-drip infusion sets allow control of medication dose delivery by adjusting drops per minute. When the roller clamp is fully open, flow in the drip chamber can be a continuous fluid column rather than discrete, countable, drops. We hypothesized that during this "wide-open" state, drug delivery becomes dependent on factors extrinsic to the micro-drip set and is therefore difficult to predict. We conducted laboratory experiments to characterize volume delivery under various clinically relevant conditions of wide-open flow in an in vitro laboratory model. A micro-drip infusion set, plugged into a bag of normal saline, was connected to a high-flow stopcock at the distal end. Vertically oriented IV catheters (gauges 14-22) were connected to the stopcock. The fluid meniscus height in the bag was fixed (60-120 cm) above the outflow point. The roller clamp on the infusion set was in fully open position for all experiments resulting in a continuous column of fluid in the drip chamber. Fluid volume delivered in 1 minute was measured 4 times with each condition. To model resistive effects of carrier flow, volumetric infusion pumps were used to deliver various flow rates of normal saline through a carrier IV set into which a micro-drip infusion was "piggybacked." We also compared delivery by micro-drip infusion sets from 3 manufacturers. The volume of fluid delivered by gravity-driven infusion under wide-open conditions (continuous fluid column in drip chamber) varied 2.9-fold (95% confidence interval, 2.84-2.96) depending on catheter size and fluid column height. Total model resistance of the micro-drip with stopcock and catheter varied with flow rate. Volume delivered by the piggybacked micro-drip decreased up to 29.7% ± 0.8% (mean ± SE) as the carrier flow increased from 0 to 1998 mL/min. Delivery characteristics of the micro-drip infusion sets from 3 different manufacturers were similar. Laboratory simulation of clinical situations with gravity-driven micro-drip infusion sets under wide-open flow conditions revealed that infusion rate (drug and/or volume delivery) can vary widely depending on extrinsic factors including catheter size, fluid column height, and carrier flow. The variable resistance implies nonlaminar flow in the micro-drip model that cannot be easily predicted mathematically. These findings support the use of mechanical pumps instead of gravity-driven micro-drips to enhance the precision and safety of IV infusions, especially for vasoactive drugs.

Fully integrated and encapsulated micro-fabricated vacuum diode and method of manufacturing same

DOEpatents

Resnick, Paul J.; Langlois, Eric

2015-12-01

Disclosed is an encapsulated micro-diode and a method for producing same. The method comprises forming a plurality columns in the substrate with a respective tip disposed at a first end of the column, the tip defining a cathode of the diode; disposing a sacrificial oxide layer on the substrate, plurality of columns and respective tips; forming respective trenches in the sacrificial oxide layer around the columns; forming an opening in the sacrificial oxide layer to expose a portion of the tips; depositing a conductive material in of the opening and on a surface of the substrate to form an anode of the diode; and removing the sacrificial oxide layer.

Method of manufacturing a fully integrated and encapsulated micro-fabricated vacuum diode

DOEpatents

Resnick, Paul J.; Langlois, Eric

2014-08-26

Disclosed is an encapsulated micro-diode and a method for producing same. The method comprises forming a plurality columns in the substrate with a respective tip disposed at a first end of the column, the tip defining a cathode of the diode; disposing a sacrificial oxide layer on the substrate, plurality of columns and respective tips; forming respective trenches in the sacrificial oxide layer around the columns; forming an opening in the sacrificial oxide layer to expose a portion of the tips; depositing a conductive material in of the opening and on a surface of the substrate to form an anode of the diode; and removing the sacrificial oxide layer.

The study on the extraction method of indirubin from Indigo Naturalis.

PubMed

Cheng, Li-hui

2007-01-01

To discuss how to extract the indirubin of the higher purity from Indigo Naturalis. After extracting the indirubin from Indigo Naturalis by acetic ether, compare the separation effect of the extract in Si gel column with that in alumina column. The indirubin in Indigo Naturalis by Si gel column chromatography is chosen. The purity of indirubin is 98.3% after Si gel column chromatography. The indiruhbin of the higher purity was attained by the simple experimental method.

Improved method for extraction and detection of Helicobacter pylori DNA in formalin-fixed paraffin embedded gastric biopsies using laser micro-dissection.

PubMed

Loayza, María Fernanda; Villavicencio, Fernando Xavier; Santander, Stephanie Carolina; Baldeón, Manuel; Ponce, Lourdes Karina; Salvador, Iván; Vivar Díaz, Nicolás

2015-01-01

To assess the molecular events exerted by Helicobacter pylori interacting directly with gastric epithelial cells, an improved procedure for microbial DNA isolation from stained hematoxilin-eosin gastric biopsies was developed based on laser micro-dissection (LM) [1]. Few articles have described the use of LM to select and detect H. pylori genome from formalin-fixed paraffin embedded gastric tissue [2]. To improve the yield and quality of DNA isolated from H. pylori contacting intestinal epithelial cells, the following conditions were established after modification of the QIAamp DNA Micro kit. •Use of at least 25 cut sections of 10-20 μm of diameter and 3 μm thick with more than 10 bacteria in each cut.•Lysis with 30 μL of tissue lysis buffer and 20 μL of proteinase K (PK) with the tube in an upside-down position.•The use of thin purification columns with 35 μL of elution buffer. The mean of DNA concentration obtained from 25 LM cut sections was 1.94± 0 .16 ng/μL, and it was efficiently amplified with qPCR in a Bio Rad iCycler instrument. The LM can improve the sample selection and DNA extraction for molecular analysis of H. pylori associated with human gastric epithelium.

Semi-micro high-performance liquid chromatographic analysis of tiropramide in human plasma using column-switching.

PubMed

Baek, Soo Kyoung; Lee, Seung Seok; Park, Eun Jeon; Sohn, Dong Hwan; Lee, Hye Suk

2003-02-05

A rapid and sensitive column-switching semi-micro high-performance liquid chromatography method was developed for the direct analysis of tiropramide in human plasma. The plasma sample (100 microl) was directly injected onto Capcell Pak MF Ph-1 precolumn where deproteinization and analyte fractionation occurred. Tiropramide was then eluted into an enrichment column (Capcell Pak UG C(18)) using acetonitrile-potassium phosphate (pH 7.0, 50 mM) (12:88, v/v) and was analyzed on a semi-micro C(18) analytical column using acetonitrile-potassium phosphate (pH 7.0, 10 mM) (50:50, v/v). The method showed excellent sensitivity (limit of quantification 5 ng/ml), and good precision (C.V.

Microfabricated thermal modulator for comprehensive two-dimensional micro gas chromatography: design, thermal modeling, and preliminary testing.

PubMed

Kim, Sung-Jin; Reidy, Shaelah M; Block, Bruce P; Wise, Kensall D; Zellers, Edward T; Kurabayashi, Katsuo

2010-07-07

In comprehensive two-dimensional gas chromatography (GC x GC), a modulator is placed at the juncture between two separation columns to focus and re-inject eluting mixture components, thereby enhancing the resolution and the selectivity of analytes. As part of an effort to develop a microGC x microGC prototype, in this report we present the design, fabrication, thermal operation, and initial testing of a two-stage microscale thermal modulator (microTM). The microTM contains two sequential serpentine Pyrex-on-Si microchannels (stages) that cryogenically trap analytes eluting from the first-dimension column and thermally inject them into the second-dimension column in a rapid, programmable manner. For each modulation cycle (typically 5 s for cooling with refrigeration work of 200 J and 100 ms for heating at 10 W), the microTM is kept approximately at -50 degrees C by a solid-state thermoelectric cooling unit placed within a few tens of micrometres of the device, and heated to 250 degrees C at 2800 degrees C s(-1) by integrated resistive microheaters and then cooled back to -50 degrees C at 250 degrees C s(-1). Thermal crosstalk between the two stages is less than 9%. A lumped heat transfer model is used to analyze the device design with respect to the rates of heating and cooling, power dissipation, and inter-stage thermal crosstalk as a function of Pyrex-membrane thickness, air-gap depth, and stage separation distance. Experimental results are in agreement with trends predicted by the model. Preliminary tests using a conventional capillary column interfaced to the microTM demonstrate the capability for enhanced sensitivity and resolution as well as the modulation of a mixture of alkanes.

Low-energy route for alcohol/gasohol recovery from fermentor beer. Final report

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

Mix, T.W.

1982-03-01

The production of gasohol directly from fermentor beer and gasoline is feasible and will enable a major reduction in the energy requirements for gasohol production. The fermentor beer is first enriched in a beer still to a 69 mol % ethanol, 31 mol % water product which is then dehydrated by extractive distillation with gasoline as the extractive agent. Gasohol is produced directly. In one version of the process, a heavy cut of gasoline, presumed available at a refinery before blending in of light components, is used as the extractive agent. The enriching column overhead vapors are used to reboilmore » the extractive distillation and steam stripping columns and to contribute to the preheating of the fermentor beer feed. Light components are blended into the heavy cut-ethanol bottom product from the extractive distillation column to form the desired gasohol. Energy requirements, including feed preheat, are 11,000 Btu per gallon of ethanol in the product gasohol. One hundred and fifty pound steam is required. In a second version, full range gasoline is used as the extractive agent. The enriching column overhead vapors are again used to reboil the extractive distillation and steam stripping columns and to contribute to the preheating of the fermentor beer feed. Light gasoline components recovered from the decanter following the overhead condenser of the extractive distillation column are blended in with the gasoline-ethanol product leaving the bottom of the extractive distillation column to form the desired gasohol. Energy requirements in this case are 13,000 Btu/gallon of ethanol in the product gasohol. In both of the above cases it is energy-conservative and desirable from a process standpoint to feed the enriched alcohol to the extractive distillation column as a liquid rather than as a vapor.« less

Application of Nanofiber-packed SPE for Determination of Urinary 1-Hydroxypyrene Level Using HPLC.

PubMed

Ifegwu, Okechukwu Clinton; Anyakora, Chimezie; Chigome, Samuel; Torto, Nelson

2014-01-01

It is always desirable to achieve maximum sample clean-up, extraction, and pre-concentration with the minimum possible organic solvent. The miniaturization of sample preparation devices was successfully demonstrated by packing 10 mg of 11 electrospun polymer nanofibers into pipette tip micro column and mini disc cartridges for efficient pre-concentration of 1-hydroxypyrene in urine samples. 1-hydroxypyrene is an extensively studied biomarker of the largest class of chemical carcinogens. Excretory 1-hydroxypyrene was monitored with HPLC/fluorescence detector. Important parameters influencing the percentage recovery such as fiber diameter, fiber packing amount, eluent, fiber packing format, eluent volume, surface area, porosity, and breakthrough parameters were thoroughly studied and optimized. Under optimized condition, there was a near perfect linearity of response in the range of 1-1000 μg/L with a coefficient of determination (r (2)) between 0.9992 and 0.9999 and precision (% RSD) ≤7.64% (n = 6) for all the analysis (10, 25, and 50 μg/L). The Limit of detection (LOD) was between 0.022 and 0.15 μg/L. When compared to the batch studies, both disc packed nanofiber sorbents and pipette tip packed sorbents exhibited evident dominance based on their efficiencies. The experimental results showed comparable absolute recoveries for the mini disc packed fibers (84% for Nylon 6) and micro columns (80% for Nylon 6), although the disc displayed slightly higher recoveries possibly due to the exposure of the analyte to a larger reacting surface. The results also showed highly comparative extraction efficiencies between the nanofibers and conventional C-18 SPE sorbent. Nevertheless, miniaturized SPE devices simplified sample preparation, reducing back pressure, time of the analysis with acceptable reliability, selectivity, detection levels, and environmental friendliness, hence promoting green chemistry.

Dispersive micro-solid-phase extraction of benzoylurea insecticides in honey samples with a β-cyclodextrin-modified attapulgite composite as sorbent.

PubMed

Zhang, Panjie; Cui, Xiangqian; Yang, Xiaoling; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang; Lu, Runhua

2016-01-01

A β-cyclodextrin-modified attapulgite composite was prepared and used as a dispersive micro-solid-phase extraction sorbent for the determination of benzoylurea insecticides in honey samples. Parameters that may influence the extraction efficiency, such as the type and volume of the eluent, the amount of the sorbent, the extraction time and the ionic strength were investigated and optimized using batch and column procedures. Under optimized conditions, good linearity was obtained for all of the tested compounds, with R(2) values of at least 0.9834. The limits of detection were determined in the range of 0.2-1.0 μg/L. The recoveries of the four benzoylurea insecticides in vitex honey and acacia honey increased from 15.2 to 81.4% and from 14.2 to 82.0%, respectively. Although the β-cyclodextrin-modified attapulgite composite did not show a brilliant adsorption capacity for the selected benzoylurea insecticides, it exhibited a higher adsorption capacity toward relatively hydrophobic compounds, such as chlorfluazuron and hexaflumuron (recoveries in vitex honey samples ranged from 70.0 to 81.4% with a precision of 1.0-3.7%). It seemed that the logPow of the benzoylurea insecticides is related to their recoveries. The results confirmed the possibility of using cyclodextrin-modified palygorskite in the determination of relatively hydrophobic trace pharmaceutical residues. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A parallel bubble column system for the cultivation of phototrophic microorganisms.

PubMed

Havel, Jan; Franco-Lara, Ezequiel; Weuster-Botz, Dirk

2008-07-01

An incubator with up to 16 parallel bubble columns was equipped with artificial light sources assuring a light supply with a homogenous light spectrum directly above the bioreactors. Cylindrical light reflecting tubes were positioned around every single bubble column to avoid light scattering effects and to redirect the light from the top onto the cylindrical outer glass surface of each bubble column. The light reflecting tubes were equipped with light intensity filters to control the total light intensity for every single photo-bioreactor. Parallel cultivations of the unicellular obligate phototrophic cyanobacterium, Synechococcus PCC7942, were studied under different constant light intensities ranging from 20 to 102 microE m(-2)s(-1) at a constant humidified air flow rate supplemented with CO(2).

Development of High Precision Metal Micro-Electro-Mechanical-Systems Column for Portable Surface Acoustic Wave Gas Chromatograph

NASA Astrophysics Data System (ADS)

Iwaya, Takamitsu; Akao, Shingo; Sakamoto, Toshihiro; Tsuji, Toshihiro; Nakaso, Noritaka; Yamanaka, Kazushi

2012-07-01

In the field of environmental measurement and security, a portable gas chromatograph (GC) is required for the on-site analysis of multiple hazardous gases. Although the gas separation column has been downsized using micro-electro-mechanical-systems (MEMS) technology, an MEMS column made of silicon and glass still does not have sufficient robustness and a sufficiently low fabrication cost for a portable GC. In this study, we fabricated a robust and inexpensive high-precision metal MEMS column by combining diffusion-bonded etched stainless-steel plates with alignment evaluation using acoustic microscopy. The separation performance was evaluated using a desktop GC with a flame ionization detector and we achieved the high separation performance comparable to the best silicon MEMS column fabricated using a dynamic coating method. As an application, we fabricated a palm-size surface acoustic wave (SAW) GC combining this column with a ball SAW sensor and succeeded in separating and detecting a mixture of volatile organic compounds.

Determination of organic peroxides by liquid chromatography with on-line post-column ultraviolet irradiation and peroxyoxalate chemiluminescence detection.

PubMed

Wada, Mitsuhiro; Inoue, Keiyu; Thara, Ayuko; Kishikawa, Naoya; Nakashima, Kenichiro; Kuroda, Naotaka

2003-02-14

A HPLC method was developed for the simultaneous determination of organic peroxides and hydrogen peroxide with peroxyoxalate chemiluminescence (PO-CL) detection following on-line UV irradiation. Organic peroxides [i.e., benzoyl peroxide (BP), tert.-butyl hydroperoxide (BHP), tert.-butyl perbenzoate (BPB), cumene hydroperoxide (CHP)] were UV irradiated (254 nm, 15 W) to generate hydrogen peroxide, which was determined by PO-CL detection. The conditions for UV irradiation and PO-CL detection were optimized by a flow injection analysis (FIA) system. Generation of hydrogen peroxide from peroxides with on-line UV irradiation also was confirmed by the FIA system by incorporating an enzyme column reactor immobilized with catalase. The separation of four organic peroxides and hydrogen peroxide by HPLC was accomplished isocratically on an ODS column within 30 min. The detection limits (signal-to-noise ratio=3) were 1.1 microM for hydrogen peroxide, 6.8 microM for BP, 31.3 microM for BHP, 7.5 microM for BPB and 1.3 microM for CHP. The proposed method was applied to the determination of BP in wheat flour.

Quantitation of acrylamide in food products by liquid chromatography/mass spectrometry.

PubMed

Eberhart, B Loye; Ewald, Deborah K; Sanders, Robert A; Tallmadge, Daniel H; Zyzak, David V; Strothers, Melissa A

2005-01-01

A simple and inexpensive liquid chromatography/mass spectrometry (LC/MS) method was developed for the quantitation of acrylamide in various food products. The method involved spiking the isotope-substituted internal standard (1-C13 acrylamide) onto 6.00 g of the food product, adding 40 mL distilled/deionized water, and heating at 65 degrees C for 30 min. Afterwards, 10 mL ethylene dichloride was added and the mixture was homogenized for 30 s and centrifuged at 2700 x g for 30 min, and then 8 g supernatant was extracted with 10, 5, and 5 mL portions of ethyl acetate. The extracts were combined, dried with sodium sulfate, and concentrated to 100-200 microL. Acrylamide was determined by analysis of the final extract on a single quadrupole, bench-top mass spectrometer with electrospray ionization, using a 2 mm id C18 column and monitoring m/z = 72 (acrylamide) and m/z = 73 (internal standard). For difficult food matrixes, such as coffee and cocoa, a solid-phase extraction cleanup step was incorporated to improve both chromatography and column lifetime. The method had a limit of quantitation of 10 ppb, and coefficients of determination (r2) for calibration curves were typically better than 0.998. Acceptable spike recovery results were achieved in 11 different food matrixes. Precision in potato chip analyses was 5-8% (relative standard deviation). This method provides an LC/MS alternative to the current LC/MS/MS methods and derivatization gas chromatography/mass spectrometry methods, and is applicable to difficult food products such as coffee, cocoa, and high-salt foods.

Determination of trihalomethanes in waters by ionic liquid-based single drop microextraction/gas chromatographic/mass spectrometry.

PubMed

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

2008-10-31

A simple, rapid, solventless method for the determination of trihalomethanes (THMs) (chloroform, bromodichloromethane, dibromochloromethane and bromoform) in water samples is presented. The analytes are extracted from the headspace of the aqueous matrix into a 2 microL drop of the ionic liquid 1-octyl-3-methyl-imidazolium hexafluorophosphate working at 30 degrees C for 30 min. The separation and detection of the target compounds is accomplished by gas chromatography/mass spectrometry owing to the use of an interface that efficiently transfers the analytes extracted in the ionic liquid drop to the gas chromatograph while preventing the ionic liquid from entering the column. The detection limits obtained are below the values compelled by the legislation, ranging from 0.5 microg L(-1) for chloroform and bromodichloromethane to 0.9 microg L(-1) for dibromochloromethane. The use of ionic liquid in the extraction procedure avoids the use of organic solvents and leads to relative standard deviations that range from 3.1% to 4.8%.

Signal Enhancement in HPLC/Micro-Coil NMR Using Automated Column Trapping

PubMed Central

Djukovic, Danijel; Liu, Shuhui; Henry, Ian; Tobias, Brian; Raftery, Daniel

2008-01-01

A new HPLC-NMR system is described that performs analytical separation, pre-concentration, and NMR spectroscopy in rapid succession. The central component of our method is the online pre-concentration sequence that improves the match between post-column analyte peak volume and the micro-coil NMR detection volume. Separated samples are collected on to a C18 guard column with a mobile phase composed of 90% D2O/10% acetonitrile-D3, and back-flashed to the NMR micro-coil probe with 90% acetonitrile-D3/10% D2O. In order to assess the performance of our unit, we separated a standard mixture of 1 mM ibuprofen, naproxen, and phenylbutazone using a commercially available C18 analytical column. The S/N measurements from the NMR acquisitions indicated that we achieved signal enhancement factors up to 10.4 (±1.2)-fold. Furthermore, we observed that pre-concentration factors increased as the injected amount of analyte decreased. The highest concentration enrichment of 14.7 (±2.2)-fold was attained injecting 100 μL solution of 0.2 mM (~4 μg) ibuprofen. PMID:17037915

Replication fidelity improvement of PMMA microlens array based on weight evaluation and optimization

NASA Astrophysics Data System (ADS)

Jiang, Bing-yan; Shen, Long-jiang; Peng, Hua-jiang; Yin, Xiang-lin

2007-12-01

High replication fidelity is a prerequisite of high quality plastic microlens array in injection molding. But, there's not an economical and practical method to evaluate and improve the replication fidelity until now. Based on part weight evaluation and optimization, this paper presents a new method of replication fidelity improvement. Firstly, a simplified analysis model of PMMA micro columns arrays (5×16) with 200μm diameter was set up. And then, Flow (3D) module of Moldflow MPI6.0 based on Navier-Stokes equations was used to calculate the weight of the micro columns arrays in injection molding. The effects of processing parameters (melt temperature, mold temperature, injection time, packing pressure and packing time) on the part weight were investigated in the simulations. The simulation results showed that the mold temperature and the injection time have important effects on the filling of micro columns; the optimal mold temperature and injection time for better replication fidelity could be determined by the curves of mold temperature vs part weight and injection time vs part weight. At last, the effects of processing parameters on part weight of micro columns array were studied experimentally. The experimental results showed that the increase of melt temperature and mold temperature can make the packing pressure transfer to micro cavity more effectively through runner system, and increase the part weight. From the observation results of the image measuring apparatus, it was discovered that the higher the part weight, the better the filling of the microstructures. In conclusion, part weight can be used to evaluate the replication fidelity of micro-feature structured parts primarily; which is an economical and practical method to improve the replication fidelity of microlens arrays based on weight evaluation and optimization.

Rapid micro-scale proteolysis of proteins for MALDI-MS peptide mapping using immobilized trypsin

NASA Astrophysics Data System (ADS)

Gobom, Johan; Nordhoff, Eckhard; Ekman, Rolf; Roepstorff, Peter

1997-12-01

In this study we present a rapid method for tryptic digestion of proteins using micro-columns with enzyme immobilized on perfusion chromatography media. The performance of the method is exemplified with acyl-CoA-binding protein and reduced carbamidomethylated bovine serum albumin. The method proved to be significantly faster and yielded a better sequence coverage and an improved signal-to-noise ratio for the MALDI-MS peptide maps, compared to in-solution- and on-target digestion. Only a single sample transfer step is required, and therefore sample loss due to adsorption to surfaces is reduced, which is a critical issue when handling low picomole to femtomole amounts of proteins. An example is shown with on-column proteolytic digestion and subsequent elution of the digest into a reversed-phase micro-column. This is useful if the sample contains large amounts of salt or is too diluted for MALDI-MS analysis. Furthermore, by step-wise elution from the reversedphase column, a complex digest can be fractionated, which reduces signal suppression and facilitates data interpretation in the subsequent MS-analysis. The method also proved useful for consecutive digestions with enzymes of different cleavage specificity. This is exemplified with on-column tryptic digestion, followed by reversed-phase step-wise elution, and subsequent on-target V8 protease digestion.

CFD-DEM modeling the effect of column size and bed height on minimum fluidization velocity in micro fluidized beds with Geldart B particles

DOE PAGES

Xu, Yupeng; Li, Tingwen; Musser, Jordan; ...

2017-06-07

The fluidization behavior of Geldart B particles in micro fluidized beds is investigated numerically using Computational Fluid Dynamics coupled with Discrete Element Method (CFD-DEM) available in the open-source Multiphase Flow with Interphase eXchanges (MFIX) code. The effects of different bed inner diameters (D) of 8 mm, 12 mm, 16 mm and various initial static bed heights (H) were examined. It is found that both decreasing the column diameter and increasing the bed height in a micro fluidized bed increases the minimum fluidization velocity (Umf). The observed overshoot in pressure drop that occurs before the onset of fluidization decreases in magnitudemore » with increasing column diameter, however there is less sensitivity to bed height. Overall, the numerical results agree qualitatively with existing theoretical correlations and experimental studies. The simulations show that both column diameter and particle-wall friction contribute to the variation in minimum fluidization velocity. Finally, these two factors are coupled and hard to separate. The detailed influences of wall friction on minimum fluidization velocity are then investigated for a prescribed column diameter of 8 mm by varying the wall friction from 0 to 0.4.« less

CFD-DEM modeling the effect of column size and bed height on minimum fluidization velocity in micro fluidized beds with Geldart B particles

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

Xu, Yupeng; Li, Tingwen; Musser, Jordan

The fluidization behavior of Geldart B particles in micro fluidized beds is investigated numerically using Computational Fluid Dynamics coupled with Discrete Element Method (CFD-DEM) available in the open-source Multiphase Flow with Interphase eXchanges (MFIX) code. The effects of different bed inner diameters (D) of 8 mm, 12 mm, 16 mm and various initial static bed heights (H) were examined. It is found that both decreasing the column diameter and increasing the bed height in a micro fluidized bed increases the minimum fluidization velocity (Umf). The observed overshoot in pressure drop that occurs before the onset of fluidization decreases in magnitudemore » with increasing column diameter, however there is less sensitivity to bed height. Overall, the numerical results agree qualitatively with existing theoretical correlations and experimental studies. The simulations show that both column diameter and particle-wall friction contribute to the variation in minimum fluidization velocity. Finally, these two factors are coupled and hard to separate. The detailed influences of wall friction on minimum fluidization velocity are then investigated for a prescribed column diameter of 8 mm by varying the wall friction from 0 to 0.4.« less

Separation and screening of short-chain chlorinated paraffins in environmental samples using comprehensive two-dimensional gas chromatography with micro electron capture detection.

PubMed

Xia, Dan; Gao, Lirong; Zhu, Shuai; Zheng, Minghui

2014-11-01

Short-chain chlorinated paraffins (SCCPs) are highly complex technical mixtures with thousands of isomers and numerous homologs. They are classified as priority candidate persistent organic pollutants under the Stockholm Convention for their persistence, bioaccumulation, and toxicity. Analyzing SCCPs is challenging because of the complexity of the mixtures. Chromatograms of SCCPs acquired using one-dimensional (1D) gas chromatography (GC) contain a large characteristic "peak" with a broad and unresolved profile. Comprehensive two-dimensional GC (GC×GC) shows excellent potential for separating complex mixtures. In this study, GC×GC coupled with micro electron capture detection (μECD) was used to separate and screen SCCPs. The chromatographic parameters, including the GC column types, oven temperature program, and modulation period, were systematically optimized. The SCCP congeners were separated into groups using a DM-1 column connected to a BPX-50 column. The SCCP congeners in technical mixtures were separated according to the number of chlorine substituents for a given carbon chain length and according to the number of carbon atoms plus chlorine atoms for different carbon chain lengths. A fish tissue sample was analyzed to illustrate the feasibility of the GC×GC-μECD method in analyzing biological samples. Over 1,500 compounds were identified in the fish extract, significantly more than were identified using 1D GC. The detection limits for five selected SCCP congeners were between 1 and 5 pg/L using the GC×GC method, and these were significantly lower than those achieved using 1D GC. This method is a good choice for analysis of SCCPs in environmental samples, exhibiting good separation and good sensitivity.

Microfluidic direct injection method for analysis of urinary 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) using molecularly imprinted polymers coupled on-line with LC-MS/MS.

PubMed

Shah, Kumar A; Peoples, Michael C; Halquist, Matthew S; Rutan, Sarah C; Karnes, H Thomas

2011-01-25

The work described in this paper involves development of a high-throughput on-line microfluidic sample extraction method using capillary micro-columns packed with MIP beads coupled with tandem mass spectrometry for the analysis of urinary NNAL. The method was optimized and matrix effects were evaluated and resolved. The method enabled low sample volume (200 μL) and rapid analysis of urinary NNAL by direct injection onto the microfluidic column packed with molecularly imprinted beads engineered to NNAL. The method was validated according to the FDA bioanalytical method validation guidance. The dynamic range extended from 20.0 to 2500.0 pg/mL with a percent relative error of ±5.9% and a run time of 7.00 min. The lower limit of quantitation was 20.0 pg/mL. The method was used for the analysis of NNAL and NNAL-Gluc concentrations in smokers' urine. Copyright © 2010 Elsevier B.V. All rights reserved.

Small RNA profiling of low biomass samples: identification and removal of contaminants.

PubMed

Heintz-Buschart, Anna; Yusuf, Dilmurat; Kaysen, Anne; Etheridge, Alton; Fritz, Joëlle V; May, Patrick; de Beaufort, Carine; Upadhyaya, Bimal B; Ghosal, Anubrata; Galas, David J; Wilmes, Paul

2018-05-14

Sequencing-based analyses of low-biomass samples are known to be prone to misinterpretation due to the potential presence of contaminating molecules derived from laboratory reagents and environments. DNA contamination has been previously reported, yet contamination with RNA is usually considered to be very unlikely due to its inherent instability. Small RNAs (sRNAs) identified in tissues and bodily fluids, such as blood plasma, have implications for physiology and pathology, and therefore the potential to act as disease biomarkers. Thus, the possibility for RNA contaminants demands careful evaluation. Herein, we report on the presence of small RNA (sRNA) contaminants in widely used microRNA extraction kits and propose an approach for their depletion. We sequenced sRNAs extracted from human plasma samples and detected important levels of non-human (exogenous) sequences whose source could be traced to the microRNA extraction columns through a careful qPCR-based analysis of several laboratory reagents. Furthermore, we also detected the presence of artefactual sequences related to these contaminants in a range of published datasets, thereby arguing in particular for a re-evaluation of reports suggesting the presence of exogenous RNAs of microbial and dietary origin in blood plasma. To avoid artefacts in future experiments, we also devise several protocols for the removal of contaminant RNAs, define minimal amounts of starting material for artefact-free analyses, and confirm the reduction of contaminant levels for identification of bona fide sequences using 'ultra-clean' extraction kits. This is the first report on the presence of RNA molecules as contaminants in RNA extraction kits. The described protocols should be applied in the future to avoid confounding sRNA studies.

Simple gas chromatographic system for analysis of microbial respiratory gases

NASA Technical Reports Server (NTRS)

Carle, G. C.

1972-01-01

Dual column ambient temperature system, consisting of pair of capillary columns, microbead thermistor detector and micro gas-sampling valve, is used in remote life-detection equipment for space experiments. Performance outweighs advantage gained by utilizing single-column systems to reduce weight, conserve carrier gas and operate at lower power levels.

Liquid chromatographic extraction medium

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1994-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

A rapid method based on hot water extraction and liquid chromatography-tandem mass spectrometry for analyzing tetracycline antibiotic residues in cheese.

PubMed

Bogialli, Sara; Coradazzi, Cristina; Di Corcia, Antonio; Lagana, Aldo; Sergi, Manuel

2007-01-01

A rapid, specific, and sensitive procedure for determining residues of 4 widely used tetracycline antibiotics and 3 of their 4-epimers in cheese is presented. The method is based on the matrix solid-phase dispersion (MSPD) technique followed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). After dispersing samples of mozzarella, asiago, parmigiano, gruyere, emmenthal, and camembert on sand, target compounds were eluted from the MSPD column by passing through it 6 mL water heated at 70 degrees C. After acidification and filtration, 200 microL of the aqueous extract was directly injected into the LC column. For analyte identification and quantification, MS data acquisition was performed in the multireaction monitoring mode, selecting 2 precursor ion-to-product ion transitions for each target compound. Hot water appeared to be an efficient extractant, because absolute recoveries were no lower than 78%. Using demeclocycline as a surrogate analyte, recoveries of analyte added to the 6 types of cheeses at the 30 ng/g level were 96-117%, with relative standard deviation (RSD) not higher than 9%. Statistical analysis of the mean recovery data showed that the extraction efficiency was not dependent on the type of cheese analyzed. This result indicates that this method could be applied to other cheese types not considered here. At the lowest concentration considered, i.e., 10 ng/g, the accuracy of the method ranged between 90 and 107%, with RSDs not larger than 12%. Based on a signal-to-noise ratio of 10, limits of quantitation were estimated to be 1-2 ng/g.

Separation and determination of methyl tert-butyl ether and its degradation products by a laboratory-constructed micro-cryogenic chromatographic oven.

PubMed

Liu, Jiemin; Jiang, Guibin; Zhou, Qunfang; Liu, Jingfu; Wen, Meijuan

2003-10-01

A laboratory-made micro-cryogenic chromatographic oven was mainly improved in size, which was controlled at 6 x 6 x 2.5 cm. A thermoelectric system was used to cool the capillary column instead of the traditional liquid cryogen. A cold block connected to the cryogenic module was directly solidified at room temperature with thermally conductive adhesive so that the uniformity of transferring heat was greatly improved, and the size of the system was reduced. Moreover, this system was inexpensive and convenient for both operation and control. The newly developed device coupled with headspace solid-phase microextraction (SPME) was successfully applied to the determination of methyl tert-butyl ether (MTBE) and its degradation products. During the analysis procedure, a 65 microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was used to extract MTBE and its degradation products. The extraction was controlled at 50 degrees C for 30 min and the NaCl content in the sample was maintained at 35%. The limits of detection (LODs) ranged from 0.006 microg mL(-1) (for MTBE) to 0.206 microg mL(-1) (for methyl acetate) and the relative standard deviations (RSD%) were below 4%. The spiked recoveries for the developed method were evaluated using various water samples as a matrix.

Automation of nanoflow liquid chromatography-tandem mass spectrometry for proteome analysis by using a strong cation exchange trap column.

PubMed

Jiang, Xiaogang; Feng, Shun; Tian, Ruijun; Han, Guanghui; Jiang, Xinning; Ye, Mingliang; Zou, Hanfa

2007-02-01

An approach was developed to automate sample introduction for nanoflow LC-MS/MS (microLC-MS/MS) analysis using a strong cation exchange (SCX) trap column. The system consisted of a 100 microm id x 2 cm SCX trap column and a 75 microm id x 12 cm C18 RP analytical column. During the sample loading step, the flow passing through the SCX trap column was directed to waste for loading a large volume of sample at high flow rate. Then the peptides bound on the SCX trap column were eluted onto the RP analytical column by a high salt buffer followed by RP chromatographic separation of the peptides at nanoliter flow rate. It was observed that higher performance of separation could be achieved with the system using SCX trap column than with the system using C18 trap column. The high proteomic coverage using this approach was demonstrated in the analysis of tryptic digest of BSA and yeast cell lysate. In addition, this system was also applied to two-dimensional separation of tryptic digest of human hepatocellular carcinoma cell line SMMC-7721 for large scale proteome analysis. This system was fully automated and required minimum changes on current microLC-MS/MS system. This system represented a promising platform for routine proteome analysis.

A microfluidic chip with a staircase pH gradient generator, a packed column and a fraction collector for chromatofocusing of proteins.

PubMed

Rho, Hoon Suk; Hanke, Alexander Thomas; Ottens, Marcel; Gardeniers, Han J G E

2018-04-01

A microfluidic device for pH gradient chromatofocusing is presented, which performs creation of a micro-column, pH gradient generation, and fraction collection in a single device. Using a sieve micro-valve, anion exchange particles were packed into a microchannel in order to realize a solid-phase absorption column. To fractionate proteins according to their isoelectric points, elution buffer solutions with a stepwise pH gradient were prepared in 16 parallel mixing reactors and flowed through the micro-column, wherein a protein mixture was previously loaded. The volume of the column is only 20 nL, hence it allows extremely low sample consumption and fast analysis compared with a conventional system. We demonstrated separation of two proteins, albumin-fluorescein isothiocyanate conjugate (FITC-BSA) and R-Phycoerythrin (R-PE), by using a microcolumn of commercial charged polymeric particles (Source 15Q). The microfluidic device can be used as a rapid diagnostic tool to analyse crude mixtures of proteins or nucleic acids and determine adsorption/desorption characteristics of various biochemical products, which can be helpful for scientific fundamental understanding as well as instrumental in various industrial applications, especially in early stage screening and process development. © 2018 The Authors Electrophoresis Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Measurement by reversed-phase high-performance liquid chromatography of malondialdehyde in normal human urine following derivatisation with 2,4-dinitrophenylhydrazine.

PubMed

Korchazhkina, Olga; Exley, Christopher; Andrew Spencer, Stephen

2003-09-05

A selective and sensitive method based on derivatisation with 2,4-dinitrophenylhydrazine (DNPH) and consecutive HPLC gradient separation is described for the determination of malondialdehyde (MDA) in urine. Preparation of urine samples involved a one-step derivatisation/extraction procedure. Separation was achieved using a Waters SymmetryC(18) column (3.9 x 150 mm) and linear gradient of acetonitrile in water (from 30% to 70% in 30 min). The overall detection limit of the method was 56 nM of MDA in urine. The recovery of MDA was 94.3+/-8.6%. MDA in urine of healthy volunteers, measured using the method of standard additions, was 0.019+/-0.012 microM/mmol creatinine. MDA in the same samples measured using the 2-thiobarbituric acid (TBA) assay was 0.181+/-0.063 microM/mmol creatinine. We demonstrate that the commonly used TBA assay in conjunction with HPLC may overestimate the MDA concentration in human urine by almost 10-fold.

Transport and Transformation of Selenium and Other Constituents of Flue-Gas Desulfurization Wastewater in Water-Saturated Soil Materials.

PubMed

Galkaduwa, Madhubhashini B; Hettiarachchi, Ganga M; Kluitenberg, Gerard J; Hutchinson, Stacy L; Davis, Lawrence; Erickson, Larry E

2017-03-01

Constructed wetland treatment systems are used to remove selenium (Se) from flue-gas desulfurization (FGD) wastewater (WW). However, direct confirmation of the mechanism responsible for FGD WW Se retention in soil is lacking. A laboratory-based soil column study was performed to develop an evidence-based mechanism of Se retention and to study the behavior and the retention capacity of FGD WW constituents in water-saturated soil. A deoxygenated 1:1 mixture of FGD WW and raw water was delivered to the columns bottom-up at a flux of 1.68 cm d for 100 d. Some of the columns were flushed with the raw water at the same rate for an additional 100 d. Column effluent was analyzed for constituents of concern. Results showed a complete retention of FGD WW Se in the soil materials. Boron and fluorine were partially retained; however, sulfur, sodium, and chlorine retention was poor, agreeing with field observations. The FGD WW Se was retained in soil near the inlet end of the columns, indicating its limited mobility under reduced conditions. Sequential extraction procedure revealed that retained Se was mainly sequestered as stable/residual forms. Bulk- and micro-X-ray absorption near-edge structure spectroscopy confirmed that Se was mainly retained as reduced/stable species [Se(IV), organic Se, and Se(0)]. This study provides direct evidence for FGD WW Se retention in water-saturated soil via the transformation of oxidized Se into reduced/stable forms. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Micro-columns packed with Chlorella vulgaris immobilised on silica gel for mercury speciation.

PubMed

Tajes-Martínez, P; Beceiro-González, E; Muniategui-Lorenzo, S; Prada-Rodríguez, D

2006-02-28

A method has been developed for mercury speciation in water by using columns packed with Chlorella vulgaris immobilised on silica gel. The method involves the retention of CH(3)Hg(+) and Hg(2+) in micro-columns prepared by packing immobilised algae in polypropylene tubes, followed by selective and sequential elution with 0.03 and 1.5M HCl for CH(3)Hg(+) and Hg(2+), respectively. The adsorption capacity of the micro-algae for Hg(2+) and CH(3)Hg(+) has been evaluated using free and immobilised C. vulgaris. The efficiency uptake for both species at pH 3 was higher than 97%. Studies were carried out on the effect of retention and elution conditions for both species. Furthermore, the stability of mercury species retained on algae-silica gel micro-columns and lifetime of the columns were also investigated. Hg(2+) showed a higher stability than CH(3)Hg(+) at 0 degrees C (21 and 3 days, respectively) and a better lifetime than for the organic species. The developed method was applied to the analysis of spiked tap, sea and wastewater samples. Recovery studies on tap and filtered seawater provided results between 96+/-3 and 106+/-2 for Hg(2+) and from 98+/-5 to 107+/-5 for CH(3)Hg(+), for samples spiked with single species. For samples spiked with both CH(3)Hg(+) and Hg(2+), the average recoveries varied from 96+/-5 to 99+/-3 and from 103+/-6 to 115+/-5 for Hg(2+) and CH(3)Hg(+), respectively. However, the percentages of retention and elution on wastewater and unfiltered seawater were only adequate for the inorganic species.

Fudecalone, a new anticoccidial agent produced by Penicillium sp. FO-2030.

PubMed

Tabata, N; Tomoda, H; Masuma, R; Iwai, Y; Omura, S

1995-01-01

Penicillium sp. FO-2030, a soil isolate, was found to produce a new anticoccidial compound. The active compound, designated fudecalone, was isolated from the fermentation broth of the producing strain by solvent extraction, silica gel column chromatography and preparative HPLC. The structure of fudecalone was elucidated to be 3,3a,6,6a,7,8,9,10-octahydro-1-hydroxy-4,7,7-trimethyl-1H-naphtho[1,8a- c]furan-6-one mainly by spectroscopic studies including various NMR measurements. The anticoccidial activity using cell systems indicated that schizont formation of monensin-resistant Eimeria tenella was completely inhibited by fudecalone at concentrations more than 16 microM.

Characterization of Chlorinated Solvent Degradation in a Constructed Wetland

DTIC Science & Technology

2003-03-25

the flows to be different under the same pressure. A 30m Restek RTX- VRX (Model 49314) column was connected to the micro-Electron Capture Detector...min) 2.00 Gas Type: Helium Column 1 (Restek 49314 RTX- VRX ) Column 2 (J&W 113-4332 GS-GASPRO) Max Temp (deg C) 260 Max Temp (deg C

Influence of soil moisture on sunflower oil extraction of polycyclic aromatic hydrocarbons from a manufactured gas plant soil.

PubMed

Gong, Zongqiang; Wilke, B-M; Alef, Kassem; Li, Peijun

2005-05-01

The influence of soil moisture on efficiency of sunflower oil extraction of polycyclic aromatic hydrocarbons (PAHs) from contaminated soil was investigated. The PAH-contaminated soil was collected from a manufactured gas plant (MGP) site in Berlin, Germany. Half of the soil was air-dried, and the other half was kept as field-moist soil. Batch experiments were performed using air-dried and field-moist soils, and sunflower oil was used as extractant at oil/soil ratios of 2:1 and 1:1 (v/m). The experimental data were fitted to a first-order empirical model to describe mass-transfer profiles of the PAHs. Column extraction experiments were also conducted. Field-moist and air-dried soils in the column were extracted using sunflower oil at an oil/soil ratio of 2:1. In the batch experiments, PAHs were more rapidly extracted from air-dried soil than from field-moist soil. Removal rate of total PAH increased 23% at oil/soil ratio of 1:1 and 15.5% at oil/soil ratio of 2:1 after the soil was air dried. The most favorable conditions for batch extraction were air-dried soil, with an oil/soil ratio of 2:1. In the column experiments, the removal rate of total PAH from air-dried soil was 30.7% higher than that from field-moist soil. For field-moist soil, extraction efficiencies of the batch extraction (67.2% and 81.5%) were better than that for column extraction (65.6%). However, this difference between the two methods became less significant for the air-dried soil, with a total removal rate of 96.3% for column extraction and 90.2% and 97% for batch extractions. A mass-balance test was carried out for analytical quality assurance. The results of both batch and column experiments indicated that drying the soil increased efficiency of extraction of PAHs from the MGP soil.

Ultrasonically Modified Amended-Cloud Point Extraction for Simultaneous Pre-Concentration of Neonicotinoid Insecticide Residues.

PubMed

Kachangoon, Rawikan; Vichapong, Jitlada; Burakham, Rodjana; Santaladchaiyakit, Yanawath; Srijaranai, Supalax

2018-05-12

An effective pre-concentration method, namely amended-cloud point extraction (CPE), has been developed for the extraction and pre-concentration of neonicotinoid insecticide residues. The studied analytes including clothianidin, imidacloprid, acetamiprid, thiamethoxam and thiacloprid were chosen as a model compound. The amended-CPE procedure included two cloud point processes. Triton™ X-114 was used to extract neonicotinoid residues into the surfactant-rich phase and then the analytes were transferred into an alkaline solution with the help of ultrasound energy. The extracts were then analyzed by high-performance liquid chromatography (HPLC) coupled with a monolithic column. Several factors influencing the extraction efficiency were studied such as kind and concentration of surfactant, type and content of salts, kind and concentration of back extraction agent, and incubation temperature and time. Enrichment factors (EFs) were found in the range of 20⁻333 folds. The limits of detection of the studied neonicotinoids were in the range of 0.0003⁻0.002 µg mL −1 which are below the maximum residue limits (MRLs) established by the European Union (EU). Good repeatability was obtained with relative standard deviations lower than 1.92% and 4.54% for retention time ( t R ) and peak area, respectively. The developed extraction method was successfully applied for the analysis of water samples. No detectable residues of neonicotinoids in the studied samples were found.

40 CFR 141.40 - Monitoring requirements for unregulated contaminants.

Code of Federal Regulations, 2011 CFR

2011-07-01

... monitoring to be completed Reserved i Reserved i Reserved i Reserved i Reserved i Reserved i Column headings... Pesticides and Flame Retardants in Drinking Water by Solid Phase Extraction and Capillary Column Gas... Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS...

Determination of aflatoxins and ochratoxin A in high-sugar-content traditional Turkish foods by affinity column cleanup and LC fluorescence detection.

PubMed

Senyuva, Hamide Z; Cimen, Dilek; Gilbert, John

2009-01-01

The effectiveness of an affinity column cleanup procedure followed by LC with fluorescence detection was established for the determination of aflatoxins and ochratoxin A in high-sugar-content traditional Turkish foods. Traditional foods, such as baklava (finely layered pastry filled with nuts and steeped in syrup), halvah (containing sesame paste and pistachios), cevizli sucuk (a confection made of grape juice boiled and dried on strings of nuts), Turkish delight (containing hazelnuts, pistachios, or walnuts), and pişmaniye (candy made of sugar, butter, and flour), were tested, and the performance of the method was established with spiked samples. To examine the robustness of the methodology, baklava was prepared from raw materials and spiked at the initial stage of dry ingredients and through subsequent stages of preparation of dough, after cooking, and after addition of syrup and nuts. For all products, the analytical method required grinding the composite foodstuff under liquid nitrogen to form a fine powder, which was then thoroughly mixed before subsampling. After vortex extraction into methanol-water (aflatoxins) and aqueous sodium bicarbonate (ochratoxin A), the sample was filtered, diluted with phosphate-buffered saline, and then passed through either an aflatoxin or ochratoxin A affinity column before HPLC analysis with fluorescence detection (using post-column bromination for the aflatoxins). In all the traditional Turkish products, the recovery of aflatoxin B1 ranged from 77 to 98%, and LODs were <0.1 microg/kg. For ochratoxin A, the recoveries were from 88 to 93% and LODs were similarly <0.1 microLg/kg. Despite the complex nature of these traditional Turkish foods, which frequently contain products from sugar caramelization, there was no evidence of any interfering co-extractives, and the method has proved to be robust enough to be used for food control purposes.

Liquid chromatographic extraction medium

DOEpatents

Horwitz, E.P.; Dietz, M.L.

1994-09-13

A method and apparatus are disclosed for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water. 1 fig.

[Study on preparation of composite nano-scale Fe3O4 for phosphorus control].

PubMed

Li, Lei; Pan, Gang; Chen, Hao

2010-03-01

Composite nano-scale Fe3O4 particles were prepared in sodium carboxymethyl cellulose (CMC) solution by the oxidation deposition method. The adsorptions of phosphorus by micro-scale Fe3O4 and composite nano-scale Fe3O4 were investigated in water and soil, and the role of cellulase in the adsorption of composite nano-scale Fe3O4 was studied. Kinetic tests indicated that the equilibrium adsorption capacity of phosphorous on the composite nano-scale Fe3O4 (2.1 mg/g) was less than that of micro-scale Fe3O4 (3.2 mg/g). When cellulase was added to the solution of composite nano-scale Fe3O4 to degrade CMC, the removal rate of P by the nanoparticles (86%) was enhanced to the same level as the microparticles (90%). In the column tests, when the composite nano-scale Fe3O4 suspension was introduced in the downflow mode through the soil column, 72% of Fe3O4 penetrated through the soil bed under gravity. In contrast, the micro-scale Fe3O4 failed to pass through the soil column. The retention rate of P was 45% in the soil column when treated by the CMC-stabilized nanoparticles, in comparison with only 30% for the untreated soil column, however it could be improved to 74% in the soil column when treated by both the CMC-stabilized nanoparticles and cellulase, which degraded CMC after the nanoparticles were delivered into the soil.

Void fraction, bubble size and interfacial area measurements in co-current downflow bubble column reactor with microbubble dispersion

DOE PAGES

Hernandez-Alvarado, Freddy; Kalaga, Dinesh V.; Turney, Damon; ...

2017-05-06

Micro-bubbles dispersed in bubble column reactors have received great interest in recent years, due to their small size, stability, high gas-liquid interfacial area concentrations and longer residence times. The high gas-liquid interfacial area concentrations lead to high mass transfer rates compared to conventional bubble column reactors. In the present work, experiments have been performed in a down-flow bubble column reactor with micro-bubbles generated and dispersed by a novel mechanism to determine the gas-liquid interfacial area concentrations by measuring the void fraction and bubble size distributions. Gamma-ray densitometry has been employed to determine the axial and radial distributions of void fractionmore » and a high speed camera equipped with a borescope is used to measure the axial and radial variations of bubble sizes. Also, the effects of superficial gas and liquid velocities on the two-phase flow characteristics have been investigated. Further, reconstruction techniques of the radial void fraction profiles from the gamma densitometry's chordal measurements are discussed and compared for a bubble column reactor with dispersed micro-bubbles. The results demonstrate that the new bubble generation technique offers high interfacial area concentrations (1,000 to 4,500 m 2/m 3) with sub-millimeter bubbles (500 to 900 µm) and high overall void fractions (10% – 60%) in comparison with previous bubble column reactor designs. The void fraction data was analyzed using slip velocity model and empirical correlation has been proposed to predict the Sauter mean bubble diameter.« less

Void fraction, bubble size and interfacial area measurements in co-current downflow bubble column reactor with microbubble dispersion

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

Hernandez-Alvarado, Freddy; Kalaga, Dinesh V.; Turney, Damon

Micro-bubbles dispersed in bubble column reactors have received great interest in recent years, due to their small size, stability, high gas-liquid interfacial area concentrations and longer residence times. The high gas-liquid interfacial area concentrations lead to high mass transfer rates compared to conventional bubble column reactors. In the present work, experiments have been performed in a down-flow bubble column reactor with micro-bubbles generated and dispersed by a novel mechanism to determine the gas-liquid interfacial area concentrations by measuring the void fraction and bubble size distributions. Gamma-ray densitometry has been employed to determine the axial and radial distributions of void fractionmore » and a high speed camera equipped with a borescope is used to measure the axial and radial variations of bubble sizes. Also, the effects of superficial gas and liquid velocities on the two-phase flow characteristics have been investigated. Further, reconstruction techniques of the radial void fraction profiles from the gamma densitometry's chordal measurements are discussed and compared for a bubble column reactor with dispersed micro-bubbles. The results demonstrate that the new bubble generation technique offers high interfacial area concentrations (1,000 to 4,500 m 2/m 3) with sub-millimeter bubbles (500 to 900 µm) and high overall void fractions (10% – 60%) in comparison with previous bubble column reactor designs. The void fraction data was analyzed using slip velocity model and empirical correlation has been proposed to predict the Sauter mean bubble diameter.« less

Genotoxicity of mercury used in chromosome aberration tests.

PubMed

Akiyama, M; Oshima, H; Nakamura, M

2001-01-01

The purpose of this study was to investigate the genotoxic effects of Hg released from dental amalgams. The chromosome aberration test was conducted using original extracts and their diluted solutions of conventional type amalgam and high copper amalgam. The concentrations of Hg, Cu and Ag in the original extract of high copper amalgam were 17.64, 7.97 and 43.90 microM, respectively. Those in the original extract of conventional type amalgam were 20.63, 7.87 and 14.79 microM, respectively. 10 and 30 microM Hg(2+) were also used for comparison. The frequency of chromosome aberrations was below 5% with 0 microM Hg(2+) and with a triple dilution of high copper amalgam extract, containing 5.88 microM Hg, 14.63 microM Cu and 2.65 microM Ag. However, 9.5% of the cells showed chromosome aberrations with a quadruple dilution of conventional type amalgam, containing 5.15 microM Hg, 3.69 microM Cu and 1.96 microM Ag. The amount of Hg in the quadruple dilution of conventional type amalgam was less than that in the triple dilution of high copper amalgam extract and 10 microM Hg(2+). A concentration of 30 microM Hg(2+) caused 34.5% of the cells to show chromosome aberrations while with a two-thirds dilution of high copper amalgam extract, containing 11.76 microM Hg, 29.26 microM Cu and 5.31 microM Ag, 58.5% of the cells showed chromosome aberrations. A two-thirds dilution of high copper amalgam extract induced more chromosome aberrations than 30 microM Hg(2+), although the amount of Hg was less than 30 microM Hg(2+). A triple dilution of conventional type amalgam extract, original extracts of conventional type amalgam and high copper amalgam and 100 microM Hg(2+) were induced few metaphases. It was revealed that the conventional type amalgam induced chromosome aberrations with quadruple dilution where cell viability was about 80% and that the high copper amalgam induced a high level of chromosome aberrations with the two-thirds dilution. The effects of low level Hg on humans are not clear.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Zaugg, Steven D.; Sandstrom, Mark W.; Smith, Steven G.; Fehlberg, Kevin M.

1995-01-01

A method for the isolation of 41 pesticides and pesticide metabolites in natural-water samples using C-18 solid-phase extraction and determination by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction columns containing octadecyl-bonded porous silica to extract the pesticides. The columns are dried using carbon dioxide or nitrogen gas, and adsorbed pesticides are removed from the columns by elution with 3.0 milliliters of hexane-isopropanol (3:1). Extracted pesticides are determined by capillary- column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 4 micrograms per liter (g/L) for most pesticides, with the exception of widely used corn herbicides--atrazine, alachlor, cyanazine, and metolachlor--which have upper concentration limits of 20 g/L. Single- operator method detection limits in reagent-water samples range from 0.001 to 0.018 g/L. Average short-term single-operator precision in reagent- water samples is 7 percent at the 0.1- and 1.0-g/L levels and 8 percent at the 0.01-g/L level. Mean recoveries in reagent-water samples are 73 percent at the 0.1- and 1.0-g/L levels and 83 percent at the 0.01-g/L level. The estimated holding time for pesticides after extraction on the solid-phase extraction columns was 7 days. 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.

High performance liquid chromatographic method for the determination of cetirizine and ambroxol in human plasma and urine--a boxcar approach.

PubMed

Dharuman, J; Vasudhevan, M; Ajithlal, T

2011-09-01

A column switching high performance liquid chromatographic method with estimable sensitivity and accuracy was developed for the determination of cetirizine and ambroxol in human plasma using nebivolol as the internal standard. Plasma samples were prepared by liquid-liquid extraction in methylene chloride and a mixture of diethylether (80:20, v/v). The extracted samples were injected into a multifunctional clean-up column Supelcosil LCABZ (50 mm × 4.6 mm, 5 μm particle size) using mobile phase 1 comprising acetonitrile-phosphate buffer (pH 3.5; 20 mM) (20:80, v/v). The eluate of cetirizine and ambroxol were separated to an analytical Kromasil C(8) micro bore column (50 mm × 0.3 mm, 5 μm particle size) via a column switching device. A Kromasil C(18) analytical column (250 mm × 2.1 mm, 5 μm particle size) was used as a separation column. Mobile phase 2 consisting acetonitrile-triethylamine (0.5%) in phosphate buffer (pH 3.5; 20mM) (55:45, v/v) was used for the compound elution. The eluents were detected at 230 nm with photodiode array detector. An aliquot of 150 μl of plasma sample was introduced into the pretreatment column via the auto sampler using mobile phase 1 at a flow rate of 0.5 ml/min, column switching valve being positioned at A. The pretreatment column retained cetirizine, ambroxol and nebivolol (IS) in the column leaving the residual proteins of plasma eluted in void volume and drained out. The switching valve was shifted to position B at 7.5 min. Cetirizine, ambroxol and IS were eluted from the pretreatment column between 7. 5 and 11.5 min and introduced to the concentration column. Finally, cetirizine, ambroxol and IS were introduced to the separation column by switching valve using mobile phase 2 at a flow rate of 0.4 ml/min. During the analysis the pretreatment column was washed for the next analysis and resume to the position A. The total run time was 25 min for a sample. The procedure was repeated for urine analysis also. The method was linear from 2 to 450 ng/ml and 7-300 ng/ml for cetirizine and ambroxol respectively in plasma and 1-500 ng/ml and 5-400 ng/ml, respectively for cetirizine and ambroxol in urine. Intra-day and inter-day precision of cetirizine and ambroxol was below 15% in terms of coefficient of variation and accuracy of cetirizine and ambroxol was ranged from 94 to 101.6% and 91.1 to 100.2%, respectively. The method demonstrated high sensitivity and selectivity and therefore, applied to evaluate pharmacokinetics of cetirizine and ambroxol in healthy human volunteer after a single oral administration. Urine samples obtained from healthy human volunteers and clinical subjects with renal impairment have also been analyzed by the method to compare the elimination pattern. The method was precise and accurate for the estimation of cetirizine and ambroxol both in blood and in urine. Copyright © 2011 Elsevier B.V. All rights reserved.

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

Surface micro-structuring of silicon by excimer-laser irradiation in reactive atmospheres

NASA Astrophysics Data System (ADS)

Pedraza, A. J.; Fowlkes, J. D.; Jesse, S.; Mao, C.; Lowndes, D. H.

2000-12-01

The formation mechanisms of cones and columns by pulsed-laser irradiation in reactive atmospheres were studied using scanning electron microscopy and profilometry. Deep etching takes place in SF6- and O2- rich atmospheres and consequently, silicon-containing molecules and clusters are released. Transport of silicon from the etched/ablated regions to the tip of columns and cones and to the side of the cones is required because both structures, columns and cones, protrude above the initial surface. The laser-induced micro-structure is influenced not only by the nature but also by the partial pressure of the reactive gas in the atmosphere. Irradiation in Ar following cone formation in SF6 produced no additional growth but rather melting and resolidification. Subsequent irradiation using again a SF6 atmosphere lead to cone restructuring and growth resumption. Thus the effects of etching plus re-deposition that produce column/cone formation and growth are clearly separated from the effects of just melting. On the other hand, irradiation continued in air after first performed in SF6 resulted in: (a) an intense etching of the cones and a tendency to transform them into columns; (b) growth of new columns on top of the existing cones and (c) filamentary nano-structures coating the sides of the columns and cones.

Characterization of peak capacity of microbore liquid chromatography columns using gradient kinetic plots.

PubMed

Hetzel, Terence; Blaesing, Christina; Jaeger, Martin; Teutenberg, Thorsten; Schmidt, Torsten C

2017-02-17

The performance of micro-liquid chromatography columns with an inner diameter of 0.3mm was investigated on a dedicated micro-LC system for gradient elution. Core-shell as well as fully porous particle packed columns were compared on the basis of peak capacity and gradient kinetic plot limits. The results for peak capacity showed the superior performance of columns packed with sub-2μm fully porous particles compared to 3.0μm fully porous and 2.7μm core-shell particles within a range of different gradient time to column void time ratios. For ultra-fast chromatography a maximum peak capacity of 16 can be obtained using a 30s gradient for the sub-2μm fully porous particle packed column. A maximum peak capacity of 121 can be achieved using a 5min gradient. In addition, the influence of an alternative detector cell on the basis of optical waveguide technology and contributing less to system variance was investigated showing an increased peak capacity for all applied gradient time/column void time ratios. Finally, the influence of pressure was evaluated indicating increased peak capacity for maximum performance whereas a limited benefit for ultra-fast chromatography with gradient times below 30s was observed. Copyright © 2017 Elsevier B.V. All rights reserved.

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2010 CFR

2010-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

On-line solid phase extraction coupled to capillary LC-ESI-MS for determination of fluoxetine in human blood plasma.

PubMed

Saber, Amr L

2009-04-15

An instrumental setup including on-line solid phased extraction coupled to capillary liquid chromatography-electrospray ionization-mass spectrometry (SPE-capLC-ESI-MS) has been constructed to improve the sensitivity for quantification of fluoxetine hydrochloride in human plasma. Prior to injection, 0.5 mL of plasma spiked with metronidazole (internal standard) was mixed with ammonium formate buffer for effective chloroform liquid-liquid extraction. The method was validated in the range 5-60 ng mL(-1) fluoxetine, yielding a correlation coefficient of 0.999 (r(2)). The within-assay and between-assay precisions were between (8.5 and 11%) and (6.6 and 7.5%), respectively. The method was used to determine the amount of fluoxetine in a healthy male 14 h after an intake of one capsule of the antidepressant and anorectic Flutin, which contains 20mg fluoxetine per each capsule. Fluoxetine was detected, and the concentration was calculated to 9.0 ng mL(-1) plasma. In the preliminary experiments, conventional LC-UV instrumentation was employed. However, it was found that employing a capillary column with an inner diameter of (0.3mm I.D. x 50 mm, Zorbax C(18)) increased the sensitivity by a factor of approximately 100, when injecting the same mass of analyte. Incorporating an easily automated C(18) reversed phase column switching system with SPE (1.0mm I.D. x 5.0mm, 5 microm) made it possible to inject up to 100 microL of solution, and the total analysis time was 5.5 min.

Molecularly imprinted polymers as the extracted sorbents of clenbuterol ahead of liquid chromatographic determination*

PubMed Central

Lay, Sovichea; Yu, Hai-ning; Hu, Bao-xiang; Shen, Sheng-rong

2016-01-01

A pre-treatment methodology for clenbuterol hydrochloride (CLEN) isolation and enrichment in a complex matrix environment was developed through exploiting molecularly imprinted polymers (MIPs). CLEN-imprinted polymers were synthesized by the combined use of ally-β-cyclodextrin (ally-β-CD) and methacrylic acid (MAA), allyl-β-CD and acrylonitrile (AN), and allyl-β-CD and methyl methacrylate (MMA) as the binary functional monomers. MAA-linked allyl-β-CD MIPs (M-MAA) were characterized by Fourier transform-infrared (FT-IR) spectroscopy and a scanning electron microscope (SEM). Based upon the results, M-MAA polymers generally proved to be an excellent selective extraction compared to its references: AN-linked allyl-β-CD MIPs (M-AN) and MMA-linked allyl-β-CD MIPs (M-MMA). M-MAA polymers were eventually chosen to run through a molecularly imprinted solid-phase extraction (MISPE) micro-column to enrich CLEN residues spiked in pig livers. A high recovery was achieved, ranging from 91.03% to 96.76% with relative standard deviation (RSD) ≤4.45%. PMID:27256680

High-performance liquid chromatography-mass spectrometry-based acetylcholinesterase assay for the screening of inhibitors in natural extracts.

PubMed

de Jong, Camiel F; Derks, Rico J E; Bruyneel, Ben; Niessen, Wilfried; Irth, Hubertus

2006-04-21

The present paper describes a High-performance liquid chromatography-mass spectrometry (LC-MS) methodology for the screening of acetylcholinesterase (AChE) inhibitors in natural extracts. AChE activity of sample components is monitored by a post-column biochemical assay that is based on the separate, sequential mixing of AChE and acetylcholine, respectively, with the HPLC eluate. AChE inhibitors are detected by measuring a decrease of product formation using electrospray MS. Ammonium bicarbonate was used as buffer in order to achieve optimum compatibility between biochemical assay and MS detection conditions. The assay is robust and stable for over 13 h and compares favourably with other AChE assays in terms of stability and sensitivity. IC(50) values of 9-aminoacridine, galanthamine, gallamine, (-)-huperzine A and thioflavin T were determined to be 0.12, 0.38, 6.4, 0.46 and 3.2 microM, respectively. The assay was used to effectively identify an AChE inhibitor present in a crude extract of Narcissus c.v. "Bridal Crown".

Repetitive Regeneration of Media #1 in a Dynamic Column Extraction using Brine #1

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

Gary Garland

This data is from a regeneration study from a dynamic column extraction experiment where we ran a solution of REE's through a column of media #1 then stripped the REE's off the media using 2M HNO3 solution. We then re-equilibrated the media and repeated the process of running a REE solution through the column and stripping the REE's off the media and comparing the two runs.

Study on the extraction and purification of glycoprotein from the yellow seahorse, Hippocampus kuda Bleeker

PubMed Central

Su, Yuting; Xu, Yongjian

2015-01-01

The optimum parameters of extraction for glycoprotein from seahorse were examined and determined by Box-Behnken combined with ultrasonic extraction technology. Column chromatography of glycoprotein was used for further purification. The optimal extraction conditions of seahorse glycoprotein were extracting time 4.3 h, salt concentration 0.08 mol/L, extracting temperature 73°C, raw material, and water ratio 1:6. At the optimal conditions, the yield of saccharide reached to 1.123%, and the yield of protein reached to 5.898%. For purifying the crude glycoprotein, the stage renounces of DEAE-52 column chromatography were done, respectively, with 0.05, 0.1, 0.5 mol/L NaHCO3 solution, and further purification was done with Sephadex G-100 column chromatography. Finally, two pieces of seahorse glycoprotein were obtained by the column chromatography, that is, HG-11 and HG-21. The saccharide content was 56.7975% and 39.479%, the protein content was 30.5475% and 51.747%, respectively. PMID:26288722

Survey of simulation methods for modeling pulsed sieve-plate extraction columns

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

Burkhart, L.

1979-03-01

The report first considers briefly the use of liquid-liquid extraction in nuclear fuel reprocessing and then describes the operation of the pulse column. Currently available simulation models of the column are reviewed, and followed by an analysis of the information presently available from which the necessary parameters can be obtained for use in a model of the column. Finally, overall conclusions are given regarding the information needed to develop an accurate model of the column for materials accountability in fuel reprocessing plants. 156 references.

Factorial-design optimization of gas chromatographic analysis of tetrabrominated to decabrominated diphenyl ethers. Application to domestic dust.

PubMed

Regueiro, Jorge; Llompart, Maria; Garcia-Jares, Carmen; Cela, Rafael

2007-07-01

Gas chromatographic analysis of polybrominated diphenyl ethers (PBDEs) has been evaluated in an attempt to achieve better control of the separation process, especially for highly substituted congeners. Use of a narrow-bore capillary column enabled adequate determination of tetra, penta, hexa, hepta, octa, nona and decaBDE congeners in only one chromatographic run while maintaining resolution power similar to that of conventional columns. A micro electron-capture detector (GC-microECD) was used. Chromatographic conditions were optimized by multifactorial experimental design, with the objective of obtaining not only high sensitivity but also good precision. In this way two different approaches to maximizing response and minimizing variability were tested, and are fully discussed. These optimum chromatographic conditions were then used to determine PBDEs extracted from domestic dust samples by microwave-assisted solvent extraction (MASE). Quantitative recovery (90-108%) was achieved for all the PBDEs and method precision (RSD < 13%) was satisfactory. Accuracy was tested by use of the standard reference material SRM 2585, and sub-ng g(-1) limits of detection were obtained for all compounds except BDE-209 (1.44 ng g(-1)). Finally, several samples of house dust were analysed by use of the proposed method and all the target PBDEs were detected in all the samples. BDE-209 was the predominant congener. Amounts varied from 58 to 1615 ng g(-1) and the average contribution to the total PBDE burden of 52%. The main congeners of the octaBDE mixture (BDE-183, BDE-197, BDE-207 and BDE-196) also made an important contribution (29%) to the total. These are the first data about the presence of these compounds in European house-dust samples. Finally, the sum of the main congeners in the pentaBDE commercial mixture (BDE-47, BDE-99, and BDE-100) contributed 14% to the total. Figure Polybrominated diphenyl ethers in House Dust.

Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.

PubMed

Nonaka, Y; Saito, K; Hanioka, N; Narimatsu, S; Kataoka, H

2009-05-15

A simple and sensitive automated method for determination of aflatoxins (B1, B2, G1, and G2) in nuts, cereals, dried fruits, and spices was developed consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Aflatoxins were separated within 8 min by high-performance liquid chromatography using a Zorbax Eclipse XDB-C8 column with methanol/acetonitrile (60/40, v/v): 5mM ammonium formate (45:55) as the mobile phase. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of aflatoxins. The pseudo-molecular ions [M+H](+) were used to detect aflatoxins in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25draw/eject cycles of 40 microL of sample using a Supel-Q PLOT capillary column as an extraction device. The extracted aflatoxins were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r>0.9994) was obtained in the concentration range of 0.05-2.0 ng/mL using aflatoxin M1 as an internal standard, and the detection limits (S/N=3) of aflatoxins were 2.1-2.8 pg/mL. The in-tube SPME method showed >23-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) at the concentration of 1 ng/mL aflatoxin mixture were below 3.3% and 7.7% (n=5), respectively. This method was applied successfully to analysis of food samples without interference peaks. The recoveries of aflatoxins spiked into nuts and cereals were >80%, and the relative standard deviations were <11.2%. Aflatoxins were detected at <10 ng/g in several commercial food samples.

Analysis of honeybush tea (Cyclopia spp.) volatiles by comprehensive two-dimensional gas chromatography using a single-stage thermal modulator.

PubMed

Ntlhokwe, Gaalebalwe; Tredoux, Andreas G J; Górecki, Tadeusz; Edwards, Matthew; Vestner, Jochen; Muller, Magdalena; Erasmus, Lené; Joubert, Elizabeth; Christel Cronje, J; de Villiers, André

2017-07-01

The applicability of comprehensive two-dimensional gas chromatography (GC×GC) using a single-stage thermal modulator was explored for the analysis of honeybush tea (Cyclopia spp.) volatile compounds. Headspace solid phase micro-extraction (HS-SPME) was used in combination with GC×GC separation on a non-polar × polar column set with flame ionisation (FID) detection for the analysis of fermented Cyclopia maculata, Cyclopia subternata and Cyclopia genistoides tea infusions of a single harvest season. Method optimisation entailed evaluation of the effects of several experimental parameters on the performance of the modulator, the choice of columns in both dimensions, as well as the HS-SPME extraction fibre. Eighty-four volatile compounds were identified by co-injection of reference standards. Principal component analysis (PCA) showed clear differentiation between the species based on their volatile profiles. Due to the highly reproducible separations obtained using the single-stage thermal modulator, multivariate data analysis was simplified. The results demonstrate both the complexity of honeybush volatile profiles and the potential of GC×GC separation in combination with suitable data analysis techniques for the investigation of the relationship between sensory properties and volatile composition of these products. The developed method therefore offers a fast and inexpensive methodology for the profiling of honeybush tea volatiles. Graphical abstract Surface plot obtained for the GC×GC-FID analysis of honeybush tea volatiles.

[Determination of ten photoinitiators in fruit juices and tea beverages by solid-phase micro-extraction coupled with gas chromatography/mass spectrometry].

PubMed

Liu, Pengyan; Chen, Yanjie; Zhao, Chunxia; Tian, Lei

2013-12-01

A method for the determination of ten photoinitiators (PIs), benzophenone, ethyl 4-dimethylaminobenzoate, 1-hydroxycyclohexyl-phenylketone, 4-methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 4-chlorobenzophenone, 2-chlorothioxanthone, 2-isopropylthio-xanthone, 2,2-dimethoxy-2-phenylacetophenone, methyl 2-benzoylbenzoate, in 13 kinds of fruit juice and 3 kinds of tea beverage has been established, using solid-phase micro-extraction (SPME) combined with chromatography/mass spectrometry (GC/MS). At first, the major factors of SPME, extraction time and temperature, were studied through orthogonal experiment. Then the optimal operation conditions were obtained via the refinement of various factors. After the sample was extracted by SPME, it was desorbed for target analytes in sampling inlet for 3 min, and separated on an HP-5MS column, then detected by MS in selected ion monitoring mode, and quantified through calibration curve. The working curves were obtained using sample matrix in order to eliminate the matrix interference. The linear range was from 0.3 microg/L to 60 microg/L and the detection limit range was from 3 ng/L to 16 ng/L. The samples were determined five times with four different spiked levels individually and the relative standard deviations of all the samples were less than 14.5%. This determination method was applied in 16 kinds of packed beverages with different brands and different species. Benzophenone had been detected from all the samples. 4-Methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 2-isopropylthioxanthone, 1-hydroxycyclohexyl-phenylketone and 2-chlorothioxanthone had been detected from a portion of samples. Simultaneous determination was achieved for the ten PIs. These results provide a reference to determine the PIs migrated from packing materials in beverage. This method is simple, high sensitive and non-polluting.

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review.

PubMed

Rahman, Md Musfiqur; Abd El-Aty, A M; Kim, Sung-Woo; Shin, Sung Chul; Shin, Ho-Chul; Shim, Jae-Han

2017-01-01

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

REDISTRIBUTOR FOR LIQUID-LIQUID EXTRACTION COLUMNS

DOEpatents

Bradley, J.G.

1957-10-29

An improved baffle plate construction to intimately mix immiscible liquid solvents for solvent extraction processes in a liquid-liquid pulse column is described. To prevent the light and heavy liquids from forming separate continuous homogeneous vertical channels through sections of the column, a baffle having radially placed rectangular louvers with deflection plates opening upon alternate sides of the baffle is placed in the column, normal to the axis. This improvement substantially completely reduces strippiig losses due to poor mixing.

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2011 CFR

2011-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... UF4 to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

The setup of an extraction system coupled to a hydrogen isotopes distillation column

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

Zamfirache, M.; Bornea, A.; Stefanescu, I.

2008-07-15

Among the most difficult problems of cryogenic distillation one stands apart: the extraction of the heavy fraction. By an optimal design of the cycle scheme, this problem could be avoided. A 'worst case scenario' is usually occurring when the extracted fraction consists of one prevalent isotope such as hydrogen and small amounts of the other two hydrogen isotopes (deuterium and/or tritium). This situation is further complicated by two parameters of the distillation column: the extraction flow rate and the hold-up. The present work proposes the conceptual design of an extraction system associated to the cryogenic distillation column used in hydrogenmore » separation processes. During this process, the heavy fraction (DT, T{sub 2}) is separated, its concentration being the highest at the bottom of the distillation column. From this place the extraction of the gaseous phase can now begin. Being filled with adsorbent, the extraction system is used to temporarily store the heavy fraction. Also the extraction system provides samples for the gas Chromatograph. The research work is focused on the existent pilot plant for tritium and deuterium separation from our institute to validate the experiments carried out until now. (authors)« less

On-Line 1D and 2D PLOT/LC-ESI-MS Using 10 μm i.d. Poly(styrene–divinylbenzene) Porous Layer Open Tubular (PLOT) Columns For Ultrasensitive Proteomic Analysis

PubMed Central

Luo, Quanzhou; Yue, Guihua; Valaskovic, Gary A; Gu, Ye; Wu, Shiaw-Lin; Karger, Barry L.

2008-01-01

Following on our recent work, on-line one dimensional (1D) and two dimensional (2D) PLOT/LC-ESI-MS platforms using 3.2 m × 10 μm i.d. poly(styrenedivinylbenzene) (PS-DVB) porous layer open tubular (PLOT) columns have been developed to provide robust, high performance and ultrasensitive proteomic analysis. Using a PicoClear tee, the dead volume connection between a 50 μm i.d. PS-DVB monolithic microSPE column and the PLOT column was minimized. The microSPE/PLOT column assembly provided a separation performance similar to that obtained with direct injection onto the PLOT column at a mobile phase flow rate of 20 nL/min. The trace analysis potential of the platform was evaluated using an in-gel tryptic digest sample of a gel fraction (15 to 40 kDa) of a cervical cancer (SiHa) cell line. As an example of the sensitivity of the system, ∼2.5 ng of protein in 2 μL solution, an amount corresponding to 20 SiHa cells, was subjected to on-line microSPE-PLOT/LC-ESIMS/MS analysis using a linear ion trap MS. 237 peptides associated with 163 unique proteins were identified from a single analysis when using stringent criteria associated with a false positive rate less than 1% . The number of identified peptides and proteins increased to 638 and 343, respectively, as the injection amount was raised to ∼45 ng of protein, an amount corresponding to 350 SiHa cells. In comparison, only 338 peptides and 231 unique proteins were identified (false positive rate again less than 1%) from 750 ng of protein from the identical gel fraction, an amount corresponding to 6000 SiHa cells, using a typical 15 cm × 75 μm i.d. packed capillary column. The greater sensitivity, higher recovery, and higher resolving power of the PLOT column resulted in the increased number of identifications from only ∼5% of the injected sample amount. The resolving power of the microSPE/PLOT assembly was further extended by 2D chromatography via combination of the high-efficiency reversed phase PLOT column with strong cation exchange chromatography (SCX). As an example, 1071 peptides associated with 536 unique proteins were identified from 75 ng of protein from the same gel fraction, an amount corresponding to 600 cells, using 5 ion exchange fractions in online 2D SCX-PLOT/LC-MS. The 2D system, implemented in an automated format, led to simple and robust operation for proteomic analysis. These promising results demonstrate the potential of the PLOT column for ultratrace analysis. PMID:17625912

Application of EDTA decontamination on soils affected by mining activities and impact of treatment on the geochemical partition of metal contaminants.

PubMed

Xia, Wenbin; Gao, Hui; Wang, Xianhai; Zhou, Chunhua; Liu, Yunguo; Fan, Ting; Wang, Xin

2009-05-30

Two soil samples were collected at mining areas located in southern Hunan Province, China. EDTA extraction of Pb, Zn, Cu and Cd from these two tailing soils was studied using column leaching experiments. The redistributions of heavy metals (HMs) were determined using the modified BCR (Community Bureau of Reference) sequential extraction procedure, before and after EDTA extraction. The results indicated that EDTA was an effective extractant because of its strong chelating ability for various HMs. The proportions of Pb, Zn, Cu and Cd in the four fractions varied largely after EDTA extraction. The extraction efficiency of EDTA of the acid-extractable fraction (AEX) was significant in shallow soil column, while in deeper soil column, decrease of the extraction efficiency of reduced (RED), oxidizable (OX) and residual fractions (RES) was obtained, which was mainly due to the decrease of EDTA concentration.

Determination of phenoxyacid herbicides and their phenolic metabolites in surface and drinking water.

PubMed

Marchese, Stefano; Perret, Daniela; Gentili, Alessandra; D'Ascenzo, Guiseppe; Faberi, Angelo

2002-01-01

An evaluation was made of the feasibility of using reversed-phase liquid chromatography/tandem mass spectrometry with an electrospray interface (LC/ESI-MS/MS) to measure traces of phenoxyacid herbicides and their metabolites in surface and drinking water samples. The procedure involved passing 0.5 L of river and drinking water samples through a 0.5 g graphitized carbon black (GCB) extraction cartridge. Recovery was higher than 85% irrespective of the aqueous matrix in which the analytes were dissolved. A conventional 4.6-mm i.d. reversed-phase LC C-18 column operating with a mobile phase flow rate of 1 mL/min was used to chromatograph the analytes. A flow of 200 microL/min of the column effluent was diverted to the ESI source. The limits of detection (signal-to-noise ratio = 3) of the method for the pesticides considered in drinking and surface water samples are less than 0.1 ng/L for phenoxyacid herbicides, and about 5-10 ng/L for their metabolites (2,4-dichlorophenol and 4-chloro-2-methylphenol). Copyright 2001 John Wiley & Sons, Ltd.

Microscale depletion of high abundance proteins in human biofluids using IgY14 immunoaffinity resin: Analysis of human plasma and cerebrospinal fluid

DOE PAGES

Hyung, Seok Won; Piehowski, Paul D.; Moore, Ronald J.; ...

2014-09-06

Removal of highly abundant proteins in plasma is often carried out using immunoaffinity depletion to extend the dynamic range of measurements to lower abundance species. While commercial depletion columns are available for this purpose, they generally are not applicable to limited sample quantities (<20 µL) due to low yields stemming from losses caused by nonspecific binding to the column matrix. Additionally, the cost of the depletion media can be prohibitive for larger scale studies. Modern LC-MS instrumentation provides the sensitivity necessary to scale-down depletion methods with minimal sacrifice to proteome coverage, which makes smaller volume depletion columns desirable for maximizingmore » sample recovery when samples are limited, as well as for reducing the expense of large scale studies. We characterized the performance of a 346 µL column volume micro-scale depletion system, using four different flow rates to determine the most effective depletion conditions for ~6 μL injections of human plasma proteins and then evaluated depletion reproducibility at the optimum flow rate condition. Depletion of plasma using a commercial 10 mL depletion column served as the control. Results showed depletion efficiency of the micro-scale column increased as flow rate decreased, and that our micro-depletion was reproducible. We found, in an initial application, a 600 µL sample of human cerebral spinal fluid (CSF) pooled from multiple sclerosis patients was depleted and then analyzed using reversed phase liquid chromatography-mass spectrometry to demonstrate the utility of the system for this important biofluid where sample quantities are more commonly limited.« less

Separation of actinides using capillary extraction chromatography-inductively coupled plasma mass spectrometry.

PubMed

Peterson, Dominic S; Montoya, Velma M

2009-08-01

Trace levels of actinides have been separated on capillary extraction chromatography columns. Detection of the actinides was achieved using an inductively coupled plasma mass spectrometer, which was coupled with the extraction chromatography system. In this study, we compare 30-cm long, 4.6 mm i.d. columns to capillary columns (750 microm i.d.) with lengths from 30 cm up to 150 cm. The columns that were tested were packed with TRU resin. We were able to separate a mixture of five actinides ((232)Th, (238)U, (237)Np, (239)Pu, and (241)Am). This work has application to rapid bioassay as well as automated separations of actinide materials.

[Determination and analysis of toluene diisocyanate metabolites in mice using gas chromatography-mass spectrometry].

PubMed

Ji, Yu-Bin; Ji, Chen-Feng; Zou, Xiang; Liu, Hui-Xin

2007-09-01

In the present research we used gas chromatography-mass spectrometry (G C-MS) to determine metabolites of toluene diisocyanate (TDI) in mice and deduce the pathway for toluene diisocyanate metabolism in the organism. Conditions for TDI chromatography: Supelco PTETM-5 chromatographic column (30 mm x 0.25 mm x 0.25 microm); initial column temperature: 90 degrees C, which was maintained for 30 min, then the temperature was increased at a rate of 40 degrees C x min(-1) to 280 degrees C, and maintained for 5.25 min; temperature for the vaporizing chamber: 250 degrees C; carrier gas: helium flowing at 1.0 microL x min(-1). Conditions for chromatography of TDI metabolites in the organism: 94% methyl, 4% ethenyl-bonded-phase fused-silica capillary column (30 + 2 m x 0.25 + 0.02 mm); initial column temperature: 30 degrees C, which was maintained for 5 min, after and then was increased at a rate of 80 degrees C x min(-1) to 280 degrees C, and maintained for 5 min; temperature for the vaporizing chamber: 250 degrees C; carrier gas: helium flowing at 1.0 microL x min(-1). Conditions for mass spectrometry: EI for ionization; 70 eV for ionization energy; 280 degrees C for connecting tube temperature; 35-350 micro for range of scanning; and 1.0 microL for sample size. The results showed that 2 ,4-toluene diisocyanate was metabolized into 2,4-diaminotoluene. Under the conditions selected for GC-MS, TDI metabolites in the organism can be isolated and identified.

Comparison of protocols and RNA carriers for plasma miRNA isolation. Unraveling RNA carrier influence on miRNA isolation

PubMed Central

Martos, Laura; Fernández-Pardo, Álvaro; Oto, Julia; Medina, Pilar; España, Francisco; Navarro, Silvia

2017-01-01

microRNAs are promising biomarkers in biological fluids in several diseases. Different plasma RNA isolation protocols and carriers are available, but their efficiencies have been scarcely compared. Plasma microRNAs were isolated using a phenol and column-based procedure and a column-based procedure, in the presence or absence of two RNA carriers (yeast RNA and MS2 RNA). We evaluated the presence of PCR inhibitors and the relative abundance of certain microRNAs by qRT-PCR. Furthermore, we analyzed the association between different isolation protocols, the relative abundance of the miRNAs in the sample, the GC content and the free energy of microRNAs. In all microRNAs analyzed, the addition of yeast RNA as a carrier in the different isolation protocols used gave lower raw Cq values, indicating higher microRNA recovery. Moreover, this increase in microRNAs recovery was dependent on their own relative abundance in the sample, their GC content and the free-energy of their own most stable secondary structure. Furthermore, the normalization of microRNA levels by an endogenous microRNA is more reliable than the normalization by plasma volume, as it reduced the difference in microRNA fold abundance between the different isolation protocols evaluated. Our thorough study indicates that a standardization of pre- and analytical conditions is necessary to obtain reproducible inter-laboratory results in plasma microRNA studies. PMID:29077772

Measurement of bromate in bread by liquid chromatography with post-column flow reactor detection.

PubMed

Himata, K; Noda, M; Ando, S; Yamada, Y

2000-01-01

This method is suitable for the determination of bromate residues in a variety of baked goods. The peer-verified method trial was performed on white bread, multigrain bread, and coffee cake spiked with known levels of potassium bromate. The analytical portion is extracted with deionized water to remove bromate from the bulk of the baked product. The aqueous extract is carried through a series of steps to remove co-extractives that would interfere with the liquid chromatography (LC) in the determinative step or hasten the deterioration of the LC column. The extract is filtered before passing it through a reversed-phase solid-phase extraction (SPE) column and a cation-exchange column in the silver form to remove lipids and chloride, respectively. Ultrafiltration is then used to remove proteins with molecular weights of >30,000 daltons. Finally, a cation-exchange column in the sodium form is used to remove silver ions from the extract. The determinative step uses LC with a reversed-phase column and an ion-pairing agent in the mobile phase. Detection is based on the post-column reaction of bromate with o-dianisidine to form an oxidation product that is quantitated spectrophotometrically at 450 nm. Overall agreement between the submitting and peer laboratories was quite good. For bromate levels of 10-52 ppb, overall mean recoveries were 76.9 and 78.8% for the submitting and peer laboratories, respectively. The standard deviations were higher for the results of the peer laboratory, probably because of the generally higher level of baseline noise present in the chromatograms. The results demonstrate that the method provides adequate accuracy with low-fat as well as high-fat foods. Bromate at levels as low as 5 ppb (ng/g) can be detected with the method.

Linking Water Table Dynamics to Carbon Cycling in Artificial Soil Column Incubations

NASA Astrophysics Data System (ADS)

Geertje, Pronk; Adrian, Mellage; Tatjana, Milojevic; Fereidoun, Rezanezhad; Cappellen Philippe, Van

2016-04-01

The biogeochemistry of wetlands soils is closely tied to their hydrology. Water table fluctuations that cause flooding and drying of these systems may lead to enhanced degradation of organic matter and release of greenhouse gasses (e.g. CO2, CH4) to the atmosphere. However, predicting the influence of water table fluctuations on the biogeochemical functioning of soils requires an understanding of the interactions of soil hydrology with biogeochemical and microbial processes. To determine the effects of water table dynamics on carbon cycling, we are carrying out state-of-the-art automated soil column experiments with fully integrated monitoring of hydro-bio-geophysical process variables under both constant and oscillating water table conditions. An artificial, homogeneous mixture consisting of minerals and organic matter is used to provide a well-defined starting material. The artificial soils are composed of quartz sand, montmorillonite, goethite and humus from a forested riparian zone, from which we also extracted the microbial inoculum added to the soil mixture. The artificial soils are packed into 60 cm high, 7.5 cm wide columns. In the currently ongoing experiment, three replicate columns are incubated while keeping the water table constant water at mid-depth, while another three columns alternate between drained and saturated conditions. Micro-sensors installed at different depths below the soil surface record time-series redox potentials (Eh) varying between oxidizing (~+700 mV) and reducing (~-200 mV) conditions. Continuous O2 levels throughout the soil columns are monitored using high-resolution, luminescence-based, Multi Fiber Optode (MuFO) microsensors. Pore waters are collected periodically with MicroRhizon samplers from different depths, and analyzed for pH, EC, dissolved inorganic and organic carbon and ion/cation compositions. These measurements allow us to track the changes in pore water geochemistry and relate them to differences in carbon cycling between the contrasting water table regimes. Particular attention is given to the mobilization and redistribution of iron from the initially homogeneously distributed goethite. In addition, small solid-phase samples are collected monthly from the saturated and unsaturated zones of the soil columns to characterize the microbial communities and changes in soil microstructure and organo-mineral associations. Headspace gas measurements are used to derive the effluxes of CO2 and CH4 during the experiment. Together, the experimental data will provide a comprehensive picture of the early development of the soil and the accompanying establishment of biogeochemical gradients under dynamic hydrological conditions. They will allow us to relate the degradation of soil organic matter and greenhouse gas emissions to the saturation conditions and redox chemistry under controlled conditions. The experiment is in progress with an expected total duration of 6 months.

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

PubMed

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

1988-03-01

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

A modified approach for isolation of essential oil from fruit of Amorpha fruticosa Linn using microwave-assisted hydrodistillation concatenated liquid-liquid extraction.

PubMed

Chen, Fengli; Jia, Jia; Zhang, Qiang; Gu, Huiyan; Yang, Lei

2017-11-17

In this work, a modified technique was developed to separate essential oil from the fruit of Amorpha fruticosa using microwave-assisted hydrodistillation concatenated liquid-liquid extraction (MHD-LLE). The new apparatus consists of two series-wound separation columns for separating essential oil, one is the conventional oil-water separation column, and the other is the extraction column of components from hydrosol using an organic solvent. Therefore, the apparatus can simultaneously collect the essential oil separated on the top of hydrosol and the components extracted from hydrosol using an organic solvent. Based on the yield of essential oil in the first and second separation columns, the effects of parameters were investigated by single factor experiments and Box-Behnken design. Under the optimum conditions (2mL ethyl ether as the extraction solvent in the second separation column, 12mL/g liquid-solid ratio, 4.0min homogenate time, 35min microwave irradiation time and 540W microwave irradiation power), satisfactory yields for the essential oil in the first separation column (10.31±0.33g/kg) and second separation column (0.82±0.03g/kg) were obtained. Compared with traditional methods, the developed method gave a higher yield of essential oil in a shorter time. In addition, GC-MS analysis of the essential oil indicated significant differences of the relative contents of individual volatile components in the essential oils obtained in the two separation columns. Therefore, the MHD-LLE technique developed here is a good alternative for the isolation of essential oil from A. fruticosa fruit as well as other herbs. Copyright © 2017 Elsevier B.V. All rights reserved.

Online hyphenation of extraction, Sephadex LH-20 column chromatography, and high-speed countercurrent chromatography: A highly efficient strategy for the preparative separation of andrographolide from Andrographis paniculata in a single step.

PubMed

Zhang, Ying-Qi; Wang, Shan-Shan; Han, Chao; Xu, Jin-Fang; Luo, Jian-Guang; Kong, Ling-Yi

2017-12-01

A novel isolation strategy, online hyphenation of ultrasonic extraction, Sephadex LH-20 column chromatography combined with high-speed countercurrent chromatography, was developed for pure compounds extraction and purification. Andrographolide from Andrographis paniculata was achieved only in a single step purification protocol via the present strategy. The crude powder was ultrasonic extracted and extraction was pumped into Sephadex LH-20 column directly to cut the nontarget fractions followed by the second-dimensional high-speed countercurrent chromatography, hyphenated by a six-port valve equipped at the post-end of Sephadex LH-20 column, for the final purification. The results yielded andrographolide with the amount of 1.02 mg and a purity of 98.5% in a single step, indicating that the present method is effective to harvest target compound from medicinal plant. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A poly(alkyl methacrylate-divinylbenzene-vinylbenzyl trimethylammonium chloride) monolithic column for solid-phase microextraction.

PubMed

Liu, Wan-Ling; Lirio, Stephen; Yang, Yicong; Wu, Lin-Tai; Hsiao, Shu-Ying; Huang, Hsi-Ya

2015-05-22

In this study, an organic polymer monolithic columns, which were prepared via in situ polymerization of alkyl methacrylate-ester (AMA), divinylbenzene (DVB) and vinylbenzyl trimethylammonium chloride (VBTA, charged monomer), were developed as adsorbent for solid-phase microextraction (SPME). Different parameters affecting the extraction efficiency for nine (9) non-steroidal anti-inflammatory drugs (NSAIDs) such as the ratio of the stearyl methacrylate (SMA) to DVB monomer, column length, sample pH, extraction flow rate and desorption solvent were investigated to obtain the optimal SPME condition. Also, the permeability for each poly(AMA-DVB-VBTA) monolithic column was investigated by adding porogenic solvent (poly(ethylene glycol), PEG). Using the optimized condition, a series of AMA-based poly(AMA-DVB-VBTA) monolith columns were developed to determine the effect the extraction efficiency of NSAIDs by varying the alkyl chain length of the methacrylate ester (methyl-, butyl-, octyl-, or lauryl-methacrylate; (MMA, BMA, OMA, LMA)). Results showed that decreasing the AMA chain length increases the extraction efficiency of some NSAIDs (i.e. sulindac (sul), naproxen (nap), ketoprofen (ket) and indomethacin (idm)). Among the poly(AMA-DVB-VBTA) monolithic columns, poly(BMA-DVB-VBTA) showed a highly repeatable extraction efficiency for NSAIDs with recoveries ranging from 85.0 to 100.2% with relative standard deviation (RSD) less than 6.8% (n=3). The poly(BMA-DVB-VBTA) can also be reused for at least 50 times without any significant effect in extraction efficiency for NSAIDs. Finally, using the established conditions, the poly(BMA-DVB-VBTA) was used to extract trace-level NSAIDs (100μgL(-1)) in river water with good recoveries ranging from 75.8 to 90.8% (RSD<14.9%). Copyright © 2015 Elsevier B.V. All rights reserved.

Novel approach to microwave-assisted extraction and micro-solid-phase extraction from soil using graphite fibers as sorbent.

PubMed

Xu, Li; Lee, Hian Kee

2008-05-30

A single-step extraction-cleanup procedure involving microwave-assisted extraction (MAE) and micro-solid-phase extraction (micro-SPE) has been developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) from soil samples. Micro-SPE is a relatively new extraction procedure that makes use of a sorbent enclosed within a sealed polypropylene membrane envelope. In the present work, for the first time, graphite fiber was used as a sorbent material for extraction. MAE-micro-SPE was used to cleanup sediment samples and to extract and preconcentrate five PAHs in sediment samples prepared as slurries with addition of water. The best extraction conditions comprised of microwave heating at 50 degrees C for a duration of 20 min, and an elution (desorption) time of 5 min using acetonitrile with sonication. Using gas chromatography (GC)-flame ionization detection (FID), the limits of detection (LODs) of the PAHs ranged between 2.2 and 3.6 ng/g. With GC-mass spectrometry (MS), LODs were between 0.0017 and 0.0057 ng/g. The linear ranges were between 0.1 and 50 or 100 microg/g for GC-FID analysis, and 1 and 500 or 1000 ng/g for GC-MS analysis. Granular activated carbon was also used for the micro-SPE device but was found to be not as efficient in the PAH extraction. The MAE-micro-SPE method was successfully used for the extraction of PAHs in river and marine sediments, demonstrating its applicability to real environmental solid matrixes.

"Supermarket Column Chromatography of Leaf Pigments" Revisited: Simple and Ecofriendly Separation of Plant Carotenoids, Chlorophylls, and Flavonoids from Green and Red Leaves

ERIC Educational Resources Information Center

Dias, Alice M.; Ferreira, Maria La Salete

2015-01-01

A simple and ecofriendly procedure was developed in order to prepare extracts from red and green leaves. This procedure enables the separation of yellow, green, and red band pigments and optimizes the previously reported baking soda "supermarket column". The same extract also led to a novel and colorful potato starch column, which can…

Two-column sequential injection chromatography--new approach for fast and effective analysis and its comparison with gradient elution chromatography.

PubMed

Chocholous, Petr; Satínský, Dalibor; Sklenárová, Hana; Solich, Petr

2010-05-23

This work presents novel approach in low-pressure chromatography flow systems--two-column Sequential Injection Chromatography (2-C SIC) and its comparison with gradient elution chromatography on the same instrument. The system was equipped with two different chromatographic columns (connected to selection valve in parallel design) for isocratic separation and determination of all components in composed anti-inflammatory pharmaceutical preparation (tablets). The sample was first injected on the first column of length 30 mm where less retained analytes were separated and then the sample was injected on the second column of length 10 mm where more retained analytes were separated. The SIC system was based on a commercial SIChrom manifold (8-port high-pressure selection valve and medium-pressure syringe pump with 4 mL reservoir) (FIAlab, USA) with two commercially available monolithic columns the "first column" Chromolith Flash RP-18e (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.) and the "second column" Chromolith RP-18e (10 mm x 4.6 mm i.d.) and CCD UV-vis detector USB 4000 with micro-volume 1.0 cm Z flow cell. Two mobile phases were used for analysis (one for each column). The mobile phase 1 used for elution of paracetamol, caffeine and salicylic acid (internal standard) was acetonitrile/water (10:90, v/v, the water part of pH 3.5 adjusted with acetic acid), flow rate was 0.9 mL min(-1) (volume 3.0 mL of mobile phase per analysis). The mobile phase 2 used for elution of propyphenazone was acetonitrile/water (30:70, v/v); flow rate was 1.2 mL min(-1) (volume 1.5 mL of mobile phase per analysis). Absorbance was monitored at 210 nm. Samples were prepared by dissolving of one tablet in 30% acetonitrile and 10 microL of filtered supernatant was injected on each column (2 x 10 microL). The chromatographic resolution between all compounds was >1.45 and analysis time was 5.5 min under the optimal conditions. Limits of detection were determined at 0.4 microg mL(-1) for paracetamol, at 0.5 microg mL(-1) for caffeine and at 0.7 microg mL(-1) for propyphenazone. The new two-column chromatographic set-up developed as an alternative approach to gradient elution chromatography shows evident advantages (time and solvent reduction more than one-third) as compared with single-column gradient SIC method with Chromolith Flash RP-18 (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.). Copyright 2010 Elsevier B.V. All rights reserved.

[Application of micro-power system in the surgery of tooth extraction].

PubMed

Kaijin, Hu; Yongfeng, Li

2015-02-01

Tooth extraction is a common operation in oral surgery. Traditional-extraction instruments, such as bone chisel, elevator, and bone hammer, lead to not only severe trauma but also unnecessary complications, and patients easily become nervous and apprehensive if tooth extraction is performed using these violent instruments. In recent years, with the develop- ment of minimally invasive concept and technology, various micro-power instruments have been used for tooth extraction. This innovative technology can reduce the iatrogenic trauma and complications of tooth extraction. Additionally, this technology can greatly decrease the patient's physical and mental pressure. The new equipment compensates for the deficiency of traditional tooth extraction equipment and facilitates the gradual replacement of the latter. Diverse micro-power systems have distinct strengths and weaknesses, so some auxiliary instruments are still needed during tooth extraction. This paper focuses on the various micro-power systems for tooth extraction and tries to compare the advantages and disadvantages of these systems. Selection and usage of auxiliary equipment are also introduced. Thus, this paper provides reference for the proper application of the micro-power systems in tooth extraction.

Design of a compressed air modulator to be used in comprehensive multidimensional gas chromatography and its application in the determination of pesticide residues in grapes.

PubMed

Pizzutti, Ionara R; Vreuls, René J J; de Kok, André; Roehrs, Rafael; Martel, Samile; Friggi, Caroline A; Zanella, Renato

2009-04-10

In this study, a new modulator that is simple, robust and presents low operation costs, was developed. This modulator uses compressed air to cool two small portions in the first centimeters of the second chromatographic column of a comprehensive multidimensional gas chromatography (GCxGC) system. The results show a variation in the peak area less than 3 and 5% to alkanes and pesticides, respectively. The standard deviations for the retention times in the first and second dimension are around 0.05 min and 0.05s for all the compounds. The system was optimized with n-alkanes. The GCxGC system proposed was applied in the determination of pyrethroid pesticides (bifenthrin, cypermethrin, deltamethrin, fenvalerate, esfenvalerate, cis- and trans-permethrin) in grape samples. Samples were extracted by the mini-Luke modified method and pesticides were quantified by comprehensive multidimensional gas chromatography with micro electron-capture detection (microECD). The values of method limit of quantification (LOQ) were 0.01-0.02 mg kg(-1) for all studied pyrethroid and the values of recovery were between 94.3 and 115.2%, with good precision (RSD<18.4%), demonstrating that the performance of the total method consisting of a modified Luke extraction method and determination by GCxGC-microECD are satisfactory. This study also showed that the system using a modulator with a double jet of compressed air has the potential for application in the analysis of a wider range of pesticide residues in other commodities since it provides low values of LOQ with acceptable accuracy and precision.

Online liquid chromatography-tandem mass spectrometry cyanide determination in blood.

PubMed

Lacroix, C; Saussereau, E; Boulanger, F; Goullé, J P

2011-04-01

An original liquid chromatography-tandem mass spectrometry (LC-MS-MS) method coupled to online extraction has been developed for cyanide determination in blood. A method involving fluorimetric detection after naphthalene-2,3-dicarboxyaldehyde (NDA) complexation by taurine in the presence of cyanide was previously described. Its performance was limited because of the absence of an internal standard (IS). Using cyanide isotope (13)C(15)N as IS allowed quantification in MS-MS. After the addition of (13)C(15)N, 25 μL of blood were diluted in water and deproteinized with methanol. Following derivatization with NDA and taurine for 10 min at 4°C, 100 μL was injected into the online LC-MS-MS system. An Oasis HLB was used as an extraction column, and a C18 Atlantis was the analytical column. The chromatographic cycle was performed with an ammonium formate (20 mM, pH 2.8) (solvent A) and acetonitrile/solvent A (90:10, v/v) gradient in 6 min. Detection was performed in negative electrospray ionization mode (ESI(-)) with a Quattro Micro. For quantification, transitions of derivatives formed with CN and (13)C(15)N were monitored, respectively, as follows: 299.3/191.3 and 301.3/193.3. The procedure was fully validated, linear from 26 to 2600 ng/mL with limit of detection of 10 ng/mL. This method, using a small blood sample, is not only simple, but also time saving. The specificity and sensitivity of LC-MS-MS coupled to online extraction and using (13)C(15)N as the IS make this method very suitable for cyanide determination in blood and could be useful in forensic toxicology.

Multiresidue determination of chlorophenoxy acid herbicides in human urine samples by use of solid-phase extraction and capillary LC-UV detection.

PubMed

Rosales-Conrado, N; León-González, M E; Pérez-Arribas, L V; Polo-Díez, L M

2008-01-01

Chlorophenoxy acid herbicides are intensively applied to get rid of unwanted plants because of their low cost and selectivity. Due to their toxicity, which depends on their chemical form, the European Community has established legal directives to restrict their use and to control their maximum residue levels in several matrices. Determination of chlorophenoxy acids-2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA), 2-(2,4-dichlorophenoxy)propanoic acid (2,4-DP), 2-(4-chloro-2-methylphenoxy)propanoic acid (MCPP), 4-(4-chloro-2-methylphenoxy)butanoic acid (MCPB) and 2-(2,4,5-trichlorophenoxy)propanoic acid (2,4,5-TP) in spiked human urine samples has been carried out by capillary LC, after solid-phase extraction on a column packed with silica C18 restricted-access material. Chromatographic analysis was performed in gradient-elution mode at 25 degrees C, with injection of 20 microL low-organic-solvent composition herbicide solutions for focusing purposes on the head of the capillary column, and diode array detection at 232 nm. Urine samples collected during 24 h from healthy and unexposed volunteers were spiked in the concentration range 25-150 microg L(-1); recoveries obtained were between 66 and 100% (n = 6 for each spiked level) and RSDs (relative standard deviations) were between 1 and 5%. Detection limits in the urine samples from volunteers were between 3.5 and 6.0 microg L(-1). The developed methodology has allowed the clean-up and preconcentration of low volumes of untreated human urine without previous treatment, showing the effectiveness of the employed SPE sorbent for extracting the target analytes and ultimately resulting in the reduction of the sample-preparation time.

Hydrolysis of proteins with methanesulfonic acid for improved HPLC-ICP-MS determination of seleno-methionine in yeast and nuts.

PubMed

Wrobel, Katarzyna; Kannamkumarath, Sasi S; Wrobel, Kazimierz; Caruso, Joseph A

2003-01-01

In this work, the use of methanesulfonic acid for protein hydrolysis is proposed for evaluation of Se-methionine in yeast, Brazil nuts, and possibly other selenium-rich biological samples. The hydrolysis was carried out by heating the sample with 4 mol L(-1) acid at reflux for 8 h. Two chromatographic techniques (size-exclusion and ion-pairing) coupled with ICP-MS detection were used to compare the release of Se-methionine from proteins by enzymatic (proteinase K, protease XIV) and acid hydrolyses. A more efficient liberation of Se-methionine was observed by acid hydrolysis. For quantification, the sample extracts were introduced onto a C8 Alltima column, and the separation was achieved with a mobile phase containing 5 mmol L(-1) hexanesulfonic acid in citrate buffer (pH 4.5)/methanol (95:5). The results obtained by standard addition showed 816+/-17 micro g g(-1) and 36.2+/-1.5 micro g g(-1) of selenium in the form of Se-methionine in yeast and nuts, respectively (65% and 75% of total selenium).

Adsorption experiment of toxic micro-pollutants derived from automobiles using red soil.

PubMed

Kawai, Takahiro; Ichiki, Atsushi; Sawada, Yasunori

2015-01-01

In some countries, non-point source pollution derived from a city's economic activities tends to be a barrier to the improvement of water quality. Roadway runoff is known to contain toxic micro-pollutants such as polycyclic aromatic hydrocarbons (PAHs). Conversely, red soil is known to adsorb some organic matter. In this study, artificial roadway runoff water containing toxic micro-pollutants was made using roadway dust collected from a highway, and used for both batch-type tests and soil column tests with red soil in order to understand adsorption ability of the red soil on such toxic micro-pollutants, especially PAHs. In the batch-type tests, PAHs could be removed by approximately 40% when the contact time was 90 minutes. In the soil column tests, PAHs were removed by more than 80% while suspended solids were removed by more than 90%. Notably, PAHs with a high molecular weight were removed more readily in the tests than PAHs with a low molecular weight.

Chip-based device for parallel sorting, amplification, detection, and identification of nucleic acid subsequences

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

Beer, Neil Reginald; Colston, Jr, Billy W.

An apparatus for chip-based sorting, amplification, detection, and identification of a sample having a planar substrate. The planar substrate is divided into cells. The cells are arranged on the planar substrate in rows and columns. Electrodes are located in the cells. A micro-reactor maker produces micro-reactors containing the sample. The micro-reactor maker is positioned to deliver the micro-reactors to the planar substrate. A microprocessor is connected to the electrodes for manipulating the micro-reactors on the planar substrate. A detector is positioned to interrogate the sample contained in the micro-reactors.

The uterotonic activity of compounds isolated from the supercritical fluid extract of Ekebergia capensis.

PubMed

Sewram, V; Raynor, M W; Mulholland, D A; Raidoo, D M

2000-12-01

The wood of Ekebergia capensis Sparrm. is used by the local Zulu community in KwaZulu-Natal Province, South Africa to facilitate childbirth. In this investigation, the uterotonic properties of extracts from this tree were evaluated using both pregnant and non-pregnant guinea pig uterine smooth muscle in vitro. The extracts were prepared using water modified supercritical carbon dioxide at 400 atm and 80 degrees C. As samples of these extracts displayed positive results when screened for uterotonic activity, gravity column chromatography followed by NMR spectroscopy was performed in an attempt to isolate and elucidate the structures of the compounds that were present in the extract. The extract yielded five known compounds of which only two, viz. oleanonic acid and 3-epioleanolic acid, displayed uterotonic activity. Receptor binding assays were subsequently performed with 3-epioleanolic acid to ascertain its mode of action. Bradykinin (30 ng/100 microl) and acetylcholine (1 microg/100 microl) were used as the B2 and cholinergic receptor agonists respectively with icatibant (HOE 140) (30 ng/100 microl) and atropine (60 micro/100 microl) as their corresponding antagonists. 3-epioleanolic acid was observed to mediate its effect through the cholinergic receptor. The results of this study show that two compounds from the extract of this tree possess varying degrees of agonist activity on uterine smooth muscle with minor changes in the molecular structure affecting its intrinsic activity on uterine muscle.

Determination of the Antibiotic Oxytetracycline in Commercial Milk by Solid-Phase Extraction: A High-Performance Liquid Chromatography (HPLC) Experiment for Quantitative Instrumental Analysis

ERIC Educational Resources Information Center

Mei-Ratliff, Yuan

2012-01-01

Trace levels of oxytetracylcine spiked into commercial milk samples are extracted, cleaned up, and preconcentrated using a C[subscript 18] solid-phase extraction column. The extract is then analyzed by a high-performance liquid chromatography (HPLC) instrument equipped with a UV detector and a C[subscript 18] column (150 mm x 4.6 mm x 3.5 [mu]m).…

The optional selection of micro-motion feature based on Support Vector Machine

NASA Astrophysics Data System (ADS)

Li, Bo; Ren, Hongmei; Xiao, Zhi-he; Sheng, Jing

2017-11-01

Micro-motion form of target is multiple, different micro-motion forms are apt to be modulated, which makes it difficult for feature extraction and recognition. Aiming at feature extraction of cone-shaped objects with different micro-motion forms, this paper proposes the best selection method of micro-motion feature based on support vector machine. After the time-frequency distribution of radar echoes, comparing the time-frequency spectrum of objects with different micro-motion forms, features are extracted based on the differences between the instantaneous frequency variations of different micro-motions. According to the methods based on SVM (Support Vector Machine) features are extracted, then the best features are acquired. Finally, the result shows the method proposed in this paper is feasible under the test condition of certain signal-to-noise ratio(SNR).

Development and validation of a rapid and sensitive high-performance liquid chromatography-mass spectroscopy assay for determination of 17-(allylamino)-17-demethoxygeldanamycin and 17-(amino)-17-demethoxygeldanamycin in human plasma.

PubMed

Johnston, Jeffrey S; Phelps, Mitch A; Blum, Kristie A; Blum, William; Grever, Michael R; Farley, Katherine L; Dalton, James T

2008-08-01

A sensitive method was developed and validated for the measurement of 17-(allylamino)-17-demethoxygeldanamycin (17AAG) and its active metabolite 17-amino-17-demethoxygeldanamycin (17AG) in human plasma using 17-(dimethylaminoethylamino)-17-demethoxygeldanamycin (17DMAG) as an internal standard. After the addition of internal standard, 200 microL of plasma was extracted using ice cold acetonitrile followed by analysis on a Thermo Finnigan triple-quadruple mass spectrometer coupled to an Agilent 1100 HPLC system. Chromatography was carried out on a 50 mm x 2.1 mm Agilent Zorbax SB-phenyl 5 microm column coupled to a 3mm Varian metaguard diphenyl pre-column using glacial acetic acid 0.1% and a gradient of acetonitrile and water at a flow rate of 500 microL/min. Atmospheric pressure chemical ionization and detection of 17AAG, 17AG and 17DMAG were accomplished using selected reaction monitoring of m/z 584.3>541.3, 544.2>501.2, and 615.3>572.3, respectively in negative ion mode. Retention times for 17AAG, 17AG, and 17DMAG were 4.1, 3.5, and 2.9 min, respectively, with a total run time of 7 min. The assay was linear over the range 0.5-3000 ng/mL for 17AAG and 17AG. Replicate sample analysis indicated within- and between-run accuracy and precision within 15%. The recovery of 17AAG and 17AG from 200 microL of plasma containing 1, 25, 300, and 2500 ng/mL was 93% or greater. This high-performance liquid chromatographic tandem mass spectroscopy (HPLC/MS/MS) method is superior to previous methods. It is the first analytical method reported to date for the quantitation of both 17AAG and its metabolite 17AG and can reliably quantitate concentrations of both compounds as low as 0.5 ng/mL.

Comparison of Total RNA Isolation Methods for Analysis of Immune-Related microRNAs in Market Milks

PubMed Central

2015-01-01

Bovine milk provides essential nutrients, including immunologically important molecules, as the primary source of nutrition to newborns. Recent studies showed that RNAs from bovine milk contain immune-related microRNAs (miRNA) that regulate various immune systems. To evaluate the biological and immunological activity of miRNAs from milk products, isolation methods need to be established. Six methods for extracting total RNAs from bovine colostrums were adopted to evaluate the isolating efficiency and expression of miRNAs. Total RNA from milk was presented in formulation of small RNAs, rather than ribosomal RNAs. Column-combined phenol isolating methods showed high recovery of total RNAs, especially the commercial columns for biofluid samples, which demonstrated outstanding efficiency for recovering miRNAs. We also evaluated the quantity of five immune-related miRNAs (miR-93, miR-106a, miR-155, miR-181a, miR-451) in milk processed by temperature treatments including low temperature for long time (LTLT, 63℃ for 30 min)-, high temperature for short time (HTST, 75℃ for 15 s)-, and ultra heat treatment (UHT, 120-130℃ for 0.5-4 s). All targeted miRNAs had significantly reduced levels in processed milks compared to colostrum and raw mature milk. Interestingly, the amount of immune-related miRNAs from HTST milk was more resistant than those of LTLT and UHT milks. Our present study examined defined methods of RNA isolation and quantification of immune-specific miRNAs from small volumes of milk for use in further analysis. PMID:26761866

Comparison of Total RNA Isolation Methods for Analysis of Immune-Related microRNAs in Market Milks.

PubMed

Oh, Sangnam; Park, Mi Ri; Son, Seok Jun; Kim, Younghoon

2015-01-01

Bovine milk provides essential nutrients, including immunologically important molecules, as the primary source of nutrition to newborns. Recent studies showed that RNAs from bovine milk contain immune-related microRNAs (miRNA) that regulate various immune systems. To evaluate the biological and immunological activity of miRNAs from milk products, isolation methods need to be established. Six methods for extracting total RNAs from bovine colostrums were adopted to evaluate the isolating efficiency and expression of miRNAs. Total RNA from milk was presented in formulation of small RNAs, rather than ribosomal RNAs. Column-combined phenol isolating methods showed high recovery of total RNAs, especially the commercial columns for biofluid samples, which demonstrated outstanding efficiency for recovering miRNAs. We also evaluated the quantity of five immune-related miRNAs (miR-93, miR-106a, miR-155, miR-181a, miR-451) in milk processed by temperature treatments including low temperature for long time (LTLT, 63℃ for 30 min)-, high temperature for short time (HTST, 75℃ for 15 s)-, and ultra heat treatment (UHT, 120-130℃ for 0.5-4 s). All targeted miRNAs had significantly reduced levels in processed milks compared to colostrum and raw mature milk. Interestingly, the amount of immune-related miRNAs from HTST milk was more resistant than those of LTLT and UHT milks. Our present study examined defined methods of RNA isolation and quantification of immune-specific miRNAs from small volumes of milk for use in further analysis.

Vigabatrin in dried plasma spots: validation of a novel LC-MS/MS method and application to clinical practice.

PubMed

Kostić, Nađa; Dotsikas, Yannis; Jović, Nebojša; Stevanović, Galina; Malenović, Anđelija; Medenica, Mirjana

2014-07-01

This paper presents a LC-MS/MS method for the determination of antiepileptic drug vigabatrin in dried plasma spots (DPS). Due to its zwitterionic chemical structure, a pre-column derivatization procedure was performed, aiming to yield enhanced ionization efficiency and improved chromatographic behaviour. Propyl chloroformate, in the presence of propanol, was selected as the best derivatization reagent, providing a strong signal along with reasonable run time. A relatively novel sample collection technique, DPS, was utilized, offering easy sample handling and analysis, using a sample in micro amount (∼5μL). Derivatized vigabatrin and its internal standard, 4-aminocyclohexanecarboxylic acid, were extracted by liquid-liquid extraction (LLE) and determined in positive ion mode by applying two SRM transitions per analyte. A Zorbax Eclipse XDB-C8 column (150×4.6mm, 5μm particle size) maintained at 30°C, was utilized with running mobile phase composed of acetonitrile: 0.15% formic acid (85:15, v/v). Flow rate was 550μL/min and total run time 4.5min. The assay exhibited excellent linearity over the concentration range of 0.500-50.0μg/mL, which is suitable for the determination of vigabatrin level after per os administration in children and youths with epilepsy, who were on vigabatrin therapy, with or without co-medication. Specificity, accuracy, precision, recovery, matrix-effect and stability were also estimated and assessed within acceptance criteria. Copyright © 2014 Elsevier B.V. All rights reserved.

An integrated evaluation of the persistence and effects of 4-nonylphenol in an experimental littoral ecosystem

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

Liber, K.; Knuth, M.L.; Stay, F.S.

1999-03-01

A comprehensive littoral enclosure study was conducted to assess the persistence and distribution of 4-nonylphenol (NP) in a littoral ecosystem, and to evaluate the compound`s effects on resident aquatic biota. Enclosures with a mean ({+-} SD) surface area and volume of 31.4 {+-} 3.3 m{sup 2} and 32.0 {+-} 6.4 m{sup 3}, respectively, received eleven applications at 48-h intervals with one of four different rates of NP. This created a 20-d application period which was followed by a three to fourteen month observation period, depending on the endpoint measured. Mean {+-} SD NP concentrations in the water column measured 2more » h after each application averaged 5 {+-} 4, 23 {+-} 11, 76 {+-} 21, and 243 {+-} 41 {micro}g/L at nominal treatments of 3, 30, 100, and 300 {micro}g/L, respectively. Persistence in the water column was relatively short, with a dissipation half-life estimated at {le} 1.2 d. Persistence of NP in sediment and on macrophytes was substantially longer, with estimated half-lives of 28 to 104 d and 8 to 13 d, respectively. Zooplankton was the most sensitive group of organisms evaluated, with significant reductions in population abundances of some copepod taxa observed at the 23 {+-} 11-{micro}g/L treatment. Fish survival was affected at 243 {+-} 41 {micro}g/L. The most sensitive benthic macroinvertebrate taxon, Pisidium (Bivalvia) was affected at 76 {+-} 21 {micro}g/L, but most taxa were only affected at the 243 {+-} 41-{micro}g/L treatment. None of the assessed populations were affected at the 5 {+-} 4-{micro}g/L treatment. Macrophytes and periphyton were not adversely affected by any of the treatments. Overall community composition, assessed at the family level or higher, was not affected at or below the 23 {+-} 11-{micro}g/L treatment, but did exhibit substantial changes at the 243 {+-} 41-{micro}g/L treatment. Some minor changes were observed at the 76 {+-} 21-{micro}g/L treatment. The maximum acceptable toxicant concentration in the water column, based on protection of the most sensitive taxa in the test system, was estimated at {approximately} 10 {micro}g/L. Details on NP persistence and distribution within the enclosures, and detailed effects on zooplankton, benthic macroinvertebrates, and fish are described in four separate papers immediately following this overview.« less

Validation and application of a high-performance liquid chromatography-tandem mass spectrometric method for simultaneous quantification of lopinavir and ritonavir in human plasma using semi-automated 96-well liquid-liquid extraction.

PubMed

Wang, Perry G; Wei, Jack S; Kim, Grace; Chang, Min; El-Shourbagy, Tawakol

2006-10-20

Kaletra is an important antiretroviral drug, which has been developed by Abbott Laboratories. It is composed of lopinavir (low-pin-a-veer) and ritonavir (ri-toe-na-veer). Both have been proved to be human immunodeficiency virus (HIV) protease inhibitors and have substantially reduced the morbidity and mortality associated with HIV-1 infection. We have developed and validated an assay, using liquid chromatography coupled with atmospheric pressure chemical ionization tandem mass spectrometry (LC/MS/MS), for the routine quantification of lopinavir and ritonavir in human plasma, in which lopinavir and ritonavir can be simultaneously analyzed with high throughput. The sample preparation consisted of liquid-liquid extraction with a mixture of hexane: ethyl acetate (1:1, v/v), using 100 microL of plasma. Chromatographic separation was performed on a Waters Symmetry C(18) column (150 mm x 3.9 mm, particle size 5 microm) with reverse-phase isocratic using mobile phase of 70:30 (v/v) acetonitrile: 2 mM ammonium acetate aqueous solution containing 0.01% formic acid (v/v) at a flow rate of 1.0 mL/min. A Waters symmetry C(18) guard column (20 mm x 3.9 mm, particle size 5 microm) was connected prior to the analytical column, and a guard column back wash was performed to reduce the analytical column contamination using a mixture of tetrahydrofuran (THF), methanol and water (45:45:10, v/v/v). The analytical run was 4 min. The use of a 96-well plate autosampler allowed a batch size up to 73 study samples. A triple-quadrupole mass spectrometer was operated in a positive ion mode and multiple reaction monitoring (MRM) was used for drug quantification. The method was validated over the concentration ranges of 19-5,300 ng/mL for lopinavir and 11-3,100 ng/mL for ritonavir. A-86093 was used as an internal standard (I.S.). The relative standard deviation (RSD) were <6% for both lopinavir and ritonavir. Mean accuracies were between the designed limits (+/-15%). The robust and rapid LC/MS/MS assay has been successfully applied for routine assay to support bioavailability, bioequivalence, and pharmacokinetics studies.

Determining concentrations of 2-bromoallyl alcohol and dibromopropene in ground water using quantitative methods

USGS Publications Warehouse

Panshin, Sandra Y.

1997-01-01

A method for determining levels of 2-bromoallyl alcohol and 2,3-dibromopropene from ground-water samples using liquid/liquid extraction followed by gas chromatography/mass spectrometry is described. Analytes were extracted from the water using three aliquots of dichloromethane. The aliquots were combined and reduced in volume by rotary evaporation followed by evaporation using a nitrogen stream. The extracts were analyzed by capillary-column gas chromatography/mass spectrometry in the full-scan mode. Estimated method detection limits were 30 nanograms per liter for 2-bromoallyl alcohol and 10 nanograms per liter for 2,3-dibromopropene. Recoveries were determined by spiking three matrices at two concentration levels (0.540 and 5.40 micrograms per liter for 2-bromoallyl alcohol; and 0.534 and 5.34micro-grams per liter for dibromopropene). For seven replicates of each matrix at the high concentration level, the mean percent recoveries ranged from 43.9 to 64.9 percent for 2-bromoallyl alcohol, and from 87.5 to 99.3 percent for dibromopropene. At the low concentration level, the mean percent recoveries ranged from 43.8 to 95.2 percent for 2-bromoallyl alcohol, and from 71.3 to 84.9 percent for dibromopropene.

Automated clean-up, separation and detection of polycyclic aromatic hydrocarbons in particulate matter extracts from urban dust and diesel standard reference materials using a 2D-LC/2D-GC system.

PubMed

Ahmed, Trifa M; Lim, Hwanmi; Bergvall, Christoffer; Westerholm, Roger

2013-10-01

A multidimensional, on-line coupled liquid chromatographic/gas chromatographic system was developed for the quantification of polycyclic aromatic hydrocarbons (PAHs). A two-dimensional liquid chromatographic system (2D-liquid chromatography (LC)), with three columns having different selectivities, was connected on-line to a two-dimensional gas chromatographic system (2D-gas chromatography (GC)). Samples were cleaned up by combining normal elution and column back-flush of the LC columns to selectively remove matrix constituents and isolate well-defined, PAH enriched fractions. Using this system, the sequential removal of polar, mono/diaromatic, olefinic and alkane compounds from crude extracts was achieved. The LC/GC coupling was performed using a fused silica transfer line into a programmable temperature vaporizer (PTV) GC injector. Using the PTV in the solvent vent mode, excess solvent was removed and the enriched PAH sample extract was injected into the GC. The 2D-GC setup consisted of two capillary columns with different stationary phase selectivities. Heart-cutting of selected PAH compounds in the first GC column (first dimension) and transfer of these to the second GC column (second dimension) increased the baseline resolutions of closely eluting PAHs. The on-line system was validated using the standard reference materials SRM 1649a (urban dust) and SRM 1975 (diesel particulate extract). The PAH concentrations measured were comparable to the certified values and the fully automated LC/GC system performed the clean-up, separation and detection of PAHs in 16 extracts in less than 24 h. The multidimensional, on-line 2D-LC/2D-GC system eliminated manual handling of the sample extracts and minimised the risk of sample loss and contamination, while increasing accuracy and precision.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

USGS Publications Warehouse

Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

1996-01-01

A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

Automated solid-phase extraction and liquid chromatography for assay of cyclosporine in whole blood.

PubMed

Kabra, P M; Wall, J H; Dimson, P

1987-12-01

In this rapid, precise, accurate, cost-effective, automated liquid-chromatographic procedure for determining cyclosporine in whole blood, the cyclosporine is extracted from 0.5 mL of whole blood together with 300 micrograms of cyclosporin D per liter, added as internal standard, by using an Advanced Automated Sample Processing unit. The on-line solid-phase extraction is performed on an octasilane sorbent cartridge, which is interfaced with a RP-8 guard column and an octyl analytical column, packed with 5-microns packing material. Both columns are eluted with a mobile phase containing acetonitrile/methanol/water (53/20/27 by vol) at a flow rate of 1.5 mL/min and column temperature of 70 degrees C. Absolute recovery of cyclosporine exceeded 85% and the standard curve was linear to 5000 micrograms/L. Within-run and day-to-day CVs were less than 8%. Correlation between automated and manual Bond-Elut extraction methods was excellent (r = 0.987). None of 18 drugs and four steroids tested interfered.

Preparation and evaluation of a mixed-bed immunoaffinity column for selective purification of sixteen sulfonamides in pork muscle.

PubMed

Li, Yingguo; Chen, Yiqiang; Li, Zhengguo; Zhang, Lei; Li, Xianliang; Xi, Cunxian; Wang, Guomin; Wang, Xiong; Guo, Qi; Li, Na

2012-03-01

This paper describes the preparation of a novel mixed-bed immunoaffinity chromatography (IAC) column by coupling four monoclonal antibodies against different sulfonamides (SAs) to Sepharose 4B. The IAC column can be used to simultaneously extract and purify 16 SAs in pork muscle. The dynamic column capacities for all SAs in mixed standard solution were between 312 and 479 ng/mL gel. After simple extraction and IAC cleanup, the sample solution can be directly injected for liquid chromatography-ultraviolet analysis. The recoveries of SAs from spiked samples at levels of 25, 50 and 100 µg/kg ranged from 83.3 to 103.1% with variation coefficient less than 8.6%. The comparison of IAC with liquid-liquid extraction and solid phase extraction indicated that IAC has better purification effect and needs less organic solution than conventional methods, thus it would be an ideal method for selective purification of SAs in pork muscle.

A novel approach to the simultaneous extraction and non-targeted analysis of the small molecules metabolome and lipidome using 96-well solid phase extraction plates with column-switching technology.

PubMed

Li, Yubo; Zhang, Zhenzhu; Liu, Xinyu; Li, Aizhu; Hou, Zhiguo; Wang, Yuming; Zhang, Yanjun

2015-08-28

This study combines solid phase extraction (SPE) using 96-well plates with column-switching technology to construct a rapid and high-throughput method for the simultaneous extraction and non-targeted analysis of small molecules metabolome and lipidome based on ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry. This study first investigated the columns and analytical conditions for small molecules metabolome and lipidome, separated by an HSS T3 and BEH C18 columns, respectively. Next, the loading capacity and actuation duration of SPE were further optimized. Subsequently, SPE and column switching were used together to rapidly and comprehensively analyze the biological samples. The experimental results showed that the new analytical procedure had good precision and maintained sample stability (RSD<15%). The method was then satisfactorily applied to more widely analyze the small molecules metabolome and lipidome to test the throughput. The resulting method represents a new analytical approach for biological samples, and a highly useful tool for researches in metabolomics and lipidomics. Copyright © 2015 Elsevier B.V. All rights reserved.

A Column Experiment To Determine Black Shale Degradation And Colonization By Means of δ13C and 14C Analysis Of Phospholipid Fatty Acids And DNA Extraction

NASA Astrophysics Data System (ADS)

Seifert, A.; Gleixner, G.

2008-12-01

We investigated the degradation of black shale organic matter by microbial communities. We inoculated two columns respectively, with the fungi Schizophyllum commune, the gram-positive bacterium Pseudomonas putida and the gram-negative bacteria Streptomyces griseus and Streptomyces chartreusis. These microorganisms are known to degrade a wide variety of organic macromolecules. Additionally, we had two sets of control columns. To one set the same nutrient solution was added as to the inoculated columns and to the other set only sterile deionised water was supplied. All columns contained 1.5 kg of freshly crushed not autoclaved black shale material with a particle size of 0.63-2 mm. The columns were incubated at 28° C and 60% humidity in the dark. The aim was to investigate, which microorganisms live on black shales and if these microorganisms are able to degrade ancient organic matter. We used compound specific stable isotope measurement techniques and compound specific 14C-dating methods. After 183 days PLFAs were extracted from the columns to investigate the microbial community, furthermore we extracted on one hand total-DNA of column material and on the other hand DNA from pure cultures isolates which grew on Kinks-agar B, Starch-casein-nitrate-agar (SCN) and on complete-yeast-medium-agar (CYM). According to the PLFA analysis bacteria dominated in the columns, whereas in pure cultures more fungi were isolated. A principal component analysis revealed differences between the columns in accordance with the inoculation, but it seems that the inoculated microorganisms were replaced by the natural population. For AMS measurements palmitic acid (C 16:0) was re-isolated from total-PLFA-extract with a preparative fraction collector (PFC). Preliminary results of the study revealed that microorganisms are able to degrade black shale material and that PLFA analysis are useful methods to be combined with analysis of stable isotope and 14C measurements to study microbial degradation processes.

Mechanisms involved in the relaxant action of the ethanolic extract of propolis in the guinea-pig trachea in-vitro.

PubMed

Paulino, Niraldo; Scremin, Fernando M; Raichaski, Lisiane B; Marcucci, Maria Cristina; Scremin, Amarilis; Calixto, João B

2002-06-01

This study examines the mechanisms by which the standardised ethanolic extract of propolis induces relaxation of the guinea-pig trachea in-vitro. In guinea-pig trachea with or without epithelium and contracted by histamine, the propolis extract caused reproducible and graded relaxation, with a mean EC50 value of 3.8 or 10.5 microg mL(-1) and Emax of 100%, respectively. The propolis extract-induced relaxation was markedly reduced (26+/-9 and 96+/-3%) when guinea-pig tracheas were exposed to Krebs solution containing elevated K+ in the medium (40 or 80 mM). Pre-incubation of guinea-pig tracheas with tetraethylamonium (100 mM) or with 4-aminopyridine (10mM) reduced the propolis extract-induced relaxation by 31+/-10% and 28+/-2%. Likewise, apamin (0.1 microM), charybdotoxin (0.1 microM) or iberiotoxin (0.1 microM) caused marked inhibition of propolis extract-mediated relaxation in guinea-pig trachea (percentage of inhibition: 65+/-3%, 60+/-5% and 65+/-9%, respectively). Also, glibenclamide (1 microM) inhibited the relaxant response caused by the propolis extract by 57+/-4%. Omega-conotoxin GIVA (0.1 microM) or capsaicin (1 microM) produced small but significant inhibition (30+/-5% or 47+/-7%, respectively) of the propolis extract-induced relaxation. The vasoactive intestinal peptide (VIP) antagonist D-p-Cl-Phe6,Leu17[VIP] porcine (0.1 microM) inhibited relaxation by 55+/-5%, while propranolol (1 microM) induced a parallel rightward displacement (about 20 fold) of the propolis extract concentration-response curve. Finally, the propolis extract-induced relaxation was inhibited by the nitric oxide synthase inhibitor L-N(G)-nitroarginine (L-NOArg, 100 microM) (48+/-6%), and by the soluble guanylatecyclase inhibitormethylene blue (10 microM) (37+/-6%), whilethe moreselectivesoluble guanylate cyclase inhibitor 1H-[1,2,4]oxadiazolol[4,3-alquinoxalin-1-one (ODQ, 1 microM) produced only a parallel (about 3 fold) rightward displacement of the propolis extract concentration-response curve. Collectively, these results support the notion that the propolis extract-mediated relaxation in the guinea-pig trachea involves the release of nitric oxide, probably from sensory neurons, besides the activation of soluble guanylate cyclase and activation of Ca2+- and ATP-sensitive K+ channels. Furthermore, the stimulation of beta2-adrenergic and VIP receptors also seems to account for its relaxant action.

Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching

NASA Technical Reports Server (NTRS)

Song, Q.; Putcha, L.; Harm, D. L. (Principal Investigator)

2001-01-01

A chromatographic method for the quantitation of promethazine (PMZ) and its three metabolites in urine employing on-line solid-phase extraction and column-switching has been developed. The column-switching system described here uses an extraction column for the purification of PMZ and its metabolites from a urine matrix. The extraneous matrix interference was removed by flushing the extraction column with a gradient elution. The analytes of interest were then eluted onto an analytical column for further chromatographic separation using a mobile phase of greater solvent strength. This method is specific and sensitive with a range of 3.75-1400 ng/ml for PMZ and 2.5-1400 ng/ml for the metabolites promethazine sulfoxide, monodesmethyl promethazine sulfoxide and monodesmethyl promethazine. The lower limits of quantitation (LLOQ) were 3.75 ng/ml with less than 6.2% C.V. for PMZ and 2.50 ng/ml with less than 11.5% C.V. for metabolites based on a signal-to-noise ratio of 10:1 or greater. The accuracy and precision were within +/- 11.8% in bias and not greater than 5.5% C.V. in intra- and inter-assay precision for PMZ and metabolites. Method robustness was investigated using a Plackett-Burman experimental design. The applicability of the analytical method for pharmacokinetic studies in humans is illustrated.

Phenylboronic acid modified solid-phase extraction column: Preparation, characterization, and application to the analysis of amino acids in sepia capsule by removing the maltose.

PubMed

Guo, Mengzhe; Yin, Dengyang; Han, Jie; Zhang, Liyan; Li, Xiao; He, Dandan; Du, Yan; Tang, Daoquan

2016-09-01

Maltose, a common auxiliary material of pharmaceutical preparation, may disturb the analysis of total amino acids in sepia capsule by aldolization. Therefore, it is necessary to remove the maltose through a convenient method. In this work, a phenylboronic acid modified solid-phase extraction column has been synthesized and used to remove the maltose. The materials were synthesized by one step "thiol-ene" reaction and the parameters of the column such as absorption capacity, recovery, and absorption specificity have been investigated. The results showed the column (0.5 cm of length × 0.5 cm of inner diameter) can absorb 4.6 mg maltose with a linear absorption and absorption specificity. Then this technique was applied in the quantification of amino acids in sepia capsule. After the optimization of the method, four kinds of amino acids, which were the most abundant, were quantified by high-performance liquid chromatography with diode array detection. The amounts of the four kinds of amino acids are 1.5∼2 times more than that without the treatment of solid-phase extraction column, which almost overcomes the influence of the maltose. All the results indicate that the phenylboronic acid modified solid-phase extraction column can successfully help to accurately quantify the total amino acids in sepia capsule. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids.

PubMed

Yahaya, Noorfatimah; Sanagi, Mohd Marsin; Abd Aziz, Noorizan; Wan Ibrahim, Wan Aini; Nur, Hadi; Loh, Saw Hong; Kamaruzaman, Sazlinda

2017-02-01

A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C 18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile-0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1-10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3-114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis. Copyright © 2016 John Wiley & Sons, Ltd.

Longevity of granular iron in groundwater treatment processes: corrosion product development.

PubMed

Kohn, Tamar; Livi, Kenneth J T; Roberts, A Lynn; Vikesland, Peter J

2005-04-15

Permeable reactive barriers employing iron as a reactive surface have received extensive attention. A remaining issue, however, relates to their longevity. As an integral part of a long-term column study conducted to examine the influence of inorganic cosolutes on iron reactivity toward chlorinated solvents and nitroaromatic compounds, Master Builder iron grains were characterized via scanning and transmission electron microscopy, electron energy loss spectroscopy (EELS), micro-Raman spectroscopy, and X-ray diffraction. Prior to exposure to carbonate solutions, the iron grains were covered by a surface scale that consisted of fayalite (Fe2SiO4), wüstite (FeO), magnetite (Fe3O4), maghemite (gamma-Fe2O3), and graphite. After 1100 days of exposure to solutions containing carbonate, other inorganic solutes, and organic contaminants, the wüstite, fayalite, and graphite of the original scale partially dissolved, and magnetite and iron carbonate hydroxide (Fe3(OH)2.2CO3) precipitated on top of the scale. Raman results indicate the presence of green rust (e.g., [Fe4(2+)Fe2(3+)(OH)12]-[CO3 x 2H2O]) toward the column outlet after 308 days of operation, although this mineral phase disappears at longer operation times. Grains extracted from a column exposed to a high concentration (20 mM) of sodium bicarbonate were more extensively weathered than those from columns exposed to 2 mM sodium bicarbonate. An iron carbonate hydroxide layer up to 100 microm thick was observed. Even though EELS analysis of iron carbonate hydroxide indicates that this is a redox-active phase, the thickness of this layer is presumed responsible for the previously observed decline in the reactivity of this column relative to low-bicarbonate columns. A silica-containing feed resulted in reduced reactivity toward TCE. Grains from this column had a strong enrichment of silicon in the precipitates, although no distinct silica-containing mineral phases were identified. The substitution of 2 mM calcium carbonate for 2 mM sodium bicarbonate in the feed did not produce a measurable reactivity loss, asthe discrete calcium carbonate precipitates that formed in this system did not severely restrict access to the reactive surface.

Study of axial mixing, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column using radiotracer technique.

PubMed

Ghiyas Ud Din; Imran Rafiq Chughtai; Hameed Inayat, Mansoor; Hussain Khan, Iqbal

2009-01-01

Axial mixing, holdup and slip velocity of dispersed phase which are parameters of fundamental importance in the design and operation of liquid-liquid extraction pulsed sieve plate columns have been investigated. Experiments for residence time distribution (RTD) analysis have been carried out for a range of pulsation frequency and amplitude in a liquid-liquid extraction pulsed sieve plate column with water as dispersed and kerosene as continuous phase using radiotracer technique. The column was operated in emulsion region and (99m)Tc in the form of sodium pertechnetate eluted from a (99)Mo/(99m)Tc generator was used to trace the dispersed phase. Axial dispersed plug flow model with open-open boundary condition and two points measurement method was used to simulate the hydrodynamics of dispersed phase. It has been observed that the axial mixing and holdup of dispersed phase increases with increase in pulsation frequency and amplitude until a maximum value is achieved while slip velocity decreases with increase in pulsation frequency and amplitude until it approaches a minimum value. Short lived and low energy radiotracer (99m)Tc in the form of sodium pertechnetate was found to be a good water tracer to study the hydrodynamics of a liquid-liquid extraction pulsed sieve plate column operating with two immiscible liquids, water and kerosene. Axial dispersed plug flow model with open-open boundary condition was found to be a suitable model to describe the hydrodynamics of dispersed phase in the pulsed sieve plate extraction column.

Quantitative high-throughput determination of endogenous retinoids in human plasma using triple-stage liquid chromatography/tandem mass spectrometry.

PubMed

Gundersen, Thomas E; Bastani, Nasser E; Blomhoff, Rune

2007-01-01

A high-throughput ultrasensitive analytical method based on liquid chromatography with positive ion atmospheric pressure chemical ionization (APCI) coupled to tandem mass spectrometric detection (LC/MS/MS) was developed for the determination of all-trans-4-oxo-retinoic acid (at4oxoRA), 13-cis-4-oxo-retinoic acid (13c4oxoRA), 13-cis-retinoic acid (13cRA), all-trans-retinoic acid (atRA) and all-trans-retinol (atROH) in human plasma. A stable isotope of atRA was used as internal standard (IS). The analytes and IS were isolated from 100 microL plasma by acetonitrile mono-phase extraction (MPE) performed in black 96-well microtiterplates. A 100 microL injection was focused on-column and chromatographed on an Agilent ZORBAX SB-C18 rapid-resolution high-throughput (RRHT) column with 1.8-microm particles (4.6 mmx50 mm) maintained at 60 degrees C. The initial mobile phase composition was acetonitrile/water/formic acid (10:90:0.1, v/v/v) delivered at 1.8 mL/min. Elution was accomplished by a fast gradient to acetonitrile/methanol/formic acid (90:10:0.1, v/v/v). The method had a chromatographic total run time of 7 min. An Applied Biosystems 4000 Q TRAP linear tandem mass spectrometer equipped with a heated nebulizer (APCI) ionization source was operated in multiple reaction monitoring (MRM) mode with the precursor-to-product ion transitions m/z 315.4-->297 (4-oxo-retinoic acids), 301.2-->205 (retinoic acids), 305.0-->209 (IS) and 269.2-->93 (retinol) used for quantification. The assay was fully validated and found to have acceptable accuracy, precision, linearity, sensitivity and selectivity. The mean extraction recoveries from spiked plasma samples were 80-105% for the various retinoids at three different levels. The intra-day accuracy of the assay was within 8% of nominal and intra-day precision was better than 8% coefficient of variance (CV) for retinoic acids. Inter-day precision results for quality control samples run over a 12-day period alongside clinical samples showed mean precision better than 12.5% CV. The limit of quantification was in the range of 0.1-0.2 ng/mL and the mass limit of detection (mLOD) was in the range 1-4 pg on column for the retinoic acids. The assay has been successfully applied to the analysis of 1700 plasma samples. Copyright (c) 2007 John Wiley & Sons, Ltd.

Silica particles encapsulated poly(styrene-divinylbenzene) monolithic stationary phases for micro-high performance liquid chromatography.

PubMed

Bakry, R; Stöggl, W M; Hochleitner, E O; Stecher, G; Huck, C W; Bonn, G K

2006-11-03

In the paper we demonstrate a new approach for the preparation and application of continuous silica bed columns that involve encapsulation (entrapment) of functionalized silica microparticles, which can be used as packing material in micro high performance liquid chromatography (micro-HPLC) and capillary electrochromatography (CEC). Like traditional packed columns, these capillaries possess characterized silica particles that offer high phase ratio and narrow pore size distribution leading to high retention and separation efficiency, respectively. More importantly, immobilization of the microparticles stabilizes the separation bed and eliminates the need for retaining frits. The developed capillary columns were fabricated in exactly the same way as a packed capillary column (slurry packing) but with an additional entrapment step. This immobilization of the packed bed was achieved by in situ polymerization of styrene and divinylbenzene in presence of decanol as a porogen and azobisisobutyronitrile as thermal initiator. Silica particles with different particle sizes and pore sizes ranging from 60 to 4000 A were studied. In addition different modified silica was used, including C-18 reversed phase, anion exchange and chiral stationary phases. Efficient separation of polyphenolic compounds, peptides, proteins and even DNA mutation were achieved using the developed technique depending on the properties of the silica particles used (particles pore size). For example, using 3 microm ProntoSIL C-18 particles with 300 A pore size, separation efficiencies in the range of 120,000-200,000 plates/m were obtained for protein separation, in a 6 cm x 200 microm i.d. capillary column. Using encapsulated silica C-18 with 1000 A pore size, separation of DNA homo and hetero duplexes were achieved under denaturing HPLC conditions for mutation detection. In addition, nucleotides were separated using anion exchange material encapsulated with poly(styrene-divinylbenzene) (PS/DVB), which indicated that the chromatographic properties of the silica packing material were still active after polymerization. The prepared capillary columns were found to be stable and could easily be operated continuously up to a pressure of 350 bar without column damage and capillary can be cut to any desired length.

ANALYSIS OF FERRIC AND FERROUS IONS IN SOIL EXTRACTS BY ION CHROMATOGRAPHY

EPA Science Inventory

A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

[Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

PubMed

Lü, Weichao; Shen, Shuchang; Wang, Chao

2017-11-08

With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

Sequential injection-bead injection-lab-on-valve coupled to high-performance liquid chromatography for online renewable micro-solid-phase extraction of carbamate residues in food and environmental samples.

PubMed

Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax; Grudpan, Kate

2011-07-01

A sequential injection-bead injection-lab-on-valve system was hyphenated to HPLC for online renewable micro-solid-phase extraction of carbamate insecticides. The carbamates studied were isoprocarb, methomyl, carbaryl, carbofuran, methiocarb, promecarb, and propoxur. LiChroprep(®) RP-18 beads (25-40 μm) were employed as renewable sorbent packing in a microcolumn situated inside the LOV platform mounted above the multiposition valve of the sequential injection system. The analytes sorbed by the microcolumn were eluted using 80% acetonitrile in 0.1% acetic acid before online introduction to the HPLC system. Separation was performed on an Atlantis C-18 column (4.6 × 150 mm, 5 μm) utilizing gradient elution with a flow rate of 1.0 mL/min and a detection wavelength at 270 nm. The sequential injection system offers the means of performing automated handling of sample preconcentration and matrix removal. The enrichment factors ranged between 20 and 125, leading to limits of detection (LODs) in the range of 1-20 μg/L. Good reproducibility was obtained with relative standard deviations of <0.7 and 5.4% for retention time and peak area, respectively. The developed method has been successfully applied to the determination of carbamate residues in fruit, vegetable, and water samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Feature extraction of micro-motion frequency and the maximum wobble angle in a small range of missile warhead based on micro-Doppler effect

NASA Astrophysics Data System (ADS)

Li, M.; Jiang, Y. S.

2014-11-01

Micro-Doppler effect is induced by the micro-motion dynamics of the radar target itself or any structure on the target. In this paper, a simplified cone-shaped model for ballistic missile warhead with micro-nutation is established, followed by the theoretical formula of micro-nutation is derived. It is confirmed that the theoretical results are identical to simulation results by using short-time Fourier transform. Then we propose a new method for nutation period extraction via signature maximum energy fitting based on empirical mode decomposition and short-time Fourier transform. The maximum wobble angle is also extracted by distance approximate approach in a small range of wobble angle, which is combined with the maximum likelihood estimation. By the simulation studies, it is shown that these two feature extraction methods are both valid even with low signal-to-noise ratio.

Extracting alveolar structure of human lung tissue specimens based on surface skeleton representation from 3D micro-CT images

NASA Astrophysics Data System (ADS)

Ishimori, Hiroyuki; Kawata, Yoshiki; Niki, Noboru; Nakaya, Yoshihiro; Ohmatsu, Hironobu; Matsui, Eisuke; Fujii, Masashi; Moriyama, Noriyuki

2007-03-01

We have developed a Micro CT system for understanding lung function at a high resolution of the micrometer order (up to 5µm in spatial resolution). Micro CT system enables the removal specimen of lungs to be observed at micro level, has expected a big contribution for micro internal organs morphology and the image diagnosis study. In this research, we develop system to visualize lung microstructures in three dimensions from micro CT images and analyze them. They characterize in that high CT value of the noise area is, and the difficulty of only using threshold processing to extract the alveolar wall of micro CT images. Thus, we are developing a method of extracting the alveolar wall with surface thinning algorithm. In this report, we propose the method which reduces the excessive degeneracy of figure which caused by surface thinning process. And, we apply this algorithm to the micro CT image of the actual pulmonary specimen. It is shown that the extraction of the alveolus wall becomes possible in the high precision.

Interactions between polystyrene microplastics and marine phytoplankton lead to species-specific hetero-aggregation.

PubMed

Long, Marc; Paul-Pont, Ika; Hégaret, Hélène; Moriceau, Brivaela; Lambert, Christophe; Huvet, Arnaud; Soudant, Philippe

2017-09-01

To understand the fate and impacts of microplastics (MP) in the marine ecosystems, it is essential to investigate their interactions with phytoplankton as these may affect MP bioavailability to marine organisms as well as their fate in the water column. However, the behaviour of MP with marine phytoplanktonic cells remains little studied and thus unpredictable. The present study assessed the potential for phytoplankton cells to form hetero-aggregates with small micro-polystyrene (micro-PS) particles depending on microalgal species and physiological status. A prymnesiophycea, Tisochrysis lutea, a dinoflagellate, Heterocapsa triquetra, and a diatom, Chaetoceros neogracile, were exposed to micro-PS (2 μm diameter; 3.96 μg L -1 ) during their growth culture cycles. Micro-PS were quantified using an innovative flow-cytometry approach, which allowed the monitoring of the micro-PS repartition in microalgal cultures and the distinction between free suspended micro-PS and hetero-aggregates of micro-PS and microalgae. Hetero-aggregation was observed for C. neogracile during the stationary growth phase. The highest levels of micro-PS were "lost" from solution, sticking to flasks, with T. lutea and H. triquetra cultures. This loss of micro-PS sticking to the flask walls increased with the age of the culture for both species. No effects of micro-PS were observed on microalgal physiology in terms of growth and chlorophyll fluorescence. Overall, these results highlight the potential for single phytoplankton cells and residual organic matter to interact with microplastics, and thus potentially influence their distribution and bioavailability in experimental systems and the water column. Copyright © 2017 Elsevier Ltd. All rights reserved.

Lethality and bioaccumulation of 4-nonylphenol in bluegill sunfish in littoral enclosures

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

Liber, K.; Gangl, J.A.; Corry, T.D.

1999-03-01

Toxicity and bioaccumulation in bluegill sunfish (Lepomis macrochirus) of 4-nonylphenol (NP), a common precursor and degradation intermediate of certain nonionic surfactants, were evaluated in a set of 18 aquatic mesocosms (littoral enclosures) in northeastern Minnesota. Nonylphenol was applied to enclosures every 48 h over a 20-d period (11 applications) at rates of 3, 30, 100, and 300 {micro}g/L. Additional enclosures served as untreated controls. Maximum NP levels in the integrated water column 2 h after each application averaged 5 {+-} 4, 23 {+-} 11, 76 {+-} 21, and 243 {+-} 41 {micro}g/L over the 11 applications at the 3-, 30-,more » 100-, and 300-{micro}g/L treatments, respectively. Sixty-one percent of the NP dissipated from the water column within {approximately} 39 h of each application. Estimated survival of stocked juvenile bluegills was significantly reduced at the 300-{micro}g/L NP treatment. No significant effects were noted at the other NP treatments; however, the 100-{micro}g/L enclosure with the highest mean NP concentration (93 {+-} 39 {micro}g/L) within that treatment had four to nine times more dead bluegills and four to six times fewer bluegills captured at the end of the season than the other two 100-{micro}g/L enclosures (64 {+-} 23 and 71 {+-} 32 {micro}g/L) and the controls, suggesting increased mortality in this enclosure. Nonylphenol tissue concentrations in juvenile bluegills collected from enclosures treated with 3 and 30 {micro}g/L NP ranged from 0.01 to 2.94 {micro}g/g wet weight and showed a significant positive relationship with the average measured NP concentration in the water. The mean wet weight nonequilibrium NP bioaccumulation factor was 87 {+-} 124. There was no relationship between fish lipid content and NP tissue concentration.« less

Liquid-chromatographic analysis for cyclosporine with use of a microbore column and small sample volume.

PubMed

Annesley, T; Matz, K; Balogh, L; Clayton, L; Giacherio, D

1986-07-01

This liquid-chromatographic assay requires 0.2 to 0.5 mL of whole blood, avoids the use of diethyl ether, and consumes only 10 to 20% of the solvents used in prior methods. Sample preparation involves an acidic extraction with methyl-t-butyl ether, performed in a 13 X 100 mm disposable glass tube, then a short second extraction of the organic phase with sodium hydroxide. After evaporation of the methyl-t-butyl ether, chromatography is performed on an "Astec" 2.0-mm (i.d.) octyl column. We compared results by this procedure with those by use of earlier larger-scale extractions and their respective 4.6-mm (i.d.) columns; analytical recoveries of cyclosporins A and D were comparable with previous findings and results for patients' specimens were equivalent, but the microbore columns provided greatly increased resolution and sensitivity.

LIQUID-LIQUID EXTRACTION COLUMNS

DOEpatents

Thornton, J.D.

1957-12-31

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

3D printed titanium micro-bore columns containing polymer monoliths for reversed-phase liquid chromatography.

PubMed

Gupta, Vipul; Talebi, Mohammad; Deverell, Jeremy; Sandron, Sara; Nesterenko, Pavel N; Heery, Brendan; Thompson, Fletcher; Beirne, Stephen; Wallace, Gordon G; Paull, Brett

2016-03-03

The potential of 3D selective laser melting (SLM) technology to produce compact, temperature and pressure stable titanium alloy chromatographic columns is explored. A micro bore channel (0.9 mm I.D. × 600 mm long) was produced within a 5 × 30 × 30 mm titanium alloy (Ti-6Al-4V) cuboid, in form of a double handed spiral. A poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) (BuMA-co-EDMA) monolithic stationary phase was thermally polymerised within the channel for application in reversed-phase high-performance liquid chromatography. The prepared monolithic column was applied to the liquid chromatographic separation of intact proteins and peptides. Peak capacities of 69-76 (for 6-8 proteins respectively) were observed during isothermal separation of proteins at 44 °C which were further increased to 73-77 using a thermal step gradient with programmed temperature from 60 °C to 35 °C using an in-house built direct-contact heater/cooler platform based upon matching sized Peltier thermoelectric modules. Rapid temperature gradients were possible due to direct-contact between the planar metal column and the Peltier module, and the high thermal conductivity of the titanium column as compared to a similar stainless steel printed column. The separation of peptides released from a digestion of E.coli was also achieved in less than 35 min with ca. 40 distinguishable peaks at 210 nm. Copyright © 2016 Elsevier B.V. All rights reserved.

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%.

Induction of trap formation in nematode-trapping fungi by bacteria-released ammonia.

PubMed

Su, H N; Xu, Y Y; Wang, X; Zhang, K Q; Li, G H

2016-04-01

A total of 11 bacterial strains were assayed for bacteria-induced trap formation in the nematode-trapping fungus Arthrobotrys oligospora YMF1·01883 with two-compartmented Petri dish. These strains were identified on the basis of their 16S rRNA gene sequences. Volatile organic compounds (VOCs) of eight isolates were extracted using solid-phase micro-extraction (SPME) and their structures were identified based on gas chromatography-mass spectrometry (GC-MS). At the same time, all isolates were used for quantitative measurement of ammonia by the indophenol blue method. The effects of pure commercial compounds on inducement of trap formation in A. oligospora were tested. Taken together, results demonstrated that the predominant bacterial volatile compound inducing trap formation was ammonia. Meanwhile, ammonia also played a role in other nematode-trapping fungi, including Arthrobotrys guizhouensis YMF1·00014, producing adhesive nets; Dactylellina phymatopaga YMF1·01474, producing adhesive knobs; Dactylellina cionopaga YMF1·01472, producing adhesive columns and Drechslerella brochopaga YMF1·01829, producing constricting rings. © 2016 The Society for Applied Microbiology.

Development of a rapid screening technique for organochlorine pesticides using solvent microextraction (SME) and fast gas chromatography (GC).

PubMed

de Jager, L S; Andrews, A R

2000-11-01

A novel, fast screening method for organochlorine pesticides (OCPs) in water samples has been developed. Total analysis time was less than 9 min, allowing 11 samples to be screened per hour. The relatively new technique of solvent microextraction (SME) was used to extract and preconcentrate the pesticides into a single drop of hexane. The use of a conventional carbon dioxide cryotrap was investigated for introduction of the extract onto a micro-bore (0.1 mm) capillary column for fast GC analysis. A pulsed-discharge electron capture detector was used which yielded selective and sensitive measurement of the pesticide peaks. Fast GC conditions were optimised and tested with the previously developed SME procedure. Calibration curves yielded good linearity and concentrations down to 0.25 ng mL-1 were detectable with RSD values ranging from 12.0 to 28% and LOD for most OCPs at 0.25 ng mL-1. Spiked river water samples were tested and using the developed screen we were able to differentiate between spiked samples and samples containing no OCPs.

Split Flow Online Solid-Phase Extraction Coupled with Inductively Coupled Plasma Mass Spectrometry System for One-Shot Data Acquisition of Quantification and Recovery Efficiency.

PubMed

Furukawa, Makoto; Takagai, Yoshitaka

2016-10-04

Online solid-phase extraction (SPE) coupled with inductively coupled plasma mass spectrometry (ICPMS) is a useful tool in automatic sequential analysis. However, it cannot simultaneously quantify the analytical targets and their recovery percentages (R%) in one-shot samples. We propose a system that simultaneously acquires both data in a single sample injection. The main flowline of the online solid-phase extraction is divided into main and split flows. The split flow line (i.e., bypass line), which circumvents the SPE column, was placed on the main flow line. Under program-controlled switching of the automatic valve, the ICPMS sequentially measures the targets in a sample before and after column preconcentration and determines the target concentrations and the R% on the SPE column. This paper describes the system development and two demonstrations to exhibit the analytical significance, i.e., the ultratrace amounts of radioactive strontium ( 90 Sr) using commercial Sr-trap resin and multielement adsorbability on the SPE column. This system is applicable to other flow analyses and detectors in online solid phase extraction.

Pretreatment method for immunoassay of polychlorinated biphenyls in transformer oil using multilayer capillary column and microfluidic liquid-liquid partitioning.

PubMed

Aota, Arata; Date, Yasumoto; Terakado, Shingo; Ohmura, Naoya

2013-01-01

Polychlorinated biphenyls (PCBs) are persistent organic pollutants that are present in the insulating oil inside a large number of transformers. To aid in eliminating PCB-contaminated transformers, PCBs in oil need to be measured using a rapid and cost-effective analytical method. We previously reported a pretreatment method for the immunoassay of PCBs in oil using a large-scale multilayer column and a microchip with multiple microrecesses, which permitted concentrated solvent extraction. In this paper, we report on a more rapid and facile pretreatment method, without an evaporation process, by improving the column and the microchip. In a miniaturized column, the decomposition and separation of oil were completed in 2 min. PCBs can be eluted from the capillary column at concentrations seven-times higher than those from the previous column. The total volume of the microrecesses was increased by improving the microrecess structure, the enabling extraction of four-times the amount of PCBs achieved with the previous system. By interfacing the capillary column with the improved microchip, PCBs in the eluate from the column were extracted into dimethyl sulfoxide in microrecesses with high enrichment and without the need for evaporation. Pretreatment was completed within 20 min. The pretreated oil was analyzed using a flow-based kinetic exclusion immunoassay. The limit of detection of PCBs in oil was 0.15 mg kg(-1), which satisfies the criterion set in Japan of 0.5 mg kg(-1).

Blind column selection protocol for two-dimensional high performance liquid chromatography.

PubMed

Burns, Niki K; Andrighetto, Luke M; Conlan, Xavier A; Purcell, Stuart D; Barnett, Neil W; Denning, Jacquie; Francis, Paul S; Stevenson, Paul G

2016-07-01

The selection of two orthogonal columns for two-dimensional high performance liquid chromatography (LC×LC) separation of natural product extracts can be a labour intensive and time consuming process and in many cases is an entirely trial-and-error approach. This paper introduces a blind optimisation method for column selection of a black box of constituent components. A data processing pipeline, created in the open source application OpenMS®, was developed to map the components within the mixture of equal mass across a library of HPLC columns; LC×LC separation space utilisation was compared by measuring the fractional surface coverage, fcoverage. It was found that for a test mixture from an opium poppy (Papaver somniferum) extract, the combination of diphenyl and C18 stationary phases provided a predicted fcoverage of 0.48 and was matched with an actual usage of 0.43. OpenMS®, in conjunction with algorithms designed in house, have allowed for a significantly quicker selection of two orthogonal columns, which have been optimised for a LC×LC separation of crude extractions of plant material. Copyright © 2016 Elsevier B.V. All rights reserved.

Polymeric monolith column composited with multiwalled carbon nanotubes-β-cyclodextrin for the selective extraction of psoralen and isopsoralen.

PubMed

Ling, Xu; Zou, Li; Chen, Zilin

2017-09-01

A polymeric column that contains multiwalled carbon nanotubes-β-cyclodextrin composite was developed. The composite was wrapped into the poly(butyl methacrylate-ethylene dimethacrylate) monolith column (0.76 mm id and 10 cm in length). The column was then applied for the online solid-phase microextraction of psoralen and isopsoralen from Fructus Psoraleae. Following microextraction, the coumarins were quantified by high-performance liquid chromatography with C 18 separation column and UV detection. The effects of sample flow rate, sample volume, and pH value were optimized. The method showed low limits of detection (20 pg/mL, S/N = 3) for both psoralen and isopsoralen. Finally the method was successfully applied to the determination of psoralen and isopsoralen in spiked herb extracts and rat plasma where it gave recoveries that ranged between 93.2 and 102.1%. The empty hydrophobic cavities of β-cyclodextrin and the hydrophobicity of multiwalled carbon nanotubes provided specific extraction capability for psoralen and isopsoralen. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Moderate-Use Pesticides and Selected Degradates in Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Sandstrom, Mark W.; Stroppel, Max E.; Foreman, William T.; Schroeder, Michael P.

2001-01-01

A method for the isolation and analysis of 21 parent pesticides and 20 pesticide degradates in natural-water samples is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase-extraction columns that contain octadecyl-bonded porous silica to extract the analytes. The columns are dried by using nitrogen gas, and adsorbed analytes are eluted with ethyl acetate. Extracted analytes are determined by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 2 micrograms per liter (?g/L) for most analytes. Single-operator method detection limits in reagent-water samples range from 0.00 1 to 0.057 ?g/L. Validation data also are presented for 14 parent pesticides and 20 degradates that were determined to have greater bias or variability, or shorter holding times than the other compounds. The estimated maximum holding time for analytes in pesticide-grade water before extraction was 4 days. The estimated maximum holding time for analytes after extraction on the dry solid-phase-extraction columns was 7 days. 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. The method complements existing U.S. Geological Survey Method O-1126-95 (NWQL Schedules 2001 and 2010) by using identical sample preparation and comparable instrument analytical conditions so that sample extracts can be analyzed by either method to expand the range of analytes determined from one water sample.

Rapid analysis of pharmaceuticals and personal care products in fish plasma micro-aliquots using liquid chromatography tandem mass spectrometry.

PubMed

Chen, Fangfang; Gong, Zhiyuan; Kelly, Barry C

2015-02-27

A sensitive analytical method based on liquid-liquid extraction (LLE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for rapid analysis of 11 pharmaceuticals and personal care products (PPCPs) in fish plasma micro-aliquots (∼20μL). Target PPCPs included, bisphenol A, carbamazepine, diclofenac, fluoxetine, gemfibrozil, ibuprofen, naproxen, risperidone, sertraline, simvastatin and triclosan. A relatively quicker and cheaper LLE procedure exhibited comparable analyte recoveries with solid-phase extraction. Rapid separation and analysis of target compounds in fish plasma extracts was achieved by employing a high efficiency C-18 HPLC column (Agilent Poroshell 120 SB-C18, 2.1mm×50mm, 2.7μm) and fast polarity switching, enabling effective monitoring of positive and negative ions in a single 9min run. With the exception of bisphenol A, which exhibited relatively high background contamination, method detection limits of individual PPCPs ranged between 0.15 and 0.69pg/μL, while method quantification limits were between 0.05 and 2.3pg/μL. Mean matrix effect (ME) values ranged between 65 and 156% for the various target analytes. Isotope dilution quantification using isotopically labelled internal surrogates was utilized to correct for signal suppression or enhancement and analyte losses during sample preparation. The method was evaluated by analysis of 20μL plasma micro-aliquots collected from zebrafish (Danio rerio) from a laboratory bioaccumulation study, which included control group fish (no exposure), as well as fish exposed to environmentally relevant concentrations of PPCPs. Using the developed LC-MS/MS based method, concentrations of the studied PPCPs were consistently detected in the low pg/μL (ppb) range. The method may be useful for investigations requiring fast, reliable concentration measurements of PPCPs in fish plasma. In particular, the method may be applicable for in situ contaminant biomonitoring, as well as bioaccumulation and toxicology studies employing small fishes with low blood compartment volumes. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of Cloretazine (VNP40101M) and its active metabolite (VNP4090CE) in human plasma by liquid chromatography electrospray tandem mass spectrometry (LC-ESI-MS/MS).

PubMed

Bai, Feng; Minkin, Patton; Fraga, Charles H; O'Shaughnessy, Melinda A; Gururangan, Sri; Stewart, Clinton F

2007-06-15

A sensitive method for the determination of Cloretazine (VNP40101M) and its metabolite (VNP4090CE) with an internal standard (ISTD) in human plasma was developed using high-performance liquid chromatographic separation with tandem mass spectrometric detection. Acidified plasma samples (500 microL) were prepared using solid phase extraction (SPE) columns, and 25 microL of the reconstituted sample was injected onto an Ascentis C18 HPLC column (3 microm, 5 cmx2.1 mm) with an isocratic mobile phase. Analytes were detected with an API-3000 LC-MS/MS System at unit (Q1) and low (Q3) resolution in negative multiple reaction monitoring mode: m/z 249.0 (precursor ion) to m/z 114.9 (product ion) for both Cloretazine (at 3.64 min) and VNP4090CE (at 2.91 min), and m/z 253.0 (precursor ion) to m/z 116.9 (product ion) for the ISTD. The mean recovery for Cloretazine (VNP40101M) and its metabolite (VNP4090CE) was greater than 87% with a lower limit of quantification of 1.0 ng/mL for Cloretazine (S/N=9.7, CV

FY13 Progress Report on the Phase I Mini-SHINE Water Irradiations and Micro-SHINE Irradiations

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

Youker, Amanda J.; Krebs, John F.; Kalensky, Michael

2014-02-19

The original goal of the micro-SHINE experiments was to confirm that precipitation of uranyl peroxide can be prevented by adding a catalyst such as FeSO 4 to destroy peroxide. After successfully demonstrating that FeSO 4 is an effective catalyst for peroxide destruction, subsequent micro-SHINE solutions were used as tracers to perform a Mo-separation and recovery column experiment, a sulfate-to-nitrate conversion, and iodine speciation experiments.

Rapid and sensitive ultra-high-pressure liquid chromatography-tandem mass spectrometry analysis of the novel anticancer agent PR-104 and its major metabolites in human plasma: Application to a pharmacokinetic study.

PubMed

Gu, Yongchuan; Wilson, William R

2009-10-01

PR-104 is a dinitrobenzamide mustard currently in clinical trial as a hypoxia-activated prodrug. It is converted systemically to the corresponding alcohol, PR-104A, which is activated by nitroreduction to the hydroxylamine (PR-104H) and amine (PR-104M). PR-104A is also metabolised to the O-glucuronide (PR-104G), and by oxidative debromoethylation to the semi-mustard PR-104S. We now report a validated ultra-high-pressure liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS) method for the determination of these metabolites in human plasma. Plasma proteins were precipitated with acidified methanol and the supernatant diluted into water. Aliquots were analysed by UHPLC-MS/MS using a Zorbax Eclipse XDB-C18 Rapid Resolution HT (50mmx2.1mm, 1.8microm) column and gradient of acetonitrile and 0.01% formic acid with a 6min run time. The method had a linear range of 0.1-50microM for PR-104, PR-104A and PR-104G, 0.05-5microM for PR-104H, 0.025-2.5microM for PR-104M and 0.01-1microM for PR-104S. The intra-day and inter-day precision and accuracy were within 14%. The extraction recovery of all analytes was over 87%. The validated method was illustrated by using it to study the pharmacokinetics of PR-104 and its metabolites in a human patient.

Tooth enamel surface micro-hardness with dual species Streptococcus biofilm after exposure to Java turmeric (Curcuma xanthorrhiza Roxb.) extract

NASA Astrophysics Data System (ADS)

Isjwara, F. R. G.; Hasanah, S. N.; Utami, Sri; Suniarti, D. F.

2017-08-01

Streptococcus biofilm on tooth surfaces can decrease mouth environment pH, thus causing enamel demineralization that can lead to dental caries. Java Turmeric extract has excellent antibacterial effects and can maintain S. mutans biofilm pH at neutral levels for 4 hours. To analyze the effect of Java Turmeric extract on tooth enamel micro-hardness, the Java Turmeric extract was added on enamel tooth samples with Streptococcus dual species biofilm (S. sanguinis and S. mutans). The micro-hardness of enamel was measured by Knoop Hardness Tester. Results showed that Curcuma xanthorrhiza Roxb. could not maintain tooth enamel surface micro-hardness. It is concluded that Java Turmeric extract ethanol could not inhibit the hardness of enamel with Streptococcus dual species biofilm.

Zwitterionic, cationic, and anionic fluorinated chemicals in aqueous film forming foam formulations and groundwater from U.S. military bases by nonaqueous large-volume injection HPLC-MS/MS.

PubMed

Backe, Will J; Day, Thomas C; Field, Jennifer A

2013-05-21

A new analytical method was developed to quantify 26 newly-identified and 21 legacy (e.g. perfluoroalkyl carboxylates, perfluoroalkyl sulfonates, and fluorotelomer sulfonates) per and polyfluorinated alkyl substances (PFAS) in groundwater and aqueous film forming foam (AFFF) formulations. Prior to analysis, AFFF formulations were diluted into methanol and PFAS in groundwater were micro liquid-liquid extracted. Methanolic dilutions of AFFF formulations and groundwater extracts were analyzed by large-volume injection (900 μL) high-performance liquid chromatography tandem mass spectrometry. Orthogonal chromatography was performed using cation exchange (silica) and anion exchange (propylamine) guard columns connected in series to a reverse-phase (C18) analytical column. Method detection limits for PFAS in groundwater ranged from 0.71 ng/L to 67 ng/L, and whole-method accuracy ranged from 96% to 106% for analytes for which matched authentic analytical standards were available. For analytes without authentic analytical standards, whole-method accuracy ranged from 78 % to 144 %, and whole-method precision was less than 15 % relative standard deviation for all analytes. A demonstration of the method on groundwater samples from five military bases revealed eight of the 26 newly-identified PFAS present at concentrations up to 6900 ng/L. The newly-identified PFAS represent a minor fraction of the fluorinated chemicals in groundwater relative to legacy PFAS. The profiles of PFAS in groundwater differ from those found in fluorotelomer- and electrofluorination-based AFFF formulations, which potentially indicates environmental transformation of PFAS.

On-line coupling of capillary isotachophoresis and zone electrophoresis for the assay of phenolic compounds in plant extracts.

PubMed

Urbánek, Marek; Pospísilová, Marie; Polásek, Miroslav

2002-04-01

The combination of capillary isotachophoresis (ITP) and capillary zone electrophoresis (CZE) in the column coupling configuration was optimized in a mode where the electrolyte for the CZE step is different from the leading and terminating ITP electrolytes. Two colored markers, picric acid and 1-nitroso-2-naphthol, were used for exact timing of the transfer of isotachophoretically stacked analyte zones into the CZE column and for the control of the residual amount of the leading and terminating ITP electrolytes entering the CZE capillary together with the analytes, thus controlling the duration of transient ITP migration in the CZE capillary and ensuring good separation of the analytes and reproducibility of the migration times (relative standard deviations 1%). ITP-CZE was applied to the simultaneous assay of several cinnamic acid derivatives and flavonoids in methanolic extracts of Sambucus flowers and Crataegus leaves and flowers. The preconcentrating and cleansing effect of the ITP step allowed injection of relatively large sample volumes (30 microL). The limits of detection were approximately 20-50 ng x mL(-1) and 100 ng x mL(-1) for the acids and flavonoids, respectively ( thick similar 200-times lower compared to conventional CE) with spectrophotometric detection at 254 nm. The ITP-CZE exhibited satisfactory linearity and precision when using CZE buffer of pseudo "pH" 9.0; 1-nitroso-2-naphthol was employed as the internal standard. The separation took approximately 35 min. The ITP-CZE results for rutin, hyperoside, and vitexin-2-O"-rhamnoside were in good accordance with those obtained previously by high-performance liquid chromatography.

Paired-ion chromatography and high performance liquid chromatography of labetalol in feeds.

PubMed

Townley, E R; Ross, B

1980-11-01

A high performance liquid chromatographic (HPLC) method using reverse phase paired-ion chromatography and ultraviolet detection at 280 nm has been developed to determine labetalol, an alpha and beta adrenoceptor blocking agent, in Purina No. 5001 rodent chow. The method is simple and rapid, and demonstrates a separation technique applicable to other acidic and basic drugs. It requires only extraction of the drug with methanol--water--acetic acid (66 + 33 + 1) and separation of insoluble material by filtration before HPLC. Labetalol, is chromatographically separated from soluble feed components by means of a microBondapak C18 column and methanol--water--acetic acid (66 + 33 + 1) mobile phase, 0.005M with respect to sodium dioctylsulfosuccinate paired-ion reagent. Average recovery is 98.7% with a relative standard deviation of +/- 2.3% for the equipment described.

Effects of a malfunctional column on conventional and FeedCol-simulated moving bed chromatography performance.

PubMed

Song, Ji-Yeon; Oh, Donghoon; Lee, Chang-Ha

2015-07-17

The effects of a malfunctional column on the performance of a simulated moving bed (SMB) process were studied experimentally and theoretically. The experimental results of conventional four-zone SMB (2-2-2-2 configuration) and FeedCol operation (2-2-2-2 configuration with one feed column) with one malfunctional column were compared with simulation results of the corresponding SMB processes with a normal column configuration. The malfunctional column in SMB processes significantly deteriorated raffinate purity. However, the extract purity was equivalent or slightly improved compared with the corresponding normal SMB operation because the complete separation zone of the malfunctional column moved to a lower flow rate range in zones II and III. With the malfunctional column configuration, FeedCol operation gave better experimental performance (up to 7%) than conventional SMB operation because controlling product purity with FeedCol operation was more flexible through the use of two additional operating variables, injection time and injection length. Thus, compared with conventional SMB separation, extract with equivalent or slightly better purity could be produced from FeedCol operation even with a malfunctional column, while minimizing the decrease in raffinate purity (less than 2%). Copyright © 2015 Elsevier B.V. All rights reserved.

Extraction and preparation of high-aroma and low-caffeine instant green teas by the novel column chromatographic extraction method with gradient elution.

PubMed

Li, Qing-Rong; Wu, Min; Huang, Rui-Jie; Chen, Ya-Fei; Chen, Chan-Jian; Li, Hui; Ni, He; Li, Hai-Hang

2017-06-01

The lack of aroma and natural taste is a critical problem in production and consumption of instant green teas. A method to prepare instant green teas high in-natural-aroma and low-caffeine by the novel column chromatographic extraction with gradient elution is reported. This method simultaneously extracted aroma (or volatile) and non-aroma compounds from green tea. Green tea was loaded into columns with 2.0-fold of petroleum ether (PE): ethanol (8:2). After standing for 3 h until the aroma compounds dissolved, the column was sequentially eluted with 3.0-fold 40% ethanol and 3.5-fold water. The eluant was collected together and automatically separated into PE and ethanol aqueous phases. The aroma extracts was obtained by vacuum-evaporation of PE phase at 45 °C. The ethanol aqueous phase was vacuum-concentrated to aqueous and partially or fully decaffeinated with 4% or 9% charcoal at 70 °C. A regular instant green tea with epigallocatechin-3-gallate: caffeine of 3.5:1 and a low-caffeine instant green tea (less than 1% caffeine) with excellent aroma and taste were prepared, by combining the aroma and non-aroma extracts at a 1:10 ratio. This work provides a practical approach to solve the low-aroma and low-taste problems in the production of high quality instant green teas.

The Effect of Hierarchical Micro/Nanotextured Titanium Implants on Osseointegration Immediately After Tooth Extraction in Beagle Dogs.

PubMed

Fu, Qian; Bellare, Anuj; Cui, Yajun; Cheng, Bingkun; Xu, Shanshan; Kong, Liang

2017-06-01

Owing to simplify the operation and shorten the overall duration of treatment, immediate implantation earned much satisfactory from patients and dentists. The results of immediate implantation determined by osseointegration, we fabricated a micro/nanotextured titanium implants to improve osseointegration immediately after tooth extraction. The aim of this study was to investigate the effect of hierarchical micro/nanotextured titanium implant on osseointegration immediately after tooth extraction. The micro/nanotextured titanium implants were fabricated by etching with 0.5 wt% hydrofluoric (HF) acid followed by anodization in HF electrolytes. Implants with a machined surface as well as implants a microtextured surface prepared by 0.5 wt% HF etching served as control groups. The machined, microtextured, and micro/nanotextured implants were inserted into fresh sockets immediately after tooth extraction in beagle dogs. Twelve weeks after implantation, the animals were sacrificed for micro-CT scanning, histological analysis and biomechanical test. The micro-CT imaging revealed that the bone volume/total volume (BV/TV) and trabecular thickness (Tb.Th) in the micro/nanotextured group was significantly higher than that in the machined group and microtextured group, and the trabecular separation (Tb.Sp) in the micro/nanotextured group was significantly lower than that in the other groups. For the histological analysis, the bone-to-implant contact in the machined, micro and micro/nanotextured groups were 47.13 ± 6.2%, 54.29 ± 4.18%, and 63.38 ± 7.63%, respectively, and the differences significant. The maximum pull-out force in the machined, micro, and micro/nanotextured groups were 216.58 ± 38.71 N, 259.42 ± 28.93 N, and 284.73 ± 47.09 N, respectively. The results indicated that implants with a hierarchical micro/nanotextured can promote osseointegration immediately after tooth extraction. © 2016 Wiley Periodicals, Inc.

[Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

PubMed

Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

2012-08-01

A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

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.

Hexahedral finite element mesh coarsening using pillowing technique

DOEpatents

Staten, Matthew L [Pittsburgh, PA; Woodbury, Adam C [Provo, UT; Benzley, Steven E [Provo, UT; Shepherd, Jason F [Edgewood, NM

2012-06-05

A techniques for coarsening a hexahedral mesh is described. The technique includes identifying a coarsening region within a hexahedral mesh to be coarsened. A boundary sheet of hexahedral elements is inserted into the hexahedral mesh around the coarsening region. A column of hexahedral elements is identified within the boundary sheet. The column of hexahedral elements is collapsed to create an extraction sheet of hexahedral elements contained within the coarsening region. Then, the extraction sheet of hexahedral elements is extracted to coarsen the hexahedral mesh.

An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography - A case study on the determination of bisphenol A in environmental water samples.

PubMed

Háková, Martina; Chocholoušová Havlíková, Lucie; Chvojka, Jiří; Solich, Petr; Šatínský, Dalibor

2018-02-01

Polyamide 6 nanofiber polymers were used as modern sorbents for on-line solid phase extraction (SPE) coupled with liquid chromatography. The on-line SPE system was tested for the determination of bisphenol A in river water samples. Polyamide nanofibers were prepared using needleless electrospinning, inserted into a mini-column cartridge (5 × 4.6mm) and coupled with HPLC. The effect of column packing and the amount of polyamide 6 on extraction efficiency was tested and the packing process was optimized. The proposed method was performed using a 50-µL sample injection followed by an on-line nanofibrous extraction procedure. The influence of the washing mobile phase on the retention of bisphenol A during the extraction procedure was evaluated. Ascentis ® Express C18 (10cm × 4.6mm) core-shell column was used as an analytical column. Fluorescence detection wavelengths (λ ex = 225nm and λ em = 320nm) were used for identification and quantification of Bisphenol A in river waters. The linearity was tested in the range from 2 to 500µgL -1 (using nine calibration points). The limits of detection and quantification were 0.6 and 2µgL -1 , respectively. The developed method was successfully used for the determination of bisphenol A in various samples of river waters in the Czech Republic (The Ohře, Labe, Nisa, Úpa, and Opava Rivers). Copyright © 2017 Elsevier B.V. All rights reserved.

Advanced biomaterial strategies to transplant preformed micro-tissue engineered neural networks into the brain

NASA Astrophysics Data System (ADS)

Harris, J. P.; Struzyna, L. A.; Murphy, P. L.; Adewole, D. O.; Kuo, E.; Cullen, D. K.

2016-02-01

Objective. Connectome disruption is a hallmark of many neurological diseases and trauma with no current strategies to restore lost long-distance axonal pathways in the brain. We are creating transplantable micro-tissue engineered neural networks (micro-TENNs), which are preformed constructs consisting of embedded neurons and long axonal tracts to integrate with the nervous system to physically reconstitute lost axonal pathways. Approach. We advanced micro-tissue engineering techniques to generate micro-TENNs consisting of discrete populations of mature primary cerebral cortical neurons spanned by long axonal fascicles encased in miniature hydrogel micro-columns. Further, we improved the biomaterial encasement scheme by adding a thin layer of low viscosity carboxymethylcellulose (CMC) to enable needle-less insertion and rapid softening for mechanical similarity with brain tissue. Main results. The engineered architecture of cortical micro-TENNs facilitated robust neuronal viability and axonal cytoarchitecture to at least 22 days in vitro. Micro-TENNs displayed discrete neuronal populations spanned by long axonal fasciculation throughout the core, thus mimicking the general systems-level anatomy of gray matter—white matter in the brain. Additionally, micro-columns with thin CMC-coating upon mild dehydration were able to withstand a force of 893 ± 457 mN before buckling, whereas a solid agarose cylinder of similar dimensions was predicted to withstand less than 150 μN of force. This thin CMC coating increased the stiffness by three orders of magnitude, enabling needle-less insertion into brain while significantly reducing the footprint of previous needle-based delivery methods to minimize insertion trauma. Significance. Our novel micro-TENNs are the first strategy designed for minimally invasive implantation to facilitate nervous system repair by simultaneously providing neuronal replacement and physical reconstruction of long-distance axon pathways in the brain. The micro-TENN approach may offer the ability to treat several disorders that disrupt the connectome, including Parkinson’s disease, traumatic brain injury, stroke, and brain tumor excision.

Advanced biomaterial strategies to transplant preformed micro-tissue engineered neural networks into the brain

PubMed Central

Harris, J P; Struzyna, L A; Murphy, P L; Adewole, D O; Kuo, E; Cullen, D K

2017-01-01

Objective Connectome disruption is a hallmark of many neurological diseases and trauma with no current strategies to restore lost long-distance axonal pathways in the brain. We are creating transplantable micro-tissue engineered neural networks (micro-TENNs), which are preformed constructs consisting of embedded neurons and long axonal tracts to integrate with the nervous system to physically reconstitute lost axonal pathways. Approach We advanced micro-tissue engineering techniques to generate micro-TENNs consisting of discrete populations of mature primary cerebral cortical neurons spanned by long axonal fascicles encased in miniature hydrogel micro-columns. Further, we improved the biomaterial encasement scheme by adding a thin layer of low viscosity carboxymethylcellulose (CMC) to enable needle-less insertion and rapid softening for mechanical similarity with brain tissue. Main results The engineered architecture of cortical micro-TENNs facilitated robust neuronal viability and axonal cytoarchitecture to at least 22 days in vitro. Micro-TENNs displayed discrete neuronal populations spanned by long axonal fasciculation throughout the core, thus mimicking the general systems-level anatomy of gray matter—white matter in the brain. Additionally, micro columns with thin CMC-coating upon mild dehydration were able to withstand a force of 893 ± 457 mN before buckling, whereas a solid agarose cylinder of similar dimensions was predicted to withstand less than 150 μN of force. This thin CMC coating increased the stiffness by three orders of magnitude, enabling needle-less insertion into brain while significantly reducing the footprint of previous needle-based delivery methods to minimize insertion trauma. Significance Our novel micro-TENNs are the first strategy designed for minimally invasive implantation to facilitate nervous system repair by simultaneously providing neuronal replacement and physical reconstruction of long-distance axon pathways in the brain. The micro-TENN approach may offer the ability to treat several disorders that disrupt the connectome, including Parkinson’s disease, traumatic brain injury, stroke, and brain tumor excision PMID:26760138

Development of andrographolide molecularly imprinted polymer for solid-phase extraction

NASA Astrophysics Data System (ADS)

Yin, Xiaoying; Liu, Qingshan; Jiang, Yifan; Luo, Yongming

2011-06-01

A method employing molecularly imprinted polymer (MIP) as selective sorbent for solid-phase extraction (SPE) to pretreat samples was developed. The polymers were prepared by precipitation polymerization with andrographolide as template molecule. The structure of MIP was characterized and its static adsorption capacity was measured by the Scatchard equation. In comparison with C 18-SPE and non-imprinted polymer (NIP) SPE column, MIP-SPE column displays high selectivity and good affinity for andrographolide and dehydroandrographolide for extract of herb Andrographis paniculata ( Burm.f.) Nees (APN). MIP-SPE column capacity was 11.9 ± 0.6 μmol/g and 12.1 ± 0.5 μmol/g for andrographolide and dehydroandrographolide, respectively and was 2-3 times higher than that of other two columns. The precision and accuracy of the method developed were satisfactory with recoveries between 96.4% and 103.8% (RSD 3.1-4.3%, n = 5) and 96.0% and 104.2% (RSD 2.9-3.7%, n = 5) for andrographolide and dehydroandrographolide, respectively. Various real samples were employed to confirm the feasibility of method. This developed method demonstrates the potential of molecularly imprinted solid phase extraction for rapid, selective, and effective sample pretreatment.

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

USGS Publications Warehouse

Krynitsky, A.J.; Stafford, C.J.; Wiemeyer, Stanley N.

1988-01-01

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

A hybrid monolithic column based on boronate-functionalized graphene oxide nanosheets for online specific enrichment of glycoproteins.

PubMed

Zhou, Chanyuan; Chen, Xiaoman; Du, Zhuo; Li, Gongke; Xiao, Xiaohua; Cai, Zongwei

2017-05-19

A hybrid monolithic column based on aminophenylboronic acid (APBA)-functionalized graphene oxide (GO) has been developed and used for selective enrichment of glycoproteins. The APBA/GO composites were homogeneously incorporated into a polymer monolithic column with the help of oligomer matrix and followed by in situ polymerization. The effect of dispersion of APBA/GO composites in the polymerization mixture on the performance of the monolithic column was explored in detail. The presence of graphene oxide not only enlarged the BET surface area from 6.3m 2 /g to 169.4m 2 /g, but also provided abundant boronic acid moieties for glycoprotein extraction, which improved the enrichment selectivity and efficiency for glycoproteins. The APBA/GO hybrid monolithic column was incorporated into a sequential injection system, which facilitated online extraction of proteins. Combining the superior properties of extraordinary surface area of GO and the affinity interaction of APBA to glycoproteins, the APBA/GO hybrid monolithic column showed higher enrichment factors for glycoproteins than other proteins without cis-diol-containing groups. Also, under comparable or even shorter processing time and without the addition of any organic solvent, it showed higher binding capacity toward glycoproteins compared with the conventional boronate affinity monolithic column. The practical applicability of this system was demonstrated by processing of egg white samples for extraction of ovalbumin and ovotransferrin, and satisfactory results were obtained by assay with SDS-PAGE. Copyright © 2017 Elsevier B.V. All rights reserved.

Phyto (in)stabilization of elements.

PubMed

Jacob, Donna L; Otte, Marinus L; Hopkins, David G

2011-01-01

The effects of plants (corn, soybean, and sunflower) and fertilizer on mobility of more than 60 elements were assessed in a greenhouse experiment. Unplanted columns with the same soil served as controls. Half the columns received fertilizer and all columns were watered at the same rate. At the end of the experiment, the columns were watered to mimic a rainstorm event such that water drained from the bases of the columns, which was collected and analyzed for element content. Soil from between the roots of the plants was also collected and the water-extractable fraction determined. It was expected that (1) more mobile elements, as measured by water extraction, would be leached from the soils at a higher rate compared to less mobile elements, (2) plants would immobilize most elements, but that some would be immobilized, and (3) that this would depend on plant species. The results led to the following conclusions: plants cause metal mobility to vary over a wide range for a specific soil and do mobilize some elements (e.g., Th) while immobilizing others (e.g., U). The effects depended on plant species for some elements. Water-extractable fractions of elements do not predict mobility.

Analysis of light extraction efficiency enhancement for thin-film-flip-chip InGaN quantum wells light-emitting diodes with GaN micro-domes.

PubMed

Zhao, Peng; Zhao, Hongping

2012-09-10

The enhancement of light extraction efficiency for thin-film flip-chip (TFFC) InGaN quantum wells (QWs) light-emitting diodes (LEDs) with GaN micro-domes on n-GaN layer was studied. The light extraction efficiency of TFFC InGaN QWs LEDs with GaN micro-domes were calculated and compared to that of the conventional TFFC InGaN QWs LEDs with flat surface. The three dimensional finite difference time domain (3D-FDTD) method was used to calculate the light extraction efficiency for the InGaN QWs LEDs emitting at 460nm and 550 nm, respectively. The effects of the GaN micro-dome feature size and the p-GaN layer thickness on the light extraction efficiency were studied systematically. Studies indicate that the p-GaN layer thickness is critical for optimizing the TFFC LED light extraction efficiency. Significant enhancement of the light extraction efficiency (2.5-2.7 times for λ(peak) = 460nm and 2.7-2.8 times for λ(peak) = 550nm) is achievable from TFFC InGaN QWs LEDs with optimized GaN micro-dome diameter and height.

Nanoscale petrographic and geochemical insights on the origin of the Palaeoproterozoic stromatolitic phosphorites from Aravalli Supergroup, India.

PubMed

Papineau, D; De Gregorio, B; Fearn, S; Kilcoyne, D; McMahon, G; Purohit, R; Fogel, M

2016-01-01

Stromatolites composed of apatite occur in post-Lomagundi-Jatuli successions (late Palaeoproterozoic) and suggest the emergence of novel types of biomineralization at that time. The microscopic and nanoscopic petrology of organic matter in stromatolitic phosphorites might provide insights into the suite of diagenetic processes that formed these types of stromatolites. Correlated geochemical micro-analyses of the organic matter could also yield molecular, elemental and isotopic compositions and thus insights into the role of specific micro-organisms among these communities. Here, we report on the occurrence of nanoscopic disseminated organic matter in the Palaeoproterozoic stromatolitic phosphorite from the Aravalli Supergroup of north-west India. Organic petrography by micro-Raman and Transmission Electron Microscopy demonstrates syngeneity of the organic matter. Total organic carbon contents of these stromatolitic phosphorite columns are between 0.05 and 3.0 wt% and have a large range of δ(13) Corg values with an average of -18.5‰ (1σ = 4.5‰). δ(15) N values of decarbonated rock powders are between -1.2 and +2.7‰. These isotopic compositions point to the important role of biological N2 -fixation and CO2 -fixation by the pentose phosphate pathway consistent with a population of cyanobacteria. Microscopic spheroidal grains of apatite (MSGA) occur in association with calcite microspar in microbial mats from stromatolite columns and with chert in the core of diagenetic apatite rosettes. Organic matter extracted from the stromatolitic phosphorites contains a range of molecular functional group (e.g. carboxylic acid, alcohol, and aliphatic hydrocarbons) as well as nitrile and nitro groups as determined from C- and N-XANES spectra. The presence of organic nitrogen was independently confirmed by a CN(-) peak detected by ToF-SIMS. Nanoscale petrography and geochemistry allow for a refinement of the formation model for the accretion and phototrophic growth of stromatolites. The original microbial biomass is inferred to have been dominated by cyanobacteria, which might be an important contributor of organic matter in shallow-marine phosphorites. © 2015 John Wiley & Sons Ltd.

Determination of Total Biotin by Liquid Chromatography Coupled with Immunoaffinity Column Cleanup Extraction: Multilaboratory Testing, Final Action 2016.02.

PubMed

Joseph, George; Devi, Ranjani; Marley, Elaine C; Leeman, David

2018-05-01

Single- and multilaboratory testing data have provided systematic scientific evidence that a simple, selective, accurate, and precise method can be used as a potential candidate reference method for dispute resolution in determining total biotin in all forms of infant, adult, and/or pediatric formula. Using LC coupled with immunoaffinity column cleanup extraction, the method fully meets the intended purpose and applicability statement in AOAC Standard Method Performance Requirement 2014.005. The method was applied to a cross-section of infant formula and adult nutritional matrixes, and acceptable precision and accuracy were established. The analytical platform is inexpensive, and the method can be used in almost any laboratory worldwide with basic facilities. The immunoaffinity column cleanup extraction is the key step to successful analysis.

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

PubMed

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

2007-07-23

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

Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

PubMed

Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

2015-12-01

A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Development of Molybdenum Speciation as a Paleoredox Tool

NASA Astrophysics Data System (ADS)

Rodley, J.; Peacock, C.; Mosselmans, J. F. W.; Poulton, S.

2017-12-01

The redox state of the oceans has changed throughout geological time and an understanding of these changes is essential to elucidate links between ocean chemistry, climate and life. Due to its abundance in seawater and redox-sensitive nature, molybdenum has enormous potential as a paleoredox proxy. Although a significant amount of research has been done on molybdenum in ancient and modern sediments in terms of its concentrations and isotopic ratios there remains a limited understanding of the drawdown mechanisms of molybdenum under different redox conditions restricting its use in identifying a range of redox states. In order to address these uncertainties, we have developed a novel sequential extraction technique to examine molybdenum concentrations in six sediment fractions from modern samples that represent oxic, nitrogenous, ferruginous and euxinic environments. In addition we use µ-XRF and µ-XANES synchrotron spectroscopy to examine the molybdenum speciation within these fractions and environments. To interpret our µ-XANES data we have developed an extensive library of molybdenum XANES standards that represent molybdenum sequestration by the sediment fractions identified from the sequential extraction. To further verify our synchrotron results we developed a series of µ-XANES micro-column experiments to examine preferential uptake pathways of molybdenum to different sediment phases under a euxinic water column. The initial data from both the sequential extraction and µ-XANES methods indicate that molybdenum is not limited to a single burial pathway in any of the redox environments. We find that each of the redox environments can be characterised by a limited set of molybdenum phase associations, with molybdenum adsorption to pyrite likely the dominant burial pathway. These findings agree with existing research for molybdenum speciation in euxinic environments suggesting that both pyrite and sulphidised organic matter act as important molybdenum sinks. Our new research shows that pyrite is also an important sink for molybdenum in other redox environments.

[Immunoaffinity columns and determination of ochratoxin A in cereals by HPLC. Part I.: Evaluation of extraction using methanol/water].

PubMed

Czerwiecki, Ludwik; Czyzyk, Kamila; Kwiecień, Agnieszka; Wilczyńska, Grazyna

2004-01-01

The method for ochratoxin A determination in cereals (wheat, rye) was described. Application of immunoaffinity columns (IAC) for clean-up of extracts was investigated. The ochratoxin A content was determined by high-performance liquid chromatography using C18 column and fluorimetric detection at 330 nm (excitation) and 460 nm (emission). The mean recovery of ochratoxin A was 65-78%. The limits of detection (LOD) and quantification (LOQ) were 0.015 and 0.025 microg/kg, respectively. The positive results were confirmed by reaction with BF3 complex in methanol.

Functionalized nanoparticles based solid-phase membrane micro-tip extraction and high-performance liquid chromatography analyses of vitamin B complex in human plasma.

PubMed

Ali, Imran; Kulsum, Umma; Al-Othman, Zeid A; Alwarthan, Abdulrahman; Saleem, Kishwar

2016-07-01

Iron nanoparticles were prepared by a green method following functionalization using 1-butyl-3-methylimidazolium bromide. 1-Butyl-3-methylimidazole iron nanoparticles were characterized using FTIR spectroscopy, energy dispersive X-ray fluorescence, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The nanoparticles were used in solid-phase membrane micro-tip extraction to separate vitamin B complex from plasma before high-performance liquid chromatography. The optimum conditions obtained were sorbent (15 mg), agitation time (30 min), pH (9.0), desorbing solvent [water (5 mL) + methanol (5 mL) + sodium hydroxide (0.1 N) + acetic acid (d = 1.05 kg/L, pH 5.5), desorbing volume (10 mL) and desorption time (30 min). The percentage recoveries of all the eight vitamin B complex were from 60 to 83%. A high-performance liquid chromatography method was developed using a PhE column (250 × 4.6 mm, 5.0 μm) and water/acetonitrile (95:5, v/v; pH 4.0 with 0.1% formic acid) mobile phase. The flow rate was 1.0 mL/min with detection at 270 and 210 nm. The values of the capacity, separation and resolution factor were 0.57-39.47, 1.12-6.00 and 1.84-26.26, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economic and reproducible. The developed method can be applied for analyzing these drugs in biological and environmental matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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).

Synthesis of Biofluidic Microsystems (SYNBIOSYS)

DTIC Science & Technology

2007-10-01

reaction system. 58 FIGURE 41. The micro reactor is represented by a PFR network model. The calculation of reaction and convection is conducted in...one column of PFRs and the calculation of diffusional mixing is conducted between two columns of PFRs. 59 FIGURE 42. Apply the numerical method of...lines to calculate the diffusion in the channel width direction. Here, we take 10 discretized concentration points in the channel: ci1 - ci10. Points

Sand filter clogging by septic tank effluent.

PubMed

Spychała, M; Błazejewski, R

2003-01-01

The aim of this study was to characterise conditions and factors affecting fine sand clogging by septic tank effluent on the basis of physical modelling. The physical model consisted of 12 sand columns dosed with sewage from one household (5 persons), preliminary treated in a septic tank. Hydraulic loadings of the sand filters were equal to 82 mm/d. The mean discharge from sand columns, measured as the effluent volume collected during 10 minutes, decreased significantly over the experiment period from 34 cm3/min in August 2000 to 20 cm3/min in August 2001 at the same temperature of about 20 degrees C. First the columns clogged almost completely after 480 days in December 2001, however six columns had remained unclogged till the end of the experiment (March 2002). The temperature had a significant impact on hydraulic conductivity. A vertical distribution of accumulated mass and biomass was investigated in partly clogged sand. Microscopic survey of the clogging layer showed a presence of live micro-organisms, residuals of dead micro-organisms, particularly pieces of small animal armour and many fibres. These particles accelerated the accumulation of solids in the upper clogging layer. The study indicated that temperature impact on the filter hydraulic conductivity was more significant for biological activity, than for sewage viscosity.

[Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].

PubMed

Huang, Juan; Chen, Guosong; Zhang, Xiaoyan; Shen, Chongyu; Lü, Chen; Wu, Bin; Liu, Yan; Chen, Huilan; Ding, Tao

2012-11-01

A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm x4. 6 mm, 2.6 microm) with a gradient elution using 0.3% per hundred ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N= 3) and the limit of quantification (LOQ, S/N = 10) were 20 microg/kg and 50 microg/kg, respectively. A good linearity (r > 0.99) was achieved for the target compound over the range of 20-1000 pg/L. The recoveries at the three spiked levels (50, 100, 500 microg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, cassava and wheat, were varied from 75.6% to 111.0% with the relative standard deviations no more than 13. 0%. The method is accurate, efficient, sensitive and practical. The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

Copper extraction from ammoniacal medium in a pulsed sieve-plate column with LIX 84-I.

PubMed

Gameiro, M Lurdes F; Machado, Remígio M; Ismael, M Rosinda C; Reis, M Teresa A; Carvalho, Jorge M R

2010-11-15

This article reports on a study of copper removal from ammoniacal aqueous solution (1.0 kg m(-3) Cu, pH 9.5) by liquid-liquid extraction using a pulsed sieve-plate column. The extractant tested was the hydroxyoxime LIX 84-I (2-hydroxy-5-nonylacetophenone oxime) in the aliphatic diluent Shellsol D-70. The results of the pilot plant experiments demonstrated the feasibility of operating the extraction process in this type of column, with efficiencies of copper removal in the range of 90.5-99.5%. Several effects on the column performance were examined, namely the aqueous and organic flow rates and the pulse velocity. The axial dispersion model was applied to simulate the concentration profiles, which reasonably predicted the experimental data. The overall mass transfer coefficient was evaluated from the experimental data and was found to be between 9×10(-6) and 1.2×10(-5) m s(-1). These data were compared with the ones obtained from the resistances in series model, which indicated that the resistance due to chemical reaction was 84-91% of the overall resistance to mass transfer. The extraction using a hollow fiber contactor was also carried out to compare the membrane process performance with the one of conventional process. Copyright © 2010 Elsevier B.V. All rights reserved.

[Poetry Instruction.] Motivator of the Month. [Compiled from Columns in Three issues of "Notes Plus," January and November 1984 and September 1985.

ERIC Educational Resources Information Center

Notes Plus, 1985

1985-01-01

The teaching activities presented in the four journal columns extracted here focus on understanding and writing poetry. The first column (by Carol Case) presents an introduction to poetry unit containing five preliminary steps designed to help students develop an understanding of poetry. The second column (by Carol Anderson) describes a week of…

Separation of the Components of a Commercial Analgesic Tablet: A Two-Week Sequence Comparing Purification by Two-Base Extraction and Column Chromatography

ERIC Educational Resources Information Center

Revell, Kevin D.

2011-01-01

A new laboratory experiment is described in which students compare two benchtop separation methods to isolate the three active components of the commercial analgesic Excedrin. In the two-week sequence, aspirin, acetaminophen, and caffeine are separated using either a two-base liquid-liquid extraction or silica column chromatography. Students then…

An on-line SPE-HPLC method for effective sample preconcentration and determination of fenoxycarb and cis, trans-permethrin in surface waters.

PubMed

Šatínský, Dalibor; Naibrtová, Linda; Fernández-Ramos, Carolina; Solich, Petr

2015-09-01

A new on-line SPE-HPLC method using fused-core columns for on-line solid phase extraction and large volume sample injection for increasing the sensitivity of detection was developed for the determination of insecticides fenoxycarb and cis-, trans-permethrin in surface waters. The separation was carried out on fused-core column Phenyl-Hexyl (100×4.6 mm), particle size 2.7 µm with mobile phase acetonitrile:water in gradient mode at flow rate 1.0 mL min(-1), column temperature 45°C. Large volume sample injection (1500 µL) to the extraction dimension using short precolumn Ascentis Express RP C-18 (5×4.6 mm); fused-core particle size 2.7 µm allowed effective sample preconcentration and efficient ballast sample matrix removal. The washing mobile phase consisting of a mixture of acetonitrile:water; 30:70, (v/v) was pumped at flow rate of 0.5 mL min(-1) through the extraction precolumn to the waste. Time of the valve switch for transferring the preconcentrated sample zone from the extraction to the separation column was set at 3rd min. Elution of preconcentrated insecticides from the extraction precolumn and separation on the analytical column was performed in gradient mode. Linear gradient elution started from 40% of acetonitrile at time of valve switch from SPE column (3rd min) to 95% of acetonitrile at 7th min. Synthetic dye sudan I was chosen as an internal standard. UV detection at wavelength 225 nm was used and the method reached the limits of detection (LOD) at ng mL(-1) levels for both insecticides. The method showing on-line sample pretreatment and preconcentration with highly sensitive determination of insecticides was applied for monitoring of fenoxycarb and both permethrin isomers in different surface water samples in Czech Republic. The time of whole analysis including on-line extraction, interferences removal, chromatography separation and system equilibration was less than 8 min. Copyright © 2015 Elsevier B.V. All rights reserved.

Re-evaluation of solid-phase adsorption and desorption techniques for isolation of trace organic pollutants from chlorinated water.

PubMed

Onodera, S; Nagatsuka, A; Rokuhara, T; Asakura, T; Hirayama, N; Suzuki, S

1993-07-16

Amberlite XAD resin and activated carbon columns were tested for their abilities to concentrate trace organic pollutants in chlorinated water. Both XAD-2 and XAD-7 resin columns (20 ml) were capable of adsorbing about 30% of total organic halogen (TOX) present in 20 l of drinking water (pH 7) containing about 100 micrograms/l of TOX, whereas the carbon column (10 ml) adsorbed over 90% of TOX. The adsorption capacity of XAD-7 resin was found to be strongly dependent on the solution pH, as compared with those of XAD-2 and carbon adsorbents. Soxhlet and sonication extractions were also evaluated for their abilities to recover the adsorbed organics from the adsorbents, by measurements of TOX, chromatographable compounds and mutagenicity in the eluates. Soxhlet extraction gave higher recoveries than sonication, as measured with the above indices, but these differences were generally small (ca. 20%), with exception of the carbon extracts. The XAD-2 and XAD-7 extracts of drinking water also showed about 3-4 times higher mutagenic activity than the carbon extracts.

Pore Water PAH Transport in Amended Sediment Caps

NASA Astrophysics Data System (ADS)

Gidley, P. T.; Kwon, S.; Ghosh, U.

2009-05-01

Capping is a common remediation strategy for contaminated sediments that creates a physical barrier between contaminated sediments and the water column. Diffusive flux of contaminants through a sediment cap is small. However, under certain hydrodynamic conditions such as groundwater potential and tidal pumping, groundwater advection can accelerate contaminant transport. Hydrophobic organic contaminants such as polycyclic aromatic hydrocarbons (PAHs) could be transported through the cap under advective conditions. To better understand PAH migration under these conditions, physical models of sediment caps were evaluated in the laboratory through direct measurement of pore water using solid phase micro-extraction with gas chromatography and mass spectrometry. Contaminated sediment and capping material was obtained from an existing Superfund site that was capped at Eagle Harbor, Washington. A PAH dissolution model linked to an advection-dispersion equation with retardation using published organic carbon-water partitioning coefficients (Koc) was compared to measured PAHs in the sediment and cap porewater of the physical model.

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.

Ion mobility based on column leaching of South African gold tailings dam with chemometric evaluation.

PubMed

Cukrowska, Ewa M; Govender, Koovila; Viljoen, Morris

2004-07-01

New column leaching experiments were designed and used as an alternative rapid screening approach to element mobility assessment. In these experiments, field-moist material was treated with an extracting solution to assess the effects of acidification on element mobility in mine tailings. The main advantage of this version of column leaching experiments with partitioned segments is that they give quick information on current element mobility in conditions closely simulating field conditions to compare with common unrepresentative air-dried, sieved samples used for column leaching experiments. Layers from the tailings dump material were sampled and packed into columns. The design of columns allows extracting leachates from each layer. The extracting solutions used were natural (pH 6.8) and acidified (pH 4.2) rainwater. Metals and anions were determined in the leachates. The concentrations of metals (Ca, Mg, Fe, Mn, Al, Cr, Ni, Co, Zn, and Cu) in sample leachates were determined using ICP OES. The most important anions (NO3-, Cl-, and SO4(2)-) were determined using the closed system izotacophoresis ITP analyser. The chemical analytical data from tailings leaching and physico-chemical data from field measurements (including pH, conductivity, redox potential, temperature) were used for chemometric evaluation of element mobility. Principal factor analysis (PFA) was used to evaluate ions mobility from different layers of tailings dump arising from varied pH and redox conditions. It was found that the results from the partitioned column leaching illustrate much better complex processes of metals mobility from tailings dump than the total column. The chemometric data analysis (PFA) proofed the differences in the various layers leachability that are arising from physico-chemical processes due to chemical composition of tailings dump deposit. Copyright 2004 Elsevier Ltd.

Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak's extracts

NASA Astrophysics Data System (ADS)

Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat, Suzery, Meiny

2015-12-01

Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak's extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r2=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak's extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

Enrichment of light hydrocarbon mixture

DOEpatents

Yang, Dali [Los Alamos, NM; Devlin, David [Santa Fe, NM; Barbero, Robert S [Santa Cruz, NM; Carrera, Martin E [Naperville, IL; Colling, Craig W [Warrenville, IL

2011-11-29

Light hydrocarbon enrichment is accomplished using a vertically oriented distillation column having a plurality of vertically oriented, nonselective micro/mesoporous hollow fibers. Vapor having, for example, both propylene and propane is sent upward through the distillation column in between the hollow fibers. Vapor exits neat the top of the column and is condensed to form a liquid phase that is directed back downward through the lumen of the hollow fibers. As vapor continues to ascend and liquid continues to countercurrently descend, the liquid at the bottom of the column becomes enriched in a higher boiling point, light hydrocarbon (propane, for example) and the vapor at the top becomes enriched in a lower boiling point light hydrocarbon (propylene, for example). The hollow fiber becomes wetted with liquid during the process.

Enrichment of light hydrocarbon mixture

DOEpatents

Yang,; Dali, [Los Alamos, NM; Devlin, David [Santa Fe, NM; Barbero, Robert S [Santa Cruz, NM; Carrera, Martin E [Naperville, IL; Colling, Craig W [Warrenville, IL

2010-08-10

Light hydrocarbon enrichment is accomplished using a vertically oriented distillation column having a plurality of vertically oriented, nonselective micro/mesoporous hollow fibers. Vapor having, for example, both propylene and propane is sent upward through the distillation column in between the hollow fibers. Vapor exits neat the top of the column and is condensed to form a liquid phase that is directed back downward through the lumen of the hollow fibers. As vapor continues to ascend and liquid continues to countercurrently descend, the liquid at the bottom of the column becomes enriched in a higher boiling point, light hydrocarbon (propane, for example) and the vapor at the top becomes enriched in a lower boiling point light hydrocarbon (propylene, for example). The hollow fiber becomes wetted with liquid during the process.

Identification of nonvolatile coal derived products via chromatography coupled with on-line FTIR detection. Quarterly progress report, March 1-May 31, 1985. [C/sub 2/H/sub 2/ extracts of ground coal, coffee and paprika

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

Taylor, L.T.

Because it has been our goal to interface the supercritical fluid chromatograph with a Fourier transform infrared spectrometer we have initially chosen packed columns due to their increased sample capacities, and supercritical CO/sub 2/ because of its infrared transparency. This paper compares two sampling techniques that can be utilized in packed column supercritical fluid Chromatography (SFC). Traditional sample introduction is accomplished using an injector with a sample loop. The loop is filled with the appropriate amount of material, and subsequently inserted into the mobile phase path. In most cases the sample must be either dissolved or extracted into an appropriatemore » solvent for such sample introduction. Note that unlike HPLC, where the solvent can be the same as the mobile phase, traditional sampling with SFC must use a solvent that is very different from the mobile phase. As a result, solvent peaks are almost always present, especially with universal detectors like FTIR. An alternative method is described here whereby both extraction of the sample and introduction of the extract onto the column is accomplished on-line using only the supercritical fluid mobile phase. This sampling technique is made possible by a simple valving scheme which ties directly the extraction vessel, the injector, the packed column and the detector. This technique has several advantages over the traditional methods, not the least of which is the absence of a large amount of foreign solvent introduced on the column. 11 refs., 7 figs.« less

Characterization of the efficiency of microbore liquid chromatography columns by van Deemter and kinetic plot analysis.

PubMed

Hetzel, Terence; Loeker, Denise; Teutenberg, Thorsten; Schmidt, Torsten C

2016-10-01

The efficiency of miniaturized liquid chromatography columns with inner diameters between 200 and 300 μm has been investigated using a dedicated micro-liquid chromatography system. Fully porous, core-shell and monolithic commercially available stationary phases were compared applying van Deemter and kinetic plot analysis. The sub-2 μm fully porous as well as the 2.7 μm core-shell particle packed columns showed superior efficiency and similar values for the minimum reduced plate heights (2.56-2.69) before correction for extra-column contribution compared to normal-bore columns. Moreover, the influence of extra-column contribution was investigated to demonstrate the difference between apparent and intrinsic efficiency by replacing the column by a zero dead volume union to determine the band spreading caused by the system. It was demonstrated that 72% of the intrinsic efficiency could be reached. The results of the kinetic plot analysis indicate the superior performance of the sub-2 μm fully porous particle packed column for ultra-fast liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Column chromatography isolation of nicotine from tobacco leaf extract (Nicotiana tabaccum L.)

NASA Astrophysics Data System (ADS)

Fathi, Raden Muhammad; Fauzantoro, Ahmad; Rahman, Siti Fauziyah; Gozan, Misri

2018-02-01

Restrictions on the use of dried tobacco leaf for cigarette production must be accompanied by the development of non-cigarette alternative products that are made from tobacco leaves. One of the alternative that can be done is to use the nicotine compound in tobacco leaf extract as medical product, such as Parkinson's medication or to be used as active substance in biopesticide. Nicotine was isolated using column chromatography method with the variation of mobile phase mixture ratio (petroleum ether and ethanol), started from 8:2, 6:4, 4:6, 2:8, to 0:10. All of the chromatographic fraction from each mobile phase's ratio was then tested qualitatively using thin layer chromatography (TLC) and also quantitatively using HPLC instrument. The column chromatography process could isolate 4.006% of nicotine compound from 4.19% tobacco leaf extract's nicotine. It is also known that ethanol is a good solution to be used as chromatography's mobile phase for nicotine isolation from tobacco leaf extract.

The GPU implementation of micro - Doppler period estimation

NASA Astrophysics Data System (ADS)

Yang, Liyuan; Wang, Junling; Bi, Ran

2018-03-01

Aiming at the problem that the computational complexity and the deficiency of real-time of the wideband radar echo signal, a program is designed to improve the performance of real-time extraction of micro-motion feature in this paper based on the CPU-GPU heterogeneous parallel structure. Firstly, we discuss the principle of the micro-Doppler effect generated by the rolling of the scattering points on the orbiting satellite, analyses how to use Kalman filter to compensate the translational motion of tumbling satellite and how to use the joint time-frequency analysis and inverse Radon transform to extract the micro-motion features from the echo after compensation. Secondly, the advantages of GPU in terms of real-time processing and the working principle of CPU-GPU heterogeneous parallelism are analysed, and a program flow based on GPU to extract the micro-motion feature from the radar echo signal of rolling satellite is designed. At the end of the article the results of extraction are given to verify the correctness of the program and algorithm.

Red Mexican grapefruit: a novel source for bioactive limonoids and their antioxidant activity.

PubMed

Mandadi, Kranthi K; Jayaprakasha, Guddadarangavvanahally K; Bhat, Narayan G; Patil, Bhimanagouda S

2007-01-01

Citrus limonoids have shown to inhibit the growth of cancer in colon, lung, mouth, stomach and breast in animal and cell culture studies. For the first time in the present study, an attempt has been made to isolate antioxidant fractions and five limonoids from red Mexican grapefruit seeds. Defatted seed powder was successively extracted with hexane, ethyl acetate (EtOAc), acetone, methanol (MeOH) and MeOH/water and the extracts were concentrated under vacuum. Radical scavenging activity of 1,1-diphenyl-2-picrylhydrazyl (DPPH) and total phenolic content were also measured for comparison with the antioxidant capacity in the phosphomolybdenum method for the above extracts. Acetone and MeOH extracts, respectively, showed the highest (85.7%) and lowest (53.3%) radical scavenging activity, at 500 ppm. The total phenolic contents were found to be highest in the acetone extract (15.94%) followed by the MeOH extract (5.92%), ethyl acetate extract (5.54%) and water extract (5.26%). Antioxidant capacity of the extracts as equivalents to ascorbic acid (micromol/g of the extract) was in the order, EtOAc extract > acetone extract > water extract > methanol extract. Furthermore, the EtOAC and acetone extracts were loaded onto silica gel columns to obtain four limonoid aglycons. MeOH fraction was loaded onto a dowex-50 and sepabeads resin column to obtain a limonoid glucoside. The purity of the isolated five compounds was analyzed by HPLC using a C18 column and UV detection at 210 nm. Finally, the structures of the compounds were identified as obacunone, nomilin, limonin, deacetylnomilin (DAN) and limonin-17-beta-D-glucopyranoside (LG) using 1H and 13C NMR studies.

[Determination of aflatoxin B1, B2, G1, G2 in armeniacae semen amarum by high-performance liquid chromatography-tandem mass spectrometry].

PubMed

Zheng, Run-Sheng; Xu, Hui; Wang, Wen-Li; Zhan, Ruo-Ting; Chen, Wei-Wen

2013-10-01

A simple, rapid and cost-effective high-performance liquid chromatography-tandem mass spectrometry (LC-MS/ MS) method was established for simultaneous determination of aflatoxins (AFB1, AFB2, AFG1, AFG2) in Armeniacae Semen Amarum and the application was performance in 11 samples collected from different markets, medical stores and hospitals. The sample was extracted with 84% acetonitrile/water and 250 microL extraction was directly injected into a LC-MS/MS system without further purification procedure after being redissolved with methanol. The LC separation was performed on a C18 column with a linear gradient elution program of 4 mmol x L(-1) NH4 Ac-0.1% formic acid solution and menthol as the mobile phase. Selected reaction monitoring (SRM) was used for selective determination of the four aflatoxins on a triple quadruple mass spectrometer, which was operated in positive ionization modes. All the four aflatoxins showed a good linear relationship with r > 0.999 0, the average recoveries were between 87.88% and 102.9% and the matrix effect was ranged from 90.71% to 99.30% in low, intermediate and high levels. Furthermore, the higher recovery was obtained by the method reported in this study, comparing to the cleanup procedure with the Mycosep 226 purification column. Eleven samples collected were detected and the contamination levels of the AFB1 were between 1.590-2.340 microg x kg(-1) and the AF (B1 + B2 + G1 + G2) was ranged from 2.340 to 3.340 microg x kg(-1). In summary, the developed method was suitable to detect and screen AFB1, AFB2, AFG1, AFG2 in Armeniacae Semen Amarum.

Method for making a non-extractable stationary phase of polymer within a capillary column

DOEpatents

Springston, Stephen R.

1990-01-01

A method for coating interior capillary column surfaces, or packing material of a packed column, used for gas chromatography, with a stationary polymer phase that is cross-linked by exposing it to a low-temperature plasma that is uniformly distributed over the column or packing material for a predetermined period of time to effect the desired degree of cross-linking of the coating.

Low-density solvent based ultrasound-assisted emulsification microextraction and on-column derivatization combined with gas chromatography-mass spectrometry for the determination of carbamate pesticides in environmental water samples.

PubMed

Guo, Liang; Lee, Hian Kee

2012-04-27

A fast and efficient method for the determination of trace level of carbamate pesticides using a lower-density-than-water solvent for ultrasound-assisted emulsification microextraction coupled to on-column derivatization and analysis by GC-MS has been developed and studied. In this approach, a soft plastic Pasteur pipette was employed as a convenient extraction device. Fifty microliters of extraction solvent, of lower density than water, was injected into the sample solution held in the pipette. The latter was immediately immersed in an ultrasound water bath to form an emulsion. After 2 min extraction, the emulsion was fractionated into two layers by centrifugation. The upper layer (organic extract) could be collected conveniently by squeezing the bulb of the pipette, now held upside down, to move it into the narrow stem of the device, facilitating its retrieval for analysis. The extract was then combined with trimethylphenylammonium hydroxide and directly injected into a gas chromatography-mass spectrometry (GC-MS) system for on-column derivatization and analysis. The on-column derivatization provided an added convenience (since a separate step was not necessary). Parameters affecting the derivatization and extraction were investigated. Under the most favorable conditions, the method demonstrated high extraction efficiency with low limits of detection of between 0.01 and 0.1 μg/L, good linearity in the range of 0.05-50 μg/L, to 0.5-100 μg/L, and good repeatability (RSD below 9.2%, n=5). The proposed method was evaluated by determining carbamate pesticides in river water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

RNA isolation from mammalian cells using porous polymer monoliths: an approach for high-throughput automation.

PubMed

Chatterjee, Anirban; Mirer, Paul L; Zaldivar Santamaria, Elvira; Klapperich, Catherine; Sharon, Andre; Sauer-Budge, Alexis F

2010-06-01

The life science and healthcare communities have been redefining the importance of ribonucleic acid (RNA) through the study of small molecule RNA (in RNAi/siRNA technologies), micro RNA (in cancer research and stem cell research), and mRNA (gene expression analysis for biologic drug targets). Research in this field increasingly requires efficient and high-throughput isolation techniques for RNA. Currently, several commercial kits are available for isolating RNA from cells. Although the quality and quantity of RNA yielded from these kits is sufficiently good for many purposes, limitations exist in terms of extraction efficiency from small cell populations and the ability to automate the extraction process. Traditionally, automating a process decreases the cost and personnel time while simultaneously increasing the throughput and reproducibility. As the RNA field matures, new methods for automating its extraction, especially from low cell numbers and in high throughput, are needed to achieve these improvements. The technology presented in this article is a step toward this goal. The method is based on a solid-phase extraction technology using a porous polymer monolith (PPM). A novel cell lysis approach and a larger binding surface throughout the PPM extraction column ensure a high yield from small starting samples, increasing sensitivity and reducing indirect costs in cell culture and sample storage. The method ensures a fast and simple procedure for RNA isolation from eukaryotic cells, with a high yield both in terms of quality and quantity. The technique is amenable to automation and streamlined workflow integration, with possible miniaturization of the sample handling process making it suitable for high-throughput applications.

Quantification of Complex Polycyclic Aromatic Hydrocarbon Mixtures in Standard Reference Materials Using GC×GC/ToF-MS

PubMed Central

Manzano, Carlos; Hoh, Eunha; Massey Simonich, Staci L.

2014-01-01

This research is the first to quantify complex PAH mixtures in NIST SRMs using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/ToF-MS), with and without extract cleanup, and reports previously unidentified PAH isomers in the NIST SRMs. We tested a novel, high orthogonality GC column combination (LC-50×NSP-35), as well as with a commonly used column combination (Rtx-5ms×Rxi-17) for the quantification of a complex mixture of 85 different PAHs, including parent (PAHs), alkyl- (MPAHs), nitro- (NPAHs), oxy- (OPAHs), thio- (SPAHs), bromo- (BrPAHs), and chloro-PAHs (ClPAHs) in extracts from two standard reference materials: NIST SRM1650b (diesel particulate matter), with cleanup and NIST SRM1975 (diesel particulate extract), with and without extract cleanup. The LC-50×NSP-35 column combination resulted in an average absolute percent difference of 33.8%, 62.2% and 30.8% compared to the NIST certified PAH concentrations for NIST SRM1650b, NIST SRM1975 with cleanup and NIST SRM1975 without cleanup, while the Rtx-5ms×Rxi-17 resulted in an absolute percent difference of 38.6%, 67.2% and 79.6% for NIST SRM1650b, NIST SRM1975 with cleanup and NIST SRM1975 without cleanup, respectively. This GC×GC/ToF-MS method increases the number of PAHs detected and quantified in complex environmental extracts using a single chromatographic run. Without clean-up, 7 additional compounds were detected and quantified in NIST SRM1975 using the LC-50×NSP-35 column combination. These results suggest that the use of the LC-50×NSP-35 column combination in GC×GC/ToF-MS not only results in better chromatographic resolution and greater orthogonality for the separation of complex PAH mixtures, but can also be used for the accurate quantification of complex PAH mixtures in environmental extracts without cleanup. PMID:23932031

Modeling of rotating disc contactor (RDC) column

NASA Astrophysics Data System (ADS)

Ismail, Wan Nurul Aiffah; Zakaria, Siti Aisyah; Noor, Nor Fashihah Mohd; Sulong, Ibrahim; Arshad, Khairil Anuar

2014-12-01

Liquid-liquid extraction is one of the most important separation processes. Different kinds of liquid-liquid extractor such as Rotating Disc Contactor (RDC) Column being used in industries. The study of liquid-liquid extraction in an RDC column has become a very important subject to be discussed not just among chemical engineers but mathematician as well. In this research, the modeling of small diameter RDC column using the chemical system involving cumene/isobutryric asid/water are analyzed by the method of Artificial Neural Network (ANN). In the previous research, we begin the process of analyzed the data using methods of design of the experiments (DOE) to identify which factor and their interaction factor are significant and to determine the percentage of contribution of the variance for each factor. From the result obtained, we continue the research by discussed the development and validation of an artificial neural network model in estimating the concentration of continuous and concentration of dispersed outlet for an RDC column. It is expected that an efficient and reliable model will be formed to predict RDC column performance as an alternative to speed up the simulation process.

Analysis of trifluralin, methyl paraoxon, methyl parathion, fenvalerate and 2,4-D dimethylamine in pond water using solid-phase extraction

USGS Publications Warehouse

Swineford, D.M.; Belisle, A.A.

1989-01-01

A method was developed for the simultaneous extraction of trifluralin, methyl paraoxon, methyl parathion, fenvalerate, and 2,4-D dimethylamine salt in pond water using a solid-phase C18 column. After elution from the C18 column, the eluate was analyzed on a capillary gas chromatograph equipped with an electron-capture or flame photometric detector.

Synthesis and Development of Porous Polymeric Column Packing and Microchip Detectors for GC Analysis of Extraterrestrial Atmospheres

NASA Technical Reports Server (NTRS)

Shen, Thomas C.

1999-01-01

This report summarizes the last nine years research accomplishments under Cooperative Agreement NCC2-650 between NASA, Ames Research Center and SETI Institute. Four Major research tasks are conducted: 1. Gas chromatography column development. 2. Pyrosensor development. 3. Micro-machining gas chromatography instrument development. 4. Amino acid analysis and high molecular weight polyamino acid synthesis under prebiotic conditions. The following describes these results.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chlorinated pesticides in aquatic tissue by capillary-column gas chromatography with electron-capture detection

USGS Publications Warehouse

Leiker, Thomas J.; Madsen, J.E.; Deacon, J.R.; Foreman, W.T.

1995-01-01

A method for the determination of chlorinated organic compounds in aquatic tissue by dual capillary-column gas chromatography with electron-capture detection is described. Whole-body-fish or corbicula tissue is homogenized, Soxhlet extracted, lipid removed by gel permeation chromatography, and fractionated using alumina/silica adsorption chromatography. The extracts are analyzed by dissimilar capillary-column gas chromatography with electron-capture detection. The method reporting limits are 5 micrograms per kilogram (μg/kg) for chlorinated compounds, 50 μg/kg for polychlorinated biphenyls, and 200 μg/kg for toxaphene.

Solid-phase microextraction of phthalate esters in water sample using different activated carbon-polymer monoliths as adsorbents.

PubMed

Lirio, Stephen; Fu, Chung-Wei; Lin, Jhih-Yun; Hsu, Meng-Ju; Huang, Hsi-Ya

2016-07-13

In this study, the application of different activated carbon-polymer (AC-polymer) monoliths as adsorbents for the solid-phase microextraction (SPME) of phthalate esters (PAEs) in water sample were investigated. The activated carbon (AC) was embedded in organic polymers, poly(butyl methacrylate-co-ethylene dimethacrylate) (poly(BMA-EDMA)) or poly(styrene-co-divinylbenzene) (poly(STY-DVB)), via a 5-min microwave-assisted or a 15-min water bath heating polymerization. Preliminary investigation on the performance of the native poly(BMA-EDMA) and poly(STY-DVB) demonstrated remarkable adsorption efficiencies for PAEs. However, due to the strong hydrophobic, π-π, and hydrogen bonding interactions between the analytes and polymers, low extraction recoveries were achieved. In contrast, the presence of AC in native polymers not only enhanced the adsorption efficiencies but also assisted the PAE desorption, especially for AC-poly(STY-DVB) with extraction recovery ranged of 76.2-99.3%. Under the optimized conditions, the extraction recoveries for intra-, inter-day and column-to-column were in the range of 76.5-100.8% (<3.7% RSDs), 77.2-97.6% (<5.6% RSDs) and 75.5-99.7% (<6.2% RSDs), respectively. The developed AC-poly(STY-DVB) monolithic column showed good mechanical stability, which can be reused for more than 30 extraction times without any significant loss in the extraction recoveries of PAEs. The AC-poly(STY-DVB) monolithic column was successfully applied in SPME of PAEs in water sample with extraction recovery ranged of 78.8%-104.6% (<5.5% RSDs). Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Ionic liquid-based microwave-assisted extraction for the determination of flavonoid glycosides in pigeon pea leaves by high-performance liquid chromatography-diode array detector with pentafluorophenyl column.

PubMed

Wei, Wei; Fu, Yu-jie; Zu, Yuan-gang; Wang, Wei; Luo, Meng; Zhao, Chun-jian; Li, Chun-ying; Zhang, Lin; Wei, Zuo-fu

2012-11-01

In this study, an ionic liquid-based microwave-assisted extraction (ILMAE) followed by high-performance liquid chromatography-diode array detector with a pentafluorophenyl column for the extraction and quantification of eight flavonoid glycosides in pigeon pea leaves is described. Compared with conventional extraction methods, ILMAE is a more effective and environment friendly method for the extraction of nature compounds from herbal plants. Nine different types of ionic liquids with different cations and anions were investigated. The results suggested that varying the anion and cation had significant effects on the extraction of flavonoid glycosides, and 1.0 M 1-butyl-3-methylimidazolium bromide ([C4MIM]Br) solution was selected as solvent. In addition, the extraction procedures were also optimized using a series of single-factor experiments. The optimum parameters were obtained as follows: extraction temperature 60°C, liquid-solid ratio 20:1 mL/g and extraction time 13 min. Moreover, an HPLC method using pentafluorophenyl column was established and validated. Good linearity was observed with the regression coefficients (r(2)) more than 0.999. The limit of detection (LODs) (S/N = 3) and limit of quantification (LOQs) (S/N = 10) for the components were less than 0.41 and 1.47 μg/mL, respectively. The inter- and intraday precisions that were used to evaluate the reproducibility and relative standard deviation (RSD) values were less than 4.57%. The recoveries were between 97.26 and 102.69%. The method was successfully used for the analysis of samples of pigeon pea leaves. In conclusion, the developed ILMAE-HPLC-diode array detector using pentafluorophenyl column method can be applied for quality control of pigeon pea leaves and related medicinal products. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fingerprinting of traditional Chinese medicines on the C18-Diol mixed-mode column in online or offline two-dimensional liquid chromatography on the single column modes.

PubMed

Wang, Qing; Tong, Ling; Yao, Lin; Zhang, Peng; Xu, Li

2016-06-05

In the present study, a mixed-mode stationary phase, C18-Diol, was applied for fingerprint analysis of traditional Chinese medicines. Hydrophobic, hydrogen bonding and electrostatic interactions were demonstrated to contribute the retention separately or jointly, which endowed the C18-Diol stationary phase with distinct selectivity compared to the bare C18 one. The separation of total alkaloids extracted from Fritillaria hupehensis was compared on the C18-Diol and conventional C18 column with the greater resolving power and better symmetry responses on the former one. Besides, a novel two-dimensional liquid chromatography on the single column (2D-LC-1C) was realized on C18-Diol with the offline mode for the alcohol extract of Fritillaria hupehensis and online mode for Ligusticum chuanxiong Hort. The early co-eluted extracted components with great polarity on the first dimension were reinjected on the same column and well separated on the second dimension. The results exhibited that the two complementary RPLC and HILIC modes on C18-Diol stationary phase enhanced the separation capacity and revealed more abundant chemical information of the sample, which was a powerful tool in analyzing complex herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

Development and validation of a dried blood spot-HPLC assay for the determination of metronidazole in neonatal whole blood samples.

PubMed

Suyagh, Maysa Faisal; Iheagwaram, Godwill; Kole, Prashant Laxman; Millership, Jeff; Collier, Paul; Halliday, Henry; McElnay, James C

2010-05-01

A selective and sensitive high-performance liquid chromatography method with UV detection for the determination of metronidazole in dried blood spots (DBS) has been developed and validated. DBS samples [spiked or patient samples] were prepared by applying blood (30 microL) to Guthrie cards. Discs (6 mm diameter) were punched from the cards and extracted using water containing the internal standard, tinidazole. The extracted sample was chromatographed without further treatment using a reversed phase system involving a Symmetry(R) C18 (5 microm, 3.9 x 150 mm) preceded by a Symmetry(R) guard column of matching chemistry and a detection wavelength of 317 nm. The mobile phase comprised acetonitrile/0.01 M phosphate solution (KH(2)PO(4)), pH 4.7, 15:85, v/v, with a flow rate of 1 mL/min. The calibration was linear over the range 2.5-50 mg/mL. The limits of detection and quantification were 0.6 and 1.8 microg/mL, respectively. The method has been applied to the determination of 203 DBS samples from neonatal patients for a phamacokinetic/pharmacodynamic study.

Determination of 3-hydroxypropylmercapturic acid in urine by three column-switching high-performance liquid chromatography with electrochemical detection using a diamond electrode.

PubMed

Higashi, Kyohei; Shibasaki, Mana; Kuni, Kyoshiro; Uemura, Takeshi; Waragai, Masaaki; Uemura, Kenichi; Igarashi, Kazuei; Toida, Toshihiko

2017-09-29

A three column-switching high-performance liquid chromatography (HPLC) using an electrochemical detector (ECD) equipped with a diamond electrode was established to determine 3-hydroxypropylmercapturic acid (3-HPMA) in urine. An extracted urine sample was consecutively fractionated using a strong anion-exchange column (first column) and a C8 column (second column) via a switching valve before application on an Octa Decyl Silyl (ODS) column (third column), followed by ECD analysis. The% recovery of 3-HPMA standard throughout the three-column process and limit of detection (LOD) were 94±1% and 0.1pmol, respectively. A solid phase extraction step is required for the sensitive analysis of 3-HPMA in urine by column-switching HPLC-ECD despite a decreased% recovery (55%) of urine sample spiked with 100pmol of 3-HPMA. To test the utility of our column-switching HPLC-ECD method, 3-HPMA levels of 27 urine samples were determined, and the correlation between HPLC-ECD and LC-Electrospray ionization (ESI)-MS/MS method was examined. As a result, the median values of μmol 3-HPMA/g Creatinine (Cre) in urine obtained by column-switching HPLC-ECD and LC-MS/MS were 2.19±2.12μmol/g Cre and 2.13±3.38μmol/g Cre, respectively, and the calibration curve (y=1.5171x-1.007) exhibited good linearity within a defined range (r 2 =0.907). These results indicate that the combination of column-switching HPLC and ECD is a powerful tool for the specific, reliable detection of 3-HPMA in urine. Copyright © 2017 Elsevier B.V. All rights reserved.

Dispersive micro solid phase extraction (DMSPE) using polymer anion exchange (PAX) as the sorbent followed by UPLC-MS/MS for the rapid determination of four bisphenols in commercial edible oils.

PubMed

Xian, Yanping; Wu, Yuluan; Dong, Hao; Guo, Xindong; Wang, Bin; Wang, Li

2017-09-29

The present work presents a novel and rapid analytical method for the simultaneous analysis of bisphenol A (BPA), bisphenol B (BPB), bisphenol F (BPF) and bisphenol S (BPS) in edible oil based on dispersive micro solid phase extraction (DMSPE) for the first time followed by isotope dilution-ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The edible oil sample was dispersed by n-hexane and extracted with ammoniated methanol-water solution. Then the target analytes were dispersedly absorbed using the polymer anion exchange (PAX) as the sorbent and eluted by acidic methanol. After that, four bisphenols were separated on a C18 column by gradient elution with methanol and 0.05% ammonium hydroxide in water as mobile phase, detected by MS/MS under multiple reactions monitoring (MRM) mode and quantified by internal standard method. The PAX amounts, adsorption time, concentrations of formic acid in the elution solvent and volume of elution solvent for the DMSPE technique were optimized. The limit of detection and quantitation (LOD and LOQ), matrix effect, recovery and precision of the developed method were investigated. Results indicated that BPS and the rest three bisphenols displayed excellent linearity in the concentration ranges of 0.1-50μg/L and 0.5-250μg/L, respectively, with correlation coefficients (R 2 ) all larger than 0.998. Achieved MLODs (S/N=3) varied between 0.1-0.4μg/kg for all bisphenols. The mean recoveries at three spiked levels in edible oil were in the range of 87.3-108%. Intra-day precision (n=6) and inter-day precision (n=5) were <9% and <11%, respectively. This method is of rapid-and-simple pretreatment, accurate and sensitive, and suitable for the simultaneous determination of bisphenols in edible oil. Copyright © 2017. Published by Elsevier B.V.

Polytetrafluorethylene film-based liquid-three phase micro extraction coupled with differential pulse voltammetry for the determination of atorvastatin calcium.

PubMed

Ensafi, Ali A; Khoddami, Elaheh; Rezaei, Behzad

2013-01-01

In this paper, we describe a new combination method based on polytetrafluorethylene (PTFE) film-based liquid three-phase micro extraction coupled with differential pulse voltammetry (DPV) for the micro extraction and quantification of atorvastatin calcium (ATC) at the ultra-trace level. Different factors affecting the liquid-three phases micro extraction of atorvastatin calcium, including organic solvent, pH of the donor and acceptor phases, concentration of salt, extraction time, stirring rate and electrochemical factors, were investigated, and the optimal extraction conditions were established. The final stable signal was achieved after a 50 min extraction time, which was used for analytical applications. An enrichment factor of 21 was achieved, and the relative standard deviation (RSD) of the method was 4.5% (n = 4). Differential pulse voltammetry exhibited two wide linear dynamic ranges of 20.0-1000.0 pmol L(-1) and 0.001-11.0 µmol L(-1) of ATC. The detection limit was found to be 8.1 pmol L(-1) ATC. Finally, the proposed method was used as a new combination method for the determination of atorvastatin calcium in real samples, such as human urine and plasma.

Evaluation of a method for assaying sulfonamide antimicrobial residues in cheese: hot-water extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Berardi, Giorgio; Bogialli, Sara; Curini, Roberta; Di Corcia, Antonio; Laganá, Aldo

2006-06-28

Several sulfonamide antimicrobials (SAAs) are largely used in veterinary medicine. A rapid, specific, and sensitive procedure for determining 12 SAAs in cheese is presented. The method is based on the matrix solid-phase dispersion technique followed by liquid chromatography (LC)-tandem mass spectrometry (MS) equipped with an electrospray ion source. Target compounds were extracted from Mozzarella, Asiago, Parmigiano, Emmenthal, and Camembert cheese samples by 6 mL of water modified with 10% methanol and heated at 120 degrees C. The addition of methanol to hot water served to improve remarkably extraction yields of the most lipophilic SAAs, that is, sulfadimethoxine and sulfaquinoxaline. After acidification and filtration, 100 microL of the aqueous extract was injected in the LC column. MS data acquisition was performed in the multireaction monitoring mode, selecting two precursor-to-product ion transitions for each target compound. Methanol-modified hot water appeared to be an efficient extractant, because absolute recovery ranged between 67 and 88%. Using sulfamoxole as surrogate analyte, recovery of the 12 analytes spiked in the five types of cheese considered at the 50 ng/g level ranged between 75 and 105% with RSD not higher than 11%. Statistical analysis of the mean recovery data showed that the extraction efficiency was not affected by the type of cheese analyzed. This result indicates this method could be applied to other cheese types not considered here. The accuracy of the method was determined at three spike levels, that is, 20, 50, and 100 ng/g, and varied between 73 and 102% with relative standard deviations ranging between 4 and 12%. On the basis of a signal-to-noise ratio of 10, limits of quantification were estimated to be <1 ng/g.

Isolation, characterization and HPLC quantification of compounds from Aquilegia fragrans Benth: Their in vitro antibacterial activities against bovine mastitis pathogens.

PubMed

Mushtaq, Saleem; Aga, Mushtaq A; Qazi, Parvaiz H; Ali, Md Niamat; Shah, Aabid Manzoor; Lone, Sajad Ahmad; Shah, Aiyatullah; Hussain, Aehtesham; Rasool, Faheem; Dar, Hafizullah; Shah, Zeeshan Hamid; Lone, Shabir H

2016-02-03

The underground parts of Aquilegia fragrans are traditionally used for the treatment of wounds and various inflammatory diseases like bovine mastitis. However, there are no reports on the phytochemical characterization and antibacterial studies of A. fragrans. To isolate compounds from the methanol extract of the underground parts of A. fragrans and determine their antibacterial activity against the pathogens of bovine mastitis. The study was undertaken in order to scientifically validate the traditional use of A. fragrans. Five compounds were isolated from the methanol extract of the underground parts of A. fragrans using silica gel column chromatography. Structural elucidation of the isolated compounds was done using spectral data analysis and comparison with literature. High performance liquid chromatography (HPLC) was used for the qualitative and quantitative determination of isolated compounds in the crude methanol extract. The methanol extract and isolated compounds were evaluated for antibacterial activities against mastitis pathogens using broth micro-dilution technique. The five isolated compounds were identified as (1) 2, 4-dihydroxyphenylacetic acid methyl ester (2) β-sitosterol (3) Aquilegiolide (4) Glochidionolactone-A and (5) Magnoflorine. A quick and sensitive HPLC method was developed for the first time for qualitative and quantitative determination of four isolated marker compounds from A. fragrans. The crude methanol extract and compound 5 exhibited weak antibacterial activities that varied between the bacterial species (MIC=500-3000 µg/ml). The above results show that the crude methanol extract and isolated compounds from A. fragrans exhibit weak antibacterial activities. Further phytochemical and pharmacological studies are required for proper scientific validation of the folk use of this plant species in the treatment of various inflammatory diseases like bovine mastitis. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Reprogramming hMSCs morphology with silicon/porous silicon geometric micro-patterns.

PubMed

Ynsa, M D; Dang, Z Y; Manso-Silvan, M; Song, J; Azimi, S; Wu, J F; Liang, H D; Torres-Costa, V; Punzon-Quijorna, E; Breese, M B H; Garcia-Ruiz, J P

2014-04-01

Geometric micro-patterned surfaces of silicon combined with porous silicon (Si/PSi) have been manufactured to study the behaviour of human Mesenchymal Stem Cells (hMSCs). These micro-patterns consist of regular silicon hexagons surrounded by spaced columns of silicon equilateral triangles separated by PSi. The results show that, at an early culture stage, the hMSCs resemble quiescent cells on the central hexagons with centered nuclei and actin/β-catenin and a microtubules network denoting cell adhesion. After 2 days, hMSCs adapted their morphology and cytoskeleton proteins from cell-cell dominant interactions at the center of the hexagonal surface. This was followed by an intermediate zone with some external actin fibres/β-catenin interactions and an outer zone where the dominant interactions are cell-silicon. Cells move into silicon columns to divide, migrate and communicate. Furthermore, results show that Runx2 and vitamin D receptors, both specific transcription factors for skeleton-derived cells, are expressed in cells grown on micropatterned silicon under all observed circumstances. On the other hand, non-phenotypic alterations are under cell growth and migration on Si/PSi substrates. The former consideration strongly supports the use of micro-patterned silicon surfaces to address pending questions about the mechanisms of human bone biogenesis/pathogenesis and the study of bone scaffolds.

Determination of the cyanobacterial toxin cylindrospermopsin in algal food supplements.

PubMed

Liu, H; Scott, P M

2011-06-01

For the analysis of blue-green algal food supplements for cylindrospermopsin (CYN), a C18 solid-phase extraction column and a polygraphitized carbon solid-phase extraction column in series was an effective procedure for the clean-up of extracts. Determination of CYN was by liquid chromatography with ultraviolet light detection. At extract spiking levels of CYN equivalent to 25-500 µg g(-1), blue-green algal supplement recoveries were in the range 70-90%. CYN was not detected in ten samples of food supplements and one chocolate product, all containing blue-green algae. The limit of detection for the method was 16 µg g(-1), and the limit of quantification was 52 µg g(-1).

Extraction and speciation of arsenic in lacustrine sediments

USGS Publications Warehouse

Ficklin, W.H.

1990-01-01

Arsenic was partially extracted with 4.OM hydrochloric acid, from samples collected at 25-cm intervals in a 350-cm column of sediment at Milltown Reservoir, Montana and from a 60-cm core of sediment collected at the Cheyenne River Embayment of Lake Oahe, South Dakota. The sediment in both reservoirs is highly contaminated with arsenic. The extracted arsenic was separated into As(III) and As(V) on acetate form Dowex 1-X8 ion-exchange resin with 0.12M HCl eluent. Residual arsenic was sequentially extracted with KClO3 and HCl. Arsenic was determined by graphite-furnace atomic-absorption spectrometry. The analytical results define oxidized and reduced zones in the sediment columns. ?? 1990.

Method for making a non-extractable stationary phase of polymer within a capillary column

DOEpatents

Springston, S.R.

1990-10-30

A method is described for coating interior capillary column surfaces, or packing material of a packed column, used for gas chromatography, with a stationary polymer phase that is cross-linked by exposing it to a low-temperature plasma that is uniformly distributed over the column or packing material for a predetermined period of time to effect the desired degree of cross-linking of the coating. 7 figs.

Capillary electrochromatography of inorganic cations in open tubular columns with a controllable capacity multilayered stationary phase architecture.

PubMed

Kubán, Pavel; Kubán, Petr; Kubán, Vlastimil; Hauser, Peter C; Bocek, Petr

2008-05-09

In this paper capillary electrochromatography of alkali and alkaline-earth metal cations in open tubular capillary columns is described. Capillary columns are prepared by coating fused silica capillaries of 75 microm I.D. with poly(butadiene-maleic acid) copolymer (PBMA) in multiple layers. Thermally initiated radical polymerization is used to crosslink the stationary phase. Capillary columns with different number of stationary phase layers can be prepared and allow for the adjustment of separation selectivity in the electrochromatographic mode. Fast and sensitive separations of common inorganic cations are achieved in less than 6 min in a 60 cm capillary column with on-column capacitively coupled contactless conductivity detector. Limits of detection (S/N=3) for the determination of alkali and alkaline-earth metal cations range from 0.3 to 2.5 microM and repeatability is better than 0.5, 4.5 and 6.1% for migration times, peak heights and peak areas, respectively.

Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

USGS Publications Warehouse

Belisle, A.A.; Swineford, D.M.

1988-01-01

A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

High resolution photolithography using arrays of polystyrene and SiO2 micro- and nano-sized spherical lenses

NASA Astrophysics Data System (ADS)

Dvoretckaia, L. N.; Mozharov, A. M.; Mukhin, I. S.

2017-11-01

Photolithography mask made of close-packed array of micro- and nano-sized spherical lenses allows to obtain the ordered structures and provides highest “optical resolution/cost” ratio between all existing photolithography and laser direct writing methods. In this letter, we present results of modeling the propagation of a plane wave falling on the array of quartz (SiO2) microspherical lenses and focusing in the image reverse photoresist layer. We present here experimental results on fabrication of ordered arrays of submicron wells and columns and substrate preparation for growth of monocrystalline nanowires on metal surface using photolithography with mask of SiO2 microspheres. Such ordered nano-sized arrays of wells and columns can be used in fabrication of further growth of monocrystalline nanowires, quantum dots and production of plasmon structures.

MicroSPE-nanoLC-ESI-MS/MS Using 10-μm-i.d. Silica-Based Monolithic Columns for Proteomics

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

Luo, Quanzhou; Page, Jason S.; Tang, Keqi

2007-01-01

Silica-based monolithic narrow bore capillary columns (25 cm x 10 µm i.d.) with an integrated nanoESI emitter has been developed to provide high quality and robust microSPE-nanoLC-ESI-MS analyses. The integrated nanoESI emitter adds no dead volume to the LC separation, allowing stable electrospray performance to be obtained at flow rates of ~10 nL/min. In an initial application we identified 5510 unique peptides covering 1443 distinct Shewanella oneidensis proteins from a 300 ng tryptic digest sample in a single 4-h LC-MS/MS analysis using a linear ion trap MS (LTQ). We found the use of an integrated monolithic ESI emitter provided enhancedmore » resistance to clogging and good run-to-run reproducibility.« less

Footprints of Urban Micro-Pollution in Protected Areas: Investigating the Longitudinal Distribution of Perfluoroalkyl Acids in Wildlife Preserves

PubMed Central

Rodriguez-Jorquera, Ignacio A.; Silva-Sanchez, Cecilia; Strynar, Mark; Denslow, Nancy D.; Toor, Gurpal S.

2016-01-01

Current approaches to protect biodiversity by establishing protected areas usually gloss over water pollution as a threat. Our objective was to determine the longitudinal and seasonal distribution of perfluoroalkyl acids (PFAAs) in water column and sediments from a wastewater dominated stream that enters preservation areas. Water samples were collected along the longitudinal section (six sites, 1000 m away from each other) of the stream during the dry and wet seasons. Sediments were collected from three sites along the stream from three depths. Water and sediments were analyzed for PFAAs using high performance liquid chromatography-tandem mass spectrometry. Eleven PFAAs with 5 to 14 carbon atoms were detected in the water column at all sampling points, with a minor reduction at the last point suggesting a dilution effect. The most detected PFAAs was PFOS, followed by perfluorooctanoic acid (PFOA), and perfluorohexanoic acid (PFHxA). Seasonal differences in PFAAs concentrations suggested contribution of stormwater runoff during the wet season. All analyzed PFAAs in sediments were under the limit of quantification, likely due to the high proportion of sand and low organic matter. However, high concentrations of PFAAs were detected in the water column inside the protected areas, which includes PFOS in concentrations considered not safe for avian wildlife. Water samples appear to be more relevant than sediments to determine PFAAs micro-pollution in water bodies with sandy sediments. Inclusion of a management plans on micro-pollution research, monitoring, and mitigation is recommended for protected areas. PMID:26909512

Coupled factors influencing detachment of nano- and micro-sized particles from primary minima.

PubMed

Shen, Chongyang; Lazouskaya, Volha; Jin, Yan; Li, Baoguo; Ma, Zhiqiang; Zheng, Wenjuan; Huang, Yuanfang

2012-06-01

This study examined the detachments of nano- and micro-sized colloids from primary minima in the presence of cation exchange by laboratory column experiments. Colloids were initially deposited in columns packed with glass beads at 0.2 M CaCl(2) in the primary minima of Derjaguin-Landau-Verwey-Overbeek (DLVO) interaction energies. Then, the columns were flushed with NaCl solutions with different ionic strengths (i.e., 0.001, 0.01, 0.1 and 0.2 M). Detachments were observed at all ionic strengths and were particularly significant for the nanoparticle. The detachments increased with increasing electrolyte concentration for the nanoparticle whereas increased from 0.001 M to 0.01 M and decreased with further increasing electrolyte concentration for the micro-sized colloid. The observations were attributed to coupled influence of cation exchange, short-range repulsion, surface roughness, surface charge heterogeneity, and deposition in the secondary minima. The detachments of colloids from primary minima challenge the common belief that colloid interaction in primary minimum is irreversible and resistant to disturbance in solution ionic strength and composition. Although the significance of surface roughness, surface charge heterogeneity, and secondary minima on colloid deposition has been widely recognized, our study implies that they also play important roles in colloid detachment. Whereas colloid detachment is frequently associated with decrease of ionic strength, our results show that increase of ionic strength can also cause detachment due to influence of cation exchange. Copyright © 2012 Elsevier B.V. All rights reserved.

Acaricidal activity of extracts of neem (Azadirachta indica) oil against the larvae of the rabbit mite Sarcoptes scabiei var. cuniculi in vitro.

PubMed

Du, Yong-Hua; Jia, Ren-Yong; Yin, Zhong-Qiong; Pu, Zhong-Hui; Chen, Jiao; Yang, Fan; Zhang, Yu-Qun; Lu, Yang

2008-10-20

The acaricidal activity of the petroleum ether extract, the chloroform extract and the acetic ether extract of neem (Azadirachta indica) oil against Sarcoptes scabiei var. cuniculi larvae was tested in vitro. A complementary log-log (CLL) model was used to analyze the data of the toxicity tests. The results showed that at all test time points, the petroleum ether extract demonstrated the highest activity against the larvae of S. scabiei var. cuniculi, while the activities of the chloroform extract and the acetic ether extract were similar. The activities of both the petroleum ether extract and the chloroform extract against the larvae showed the relation of time and concentration dependent. The median lethal concentration (LC50) of the petroleum ether extract (1.3 microL/mL) was about three times that of the chloroform extract (4.1 microL/mL) at 24 h post-treatment. At the concentrations of 500.0 microL/mL, the median lethal time (LT50) of the petroleum ether extract and the chloroform extract was 8.4 and 9.6 h, respectively.

Effect of surfactant on single drop mass transfer for extraction of aromatics from lubricating oils

NASA Astrophysics Data System (ADS)

Izza, H.; Ben Abdessalam, S.; Korichi, M.

2018-03-01

Solvent extraction is an effective method for the reduction of the content of aromatic of lubricating oil. Frequently, with phenol, furfural, the NMP (out of N-methyl pyrrolidone). The power solvent and the selectivity can be still to increase while using surfactant as additive which facilitates the separation of phase and increases the yeild in raffinat. Liquid-liquid mass transfer coefficients for single freely rising drops in the presence of surfactant in an extraction column have been investigated. The surfactant used in this study was sodium lauryl ether sulfate (SLES). The experiments were performed by bubbling a solvent as a series of individual drops from the top of the column containing furfural-SLES solution. The column used in this experiment was made from glass with 17 mm inner diameter and a capacity of 125ml. The effects of the concentration of surfactant on the overall coefficient of mass transfer was investigated.

Isolation and identification of arctiin and arctigenin in leaves of burdock (Arctium lappa L.) by polyamide column chromatography in combination with HPLC-ESI/MS.

PubMed

Liu, Shiming; Chen, Kaoshan; Schliemann, Willibald; Strack, Dieter

2005-01-01

A simple method involving polyamide column chromatography in combination with HPLC-PAD and HPLC-ESI/MS for isolating and identifying two kinds of lignans, arctiin and arctigenin, in the leaves of burdock (Arctium lappa L.) has been established. After extraction of burdock leaves with 80% methanol, the aqueous phase of crude extracts was partitioned between water and chloroform and the aqueous phase was fractionated on a polyamide glass column. The fraction, eluting with 100% methanol, was concentrated and gave a white precipitate at 4 degrees C from which two main compounds were purified by semi-preparative HPLC. In comparison with the UV and ESI-MS spectra and the HPLC retention time of authentic standards, the compounds were determined to be arctiin and arctigenin. The extraction/separation technique was validated using an internal standard method.

Antimicrobial and cytotoxic constituents from leaves of Sapium baccatum.

PubMed

Ahmed, Yunus; Sohrab, Md Hossain; Al-Reza, Sharif M; Tareq, Faqir Shahidulla; Hasan, Choudhury M; Sattar, M A

2010-02-01

Six compounds, namely, Lupeol (1), Betulin (2), beta-Taraxerol (3), Taraxerone (4), Stigmasterol (5) and beta-Sitosterol (6) were isolated from the petroleum ether extract of the leaves of Sapium baccatum based on spectroscopic evidence. Lupeol (1), Betulin (2) and Stigmasterol (5) were isolated for the first time from this plant. The cytotoxic potential of the different solvent extracts (methanol, petroleum ether, carbon-tetrachloride and dichloromethane); six column fractions (F-4, F-7, F-10, F-12, F-18 and F-22) of petroleum ether extract and three pure compounds 1, 4 and 6 were determined by using brine shrimp lethality bioassay. The LC50 of all the tested samples were showed to be lethal to brine shrimp nauplii. However, petroleum ether, carbon-tetrachloride extract, column fractions F-4 and F-18 of petroleum ether extract and pure compound 6 showed quite potent activity in brine shrimp lethality bioassay with LC50 1.33, 1.35, 1.40, 1.58 and 1.58 microg/ml, respectively. These result suggested that they might be contain antitumor or pesticidal activity. Further, the methanol extract and four column fractions (F-7, F-12, F-18 and F-22) of petroleum ether showed significant activity against the tested microorganisms. Copyright 2009 Elsevier Ltd. All rights reserved.

Polypyrrole-magnetite dispersive micro-solid-phase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater.

PubMed

Kamaruddin, Amirah Farhan; Sanagi, Mohd Marsin; Wan Ibrahim, Wan Aini; Md Shukri, Dyia S; Abdul Keyon, Aemi S

2017-11-01

Polypyrrole-magnetite dispersive micro-solid-phase extraction method combined with ultraviolet-visible spectrophotometry was developed for the determination of selected cationic dyes in textile wastewater. Polypyrrole-magnetite was used as adsorbent due to its thermal stability, magnetic properties, and ability to adsorb Rhodamine 6G and crystal violet. Dispersive micro-solid-phase extraction parameters were optimized, including sample pH, adsorbent amount, extraction time, and desorption solvent. The optimum polypyrrole-magnetite dispersive micro-solid phase-extraction conditions were sample pH 8, 60 mg polypyrrole-magnetite adsorbent, 5 min of extraction time, and acetonitrile as the desorption solvent. Under the optimized conditions, the polypyrrole-magnetite dispersive micro-solid-phase extraction with ultraviolet-visible method showed good linearity in the range of 0.05-7 mg/L (R 2  > 0.9980). The method also showed a good limit of detection for the dyes (0.05 mg/L) and good analyte recoveries (97.4-111.3%) with relative standard deviations < 10%. The method was successfully applied to the analysis of dyes in textile wastewater samples where the concentration found was 1.03 mg (RSD ±7.9%) and 1.13 mg/L (RSD ± 4.6%) for Rhodamine 6G and crystal violet, respectively. It can be concluded that this method can be adopted for the rapid extraction and determination of dyes at trace concentration levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enantioseparation on cellulose dimethylphenylcarbamate-modified zirconia monolithic columns by reversed-phase capillary electrochromatography.

PubMed

Kumar, Avvaru Praveen; Park, Jung Hag

2010-06-25

This work reports the preparation of monolithic zirconia chiral columns for separation of enantiomeric compounds by capillary electrochromatography (CEC). Using sol-gel technology, a porous monolith having interconnected globular-like structure with through-pores is synthesized in the capillary column as a first step in the synthesis of monolithic zirconia chiral capillary columns. In the second step, the surface of the monolith is modified by coating with cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) as the chiral stationary phase to obtain a chiral column (CDMPCZM). The process of the preparation of the zirconia monolithic capillary column was investigated by varying the concentrations of the components of the sol solution including polyethylene glycol, water and acetic acid. CDMPCZM is mechanically stable and no bubble formation was detected with the applied current of up to 30 microA. The enantioseparation behavior of the CDMPCZM columns was investigated by separating a set of 10 representative chiral compounds by varying the applied voltage and pH and organic composition of the aqueous organic mobile phases. Copyright 2010 Elsevier B.V. All rights reserved.

Recovery of 1,3-, 2,3-dichloropropenes, 1,2-dibromo-3-chloropropane, and o-, p-dichlorobenzenes from fatty and non-fat foodstuffs by liquid extraction technique.

PubMed

Daft, J L

1990-01-01

Food samples including fatty, non-fatty, grain-based, and nongrain-based types were fortified with the following five nematocides and fumigants: 1,3-dichloropropene, 2,3-dichloropropene, 1,2-dibromo-3-chloropropane, o-dichlorobenzene, and p-dichlorobenzene. Then, depending on sample consistency and type, the samples were diluted in, or extracted with organic solvent such as isooctane. A few of the high-fat extracts were passed through Florisil to remove excess fat or endogenous interferences. Analysis of the initial or cleaned up extracts was done by gas chromatography (GC) at 90 degrees C. The dichloropropenes were determined on 20% OV-101 columns with electron-capture and Hall electroconductivity detectors. The dichlorobenzenes and 1,2-dibromo-3-chloropropane, which elute beyond 30 min on the above columns, were determined on 5%-loaded columns using the same detectors. All five analytes were recovered from these techniques. Mean analyte recovery following a direct dilution or extraction was 83%, and following the Florisil cleanup step, was 52%. In 1986, a fumigant survey of about 200 foodstuffs by using this overall technique gave no findings of the five compounds studied here.

Determination of trigonelline, nicotinic acid, and caffeine in Yunnan Arabica coffee by microwave-assisted extraction and HPLC with two columns in series.

PubMed

Liu, Hongcheng; Shao, Jinliang; Li, Qiwan; Li, Yangang; Yan, Hong Mei; He, Lizhong

2012-01-01

A simple, rapid method was developed for simultaneous extraction of trigonelline, nicotinic acid, and caffeine from coffee, and separation by two chromatographic columns in series. The trigonelline, nicotinic acid, and caffeine were extracted with microwave-assisted extraction (MAE). The optimal conditions selected were 3 min, 200 psi, and 120 degrees C. The chromatographic separation was performed with two columns in series, polyaromatic hydrocarbon C18 (250 x 4.6 mm id, 5 microm particle size) and Bondapak NH2 (300 x 3.9 mm id, 5 microm particle size). Isocratic elution was with 0.02 M phosphoric acid-methanol (70 + 30, v/v) mobile phase at a flow rate of 0.8 mL/min. Good recoveries and RSD values were found for all analytes in the matrix. The LOD of the three compounds was 0.02 mg/L, and the LOQ was 0.005% in the matrix. The concentrations of trigonelline, nicotinic acid, and caffeine in instant coffee, roasted coffee, and raw coffee (Yunnan Arabica coffee) were assessed by MAE and hot water extraction; the correlation coefficients between concentrations of the three compounds obtained were close to 1.

The influence of alendronate on the healing of extraction sockets of ovariectomized rats assessed by in vivo micro-computed tomography.

PubMed

Jee, Jeong-Hyun; Lee, Wan; Lee, Byung Do

2010-08-01

Many dental patients take bisphosphonates to reduce the risk of hip and vertebral fractures. In vivo micro-computed tomography (micro-CT) was used to examine the longitudinal inhibitory effect of alendronate on the healing of extraction sockets in ovariectomized rats. Twenty 5-week-old Sprague-Dawley rats were assigned randomly to 1 of 3 groups: sham-operated (n = 5), and 2 ovariectomized (OVX) groups: saline treated (0.1 mL/100 g/d, n = 7) and alendronate treated (1 mg/kg/d, n = 8). Before micro-CT scanning, the left maxillary first molars of the rats were extracted. In vivo micro-CT (spatial resolution 50 x 50 mum) of the jaw was performed at baseline and at 2-week intervals for 6 weeks. Alveolar-bone radiographic densities and dimensions were analyzed with repeated measures analysis of variance. The bony healing patterns of the extraction sockets were also evaluated in each group. The radiographic socket densities of the sham-treated and OVX-alendronate groups significantly increased during the first 4 weeks after extraction (P < .05). At 2 weeks, the radiographic densities of the sockets in the OVX-saline group increased, but the increase was significantly lower than for the other groups at 4 weeks (P < .05). Newly formed bone was identified in the extraction sockets in all groups 2 to 6 weeks after extraction. There was a significant loss of alveolar ridge height at the second week postextraction compared with baseline, and at the fourth week compared with the second week (P < .05) except in the alendronate group. Alendronate appears to promote the healing of extraction sockets in estrogen-deficient rats and helps resist the loss of alveolar bone adjacent to extraction sockets. Copyright 2010 Mosby, Inc. All rights reserved.

Evaluation of an ODS column modified with zwitterionic/nonionic mixed surfactants and its application to direct injection determination of inorganic anions.

PubMed

Hasegawa, Takuya; Umemura, Tomonari; Koide, Akira; Chiba, Koichi; Ueki, Yuji; Tsunoda, Kin-ichi; Haraguchi, Hiroki

2005-08-01

An octadecylsilica (ODS) column modified with zwitterionic/nonionic mixed surfactants was evaluated for the direct injection determination of inorganic anions in biological fluids by ion chromatography. A zwitterionic surfactant (sulfobetaine-type) and a nonionic surfactant (polyoxyethylene-type) were used for a stationary-phase modification. When aqueous electrolyte solutions with concentrations of sub-mM to several mM were used as a mobile phase, the zwitterionic surfactant coated on the ODS surface exhibited unique separation selectivity for ionic species, while the nonionic surfactant coated on the ODS might have formed a hydrophilic network over the ODS surface and restricted matrix proteins from adsorbing on the stationary phase. Consequently, the mixed surfactant-modified column system allowed an efficient ion chromatographic separation of inorganic anions as well as a size-exclusive removal of column-fouling proteins. This separation system was applied to the direct injection determination of UV-absorbing anions in human saliva. The detection limits for nitrite, nitrate, iodide and thiocyanate were 3.1, 2.7, 4.5 and 25 microM, respectively, with UV detection at 210 nm (injection volume; 20 microl), and their relative standard deviations for 5 replicate measurements of saliva samples spiked with 100 microM each of those anions were 1.4, 0.9, 2.2 and 5.5%, respectively.

Evaluation of needle trap micro-extraction and solid-phase micro-extraction: Obtaining comprehensive information on volatile emissions from in vitro cultures.

PubMed

Oertel, Peter; Bergmann, Andreas; Fischer, Sina; Trefz, Phillip; Küntzel, Anne; Reinhold, Petra; Köhler, Heike; Schubert, Jochen K; Miekisch, Wolfram

2018-05-14

Volatile organic compounds (VOCs) emitted from in vitro cultures may reveal information on species and metabolism. Owing to low nmol L -1 concentration ranges, pre-concentration techniques are required for gas chromatography-mass spectrometry (GC-MS) based analyses. This study was intended to compare the efficiency of established micro-extraction techniques - solid-phase micro-extraction (SPME) and needle-trap micro-extraction (NTME) - for the analysis of complex VOC patterns. For SPME, a 75 μm Carboxen®/polydimethylsiloxane fiber was used. The NTME needle was packed with divinylbenzene, Carbopack X and Carboxen 1000. The headspace was sampled bi-directionally. Seventy-two VOCs were calibrated by reference standard mixtures in the range of 0.041-62.24 nmol L -1 by means of GC-MS. Both pre-concentration methods were applied to profile VOCs from cultures of Mycobacterium avium ssp. paratuberculosis. Limits of detection ranged from 0.004 to 3.93 nmol L -1 (median = 0.030 nmol L -1 ) for NTME and from 0.001 to 5.684 nmol L -1 (median = 0.043 nmol L -1 ) for SPME. NTME showed advantages in assessing polar compounds such as alcohols. SPME showed advantages in reproducibility but disadvantages in sensitivity for N-containing compounds. Micro-extraction techniques such as SPME and NTME are well suited for trace VOC profiling over cultures if the limitations of each technique is taken into account. Copyright © 2018 John Wiley & Sons, Ltd.

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

PubMed

Cools, Katherine; Terry, Leon A

2012-07-15

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

Human Milk MicroRNA and Total RNA Differ Depending on Milk Fractionation

PubMed Central

Alsaweed, Mohammed; Hepworth, Anna R.; Lefèvre, Christophe; Hartmann, Peter E.; Geddes, Donna T.

2015-01-01

ABSTRACT MicroRNA have been recently discovered in human milk signifying potentially important functions for both the lactating breast and the infant. Whilst human milk microRNA have started to be explored, little data exist on the evaluation of sample processing, and analysis to ensure that a full spectrum of microRNA can be obtained. Human milk comprises three main fractions: cells, skim milk, and lipids. Typically, the skim milk fraction has been measured in isolation despite evidence that the lipid fraction may contain more microRNA. This study aimed to standardize isolation of microRNA and total RNA from all three fractions of human milk to determine the most appropriate sampling and analysis procedure for future studies. Three different methods from eight commercially available kits were tested for their efficacy in extracting total RNA and microRNA from the lipid, skim, and cell fractions of human milk. Each fraction yielded different concentrations of RNA and microRNA, with the highest quantities found in the cell and lipid fractions, and the lowest in skim milk. The column‐based phenol‐free method was the most efficient extraction method for all three milk fractions. Two microRNAs were expressed and validated in the three milk fractions by qPCR using the three recommended extraction kits for each fraction. High expression levels were identified in the skim and lipid milk factions for these microRNAs. These results suggest that careful consideration of both the human milk sample preparation and extraction protocols should be made prior to embarking upon research in this area. J. Cell. Biochem. 116: 2397–2407, 2015. © 2015 The Authors. Journal of Cellular Biochemistry Published by Wiley Periodicals, Inc. PMID:25925799

Antispasmodic effect of Piper nigrum fruit hot water extract on rat ileum.

PubMed

Naseri, Mohammad Kazem Gharib; Yahyavi, Hoda

2008-06-01

The aim of this study was to investigate the effect of black pepper fruit hot water extract (BPE) on rat ileum contractility and the mechanism(s) of its action. The extract was prepared by adding black pepper powder to boiling distilled water followed by evaporated the solvent. Ileum was dissected from male adult rat (Wistar) and in Tyrode solution the tissue contractions were recorded by an isotonic transducer under 1 g tension. The cumulative concentrations of the BPE (0.0625-1 mg mL(-1)) reduced the ileum contractions induced by KCl (60 mM) or carbachol (10 microM) concentration dependently (p<0.001). In Ca2+-free Tyrode solution with high potassium (60 mM), BPE, (0.0625-1 mg mL(-1)) attenuated the contractions induced by cumulative concentrations of CaCl2 (0.225-2.7 mM) concentration dependently (ANOVA, p<0.05). The incubation of the tissue preparation (20 or 30 min) with L-NAME (100 microM), naloxone (1 microM) or propranolol (1 microM) did not reduce the extract antispasmodic effect on KCl-induced ileum contraction. The extract spasmolytic effect was attenuated neither by glibenclamide (10 microM) nor by tetraethylammonium (1 mM). Present results suggest that the spasmolytic effect of the extract on rat ileum was possibly mediated via Ca2+ influx.

Comparison of extraction techniques of robenidine from poultry feed samples.

PubMed

Wilga, Joanna; Wasik, Agata Kot-; Namieśnik, Jacek

2007-10-31

In this paper, effectiveness of six different commonly applied extraction techniques for the determination of robenidine in poultry feed has been compared. The sample preparation techniques included shaking, Soxhlet, Soxtec, ultrasonically assisted extraction, microwave - assisted extraction and accelerated solvent extraction. Comparison of these techniques was done with respect to the recovery extraction, temperature and time, reproducibility and solvent consumption. Every single extract was subjected to clean - up using aluminium oxide column (Pasteur pipette filled with 1g of aluminium oxide), from which robenidine was eluted with 10ml of methanol. The eluate from the clean-up column was collected in a volumetric flask, and finally it was analysed by HPLC-DAD-MS. In general, all extraction techniques were capable of isolating of robenidine from poultry feed, but the recovery obtained using modern extraction techniques was higher than that obtained using conventional techniques. In particular, accelerated solvent extraction was more superior to other techniques, which highlights the advantages of this sample preparation technique. However, in routine analysis, shaking and ultrasonically assisted extraction is still the preferred method for the solution of robenidine and other coccidiostatics.

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.

Kinetic performance of narrow-bore columns on a micro-system for high performance liquid chromatography.

PubMed

Gritti, Fabrice; Guiochon, Georges

2012-05-04

The kinetic performance of 0.5 mm × 50 mm columns packed with 2.7 μm Halo-C(18) core-shell particles and 3 μm EP-120-C(18) fully porous particles fitted on an Eksigent LC-Express Ultra μHPLC system were measured. The instrument contribution to band broadening was obtained by directly connecting the injection valve and the detector cell with a short, narrow PEEKSIL tube. The connections between the column and the connecting tubes, the column endfittings and its frits contribute to band spreading and are responsible for a significant rear peak tailing, even for retained compounds, resulting in a significant loss of efficiency. Our results show that the μHPLC system could outperform the current VHPLC systems using 2.1mm I.D. columns packed with 1.7 μm particles if it were using 0.5mm I.D. columns packed with 1 μm particles, if it could operate at a few kbar pressure drop, and if the sum of the contributions of the instrument, column endfittings and the column frits to band dispersion were three times smaller than it is at present. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-10-15

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

In vitro vascular effects produced by crude aqueous extract of green marine algae, Cladophora patentiramea (Mont.) Kützing, in aorta from normotensive rats.

PubMed

Lim, Yee-Ling; Mok, Shiueh-Lian

2010-01-01

To investigate the antihypertensive activity of aqueous extracts obtained from Malaysian coastal seaweeds and to determine the pharmacological mechanisms of the extracts on rat aorta in vitro. The antihypertensive activity of 11 species of seaweeds (5 brown, 1 red and 5 green algae) were tested by cumulative addition of the extracts to phenylephrine (PE)-precontracted Wistar-Kyoto (WKY) aortic rings in in vitro isometric contraction studies. Mechanisms for vasorelaxant effect were investigated in the presence of various antagonists. Of the 11 species tested, 2 showed a vasorelaxant effect. Further investigation of the mechanisms of action of the aqueous extract of green alga, Cladophora patentiramea (AECP),showed that the vascular relaxant effect was endothelium- and concentration-dependent. A maximum relaxation of 45.8 +/- 4.6% (n = 8, p < 0.001) was obtained at 0.1 mg/ml of extract, after which the response was found to reduce in a concentration-dependent manner to 15.7 +/- 4.9% (n = 8, p < 0.001) at the highest extract concentration tested. Pretreatment of endothelium-intact aortic rings with Nomega-nitro-L-arginine methyl ester (L-NAME, 30 microM), (1)H-[1,2,4]oxadiazolo[4,3-a]quinoxalin-1-one (ODQ, 10 microM) and methylene blue (100 microM) resulted in a complete blockade of AECP-induced vasorelaxation. However, the relaxant effects of the extract were not blocked by atropine (1 microM), indomethacin (10 microM) and glibenclamide (10 microM), although the maximum relaxant responses were enhanced in the presence of glibenclamide. Our data showed that the in vitro vascular relaxant effect of AECPwas mediated through endothelium-dependent nitric oxide-cGMP pathway, and was not associated with the release of vasodilator prostaglandins, activation of muscarinic receptors, or ATP-sensitive potassium channels opening. Copyright 2010 S. Karger AG, Basel.

Effects of repeated exposure to 4-nonylphenol on the zooplankton community in littoral enclosures

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

O`Halloran, S.L.; Liber, K.; Gangl, J.A.

1999-03-01

The effects of 4-nonylphenol (NP) on freshwater zooplankton were evaluated in 18 littoral enclosure mesocosms in northeastern Minnesota. The 18 enclosures were allocated to three blocks of six units with each block including two untreated control enclosures and one enclosure for each of four NP treatments. Treated enclosures received 11 applications of NP over a 20-d period between July 8 and 28, 1993. Maximum NP concentrations measured in the water column 2 h after each application averaged ({+-} SD) 5 {+-} 4, 23 {+-} 11, 76 {+-} 21, and 243 {+-} 41 {micro}g/L over the 11 applications. Nonylphenol dissipated rapidlymore » from the water column but was more persistent in sediments and in/on macrophytes. All cladoceran and copepod taxa were significantly reduced in abundance at 243 {+-} 41 {micro}g/L; some sensitive taxa were also affected by 76 {+-} 21 and 23 {+-} 11 {micro}g/L. While many rotifer taxa were unaffected at any of the test concentrations, several were affected at {ge} 76 {+-} 21 {micro}g/L. Ostracods were only affected at 2,243 {+-} 41 {micro}g/L. No zooplankton taxon was affected at 5 {+-} 4 {micro}g/L. The period of maximum impact usually occurred within 1 to 7 d of the last NP application, and recovery to control abundance levels generally occurred within 7 to 28 d of the last NP application. Two sensitive taxa, Acroperus and Calanoida, did not recover at {ge} 76 {+-} 21 {micro}g/L by the end of the study. The maximum acceptable toxicant concentration for protection of all zooplankton taxa was estimated at {approximately} 10 {micro}g/L, although overall community diversity was unaffected at 23 {+-} 11. The water was the most probable route of NP exposure, but the greater persistence of NP residues in/on macrophytes may have contributed to the lack of recovery of some macrophyte-associated taxa.« less

Simultaneous determination of intracellular UDP-sugars in hyaluronic acid-producing Streptococcus zooepidemicus.

PubMed

Franke, Lukáš; Čožíková, Dagmar; Smirnou, Dzianis; Hermannová, Martina; Hanová, Tereza; Růžičková, Andrea; Velebný, Vladimír

2015-08-01

Two chromatographic methods for the quantitative analysis of uridine diphosphate (UDP) sugars involved in hyaluronan pathway of Streptococcus zooepidemicus (SEZ) were developed and compared. The sample preparation protocol using centrifugation and extraction in hot ethanol was employed prior to the analyses. Separation was achieved using an anion exchange Spherisorb SAX column or a Shodex QA-825 column connected with a photodiode array (PDA) detector. To increase the throughput of the chromatography method employing the Spherisorb SAX column, the solid phase extraction (SPE) procedure was introduced. Method validation results displayed that limits of detection (LODs) of UDP-glucose (UDP-Glc), UDP-N-acetylglucosamine (UDP-GlcNAc) and UDP-glucuronic acid (UDP-GlcA) calculated according to QC Expert software were in the low micromolar range and the coefficient of correlation (R(2)) was above 0.997. However, the analytical technique using the Spherisorb SAX column resulted in 80-90% recoveries and low LODs (≤6.19μM), the Shodex QA-825 column showed better long-term stability and reproducible chromatographic properties (RSD≤5.60%). The Shodex QA-825 column was successfully used to monitor UDP-sugar levels during the growth rate of SEZ cells. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous determination of quinolones in fish by liquid chromatography coupled with fluorescence detection: comparison of sub-2 microm particles and conventional C18 columns.

PubMed

Zhang, Hong; Chen, Si; Lu, Yanbin; Dai, Zhiyuan

2010-07-01

A simple and effective multi-residue analysis method is presented for the extraction and determination of eleven quinolones (pipemidic acid, enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin, gatifloxacin, difloxacin, oxolinic acid, nalidixic acid and flumequine) in fish tissues. In this study, multi-residue separations on four columns packed with 5 microm or sub-2 microm particles were simultaneously developed for the purpose of comparison. Various gradients were optimized and best resolutions were achieved on each column. A short and sub-2 microm particle-sized HPLC column was chosen for its advantages in analysis time and column performance. Additionally, considering the matrix effect of the complex crude fish tissue, an effective extraction protocol was also established for sample pre-treatment procedure. Good recoveries (71-98%) were obtained from samples fortified with a mix of eleven quinolones at three levels, with satisfactory relative standard deviations and limits of detection. As a result, the sub-2 microm HPLC column and proposed analytical procedures have been evaluated and applied to the analysis of different fish tissues. Detectable residues were observed in 8 of 30 samples, at concentrations ranging from 4.74 to 23.27 microg/kg.

Comparison of a novel passive sampler to standard water-column sampling for organic contaminants associated with wastewater effluents entering a New Jersey stream

USGS Publications Warehouse

Alvarez, D.A.; Stackelberg, P.E.; Petty, J.D.; Huckins, J.N.; Furlong, E.T.; Zaugg, S.D.; Meyer, M.T.

2005-01-01

Four water samples collected using standard depth and width water-column sampling methodology were compared to an innovative passive, in situ, sampler (the polar organic chemical integrative sampler or POCIS) for the detection of 96 organic wastewater-related contaminants (OWCs) in a stream that receives agricultural, municipal, and industrial wastewaters. Thirty-two OWCs were identified in POCIS extracts whereas 9-24 were identified in individual water-column samples demonstrating the utility of POCIS for identifying contaminants whose occurrence are transient or whose concentrations are below routine analytical detection limits. Overall, 10 OWCs were identified exclusively in the POCIS extracts and only six solely identified in the water-column samples, however, repetitive water samples taken using the standard method during the POCIS deployment period required multiple trips to the sampling site and an increased number of samples to store, process, and analyze. Due to the greater number of OWCs detected in the POCIS extracts as compared to individual water-column samples, the ease of performing a single deployment as compared to collecting and processing multiple water samples, the greater mass of chemical residues sequestered, and the ability to detect chemicals which dissipate quickly, the passive sampling technique offers an efficient and effective alternative for detecting OWCs in our waterways for wastewater contaminants.

Enhanced reductive dechlorination in columns treated with edible oil emulsion

NASA Astrophysics Data System (ADS)

Long, Cameron M.; Borden, Robert C.

2006-09-01

The effect of edible oil emulsion treatment on enhanced reductive dechlorination was evaluated in a 14 month laboratory column study. Experimental treatments included: (1) emulsified soybean oil and dilute HCl to inhibit biological activity; (2) emulsified oil only; (3) emulsified oil and anaerobic digester sludge; and (4) continuously feeding soluble substrate. A single application of emulsified oil was effective in generating strongly reducing, anaerobic conditions for over 14 months. PCE was rapidly reduced to cis-DCE in all three live columns. Bioaugmentation with a halorespiring enrichment culture resulted in complete dechlorination of PCE to ethene in the soluble substrate column (yeast extract and lactate). However, an additional treatment with a pulse of yeast extract and bioaugmentation culture was required to stimulate complete dechlorination in the emulsion treated columns. Once the dechlorinating population was established, the emulsion only column degraded PCE from 90-120 μM to below detection with concurrent ethene production in a 33 day contact time. The lower biodegradation rates in the emulsion treated columns compared to the soluble substrate column suggest that emulsified oil barriers may require a somewhat longer contact time for effective treatment. In the HCl inhibited column, partitioning of PCE to the retained oil substantially delayed PCE breakthrough. However, reduction of PCE to more soluble degradation products ( cis-DCE, VC and ethene) greatly reduced the impact of oil-water partitioning in live columns. There was only a small decline in the hydraulic conductivity ( K) of column #1 (low pH + emulsion, Kfinal/ Kinitial = 0.57) and column #2 (live + emulsion, Kfinal/ Kinitial = 0.73) indicating emulsion injection did not result in appreciable clogging of the clayey sand. However, K loss was greater in column #3 (sludge +emulsion, Kfinal/ Kinitial = 0.12) and column #4 (soluble substrate, Kfinal/ Kinitial = 0.03) indicating clogging due to biomass and/or gas production can be significant.

A simple HPLC method for simultaneous determination of lopinavir, ritonavir and efavirenz.

PubMed

Usami, Yoshiko; Oki, Tsuyoshi; Nakai, Masahiko; Sagisaka, Masafumi; Kaneda, Tsuguhiro

2003-06-01

We developed a simple HPLC method for the simultaneous determination of lopinavir (LPV), ritonavir (RTV) and efavirenz (EFV) to evaluate the efficiency of co-administration of LPV/RTV and EFV in Japanese patients enrolled in a clinical study. The monitoring of LPV plasma concentration is important because co-administration of LPV/RTV with EFV sometimes decreases plasma concentrations of LPV caused by EFV activation of cytochrome P-450 3A. A solution of acetonitrile, methanol and tetramethylammonium perchlorate (TMAP) in dilute aqueous trifluoroacetic acid (TFA) has been used as the mobile phase in a HPLC method to elute LPV and RTV. We found that a solvent ratio of 45 : 5 : 50 (v/v/v) of acetonitrile/methanol/0.02 M TMAP in 0.2% TFA optimized separation of LPV, RTV and EFV. A column temperature of 30 degrees C was necessary for the reproducibility of the analyses. Standard curves were linear in the range 0.060 to 24.06 micro g/ml for LPV, 0.010 to 4.16 micro g/ml for RTV, and 0.047 to 37.44 micro g/ml for EFV. Coefficients of variation (CVs) of LPV, RTV and EFV in intraday and interday assays ranged from 1.5 to 4.0%, 2.5 to 16.8% and 1.0 to 7.7%, respectively. Accuracies ranged from 100 to 110%, 101 to 116% and 99 to 106% for LPV, RTV and EFV, respectively. The extraction recoveries were 77-87, 77-83 and 81-91% for LPV, RTV and EFV, respectively.

Evaluation of injection methods for fast, high peak capacity separations with low thermal mass gas chromatography.

PubMed

Fitz, Brian D; Mannion, Brandyn C; To, Khang; Hoac, Trinh; Synovec, Robert E

2015-05-01

Low thermal mass gas chromatography (LTM-GC) was evaluated for rapid, high peak capacity separations with three injection methods: liquid, headspace solid phase micro-extraction (HS-SPME), and direct vapor. An Agilent LTM equipped with a short microbore capillary column was operated at a column heating rate of 250 °C/min to produce a 60s separation. Two sets of experiments were conducted in parallel to characterize the instrumental platform. First, the three injection methods were performed in conjunction with in-house built high-speed cryo-focusing injection (HSCFI) to cryogenically trap and re-inject the analytes onto the LTM-GC column in a narrower band. Next, the three injection methods were performed natively with LTM-GC. Using HSCFI, the peak capacity of a separation of 50 nl of a 73 component liquid test mixture was 270, which was 23% higher than without HSCFI. Similar peak capacity gains were obtained when using the HSCFI with HS-SPME (25%), and even greater with vapor injection (56%). For the 100 μl vapor sample injected without HSCFI, the preconcentration factor, defined as the ratio of the maximum concentration of the detected analyte peak relative to the analyte concentration injected with the syringe, was determined to be 11 for the earliest eluting peak (most volatile analyte). In contrast, the preconcentration factor for the earliest eluting peak using HSCFI was 103. Therefore, LTM-GC is demonstrated to natively provide in situ analyte trapping, although not to as great an extent as with HSCFI. We also report the use of LTM-GC applied with time-of-flight mass spectrometry (TOFMS) detection for rapid, high peak capacity separations from SPME sampled banana peel headspace. Copyright © 2015 Elsevier B.V. All rights reserved.

Anticonvulsant effect of aqueous extract of Valeriana officinalis in amygdala-kindled rats: possible involvement of adenosine.

PubMed

Rezvani, Mohammad Ebrahim; Roohbakhsh, Ali; Allahtavakoli, Mohammad; Shamsizadeh, Ali

2010-02-03

Valeriana officinalis L. (valerian) root extract has been used as an antiepileptic herbal medicine in Iran. In the present study the effect of valerian extracts on an experimental model of temporal lobe epilepsy (TLE) was evaluated. Moreover, the involvement of adenosine system in the actions of aqueous extract of valerian was evaluated. Bipolar stimulating and monopolar recording electrodes were implanted stereotaxically in the right basolateral amygdala of male Sprague-Dawley rats. After kindling, the effect of aqueous (200, 500 and 800 mg/kg; intraperitoneal) and petroleum ether (PE; 50 and 100mg/kg; intraperitoneal) extracts of valerian and CPT (selective A(1) receptor antagonist; 10 and 20 microM; intracerebroventricular) on afterdischarge duration (ADD), duration of stage 5 seizure (S5D) and latency to the onset of bilateral forelimb clonuses (S4L) were measured. The effect of CPT (10 microM) on the response of aqueous extract of valerian (500 mg/kg) was also determined. The results showed that aqueous extract of valerian had anticonvulsant effect. However, PE extract and CPT (20 microM) had proconvulsant effect. Administration of CPT (10 microM) before the administration of aqueous extract decreased the anticonvulsant effect of valerian. The results showed significant anticonvulsant effect for aqueous but not PE extract of valerian. Moreover, CPT as a selective adenosine A(1) receptor antagonist decreased the anticonvulsant effect of valerian aqueous extract. Therefore, we concluded that part of anticonvulsant effect of valerian probably is mediated through activation of adenosine system. Copyright 2009 Elsevier Ireland Ltd. All rights reserved.

Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

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

Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,

Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gelsmore » were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r{sup 2}=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.« less

Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

PubMed

Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

2013-05-07

A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all <2%) and average recoveries (from 79.6 to 90.8% for AFs and from 93.6 to 97.3% for OTA, respectively). The results of the application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample.

[Separation/preconcentration of trace rare earth elements in Tricholoma giganteum by micro-column with nanometer A1203 and their determination by ICP-AES].

PubMed

Liu, Hong-gao; Wang, Yuan-zhong

2010-01-01

Using a micro-column packed with immobilized 1-phenyl-3-methyl-4-bonzoil-5-pyrazone(PMBP) on nanometer Al2O3 powder as the adsorption material, the adsorption and elution behaviors of rare earth ions (Sc3+, Y3+ and La3+) on the above material under dynamic conditions were studied with inductively coupled plasma-atomic emission spectrometry. The conditions for preconcentration of rare earth ions were optimized, and the results show that the studied ions can be adsorbed quantitatively on the above material at pH 4.5 and the analytes adsorbed on the column can be eluted with 0.5 mol x L(-1) HCl solution. The detection limits of the method for Sc, Y and La were 0.15, 0.18 and 0.34 microg x L(-1), respectively, and the relative standard deviations were 2.5%, 3.0% and 1.7%, respectively (n=12, c = 0.5 mg x L(-1)). The proposed method was applied to the determination of trace amount of Sc, Y and La in Tricholoma giganteum with satisfactory results.

Antioxidant and antimicrobial activities of ethyl acetate extract, fractions and compounds from stem bark of Albizia adianthifolia (Mimosoideae).

PubMed

Tamokou, Jean de Dieu; Simo Mpetga, Deke James; Keilah Lunga, Paul; Tene, Mathieu; Tane, Pierre; Kuiate, Jules Roger

2012-07-18

Albizia adianthifolia is used traditionally in Cameroon to treat several ailments, including infectious and associated diseases. This work was therefore designed to investigate the antioxidant and antimicrobial activities of ethyl acetate extract, fractions and compounds isolated from the stem bark of this plant. The plant extract was prepared by maceration in ethyl acetate. Its fractionation was done by column chromatography and the structures of isolated compounds were elucidated using spectroscopic data in conjunction with literature data. The 1,1-diphenyl-2-picrylhydrazyl (DPPH) and trolox equivalent antioxidant capacity (TEAC) assays were used to detect the antioxidant activity. Broth micro-dilution method was used for antimicrobial test. Total phenol content was determined spectrophotometrically in the extracts by using Folin-Ciocalteu method. The fractionation of the extract afforded two known compounds: lupeol (1) and aurantiamide acetate (2) together with two mixtures of fatty acids: oleic acid and n-hexadecanoic acid (B₁); n-hexadecanoic acid, octadecanoic acid and docosanoic acid (B₂). Aurantiamide acetate was the most active compound. The total phenol concentration expressed as gallic acid equivalents (GAE) was found to vary from 1.50 to 13.49 μg/ml in the extracts. The antioxidant activities were well correlated with the total phenol content (R² = 0.946 for the TEAC method and R² = 0.980 for the DPPH free-radical scavenging assay). Our results clearly reveal that the ethyl acetate extract from the stem bark of A. adianthifolia possesses antioxidant and antimicrobial principles. The antioxidant activity of this extract as well as that of compound 2 are being reported herein for the first time. These results provide promising baseline information for the potential use of this plant as well as compound 2 in the treatment of oxidative damage and infections associated with the studied microorganisms.

Preparative electrophoresis with on-column optical fiber monitoring and direct elution into a minimized volume.

PubMed

Jackson, George W; Willson, Richard

2005-11-01

A "column-format" preparative electrophoresis device which obviates the need for gel extraction or secondary electro-elution steps is described. Separated biomolecules are continuously detected and eluted directly into a minimal volume of free solution for subsequent use. An optical fiber allows the species of interest to be detected just prior to elution from the gel column, and a small collection volume is created by addition of an ion-exchange membrane near the end of the column.

[Research on chemical constituents from stem of Gymnema sylvestre].

PubMed

Zhen, Han-shen; Zhu, Xue-yan; Lu, Ru-mei; Liang, Jie; Qiu, Qin; Meng, Qi-miao

2008-08-01

To study on the chemical constituents from the stem of Gymnema sylvestre. The constituents were extracted by percolation with ethanol. Then the extract was separated by systemic solvent separation methods. The part of n-butanol extract was isolated and purified by macroporous adsorptive resins, silica gel column chromatography, sephadex gel column chromatography and recrystallization. The isolated compounds were identified by spectrum methods. Eight compounds were isolated and identified as fallows: Conduritol A(I), 1-Heptadecanol(II), Stigmasterol glucoside(III), 1-Quercitol(IV), 1-Octadecanol(V), Potassium nitrate(VI), Lupeol cinnamate(VII), Stigmasterol(VIII). Chemical compounds II, III, V, VII are firstly obtained from this plant.

Enhanced light extraction efficiency of micro-ring array AlGaN deep ultraviolet light-emitting diodes

NASA Astrophysics Data System (ADS)

Bekele Fayisa, Gabisa; Lee, Jong Won; Kim, Jungsub; Kim, Yong-Il; Park, Youngsoo; Kim, Jong Kyu

2017-09-01

An effective approach to overcome inherently poor light extraction efficiency of AlGaN-based deep ultraviolet (DUV) light-emitting diodes (LEDs) is presented. We demonstrated the 5 × 5 array micro-ring DUV LED having an inclined sidewall at the outer perimeter and a p-GaN-removed inner circle of the micro-ring, together with MgF2/Al omnidirectional reflectors. The micro-ring array DUV LED shows remarkably higher light output power by 70% than the reference, consistent with the calculated result, as well as comparable turn-on and operational voltages, which are attributed to the effective extraction of strong transverse-magnetic polarized anisotropic emission and the reduction of the absorption loss by the p-GaN contact layer, simultaneously.

Preparation of porous hollow silica spheres via a layer-by-layer process and the chromatographic performance

NASA Astrophysics Data System (ADS)

Wei, Xiaobing; Gong, Cairong; Chen, Xujuan; Fan, Guoliang; Xu, Xinhua

2017-03-01

Hollow silica spheres possessing excellent mechanical properties were successfully prepared through a layer-by-layer process using uniform polystyrene (PS) latex fabricated by dispersion polymerization as template. The formation of hollow SiO2 micro-spheres, structures and properties were observed in detail by zeta potential, SEM, TEM, FTIR, TGA and nitrogen sorption porosimetry. The results indicated that the hollow spheres were uniform with particle diameter of 1.6 μm and shell thickness of 150 nm. The surface area was 511 m2/g and the pore diameter was 8.36 nm. A new stationary phase for HPLC was obtained by using C18-derivatized hollow SiO2 micro-spheres as packing materials and the chromatographic properties were evaluated for the separation of some regular small molecules. The packed column showed low column pressure, high values of efficiency (up to about 43 000 plates/m) and appropriate asymmetry factors.

Predicting recovery from acid rain using the micro-spatial heterogeneity of soil columns downhill the infiltration zone of beech stemflow: introduction of a hypothesis.

PubMed

Berger, Torsten W; Muras, Alexander

Release of stored sulfur may delay the recovery of soil pH from Acid Rain. It is hypothesized that analyzing the micro-spatial heterogeneity of soil columns downhill of a beech stem enables predictions of soil recovery as a function of historic acid loads and time. We demonstrated in a very simplified approach, how these two different factors may be untangled from each other using synthetic data. Thereafter, we evaluated the stated hypothesis based upon chemical soil data with increasing distance from the stem of beech trees. It is predicted that the top soil will recover from acid deposition, as already recorded in the infiltration zone of stemflow near the base of the stem. However, in the between trees areas and especially in deeper soil horizons recovery may be highly delayed.

A new approach for direct imaging of Alpha radiation by using Micro Pattern Gas Detectors in SQS mode

NASA Astrophysics Data System (ADS)

Souri, R.; Negarestani, A.; Mahani, M.

2018-03-01

In this study, the design, simulation and construction of three micro pattern gas-detectors, THGEM, with different geometric dimensions are presented. Moreover, their ability of operation in SQS mode to determine the incident rays position without using any conventional imaging system is investigated. In the presence of UV absorbing gas mixtures, the proportional mode of the gas detector operation is followed by SQS mode as soon as the visible light column appears at the ray entrance location. In the method employed, each THGEM hole as an image pixel independent of other holes can operate in SQS mode with emerging a light column. As a consequence, it can be used for alpha beam imaging since the brightness of each hole at a certain voltage is proportional to the number of primary electrons entering the hole.

Integrated protein analysis platform based on column switch recycling size exclusion chromatography, microenzymatic reactor and microRPLC-ESI-MS/MS.

PubMed

Yuan, Huiming; Zhou, Yuan; Zhang, Lihua; Liang, Zhen; Zhang, Yukui

2009-10-30

An integrated platform with the combination of proteins and peptides separation was established via the unit of on-line proteins digestion, by which proteins were in sequence separated by column switch recycling size exclusion chromatography (csrSEC), on-line digested by an immobilized trypsin microreactor, trapped and desalted by two parallel C8 precolumns, separated by microRPLC with the linear gradient of organic modifier concentration, and identified by ESI-MS/MS. A 6-protein mixture, with Mr ranging from 10 kDa to 80 kDa, was used to evaluate the performance of the integrated platform, and all proteins were identified with sequence coverage over 5.67%. Our experimental results demonstrate that such an integrated platform is of advantages such as good time compatibility, high peak capacity, and facile automation, which might be a promising approach for proteome study.

Micro-column plasma emission liquid chromatograph

DOEpatents

Gay, Don D.

1984-01-01

In a direct current plasma emission spectrometer for use in combination with a micro-column liquid chromatograph, an improved plasma source unit. The plasma source unit includes a quartz capillary tube having an inlet means, outlet off gas means and a pair of spaced electrodes defining a plasma region in the tube. The inlet means is connected to and adapted to receive eluant of the liquid chromatograph along with a stream of plasma-forming gas. There is an opening through the wall of the capillary tube penetrating into the plasma region. A soft glass capillary light pipe is disposed at the opening, is connected to the spectrometer, and is adapted to transmit light passing from the plasma region to the spectrometer. There is also a source of electromotive force connected to the electrodes sufficient to initiate and sustain a plasma in the plasma region of the tube.

An in vitro evaluation of cytochrome P450 inhibition and P-glycoprotein interaction with goldenseal, Ginkgo biloba, grape seed, milk thistle, and ginseng extracts and their constituents.

PubMed

Etheridge, Amy S; Black, Sherry R; Patel, Purvi R; So, James; Mathews, James M

2007-07-01

Drug-herb interactions can result from the modulation of the activities of cytochrome P450 (P450) and/or drug transporters. The effect of extracts and individual constituents of goldenseal, Ginkgo biloba (and its hydrolyzate), grape seed, milk thistle, and ginseng on the activities of cytochrome P450 enzymes CYP1A2, CYP2C8, CYP2C9, CYP2C19, CYP2D6, CYP2E1, and CYP3A4 in human liver microsomes were determined using enzyme-selective probe substrates, and their effect on human P-glycoprotein (Pgp) was determined using a baculovirus expression system by measuring the verapamil-stimulated, vanadate-sensitive ATPase activity. Extracts were analyzed by HPLC to standardize their concentration(s) of constituents associated with the pharmacological activity, and to allow comparison of their effects on P450 and Pgp with literature values. Many of the extracts/constituents exerted > or = 50 % inhibition of P450 activity. These include those from goldenseal (normalized to alkaloid content) inhibiting CYP2C8, CYP2D6, and CYP3A4 at 20 microM, ginkgo inhibiting CYP2C8 at 10 microM, grape seed inhibiting CYP2C9 and CYP3A4 at 10 microM, milk thistle inhibiting CYP2C8 at 10 microM, and ginsenosides F1 and Rh1 (but not ginseng extract) inhibiting CYP3A4 at 10 microM. Goldenseal extracts/constituents (20 microM, particularly hydrastine) and ginsenoside Rh1 stimulated ATPase at about half of the activity of the model substrate, verapamil (20 microM). The data suggest that the clearance of a variety of drugs may be diminished by concomitant use of these herbs via inhibition of P450 enzymes, but less so by Pgp-mediated effects.

Development of an efficient fractionation method for the preparative separation of sesquiterpenoids from Tussilago farfara by counter-current chromatography.

PubMed

Song, Kwangho; Lee, Kyoung Jin; Kim, Yeong Shik

2017-03-17

A novel application of counter-current chromatography (CCC) to enrich plant extracts using direct and continuous injection (CCC-DCI) was developed to fractionate sesquiterpenoids from the buds of Tussilago farfara L. In this study, an n-hexane-acetonitrile-water (HAcW) solvent system was separately pumped into the CCC column, and an extraction solution (45% acetonitrile) was directly and continuously injected into the CCC column. Since the extraction solution was used as a mobile phase in this method, solvent consumption could be greatly reduced. To enrich the extraction solution (315.9g/5.4L), only 4.2L water, 4.6L acetonitrile, and 1.2L n-hexane were used, including the extraction step. Finally, 6.8g of a sesquiterpenoid-enriched (STE) fraction was obtained from the crude extract (315.9g) of Tussilago farfara (1kg) in a single CCC run with a separation time of 8.5h. The sample injection capacity of CCC-DCI was greater than 300g; this amount of sample could not be handled in conventional CCC or other fractionation methods with the same column volume. Moreover, three major sesquiterpenoids (1: tussilagone, 2: 14-acetoxy-7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-notonipetranone, and 3: 7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-3, 14-dehydro-Z-notonipetranone) were purified from the STE fraction by CCC, and their chemical structures were elucidated by 1 H NMR and 13 C NMR. A quantification study was conducted, and the contents of compounds 1-3 in the CCC-DCI fraction were higher than those of conventional multi-step fractionations performed in series: solvent partitioning and open column chromatography. Furthermore, the average CCC-DCI recoveries were 96.1% (1), 96.9% (2), and 94.6% (3), whereas the open column chromatography recoveries were 77.7% (1), 66.5% (2), and 58.4% (3). The developed method demonstrates that CCC is a useful technique for enriching target components from natural products. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation of Ellagitannin-Rich Phenolics from U.S. Pecans and Chinese Hickory Nuts Using Fused-Core HPLC Columns and Their Characterization.

PubMed

Gong, Yi; Pegg, Ronald B

2017-07-19

U.S. pecans and Chinese hickory nuts possess a wide array of phenolic constituents with potential health benefits including phenolic acids and proanthocyanidins. Only limited information is available, however, on their compositions. The present study optimized the separation performance and characterized the low-molecular-weight phenolic fractions of these nuts with C18 and pentafluorophenyl (PFP) fused-core LC columns by employing a kinetic approach. Although both types of reversed-phase columns demonstrated similar performance in general, the PFP column furnished greater plate numbers and superior peak shapes for the low-molecular-weight fractions as well as overall separations of ellagic acid derivatives. The high-molecular-weight fraction of pecans, analyzed by a 3-μm HILIC column, possessed more proanthocyanidins than the Chinese hickory nuts with dimers and trimers (31.4 and 18.34 mg/g crude extract, respectively) being present at the greatest levels. Chinese hickory nuts had lower proanthocyanidin content but possessed tetramers and pentamers at 4.46 and 4.01 mg/g crude extract, respectively.

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

Hewitt, A.D.; Jenkins, T.F.

An on-site method has been developed for estimating concentrations of TNT, RDX, 2,4-DNT, and the two most commonly encountered environmental transformation products of TNT, 2-amino-4,6-dinitrotoluene and 4-amino-2,6- dinitrotoluene, in soil and groundwater using gas chromatography and the nitrogen-phosphorus detector (NPD). Soil samples (20 g) are extracted by shaking with 20 mL of acetone, and extracts are filtered through a Millex SR (0.5- micrometers) filter. Groundwater samples (1 L) were passed through SDB-RPS extraction disks that were subsequently extracted with 5 mL of acetone. A 1- micro-L volume of a soil or water extract is manually injected into a field- transportablemore » gas chromatograph equipped with a NPD and a heated injection port. Separations are conducted on a Restek Crossbond 100% dimethyl polysiloxane column, 6 m x 0.53-mm i.d., 1.5 mm, using nitrogen carrier gas at 9.5 mL/min. Retention times range from 3.0 min. for 2,4-dinitrotoluene (2,4-DNT) to 5.6 min. for 2-amino-4,6-dinitrotoluene. Method detection limits were less than 0.16 mg/ kg for soil and less than 1.0 microgram/L for groundwater. One of the major advantages of this method, over currently available colorimetric and enzyme immunoassay on-site methods, is the ability to quantify individual target analytes that often coexist in soils and groundwater contaminated with explosive residues. This method will be particularly useful at military antitank firing ranges where it is necessary to quantify residual concentrations of RDX in the presence of high concentrations of HMX, and when the transformation products of TNT need to be identified.« less

Determination of available phosphorus in soils by using a new extraction procedure and a flow injection amperometric system.

PubMed

Jakmunee, Jaroon; Junsomboon, Jaroon

2009-09-15

A new extraction procedure based on an off-line extraction column was proposed for extracting of available phosphorus from soils. The column was fabricated from a plastic syringe fitted at the bottom with a cotton wool and a piece of filter paper to support a soil sample. An aliquot (50 mL) of extracting solution (0.05 M HCl+0.0125 M H(2)SO(4)) was used to extract the sample under gravity flow and the eluate was collected in a polyethylene bottle. The extract was then analyzed for phosphorus contents by a simple flow injection amperometric system, employing a set of three-way solenoid valves as an injection valve. The method is based on the electrochemical reduction of 12-molybdophosphate which is produced on-line by the reaction of orthophosphate with acidic molybdate and the electrical current produced was directly proportional to the concentration of phosphate in range of 0.1-10.0 mg L(-1) PO(4)-P, with a detection limit of 0.02 mg L(-1). Relative standard for 11 replicate injections of 5 mg L(-1) PO(4)-P was 0.5%. A sample through put of 35 h(-1) was achieved, with consumption of 14 mg KCl, 10mg ammonium molybdate and 0.05 mL H(2)SO(4) per analysis. The detection system does not suffer from the interferences that are encountered in the photometric method such as colored substances, colloids, metal ions, silicate and refractive index effect (Schlieren effect). The results obtained by the column extraction procedure were well correlated with those obtained by the steady-state extraction procedure, but showed slightly higher extraction efficiency.

[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.

Study of Scanning Micro-arc Oxidation and Coating Development

NASA Astrophysics Data System (ADS)

Xia, Lingqin; Han, Jianmin; Domblesky, Joseph P.; Yang, Zhiyong; Li, Weijing

2017-11-01

Micro-arc oxidation (MAO) continues to be the focus of numerous investigations, whereas relatively few studies have considered scanning micro-arc oxidation (SMAO). In the present work, an experimental study was performed using stationary and moving electrodes to investigate coating development in SMAO and discern the effect of key process parameters. Examination of oxide deposits made on A356 aluminum show that coating thickness and growth rate are inversely related to inter-electrode spacing and travel speed. An evaluation of SMAO deposits made by stationary and moving nozzles revealed that coating thickness profiles follow a Gaussian distribution due to the electrolyte flow field in the impingement zone. Hardness surveys and scanning electron microscope analysis of SMAO coatings revealed that micro-hardness distributions and cross-sectional morphology are similar to MAO for a stationary nozzle but that a denser outer layer develops when a moving nozzle is used. This is attributed to a high density of discharge occurring in micropores of the oxide film and remelting which results from the moving electrolyte column. Analysis of voltage-current characteristic curves shows that the resistance of the electrolyte column is essentially linear over the range considered and results indicate that it can be modeled as a variable length resistor. While further testing is needed, results confirm that SMAO is suitable for coating large, planar parts and for repairing worn surfaces.

[Determination of azoxystrobin in tea by HPLC].

PubMed

Chonan, T

2001-08-01

A determination method has been developed for azoxystrobin in tea by HPLC. Azoxystrobin was extracted from a sample with acetone, and the extract was passed through an alumina column to remove tannin. The eluate was concentrated to ca. 25 mL and passed through a Sep-Pak Vac tC18 to remove pigments. The eluate was cleaned-up by using liquid-liquid partition, and Florisil and silica-gel columns. The HPLC analysis for azoxystrobin was carried out on a C18 column with acetonitrile-water (9:11) as the mobile phase, with ultraviolet detection at 260 nm. The recovery of azoxystrobin fortified at the level of 0.4 microgram/g was 90.2% and the limit of determination was 0.2 microgram/g.

Reproducible Tissue Homogenization and Protein Extraction for Quantitative Proteomics Using MicroPestle-Assisted Pressure-Cycling Technology.

PubMed

Shao, Shiying; Guo, Tiannan; Gross, Vera; Lazarev, Alexander; Koh, Ching Chiek; Gillessen, Silke; Joerger, Markus; Jochum, Wolfram; Aebersold, Ruedi

2016-06-03

The reproducible and efficient extraction of proteins from biopsy samples for quantitative analysis is a critical step in biomarker and translational research. Recently, we described a method consisting of pressure-cycling technology (PCT) and sequential windowed acquisition of all theoretical fragment ions-mass spectrometry (SWATH-MS) for the rapid quantification of thousands of proteins from biopsy-size tissue samples. As an improvement of the method, we have incorporated the PCT-MicroPestle into the PCT-SWATH workflow. The PCT-MicroPestle is a novel, miniaturized, disposable mechanical tissue homogenizer that fits directly into the microTube sample container. We optimized the pressure-cycling conditions for tissue lysis with the PCT-MicroPestle and benchmarked the performance of the system against the conventional PCT-MicroCap method using mouse liver, heart, brain, and human kidney tissues as test samples. The data indicate that the digestion of the PCT-MicroPestle-extracted proteins yielded 20-40% more MS-ready peptide mass from all tissues tested with a comparable reproducibility when compared to the conventional PCT method. Subsequent SWATH-MS analysis identified a higher number of biologically informative proteins from a given sample. In conclusion, we have developed a new device that can be seamlessly integrated into the PCT-SWATH workflow, leading to increased sample throughput and improved reproducibility at both the protein extraction and proteomic analysis levels when applied to the quantitative proteomic analysis of biopsy-level samples.

Chromatographic analysis of Polygalae Radix by online hyphenating pressurized liquid extraction

NASA Astrophysics Data System (ADS)

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

2016-06-01

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

FLUID CONTACTOR APPARATUS

DOEpatents

Spence, R.; Streeton, R.J.W.

1956-04-17

The fluid contactor apparatus comprises a cylindrical column mounted co- axially and adapted to rotate within a cylindrical vessel, for the purpose of extracting a solute from am aqueous solution by means of an organic solvent. The column is particularly designed to control the vortex pattern so as to reduce the height of the vortices while, at the same time, the width of the annular radius in the radial direction between the vessel and column is less than half the radius of the column. A plurality of thin annular fins are spaced apart along the rotor approximately twice the radial dimension of the column such that two contrarotating substantially circular vortices are contained within each pair of fins as the column is rotated.

High-throughput NGL electron-beam direct-write lithography system

NASA Astrophysics Data System (ADS)

Parker, N. William; Brodie, Alan D.; McCoy, John H.

2000-07-01

Electron beam lithography systems have historically had low throughput. The only practical solution to this limitation is an approach using many beams writing simultaneously. For single-column multi-beam systems, including projection optics (SCALPELR and PREVAIL) and blanked aperture arrays, throughput and resolution are limited by space-charge effects. Multibeam micro-column (one beam per column) systems are limited by the need for low voltage operation, electrical connection density and fabrication complexities. In this paper, we discuss a new multi-beam concept employing multiple columns each with multiple beams to generate a very large total number of parallel writing beams. This overcomes the limitations of space-charge interactions and low voltage operation. We also discuss a rationale leading to the optimum number of columns and beams per column. Using this approach we show how production throughputs >= 60 wafers per hour can be achieved at CDs

Fabrication of powdery polymer aerogel as the stationary phase for high-resolution gas chromatographic separation.

PubMed

Zheng, Juan; Lu, Cuiming; Huang, Junlong; Chen, Luyi; Ni, Chuyi; Xie, Xintong; Zhu, Fang; Wu, Dingcai; Ouyang, Gangfeng

2018-08-15

Novel powdery polymer aerogel (PPA) prepared via the (micro)emulsion polymerization and the following hyper crosslinking reaction was fabricated as stationary phase of capillary column for the first time. Due to its powdery morphology, unique 3D nano-network structure, high surface area and good thermostability, the PPA-coated capillary column demonstrated high-resolution chromatographic separation towards nonpolar and weakly polar organic compounds, including benzene series, n-alkanes, ketone mixtures and trichlorobenzenes. Moreover, the reproducibility, quantitative analysis ability and thermostability of PPA-coated capillary column were also evaluated. The relative standard deviations for three replicate determinations of selected analytes were 0.02-0.11%, 0.12-0.26% and 1.2-3.6% for run-to-run, day-to-day and column-to-column analyses, respectively. The PPA demonstrated good thermostability, and the PPA-coated capillary column was proved to be heat-resistant (270 °C). The results of this study show PPA is an excellent candidate to be employed as stationary phase for gas chromatography capillary. Copyright © 2018 Elsevier B.V. All rights reserved.

High sensitivity detection of bisphenol A using liposome chromatography.

PubMed

Liu, Xue-Ying; Nakamura, Chikashi; Tanimoto, Itsuro; Miyake, Shiro; Nakamura, Noriyuki; Hirano, Takashi; Miyake, Jun

2006-09-18

An antibody column in tandem with a fluorescent dye entrapped liposome column was developed for highly sensitive detection of an endocrine disruptor, bisphenol A (BPA). Anti-BPA antibody was immobilized in a protein G column with orientation control. A derivative of BPA was conjugated to phospholipase A2 (PLA2). BPA sample solutions mixed with the BPA-PLA2 conjugates were injected on to the anti-BPA antibody column and competitive binding occurred in the antibody column. The amount of the free conjugate was proportional to the concentration of the BPA sample. The eluted conjugates were injected on to the second column gel on which calcein-entrapped liposomes were immobilized and the PLA2-catalyzed hydrolysis of liposomal phospholipids causing fluorescent dye leakage as a signal amplification. In this system, the mixture of BPA and BPA-PLA2 conjugate were incubated for 60 min in the anti-BPA column, and then the collected solution was applied to the liposome column. The BPA detection range of 0.02-140 ng mL(-1) was wider than 0.03-6.6 ng mL(-1) obtained by the method of competitive ELISA using the same antibody. Moreover, this system could be adapted to an HPLC system resulting in almost the same detection limit in online detection. The method could be applied to environmental samples, river water and soil extracts. The BPA concentration of 0.1 ng mL(-1) and 10 ng g(-1) was detectable in water and soil extract, respectively.

Measurement of Atmospheric CO2 Column Concentrations to Cloud Tops With a Pulsed Multi-Wavelength Airborne Lidar

NASA Technical Reports Server (NTRS)

Mao, Jianping; Ramanathan, Anand; Abshire, James B.; Kawa, Stephan R.; Riris, Haris; Allan, Graham R.; Rodriguez, Michael R.; Hasselbrack, William E.; Sun, Xiaoli; Numata, Kenji;

Regulation of miRNAs by herbal medicine: An emerging field in cancer therapies.

PubMed

Mohammadi, Ali; Mansoori, Behzad; Baradaran, Behzad

2017-02-01

MicroRNAs' expression profiles have recently gained major attention as far as cancer research is concerned. MicroRNAs are able to inhibit target gene expression via binding to the 3' UTR of target mRNA, resulting in target mRNA cleavage or translation inhibition. MicroRNAs play significant parts in a myriad of biological processes; studies have proven, on the other hand, that aberrant microRNA expression is, more often than not, associated with the growth and progression of cancers. MicroRNAs could act as oncogenes (oncomir) or tumor suppressors and can also be utilized as biomarkers for diagnosis, prognosis, and cancer therapy. Recent studies have shown that such herbal extracts as Shikonin, Sinomenium acutum, curcumin, Olea europaea, ginseng, and Coptidis Rhizoma could alter microRNA expression profiles through inhibiting cancer cell development, activating the apoptosis pathway, or increasing the efficacy of conventional cancer therapeutics. Such findings patently suggest that the novel specific targeting of microRNAs by herbal extracts could complete the restriction of tumors by killing the cancerous cells so as to recover survival results in patients diagnosed with malignancies. In this review, we summarized the current research about microRNA biogenesis, microRNAs in cancer, herbal compounds with anti-cancer effects and novel strategies for employing herbal extracts in order to target microRNAs for a better treatment of patients diagnosed with cancer. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

EVALUATION OF THE MIDDAS SYSTEM FOR DESIGNING GAC ADSORBERS

EPA Science Inventory

The Micro-Diameter-Depth Adsorption System (MIDDAS) was evaluated for its usefulness in determining equilibrium parameters for adsorption in granular activated carbon (GAC) systems. The system employs a column configuration for determining such parameters, rather than the traditi...

Validation of a Microscale Extraction and High Throughput UHPLC-QTOF-MS Analysis Method for Huperzine A in Huperzia

PubMed Central

Cuthbertson, Daniel; Piljac-Žegarac, Jasenka; Lange, Bernd Markus

2011-01-01

Herein we report on an improved method for the microscale extraction of huperzine A (HupA), an acetylcholinesterase-inhibiting alkaloid, from as little as 3 mg of tissue homogenate from the clubmoss Huperzia squarrosa (G. Forst.) Trevis with 99.95 % recovery. We also validated a novel UHPLC-QTOF-MS method for the high-throughput analysis of H. squarrosa extracts in only 6 min, which, in combination with the very low limit of detection (20 pg on column) and the wide linear range for quantification (20 to 10,000 pg on column), allow for a highly efficient screening of extracts containing varying amounts of HupA. Utilization of this methodology has the potential to conserve valuable plant resources. PMID:22275140

Capillary trap column with strong cation-exchange monolith for automated shotgun proteome analysis.

PubMed

Wang, Fangjun; Dong, Jing; Jiang, Xiaogang; Ye, Mingliang; Zou, Hanfa

2007-09-01

A 150 microm internal diameter capillary monolithic column with a strong cation-exchange stationary phase was prepared by direct in situ polymerization of ethylene glycol methacrylate phosphate and bisacrylamide in a trinary porogenic solvent consisting dimethylsulfoxide, dodecanol, and N,N'-dimethylformamide. This phosphate monolithic column exhibits higher dynamic binding capacity, faster kinetic adsorption of peptides, and more than 10 times higher permeability than the column packed with commercially available strong cation-exchange particles. It was applied as a trap column in a nanoflow liquid chromatography-tandem mass spectrometry system for automated sample injection and online multidimensional separation. It was observed that the sample could be loaded at a flow rate as high as 40 microL/min with a back pressure of approximately 1300 psi and without compromising the separation efficiency. Because of its good orthogonality to the reversed phase separation mechanism, the phosphate monolithic trap column was coupled with a reversed-phase column for online multidimensional separation of 19 microg of the tryptic digest of yeast proteins. A total of 1522 distinct proteins were identified from 5608 unique peptides (total of 54,780 peptides) at the false positive rate only 0.46%.

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

PubMed

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

2010-06-25

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

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

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

Kiang, P.H.T.

1985-01-01

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

Micro-field evoked potentials recorded from the porcine sub-dural cortical surface utilizing a microelectrode array.

PubMed

Kitzmiller, Joseph P; Hansford, Derek J; Fortin, Linda D; Obrietan, Karl H; Bergdall, Valerie K; Beversdorf, David Q

2007-05-15

A sub-dural surface microelectrode array designed to detect micro-field evoked potentials has been developed. The device is comprised of an array of 350-microm square gold contacts, with bidirectional spacing of 150 microm, contained within a polyimide Kapton material. Cytotoxicity testing suggests that the device is suitable for use with animal and human patients. Implementation of the device in animal studies revealed that reliable evoked potentials could be acquired. Further work will be needed to determine how these micro-field potentials, which demonstrate selectivity for one eye, relate to the distribution of the ocular dominance columns of the occipital cortex.

Carbon molecular sieve based micro-matrix-solid-phase dispersion for the extraction of polyphenols in pomegranate peel by UHPLC-Q-TOF/MS.

PubMed

Du, Li-Jing; Huang, Jian-Ping; Wang, Bin; Wang, Chen-Hui; Wang, Qiu-Yan; Hu, Yu-Han; Yi, Ling; Cao, Jun; Peng, Li-Qing; Chen, Yu-Bo; Zhang, Qi-Dong

2018-06-04

A rapid, simple and efficient sample extraction method based on micro-matrix-solid-phase dispersion (micro-MSPD) was applied to the extraction of polyphenols from pomegranate peel. Five target analytes were determined by ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry. Carbon molecular sieve (CMS) was firstly used as dispersant to improve extraction efficiency in micro-MSPD. The major micro-MSPD parameters, such as type of dispersant, amount of dispersant, grinding time and the type and the volume of elution solvents, were studied and optimized. Under optimized conditions, 26 mg of pomegranate peel was dispersed with 32.5 mg of CMS, the grinding time was selected as 90 s, the dispersed sample was eluted with 100 μL of methanol. Results showed that the proposed method was of good linearity for concentrations of analytes against their peak areas (coefficient of determination r 2 >0.990), the limit of the detection was as low as 3.2 ng/mL, and the spiking recoveries were between 88.1% and 106%. Satisfactory results were obtained for the extraction of gallic acid, punicalagin A, punicalagin B, catechin and ellagic acid from pomegranate peel sample, which demonstrated nice reliability and high sensitivity of this approach. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

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

PubMed

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

2017-11-01

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

Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean.

PubMed

Zhai, Haiyun; Su, Zihao; Chen, Zuanguang; Liu, Zhenping; Yuan, Kaisong; Huang, Lu

2015-03-20

A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC-LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001-2.0 μg mL(-1) (r=0.9995) with the detection limit (S/N=3) of 0.075 ng mL(-1). Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC-LIF method can be applied to sensitively determine phloxine B in coffee bean. Copyright © 2015 Elsevier B.V. All rights reserved.

In-line phase contrast micro-CT reconstruction for biomedical specimens.

PubMed

Fu, Jian; Tan, Renbo

2014-01-01

X-ray phase contrast micro computed tomography (micro-CT) can non-destructively provide the internal structure information of soft tissues and low atomic number materials. It has become an invaluable analysis tool for biomedical specimens. Here an in-line phase contrast micro-CT reconstruction technique is reported, which consists of a projection extraction method and the conventional filter back-projection (FBP) reconstruction algorithm. The projection extraction is implemented by applying the Fourier transform to the forward projections of in-line phase contrast micro-CT. This work comprises a numerical study of the method and its experimental verification using a biomedical specimen dataset measured at an X-ray tube source micro-CT setup. The numerical and experimental results demonstrate that the presented technique can improve the imaging contrast of biomedical specimens. It will be of interest for a wide range of in-line phase contrast micro-CT applications in medicine and biology.

Testing the event witnessing status of micro-bloggers from evidence in their micro-blogs

PubMed Central

2017-01-01

This paper demonstrates a framework of processes for identifying potential witnesses of events from evidence they post to social media. The research defines original evidence models for micro-blog content sources, the relative uncertainty of different evidence types, and models for testing evidence by combination. Methods to filter and extract evidence using automated and semi-automated means are demonstrated using a Twitter case study event. Further, an implementation to test extracted evidence using Dempster Shafer Theory of Evidence are presented. The results indicate that the inclusion of evidence from micro-blog text and linked image content can increase the number of micro-bloggers identified at events, in comparison to the number of micro-bloggers identified from geotags alone. Additionally, the number of micro-bloggers that can be tested for evidence corroboration or conflict, is increased by incorporating evidence identified in their posting history. PMID:29232395

Studies on the use of sepharose-N-(6-aminohexanoyl)-2-amino-2-deoxy-D-glucopyranose for the large-scale purification of hepatic glucokinase.

PubMed Central

Holroyde, M J; Chesher, J M; Trayer, I P; Walker, D G

1976-01-01

The synthesis of N-(6-aminohexanoyl)-2-amino-2-deoxy-D-glucose is described and it was shown to be a competitive inhibitor (Ki, 0.75 mM) with respect to glucose of rat hepatic glucokinase (EC 2.7.1.2). After attachment to CNBr-activated Sepharose 4B, this derivative was able to remove glucokinase quantitatively from crude liver extracts and release it when the columns were developed with glucose, glucosamine, N-acetyl-glucosamine or KC1. Repeated exposure of the columns to liver extracts led to rapid loss in their effectiveness as affinity matrices because proteins other than glucokinase are bound to the columns. The nature of such protein binding and methods for the rejuvenation of "used" columns are discussed along with the effect of the mode of preparation of the Sepharose-ligand conjugate and the concentration of bound ligand on the purification of glucokinase. Glucose 6-phosphate dehydrogenase is cited as an example of both non-specific protein binding to the affinity column and of the importance of the control of ligand concentration in removing such non-specifically bound proteins. Some guidelines emerged that should be generally applicable to other systems, particularly those which involve affinity chromatography of enzymes that are present in tissue extracts in very low amounts and possess only a relatively low association constant for the immobilized ligand. PMID:1275893

Tall fescue seed extraction and partial purification of ergot alkaloids

PubMed Central

Ji, Huihua; Fannin, F.; Klotz, J.; Bush, Lowell

2014-01-01

Many substances in the tall fescue/endophyte association (Schedonorus arundinaceus/Epichloë coenophiala) have biological activity. Of these compounds only the ergot alkaloids are known to have significant mammalian toxicity and the predominant ergot alkaloids are ergovaline and ergovalinine. Because synthetically produced ergovaline is difficult to obtain, we developed a seed extraction and partial purification protocol for ergovaline/ergovalinine that provided a biologically active product. Tall fescue seed was ground and packed into several different sized columns for liquid extraction. Smaller particle size and increased extraction time increased efficiency of extraction. Our largest column was a 114 × 52 × 61 cm (W × L × D) stainless steel tub. Approximately 150 kg of seed could be extracted in this tub. The extraction was done with 80% ethanol. When the solvent front migrated to bottom of the column, flow was stopped and seed was allowed to steep for at least 48 h. Light was excluded from the solvent from the beginning of this step to the end of the purification process. Following elution, ethanol was removed from the eluate by evaporation at room temperature and the resulting syrup was freeze-dried. About 80% recovery of alkaloids was achieved with 18-fold increase in concentration of ergovaline. Initial purification of the dried product was accomplished by extracting with hexane/water (6:1, v/v). The aqueous fraction was extracted with chloroform, the aqueous layer discarded, after which the chloroform was removed with a resulting 20-fold increase of ergovaline. About 65% of the ergovaline was recovered from the chloroform residue for an overall recovery of 50%. The resultant partially purified ergovaline had biological activities in in vivo and in vitro bovine bioassays that approximate that of synthetic ergovaline. PMID:25566528

Tall fescue seed extraction and partial purification of ergot alkaloids

NASA Astrophysics Data System (ADS)

Bush, Lowell

2014-12-01

Many substances in the tall fescue/endophyte association (Schedonorus arundinaceus/Epichloë coenophiala) have biological activity. Of these compounds only the ergot alkaloids are known to have significant mammalian toxicity and the predominant ergot alkaloids are ergovaline and ergovalinine. Because synthetically produced ergovaline is difficult to obtain, we developed a seed extraction and partial purification protocol for ergovaline/ergovalinine that provided a biologically active product. Tall fescue seed was ground and packed into several different sized columns for liquid extraction. Smaller particle size and increased extraction time increased efficiency of extraction. Our largest column was a 114 × 52 × 61 cm (W×L×D) stainless steel tub. Approximately 150 kg of seed could be extracted in this tub. The extraction was done with 80% ethanol. When the solvent front migrated to bottom of the column, flow was stopped and seed was allowed to steep for at least 48 h. Light was excluded from the solvent from the beginning of this step to the end of the purification process. Following elution, ethanol was removed from the eluate by evaporation at room temperature. Resulting syrup was freeze-dried. About 80% recovery of alkaloids was achieved with 18-fold increase in concentration of ergovaline. Initial purification of the dried product was accomplished by extracting with hexane/water (6:1, v/v) and the hexane fraction was discarded. The aqueous fraction was extracted with chloroform, the aqueous layer discarded, after which the chloroform was removed with a resulting 20-fold increase of ergovaline. About 65% of the ergovaline was recovered from the chloroform residue for an overall recovery of 50%. The resultant partially purified ergovaline had biological activities in in vivo and in vitro bovine bioassays that approximate that of synthetic ergovaline.

A core-shell column approach to a comprehensive high-performance liquid chromatography phenolic analysis of Vitis vinifera L. and interspecific hybrid grape juices, wines, and other matrices following either solid phase extraction or direct injection.

PubMed

Manns, David C; Mansfield, Anna Katharine

2012-08-17

Four high-throughput reverse-phase chromatographic protocols utilizing two different core-shell column chemistries have been developed to analyze the phenolic profiles of complex matrices, specifically targeting juices and wines produced from interspecific hybrid grape cultivars. Following pre-fractionation via solid-phase extraction or direct injection, individual protocols were designed to resolve, identify and quantify specific chemical classes of compounds including non-anthocyanin monomeric phenolics, condensed tannins following acid hydrolysis, and anthocyanins. Detection levels ranging from 1.2 ppb to 27.5 ppb, analyte %RSDs ranging from 0.04 to 0.38, and linear ranges of quantitation approaching five orders of magnitude were achieved using conventional HPLC instrumentation. Using C(18) column chemistry, the non-anthocyanin monomeric protocol effectively separated a set of 16 relevant phenolic compounds comprised flavan-3-ols, hydroxycinnamic acids, and flavonols in under 14 min. The same column was used to develop a 15-min protocol for hydrolyzed condensed tannin analysis. Two anthocyanin protocols are presented, one utilizing the same C(18) column, best suited for anthocyanidin and monoglucoside analysis, the other utilizing a pentafluorophenyl chemistry optimized to effectively separate complex mixtures of coexisting mono- and diglucoside anthocyanins. These protocols and column chemistries have been used initially to explore a wide variety of complex phenolic matrices, including red and white juices and wines produced from Vitis vinifera and interspecific hybrid grape cultivars, juices, teas, and plant extracts. Each protocol displayed robust matrix responses as written, yet are flexible enough to be easily modified to suit specifically tailored analytical requirements. Copyright © 2012 Elsevier B.V. All rights reserved.

TEFLON BELLOWS PULSE GENERATORS FOR SOLVENT EXTRACTION PULSE COLUMNS

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

McCarthy, P.B.

1954-01-01

A Teflon bellows-type pulse generator is described which consists of two 3-in. nominal diameter Teflon bellows mounted on either end of a flanged spool piece and rigidly connected internally by a push rod so that the two of bellows move in tandem. The ends of the two bellows are closed by means of blind flanges. Tne spool piece is designed for insertion in a 6-in. diameter nozzle on a solvent extraction pulse column. The double bellows arrangement constitutes a safety feature to prevent loss of the column contents in the event of failure of the inner bellows in contact withmore » column solution. Failure of the inner bellows may be detected by a conductivity probe mounted in the air space inside of the double bellows assembly. Reciprocating motion is imcrank arm rigidly connected through a cross head and push rod to the face of the external bellows flange. The push rod is guided by means of linear ball bushings. Frequency variation over a range of 30 to 100 cycles/ min.was obtained by use of a Thymotrol-controlled electric motor to drive the crank arm. Variable stroke adjustment (0 to 1-in. range) was possible by adjustment of linkages on the crank arm. A load compensating spring was founnd desirable to counteract the thrust on the push rod resulting tom the static pressure at the bottom of the solvent extraction column. Without the spring, accelerated wear of the bearing on the crank arm occured. The pulse generator operated uneventfully for 1776 hours (6.61x lO/sup 6/ cycles) at a frequency of 62 cycles/min. and a bellows travel of l-in. (equivalent to a displacement of 1.6 in. in a 3-in. diam. column). (auth)« less

Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

1992-01-01

A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

Chromatographic Separation, and Characteristics of Nucleic Acids from HeLa Cells

PubMed Central

Philipson, Lennart

1961-01-01

The application of the phenol-duponol method to extraction of nucleic acids from HeLa cells is described. Chromatography of the phenol extract on an esterified bovine serum albumin column with a salt gradient of sodium chloride gives separation of soluble RNA, DNA, and two different high molecular RNA fractions. Ultracentrifugation of the DNA eluted from the column gives a sedimentation coefficient (s 20 o,w) of 38, which agrees with ultracentrifugation data on the phenol extract. The eluted RNA appears polydisperse at low ionic strength, but at high ionic strength and after alcohol precipitation two fractions with the sedimentation coefficients of 16 and 25 to 29, respectively, were obtained. PMID:13735276

Cold column trapping-cloud point extraction coupled to high performance liquid chromatography for preconcentration and determination of curcumin in human urine.

PubMed

Rahimi, Marzieh; Hashemi, Payman; Nazari, Fariba

2014-05-15

A cold column trapping-cloud point extraction (CCT-CPE) method coupled to high performance liquid chromatography (HPLC) was developed for preconcentration and determination of curcumin in human urine. A nonionic surfactant, Triton X-100, was used as the extraction medium. In the proposed method, a low surfactant concentration of 0.4% v/v and a short heating time of only 2min at 70°C were sufficient for quantitative extraction of the analyte. For the separation of the extraction phase, the resulted cloudy solution was passed through a packed trapping column that was cooled to 0 °C. The temperature of the CCT column was then increased to 25°C and the surfactant rich phase was desorbed with 400μL ethanol to be directly injected into HPLC for the analysis. The effects of different variables such as pH, surfactant concentration, cloud point temperature and time were investigated and optimum conditions were established by a central composite design (response surface) method. A limit of detection of 0.066mgL(-1) curcumin and a linear range of 0.22-100mgL(-1) with a determination coefficient of 0.9998 were obtained for the method. The average recovery and relative standard deviation for six replicated analysis were 101.0% and 2.77%, respectively. The CCT-CPE technique was faster than a conventional CPE method requiring a lower concentration of the surfactant and lower temperatures with no need for the centrifugation. The proposed method was successfully applied to the analysis of curcumin in human urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Liquid chromatography-tandem mass spectrometry method of loxoprofen in human plasma.

PubMed

Lee, Hye Won; Ji, Hye Young; Sohn, Dong Hwan; Kim, Se-Mi; Lee, Yong Bok; Lee, Hye Suk

2009-07-01

A rapid, sensitive and selective liquid chromatography-electrospray ionization mass spectrometric method for the determination of loxoprofen in human plasma was developed. Loxoprofen and ketoprofen (internal standard) were extracted from 20 microL of human plasma sample using ethyl acetate at acidic pH and analyzed on an Atlantis dC(18) column with the mobile phase of methanol:water (75:25, v/v). The analytes were quantified in the selected reaction monitoring mode. The standard curve was linear over the concentration range of 0.1-20 microg/mL with a lower limit of quantification of 0.1 microg/mL. The coefficient of variation and relative error for intra- and inter-assay at four quality control levels were 2.8-5.2 and 4.8-7.0%, respectively. The recoveries of loxoprofen and ketoprofen were 69.7 and 67.6%, respectively. The matrix effects for loxoprofen and ketoprofen were practically absent. This method was successfully applied to the pharmacokinetic study of loxoprofen in humans. (c) 2009 John Wiley & Sons, Ltd.

[Simultaneous determination of 6 neonicotinoid residues in soil using DLLME-HPLC and UV].

PubMed

Sun, Bao-li; Shan, Hong; Li, Yan-hua; Zeng, Ya-ling; Shen, Xiu-li; Tong, Cheng-feng

2013-09-01

A simple, cheap and rugged method was developed for simultaneous deter mination of 6 neonicotinoid residues in soil, including imidacloprid, acetamiprid, thiamethoxam, thiacloprid, clothianidin and nitenpyram. The soil sample was produced by dispersive liquid-liquid micro-extraction (DLLME) after extracted by the mixed solution of acetonitrile and CH2Cl2 (2:1, phi). The analytes were separated by HPLC with Alltima C18 column (4.6 mm x 250 mm, 5 microm) and detected by PDA at 260 nm. External standard method was used for quantification. The results showed that good linearity was obtained with correlation coefficients between 0.9982 and 0.9999 in the range of 0.5-200 microg x L(-1). The limits of detection (LODs) were in the range between 0.0005 and 0.003 microg x mL(-1) (S/N = 3). The method was validated with five soil samples spiked at three fortification levels (0.05, 0.1, 1.0 mg x kg(-1)) and recoveries were in the range of 55.3%-95.6% with RSD of 1.4%-7.0%. The effect of clean-up was evaluated by UV spectra and demonstrated that the method established is effective. In conclusion, this method is competent for the simultaneous analysis of 6 neonicotinoid residues in soil.

A method for the direct injection and analysis of small volume human blood spots and plasma extracts containing high concentrations of organic solvents using revered-phase 2D UPLC/MS.

PubMed

Rainville, Paul D; Simeone, Jennifer L; Root, Dan S; Mallet, Claude R; Wilson, Ian D; Plumb, Robert S

2015-03-21

The emergence of micro sampling techniques holds great potential to improve pharmacokinetic data quality, reduce animal usage, and save costs in safety assessment studies. The analysis of these samples presents new challenges for bioanalytical scientists, both in terms of sample processing and analytical sensitivity. The use of two dimensional LC/MS with, at-column-dilution for the direct analysis of highly organic extracts prepared from biological fluids such as dried blood spots and plasma is demonstrated. This technique negated the need to dry down and reconstitute, or dilute samples with water/aqueous buffer solutions, prior to injection onto a reversed-phase LC system. A mixture of model drugs, including bromhexine, triprolidine, enrofloxacin, and procaine were used to test the feasibility of the method. Finally an LC/MS assay for the probe pharmaceutical rosuvastatin was developed from dried blood spots and protein-precipitated plasma. The assays showed acceptable recovery, accuracy and precision according to US FDA guidelines. The resulting analytical method showed an increase in assay sensitivity of up to forty fold as compared to conventional methods by maximizing the amount loaded onto the system and the MS response for the probe pharmaceutical rosuvastatin from small volume samples.

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Short communication: Development of a novel method for the extraction of norbixin from whey and its subsequent quantification via high performance liquid chromatography.

PubMed

Campbell, R E; Boogers, I A L A; Drake, M A

2014-03-01

Norbixin is the primary carotenoid in annatto coloring, which imparts the desired orange color in Cheddar cheese. However, a portion of the colorant remains in the cheese whey and is undesirable; therefore, a bleaching step is often applied. Restrictions exist for norbixin concentrations in products destined for infant formula. As such, evaluation of norbixin concentrations in whey and whey ingredients is desirable. Current extraction methods are laborious and require solvents that are banned in many countries. The objective of this study was to develop a fast and inexpensive norbixin extraction and quantitation technique using approved solvents with similar sensitivity to current established methods. Instead of solvent extraction and column purification, acetonitrile was added directly to fluid wheys, retentates, and rehydrated whey protein concentrates. An isocratic mobile phase [70% acetonitrile and 30% water with 0.1% (wt/vol) formic acid] was used and, to increase sensitivity, a large volume (50 μL) was injected onto the column. The column used was a C18 column with a particle size of 2.6 μm and column length of 10 cm. The column inner diameter was 4.6mm and the pore size was 100 Ǻ. All of the previously described conditions allowed the run time to be only 4 min. The sample was sent through a photodiode array detector and quantified at 482 nm. Norbixin was quantified using external standard curves. The developed method had a >90% norbixin recovery in both milk and whey (9.39 μg/L-2.35 mg/L). The limit of detection of norbixin in fluid whey was 2.7 μg/kg and the limit of quantitation was 3.5 μg/kg, both of which are significantly lower than in previously described methods. The extracts were stable over 30 min at 21°C and stable over 24h at 4°C. Repeatability and precision of the method had relative standard deviations of less than 13%. The developed method provides time and cost savings for evaluation of norbixin concentration in whey and whey products. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Preparation of highly pure zeaxanthin particles from sea water-cultivated microalgae using supercritical anti-solvent recrystallization.

PubMed

Chen, Chao-Rui; Hong, Siang-En; Wang, Yuan-Chuen; Hsu, Shih-Lan; Hsiang, Daina; Chang, Chieh-Ming J

2012-01-01

Xanthophylls, including zeaxanthin, are considered dietary supplements with a potentially positive impact on age-related macular degeneration. Using pilot-scale column fractionation coupled with supercritical anti-solvent (SAS) recrystallization, highly pure zeaxanthin particulates were prepared from ultrasonic extracts of the microalgae, Nannochloropsis oculata, grown in sea water. Column partition chromatography increased the concentration of zeaxanthin from 36.2 mg/g of the ultrasonic extracts to 425.6 mg/g of the collected column fractions. A response surface methodology was systematically designed for the SAS process by changing feed concentration, CO(2) flow rate and anti-solvent pressure. Zeaxanthin-rich particles with a purity of 84.2% and a recovery of 85.3% were produced using supercritical anti-solvent recrystallization from the column eluate at a feed concentration of 1.5 mg/mL, CO(2) flow rate of 48.6 g/min and pressure of 135 bar. Copyright © 2011 Elsevier Ltd. All rights reserved.

Integrated micro thermoelectric cooler: Theory, fabrication and characterization

NASA Astrophysics Data System (ADS)

da Silva, Luciana Wasnievski

The flows of heat and electricity in a column-type micro thermoelectric (TE) cooler that uses telluride compounds for the n- and p-type elements, are analyzed by modeling the various interfacial resistances. Electron (barrier tunneling) and phonon (diffuse mismatch) boundary resistances at the TE/metal interface, and thermal non-equilibrium between electrons and phonons adjacent to this interface (cooling length), increase the thermal conduction resistance and decrease the Seebeck coefficient of the TE elements. These in turn reduce the device cooling performance, which is also affected by the thermal and electrical contact resistances at the TE/metal and the metal/electrical-insulator interfaces. From the device optimization, it is predicted (for an available voltage of 3 V) that a micro TE cooler with 50 TE pairs (Bi2Te3 and Sb2Te3 high performance TE films), column thickness of 4 mum (limited by the current fabrication process), and column cross-section area of 7 mum x 7 mum, should produce a temperature drop of 10 K with a cooling load of 10 mW. This device will operate with a current of 11 mA and will require a power of 34 mW. The coefficient of performance is 0.3. Co-evaporated Bi-Te and Sb-Te films were fabricated at various deposition conditions (evaporation rate of individual species and substrate temperature), and their TE properties (Seebeck coefficient, electrical resistivity, and carrier concentration) were measured, in search of optimal TE performance. The deposition rates were controlled such that the tellurium atomic composition changed from 48 to 74%, and the substrate temperature ranged from 130 to 300°C. The chemical composition and crystal structure of the films were recorded (using a microprobe and a X-ray diffractomer, respectively), analyzed, and compared with standard Bi2Te3 and Sb2Te 3 single crystal samples. High performance TE films had a tellurium atomic concentration around 60% and were deposited at a substrate temperature between 260 and 270°C. Due to degradation of the photoresist used for patterning the TE films, in the first-generation device, they were deposited with a maximum substrate temperature of 130°C. The TE columns were connected using Cr/Au/Ti/Pt layers at the hot junctions, and Cr/Au layers at the cold junctions. A device with 60 TE pairs and column width of 40 mum (finer device structures had limited yield) was tested using infrared thermometry. The average cooling achieved was about 1 K, which was close to the predicted value. A future-generation device is proposed, where high performance TE films can be patterned with optimized geometries (high density micro TE coolers), allowing these devices to fulfill the requirements for a wireless environmental monitor application.

Morphologies and optical and electrical properties of InGaN/GaN micro-square array light-emitting diode chips.

PubMed

Han, Dan; Ma, Shufang; Jia, Zhigang; Liu, Peizhi; Jia, Wei; Shang, Lin; Zhai, Guangmei; Xu, Bingshe

2018-04-10

InGaN/GaN micro-square array light-emitting diode (LED) chips (micro-chips) have been prepared via the focused ion beam (FIB) etching technique, which can not only reduce ohmic contact degradation but also control the aspect ratio precisely in three-dimensional (3D) structure LED (3D-LED) device fabrication. The effects of FIB beam current and micro-square array depth on morphologies and optical and electrical properties of the micro-chips have been studied. Our results show that sidewall surface morphology and optical and electrical properties of the micro-chips degrade with increased beam current. After potassium hydroxide etching with different times, an optimal current-voltage and luminescence performance can be obtained. Combining the results of cathodoluminescence mappings and light output-current characteristics, the light extraction efficiency of the micro-chips is reduced as FIB etch depth increases. The mechanisms of micro-square depth on light extraction have been revealed by 3D finite difference time domain.

Simultaneous determination of chlorinated organic compounds from environmental samples using gas chromatography coupled with a micro electron capture detector and micro-plasma atomic emission detector

NASA Astrophysics Data System (ADS)

Quan, Xie; Chen, Shuo; Platzer, Bernhard; Chen, Jingwen; Gfrerer, Marion

2002-01-01

Water and sediment samples were screened simultaneously for the presence of polychlorinated organic compounds using gas chromatography (GC) coupled with an micro electron capture detector (μ-ECD) and a newly developed helium plasma based on a micro-atomic emission detector (μ-AED). The GC column effluent was split 15:85 between two detectors. In this way, two chromatograms, one obtained by μ-ECD and another by μ-AED, were recorded simultaneously. α-, β-hexachlorocyclohexane and p, p'-DDE were detected. RSDs of the monitoring results from the two detection methods were <20% for the three compounds. A detection limit of 8.5 pg and at least 3 orders of magnitude of linear range for μ-AED was observed.

Oxygen octahedra picker: A software tool to extract quantitative information from STEM images.

PubMed

Wang, Yi; Salzberger, Ute; Sigle, Wilfried; Eren Suyolcu, Y; van Aken, Peter A

2016-09-01

In perovskite oxide based materials and hetero-structures there are often strong correlations between oxygen octahedral distortions and functionality. Thus, atomistic understanding of the octahedral distortion, which requires accurate measurements of atomic column positions, will greatly help to engineer their properties. Here, we report the development of a software tool to extract quantitative information of the lattice and of BO6 octahedral distortions from STEM images. Center-of-mass and 2D Gaussian fitting methods are implemented to locate positions of individual atom columns. The precision of atomic column distance measurements is evaluated on both simulated and experimental images. The application of the software tool is demonstrated using practical examples. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

COMPARISON OF MINIMUM INHIBITORY CONCENTRATION OF WATER SOLUBLE EXTRACTS OF EUGENIA JAMBOLANA LAM. (FAM. MYRTACEAE) BARKS OF DIFFERENT AGES ON DYSENTERY AND DIARRHOEA FORMING MICRO – ORGANISMS

PubMed Central

Maiti, Asis Prosun; Pal, Subodh Chandra; Chattopadhyay, Debaprasad; De, Samar; Nandy, Anutosh

1985-01-01

A preliminary investigations was carried out to study the antibacterial activity of the water soluble extracts of five and ten years old barks of Eugenia Jambolana Lam. (fam. Myrtaceae) on dysentery and diarrhoea forming micro organisms. It was observed that the barks of young plants have a better inhibitory effect on micro – organisms like Salmonella viballerup, Shigella dysenteriae 10, Shigella boydii 5, Sgigella dysenteriae 2. PMID:22557509

The method of micro-motion cycle feature extraction based on confidence coefficient evaluation criteria

NASA Astrophysics Data System (ADS)

Tang, Chuanzi; Ren, Hongmei; Bo, Li; Jing, Huang

2017-11-01

In radar target recognition, the micro motion characteristics of target is one of the characteristics that researchers pay attention to at home and abroad, in which the characteristics of target precession cycle is one of the important characteristics of target movement characteristics. Periodic feature extraction methods have been studied for years, the complex shape of the target and the scattering center stack lead to random fluctuations of the RCS. These random fluctuations also exist certain periodicity, which has a great influence on the target recognition result. In order to solve the problem, this paper proposes a extraction method of micro-motion cycle feature based on confidence coefficient evaluation criteria.

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

Back, H. O.; Bottenus, D. R.; Clayton, C.

The next generation of 136Xe neutrinoless double beta decay experiments will require on the order of 5 tons of enriched 136Xe. By estimating the relative volatilities of the xenon isotopes and using standard chemical engineering techniques we explore the feasibility of using cryogenic distillation to produce 5 tons of 80% enriched 136Xe in 5-6 years. With current state-of-the-art distillation column packing materials we can estimate the total height of a traditional cryogenic distillation column. We also, report on how Micro Channel Distillation may reduce the overall size of a distillation system for 136Xe production.

Homestead Valley, California, aftershocks (March 17-18, 1979) recorded on portable seismographs

USGS Publications Warehouse

Perry-Huston, Sue; Eberhart-Phillips, Donna

1994-01-01

A method for the determination of chlorinated organic compounds in aquatic tissue by dual capillary-column gas chromatography with electron- capture detection is described. Whole-body-fish or corbicula tissue is homogenized, Soxhlet extracted, lipid removed by gel permeation chromatography, and fractionated using alumina/silica adsorption chromatography. The extracts are analyzed by dissimilar capillary-column gas chromatography with electron-capture detection. The method reporting limits are 5 micrograms per kilogram (ug/kg) for chlorinated compounds, 50 ug/kg for polychlorinated biphenyls, and 200 ug/kg for toxaphene.

Rapid, direct extraction of DNA from soils for PCR analysis using polyvinylpolypyrrolidone spin columns.

PubMed

Berthelet, M; Whyte, L G; Greer, C W

1996-04-15

Polyvinylpolypyrrolidone spin columns were used to rapidly purify crude soil DNA extracts from humic materials for polymerase chain reaction (PCR) analysis. The PCR detection limit for the tfdC gene, encoding chlorocatechol dioxygenase from the 2,4-dichlorophenoxyacetic acid degradation pathway, was 10(1)-10(2) cells/g soil in inoculated soils. The procedure could be applied to the amplification of biodegradative genes from indigenous microbial populations from a wide variety of soil types, and the entire analysis could be performed within 8 h.

Water column particulate matter: A key contributor to phosphorus regeneration in a coastal eutrophic environment, the Chesapeake Bay: Particulate phosphorus in the Chesapeake Bay

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

Li, Jiying; Reardon, Patrick; McKinley, James P.

Particulate phosphorus (PP) in the water column is an essential component of phosphorus (P) cycling in aquatic ecosystems yet its composition and transformations remain largely uncharacterized. To understand the roles of suspended particulates on regeneration of inorganic P (Pi) into the water column as well as sequestration into more stable mineral precipitates, we studied seasonal variation in both organic and inorganic P speciation in suspended particles in three sites in the Chesapeake Bay using sequential P extraction, 1D (31P) and 2D (1H-31P) nuclear magnetic resonance (NMR) spectroscopies, and electron microprobe analyses (EMPA). Remineralization efficiency of particulate P average 8% andmore » 56% in shallow and deep sites respectively, suggesting the importance of PP remineralization is in resupplying water column Pi. Strong temporal and spatial variability of organic P composition, distributions, and remineralization efficiency were observed relating to water column parameters such as temperature and redox conditions: concentration of orthophosphate monoesters and diesters, and diester-to-monoester (D/M) ratios decreased with depth. Both esters and the D/M ratios were lower in the hypoxic July and September. In contrast, pyrophosphate and orthophosphate increased with depth, and polyphosphates was high in the anoxic water column. Sequential extraction and EMPA analyses of the suspended particles suggest presence of Ca-bound phosphate in the water column. We hypothesize authigenic precipitation of carbonate fluorapatite and/or its precursor mineral(s) in Pi rich water column, supported by our thermodynamic calculations. Our results, overall, reveal the important role suspended particles play in P remineralization and P sequestration in the Chesapeake Bay water column, provide important implications on P bioavailability and P sinks in similar eutrophic coastal environments.« less

Mobilization and Transport of Organic Compounds from Reservoir Rock and Caprock in Geological Carbon Sequestration Sites

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

Zhong, Lirong; Cantrell, Kirk J.; Mitroshkov, Alexandre V.

2014-05-06

Supercritical CO2 (scCO2) is an excellent solvent for organic compounds, including benzene, toluene, ethyl-benzene, and xylene (BTEX), phenols, and polycyclic aromatic hydrocarbons (PAHs). Monitoring results from geological carbon sequestration (GCS) field tests has shown that organic compounds are mobilized following CO2 injection. Such results have raised concerns regarding the potential for groundwater contamination by toxic organic compounds mobilized during GCS. Knowledge of the mobilization mechanism of organic compounds and their transport and fate in the subsurface is essential for assessing risks associated with GCS. Extraction tests using scCO2 and methylene chloride (CH2Cl2) were conducted to study the mobilization of volatilemore » organic compounds (VOCs, including BTEX), the PAH naphthalene, and n-alkanes (n-C20 – n-C30) by scCO2 from representative reservoir rock and caprock obtained from depleted oil reservoirs and coal from an enhanced coal-bed methane recovery site. More VOCs and naphthalene were extractable by scCO2 compared to the CH2Cl2 extractions, while scCO2 extractable alkane concentrations were much lower than concentrations extractable by CH2Cl2. In addition, dry scCO2 was found to extract more VOCs than water saturated scCO2, but water saturated scCO2 mobilized more naphthalene than dry scCO2. In sand column experiments, moisture content was found to have an important influence on the transport of the organic compounds. In dry sand columns the majority of the compounds were retained in the column except benzene and toluene. In wet sand columns the mobility of the BTEX was much higher than that of naphthalene. Based upon results determined for the reservoir rock, caprock, and coal samples studied here, the risk to aquifers from contamination by organic compounds appears to be relatively low; however, further work is necessary to fully evaluate risks from depleted oil reservoirs.« less

Extraction, Purification, and Spectroscopic Characterization of a Mixture of Capsaicinoids

ERIC Educational Resources Information Center

Wagner, Carl E.; Cahill, Thomas M.; Marshall, Pamela A.

2011-01-01

This laboratory experiment provides a safe and effective way to instruct undergraduate organic chemistry students about natural-product extraction, purification, and NMR spectroscopic characterization. On the first day, students extract dried habanero peppers with toluene, perform a pipet silica gel column to separate carotenoids from…

Rapid mixed mode solid phase extraction method for the determination of acrylamide in roasted coffee by HPLC-MS/MS.

PubMed

Bortolomeazzi, Renzo; Munari, Marina; Anese, Monica; Verardo, Giancarlo

2012-12-15

In this work, a rapid and reliable purification method based on a single mixed solid phase extraction (SPE) column, for the determination of acrylamide in roasted coffee by liquid chromatography-tandem mass spectrometry, was developed. Deuterium labelled d(3)-acrylamide was used as internal standard. Acrylamide was extracted by 10 mL of water and the extract purified by a single SPE column consisting of 0.5 g of an in-house prepared mixture of C18, strong cation (SCX) and anion exchange (SAX) sorbents in the ratio 2/1.5/1.5 (w/w/w). The amount of the three sorbents was optimised in order to eliminate the main interfering compounds present in coffee extracts, such as melanoidins, trigonelline, chlorogenic acids and caffeine. The SPE procedure was very simple and consisted of pushing 1 mL of an aqueous coffee extract through the SPE column followed by 1 mL of water which was collected for the analysis. The method was tested on six samples of roasted coffee of different composition and roasting level. The repeatability of the method, expressed as relative standard deviation (n=6), was lower than 5%. The recovery of acrylamide at three spiked levels ranged from 92% to 95%. The limits of detection (LOD) and quantitation (LOQ) were 5 and 16 μg kg(-1), respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

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

PubMed

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

2014-10-03

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

Application of a simple column-switching ion chromatography technique for removal of matrix interferences and sensitive fluorescence determination of acidic compounds (pharmaceutical drugs) in complex samples.

PubMed

Muhammad, Nadeem; Subhani, Qamar; Wang, Fenglian; Guo, Dandan; Zhao, Qiming; Wu, Shuchao; Zhu, Yan

2017-09-15

This work illustrates the introduction of a simple, rugged and flexible column-switching ion chromatography (IC) technique for an automated on-line QuEChERS extracted samples extracts washing followed by sensitive fluorescence (FLD) determination of five acidic pharmaceutical drugs namely; clofibric acid (CLO), ibuprofen (IBU), aspirin (ASP), naproxen (NAP) and flurobrofen (FLU) in three complex samples (spinach, apple and hospital sewage sludge). An old anion exchange column IonPac ® AS11-HC was utilized as a pre-treatment column for on-line washing of inorganic and organic interferences followed by isocratic separation of five acidic drugs with another anion exchange IonPac ® AS12A analytical column by exploiting the column-switching technique. This novel method exhibited good linearity with correlation coefficients (r 2 ) for all drugs were in the range 0.976-0.996. The limit of detection and quantification of all five acidic drugs were in the range 0.024μg/kg to 8.70μg/kg and 0.082μg/kg to 0.029mg/kg, respectively, and better recoveries in the range 81.17-112.5% with percentage relative standard deviations (RSDs) less than 17.8% were obtained. This on-line sample pre-treatment method showed minimum matrix effect in the range of 0.87-1.25 except for aspirin. This simple rugged and flexible column-switching system required only 28min for maximum elimination of matrices and interferences in three complex samples extracts, isocratic separation of five acidic drugs and for the continuous regeneration of pre-treatment column prior to every subsequent analysis. Finally, this simple automated IC system was appeared so rugged and flexible, which can eliminate and wash out most of interference, impurities and matrices in complex samples, simply by adjusting the NaOH and acetonitrile concentration in washing mobile phase with maximum recoveries of acidic analytes of interest. Copyright © 2017. Published by Elsevier B.V.

Evaluation of micro-colorimetric lipid determination method with samples prepared using sonication and accelerated solvent extraction methods

EPA Science Inventory

Two common laboratory extraction techniques were evaluated for routine use with the micro-colorimetric lipid determination method developed by Van Handel (1985) [E. Van Handel, J. Am. Mosq. Control Assoc. 1(1985) 302] and recently validated for small samples by Inouye and Lotufo ...

An RF-Powered Micro-Reactor for Efficient Extraction and Hydrolysis

NASA Astrophysics Data System (ADS)

Scott, V.

2014-12-01

An RF sample-processing micro-reactor that was developed as part of potential in situ Exploration Missions to inner- and outer-planetary bodies was designed to utilize aqueous solutions subjected to 60 GHz radiation at 730 mW of input power to extract target organic compounds and molecular and inorganic ions as well as to hydrolyze complex polymeric materials. Successful identification and characterization of these molecules relies on the sample-processing techniques utilized alongside state-of-the-art detection and analysis. For mass and power restrictions put on space exploration missions, smaller and more efficient instruments are highly desirable. The RF micro-reactor potentially offers a simplified alternative to the typical gold-standard extractions that often use solvents, chemicals, and conditions that can vary wildly and depend on the targeted molecules. Instead, this instrument uses a single solvent ­— water — that can be "tuned" under the different experimental conditions, leveraging the operating principles of the Sub-Critical Water Extractor. Proof-of-concept experiments examining the hydrolysis of glycosidic and peptide bonds were successful in demonstrating the RF micro-reactor's capabilities. Progress toward coupling the reactor with a micro-scale sample-handling system enabling slurry delivery has been made and preliminary results on heterogeneous reactions and extractions will be presented.

Chip-based molecularly imprinted monolithic capillary array columns coated GO/SiO2 for selective extraction and sensitive determination of rhodamine B in chili powder.

PubMed

Zhai, Haiyun; Huang, Lu; Chen, Zuanguang; Su, Zihao; Yuan, Kaisong; Liang, Guohuan; Pan, Yufang

2017-01-01

A novel solid-phase extraction chip embedded with array columns of molecularly imprinted polymer-coated silanized graphene oxide (GO/SiO2-MISPE) was established to detect trace rhodamine B (RB) in chili powder. GO/SiO2-MISPE monolithic columns for RB detection were prepared by optimizing the supporting substrate, template, and polymerizing monomer under mild water bath conditions. Adsorption capacity and specificity, which are critical properties for the application of the GO/SiO2-MISPE monolithic column, were investigated. GO/SiO2-MIP was examined by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy. The recovery and the intraday and interday relative standard deviations for RB ranged from 83.7% to 88.4% and 2.5% to 4.0% and the enrichment factors were higher than 110-fold. The chip-based array columns effectively eliminated impurities in chili powder, indicating that the chip-based GO/SiO2-MISPE method was reliable for RB detection in food samples using high-performance liquid chromatography. Accordingly, this method has direct applications for monitoring potentially harmful dyes in processed food. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effects of Particle Size and Bubble Characteristics on Transport of Micro- and Nano-Bubbles in Saturated Porous Media

NASA Astrophysics Data System (ADS)

Hamamoto, S.; Nihei, N.; Ueda, Y.; Moldrup, P.; Nishimura, T.

2016-12-01

The micro- and nano-bubbles (MNBs) have considerable potentials for the remediation of soil contaminated by organic compounds when used in conjunction with bioremediation technology. Understanding a transport mechanism of MNBs in soils is essential to optimize remediation techniques using MNBs. In this study, column transport experiments using glass beads with different size fractions (average particles size: 0.1 mm and 0.4 mm) were conducted, where MNBs created by oxygen gas were injected to the column with different flow rates. Effects of particle size and bubble characteristics on MNB transport in porous media were investigated based on the column experiments. The results showed that attachments of MNBs were enhanced under lower flow rate. Under higher flow rate condition, there were not significant differences of MNBs transport in porous media with different particle size. A convection-dispersion model including bubble attachment, detachment, and straining terms was applied to the obtained breakthrough curves for each experiment, showing good fitness against the measured data. Further investigations will be conducted to understand bubble characteristics including bubble size and zeta potential on MNB transport in porous media. Relations between in model parameters in the transport model and physical and chemical properties in porous media and MNBs will be discussed.

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

PubMed

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

2013-03-01

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

Suitability of polydimethylsiloxane rods for the headspace sorptive extraction of polybrominated diphenyl ethers from water samples.

PubMed

Montes, R; Rodríguez, I; Rubí, E; Cela, R

2007-03-02

The suitability of an inexpensive polydimethysiloxane (PDMS) sorbent, produced on an industrial scale, for the extraction of polybrominated diphenyl ethers (PBDEs), from tetra- to hexabrominated congeners, from water samples was assessed. Experiments were carried out using samples spiked with a pentabromo diphenyl ether (pentaBDE) mixture, PDMS rods with a diameter of 2 mm and gas chromatography with micro-electron-capture detection (GC-micro-ECD). Influence of several variables on the efficiency of the enrichment step and the further desorption of the analytes was investigated in detail. The best performance was achieved in the headspace sorptive extraction (HSSE) mode, at 95 degrees C, using 80 mL water samples containing a 30% of sodium chloride. Extractions were performed overnight using disposable PDMS rods with a length of 10 mm (31 microL volume). Analytes were further recovered from the PDMS sorbent using just 1 mL of diethyl ether. This solvent was evaporated and extracts reconstituted with 25 microL of isooctane. Under final working conditions absolute extraction efficiencies from 69 to 93% and enrichment factors higher than 2200 folds were achieved for all species. The proposed method provided acceptable precisions (relative standard deviations values under 12%), correlation coefficients higher than 0.998 and the yield of the HSSE process remained constant for different water samples.

[Absorbed doses to critical organs from full mouth dental radiography].

PubMed

Zhang, G; Yasuhiko, O; Hidegiko, Y

1999-01-01

A few studies were reported in China on radiological risk of dental radiography. The aim of this study is to evaluate the absorbed doses of patients from the full mouth radiographs, and to find out the contribution from each projection to the total absorbed dose of the organs. Absorbed doses to critical organs were measured from 14-film complete dental radiography. The organs included pituitary, optical lens, parotid glands, submandibular glands, sublingual glands, thyroid, breasts, ovary, testes and the skin in center field of each projection were studied. A-radiation analog dosimetry system (RANDO) phantom with thermoluminescent dosimeters (ILD200) was used for the study. All of the exposure parameters were fixed. The total filtration was 2 mm Al equivalent. The column collaboration was 6 cm in diameter and 20 cm in length. The absorbed doses of organs were measured three times in each projection of the full-mouth series (FMS) exposures. The absorbed dose of lenses in FMS (249 microGy) in present study was much less (10%) than the doses (2,630 microGy) reported in 1976. The doses absorbed of other organs in the present study were thyroid gland (125 microGy), pituitary gland (112 microGy), parotid gland (153 microGy), submandibular gland (629 microGy), sublingual gland (1,900 microGy), and breast gland (12 microGy). The doses of the ovary and testis were to small to further analysis. All of the results show that the radiation risk to patients in intraoral radiograph has been reduced significantly. In the pituitary, half of the dose is from both sides of the maxillary molar projection. For the lenses, the largest contribultions of radiation (60%) come from the ipsilateral molar and premolar projection of maxilla. In parotid gland, up to 57% of the dose is from the contralateral molar, pre-molar and canine of maxilla. It could be derived that about 90% of the absorbed doses could be avoided in FMS if the column collimator is 20 cm long and the filter is 2.0 mm thick. If we use the 10-film complete mouth radiograph instead of the 14-film series, more 20% of the doses would be reduced.

Intrinsic advantages of packed capillaries over narrow-bore columns in very high-pressure gradient liquid chromatography.

PubMed

Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

2016-06-17

250μm×100mm fused silica glass capillaries were packed with 1.8μm high-strength silica (HSS) fully porous particles. They were prepared without bulky stainless steel endfittings and metal frits, which both generate significant sample dispersion. The isocratic efficiencies and gradient peak capacities of these prototype capillary columns were measured for small molecules (n-alkanophenones) using a home-made ultra-low dispersive micro-HPLC instrument. Their resolution power was compared to that of standard 2.1mm×100mm very high-pressure liquid chromatography (vHPLC) narrow-bore columns packed with the same particles. The results show that, for the same column efficiency (25000 plates) and gradient steepness (0.04min(-1)), the peak capacity of the 250μm i.d. capillary columns is systematically 15-20% higher than that of the 2.1mm i.d. narrow-bore columns. A validated model of gradient chromatography enabled one to predict accurately the observed peak capacities of the capillary columns for non-linear solvation strength retention behavior and under isothermal conditions. Thermodynamics applied to the eluent quantified the temperature difference for the thermal gradients in both capillary and narrow-bore columns. Experimental data revealed that the gradient peak capacity is more affected by viscous heating than the column efficiency. Unlike across 2.1mm i.d. columns, the changes in eluent composition across the 250μm i.d. columns during the gradient is rapidly relaxed by transverse dispersion. The combination of (1) the absence of viscous heating and (2) the high uniformity of the eluent composition across the diameter of capillary columns explains the intrinsic advantage of capillary over narrow-bore columns in gradient vHPLC. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of cadmium in sediments on colonization by benthic marine organisms: Role of interstitial cadmium and acid volatile sulfide in bioavailability

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

Hansen, D.; Berry, W.; Benyi, S.

1995-12-31

The role of interstitial cadmium and acid volatile sulfide (AVS) in controlling the bioavailability of sediment-associated metal was examined using the chronic saltwater benthic colonization test. Sediments were spiked with cadmium to achieve simultaneously extracted metal (SEM)/AVS molar ratios of 0. 0 (control), 0.1, 0.8 and 3.0 in this 118-day test. Oxidation of AVS in the surficial 2.4 cm within two to four weeks resulted in sulfide profiles similar to those occurring naturally in local sediments. In the nominal 0.1 SEM/AVS treatment, measured SEM was always less than AVS. Interstitial cadmium concentrations (< 3--10 {micro}g/L) were below those likely tomore » cause biological effects. No significant biological effects were detected. In the nominal 0.8 SEM/AVS treatment, measured SEM commonly exceeded AVS in the surficial 2.4 cm of sediment. Interstitial cadmium concentrations (24--157 {micro}g/L) were likely of toxicological significance to sensitive species. Shifts were observed in presence/absence of species, and there were fewer macrobenthic polychaetes (Mediomastus ambiseta, Strebloapio benedicti and Podarke obscura) and unidentified meiofaunal nematodes. In the nominal 3.0 SEM/AVS treatment, concentrations of SEM were always greater than AVS throughout the sediment column. Interstitial cadmium ranged from 28,000 to 174,000 {micro}g/L. In addition to the effects above, these sediments were colonized by fewer macrobenthic species, polychaete species and harpacticoids; had lower densities of diatoms; lacked bivalve molluscs and exhibited other impacts. The observed biological responses were consistent with measured SEM/AVS ratios in surficial sediments and interstitial water cadmium concentrations, further supporting their utility in predicting metals bioavailability.« less

Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

PubMed

Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

2016-05-01

Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples.

Bio-inspired multi-mode optic flow sensors for micro air vehicles

NASA Astrophysics Data System (ADS)

Park, Seokjun; Choi, Jaehyuk; Cho, Jihyun; Yoon, Euisik

2013-06-01

Monitoring wide-field surrounding information is essential for vision-based autonomous navigation in micro-air-vehicles (MAV). Our image-cube (iCube) module, which consists of multiple sensors that are facing different angles in 3-D space, can be applied to the wide-field of view optic flows estimation (μ-Compound eyes) and to attitude control (μ- Ocelli) in the Micro Autonomous Systems and Technology (MAST) platforms. In this paper, we report an analog/digital (A/D) mixed-mode optic-flow sensor, which generates both optic flows and normal images in different modes for μ- Compound eyes and μ-Ocelli applications. The sensor employs a time-stamp based optic flow algorithm which is modified from the conventional EMD (Elementary Motion Detector) algorithm to give an optimum partitioning of hardware blocks in analog and digital domains as well as adequate allocation of pixel-level, column-parallel, and chip-level signal processing. Temporal filtering, which may require huge hardware resources if implemented in digital domain, is remained in a pixel-level analog processing unit. The rest of the blocks, including feature detection and timestamp latching, are implemented using digital circuits in a column-parallel processing unit. Finally, time-stamp information is decoded into velocity from look-up tables, multiplications, and simple subtraction circuits in a chip-level processing unit, thus significantly reducing core digital processing power consumption. In the normal image mode, the sensor generates 8-b digital images using single slope ADCs in the column unit. In the optic flow mode, the sensor estimates 8-b 1-D optic flows from the integrated mixed-mode algorithm core and 2-D optic flows with an external timestamp processing, respectively.

Valerian extract Ze 911 inhibits postsynaptic potentials by activation of adenosine A1 receptors in rat cortical neurons.

PubMed

Vissiennon, Z; Sichardt, K; Koetter, U; Brattström, A; Nieber, K

2006-06-01

In this study we evaluated the adenosine A1 receptor-mediated effect of valerian extract (Ze 911) on postsynaptic potentials (PSPs) in pyramidal cells of the rat cingulate cortex in a slice preparation. We first observed that N6-cyclopentyladenosine (CPA, 0.01 - 10 microM), an adenosine A1 receptor agonist, inhibited PSPs in a concentration-dependent manner. The CPA (10 microM)-induced inhibition was antagonized by 1,3-dipropyl-8-cyclopentylxanthine (DPCPX, 0.1 microM), an adenosine A1 receptor antagonist. Ze 911 concentration dependently (0.1 - 15 mg/mL) inhibited PSPs in the presence of the adenosine A2A receptor antagonist 1,3,7-trimethyl-8-(3-chlorostyryl)xanthine (CSC, 0.2 microM) and adenosine deaminase (1 U/mL). The maximal inhibition induced by 10 mg/mL was completely antagonised by DPCPX (0.1 microM), an A1 receptor blocker. The data suggest that activation of adenosine A1 receptors is involved in the pharmacological effects of the valerian extract Ze 911.

Bioactive compounds from orange epicarp to enrich fish burgers.

PubMed

Spinelli, Sara; Lecce, Lucia; Likyova, Desislava; Del Nobile, Matteo Alessandro; Conte, Amalia

2018-05-01

The orange industry produces considerable amounts of by-products, traditionally used for animal feed or fuel production. Most of these by-products could be used as functional ingredients. To assess the potential food application of orange epicarp, different percentages of micro-encapsulated orange extract were added to fresh fish burgers. Then, an in vitro digestion was also carried out, before and after micro-encapsulation, to measure the bio-accessibility of the active compounds. A significant increase of bio-accessibility of bioactive compounds has been observed in the orange epicarp extract after micro-encapsulation by spray-drying. From the sensory point of view, the fish sample enriched with 50 g kg -1 micro-encapsulated extract was the most comparable to the control burger, even if it showed a higher phenolic, flavonoid and carotenoid bio-accessibility. Orange epicarp may be used as a food additive to enhance the health content of food products. The micro-encapsulation is a valid technique to protect the bioactive compounds and increase their bio-accessibility. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

A novel convenient process to obtain a raw decaffeinated tea polyphenol fraction using a lignocellulose column.

PubMed

Sakanaka, Senji

2003-05-07

Lignocellulose prepared from sawdust was investigated for its potential application in obtaining a raw decaffeinated tea polyphenol fraction from tea extract. Tea polyphenols having gallate residues, namely, (-)epigallocatechin gallate (EGCg) and (-)epicatechin gallate (ECg), were adsorbed on the lignocellulose column, while caffeine was passed through it. Adsorbed polyphenols were eluted with 60% ethanol, and the elute was found to consist mainly of EGCg and ECg. The caffeine/EGCg ratio was 0.696 before lignocellulose column treatment, but it became 0.004 after the column treatment. These results suggest that the lignocellulose column provides a useful and convenient process of purification of tea polyphenol fraction accompanied by decaffeination.

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments NAC/SETAC 2012

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments (SETAC Europe 22nd Annual Meeting)

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Protocol for Initial Purification of Bacteriocin

DTIC Science & Technology

2015-10-01

lysate/extract preparation, column purification, and a desalting . The peptide was tracked throughout the process using a soft agar overlay activity...tris PAGE. It is necessary to desalt those samples for 150-mM and 1-M fractions, by using dialysis or G10 sephadex columns, in order to prevent

Phenolic composition of pomegranate peel extracts using an LC-MS approach with silica hydride columns

USDA-ARS?s Scientific Manuscript database

The peels of different pomegranate cultivars (Molla Nepes, Parfianka, Purple Heart, Wonderful and Vkunsyi) were compared in terms of phenolic composition and total phenolics. Analyses were performed on two silica hydride-based stationary phases: phenyl and undecenoic acid columns. Quantitation was ...

One-pot preparation of a sulfamethoxazole functionalized affinity monolithic column for selective isolation and purification of trypsin.

PubMed

Xiao, Yuan; Guo, Jialiang; Ran, Danni; Duan, Qianqian; Crommen, Jacques; Jiang, Zhengjin

2015-06-26

A facile and efficient "one-pot" copolymerization strategy was used for the preparation of sulfonamide drug (SA) functionalized monolithic columns. Two novel SA-immobilized methacrylate monolithic columns, i.e. poly(GMA-SMX-co-EDMA) and poly(GMA-SAA-co-EDMA) were prepared by one-pot in situ copolymerization of the drug ligand (sulfamethoxazole (SMX) or sulfanilamide (SAA)), the monomer (glycidyl methacrylate, GMA) and the cross-linker (ethylene dimethacrylate, EDMA) within 100 μm i.d. capillaries under optimized polymerization conditions. The physicochemical properties and column performance of the fabricated monolithic columns were characterized by elemental analysis, scanning electron microscopy and micro-HPLC. Satisfactory column permeability, efficiency and separation performance were obtained on the optimized poly(GMA-SMX-co-EDMA) monolithic column for small molecules, such as a standard test mixture and eight aromatic ketones. Notably, it was found that the poly(GMA-SMX-co-EDMA) monolith showed a selective affinity to trypsin, while the poly(GMA-SAA-co-EDMA) monolith containing sulfanilamide did not exhibit such affinity at all. This research not only provides a novel monolith for the selective isolation and purification of trypsin, but it also offers the possibility to easily prepare novel drug functionalized methacrylate monoliths through a one-pot copolymerization strategy. Copyright © 2015 Elsevier B.V. All rights reserved.

Semi-industrial experimental study on bauxite separation using a cell-column integration process

NASA Astrophysics Data System (ADS)

Zhang, Ning-ning; Zhou, Chang-chun; Cong, Long-fei; Cao, Wen-long; Zhou, You

2016-01-01

The cyclonic-static micro-bubble flotation column (FCSMC) is a highly efficient mineral processing equipment. In this study, a cell-column (FCSMC) integration process was investigated for the separation of bauxite and its feasibility was analyzed on a theoretical basis. The properties of low-grade bauxite ore from Henan Province, China were analyzed. Parameters such as reagent dosage, scraping bubble time, and pressure of the circulating pump during the sorting process were investigated and optimized to improve the flotation efficiency. On the basis of these parameters, continuous separation experiments were conducted. Bauxite concentrate with an aluminum-to-silicon (A/S) mass ratio of 6.37 and a 77.63wt% recovery rate were achieved via a flow sheet consisting of "fast flotation using a flotation cell, one roughing flotation and one cleaning flotation using flotation columns". Compared with the full-flotation-cells process, the cell-column integration process resulted in an increase of the A/S ratio by 0.41 and the recovery rate by 17.58wt%. Cell-column integration separation technology represents a new approach for the separation of middle-to-low-grade bauxite ore.

Activity of Antarctic fungi extracts against phytopathogenic bacteria.

PubMed

Purić, J; Vieira, G; Cavalca, L B; Sette, L D; Ferreira, H; Vieira, M L C; Sass, D C

2018-06-01

This study aims to obtain secondary metabolites extracts from filamentous fungi isolated from soil and marine sediments from Antarctic ecosystems and to assess its potential antibacterial activity on Xanthomonas euvesicatoria and Xanthomonas axonopodis pv. passiflorae (phytopathogenic bacteria causing diseases in pepper and tomato and passionfruit, respectively). Among the 66 crude intracellular and extracellular extracts obtained from fungi recovered from soil and 79 obtained from marine sediment samples, 25 showed the ability to prevent the growth of X. euvesicatoria in vitro and 28 showed the ability to prevent the growth of X. axonopodis pv. passiflorae in vitro. Intracellular and extracellular extracts from soil fungi inhibited around 97% of X. euvesicatoria and 98% of X. axonopodis pv. passiflorae at 2·1 mg ml -1 . The average inhibition rates against X. euvesicatoria and X. axonopodis pv. passiflorae for intracellular and extracellular extracts from marine sediments fungi were around 96 and 97%, respectively, at 3·0 mg ml -1 . Extracts containing secondary metabolites with antimicrobial activity against X. euvesicatoria and X. axonopodis pv. passiflorae were obtained, containing possible substitutes for the products currently used to control these phytopathogens. Micro-organisms from extreme ecosystems, such as the Antarctic ecosystem, need to survive in harsh conditions with low temperatures, low nutrients and high UV radiation. Micro-organisms adapt to these conditions evolving diverse biochemical and physiological adaptations essential for survival. All this makes these micro-organisms a rich source of novel natural products based on unique chemical scaffolds. Discovering novel bioactive compounds is essential because of the rise in antibiotic-resistant micro-organisms and the emergence of new infections. Fungi from Antarctic environments have been proven to produce bioactive secondary metabolites against various micro-organisms, but few studies have shown activity against Xanthomonas phytopathogens. © 2018 The Society for Applied Microbiology.

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.

Diabetic retinopathy grading by digital curvelet transform.

PubMed

Hajeb Mohammad Alipour, Shirin; Rabbani, Hossein; Akhlaghi, Mohammad Reza

2012-01-01

One of the major complications of diabetes is diabetic retinopathy. As manual analysis and diagnosis of large amount of images are time consuming, automatic detection and grading of diabetic retinopathy are desired. In this paper, we use fundus fluorescein angiography and color fundus images simultaneously, extract 6 features employing curvelet transform, and feed them to support vector machine in order to determine diabetic retinopathy severity stages. These features are area of blood vessels, area, regularity of foveal avascular zone, and the number of micro-aneurisms therein, total number of micro-aneurisms, and area of exudates. In order to extract exudates and vessels, we respectively modify curvelet coefficients of color fundus images and angiograms. The end points of extracted vessels in predefined region of interest based on optic disk are connected together to segment foveal avascular zone region. To extract micro-aneurisms from angiogram, first extracted vessels are subtracted from original image, and after removing detected background by morphological operators and enhancing bright small pixels, micro-aneurisms are detected. 70 patients were involved in this study to classify diabetic retinopathy into 3 groups, that is, (1) no diabetic retinopathy, (2) mild/moderate nonproliferative diabetic retinopathy, (3) severe nonproliferative/proliferative diabetic retinopathy, and our simulations show that the proposed system has sensitivity and specificity of 100% for grading.

Automated on-line renewable solid-phase extraction-liquid chromatography exploiting multisyringe flow injection-bead injection lab-on-valve analysis.

PubMed

Quintana, José Benito; Miró, Manuel; Estela, José Manuel; Cerdà, Víctor

2006-04-15

In this paper, the third generation of flow injection analysis, also named the lab-on-valve (LOV) approach, is proposed for the first time as a front end to high-performance liquid chromatography (HPLC) for on-line solid-phase extraction (SPE) sample processing by exploiting the bead injection (BI) concept. The proposed microanalytical system based on discontinuous programmable flow features automated packing (and withdrawal after single use) of a small amount of sorbent (<5 mg) into the microconduits of the flow network and quantitative elution of sorbed species into a narrow band (150 microL of 95% MeOH). The hyphenation of multisyringe flow injection analysis (MSFIA) with BI-LOV prior to HPLC analysis is utilized for on-line postextraction treatment to ensure chemical compatibility between the eluate medium and the initial HPLC gradient conditions. This circumvents the band-broadening effect commonly observed in conventional on-line SPE-based sample processors due to the low eluting strength of the mobile phase. The potential of the novel MSFI-BI-LOV hyphenation for on-line handling of complex environmental and biological samples prior to reversed-phase chromatographic separations was assessed for the expeditious determination of five acidic pharmaceutical residues (viz., ketoprofen, naproxen, bezafibrate, diclofenac, and ibuprofen) and one metabolite (viz., salicylic acid) in surface water, urban wastewater, and urine. To this end, the copolymeric divinylbenzene-co-n-vinylpyrrolidone beads (Oasis HLB) were utilized as renewable sorptive entities in the micromachined unit. The automated analytical method features relative recovery percentages of >88%, limits of detection within the range 0.02-0.67 ng mL(-1), and coefficients of variation <11% for the column renewable mode and gives rise to a drastic reduction in operation costs ( approximately 25-fold) as compared to on-line column switching systems.

On-line liquid chromatography/tandem mass spectrometry simultaneous determination of opiates, cocainics and amphetamines in dried blood spots.

PubMed

Saussereau, E; Lacroix, C; Gaulier, J M; Goulle, J P

2012-02-15

A novel approach has been developed for the illicit drugs quantitative determination using dried blood spots (DBS) on filter paper. The illicit drugs tested were opiates (morphine and its 3- and 6-glucuronide metabolites, codeine, 6-monoacetylmorphine), cocainics (ecgonine methylester, benzoylecgonine, cocaine, cocaethylene) and amphetamines (amphetamine, methamphetamine, MDA, MDMA, MDEA). The described method, requiring a small blood volume, is based on high performance liquid chromatography coupled to tandem mass spectrometry using on-line extraction. A Whatman card 903 was spotted with 30μL of whole blood and left overnight to dry at room temperature. A 3-mm diameter disk was removed using a manual punch, suspended in 150μL of water for 10min with ultrasonication, and then 100μL was injected in the on-line LC-MS/MS system. An Oasis HLB was used as an extraction column and a C18 Atlantis as an analytical column. The chromatographic cycle was performed with 20mM ammonium formate buffer (pH 2.8) (solvent A) and acetonitrile/solvent A (90:10, v/v) gradient in 16min. Detection was performed in positive electrospray ionization mode (ESI+) with a Quattro Micro (Waters). Recoveries of all analytes were up to 80%. DBS were stored in duplicate at 4°C and -20°C for up to 6 months. Illicit drugs seemed to be much more stabled at -20°C. Furthermore, it was tested whether analysis of DBS may be as reliable as that of whole blood investigating authentic samples; significant correlations were obtained. This DBS assay has potential as rapid, sensitive and inexpensive option for the illicit drugs determination in small blood volumes, which seems of great interest in suspected cases of driving under the influence of drugs. Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of strontium-90 in milk samples using a controlled precipitation clean-up step prior to ion-chromatography.

PubMed

Cobb, J; Warwick, P; Carpenter, R C; Morrison, R T

1995-12-01

Strontium-90 may be determined by beta-counting its yttrium-90 daughter following separation by ion-chromatography, using a three column system comprising a chelating concentrator column, a cation-exchange column and an anion-exchange separator column. The column system has previously been applied to the determination of strontium-90 in water and urine samples. The applicability of the system to the analysis of milk is hampered by the large concentrations of calcium present, which significantly reduces the extraction of yttrium-90 by the concentrator column. A maximum of approximately 200 mg of calcium can be present for the successful extraction of yttrium-90, which greatly limits the quantity of milk that can be analysed. The quantity of milk analysed can be increased by the inclusion of a controlled precipitation step prior to the ion-chromatographic separation. The precipitation is carried out on acid digested milk samples by the addition of ammonia solution until the addition of one drop causes a reduction in pH resulting in the precipitation of calcium hydrogenphosphate. Under these conditions, approximately 20% of the calcium present in the original milk sample is precipitated, yttrium-90 is precipitated whereas strontium-90 is not precipitated. Dissolution of the precipitate, followed by separation of yttrium-90 using the ion-chromatography system facilitates the analysis of a litre of milk with recoveries of greater than 80%.

Aging effect on Zn retention on a calcareous soil: column experiments and synchrotron X-ray micro-spectroscopic investigation.

PubMed

Sayen, Stéphanie; Guillon, Emmanuel

2014-07-15

In this study, a combination of column experiments and micro-analytical techniques exploiting synchrotron generated X-rays was used to assess the effect of aging time on Zn retention and mobility in the specific case of calcareous soils (high pH value, ≈ 8). The samples were subjected to aging for 2, 6, 17, and 63 days. Freshly added Zn mainly existed as an exchangeable form, and this metal fraction decreased over time due to Zn redistribution to stronger binding sites. Thus, after aging for 63 days, 45% of Zn is remobilized from exchangeable sites to stronger binding sites. μ-XRF maps were used to find correlations among elements in the sample, and μ-XANES spectra were recorded to precise Zn speciation. These analyses evidenced an increasing partitioning of Zn from organic matter to iron oxy(hydr)oxides over time. The occurrence of hydrozincite is evidenced in all samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Electro-osmotically driven liquid delivery method and apparatus

DOEpatents

Rakestraw, D.J.; Anex, D.S.; Yan, C.; Dadoo, R.; Zare, R.N.

1999-08-24

Method and apparatus are disclosed for controlling precisely the composition and delivery of liquid at sub-{micro}L/min flow rate. One embodiment of such a delivery system is an electro-osmotically driven gradient flow delivery system that generates dynamic gradient flows with sub-{micro}L/min flow rates by merging a plurality of electro-osmotic flows. These flows are delivered by a plurality of delivery arms attached to a mixing connector, where they mix and then flow into a receiving means, preferably a column. Each inlet of the plurality of delivery arms is placed in a corresponding solution reservoir. A plurality of independent programmable high-voltage power supplies is used to apply a voltage program to each of the plurality of solution reservoirs to regulate the electro-osmotic flow in each delivery arm. The electro-osmotic flow rates in the delivery arms are changed with time according to each voltage program to deliver the required gradient profile to the column. 4 figs.

Phenolic composition of pomegranate peel extracts using an liquid chromatography-mass spectrometry approach with silica hydride columns.

PubMed

Young, Joshua E; Pan, Zhongli; Teh, Hui Ean; Menon, Veena; Modereger, Brent; Pesek, Joseph J; Matyska, Maria T; Dao, Lan; Takeoka, Gary

2017-04-01

The peels of different pomegranate cultivars (Molla Nepes, Parfianka, Purple Heart, Wonderful and Vkunsyi) were compared in terms of phenolic composition and total phenolics. Analyses were performed on two silica hydride based stationary phases: phenyl and undecanoic acid columns. Quantitation was accomplished by developing a liquid chromatography with mass spectrometry approach for separating different phenolic analytes, initially in the form of reference standards and then with pomegranate extracts. The high-performance liquid chromatography columns used in the separations had the ability to retain a wide polarity range of phenolic analytes, as well as offering beneficial secondary selectivity mechanisms for resolving the isobaric compounds, catechin and epicatechin. The Vkunsyi peel extract had the highest concentration of phenolics (as determined by liquid chromatography with mass spectrometry) and was the only cultivar to contain the important compound punicalagin. The liquid chromatography with mass spectrometry data were compared to the standard total phenolics content as determined by using the Folin-Ciocalteu assay. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multiclonal plastic antibodies for selective aflatoxin extraction from food samples.

PubMed

Bayram, Engin; Yılmaz, Erkut; Uzun, Lokman; Say, Rıdvan; Denizli, Adil

2017-04-15

Herein, we focused on developing a new generation of monolithic columns for extracting aflatoxin from real food samples by combining the superior features of molecularly imprinted polymers and cryogels. To accomplish this, we designed multiclonal plastic antibodies through simultaneous imprinting of aflatoxin subtypes B1, B2, G1, and G2. We applied Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and spectrofluorimetry to characterize the materials, and conducted selectivity studies using ochratoxin A and aflatoxin M1 (a metabolite of aflatoxin B1), as well as other aflatoxins, under competitive conditions. We determined optimal aflatoxin extraction conditions in terms of concentration, flow rate, temperature, and embedded particle amount as up to 25ng/mL for each species, 0.43mL/min, 7.0, 30°C, and 200mg, respectively. These multiclonal plastic antibodies showed imprinting efficiencies against ochratoxin A and aflatoxin M1 of 1.84 and 26.39, respectively, even under competitive conditions. Finally, we tested reusability, repeatability, reproducibility, and robustness of columns throughout inter- and intra-column variation studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

Impact of the uranium (VI) speciation in mineralised urines on its extraction by calix[6]arene bearing hydroxamic groups used in chromatography columns.

PubMed

Baghdadi, S; Bouvier-Capely, C; Ritt, A; Peroux, A; Fevrier, L; Rebiere, F; Agarande, M; Cote, G

2015-11-01

Actinides determination in urine samples is part of the analyses performed to monitor internal contamination in case of an accident or a terrorist attack involving nuclear matter. Mineralisation is the first step of any of these analyses. It aims at reducing the sample volume and at destroying all organic compounds present. The mineralisation protocol is usually based on a wet ashing step, followed by actinides co-precipitation and a furnace ashing step, before redissolution and the quantification of the actinides by the appropriate techniques. Amongst the existing methods to perform the actinides co-precipitation, alkali-earth (typically calcium) precipitation is widely used. In the present work, the extraction of uranium(VI), plutonium(IV) and americium(III) from the redissolution solutions (called "mineralised urines") on calix[6]arene columns bearing hydroxamic groups was investigated as such an extraction is a necessary step before their determination by ICP-MS or alpha spectrometry. Difficulties were encountered in the transfer of uranium(VI) from raw to mineralised urines, with yield of transfer ranging between 0% and 85%, compared to about 90% for Pu and Am, depending on the starting raw urines. To understand the origin of such a difficulty, the speciation of uranium (VI) in mineralised urines was investigated by computer simulation using the MEDUSA software and the associated HYDRA database, compiled with recently published data. These calculations showed that the presence of phosphates in the "mineralised urines" leads to the formation of strong uranyl-phosphate complexes (such as UO2HPO4) which compete with the uranium (VI) extraction by the calix[6]arene bearing hydroxamic groups. The extraction constant of uranium (VI) by calix[6]arene bearing hydroxamic groups was determined in a 0.04 mol L(-1) sodium nitrate solution (logK=4.86±0.03) and implemented in an extraction model taking into account the speciation in the aqueous phase. This model allowed to simulate satisfactorily the experimental uranium extraction data and to support the preliminary conclusions about the role of the phosphates present in mineralised urines. These calculations also showed that the phosphate/calcium ratio is a key parameter as far as the efficiency of the uranium (VI) extraction by the calix[6]arene columns is concerned. It predicted that the addition of CaCl2 in mineralised urines would release uranium (VI) from phosphates by forming calcium (II)-phosphate complexes and thus facilitate the uranium (VI) extraction on calix[6]arene columns. These predictions were confirmed experimentally as the addition of 0.1 mol L(-1) CaCl2 to a mineralised urine containing naturally a high concentration of phosphate (typically 0.04 mol L(-1)) significantly increased the percentage of uranium (VI) extraction on the calix[6]arene columns. Copyright © 2015 Elsevier B.V. All rights reserved.

Rapid non-enzymatic extraction method for isolating PCR-quality camelpox virus DNA from skin.

PubMed

Yousif, A Ausama; Al-Naeem, A Abdelmohsen; Al-Ali, M Ahmad

2010-10-01

Molecular diagnostic investigations of orthopoxvirus (OPV) infections are performed using a variety of clinical samples including skin lesions, tissues from internal organs, blood and secretions. Skin samples are particularly convenient for rapid diagnosis and molecular epidemiological investigations of camelpox virus (CMLV). Classical extraction procedures and commercial spin-column-based kits are time consuming, relatively expensive, and require multiple extraction and purification steps in addition to proteinase K digestion. A rapid non-enzymatic procedure for extracting CMLV DNA from dried scabs or pox lesions was developed to overcome some of the limitations of the available DNA extraction techniques. The procedure requires as little as 10mg of tissue and produces highly purified DNA [OD(260)/OD(280) ratios between 1.47 and 1.79] with concentrations ranging from 6.5 to 16 microg/ml. The extracted CMLV DNA was proven suitable for virus-specific qualitative and, semi-quantitative PCR applications. Compared to spin-column and conventional viral DNA extraction techniques, the two-step extraction procedure saves money and time, and retains the potential for automation without compromising CMLV PCR sensitivity. Copyright (c) 2010 Elsevier B.V. All rights reserved.

[Effect of the ethanol extracts of starfish Asterias amurensis on the levels of serum IL-4 and IFN-γ in mice].

PubMed

He, Su-hui; Tang, Xiao-lei; Deng, Ye-feng; Chen, Zhang-quan

2011-11-01

To investigate the effect of the ethanol extracts of the starfish Asterias amurensis on the levels of serum IL-4 and IFN-γ in mice. The whole bodies of the starfish were chopped and extracted with ethanol. The ethanol extracts were chromatographed on silica gel column. The separating fractions of the ethanol extracts were intraperitoneally injected into mice, respectively. The levels of serum IL-4 and IFN-γ in mice were detected by ELISA. The ethanol extracts from the starfish were separated through silica gel column chromatography to obtain 8 fractions (I-VIII). The high levels of IL-4 and IFN-γ were produced in serum of the mice injected with fractions III and VIII of the ethanol extracts from the starfish Asterias amurensis. The fractions III and VIIII separated from the ethanol extracts of the starfish Asterias amurensis can stimulate the mice to produce high lelves of IL-4 and IFN-γ, which has the characteristic of natural kill T (NKT) cells activator. It is suggests that there is the active substance that can activate NKT cells in the starfish Asterias amurensis.

Design and implementation of an array of micro-electrochemical detectors for two-dimensional liquid chromatography--proof of principle.

PubMed

Abia, Jude A; Putnam, Joel; Mriziq, Khaled; Guiochon, Georges A

2010-03-05

Simultaneous two-dimensional liquid chromatography (2D-LC) is an implementation of two-dimensional liquid chromatography which has the potential to provide very fast, yet highly efficient separations. It is based on the use of time x space and space x space separation systems. The basic principle of this instrument has been validated long ago by the success of two-dimensional thin layer chromatography. The construction of a pressurized wide and flat column (100 mm x 100 mm x 1 mm) operated under an inlet pressure of up to 50 bar was described previously. However, to become a modern analytical method, simultaneous 2D-LC requires the development of detectors suitable for the monitoring of the composition of the eluent of this pressurized planar, wide column. An array of five equidistant micro-electrochemical sensors was built for this purpose and tested. Each sensor is a three-electrode system, with the working electrode being a 25 microm polished platinum micro-electrode. The auxiliary electrode is a thin platinum wire and the reference electrode an Ag/AgCl (3M sat. KCl) electrode. In this first implementation, proof of principle is demonstrated, but the final instrument will require a much larger array. 2010 Elsevier B.V. All rights reserved.

[Analysis of sialic acid in infant formulas using ultra performance liquid chromatography-triple quadrupole mass spectrometry].

PubMed

Xie, Honglei; Li, Chun; Liu, Ning

2013-08-01

The method for analysing sialic acid in infant formulas by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been established. Sialic acid in milk was released via acid hydrolysis, and purified by an HLB solid phase extraction cartridge. The UPLC separation was performed on an ACQUITY UPLC BEH HILIC column (50 mm x 2.1 mm, 1.7 microm) utilizing a gradient elution program of acetonitrile and water (containing 0.1% formic acid) as the mobile phases at a flow rate of 0.25 mL/min. Injection volume and column temperature were set at 5 microL and 30 degrees C, respectively. The identification and quantification were achieved by using electrospray ionisation (ESI)-MS/MS in positive ion mode and multiple reaction monitoring (MRM) mode. The linear range was from 0.05 to 5.0 mg/L for sialic acid and the correlation coefficient (R(2)) was greater than 0.99. The average recoveries spiked at the four concentration levels of 0.1, 0.5, 2.5 and 5.0 mg/L ranged between 84.3% and 98.9% with the relative standard deviations from 4.9% to 8.2%. The limit of detection was 0.01 mg/L. Therefore, this method has the characteristics of simple operation, high reproducibility and sensitivity. It can be widely applied to determine the total contents of sialic acid in infant formula, cow milk and human milk.

Quantitative determination of n-propane, iso-butane, and n-butane by headspace GC-MS in intoxications by inhalation of lighter fluid.

PubMed

Bouche, Marie-Paule L A; Lambert, Willy E; Van Bocxlaer, Jan F P; Piette, Michel H; De Leenheer, André P

2002-01-01

This report describes a fully elaborated and validated method for quantitation of the hydrocarbons n-propane, iso-butane, and n-butane in blood samples. The newly developed analytical procedure is suitable for both emergency cases and forensic medicine investigations. Its practical applicability is illustrated with a forensic blood sample after acute inhalative intoxication with lighter fluid; case history and toxicological findings are included. Identification and quantitation of the analytes were performed using static headspace extraction combined with gas chromatography-mass spectrometry. In order to reconcile the large gas volumes injected (0.5 mL) with the narrowbore capillary column and thus achieve preconcentration, cold trapping on a Tenax sorbent followed by flash desorption was applied. Adequate retention and separation were achieved isothermally at 35 degrees C on a thick-film capillary column. Sample preparation was kept to a strict minimum and involved simply adding 2.5 microL of a liquid solution of 1,1,2-trichlorotrifluoroethane in t-butyl-methylether as an internal standard to aliquots of blood in a capped vial. Standards were created by volumetric dilution departing from a gravimetrically prepared calibration gas mixture composed of 0.3% of n-propane, 0.7% of iso-butane, and 0.8% of n-butane in nitrogen. In the forensic blood sample, the following concentrations were measured: 90.0 microg/L for n-propane, 246 microg/L for iso-butane, and 846 microg/L for n-butane.

Water-compatible molecularly imprinted polymers for efficient direct injection on-line solid-phase extraction of ropivacaine and bupivacaine from human plasma.

PubMed

Cobb, Zoe; Sellergren, Börje; Andersson, Lars I

2007-12-01

Two novel molecularly imprinted polymers (MIPs) selected from a combinatorial library of bupivacaine imprinted polymers were used for selective on-line solid-phase extraction of bupivacaine and ropivacaine from human plasma. The MIPs were prepared using methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linking monomer and in addition hydroxyethylmethacrylate to render the polymer surface hydrophilic. The novel MIPs showed high selectivity for the analytes and required fewer and lower concentrations of additives to suppress non-specific adsorption compared with a conventional MIP. This enabled the development of an on-line system for direct extraction of buffered plasma. Selective extraction was achieved without the use of time-consuming solvent switch steps, and transfer of the analytes from the MIP column to the analytical column was carried out under aqueous conditions fully compatible with reversed-phase LC gradient separation of analyte and internal standard. The MIPs showed excellent aqueous compatibility and yielded extractions with acceptable recovery and high selectivity.

Laboratory Information Bulletin: Quantitation of Aflatoxin M1 in Bovine Milk by Liquid Chromatography with Fluorescence Detection.

PubMed

Vega, Victor A; Young, Michelle; Todd, Sarah

2016-01-01

An extraction for aflatoxin M1 from bovine milk samples is described. The samples were extracted by adding 10 mL acetonitrile to 10 g of sample. The extract was salted out with sodium chloride and magnesium sulfate to separate the water and acetonitrile. The organic layer was dried down and reconstituted in water before being subjected to an immunoaffinity column for cleanup. Once the analyte was isolated, quantitation was obtained by LC with fluorescence detection. LC/fluorescence parameters were optimized with an Agilent Poroshell 120 C18 LC column resulting in a 4 min run time. To test the procedure's robustness, three different kinds of matrixes were fortified at three different levels each. Whole milk, reduced fat milk, and skim milk samples were fortified at approximately 0.25, 0.5, and 1.0 μg/kg. Recoveries from all samples ranged from 70 to 100%. Confirmation was accomplished by injecting the samples in an ion trap mass spectrometer. The method presented here entails an extraction step followed by an immunoaffinity column clean-up that leads to fast analysis time and consistent recoveries with an uncertainty measurement of 10.5% and method detection limit of less than 0.011 μg/kg.

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

PubMed

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

2013-02-01

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

Detection of phytoconstituents in column fractions of n-hexane extract of Goldcrest honey exhibiting anti-Helicobacter pylori activity.

PubMed

Manyi-Loh, Christy E; Clarke, Anna M; Ndip, Roland N

2012-04-01

Alternative therapy for Helicobacter pylori eradication from natural products is gaining much attention. This study sought to isolate and characterize the fraction responsible for the antibacterial activity in Goldcrest (GC) n-hexane extract. Thin-layer chromatography (TLC) of the extract was carried out on Silica gel plates to determine the presence of chemical compounds, which were separated and partially purified by column chromatography. The obtained fractions GCCL, GCF2, GCF3 and GCF4 were tested for anti-H. pylori activity using the broth microdilution method. Volatile compounds in the active fractions were identified by gas chromatography-mass spectrometry (GC-MS) analysis. MINITAB was used for statistical analysis at 95% confidence interval. The best antibacterial activity was exhibited by GCF3 (5 mg/mL), which was composed of many compounds with known antimicrobial and antioxidant properties. A total of 16 volatile compounds were identified from fractions GCF2, GCF3 and GCF4 into the following families; alcohol, ketone, aliphatic acid, benzene compound, hydrocarbon, furan and pyran derivatives. The demonstration of antibacterial activity by the column fractions of GC n-hexane extract may provide new lead molecules that could serve as selective agents for H. pylori chemotherapy and control. Copyright © 2012 IMSS. Published by Elsevier Inc. All rights reserved.

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

USGS Publications Warehouse

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

2004-01-01

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

Bioactive phenolic derivatives from Acaena splendens methanol extract.

PubMed

Backhouse, N; Delporte, C; Negrete, R; Feliciano, S A San; López-Pérez, J L

2002-09-01

Acaena splendens H. et A. has been used in Chilean folk medicine for the treatment of fever and inflammation. A description of the in vivo reduction of bacterial pyrogen-induced fever in rabbits and carrageenan-induced paw oedema in guinea pigs is presented. The methanol extract named ME-1, obtained after succesive extractions with petroleum ether and dichloromethane, showed a strong antipyretic action (45.7% of effect), though the antiinflammatory activity was only observed after submitting this extract to column fractionation, giving a crude mixture of flavonoids named C4 with both activities (55.7% and 98.9% of antiinflammatory and antipyretic effect respectively at a dose of 600 mg/kg). The bioassay-guided fractionation by column chromatography afforded the active fraction, which contained (-,-)-epicatechin, tiliroside, 7-O-acetyl-3-O-beta-D-glucosyl-kaempferol and 7-beta-D-glucosyloxy-5-hydroxy-chromone. Copyright 2002 John Wiley & Sons, Ltd.

Ultrasound-assisted analyte extraction for the determination of sulfate and elemental sulfur in zinc sulfide by different liquid chromatography techniques.

PubMed

Dash, K; Thangavel, S; Krishnamurthy, N V; Rao, S V; Karunasagar, D; Arunachalam, J

2005-04-01

The speciation and determination of sulfate (SO4(2-)) and elemental sulfur (S degree) in zinc sulfide (ZnS) using ion-chromatography (IC) and reversed-phase liquid chromatography (RPLC) respectively is described. Three sample pretreatment approaches were employed with the aim of determining sulfate: (i) conventional water extraction of the analyte; (ii) solid-liquid aqueous extraction with an ultrasonic probe; and (iii) elimination of the zinc sulfide matrix via ion-exchange dissolution (IED). The separation of sulfate was carried out by an anion-exchange column (IonPac AS17), followed by suppressed conductivity detection. Elemental sulfur was extracted ultrasonically from the acid treated sample solution into chloroform and separated on a reversed phase HPLC column equipped with a diode array detector (DAD) at 264 nm. The achievable solid detection limits for sulfate and sulfur were 35 and 10 microg g(-1) respectively.

Pressure Bearing Device Affects Extraction Socket Remodeling of Maxillary Anterior Tooth. A Prospective Clinical Trial.

PubMed

Jiang, Xi; Zhang, Yu; Chen, Bo; Lin, Ye

2017-04-01

Extraction socket remodeling and ridge preservation strategies have been extensively explored. To evaluate the efficacy of applying a micro-titanium stent as a pressure bearing device on extraction socket remodeling of maxillary anterior tooth. Twenty-four patients with a extraction socket of maxillary incisor were treated with spontaneous healing (control group) or by applying a micro-titanium stent as a facial pressure bearing device over the facial bone wall (test group). Two virtual models obtained from cone beam computed tomography data before extraction and 4 months after healing were 3-dimenionally superimposed. Facial bone wall resorption, extraction socket remodeling features and ridge width preservation rate were determined and compared between the groups. Thin facial bone wall resulted in marked resorption in both groups. The greatest palatal shifting distance of facial bone located at the coronal level in the control group, but middle level in the test group. Compared with the original extraction socket, 87.61 ± 5.88% ridge width was preserved in the test group and 55.09 ± 14.46% in the control group. Due to the facial pressure bearing property, the rigid micro-titanium stent might preserve the ridge width and alter the resorption features of extraction socket. © 2016 Wiley Periodicals, Inc.

Rapid trace level determination of sulfonamide residues in honey with online extraction using short C-18 column by high-performance liquid chromatography with fluorescence detection.

PubMed

Sajid, Muhammad; Na, Na; Safdar, Muhammad; Lu, Xin; Ma, Lin; He, Lan; Ouyang, Jin

2013-11-01

A sensitive and inexpensive quantification method with online extraction using a short C-18 column for sulfonamide residues in honey by high performance liquid chromatography with fluorescence detector was developed and validated. In sample preparation, acid hydrolysis was used to break the N-glycoside bond between the honey sugar and sulfonamide drugs and derivatization of sulfonamide residues with fluorescamine was conducted at pH 3.5 using a citrate buffer (0.5M) in the honey matrix. The chromatography was carried out on Zorbax Extended C-18 (250mm×4.6mm; 5μm) column, using a mixture of acetonitrile and an acetate buffer (pH 4.50, 20mM) as a mobile phase. A Zorbax Extended C-18 (12mm×4.6mm; 5μm) column was used for online extraction of fifteen sulfonamide residues from honey sample with the help of a two position valve. The limit of quantification of sulfonamide residues in honey was less than 3ngg(-1), and the percentage recovery of study compounds in spiked honey sample was from 80% for sulfacetamide to 100% of sulfachloropyridazine. The developed method has excellent linearity for all studied sulfonamides with a correlation coefficient 0.993. Copyright © 2013 Elsevier B.V. All rights reserved.

Anti-inflammatory effect of bee pollen ethanol extract from Cistus sp. of Spanish on carrageenan-induced rat hind paw edema.

PubMed

Maruyama, Hiroe; Sakamoto, Takashi; Araki, Yoko; Hara, Hideaki

2010-06-23

Bee pollen, a honeybee product, is the feed for honeybees prepared themselves by pollens collecting from plants and has been consumed as a perfect food in Europe, because it is nutritionally well balanced. In this study, we aimed to investigate the anti-inflammatory effect of bee pollen from Cistus sp. of Spanish origin by a method of carrageenan-induced paw edema in rats, and to investigate the mechanism of anti-inflammatory action and also to elucidate components involved in bee pollen extracted with ethanol. The bee pollen bulk, its water extract and its ethanol extract were administered orally to rats. One hour later, paw edema was produced by injecting of 1% solution of carrageenan, and paw volume was measured before and after carrageenan injection up to 5 h. The ethanol extract and water extract were measured COX-1 and COX-2 inhibitory activities using COX inhibitor screening assay kit, and were compared for the inhibition of NO production in LPS-stimulated RAW 264.7 cells. The constituents of bee pollen were purified from the ethanol extract subjected to silica gel or LH-20 column chromatography. Each column chromatography fractions were further purified by repeated ODS or silica gel column chromatography. The bee pollen bulk mildly suppressed the carrageenan-induced paw edema and the water extract showed almost no inhibitory activity, but the ethanol extract showed relatively strong inhibition of paw edema. The ethanol extract inhibited the NO production and COX-2 but not COX-1 activity, but the water extract did not affect the NO production or COX activities. Flavonoids were isolated and purified from the ethanol extract of bee pollen, and identified at least five flavonoids and their glycosides. It is suggested that the ethanol extract of bee pollen show a potent anti-inflammatory activity and its effect acts via the inhibition of NO production, besides the inhibitory activity of COX-2. Some flavonoids included in bee pollen may partly participate in some of the anti-inflammatory action. The bee pollen would be beneficial not only as a dietary supplement but also as a functional food.

Anti-inflammatory effect of bee pollen ethanol extract from Cistus sp. of Spanish on carrageenan-induced rat hind paw edema

PubMed Central

2010-01-01

Background Bee pollen, a honeybee product, is the feed for honeybees prepared themselves by pollens collecting from plants and has been consumed as a perfect food in Europe, because it is nutritionally well balanced. In this study, we aimed to investigate the anti-inflammatory effect of bee pollen from Cistus sp. of Spanish origin by a method of carrageenan-induced paw edema in rats, and to investigate the mechanism of anti-inflammatory action and also to elucidate components involved in bee pollen extracted with ethanol. Methods The bee pollen bulk, its water extract and its ethanol extract were administered orally to rats. One hour later, paw edema was produced by injecting of 1% solution of carrageenan, and paw volume was measured before and after carrageenan injection up to 5 h. The ethanol extract and water extract were measured COX-1 and COX-2 inhibitory activities using COX inhibitor screening assay kit, and were compared for the inhibition of NO production in LPS-stimulated RAW 264.7 cells. The constituents of bee pollen were purified from the ethanol extract subjected to silica gel or LH-20 column chromatography. Each column chromatography fractions were further purified by repeated ODS or silica gel column chromatography. Results The bee pollen bulk mildly suppressed the carrageenan-induced paw edema and the water extract showed almost no inhibitory activity, but the ethanol extract showed relatively strong inhibition of paw edema. The ethanol extract inhibited the NO production and COX-2 but not COX-1 activity, but the water extract did not affect the NO production or COX activities. Flavonoids were isolated and purified from the ethanol extract of bee pollen, and identified at least five flavonoids and their glycosides. Conclusions It is suggested that the ethanol extract of bee pollen show a potent anti-inflammatory activity and its effect acts via the inhibition of NO production, besides the inhibitory activity of COX-2. Some flavonoids included in bee pollen may partly participate in some of the anti-inflammatory action. The bee pollen would be beneficial not only as a dietary supplement but also as a functional food. PMID:20573205

Effects of 4-nonylphenol on benthic macroinvertebrates and insect emergence in littoral enclosures

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

Schmude, K.L.; Liber, K.; Corry, T.D.

1999-03-01

The effect of 4-nonylphenol (NP) on benthic, freshwater macroinvertebrates in littoral enclosures was evaluated over a 2-year period. Enclosures received 11 NP applications, 48 h apart, with nominal rates of 3, 30, 100, and 300 {micro}g/L. Mean measured peak concentrations in integrated water column samples over the 20-d application period were 5 {+-} 4, 23 {+-} 11, 76 {+-} 21, and 243 {+-} 41 {micro}g/L NP. Concentrations of NP in the water column decreased rapidly after the last application. Maximum NP concentrations measured in sediments, pore water, and macrophytes of a 300-{micro}g/L enclosure were 27.4 mg/kg, 29.9 {micro}g/L, and 89.6more » mg/kg, respectively. The most abundant macroinvertebrate groups, Chironomidae, Oligochaeta, and Mollusca, decreased in abundance after application. Effects on Mollusca were the most severe. Their numbers were significantly reduced at the highest treatment throughout most of the study. Oligochaetes and chironomids were also significantly reduced at the highest treatment, but populations recovered within 6 weeks. Snails and naidid oligochaetes were slightly affected at the second highest treatment (76 {+-} 21 {micro}g/L NP). Insect emergence was reduced during and immediately post-application, but the effects were likely caused or compounded by a surfactant sheen on the surface of the water that interfered with emergence and/or oviposition. The observed effects on the benthic community were most likely due to exposure from the water, although more persistent macrophyte-associated residues may have contributed to effects on Gastropoda, Naididae, and Tanytarsini. Macrophyte-associated NP residues may pose a small risk to benthic organisms, but it is probably minor compared to water exposures. The no-observed and lowest-observed-effect concentration for the benthic community was 23 {+-} 11 and 76 {+-} 21 {micro}g/L NP, respectively.« less

Column chromatography as a useful step in purification of diatom pigments.

PubMed

Tokarek, Wiktor; Listwan, Stanisław; Pagacz, Joanna; Leśniak, Piotr; Latowski, Dariusz

2016-01-01

Fucoxanthin, diadinoxanthin and diatoxanthin are carotenoids found in brown algae and most other heterokonts. These pigments are involved in photosynthetic and photoprotective reactions, and they have many potential health benefits. They can be extracted from diatom Phaeodactylum tricornutum by sonication, extraction with chloroform : methanol and preparative thin layer chromatography. We assessed the utility of an additional column chromatography step in purification of these pigments. This novel addition to the isolation protocol increased the purity of fucoxanthin and allowed for concentration of diadinoxanthin and diatoxanthin before HPLC separation. The enhanced protocol is useful for obtaining high purity pigments for biochemical studies.

Isolation of atropine and scopolamine from plant material using liquid-liquid extraction and EXtrelut® columns.

PubMed

Śramska, Paula; Maciejka, Artur; Topolewska, Anna; Stepnowski, Piotr; Haliński, Łukasz P

2017-02-01

Tropane alkaloids are toxic secondary metabolites produced by Solanaceae plants. Among them, plants from Datura genus produce significant amounts of scopolamine and hyoscyamine; the latter undergoes racemization to atropine during isolation. Because of their biological importance, toxic properties and commonly reported food and animal feed contamination by different Datura sp. organs, there is a constant need for reliable methods for the analysis of tropane alkaloids in many matrices. In the current study, three extraction and sample-clean up procedures for the determination of scopolamine and atropine in plant material were compared in terms of their effectiveness and repeatability. Standard liquid-liquid extraction (LLE) and EXtrelut ® NT 3 columns were used for the sample clean-up. Combined ultrasound-assisted extraction and 24h static extraction using ethyl acetate, followed by multiple LLE steps was found the most effective separation method among tested. However, absolute extraction recovery was relatively low and reached 45-67% for atropine and 52-73% for scopolamine, depending on the compound concentration. The same method was also the most effective one for the isolation of target compounds from Datura stramonium leaves. EXtrelut ® columns, on the other hand, displayed relatively low effectiveness in isolating atropine and scopolamine from such a complex matrix and hence could not be recommended. The most effective method was also applied to the extraction of alkaloids from roots and stems of D. stramonium. Quantitative analyses were performed using validated method based on gas chromatography with flame ionization detector (GC-FID). Based on the results, the importance of the proper selection of internal standards in the analysis of tropane alkaloids was stressed out. Copyright © 2016 Elsevier B.V. All rights reserved.

Acaricidal activity of petroleum ether extract of neem (Azadirachta indica) oil and its four fractions separated by column chromatography against Sarcoptes scabiei var. cuniculi larvae in vitro.

PubMed

Deng, Yunxia; Shi, Dongxia; Yin, Zhongqiong; Guo, Jianhong; Jia, Renyong; Xu, Jiao; Song, Xu; Lv, Cheng; Fan, Qiaojia; Liang, Xiaoxia; Shi, Fei; Ye, Gang; Zhang, Wei

2012-04-01

The petroleum ether extract of neem oil and its four fractions separated by column chromatography was diluted at different concentrations with liquid paraffin. The acaricidal bioassay was conducted using a dipping method. The results indicated that the median lethal concentration (LC50) of the petroleum ether extract (at the concentration of 500.0ml/l) was 70.9ml/l, 24h after treatment. At concentrations of 500.0, 250.0, 125.0, 62.5 and 31.2ml/l, the median lethal times (LT50) of the petroleum ether extract were 8.7, 8.8, 10.8, 11.5 and 13.1h, respectively. Thin-layer chromatography (TLC) showed that the petroleum ether extract of neem oil separated into four fractions (F1-F4). Acaricidal activity of 68.3% and 100.0% in the F2 and F4 was confirmed. These results suggest that petroleum ether extracts of neem oil and its four fractions possess useful acaricidal activity in vitro. Copyright © 2012 Elsevier Inc. All rights reserved.

Rapid determination of benzo(a)pyrene in roasted coffee and coffee brew by high-performance liquid chromatography with fluorescence detection

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

de Kruijf, N.; Schouten, T.; van der Stegen, G.H.D.

A rapid and reliable analytical method is presented for the determination of trace amounts of benzo(a)pyrene in roasted coffee, coffee brew, and spent grounds. Roasted coffee and spent grounds were extracted with acetone, followed by saponification and cyclohexane extraction. Coffee brew was extracted three times with cyclohexane, and the combined extracts were purified by chromatography on a silica gel column. The extracts were analyzed by HPLC with a 5-..mu..m Vydac reversed-phase 201 TPB 5 column and fluorescence detection under isocratic conditions. The benzo(a)pyrene levels in 55 roasted coffee samples, commercially available in the Netherlands, ranged from not detectable (<0.1 ..mu..g/kg)more » to 0.5 ..mu..g/kg. Coffee brews were prepared by two different methods from an over-roasted coffee sample with an elevated benzo(a)pyrene level of 2 ..mu..g/kg. These brews yielded benzo(a)pyrene contents of approximately 1 ng/L, indicating benzo(a)pyrene extraction yields of about 1% for both coffee preparation methods.« less

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

PubMed

Ligocka, D; Lison, D; Haufroid, V

2002-10-05

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

Isolation and purification of diastereoisomeric flavonolignans from silymarin by binary-column recycling preparative high-performance liquid chromatography.

PubMed

Zhao, Weiquan; Yang, Guang; Zhong, Fanyi; Yang, Nan; Zhao, Xin; Qi, Yunpeng; Fan, Guorong

2014-09-01

Silymarin extracted from Silybum marianum (L.) Gaertn consists of a large number of flavonolignans, of which diastereoisomeric flavonolignans including silybin A and silybin B, and isosilybin A and isosilybin B are the main bioactive components, whose preparation from the crude extracts is still a difficult task. In this work, binary-column recycling preparative high-performance liquid chromatography systems without sample loop trapping, where two columns were switched alternately via one or two six-port switching valves, were established and successfully applied to the isolation and purification of the four diastereoisomeric flavonolignans from silymarin. The proposed system showed significant advantages over conventional preparative high-performance liquid chromatography with a single column in increasing efficiency and reducing the cost. To obtain the same amounts of products, the proposed system spends only one tenth of the time that the conventional system spends, and needs only one eleventh of the solvent that the conventional system consumes. Using the proposed system, the four diastereoisomers were successfully isolated from silymarin with purities over 98%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Tagiri-Endo, Misako; Suzuki, Shigeru; Nakamura, Tomoyuki; Hatakeyama, Takashi; Kawamukai, Kazuo

2009-02-01

A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 microl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01-0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.

Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

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

Owens, J; Hok, S; Alcaraz, A

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limitmore » of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.« less

Normal incidence x-ray mirror for chemical microanalysis

DOEpatents

Carr, M.J.; Romig, A.D. Jr.

1987-08-05

An x-ray mirror for both electron column instruments and micro x-ray fluorescence instruments for making chemical, microanalysis comprises a non-planar mirror having, for example, a spherical reflecting surface for x-rays comprised of a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on a substrate and whose layers have a thickness which is a multiple of the wavelength being reflected. For electron column instruments, the wavelengths of interest lie above 1.5nm, while for x-ray fluorescence instruments, the range of interest is below 0.2nm. 4 figs.

Dynamic fractionation of trace metals in soil and sediment samples using rotating coiled column extraction and sequential injection microcolumn extraction: a comparative study.

PubMed

Rosende, Maria; Savonina, Elena Yu; Fedotov, Petr S; Miró, Manuel; Cerdà, Víctor; Wennrich, Rainer

2009-09-15

Dynamic fractionation has been recognized as an appealing alternative to conventional equilibrium-based sequential extraction procedures (SEPs) for partitioning of trace elements (TE) in environmental solid samples. This paper reports the first attempt for harmonization of flow-through dynamic fractionation using two novel methods, the so-called sequential injection microcolumn (SIMC) extraction and rotating coiled column (RCC) extraction. In SIMC extraction, a column packed with the solid sample is clustered in a sequential injection system, while in RCC, the particulate matter is retained under the action of centrifugal forces. In both methods, the leachants are continuously pumped through the solid substrates by the use of either peristaltic or syringe pumps. A five-step SEP was selected for partitioning of Cu, Pb and Zn in water soluble/exchangeable, acid-soluble, easily reducible, easily oxidizable and moderately reducible fractions from 0.2 to 0.5 g samples at an extractant flow rate of 1.0 mL min(-1) prior to leachate analysis by inductively coupled plasma-atomic emission spectrometry. Similarities and discrepancies between both dynamic approaches were ascertained by fractionation of TE in certified reference materials, namely, SRM 2711 Montana Soil and GBW 07311 sediment, and two real soil samples as well. Notwithstanding the different extraction conditions set by both methods, similar trends of metal distribution were in generally found. The most critical parameters for reliable assessment of mobilizable pools of TE in worse-case scenarios are the size-distribution of sample particles, the density of particles, the content of organic matter and the concentration of major elements. For reference materials and a soil rich in organic matter, the extraction in RCC results in slightly higher recoveries of environmentally relevant fractions of TE, whereas SIMC leaching is more effective for calcareous soils.

Heat integrated ethanol dehydration flowsheets

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

Hutahaean, L.S.; Shen, W.H.; Brunt, V. Van

1995-04-01

zA theoretical evaluation of heat-integrated heterogeneous-azeotropic ethanol-water distillation flowsheets is presented. Simulations of two column flowsheets using several different hydrocarbon entrainers reveal a region of potential heat integration and substantial reduction in operating energy. In this paper, methods for comparing hydrocarbon entrainers are shown. Two aspects of entrainers are related to operating and capital costs. The binary azeotropic composition of the entrainer-ethanol mixture is related to the energy requirements of the flowsheet. A temperature difference in the azeotrophic column is related to the size of the column and overall process staging requirements. Although the hydrophobicity of an entrainer is essentialmore » for specification of staging in the dehydration column, no substantial increase in operating energy results from an entrainer that has a higher water content. Likewise, liquid-liquid equilibria between several entrainer-ethanol-water mixtures have no substantial effect on either staging or operation. Rather, increasing the alcohol content of the entrainer-ethanol azeotrope limits its recovery in the dehydration column, and increases the recycle and reflux streams. These effects both contribute to increasing the separation energy requirements and reducing the region of potential heat integration. A cost comparison with a multieffect extractive distillation flowsheet reveals that the costs are comparable; however, the extractive distillation flowsheet is more cost effective as operating costs increase.« less

Simultaneous determination of dextrose, sucrose, maltose, and lactose in sausage products by liquid chromatography.

PubMed

Ali, M S

1988-01-01

A liquid chromatographic (LC) method for the simultaneous determination of dextrose, sucrose, maltose, and lactose in sausage products has been developed. Dextrose, sucrose, maltose, and lactose are extracted from comminuted meat products with 52% ethanol. After filtration, the extracts are purified by passing them through a C18 Sep-Pak cartridge and 2 ion exchange resin Econo-columns in series. After concentration and filtration, extracts are analyzed by LC using a normal phase amino column and a differential refractometer detector. Homogeneously ground samples of cooked and fresh sausages are fortified with dextrose, sucrose, maltose, and lactose at 4 different concentrations. Average recovery for dextrose, sucrose, maltose, and lactose at all 4 levels of fortification was greater than 80% with a coefficient of variation less than 10%.

Extreme degree of ionization in homogenous micro-capillary plasma columns heated by ultrafast current pulses.

PubMed

Avaria, G; Grisham, M; Li, J; Tomasel, F G; Shlyaptsev, V N; Busquet, M; Woolston, M; Rocca, J J

2015-03-06

Homogeneous plasma columns with ionization levels typical of megaampere discharges are created by rapidly heating gas-filled 520-μm-diameter channels with nanosecond rise time current pulses of 40 kA. Current densities of up to 0.3  GA cm^{-2} greatly increase Joule heating with respect to conventional capillary discharge Z pinches, reaching unprecedented degrees of ionization for a high-Z plasma column heated by a current pulse of remarkably low amplitude. Dense xenon plasmas are ionized to Xe^{28+}, while xenon impurities in hydrogen discharges reach Xe^{30+}. The unique characteristics of these hot, ∼300:1 length-to-diameter aspect ratio plasmas allow the observation of unexpected spectroscopic phenomena. Axial spectra show the unusual dominance of the intercombination line over the resonance line of He-like Al by nearly an order of magnitude, caused by differences in opacities in the axial and radial directions. These plasma columns could enable the development of sub-10-nm x-ray lasers.

Rapid, economical qualitative method for separation of aflatoxins B-1, B-2 & G-1, G-2 by dry column chromatography.

PubMed

Megalla, S E

1983-12-01

A good correlation of four components of aflatoxins was accomplished by using the dry column chromatography method. The decolorization process of interfering substances, by 0.01 N KOH and defatting the extract with petroleum ether yields a clean residue for DCC separation. It is clear that the dry column chromatography is a very simple and time-saving procedure for separation of aflatoxins. DCC columns are more economical than precoated 'thick layer' preparative plates and, in DCC, no large developing tanks need to be used. Hazards associated with the use of large volumes of flammable solvents are greatly reduced.

Ballistic missile precession frequency extraction by spectrogram's texture

NASA Astrophysics Data System (ADS)

Wu, Longlong; Xu, Shiyou; Li, Gang; Chen, Zengping

2013-10-01

In order to extract precession frequency, an crucial parameter in ballistic target recognition, which reflected the kinematical characteristics as well as structural and mass distribution features, we developed a dynamic RCS signal model for a conical ballistic missile warhead, with a log-norm multiplicative noise, substituting the familiar additive noise, derived formulas of micro-Doppler induced by precession motion, and analyzed time-varying micro-Doppler features utilizing time-frequency transforms, extracted precession frequency by measuring the spectrogram's texture, verified them by computer simulation studies. Simulation demonstrates the excellent performance of the method proposed in extracting the precession frequency, especially in the case of low SNR.

Study of Pulsed Columns with the System. Uranyl Nitrate-Nitric Acid-Water- Tributylphosphate; ETUDE DES COLONNES A PULSATIONS A L'AIDE DU SYSTEME NITRATE D'URANYLE-ACIDE NITRIQUEEAU-TRIBUTYLPHOSPHATE

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

Durandet, J.; Defives, D.; Choffe, B.

1959-10-31

The performsnce of a pulsed column with perforated plates was studied with the aid of a uranyl nitrate-nitric acid --water --tributyl phosphate system. The extraction of uranium from an aqueous acidic solution by an organic solvent and the extraction of uranium from organic solutions by water were the two cases investigated. The variation of the efficiency and the capacity of the pulsed column was determined as a function of the pulse amplitude and frequency, of the total flow rate, of the diameter of the holes, and of the choice of dispersed phase. The results showed that for a given amplitudemore » and total flow rate the efficiency has a maximum with an increase in frequency. (J.S.R.)« less

Determination of chloramphenicol and zeranols in pig muscle by immunoaffinity column clean-up and LC-MS/MS analysis.

PubMed

Wang, Qing; Zhao, Hua; Xi, Cunxian; Wang, Guomin; Chen, Dongdong; Ding, Shijia

2014-01-01

An immunoaffinity column clean-up and LC-MS/MS method was successfully developed for simultaneous determination of chloramphenicol, zearalanone, α-zearalanol, β-zearalanol, zearalenone, α-zearalenol and β-zearalenol in pig muscle. The sample was extracted with diethyl ether after enzymatic digestion by β-glucuronidase/sulfatase. The extracted solution was evaporated to dryness and the residue was then dissolved in 1 ml of 50% acetonitrile solution. After filtration and dilution with phosphate buffer solution (PBS), the reconstituted solution was cleaned-up with an IAC-CZ immunoaffinity column and then analysed by HPLC-MS/MS. The established method were validated by linearity (r ≥ 0.9990), precision (RSD ≥ 2.9%), average recovery (74.5-105.0%) and limit of detection (0.04-0.10 μg kg(-1)). The developed method is rapid, reliable, sensitive, accurate and has good applicability for real samples.

A PROCESS FOR SEPARATING AZEOTROPIC MIXTURES BY EXTRACTIVE AND CONVECTIVE DISTILLATION

DOEpatents

Frazer, J.W.

1961-12-19

A method is described for separating an azeotrope of carbon tetrachloride and 1,1,2,2-tetrafluorodinitroethane boiling at 60 deg C. The ndethod comnprises, specifically, feeding azeotrope vapors admixed with a non- reactive gas into an extractive distillation column heated to a temperature preferably somewhat above the boiling point of the constant boiling mixture. A solvent, di-n-butylphthalate, is metered into the column above the gas inlet and permitted to flow downward, earrying with it the higher bomling fraction, while the constituent having the lower boiling point passes out of the top of the column with the non-reactive gas and is collected in a nitrogen cold trap. Other solvents which alter the vapor pressure relationship may be substituted. The method is generally applicable to azeotropic mixtures. A number of specific mixtures whicb may be separated are disclosed. (AEC)

Analysis of the reaction products from micro-vial pyrolysis of the mixture glucose/proline and of a tobacco leaf extract:Search for Amadori intermediates.

PubMed

Mitsui, Kazuhisa; David, Frank; Tienpont, Bart; Sandra, Koen; Ochiai, Nobuo; Tamura, Hirotoshi; Sandra, Pat

2015-11-27

Micro-vial pyrolysis (PyroVial) was used to study the production of compounds important for the aroma of heat-treated natural products such as tobacco. Firstly, a mixture of glucose and proline was pyrolyzed as model, as this sugar and amino acid are also abundant in tobacco leaf (Nicotiana tobacum L.). The pyrolysate was analyzed using headspace-GC–MS, liquid injection GC–MS and LC–MS. Next, micro-vial pyrolysis in combination with LC–MS was applied to tobacco leaf extract. Using MS deconvolution, molecular feature extraction and differential analysis it was possible to identify Amadori intermediates of the Maillard reaction in the tobacco leaf extract. The intermediate disappeared as was the case for 1-deoxy-1-prolino-β-d-fructose or the concentration decreased in the pyrolysate compared to the original extract such as for the 1-deoxy-1-[2-(3-pyridyl)-1-pyrrolidinyl]-β-d-fructose isomers indicating that Amadori intermediates are important precursors for aroma compound formation.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of organophosphate pesticides in filtered water by gas chromatography with flame photometric detection

USGS Publications Warehouse

Jha, Virendra K.; Wydoski, Duane S.

2002-01-01

A method for the isolation of 20 parent organophosphate pesticides and 5 pesticide degradates from filtered natural-water samples is described. Seven of these compounds are reported permanently with an estimated concentration because of performance issues. Water samples are filtered to remove suspended particulate matter, and then 1 liter of filtrate is pumped through disposable solid-phase extraction columns that contain octadecyl-bonded porous silica to extract the compounds. The C-18 columns are dried with nitrogen gas, and method compounds are eluted from the columns with ethyl acetate. The extract is analyzed by dual capillary-column gas chromatography with flame photometric detection. Single-operator method detection limits in all three water-matrix samples ranged from 0.004 to 0.012 microgram per liter. Method performance was validated by spiking all compounds into three different matrices at three different concentrations. Eight replicates were analyzed at each concentration level in each matrix. Mean recoveries of method compounds spiked in surface-water samples ranged from 39 to 149 percent and those in ground-water samples ranged from 40 to 124 percent for all pesticides except dimethoate. Mean recoveries of method compounds spiked in reagent-water samples ranged from 41 to 119 percent for all pesticides except dimethoate. Dimethoate exhibited reduced recoveries (mean of 43 percent in low- and medium-concentration level spiked samples and 20 percent in high-concentration level spiked samples) in all matrices because of incomplete collection on the C-18 column. As a result, concen-trations of dimethoate and six other compounds (based on performance issues) in samples are reported in this method with an estimated remark code.

HPLC-MS-MS Determination of ZCZ-011, A Novel Pharmacological Tool for Investigation of the Cannabinoid Receptor in Mouse Brain Using Clean Screen FASt™ Column Extraction.

PubMed

Poklis, Justin L; Clay, Deborah J; Ignatowska-Jankowska, Bogna M; Zanato, Chiara; Ross, Ruth A; Greig, Iain R; Abdullah, Rehab A; Mustafa, Mohammed A; Lichtman, Aron H; Poklis, Alphonse

2015-06-01

A high-performance liquid chromatography tandem mass spectrometry method was developed for the detection and quantification of 6-methyl-3-(2-nitro-1-(thiophen-2-yl)propyl)-2-phenyl-1H-indole (ZCZ-011) using 2-phenylindole as the internal standard (ISTD). ZCZ-011 was synthesized as a possible positive allosteric modulator with the CB1 cannabinoid receptor. The analytical method employs a rapid extraction technique using Clean Screen FASt™ columns with a Positive Pressure Manifold. FASt™ columns were originally developed for urine drug analysis but we have successfully adapted them to the extraction of brain tissue. Chromatographic separation was performed on a Restek Allure Biphenyl 5 µ, 100 × 3.2 mm column (Bellefonte, PA). The mobile phase consisted of 1:9 deionized water with 10 mmol ammonium acetate and 0.1% formic acid-methanol. The following transition ions (m/z) were monitored for ZCZ-011: 363 > 207 and 363 > 110 and for the ISTD: 194 > 165 and 194 > 89. The FASt™ columns lowered and stabilized the ion suppression over the linear range of the assay (40-4,000 ng/g). The method was evaluated for recovery, ion suppression, accuracy/bias, intraday and interday precision, bench-top stability, freeze-thaw and post-preparative stability. The method was successfully applied to brain tissue from C57BL/6J mice that received intraperitoneal (i.p.) injections with 40 mg/kg of ZCZ-011 or vehicle. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Ionization Electron Signal Processing in Single Phase LArTPCs II. Data/Simulation Comparison and Performance in MicroBooNE

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

Adams, C.; et al.

The single-phase liquid argon time projection chamber (LArTPC) provides a large amount of detailed information in the form of fine-grained drifted ionization charge from particle traces. To fully utilize this information, the deposited charge must be accurately extracted from the raw digitized waveforms via a robust signal processing chain. Enabled by the ultra-low noise levels associated with cryogenic electronics in the MicroBooNE detector, the precise extraction of ionization charge from the induction wire planes in a single-phase LArTPC is qualitatively demonstrated on MicroBooNE data with event display images, and quantitatively demonstrated via waveform-level and track-level metrics. Improved performance of inductionmore » plane calorimetry is demonstrated through the agreement of extracted ionization charge measurements across different wire planes for various event topologies. In addition to the comprehensive waveform-level comparison of data and simulation, a calibration of the cryogenic electronics response is presented and solutions to various MicroBooNE-specific TPC issues are discussed. This work presents an important improvement in LArTPC signal processing, the foundation of reconstruction and therefore physics analyses in MicroBooNE.« less

Evaluation of cytotoxic and mutagenic effects of Coriolus versicolor and Funalia trogii extracts on mammalian cells.

PubMed

Unyayar, Ali; Demirbilek, Murat; Turkoglu, Melisa; Celik, Ayla; Mazmanci, Mehmet A; Erkurt, Emrah A; Unyayar, Serpil; Cekic, Ozlem; Atacag, Hatice

2006-01-01

This study examined the in vitro cytotoxic activities of standardized aqueous bioactive extracts prepared from Coriolus versicolor and Funalia trogiiATCC 200800 on HeLa and fibroblast cell lines using a MTT (3-[4,5-dimetiltiazol-2-]-2-5-difeniltetrazolium bromide) cytotoxicity assay. F. trogii and C. versicolor extracts were cytotoxic to both cell lines. At 10 microL treatment level, F. trogii and C. versicolor extracts inhibited proliferation of HeLa cancer cells by 71.5% and 45%, respectively, compared with controls. Toxicity was lower toward normal fibroblasts. In the latter case, treatment at 10 microL level with F. trogii and C. versicolor extracts reduced cell proliferation by 51.3% and 38.7%, respectively. In separate experiments, the mitotic index (MI) obtained with 3 microL treatment level of unheated extracts of the two fungi was comparable to the MI value obtained by treatment with 4 microg/mL MMC (anticancer agent mitomycin-C). A significant induction of sister chromatid exchange (SCE) was observed in normal cultured lymphocytes treated with MMC (4 microg/mL). MMC treatment reduced replication index compared with treatment with unheated F. trogii extract and negative controls (p < 0.001). In contrast to MMC, F. trogii extracts did not affect the proliferation of human lymphocytes compared with controls (p > 0.05). Laccase and peroxidase enzyme activities in F. trogii extract were implicated in their inhibitory effect on cancer cells. F. trogii extract was concluded to have antitumor activity.

Developing Inquiry-Based Labs Using Micro-Column Chromatography

ERIC Educational Resources Information Center

Barden-Gabbei, Laura M.; Moffitt, Deborah L.

2006-01-01

Chromatography is a process by which mixtures can be separated or substances can be purified. Biological and chemical laboratories use many different types of chromatographic processes. For example, the pharmaceutical industry uses chromatographic techniques to purify drugs, medical labs use them to identify blood components such as cholesterol,…

Recognizing Excellence: From Macro to Micro to Nano

ERIC Educational Resources Information Center

Dassler, Troy

2011-01-01

This column features profiles of award-winning science programs and teachers. In this month's issue the author shares his experience of working with a university researcher. Third-grade students benefit from this relationship and learn about the nanoscale through up-to-date science equipment. (Contains 1 resource and 10 online resources.)

Dissolution enhancement and mathematical modeling of removal of residual trichloroethene in sands by ozonation during flushing with micro-nano-bubble solution

NASA Astrophysics Data System (ADS)

Sung, Menghau; Teng, Chun-Hao; Yang, Tsung-Hsien

2017-07-01

Soil flushing using micro-nano-sized bubbles (MNB) in water as the flushing solution was tested in laboratory sand columns for the cleanup of residual trichloroethene (TCE) non-aqueous-phase-liquid (NAPL). Experiments considering flushing with MNB as well as ozone MNB (OZMNB) in water to treat soils contaminated with residual TCE liquid were conducted to examine effects of ozone on dissolution enhancement. The degrees of residual TCE saturation in soils, ranging from 0.44% to 7.6%, were tested. During flushings, aqueous TCE concentrations at the column exit were monitored and TCE masses remained in the columns after flushing were determined. Experimental results between runs with MNB and OZMNB in water revealed that dissolution enhancement was dependent on residual saturation conditions, and the maximum enhancement was around 9%. Governing equations consisting of three coupled partial differential equations (PDEs) were developed to model the system, and high-order finite difference (HOFD) method was employed to solve these PDEs. From mathematical modeling of reactive mass transfer under low residual saturation conditions (0.44% and 1.9%), experimental data were simulated and important controlling mechanisms were identified. It was concluded that a specific parameter pertinent to NAPL-water interfacial area in the Sherwood number had to be modified to satisfactorily describe the dissolution of TCE in the presence of MNB in water.

[Rapid determination of 40 pesticide residues in fruits using gas chromatography-mass spectrometry coupled with analyte protectants to compensate for matrix effects].

PubMed

Xu, Xiuli; Zhao, Haixiang; Li, Li; Liu, Hanxia; Ren, Heling; Zhong, Weike

2012-03-01

A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 40 pesticides in fruits. The effects of adding analyte protectants were evaluated for compensating matrix effects and the impacts on the quantitative results. A new combination of analyte protectants - Polyethylene Glycol 400 (PEG 400) and olive oil combination, which can be dissolved in acetone, was used for the quantitative analysis. The pesticides were extracted from fruit samples with acetonitrile and the extracts were cleaned up using micro-solid phase extraction. A GC-MS method in selective ion monitoring (SIM) mode coupled with large volume injection was finally developed. Using the newly developed analyte protectant combination of PEG 400 and olive oil, a good linearity was obtained in the range of 1 - 200 microg/L with coefficients better than 0.99, and the detection limits were between 0.1 - 3.0 microg/L. The mean recoveries of the pesticides were 75% - 119% with the relative standard deviation values less than 16.6% except for dimethoate. The performance of the analyte protectants was compared with matrix-matched standards calibration curves in terms of quantitative accuracy. The results showed that the method of adding analyte protectants can replace the matrix-matched standard calibration, and can also reduce the sample pretreatment. When the devel- oped method was used for the analysis of apple, peache, orange, banana, grape and other fruit samples, a good matrix compensation effect was achieved, and thus effectively reduced the bad effects of the water-soluble agents to the gas chromatographic column.

Solid Phase Micro Extraction (SPME)

NASA Technical Reports Server (NTRS)

1998-01-01

Internation Flavors and Fragrances Inc. proprietary research technology, Solid Phase Micro Extraction (SPME) utilizes a special fiber needle placed directly next to the bloom of the living flower to collect the fragrance molecules. SPME was used in the Space Flower experiment aboard STS-95 space shuttle mission, after which Dr. Braja Mookherjee (left) and Subha Patel of IFF will analyze the effects of gravity on the Overnight Scentsation rose plant.

Polysaccharide peptides from COV-1 strain of Coriolus versicolor inhibit tolbutamide 4-hydroxylation in the rat in vitro and in vivo.

PubMed

Yeung, John H K; Chan, Siu-Lung; Or, Penelope M Y

2006-08-01

Polysaccharide peptide (PSP), isolated from COV-1 strain of Coriolus versicolor, is commonly used as an adjunct in cancer chemotherapy in China. In this study, the effects of whole PSP extract and water extract of PSP on 4-hydroxylation of tolbutamide were investigated in rat liver microsomes in vitro and in vivo in the rat. Both the whole PSP extract and the water soluble fraction (0.5-20 microM) decreased the metabolism of tolbutamide to 4-hydroxytolbutamide in vitro. Enzyme kinetics studies showed that PSP inhibited tolbutamide 4-hydroxylase activity in a competitive, concentration-dependent manner. The whole PSP extract had a Ki value of 12.6 microM and IC50 at 18.4 microM, while the water extract had a Ki value of 6.9 microM and IC50 at 9.8 microM. Sulphaphenazole, a specific human CYP2C9 inhibitor, showed a Ki value of 30.8 microM and IC50 at 44.0 microM in the test system. In the pharmacokinetic studies in vivo, acute PSP (4 micromol/kg, i.p.) treatment did not produce significant changes in tolbutamide clearance, but produced a decrease in the Cinitial (7.4%) and an increase in the Vd (7.4%). Sub-chronic pre-treatment of PSP (1-2 micromol/kg/day, i.p.) for three days did not affect the clearance and AUC of tolbutamide, but the Cinitial was decreased, together with increases in the T1/2, and Vd. The formation of 4-hydroxytolbutamide in vivo was decreased in both acute and sub-chronic studies. Taken together, this study demonstrated the PSP can inhibit tolbutamide 4-hydroxylation both in vitro and in vivo. Despite the fact that CYP isoforms that metabolise tolbutamide are different between rat and human liver due to different catalytic characteristics, and rat studies may not be directly extrapolatable to man, the concomitant use of PSP with other CYP2C substrates should be carefully monitored.

Growth of second stage mineral in Lytechinus variegatus.

PubMed

Stock, S R; Seto, Jong; Deymier, A C; Rack, A; Veis, A

2017-10-30

Purpose and Aims: Sea urchin teeth consist of calcite and form in two stages with different magnesium contents. The first stage structures of independently formed plates and needle-prisms define the shape of the tooth, and the columns of the second stage mineral cements the first stage structures together and control the fracture behavior of the mature tooth. This study investigates the nucleation and growth of the second stage mineral. Scanning electron microscopy (SEM) and synchrotron microComputed Tomography characterized the structures of the second phase material found in developing of Lytechinus variegatus teeth. Although the column development is a continuous process, defining four phases of column formation captures the changes that occur in teeth of L. variegatus. The earliest phase consists of small 1-2 µm diameter hemispheres, and the second of 5-10 µm diameter, mound-like structures with a nodular surface, develops from the hemispheres. The mounds eventually bridge the syncytium between adjacent plates and form hyperboloid structures (phase three) that appear like mesas when plates separate during the fracture. The mesa diameter increases with time until the column diameter is significantly larger than its height, defining the fourth phase of column development. Energy dispersive x-ray spectroscopy confirms that the columns contain more magnesium than the underlying plates; the ratios of magnesium to calcium are consistent with compositions derived from x-ray diffraction. Columns grow from both bounding plates. The presence of first phase columns interspersed among third stage mesas indicates very localized control of mineralization.

Simultaneous determination of three anticonvulsants using hydrophilic interaction LC-MS.

PubMed

Oertel, Reinhard; Arenz, Norman; Pietsch, Jörg; Kirch, Wilhelm

2009-01-01

A specific and automated method was developed to quantify the anticonvulsants gabapentin, pregabalin and vigabatrin simultaneously in human serum. Samples were prepared with a protein precipitation. The hydrophilic interaction chromatography (HILIC) with a mobile phase gradient was used to divide off ions of the matrix and for separation of the analytes. Four different HILIC-columns and two different column temperatures were tested. The Tosoh-Amid column gave the best results: single small peaks. The anticonvulsants were detected in the multiple reaction monitoring mode (MRM) with ESI-MS-MS. Using a volume of 100 microL biological sample the lowest point of the standard curve, i.e. the lower LOQs were 312 ng/mL. The described HILIC-MS-MS method is suitable for therapeutic drug monitoring and for clinical and pharmcokinetical investigations of the anticonvulsives.

Tomographic analysis of reactive flow induced pore structure changes in column experiments

NASA Astrophysics Data System (ADS)

Cai, Rong; Lindquist, W. Brent; Um, Wooyong; Jones, Keith W.

2009-09-01

We utilize synchrotron X-ray computed micro-tomography to capture and quantify snapshots in time of dissolution and secondary precipitation in the microstructure of Hanford sediments exposed to simulated caustic waste in flow-column experiments. The experiment is complicated somewhat as logistics dictated that the column spent significant amounts of time in a sealed state (acting as a batch reactor). Changes accompanying a net reduction in porosity of 4% were quantified including: (1) a 25% net decrease in pores resulting from a 38% loss in the number of pores <10-4mm in volume and a 13% increase in the number of pores of larger size; and (2) a 38% decrease in the number of throats. The loss of throats resulted in decreased coordination number for pores of all sizes and significant reduction in the number of pore pathways.

Development and validation of a sensitive LC-MS/MS method with electrospray ionization for quantitation of pramipexole in human plasma: application to a clinical pharmacokinetic study.

PubMed

Bharathi, D Vijaya; Hotha, Kishore Kumar; Sagar, P V Vidya; Kumar, S Sirish; Naidu, A; Mullangi, Ramesh

2009-02-01

A highly sensitive and specific LC-MS/MS method has been developed and validated for the estimation of pramipexole (PPX) with 500 microL human plasma using memantine as an internal standard (IS). The API-4000 was operated under multiple-reaction monitoring mode (MRM) using the electrospray ionization technique. Solid-phase extraction was used to extract PPX and IS from human plasma. The resolution of peaks was achieved with 0.01 m ammonium acetate buffer (pH 4.4):acetonitrile (30:70, v/v) on a Discovery CN column. The total chromatographic run time was 3.0 min and the elution of PPX and IS occurred at approximately 2.32 and 2.52, respectively. The MS/MS ion transitions monitored were 212.10 --> 153.10 for PPX and 180.20 --> 107.30 for IS. The method was proved to be accurate and precise at linearity range of 20-3540 pg/mL with a correlation coefficient (r) of > or =0.999. The intra- and inter-day precision and accuracy values found to be within the assay variability limits as per the FDA guidelines. The developed assay method was applied to a pharmacokinetic study in human volunteers following oral administration of 0.25 mg PPX tablet. Copyright (c) 2008 John Wiley & Sons, Ltd.

Measurement of Neuropeptides in Crustacean Hemolymph via MALDI Mass Spectrometry

PubMed Central

Chen, Ruibing; Ma, Mingming; Hui, Limei; Zhang, Jiang; Li, Lingjun

2009-01-01

Neuropeptides are often released into circulatory fluid (hemolymph) to act as circulating hormones and regulate many physiological processes. However, the detection of these low-level peptide hormones in circulation is often complicated by high salt interference and rapid degradation of proteins and peptides in crude hemolymph extracts. In this study, we systematically evaluated three different neuropeptide extraction protocols and developed a simple and effective hemolymph preparation method suitable for MALDI MS profiling of neuropeptides by combining acid-induced abundant protein precipitation/depletion, ultrafiltration, and C18 micro-column desalting. In hemolymph samples collected from crab Cancer borealis several secreted neuropeptides have been detected, including members from at least five neuropeptide families, such as RFamide, allatostatin, orcokinin, tachykinin-related peptide (TRP), and crustacean cardioactive peptide (CCAP). Furthermore, two TRPs were detected in the hemolymph collected from food-deprived animals, suggesting the potential role of these neuropeptides in feeding regulation. In addition, a novel peptide with a Lys-Phe-amide C-terminus was identified and de novo sequenced directly from the Cancer borealis hemolymph sample. To better characterize the hemolymph peptidome, we also identified several abundant peptide signals in C. borealis hemolymph that were assigned to protein degradation products. Collectively, our study describes a simple and effective sample preparation method for neuropeptide analysis directly from crude crustacean hemolymph. Numerous endogenous neuropeptides were detected including both known ones and new peptides whose functions remain to be characterized. PMID:19185513

A Technique for Thermal Desorption Analyses Suitable for Thermally-Labile, Volatile Compounds.

PubMed

Alborn, Hans T

2018-02-01

Many plant and insect interactions are governed by odors released by the plants or insects and there exists a continual need for new or improved methods to collect and identify these odors. Our group has for some time studied below-ground, plant-produced volatile signals affecting nematode and insect behavior. The research requires repeated sampling of volatiles of intact plant/soil systems in the laboratory as well as the field with the help of probes to minimize unwanted effects on the systems we are studying. After evaluating solid adsorbent filters with solvent extraction or solid phase micro extraction fiber sample collection, we found dynamic sampling of small air volumes on Tenax TA filters followed by thermal desorption sample introduction to be the most suitable analytical technique for our applications. Here we present the development and evaluation of a low-cost and relatively simple thermal desorption technique where a cold trap cooled with liquid carbon dioxide is added as an integral part of a splitless injector. Temperature gradient-based focusing and low thermal mass minimizes aerosol formation and eliminates the need for flash heating, resulting in low sample degradation comparable to solvent-based on-column injections. Additionally, since the presence of the cold trap does not affect normal splitless injections, on-the-fly switching between splitless and thermal desorption modes can be used for external standard quantification.

Isolation and structural characterisation of two antibacterial free fatty acids from the marine diatom, Phaeodactylum tricornutum.

PubMed

Desbois, Andrew P; Lebl, Tomas; Yan, Liming; Smith, Valerie J

2008-12-01

One solution to the global crisis of antibiotic resistance is the discovery of novel antimicrobial compounds for clinical application. Marine organisms are an attractive and, as yet, relatively untapped resource of new natural products. Cell extracts from the marine diatom, Phaeodactylum tricornutum, have antibacterial activity and the fatty acid, eicosapentaenoic acid (EPA), has been identified as one compound responsible for this activity. During the isolation of EPA, it became apparent that the extracts contained further antibacterial compounds. The present study was undertaken to isolate these additional antibacterial factors using silica column chromatography and reverse-phase high-performance liquid chromatography. Two antibacterial fractions, each containing a pure compound, were isolated and their chemical structures were investigated by mass spectrometry and nuclear magnetic resonance spectroscopy. The antibacterial compounds were identified as the monounsaturated fatty acid (9Z)-hexadecenoic acid (palmitoleic acid; C16:1 n-7) and the relatively unusual polyunsaturated fatty acid (6Z, 9Z, 12Z)-hexadecatrienoic acid (HTA; C16:3 n-4). Both are active against Gram-positive bacteria with HTA further inhibitory to the growth of the Gram-negative marine pathogen, Listonella anguillarum. Palmitoleic acid is active at micro-molar concentrations, kills bacteria rapidly, and is highly active against multidrug-resistant Staphylococcus aureus. These free fatty acids warrant further investigation as a new potential therapy for drug-resistant infections.

An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions.

PubMed

Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

2016-01-01

Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2-C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2-C7) generated in the bioconversion process were 0.01-1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane.

An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions

PubMed Central

Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

2016-01-01

Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2–C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2–C7) generated in the bioconversion process were 0.01–1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane. PMID:27695055

Enhancement of SPES source performances.

PubMed

Fagotti, E; Palmieri, A; Ren, X

2008-02-01

Installation of SPES source at LNL was finished in July 2006 and the first beam was extracted in September 2006. Commissioning results confirmed very good performance of the extracted current density. Conversely, source reliability was very poor due to glow-discharge phenomena, which were caused by the ion source axial magnetic field protruding in the high-voltage column. This problem was fixed by changing the stainless steel plasma electrode support with a ferromagnetic one. This new configuration required us to recalculate ion source solenoids positions and fields in order to recover the correct resonance pattern. Details on magnetic simulations and experimental results of high voltage column shielding are presented.

Hydrothermally tailor-made chitosan fiber for micro-solid phase extraction of petroleum acids in crude oils.

PubMed

Zhu, Gang-Tian; Hu, Xiao-Li; He, Sheng; He, Xiao-Mei; Zhu, Shu-Kui; Feng, Yu-Qi

2018-06-05

Tailor-made chitosan fiber was prepared via hydrothermal treatment to serve as a micro-solid phase extraction (micro-SPE) sorbent for the analysis of petroleum acids (PAs) in crude oils. Chitosan fiber, which is commercial and cheap, has a diameter of about 10 μm and a length of a few centimeters. The fibrous property of the sorbent enables the micro-SPE to deal with viscous crude oil samples because of the low back-pressure during extraction, while the abundant hydroxyl groups and amino groups on the surface of chitosan fiber can provide high density of specific sites for adsorption of PAs. Moreover, it was found that hydrothermal treatment at certain conditions could tune the surface properties of chitosan fiber, leading to significant improvement of the capacity of the fiber in adsorption of PAs. Using hydrothermally treated chitosan fiber as sorbent, the micro-SPE was applied to the determination of PAs in crude oils, with the advantages of easy-operation, rapidness and high sensitivity (the limits of detection range from 0.7 ng/g to 5.4 ng/g). Furthermore, coupled with comprehensive two dimensional gas chromatography-mass spectrometry (GC × GCMS), the treated chitosan fiber packed micro-SPE method showed a great potential for comprehensive profiling of PAs in crude oils. Copyright © 2018 Elsevier B.V. All rights reserved.

Insecticidal effect of plant extracts on Phlebotomus argentipes (Diptera: Psychodidae) in Bihar, India.

PubMed

Dinesh, Diwakar Singh; Kumari, Seema; Pandit, Vibhishan; Kumar, Jainendra; Kumari, Nisha; Kumar, Prahlad; Hassan, Faizan; Kumar, Vijay; Das, Pradeep

2015-12-01

Phlebotomus argentipes (Diptera: Psychodidae), the established vector for kala-azar is presently being controlled by indoor residual spray of DDT in kala-azar endemic areas in India. Search for non-hazardous and non-toxic biodegradable active molecules from botanicals may provide cost-effective and eco-friendly alternatives to synthetic insecticides. The present study was aimed at evaluating various plant extracts from endemic and non-endemic areas of Bihar for their insecticidal activity against sandfly to identify the most effective plant extract. Bio-assay test was conducted with larvae and adult of P. argentipes with different plant extracts collected in distilled water, hexane, ethyl acetate, acetone and methanol. Thin layer chromatography (TLC), column chromatography and high performance liquid chromatography (HPLC) were conducted for detection of active molecules. Adults and larvae of sandflies exposed to the aqueous extract of Nicotiana tabacum resulted in 100 per cent mortality. The hexane extract of Clerodendrum infortunatum was found to kill 77 per cent adults but was ineffective against larvae. Bio-assay test of the ninth fraction (hexane extract-methanol phase) separated by column chromatography was found to be 63 per cent effective. The purple spot on the TLC of this fraction indicated the presence of a diterpenoid. HPLC of this fraction detected nine compounds with two peaks covering 20.44 and 56.52 per cent areas with retention time of 2.439 and 5.182 min, respectively supporting the TLC results. The column separated 9 [th] fraction of C. infortunatum extract was found to be effective in killing 63 per cent of adult P. argentipes. Compounds of this fraction need to be evaluated further for identification and characterization of the active molecule by conducting individual bio-assay tests followed by further fractionation and HPLC. Once the structure of the active molecule is identified and validated, it may be synthesized and formulated as a product.

Efficient purification of paclitaxel from yews using high-performance displacement chromatography technique.

PubMed

Watchueng, Jean; Kamnaing, Pierre; Gao, Jin-Ming; Kiyota, Taira; Yeboah, Faustinus; Konishi, Yasuo

2011-05-20

Paclitaxel was purified using high-performance displacement chromatography (HPDC) technique, but not by the mechanism of HPDC. On small scale, paclitaxel was extracted with methanol from dry needles of Taxus canadensis and was enriched by extracting with chloroform after removing water-soluble hydrophilic components and hexane-soluble hydrophobic components. Then, 93-99% purity of paclitaxel was obtained using the HPDC technique. On large scale, taxanes were enriched by solvent partitioning between acetic acid/MeOH/H(2)O and hexane and extracted with CH(2)Cl(2). Taxanes except paclitaxel were further removed by extracting with methanol-water-trifluoroacetic acid (1.0:98.9:0.1, v/v/v). Applying HPDC technique to water-insoluble substances is problematic as this method requires a highly aqueous solvent system. In order to overcome this incompatibility, a system was set up where paclitaxel, although in low concentration, was extracted by methanol-water-trifluoroacetic acid (10.0:89.9:0.1, v/v/v). Recycling the extracting solvent to ensure minimal volume, the extracted paclitaxel was adsorbed on a C(18) trap column. A C(18) column of 4.6mm internal diameter was then connected to the trap column. The HPDC technique was thus carried out using an isocratic acetonitrile-water-trifluoroacetic acid (30.0:69.9:0.1, v/v/v) mobile phase consisting of a displacer cetylpyridinium trifluoroacetate (3mg/mL). Paclitaxel was co-eluted with the displacer and spontaneously crystallized. The crystal (114mg) showed 99.4% purity and only 10% of paclitaxel in the starting crude extract was lost during the enrichment/purification processes. This large scale purification method was successfully applied to purify paclitaxel from Chinese yew in small scale, suggesting general applicability of the method. This is the first report of purifying a water-insoluble natural product using HPDC technique. Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

Insecticidal effect of plant extracts on Phlebotomus argentipes (Diptera: Psychodidae) in Bihar, India

PubMed Central

Dinesh, Diwakar Singh; Kumari, Seema; Pandit, Vibhishan; Kumar, Jainendra; Kumari, Nisha; Kumar, Prahlad; Hassan, Faizan; Kumar, Vijay; Das, Pradeep

2015-01-01

Background & objectives: Phlebotomus argentipes (Diptera: Psychodidae), the established vector for kala-azar is presently being controlled by indoor residual spray of DDT in kala-azar endemic areas in India. Search for non-hazardous and non-toxic biodegradable active molecules from botanicals may provide cost-effective and eco-friendly alternatives to synthetic insecticides. The present study was aimed at evaluating various plant extracts from endemic and non-endemic areas of Bihar for their insecticidal activity against sandfly to identify the most effective plant extract. Methods: Bio-assay test was conducted with larvae and adult of P. argentipes with different plant extracts collected in distilled water, hexane, ethyl acetate, acetone and methanol. Thin layer chromatography (TLC), column chromatography and high performance liquid chromatography (HPLC) were conducted for detection of active molecules. Results: Adults and larvae of sandflies exposed to the aqueous extract of Nicotiana tabacum resulted in 100 per cent mortality. The hexane extract of Clerodendrum infortunatum was found to kill 77 per cent adults but was ineffective against larvae. Bio-assay test of the ninth fraction (hexane extract-methanol phase) separated by column chromatography was found to be 63 per cent effective. The purple spot on the TLC of this fraction indicated the presence of a diterpenoid. HPLC of this fraction detected nine compounds with two peaks covering 20.44 and 56.52 per cent areas with retention time of 2.439 and 5.182 min, respectively supporting the TLC results. Interpretation & conclusions: The column separated 9th fraction of C. infortunatum extract was found to be effective in killing 63 per cent of adult P. argentipes. Compounds of this fraction need to be evaluated further for identification and characterization of the active molecule by conducting individual bio-assay tests followed by further fractionation and HPLC. Once the structure of the active molecule is identified and validated, it may be synthesized and formulated as a product. PMID:26905249

Quantitative analysis of three chiral pesticide enantiomers by high-performance column liquid chromatography.

PubMed

Wang, Peng; Liu, Donghui; Gu, Xu; Jiang, Shuren; Zhou, Zhiqiang

2008-01-01

Methods for the enantiomeric quantitative determination of 3 chiral pesticides, paclobutrazol, myclobutanil, and uniconazole, and their residues in soil and water are reported. An effective chiral high-performance liquid chromatographic (HPLC)-UV method using an amylose-tris(3,5-dimethylphenylcarbamate; AD) column was developed for resolving the enantiomers and quantitative determination. The enantiomers were identified by a circular dichroism detector. Validation involved complete resolution of each of the 2 enantiomers, plus determination of linearity, precision, and limit of detection (LOD). The pesticide enantiomers were isolated by solvent extraction from soil and C18 solid-phase extraction from water. The 2 enantiomers of the 3 pesticides could be completely separated on the AD column using n-hexane isopropanol mobile phase. The linearity and precision results indicated that the method was reliable for the quantitative analysis of the enantiomers. LODs were 0.025, 0.05, and 0.05 mg/kg for each enantiomer of paclobutrazol, myclobutanil, and uniconazole, respectively. Recovery and precision data showed that the pretreatment procedures were satisfactory for enantiomer extraction and cleanup. This method can be used for optical purity determination of technical material and analysis of environmental residues.

Simultaneous column chromatographic extraction and purification of abscisic acid in peanut plants for direct HPLC analysis.

PubMed

Zhang, Ya-Wen; Fan, Wei-Wei; Li, Hui; Ni, He; Han, Han-Bing; Li, Hai-Hang

2015-10-01

Abscisic acid (ABA), a universal signaling molecule, plays important roles in regulating plant growth, development and stress responses. The low contents and complex components in plants make it difficult to be accurately analyzed. A novel one-step sample preparation method for ABA in plants was developed. Fresh peanut (Arachis hypogaea) plant materials were fixed by oven-drying, microwave drying, boiling or Carnoy's fixative, and loaded onto a mini-preparing column. After washed the impurities, ABA was eluted with a small amount of solvent. ABA in plant materials was completely extracted and purified in 2mL solution and directly analyzed by HPLC, with a 99.3% recovery rate. Multiple samples can be simultaneously prepared. Analyses using this method indicated that the endogenous ABA in oven-dried peanut leaves increased 20.2-fold from 1.01 to 20.37μgg(-1) dry weight within 12h and then decreased in 30% polyethylene glycol 6000 treated plants, and increased 3.34-fold from 0.85 to 2.84μgg(-1) dry weight in 5 days and then decreased in soil drought treated plants. The method combined the column chromatographic extraction and solid-phase separation technologies in one step and can completely extracted plant endogenous ABA in a purified and highly concentrated form for direct HPLC analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Immunochromatographic assay of cadmium levels in oysters.

PubMed

Nishi, Kosuke; Kim, In-Hae; Itai, Takaaki; Sugahara, Takuya; Takeyama, Haruko; Ohkawa, Hideo

2012-08-15

Oysters are one of foodstuffs containing a relatively high amount of cadmium. Here we report on establishment of an immunochromatographic assay (ICA) method of cadmium levels in oysters. Cadmium was extracted with 0.l mol L(-1) HCl from oysters and cleaned up from other metals by the use of an anion-exchange column. The behavior of five metals Mn, Fe, Cu, Zn, and Cd was monitored at each step of extraction and clean-up procedure for the ICA method in an inductively coupled plasma-mass spectrometry (ICP-MS) analysis. The results revealed that a simple extraction method with the HCl solution was efficient enough to extract almost all of cadmium from oysters. Clean-up with an anion-exchange column presented almost no loss of cadmium adsorbed on the column and an efficient removal of metals other than cadmium. When a spiked recovery test was performed in the ICA method, the recovery ranged from 98% to 112% with relative standard deviations between 5.9% and 9.2%. The measured values of cadmium in various oyster samples in the ICA method were favorably correlated with those in ICP-MS analysis (r(2)=0.97). Overall results indicate that the ICA method established in the present study is an adequate and reliable detection method for cadmium levels in oysters. Copyright © 2012 Elsevier B.V. All rights reserved.

Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

PubMed

Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

2010-02-19

A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. Copyright 2009 Elsevier B.V. All rights reserved.

Graphene oxide-based composite monolith as new sorbent for the on-line solid phase extraction and high performance liquid chromatography determination of ß-sitosterol in food samples.

PubMed

Cui, Beijiao; Guo, Bin; Wang, Huimin; Zhang, Doudou; Liu, Haiyan; Bai, Ligai; Yan, Hongyuan; Han, Dandan

2018-08-15

A composite monolithic column was prepared by redox initiation method for the on-line purification and enrichment of β-sitosterol, in which graphene oxide (GO) was embedded. The obtained monolithic column was characterized by scanning electron microscopy (SEM) and nitrogen adsorption-desorption isotherm measurement, which indicated that the monolith possessed characteristics of porous structure and high permeability. Under the optimum conditions for extraction and determination, the calibration equation was y = 47.92 × -0.1391; the linear range was 0.008-1.0 mg mL -1 ; the linear regression coefficient was 0.998; the limit of detection (LOD) is 2.4 μg mL -1 ; the limit of quantitation (LOQ) was 8 μg mL -1 ; precisions for intra-day and inter-day assays presented as relative standard deviations were less than 4.3% and 6.8%, respectively. Under the selective conditions, the enrichment factor of the method was 119. The recovery was in the range of 80.40-98.00%. Moreover, the adsorption amount of the monolith was compared with silica gel-C18 adsorbent and the monolith without graphene oxide being embedded. The polymerization monolithic column showed high selectivity and good permeability, and it was successfully used as on-line solid-phase extraction (SPE) column for determination of β-sitosterol in edible oil. Copyright © 2018 Elsevier B.V. All rights reserved.

Isolation and characterization of three benzylisoquinoline alkaloids from Thalictrum minus L. and their antibacterial activity against bovine mastitis.

PubMed

Mushtaq, Saleem; Rather, Muzafar Ahmad; Qazi, Parvaiz H; Aga, Mushtaq A; Shah, Aabid Manzoor; Shah, Aiyatullah; Ali, Md Niamat

2016-12-04

The roots of Thalictrum minus are traditionally used in the treatment of inflammation and infectious diseases such as bovine mastitis. However, there are no reports available in literature till date regarding the antibacterial studies of T. minus against bovine mastitis. The present study was undertaken to evaluate the antibacterial potential of crude extract of T. minus (root) and some of its isolated constituents against bovine mastitis in order to scientifically validate its traditional use. A total of three alkaloid compounds were isolated from the DCM: MeOH extract of roots of T. minus using silica gel column chromatography. Structural elucidation of the isolated compounds was done by using spectroscopic techniques like mass spectrometry and NMR spectroscopy. Pathogens were isolated from cases of bovine mastitis and identified by using 16S rRNA gene sequencing. The broth micro-dilution method was used to evaluate the antibacterial activities of DCM: MeOH extract and isolated compounds against mastitis pathogens. The three isolated compounds were identified as benzylisoquinoline alkaloids (1) 5'-Hydroxythalidasine, (2) Thalrugosaminine and (3) O-Methylthalicberine. Compounds (2) and (3) are reported for the first time from the roots of T. minus. Five mastitis pathogens viz., Staphylococcus xylosus, Staphylococcus lentus, Staphylococcus equorum, Enterococcus faecalis and Pantoea agglomerans were identified on the basis of sequence analysis of isolates using the nucleotide BLAST algorithm. This study reports for the first time the isolation and molecular characterization of mastitis pathogens from Kashmir valley, India. The DCM: MeOH extract exhibited broad spectrum antibacterial activities that varied between the bacterial species (MIC=250-500µg/ml). 5'-Hydroxythalidasine and Thalrugosaminine showed promising antibacterial activity with MIC values of 64-128µg/ml while Staphylococcus species were found to be the most sensitive strains. The antibacterial activities of the DCM: MeOH extract and isolated compounds support the traditional use of T. minus in the treatment of bovine mastitis. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Evaluation of DNA extraction methods for PCR-based detection of Listeria monocytogenes from vegetables.

PubMed

Vojkovska, H; Kubikova, I; Kralik, P

2015-03-01

Epidemiological data indicate that raw vegetables are associated with outbreaks of Listeria monocytogenes. Therefore, there is a demand for the availability of rapid and sensitive methods, such as PCR assays, for the detection and accurate discrimination of L. monocytogenes. However, the efficiency of PCR methods can be negatively affected by inhibitory compounds commonly found in vegetable matrices that may cause false-negative results. Therefore, the sample processing and DNA isolation steps must be carefully evaluated prior to the introduction of such methods into routine practice. In this study, we compared the ability of three column-based and four magnetic bead-based commercial DNA isolation kits to extract DNA of the model micro-organism L. monocytogenes from raw vegetables. The DNA isolation efficiency of all isolation kits was determined using a triplex real-time qPCR assay designed to specifically detect L. monocytogenes. The kit with best performance, the PowerSoil(™) Microbial DNA Isolation Kit, is suitable for the extraction of amplifiable DNA from L. monocytogenes cells in vegetable with efficiencies ranging between 29.6 and 70.3%. Coupled with the triplex real-time qPCR assay, this DNA isolation kit is applicable to the samples with bacterial loads of 10(3) bacterial cells per gram of L. monocytogenes. Several recent outbreaks of Listeria monocytogenes have been associated with the consumption of fruits and vegetables. Real-time PCR assays allow fast detection and accurate quantification of microbes. However, the success of real-time PCR is dependent on the success with which template DNA can be extracted. The results of this study suggest that the PowerSoil(™) Microbial DNA Isolation Kit can be used for the extraction of amplifiable DNA from L. monocytogenes cells in vegetable with efficiencies ranging between 29.6 and 70.3%. This method is applicable to samples with bacterial loads of 10(3) bacterial cells per gram of L. monocytogenes. © 2014 The Society for Applied Microbiology.

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

USGS Publications Warehouse

Kish, J.L.; Thurman, E.M.; Scribner, E.A.; Zimmerman, L.R.

2000-01-01

A method for the extraction and analysis of eight herbicides and five degradation products using solid-phase extraction from natural water samples followed by gas chromatography/mass spectrometry is presented in this report. This method was developed for dimethenamid; flufenacet; fluometuron and its degradation products, demethylfluometuron (DMFM), 3-(trifluromethyl)phenylurea (TFMPU), 3-(trifluromethyl)-aniline (TFMA); molinate; norflurazon and its degradation product, demethylnorflurazon; pendamethalin; the degradation product of prometryn, deisopropylprometryn; propanil; and trifluralin. The eight herbicides are used primarily in the southern United States where cotton, rice, and soybeans are produced. The exceptions are dimethenamid and flufenacet, which are used on corn in the Midwest. Water samples received by the U.S. Geological Survey's Organic Geochemistry Research Group in Lawrence, Kansas, are filtered to remove suspended particulate matter and then passed through disposable solid-phase extraction columns containing octadecyl-bonded porous silica (C-18) to extract the compounds. The herbicides and their degradation products are removed from the column by ethyl acetate elution. The eluate is evaporated under nitrogen, and components then are separated, identified, and quantified by injecting an aliquot of the concentrated extract into a high-resolution, fused-silica capillary column of a gas chromatograph/mass spectrometer under selected-ion mode. Method detection limits ranged from 0.02 to 0.05 ?g/L for all compounds with the exception of TFMPU, which has a method detection limit of 0.32 ?g/L. The mean absolute recovery is 107 percent. This method for the determination of herbicides and their degradation products is valuable for acquiring information about water quality and compound fate and transport in water.

Application of an online post-column derivatization HPLC-DPPH assay to detect compounds responsible for antioxidant activity in Sonchus oleraceus L. leaf extracts.

PubMed

Ou, Zong-Quan; Schmierer, David M; Rades, Thomas; Larsen, Lesley; McDowell, Arlene

2013-02-01

To use an online assay to identify key antioxidants in Sonchus oleraceus leaf extracts and to investigate the effect of leaf position and extraction conditions on antioxidant concentration and activity. Separation of phytochemicals and simultaneous assessment of antioxidant activity were performed online using HPLC and post-column reaction with a free-radical reagent (2, 2-diphenylpicrylhydrazyl, DPPH). Active compounds were identified using nuclear magnetic resonance spectroscopy and mass spectrometry. We applied the online HPLC-DPPH radical assay to evaluate antioxidants in leaves from different positions on the plant and to assess the effect of pre-treatment of leaves with liquid N(2) before grinding, extraction time, extraction temperature and method of concentrating extracts. Key antioxidants identified in S. oleraceus leaf extracts were caftaric acid, chlorogenic acid and chicoric acid. Middle leaves contained the highest total amount of the three key antioxidant compounds, consisting mainly of chicoric acid. Pre-treatment with liquid N(2), increasing the extraction temperature and time and freeze-drying the extract did not enhance the yield of the key antioxidants. The online HPLC-DPPH radical assay was validated as a useful screening tool for investigating individual antioxidants in leaf extracts. Optimized extraction conditions were middle leaves pre-treated with liquid N(2), extraction at 25°C for 0.5 h and solvent removal by rotary evaporation. © 2012 The Authors. JPP © 2012. Royal Pharmaceutical Society.

Unsuccessful Detection of Plant MicroRNAs in Beer, Extra Virgin Olive Oil and Human Plasma After an Acute Ingestion of Extra Virgin Olive Oil.

PubMed

Micó, Victor; Martín, Roberto; Lasunción, Miguel A; Ordovás, Jose M; Daimiel, Lidia

2016-03-01

The recent description of the presence of exogenous plant microRNAs from rice in human plasma had profound implications for the interpretation of microRNAs function in human health. If validated, these results suggest that food should not be considered only as a macronutrient and micronutrient supplier but it could also be a way of genomic interchange between kingdoms. Subsequently, several studies have tried to replicate these results in rice and other plant foods and most of them have failed to find plant microRNAs in human plasma. In this scenario, we aimed to detect plant microRNAs in beer and extra virgin olive oil (EVOO)--two plant-derived liquid products frequently consumed in Spain--as well as in human plasma after an acute ingestion of EVOO. Our hypothesis was that microRNAs present in beer and EVOO raw material could survive manufacturing processes, be part of these liquid products, be absorbed by human gut and circulate in human plasma. To test this hypothesis, we first optimized the microRNA extraction protocol to extract microRNAs from beer and EVOO, and then tried to detect microRNAs in those samples and in plasma samples of healthy volunteers after an acute ingestion of EVOO.

Sensitive method for the quantitation of droloxifene in plasma and serum by high-performance liquid chromatography employing fluorimetric detection.

PubMed

Tess, D A; Cole, R O; Toler, S M

1995-12-15

A simple and highly sensitive reversed-phase fluorimetric HPLC method for the quantitation of droloxifene from rat, monkey, and human plasma as well as human serum is described. This assay employs solid-phase extraction and has a dynamic range of 25 to 10,000 pg/ml. Sample extraction (efficiencies > 86%) was accomplished using a benzenesulfonic acid (SCX) column with water and methanol rinses. Droloxifene and internal standard were eluted with 1 ml of 3.5% (v/v) ammonium hydroxide (30%) in methanol. Samples were quantitated using post-column UV-photochemical cyclization coupled with fluorimetric detection with excitation and emission wavelengths of 260 nm and 375 nm, respectively. Relative ease of sample extraction and short run times allow for the analysis of approximately 100 samples per day.

Comparison of methods for hydrocarbon analysis of marine biota

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

Gritz, R.L.; Shaw, D.G.

1977-04-01

A comparison was made of several procedures for the isolation of hydrocarbons from other matter and for the fractionation of hydrocarbons according to chemical type. The efficiency of Soxhlet extraction followed by saponification with extraction by alkaline digestion (direct saponification) was compared using two hour and 24 hour reaction times. All procedures were performed on approximately 60 g of soft parts of Saxidomus gigantea (butter clam). The 24 hour saponification and column chromatography on partially deactivated columns constituted the best procedure tested. Soxhlet extraction followed by two hour saponification did not completely remove methyl esters and was the most laboriousmore » technique. Direct two hour saponification was also questionable in the removal of esters and led to severe emulsion problems. The recoveries of hydrocarbons by the three procedures was substantially the same.« less

Characterization of the molluscicidal activity of Bauhinia variegata and Mimusops elengi plant extracts against the fasciola vector Lymnaea acuminata.

PubMed

Singh, Kanchan Lata; Singh, D K; Singh, Vinay Kumar

2012-01-01

The molluscicidal activity of Bauhinia variegata leaf and Mimusops elengi bark was studied against vector snail Lymnaea acuminata. The toxicity of both plants was time and concentration-dependent. Among organic extracts, ethanol extracts of both plants were more toxic. Toxicity of B. variegata leaf ethanolic extract (96h LC50- 14.4 mg/L) was more pronounced than M. elengi bark ethanolic extract (96h LC50-15.0 mg/L). The 24h LC50 of column purified fraction of B. variegata and M. elengi bark were 20.3 mg/L and 18.3 mg/L, respectively. Saponin and quercetin were characterized and identified as active molluscicidal component. Co-migration of saponin (Rf 0.48) and quercetin (Rf 0.52) with column purified bark of M. elengi and leaf of B. variegata on thin layer chromatography demonstrate same Rf value i.e. 0.48 and 0.52, respectively. The present study clearly indicates the possibility of using M. elengi and/or B. variegata as potent molluscicide.

Mathematical modeling of the adsorption/desorption characteristics of anthocyanins from muscadine (Vitis rotundifolia cv. Noble) juice pomace on Amberlite FPX66 resin in a fixed bed column.

PubMed

Uzdevenes, Chad G; Gao, Chi; Sandhu, Amandeep K; Yagiz, Yavuz; Gu, Liwei

2018-03-24

Muscadine grape pomace, a by-product of juicing and wine-making, contains significant amounts of anthocyanin 3,5-diglucosides, known to be beneficial to human health. The objective of this research was to use mathematical modeling to investigate the adsorption/desorption characteristics of these anthocyanins from muscadine grape pomace on Amberlite FPX66 resin in a fixed bed column. Anthocyanins were extracted using hot water and ultrasound, and the extracts were loaded onto a resin column at five bed depths (5, 6, 8, 10 and 12 cm) using three flow rates (4, 6 and 8 mL min -1 ). It was found that adsorption on the column fitted the bed depth service time (BDST) model and the empty bed residence time (EBRT) model. Desorption was achieved by eluting the column using ethanol at four concentrations (25, 40, 55 and 70% v/v) and could be described with an empirical sigmoid model. The breakthrough curves of anthocyanins fitted the BDST model for all three flow rates with R 2 values of 0.983, 0.992 and 0.984 respectively. The EBRT model was successfully employed to find the operating lines, which allow for column scale-up while still achieving similar results to those found in a laboratory operation. Desorption with 40% (v/v) ethanol achieved the highest recovery rate of anthocyanins at 79.6%. The mathematical models established in this study can be used in designing a pilot/industrial- scale column for the separation and concentration of anthocyanins from muscadine juice pomace. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

A new solid-phase extraction and HPLC method for determination of patulin in apple products and hawthorn juice in China.

PubMed

Zhou, Yuchun; Kong, Weijun; Li, Yan; Logrieco, Antonio F; Xu, Jun; Yang, Meihua

2012-03-01

A new solid-phase extraction (SPE) pretreatment method using a home-made polyvinylpolypyrrolidone-florisil (PVPP-F) column was developed for the analysis of patulin in apple and hawthorn products in China. Fifty samples (25 apple juices, 12 apple jams, and 13 hawthorn juices) were prepared using the new method and then analyzed by high performance liquid chromatography with diode array detection (HPLC-DAD) on an Agela Venusil MP C(18) reversed-phase column (4.6 mm × 250 mm, 5 μm). The cleanup results for all samples using home-made PVPP-F column were compared with those obtained using a MycoSep®228 AflaPat column. The correlation coefficient R (0.9998) fulfilled the requirement of linearity for patulin in the concentration range of 2.5-250 μg/kg. The limits of detection (LODs) and quantification (LOQs) of patulin were 3.99 and 9.64 μg/kg for PVPP-F column, and 3.56 and 8.07 μg/kg for MycoSep®228 AflaPat column, respectively. Samples were spiked with patulin at levels ranging from 25 to 250 μg/kg, and recoveries using PVPP-F and MycoSep®228 AflaPat columns were in the range of 81.9-100.9% and 86.4-103.9%, respectively. Naturally occurring patulin was found in 2 of 25 apple juice samples (8.0%) and 1 of 13 hawthorn juice samples (7.7%) at concentrations ranging from 12.26 to 36.81 μg/kg. The positive results were further confirmed by liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS). © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation of transition metals on a poly-iminodiacetic acid grafted polymeric resin column with post-column reaction detection utilising a paired emitter-detector diode system.

PubMed

Barron, Leon; O'Toole, Martina; Diamond, Dermot; Nesterenko, Pavel N; Paull, Brett

2008-12-05

The selectivity, retention and separation of transition metals on a short (2 mm x 50 mm) column packed with a poly-iminodiacetic acid functionalised polymer 10 microm resin (Dionex ProPac IMAC-10) are presented. This stationary phase, typically used for the separation of proteins, is composed of long chain poly-iminodiacetic acid groups grafted to a hydrophilic layer surrounding a 10 microm polymeric bead. Through the use of a combination of a multi-step pH and picolinic acid gradient, the separation of magnesium, iron, cobalt, cadmium, zinc, lead and copper was possible, followed by post-column reaction with 4-(2-pyridylazo) resorcinol (PAR) and absorbance detection at 510 nm using a novel and inexpensive optical detector, comprised of two light emitting diodes with one acting as a light source and the other as a detector. Column efficiency for selective transition metals was in excess of N=10,000, with the baseline separation of seven metal cations in <3 min possible under optimised conditions. Detection limits of between 5 and 81 microg/L were possible based upon a 50 microL injection volume.

A Novel MicroElectroMechanical System (MEMS) Device for Passive Sampling of Hydrophobic Compounds

DTIC Science & Technology

2011-05-01

bioavailability  Samplers are removed, extracted for CoC, analyzed ▬ For organics: solid phase micro extraction ( SPME ) fibers, semi- permeable membrane...devices (SPMD), polyoxymethylene (POM) ▬ For metals: diffuse gradients in thin films (DGT) SPME fiber ESTCP project, Reible and Lotufo Applications to...Predict Bioaccumulation You et al. 2006, EST, 40: 6348 SPME concentrations were predictive of tissue concentrations of PCBs in field-contaminated

Development and Efficacy Testing of Next Generation Cyanide Antidotes

DTIC Science & Technology

2013-10-01

Preparation of mDMTS A-2.2. HPLC method for DMTS determination in Micelles A-2.3. Head-space solid phase micro-extraction- gas chromatography -mass...Simultaneous determination of cyanide and thiocyanate in plasma by chemical ionization gas chromatography mass-spectrometry (CI-GC-MS). Analytical and...min. Peak integration was performed using Star Chromatography Workstation Version 6.20. A-2.3. Head-space solid phase micro-extraction- gas

Curcumin affects development of zebrafish embryo.

PubMed

Wu, Jheng-Yu; Lin, Chin-Yi; Lin, Tien-Wei; Ken, Chuian-Fu; Wen, Yu-Der

2007-07-01

Embryotoxic and teratogenic effects of curcumin on the development of zebrafish embryo were investi-gated in this study. The LD(50) values of curcumin (24-h incubation) were estimated at 7.5 microM and 5 microM for embryos and larvae, respectively. The developmental defects caused by curcumin treatments include bent or hook-like tails, spinal column curving, edema in pericardial sac, retarded yolk sac resorption, and shorter body length. In curcumin-treated larvae, fluorescence signals of curcumin were found in edamae sac and some skin cells. Together, these results indicate that zebrafish are suitable model organisms to study the toxic effects of curcumin.

Sickle cell anemia: a potential nutritional approach for a molecular disease.

PubMed

Ohnishi, S T; Ohnishi, T; Ogunmola, G B

2000-05-01

A certain population of red blood cells in patients with sickle cell anemia has an elevated density and possesses an abnormal membrane. These "dense cells" have a tendency to adhere to neutrophils, platelets, and vascular endothelial cells, and, thus, they could trigger vasoocclusion and the subsequent painful crisis from which these patients suffer. We developed a laboratory method of preparing such dense cells and found that nutritional antioxidant supplements, hydroxyl radical scavengers, and iron-binding agents could inhibit the formation of dense cells in vitro. The concentrations at which effective nutritional supplements could inhibit dense cell formation by 50% were 4.0 mg/mL for aged garlic extract, 0.38 mg/mL for black tea extract, 0.13 mg/mL for green tea extract, 0.07 mg/mL for Pycnogenol, 930 microM for alpha-lipoic acid, 270 microM for vitamin E, 45 microM for coenzyme Q(10), and 32 microM for beta-carotene. Both an ex vivo study and a pilot clinical trial demonstrated that a cocktail consisting of daily doses of 6 g of aged garlic extract, 4-6 g of vitamin C, and 800 to 1200 IU of vitamin E may indeed be beneficial to the patients.

Micro-matrix solid-phase dispersion coupled with MEEKC for quantitative analysis of lignans in Schisandrae Chinensis Fructus using molecular sieve TS-1 as a sorbent.

PubMed

Chu, Chu; Wei, Mengmeng; Wang, Shan; Zheng, Liqiong; He, Zheng; Cao, Jun; Yan, Jizhong

2017-09-15

A simple and effective method was developed for determining lignans in Schisandrae Chinensis Fructus by using a micro-matrix solid phase dispersion (MSPD) technique coupled with microemulsion electrokinetic chromatography (MEEKC). Molecular sieve, TS-1, was applied as a solid supporting material in micro MSPD extraction for the first time. Parameters that affect extraction efficiency, such as type of dispersant, mass ratio of the sample to the dispersant, grinding time, elution solvent and volume were optimized. The optimal extraction conditions involve dispersing 25mg of powdered Schisandrae samples with 50mg of TS-1 by a mortar and pestle. A grinding time of 150s was adopted. The blend was then transferred to a solid-phase extraction cartridge and the target analytes were eluted with 500μL of methanol. Moreover, several parameters affecting MEEKC separation were studied, including the type of oil, SDS concentration, type and concentration of cosurfactant, and concentration of organic modifier. A satisfactory linearity (R>0.9998) was obtained, and the calculated limits of quantitation were less than 2.77μg/mL. Finally, the micro MSPD-MEEKC method was successfully applied to the analysis of lignans in complex Schisandrae fructus samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Automated mini-column solid-phase extraction cleanup for high-throughput analysis of chemical contaminants in foods by low-pressure gas chromatography – tandem mass spectrometry

USDA-ARS?s Scientific Manuscript database

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography – tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. ...

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

EPA Science Inventory

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

Ground-water contamination by organic bases derived from coal-tar wastes

USGS Publications Warehouse

Pereira, Wilfred E.; Rostad, Colleen E.; Garbarino, John R.; Hult, Marc F.

1983-01-01

A fluid sample from a shallow aquifer contaminated by coal-tar wastes was analyzed for organic bases. The sample consisted of a mixture of aqueous and oily-tar phases. The phases were separated by centrifugation and filtration. Organic bases were isolated from each phase by pH adjustment and solvent extraction. Organic bases in the oily-tar phase were further purified by neutral-alumina, micro-column adsorption chromatography. Separation and identification of the organic bases in each phase were achieved by using capillary gas chromatography-mass spectrometry-computer (GC-MS-COM) and probe distillation-high resolution mass spectrometry (PD-HRMS) techniques. Organic bases present in the aqueous phase included primary aromatic amines (such as aniline, alkylated anilines, and naphthylamines) as well as azaarenes (such as alkylated pyridines, quinolines, acridine, and benzoquinolines). The oily-tar phase contained acridine, benzacridines, dibenzacridines, and numerous other azaarenes, the elemental compositions of which were determined by PD-HRMS. Azaarenes in the oily-tar phase, varying in size from 6 to 12 rings, are reported for the first time. The origin and environmental significance of these compounds are discussed.

Groundwater contamination by organic bases derived from coal-tar wastes

USGS Publications Warehouse

Pereira, W.E.; Rostad, C.E.; Garbarino, J.R.; Hult, M.F.

1983-01-01

A fluid sample from a shallow aquifer contaminated by coal-tar wastes was analyzed for organic bases. The sample consisted of a mixture of aqueous and oily-tar phases. The phases were separated by centrifugation and filtration. Organic bases were isolated from each phase by pH adjustment and solvent extraction. Organic bases in the oily-tar phase were further purified by neutral-alumina, micro-column adsorption chromatography. Separation and identification of the organic bases in each phase were achieved by using capillary gas chromatography-mass spectrometry-computer (GC-MS-COM) and probe distillation-high resolution mass spectrometry (PD-HRMS) techniques. Organic bases present in the aqueous phase included primary aromatic amines (such as aniline, alkylated anilines, and naphthylamines) as well as azaarenes (such as alkylated pyridines, quinolines, acridine, and benzoquinolines). The oily-tar phase contained acridine, benzacridines, dibenzacridines, and numerous other azaarenes, the elemental compositions of which were determined by PD-HRMS. Azaarenes in the oily-tar phase, varying in size from 6 to 12 rings, are reported for the first time. The origin and environmental significance of these compounds are discussed. ?? 1983.

Mercury(II) and methyl mercury determinations in water and fish samples by using solid phase extraction and cold vapour atomic absorption spectrometry combination.

PubMed

Tuzen, Mustafa; Karaman, Isa; Citak, Demirhan; Soylak, Mustafa

2009-07-01

A method has been developed for mercury(II) and methyl mercury speciation on Staphylococcus aureus loaded Dowex Optipore V-493 micro-column in the presented work, by using cold vapour atomic absorption spectrometry. Selective and sequential elution with 0.1 molL(-1) HCl for methyl mercury and 2 molL(-1) HCl for mercury(II) were performed at the pH range of 2-6. Optimal analytical conditions including pH, amounts of biosorbent, sample volumes were investigated. The detection limits of the analytes were 2.5 ngL(-1) for Hg(II) and 1.7 ngL(-1) for methyl mercury. The capacity of biosorbent for mercury(II) and methyl mercury was 6.5 and 5.4 mgg(-1), respectively. The validation of the presented procedure is performed by the analysis of standard reference material. The speciation procedure established was successfully applied to the speciation of mercury(II) and methyl mercury in natural water and microwave digested fish samples.

[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.

Towards a method of rapid extraction of strontium-90 from urine: urine pretreatment and alkali metal removal

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

Hawkins, C.; Dietz, M.; Kaminski, M.

2016-03-01

A technical program to support the Centers of Disease Control and Prevention is being developed to provide an analytical method for rapid extraction of Sr-90 from urine, with the intent of assessing the general population’s exposure during an emergency response to a radiological terrorist event. Results are presented on the progress in urine sample preparation and chemical separation steps that provide an accurate and quantitative detection of Sr-90 based upon an automated column separation sequence and a liquid scintillation assay. Batch extractions were used to evaluate the urine pretreatment and the column separation efficiency and loading capacity based upon commercial,more » extractant-loaded resins. An efficient pretreatment process for decolorizing and removing organics from urine without measurable loss of radiostrontium from the sample was demonstrated. In addition, the Diphonix® resin shows promise for the removal of high concentrations of common strontium interferents in urine as a first separation step for Sr-90 analysis.« less

Molecularly imprinted solid-phase extraction sorbent for the clean-up of chlorinated phenoxyacids from aqueous samples.

PubMed

Baggiani, C; Giovannoli, C; Anfossi, L; Tozzi, C

2001-12-14

A molecularly imprinted polymer (MIP) was synthesized using the herbicide 2,4,5-trichlorophenoxyacetic acid as a template, 4-vinylpyridine as an interacting monomer, ethylendimethacrylate as a cross-linker and a methanol-water mixture as a porogen. The binding properties and the selectivity of the polymer towards the template were investigated by frontal and zonal liquid chromatography. The polymer was used as a solid-phase extraction material for the clean-up of the template molecule and some related herbicides (2,4-dichlorophenoxyacetic acid, fenoprop, dichlorprop) from river water samples at a concentration level of ng/ml with quantitative recoveries comparable with those obtained with a traditional C18 reversed-phase column when analyzed by capillary electrophoresis. The results obtained show that the MIP-based approach to the solid-phase extraction is comparable with the more traditional solid-phase extraction with C18 reversed-phase columns in terms of recovery, but it is superior in terms of sample clean-up.

Fingerprint chromatogram analysis of extracts from the leaves of Tripterygium wilfordii Hook. F. by high performance liquid chromatography.

PubMed

Li, Ke; Wang, Shudong

2005-05-01

A simple and reliable high performance liquid chromatographic (HPLC) method has been developed and validated for the study of fingerprint chromatograms of extracts from the leaves of Tripterygium wilfordii Hook. F. (TWHF) and for controlling the quality of the herb. HPLC separation of the extracts was performed on a Lichrospher RP-18 column and detected by ultraviolet absorbance at 210 nm. The column temperature was maintained at 35 degrees C. A mobile phase composed of acetonitrile:H2O in the ratio of 39:61 (v/v) was found to be most suitable for this separation at a flow rate of 0.8 mL/min with isocratic elution. Under the chromatographic conditions described, the peak profile of the 10 components collected within 35 min made up the fingerprint of the extracts from leaves of TWHF with universal features. The fingerprint chromatograms had a good stability, precision, and reproducibility. The similarity of the extracts from leaves of TWHF collected in summer and winter was studied with triptolide as a reference peak. The method is suitable for differentiation of extracts from the leaves of TWHF, and can be used as a quality control method for this herb.

Cytotoxic and multidrug resistance reversal activity of a vegetable, 'Anastasia Red', a variety of sweet pepper.

PubMed

Motohashi, Noboru; Wakabayashi, Hidetsugu; Kurihara, Teruo; Takada, Yuko; Maruyama, Shichiro; Sakagami, Hiroshi; Nakashima, Hideki; Tani, Satoru; Shirataki, Yoshiaki; Kawase, Masami; Wolfard, Kristina; Molnár, Joseph

2003-04-01

The vegetable, Anastasia Red, Capsicum annuum L. var. angulosum Mill. (Solanaceae) was successively extracted with hexane, acetone, methanol and 70% methanol, and the extracts were further separated into a total of 21 fractions by silica gel or octadecylsilane (ODS) column chromatography. The biological activities of extracts and fractions were determined. These extracts showed relatively higher cytotoxic activity against two human oral tumor cell lines (HSC-2, HSG) than against normal human gingival fibroblasts (HGF), suggesting a tumor-specific cytotoxic activity. The cytotoxic activity of these extracts was enhanced by fractionation on silica gel [H2, A2, M1-M3] or ODS column chromatography [70M]. Several fractions [H2, H4, H5, A1, A2, A3, A5, A6, A7, M2] reversed the multidrug resistance (MDR) phenotype with L5178 mouse lymphoma T cells, more efficiently than (+/-)-verapamil. The extracts and fractions did not show any detectable anti-human immunodeficiency virus (HIV) or anti-Helicobacter pylori activity. Thus, this study suggests the effective and selective antitumor potential of 'Anastasia Red' of sweet pepper for further phytochemical and biological investigation. Copyright 2003 John Wiley & Sons, Ltd.

Quantitative determination of atenolol in dried blood spot samples by LC-HRMS: a potential method for assessing medication adherence.

PubMed

Lawson, Graham; Cocks, Elizabeth; Tanna, Sangeeta

2012-05-15

The use of blood spot collection cards was investigated as a means of obtaining small volume samples for the quantification of therapeutic drugs for assessing medication adherence. A liquid chromatography-high resolution TOF mass spectrometry (LC-HRMS) method, based on the measurement at the accurate mass to charge ratio of the target analyte, was used to ensure specificity for atenolol in the dried blood spot (DBS) samples. A working method was developed and validated. For the preparation of DBS samples whole blood spiked with analyte was used to produce 30 μl blood spots on specimen collection cards. A 5mm disc was cut from the dried blood spot and extracted using methanol:water (60:40, v/v) containing the internal standard, atenolol-d(7). Extracts were vortexed, sonicated and then centrifuged. Gradient chromatographic elution was achieved using an Ascentis Express C18 100mm×2.1mm column and a mobile phase flow rate of 0.2 ml/min and the column oven temperature at 30 °C. MS detection was carried out in electrospray positive ion mode for target ions at accurate mass m/z 267.1703 for atenolol and 274.2143 for the IS. Drug extraction efficiency from spiked blood spots was demonstrated to be 96±5% and the drug was stable in DBS for at least 10 weeks. The developed LC-HRMS method was linear within the tested calibration range of 25-1500 ng/ml and validation showed the accuracy (relative error) and precision (coefficient of variation) values were within the pre-defined limits of ≤ 5% at all concentrations with a limit of quantification of 25 ng/ml. Factors with potential to affect drug quantification measurements such as the matrix effects, volume of blood applied onto the collection card and effect of different sampling cards were investigated. The developed LC-HRMS method was applied to blood spots on sampling card taken from adult healthy volunteers previously administered a 50mg atenolol tablet and a DBS concentration-time profile was obtained for atenolol. Requiring only a micro volume (30 μl) blood sample for analysis, the developed DBS based assay has the potential to assess patient adherence to atenolol. Copyright © 2012 Elsevier B.V. All rights reserved.

Laboratory evaluation of molluscicidal activity of extracts from Cotula cinerea (L) and Quercus lusitania var. infectoria galls (Oliv.).

PubMed

Redwane, A; Markouk, M; Lazrek, H B; Amarouch, H; Jana, M

1998-01-01

In this work, we have studied the molluscicidal activity of different extracts obtained from Cotula cinerea and Quercus lusitania var. infectoria galls. The hydroalcoholic extract of Cotula cinerea, acetonic extract and gallotanin of Quercus infectoria galls have presented high activity against Bulinus truncatus. The hydroalcoholic extract of Cotula cinerea was fractionated by chromatography on silica gel column. We have isolated two very active fractions at concentrations respectively of 52.5 and 27.5 ppm.

Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

NASA Astrophysics Data System (ADS)

Oliveira, J. M.; Carvalho, F. P.

2006-01-01

A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom® and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample).

On-line Analysis of Catalytic Reaction Products Using a High-Pressure Tandem Micro-reactor GC/MS.

PubMed

Watanabe, Atsushi; Kim, Young-Min; Hosaka, Akihiko; Watanabe, Chuichi; Teramae, Norio; Ohtani, Hajime; Kim, Seungdo; Park, Young-Kwon; Wang, Kaige; Freeman, Robert R

2017-01-01

When a GC/MS system is coupled with a pressurized reactor, the separation efficiency and the retention time are directly affected by the reactor pressure. To keep the GC column flow rate constant irrespective of the reaction pressure, a restrictor capillary tube and an open split interface are attached between the GC injection port and the head of a GC separation column. The capability of the attached modules is demonstrated for the on-line GC/MS analysis of catalytic reaction products of a bio-oil model sample (guaiacol), produced under a pressure of 1 to 3 MPa.

Homogenization-assisted cavitation hybrid rotation extraction and macroporous resin enrichment of dihydroquercetin from Larix gmelinii.

PubMed

Xia, Yu; Wang, Yinhang; Li, Wei; Ma, Chunhui; Liu, Shouxin

2017-12-01

Cavitation hybrid rotation, which was and is still looked upon as an unavoidable nuisance in the flow systems, for extraction processing intensification of active chemical compounds from natural products. In this study, a homogenization-assisted cavitation hybrid rotation extraction method was applied to extract dihydroquercetin (DHQ) from larch (Larix gmelinii) wood root. The extraction parameters were optimized in single factor experiments with the DHQ extraction yields as the response values. The optimum conditions were as follows: number of extractions, three; ethanol volume fraction for the extraction, 60%; liquid-solid ratio for homogenization, 10mL/g; homogenization time, 8min; liquid-solid ratio for cavitation extraction, 9mL/g, and cavitation extraction time, 35min. Under these conditions, the DHQ content in extract was 4.50±0.02mg/g, and the extraction efficiency was higher than those of traditional techniques. Cavitation can be effectively used to improve the extraction rate by increasing the mass transfer rates and possible rupture of cell wall due to formation of microcavities leading to higher product yields with reduced processing time and solvent consumption. After the extraction process, macroporous resin column chromatography was used to concentrate and purify the DHQ. Three resins were selected from fifteen macroporous resins for further investigation of their performance. Among these resins, AB-8 resin exhibited relatively better adsorption capacities and desorption ratios for DHQ. The ethanol volume fraction of the solutions for sample loading and desorption, and flow rates for loading and desorption were optimized for the macroporous resin column chromatography. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid small-scale column testing of granular activated carbon for organic micro-pollutant removal in treated domestic wastewater.

PubMed

Zietzschmann, F; Müller, J; Sperlich, A; Ruhl, A S; Meinel, F; Altmann, J; Jekel, M

2014-01-01

This study investigates the applicability of the rapid small-scale column test (RSSCT) concept for testing of granular activated carbon (GAC) for organic micro-pollutants (OMPs) removal from wastewater treatment plant (WWTP) effluent. The chosen experimental setup was checked using pure water, WWTP effluent, different GAC products, and variable hydrodynamic conditions with different flow velocities and differently sized GAC, as well as different empty bed contact times (EBCTs). The setup results in satisfying reproducibility and robustness. RSSCTs in combination with WWTP effluent are effective when comparing the OMP removal potentials of different GAC products and are a useful tool for the estimation of larger filters. Due to the potentially high competition between OMPs and bulk organics, breakthrough curves are likely to have unfavorable shapes when treating WWTP effluent. This effect can be counteracted by extending the EBCT. With respect to the strong competition observed in GAC treatment of WWTP effluent, the small organic acid and neutral substances are retained longer in the RSSCT filters and are likely to cause the majority of the observed adsorption competition with OMPs.

Sequential injection system with in-line solid phase extraction and soil mini-column for determination of zinc and copper in soil leachates.

PubMed

Paluch, Justyna; Mesquita, Raquel B R; Cerdà, Víctor; Kozak, Joanna; Wieczorek, Marcin; Rangel, António O S S

2018-08-01

A sequential injection (SI) system equipped with in-line solid phase extraction column and in-line soil mini-column is proposed for determination of zinc and copper in soil leachates. The spectrophotometric determination (560 nm) is based on the reaction of both analytes with 1-(2-Pyridylazo)-2-naphthol (PAN). Zinc is determined after retaining copper on a cationic resin (Chelex100) whereas copper is determined from the difference of the absorbance measured for both analytes, introduced into the system with the use of a different channel, and zinc absorbance. The influence of several potential interferences was studied. Using the developed method, zinc and copper were determined within the concentration ranges of 0.005-0.300 and 0.011-0.200 mg L -1 , and with a relative standard deviation lower than 6.0% and 5.1%, respectively. The detection limits are 1.4 and 3.0 µg/L for determination of zinc and copper, respectively. The developed SI method was verified by the determination of both analytes in synthetic and certified reference materials of water samples, and applied to the determination of the analytes in rain water and soil leachates from laboratory scale soil core column and in-line soil mini-column. Copyright © 2018 Elsevier B.V. All rights reserved.

Thermal and oxidative degradation studies of formulated C-ethers by gel-permeation chromatography

NASA Technical Reports Server (NTRS)

Jones, W. R., Jr.; Morales, W.

1982-01-01

Gel-permeation chromatography was used to analyze C-ether lubricant formulations from high-temperature bearing tests and from micro-oxidation tests. Three mu-styragel columns (one 500 and two 100 A) and a tetrahydrofuran mobile phase were found to adequately separate the C-ether degradation products. The micro-oxidation tests yielded degradation results qualitatively similar to those observed from the bearing tests. Micro-oxidation tests conducted in air yielded more degradation than did tests in nitrogen. No great differences were observed between the thermal-oxidative stabilities of the two C-ether formulations or between the catalytic degradation activities of silver and M-50 steel. C-ether formulation I did yield more degradation than did formulation II in 111- and 25-hour bearing tests, respectively.

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

PubMed

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

2009-07-15

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

Electron current extraction from radio frequency excited micro-dielectric barrier discharges

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

Wang, Jun-Chieh; Kushner, Mark J.; Leoni, Napoleon

Micro dielectric barrier discharges (mDBDs) consist of micro-plasma devices (10-100 {mu}m diameter) in which the electrodes are fully or partially covered by dielectrics, and often operate at atmospheric pressure driven with radio frequency (rf) waveforms. In certain applications, it may be desirable to extract electron current out of the mDBD plasma, which necessitates a third electrode. As a result, the physical structure of the m-DBD and the electron emitting properties of its materials are important to its operation. In this paper, results from a two-dimensional computer simulation of current extraction from mDBDs sustained in atmospheric pressure N{sub 2} will bemore » discussed. The mDBDs are sandwich structures with an opening of tens-of-microns excited with rf voltage waveforms of up to 25 MHz. Following avalanche by electron impact ionization in the mDBD cavity, the plasma can be expelled from the cavity towards the extraction electrode during the part of the rf cycle when the extraction electrode appears anodic. The electron current extraction can be enhanced by biasing this electrode. The charge collection can be controlled by choice of rf frequency, rf driving voltage, and permittivity of the dielectric barrier.« less

Chromatographic column evaluation for the untargeted profiling of glucosinolates in cauliflower by means of ultra-high performance liquid chromatography coupled to high resolution mass spectrometry.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Montone, Carmela Maria; Piovesana, Susy; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2018-03-01

The untargeted profiling is a promising approach for the characterization of secondary metabolites in biological matrices. Thanks to the recent rapid development of high-resolution mass spectrometry (HRMS) instrumentations, the number of applications by untargeted approaches for biological samples profiling has widely increased in the recent years. Despite the high potentialities of HRMS, however, a major issue in natural products analysis often arises in the upstream process of compounds separation. A separation technique is necessary to avoid phenomena such as signal suppression, and it is especially needed in the presence of isomeric metabolites, which are otherwise indistinguishable. Glucosinolates (GLSs), a group of secondary metabolites widely distributed among plants, resulted to be associated to the prevention of some serious diseases, such as cancer. This led to the development of several methods for the analysis of GLSs in vegetables tissues. The issue of GLSs chromatographic separation has been widely studied in the past because of the difficulty in the analysis of this highly polar and variable class of compounds. Several alternatives to reversed phase (RP) chromatography, sometimes not compatible with the coupling of liquid chromatography with mass spectrometry, have been tested for the analysis of intact GLSs. However, the availability of new stationary phases, in the last years, could allow the re-evaluation of RP chromatography for the analysis of intact GLSs. In this work, a thorough evaluation of four RP chromatographic columns for the analysis of GLSs in cauliflower (Brassica oleracea L. var. botrytis) extracts by an ultra-high performance liquid chromatographic system coupled via electrospray source to a hybrid quadrupole-Orbitrap mass spectrometer is presented. The columns tested were the following: one column Luna Omega polar C 18 , one column Kinetex Biphenyl, one column Kinetex core-shell XB-C 18 , two columns Kinetex core-shell XB-C 18 . After a previous optimization of the extraction method, cauliflower extracts were analyzed testing four different mobile phases onto the four columns for a total of sixteen different chromatographic conditions. The chromatographic systems were evaluated based on the number of detected and tentatively identified GLSs. Luna Polar stationary phase resulted to be the most suitable for the analysis of GLSs compared to Kinetex XB and Kinetex Biphenyl columns stationary phase. However, two in series Kinetex XB columns increased the number of tentatively identified GLSs compared to one Kinetex XB, showing the importance of column length in the analysis of complex mixtures. The data obtained with the best chromatographic system were deeply analyzed by MS/MS investigation for the final identification. Fiflty-one GLSs were tentatively identified, 24 of which have never been identified in cauliflower. Finally the linearity of the analytes response over the analyzed range of concentration was checked, suggesting that the developed method is suitable for both qualitative and quantitative analysis of GLSs in phytochemical mixtures. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

2008-05-01

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

Antioxidant Activity of a Red Lentil Extract and Its Fractions

PubMed Central

Amarowicz, Ryszard; Estrella, Isabell; Hernández, Teresa; Dueñas, Montserrat; Troszyńska, Agnieszka; Agnieszka, Kosińska; Pegg, Ronald B.

2009-01-01

Phenolic compounds were extracted from red lentil seeds using 80% (v/v) aqueous acetone. The crude extract was applied to a Sephadex LH-20 column. Fraction 1, consisting of sugars and low-molecular-weight phenolics, was eluted from the column by ethanol. Fraction 2, consisting of tannins, was obtained using acetone-water (1:1; v/v) as the mobile phase. Phenolic compounds present in the crude extract and its fractions demonstrated antioxidant and antiradical activities as revealed from studies using a β-carotene-linoleate model system, the total antioxidant activity (TAA) method, the DPPH radical-scavenging activity assay, and a reducing power evaluation. Results of these assays showed the highest values when tannins (fraction 2) were tested. For instance, the TAA of the tannin fraction was 5.85 μmol Trolox® eq./mg, whereas the crude extract and fraction 1 showed 0.68 and 0.33 μmol Trolox® eq./mg, respectively. The content of total phenolics in fraction 2 was the highest (290 mg/g); the tannin content, determined using the vanillin method and expressed as absorbance units at 500 nm per 1 g, was 129. There were 24 compounds identified in the crude extract using an HPLC-ESI-MS method: quercetin diglycoside, catechin, digallate procyanidin, and p-hydroxybenzoic were the dominant phenolics in the extract. PMID:20054484

High-throughput and selective solid-phase extraction of urinary catecholamines by crown ether-modified resin composite fiber.

PubMed

Chen, LiQin; Wang, Hui; Xu, Zhen; Zhang, QiuYue; Liu, Jia; Shen, Jun; Zhang, WanQi

2018-08-03

In the present study, we developed a simple and high-throughput solid phase extraction (SPE) procedure for selective extraction of catecholamines (CAs) in urine samples. The SPE adsorbents were electrospun composite fibers functionalized with 4-carboxybenzo-18-crown-6 ether modified XAD resin and polystyrene, which were packed into 96-well columns and used for high-throughput selective extraction of CAs in healthy human urine samples. Moreover, the extraction efficiency of packed-fiber SPE (PFSPE) was examined by high performance liquid chromatography coupled with fluorescence detector. The parameters affecting the extraction efficiency and impurity removal efficiency were optimized, and good linearity ranging from 0.5 to 400 ng/mL was obtained with a low limit of detection (LOD, 0.2-0.5 ng/mL) and a good repeatability (2.7%-3.7%, n = 6). The extraction recoveries of three CAs ranged from 70.5% to 119.5%. Furthermore, stable and reliable results obtained by the fluorescence detector were superior to those obtained by the electrochemical detector. Collectively, PFSPE coupled with 96-well columns was a simple, rapid, selective, high-throughput and cost-efficient method, and the proposed method could be applied in clinical chemistry. Copyright © 2018 Elsevier B.V. All rights reserved.

Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods.

PubMed

Kostić, Nađa; Dotsikas, Yannis; Jović, Nebojša; Stevanović, Galina; Malenović, Anđelija; Medenica, Mirjana

2015-05-10

In this paper, novel LC-MS/MS methods for the determination of antiepileptic drug pregabalin in dried matrix spots (DMS) are presented. This attractive technique of sample collection in micro amount was utilized in the form of dried blood spots (DBS) and dried plasma spots (DPS). Following a pre-column derivatization procedure, using n-propyl chloroformate in the presence of n-propanol, and consecutive liquid-liquid extraction, derivatized pregabalin and its internal standard, 4-aminocyclohexanecarboxylic acid, were detected in positive ion mode by applying two SRM transitions per analyte. A YMC-Pack Octyl column (50mm×4.0mm, 3μm particle size) maintained at 30°C, was utilized with running mobile phase composed of acetonitrile: 0.15% formic acid (85:15, v/v). Flow rate was 550μL/min and total run time 2min. Established methods were fully validated over the concentration range of 0.200-20.0μg/mL for DBS and 0.400-40.0μg/mL for DPS, respectively, while specificity, accuracy, precision, recovery, matrix-effect, stability, dilution integrity and spot homogeneity were found within acceptance criteria. Validated methods were applied for the determination of pregabalin levels in dried blood and plasma samples obtained from patients with epilepsy, after per os administration of commercial capsules. Comparison of drug level in blood and plasma, as well as correction steps undertaken in order to overcome hematocrit issue, when analyzing DBS, are also given. Copyright © 2015 Elsevier B.V. All rights reserved.

Changes to the Spectral Extraction Algorithm at the Third COS FUV Lifetime Position

NASA Astrophysics Data System (ADS)

Taylor, Joanna M.; Azalee Bostroem, K.; Debes, John H.; Ely, Justin; Hernandez, Svea; Hodge, Philip E.; Jedrzejewski, Robert I.; Lindsay, Kevin; Lockwood, Sean A.; Massa, Derck; Oliveira, Cristina M.; Penton, Steven V.; Proffitt, Charles R.; Roman-Duval, Julia; Sahnow, David J.; Sana, Hugues; Sonnentrucker, Paule

2015-01-01

Due to the effects of gain sag on flux on the COS FUV microchannel plate detector, the COS FUV spectra will be moved in February 2015 to a pristine location on the detector, from Lifetime Position 2 (LP2) to LP3. The spectra will be shifted in the cross-dispersion (XD) direction by -2.5", about -31 pixels, from the original LP1. In contrast, LP2 was shifted by +3.5", about 41 pixels, from LP1. By reducing the LP3-LP1 separation compared to the LP2-LP1 separation, we achieve maximal spectral resolution at LP3 while preserving more detector area for future lifetime positions. In the current version of the COS boxcar extraction algorithm, flux is summed within a box of fixed height that is larger than the PSF. Bad pixels located anywhere within the extraction box cause the entire column to be discarded. At the new LP3 position the current extraction box will overlap with LP1 regions of low gain (pixels which have lost >5% of their sensitivity). As a result, large portions of spectra will be discarded, even though these flagged pixels will be located in the wings of the profiles and contain a negligible fraction of the total source flux. To avoid unnecessarily discarding columns affected by such pixels, an algorithm is needed that can judge whether the effects of gain-sagged pixels on the extracted flux are significant. The "two-zone" solution adopted for pipeline use was tailored specifically for the COS FUV data characteristics: First, using a library of 1-D spectral centroid ("trace") locations, residual geometric distortions in the XD direction are removed. Next, 2-D template profiles are aligned with the observed spectral image. Encircled energy contours are calculated and an inner zone that contains 80% of the flux is defined, as well as an outer zone that contains 99% of the flux. With this approach, only pixels flagged as bad in the inner 80% zone will cause columns to be discarded while flagged pixels in the outer zones do not affect extraction. Finally, all good columns are summed in the XD direction to obtain a 1-D extracted spectrum. We present examples of the trace and profile libraries that are used in the two-zone extraction and compare the performance of the two-zone and boxcar algorithms.

Anti-diabetic property of Methanol extract of Musa sapientum leaves and its fractions in alloxan-induced diabetic rats.

PubMed

Adewoye, E O; Ige, A O

2013-06-30

Diabetes mellitus is a metabolic disorder resulting from necrosis of β-cell and insulin resistance at the cellular level. Musa sapientum has been shown to possess anti-diabetic properties, however, the mechanism of its action is unknown. The effect of Methanolic extract of Musa sapientum leaves (MEMSL) and its fractions were assessed for in vitro inhibitory activity of α-amylase enzyme, in vivo hypoglycemic properties and liver glycogen content in alloxan-induced diabetic rats. Dried plant powder of Musa sapientum was successively extracted using n-hexane, ethyl acetate, dichloromethane and methanol respectively. The filtrate obtained was evaporated using rotary evaporator and the extract was stored at 4°C until use. The methanolic extract obtained was further fractionated using column chromatography. In vitro alpha amylase inhibitory activity of the methanolic extract at different doses (2.5mg/ml, 5mg/ml, 10mg/ml, 25mg/ml and 50mg/ml) and column fractions (100ug/ml) were assessed and compared with that of acarbose (5mg/ml), a standard oral α-amylase inhibitor. Hypoglycemic activity and liver glycogen content was studied using alloxan -induced diabetic male rats treated with MEMSL (250mg/kg and 500mg/kg), column fractions F2 and F5 (100μg/kg) for 14 days respectively. Results obtained showed a dose -dependent increase in α-amylase inhibitory activity of the methanolic extract at 5, 10, 25 and 50mg/ml exhibiting 29%, 61%, and 72% and 80% inhibitory activities respectively. Column fractions 2 and 5 showed the highest α-amylase inhibitory activity of 79% and 74% respectively. The MEMSL at 250mg/kg and 500mg/kg exhibited 66% and 59% hypoglycemic activities respectively compared with diabetic controls. Fractions 2 and 5 showed 48% and 75% reduction in blood glucose level respectively. Liver glycogen in diabetic animals treated with MEMSL (250mg/kg and 500mg/kg), F2 and F5 were significantly increased (5.5±0.5, 5.9±0.7, 3.6±0.5, 8.0±0.4 mg/100gwt. liver) compared with Diabetic controls (1.2±0.3 mg/100gwt. liver) respectively suggesting an increase in glucose storage or reduction in glycogen breakdown. It seems possible that the anti-diabetic properties in the leaf extract of Musa sapientum and its fractions maybe due to the inhibition of α-amylase, increased storage of glucose as glycogen in the liver and/or reduced breakdown of liver glycogen stores.